# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2002data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Kinoshita, Isamu' 'Nakajo, Kunio' 'Nishioka, Takanori' 'Tanaka, Rika' 'Yano, Toshihiro' _publ_contact_author_name 'Prof Isamu Kinoshita' _publ_contact_author_address ; Molecular Materials Science Osaka City Uviversity 3-3-138 Sugimoto, Sumiyoshi-ku Osaka 558-8585 JAPAN ; _publ_contact_author_email 'ISAMU@SCI.OSAKA-CU.AC.JP' _publ_section_title ; Thia-calix[n]pyridines, synthesis and coordination to Cu(I,II) ions with both N and S donor atoms ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (2000). teXsan. Single Crystal Structure Analysis Software. Version 1.11. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. ; data_[Cu(Py3S3)(CH3CN)](PF6) _database_code_CSD 183863 #--------------------------------------------------------------------------- #-- # CHEMICAL DATA _chemical_formula_sum 'C17 H12 Cu F6 N4 P S3 ' _chemical_formula_moiety 'C17 H12 Cu F6 N4 P S3 ' _chemical_formula_weight 577.00 _chemical_melting_point ? #--------------------------------------------------------------------------- #-- # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c a 21 ' _symmetry_Int_Tables_number 29 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,1/2+z 1/2-x,y,1/2+z 1/2+x,-y,z _cell_length_a 23.748(3) _cell_length_b 12.198(2) _cell_length_c 14.594(1) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4227(1) _cell_formula_units_Z 8 _cell_measurement_reflns_used 4968 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 200.2 #--------------------------------------------------------------------------- #-- _exptl_crystal_description 'Prism' _exptl_crystal_colour 'Colorless' _exptl_crystal_size_max 0.230 _exptl_crystal_size_mid 0.070 _exptl_crystal_size_min 0.050 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.813 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.471 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Jacobson, 1998)' _exptl_absorpt_correction_T_min 0.730 _exptl_absorpt_correction_T_max 0.974 #--------------------------------------------------------------------------- #-- # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.62 _diffrn_reflns_number 32392 _diffrn_reflns_av_R_equivalents 0.099 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.48 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 18 #--------------------------------------------------------------------------- #-- # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 8038 _reflns_number_gt 3820 _reflns_threshold_expression 2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0580 _refine_ls_wR_factor_ref 0.0632 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 8038 _refine_ls_number_parameters 609 _refine_ls_goodness_of_fit_ref 0.923 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.0010P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0050 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack 0.08(1) _refine_diff_density_max 0.44 _refine_diff_density_min -0.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; 'Cu' 'Cu' 0.320 1.265 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'F' 'F' 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'P' 'P' 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #--------------------------------------------------------------------------- #-- # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu(1) Cu 0.37619(4) 0.30651(9) 0.47322(6) 0.0558(3) Uani 1.00 d . . . Cu(2) Cu 0.58090(4) 0.19604(7) 0.20884(6) 0.0446(2) Uani 1.00 d . . . S(1) S 0.3416(1) 0.1795(2) 0.6617(2) 0.0751(8) Uani 1.00 d . . . S(2) S 0.51101(8) 0.3270(2) 0.4547(1) 0.0447(6) Uani 1.00 d . . . S(3) S 0.31599(9) 0.5459(2) 0.4614(2) 0.0751(9) Uani 1.00 d . . . S(4) S 0.58808(9) 0.4634(2) 0.2015(2) 0.0576(6) Uani 1.00 d . . . S(5) S 0.64765(9) 0.1021(2) 0.3870(2) 0.0559(6) Uani 1.00 d . . . S(6) S 0.45133(8) 0.1140(1) 0.2070(2) 0.0413(5) Uani 1.00 d . . . P(1) P 0.1659(1) 0.2324(2) 0.4887(2) 0.0463(6) Uani 1.00 d . . . P(2) P 0.1773(2) -0.2228(3) 0.7492(2) 0.0813(10) Uani 1.00 d . . . F(1) F 0.2092(2) 0.3041(5) 0.4344(3) 0.099(2) Uani 1.00 d . . . F(2) F 0.1999(5) 0.214(1) 0.5829(8) 0.098(4) Uani 0.61 d P . . F(3) F 0.1854(7) 0.1266(9) 0.4420(9) 0.112(6) Uani 0.61 d P . . F(4) F 0.1268(5) 0.266(1) 0.4013(7) 0.084(4) Uani 0.61 d P . . F(5) F 0.1468(7) 0.3513(8) 0.5350(8) 0.090(5) Uani 0.61 d P . . F(6) F 0.1219(3) 0.1665(5) 0.5448(4) 0.147(3) Uani 1.00 d . . . F(7) F 0.2317(3) -0.1657(8) 0.739(1) 0.295(7) Uani 1.00 d . . . F(8) F 0.2163(5) -0.3106(9) 0.7982(6) 0.249(5) Uani 1.00 d . . . F(9) F 0.1839(6) -0.2851(9) 0.6589(5) 0.286(7) Uani 1.00 d . . . F(10) F 0.1585(4) -0.1694(6) 0.8386(4) 0.199(5) Uani 1.00 d . . . F(11) F 0.1459(2) -0.1334(4) 0.6929(5) 0.130(3) Uani 1.00 d . . . F(12) F 0.1322(4) -0.3090(6) 0.7620(6) 0.201(4) Uani 1.00 d . . . F(13) F 0.1874(8) 0.294(2) 0.574(1) 0.098(4) Uani 0.39 d P . . F(14) F 0.1162(6) 0.300(2) 0.480(2) 0.099(8) Uani 0.39 d P . . F(15) F 0.1496(9) 0.157(2) 0.403(1) 0.085(7) Uani 0.39 d P . . F(16) F 0.2237(6) 0.154(1) 0.505(1) 0.085(6) Uani 0.39 d P . . N(1) N 0.4315(3) 0.2487(5) 0.5684(4) 0.045(2) Uani 1.00 d . . . N(2) N 0.4171(2) 0.4514(5) 0.4573(4) 0.037(1) Uani 1.00 d . . . N(3) N 0.3230(2) 0.3695(7) 0.5701(5) 0.052(2) Uani 1.00 d . . . N(4) N 0.3416(3) 0.2146(6) 0.3862(5) 0.057(2) Uani 1.00 d . . . N(5) N 0.6232(3) 0.2939(6) 0.3037(4) 0.042(2) Uani 1.00 d . . . N(6) N 0.5451(3) 0.0986(5) 0.3084(4) 0.036(2) Uani 1.00 d . . . N(7) N 0.5139(2) 0.2994(4) 0.2032(4) 0.032(1) Uani 1.00 d . . . N(8) N 0.6309(3) 0.1348(6) 0.1190(4) 0.047(2) Uani 1.00 d . . . C(1) C 0.4149(3) 0.2038(7) 0.6485(6) 0.055(2) Uani 1.00 d . . . C(2) C 0.4505(4) 0.1770(6) 0.7210(6) 0.054(2) Uani 1.00 d . . . C(3) C 0.5081(4) 0.1889(7) 0.7028(7) 0.061(2) Uani 1.00 d . . . C(4) C 0.5275(3) 0.2382(6) 0.6262(6) 0.043(2) Uani 1.00 d . . . C(5) C 0.4883(3) 0.2660(6) 0.5595(5) 0.036(2) Uani 1.00 d . . . C(6) C 0.4742(3) 0.4532(6) 0.4600(5) 0.037(2) Uani 1.00 d . . . C(7) C 0.5056(3) 0.5488(7) 0.4626(6) 0.045(2) Uani 1.00 d . . . C(8) C 0.4768(4) 0.6480(7) 0.4603(6) 0.059(3) Uani 1.00 d . . . C(9) C 0.4192(4) 0.6457(7) 0.4623(6) 0.063(3) Uani 1.00 d . . . C(10) C 0.3904(3) 0.5474(7) 0.4615(5) 0.047(2) Uani 1.00 d . . . C(11) C 0.3020(3) 0.4681(9) 0.5645(6) 0.060(3) Uani 1.00 d . . . C(12) C 0.2689(4) 0.5183(10) 0.6282(7) 0.087(4) Uani 1.00 d . . . C(13) C 0.2573(4) 0.4613(10) 0.7064(8) 0.078(3) Uani 1.00 d . . . C(14) C 0.2799(3) 0.3582(8) 0.7196(6) 0.068(3) Uani 1.00 d . . . C(15) C 0.3131(3) 0.3131(8) 0.6499(6) 0.065(3) Uani 1.00 d . . . C(16) C 0.2879(4) 0.0922(7) 0.2735(6) 0.070(3) Uani 1.00 d . . . C(17) C 0.3167(3) 0.1575(7) 0.3419(6) 0.045(2) Uani 1.00 d . . . C(18) C 0.6200(3) 0.4042(7) 0.2996(5) 0.044(2) Uani 1.00 d . . . C(19) C 0.6422(3) 0.4703(6) 0.3680(5) 0.045(2) Uani 1.00 d . . . C(20) C 0.6682(3) 0.4241(8) 0.4411(5) 0.053(3) Uani 1.00 d . . . C(21) C 0.6692(3) 0.3084(8) 0.4492(5) 0.052(2) Uani 1.00 d . . . C(22) C 0.6462(3) 0.2476(7) 0.3789(6) 0.048(2) Uani 1.00 d . . . C(23) C 0.5741(3) 0.0719(5) 0.3834(5) 0.038(2) Uani 1.00 d . . . C(24) C 0.5505(4) 0.0224(6) 0.4596(6) 0.045(2) Uani 1.00 d . . . C(25) C 0.4940(4) -0.0053(7) 0.4537(6) 0.047(2) Uani 1.00 d . . . C(26) C 0.4627(3) 0.0254(6) 0.3780(6) 0.044(2) Uani 1.00 d . . . C(27) C 0.4899(3) 0.0776(5) 0.3061(4) 0.031(2) Uani 1.00 d . . . C(28) C 0.4606(3) 0.2602(5) 0.2080(5) 0.033(2) Uani 1.00 d . . . C(29) C 0.4135(3) 0.3247(6) 0.2096(6) 0.040(2) Uani 1.00 d . . . C(30) C 0.4210(4) 0.4373(6) 0.2132(6) 0.049(2) Uani 1.00 d . . . C(31) C 0.4735(4) 0.4791(6) 0.2137(6) 0.051(2) Uani 1.00 d . . . C(32) C 0.5187(3) 0.4106(5) 0.2096(5) 0.036(2) Uani 1.00 d . . . C(33) C 0.7162(4) 0.0656(7) 0.0291(6) 0.073(3) Uani 1.00 d . . . C(34) C 0.6676(3) 0.1067(6) 0.0782(6) 0.041(2) Uani 1.00 d . . . H(1) H 0.4385 0.1465 0.7752 0.0798 Uiso 1.00 calc . . . H(2) H 0.5340 0.1629 0.7489 0.0711 Uiso 1.00 calc . . . H(3) H 0.5675 0.2507 0.6148 0.0623 Uiso 1.00 calc . . . H(4) H 0.5461 0.5430 0.4683 0.0463 Uiso 1.00 calc . . . H(5) H 0.4980 0.7175 0.4516 0.0663 Uiso 1.00 calc . . . H(6) H 0.3991 0.7140 0.4708 0.0916 Uiso 1.00 calc . . . H(7) H 0.2537 0.5899 0.6248 0.1121 Uiso 1.00 calc . . . H(8) H 0.2360 0.4815 0.7592 0.1087 Uiso 1.00 calc . . . H(9) H 0.2747 0.3106 0.7752 0.0915 Uiso 1.00 calc . . . H(10) H 0.2590 0.0477 0.3054 0.0919 Uiso 1.00 calc . . . H(11) H 0.2697 0.1344 0.2296 0.0919 Uiso 1.00 calc . . . H(12) H 0.3131 0.0414 0.2462 0.0919 Uiso 1.00 calc . . . H(13) H 0.6383 0.5516 0.3616 0.0681 Uiso 1.00 calc . . . H(14) H 0.6848 0.4705 0.4869 0.0721 Uiso 1.00 calc . . . H(15) H 0.6879 0.2705 0.4990 0.0743 Uiso 1.00 calc . . . H(16) H 0.5707 0.0057 0.5155 0.0580 Uiso 1.00 calc . . . H(17) H 0.4791 -0.0466 0.5035 0.0616 Uiso 1.00 calc . . . H(18) H 0.4221 0.0129 0.3802 0.0603 Uiso 1.00 calc . . . H(19) H 0.3750 0.2939 0.2083 0.0618 Uiso 1.00 calc . . . H(20) H 0.3891 0.4865 0.2138 0.0740 Uiso 1.00 calc . . . H(21) H 0.4785 0.5577 0.2193 0.0629 Uiso 1.00 calc . . . H(22) H 0.7204 -0.0105 0.0346 0.0907 Uiso 1.00 calc . . . H(23) H 0.7104 0.0814 -0.0371 0.0907 Uiso 1.00 calc . . . H(24) H 0.7501 0.1020 0.0456 0.0907 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cu(1) 0.0403(6) 0.0831(9) 0.0439(6) -0.0109(6) 0.0021(5) -0.0214(7) Cu(2) 0.0450(6) 0.0507(6) 0.0380(6) -0.0040(6) 0.0102(5) -0.0119(6) S(1) 0.066(2) 0.078(2) 0.081(2) -0.035(2) 0.028(1) -0.015(2) S(2) 0.041(1) 0.050(1) 0.044(1) 0.005(1) 0.011(1) -0.001(1) S(3) 0.046(1) 0.124(3) 0.056(2) 0.035(2) -0.011(1) -0.007(2) S(4) 0.081(2) 0.048(1) 0.044(1) -0.032(1) 0.007(1) 0.005(1) S(5) 0.039(1) 0.057(2) 0.072(2) 0.012(1) -0.015(1) -0.005(1) S(6) 0.045(1) 0.035(1) 0.044(1) -0.004(1) -0.010(1) -0.003(1) P(1) 0.050(1) 0.052(2) 0.037(1) -0.010(1) 0.003(1) 0.003(1) P(2) 0.115(3) 0.065(2) 0.064(2) -0.003(2) -0.019(2) -0.001(2) F(1) 0.096(4) 0.091(4) 0.110(5) -0.028(4) 0.044(3) 0.019(4) F(2) 0.086(7) 0.14(1) 0.071(5) 0.007(9) -0.047(5) 0.035(9) F(3) 0.20(2) 0.052(7) 0.08(1) 0.05(1) 0.035(10) -0.021(8) F(4) 0.078(7) 0.098(10) 0.075(8) 0.000(7) -0.022(6) -0.001(7) F(5) 0.16(1) 0.057(7) 0.058(7) -0.007(7) 0.030(7) -0.018(5) F(6) 0.210(8) 0.117(5) 0.112(5) -0.118(6) 0.098(5) -0.042(4) F(7) 0.062(5) 0.23(1) 0.59(2) -0.010(6) -0.050(9) 0.08(1) F(8) 0.28(1) 0.30(1) 0.160(8) 0.06(1) -0.121(8) 0.070(9) F(9) 0.52(2) 0.24(1) 0.091(6) 0.24(1) -0.051(9) -0.054(7) F(10) 0.39(1) 0.116(6) 0.093(6) -0.003(8) 0.099(7) -0.041(4) F(11) 0.142(6) 0.066(4) 0.182(7) -0.003(4) -0.074(5) 0.034(5) F(12) 0.253(10) 0.142(7) 0.210(9) -0.148(8) -0.105(8) 0.084(6) F(13) 0.086(7) 0.14(1) 0.071(5) 0.007(9) -0.047(5) 0.035(9) F(14) 0.045(10) 0.12(2) 0.13(2) 0.06(1) 0.03(1) 0.06(2) F(15) 0.13(2) 0.09(2) 0.032(10) -0.03(1) -0.018(9) -0.02(1) F(16) 0.07(1) 0.09(1) 0.10(2) 0.036(9) 0.025(9) 0.03(1) N(1) 0.053(5) 0.039(4) 0.044(5) -0.016(4) 0.013(3) -0.016(3) N(2) 0.028(3) 0.052(4) 0.032(4) 0.005(3) -0.003(3) -0.002(3) N(3) 0.017(4) 0.090(6) 0.050(5) -0.003(4) -0.005(3) -0.021(5) N(4) 0.039(4) 0.076(6) 0.057(5) -0.004(4) -0.009(4) -0.006(5) N(5) 0.035(4) 0.042(4) 0.049(5) -0.003(4) 0.005(3) -0.010(4) N(6) 0.037(4) 0.039(4) 0.033(4) 0.004(4) -0.002(3) -0.007(3) N(7) 0.044(4) 0.029(3) 0.025(3) -0.004(3) 0.002(3) -0.006(3) N(8) 0.039(4) 0.060(5) 0.040(4) 0.001(4) 0.008(3) 0.001(4) C(1) 0.044(5) 0.060(6) 0.060(6) -0.010(5) 0.013(5) -0.002(5) C(2) 0.077(6) 0.031(5) 0.053(6) -0.004(5) 0.007(6) 0.011(5) C(3) 0.076(6) 0.047(5) 0.059(6) 0.018(5) -0.009(6) 0.022(5) C(4) 0.051(5) 0.026(5) 0.051(6) 0.004(4) -0.003(4) 0.000(4) C(5) 0.039(5) 0.032(5) 0.038(5) -0.004(4) 0.006(4) 0.000(4) C(6) 0.038(5) 0.052(5) 0.022(4) 0.005(4) 0.006(4) 0.002(4) C(7) 0.031(4) 0.051(5) 0.053(5) -0.005(4) 0.007(4) -0.005(5) C(8) 0.077(7) 0.048(6) 0.051(6) -0.010(6) 0.017(6) 0.015(5) C(9) 0.083(7) 0.054(6) 0.051(6) 0.020(6) -0.028(7) 0.001(5) C(10) 0.051(5) 0.062(6) 0.029(5) 0.020(5) -0.023(4) -0.007(5) C(11) 0.020(5) 0.104(8) 0.057(7) 0.014(6) -0.013(4) -0.023(6) C(12) 0.029(5) 0.16(1) 0.074(8) 0.029(7) -0.019(5) -0.038(8) C(13) 0.028(5) 0.14(1) 0.064(7) -0.006(7) 0.006(6) -0.057(9) C(14) 0.040(5) 0.119(9) 0.046(7) -0.036(6) 0.024(5) -0.042(7) C(15) 0.035(5) 0.113(9) 0.048(6) -0.043(6) 0.008(4) -0.028(6) C(16) 0.066(6) 0.058(6) 0.087(7) -0.001(6) -0.042(5) -0.027(5) C(17) 0.019(5) 0.055(6) 0.061(7) 0.018(5) -0.004(4) 0.001(5) C(18) 0.030(5) 0.053(6) 0.049(6) -0.004(5) 0.010(4) -0.004(5) C(19) 0.043(5) 0.054(6) 0.038(5) -0.029(5) 0.006(4) -0.025(5) C(20) 0.049(6) 0.071(7) 0.038(6) -0.011(6) -0.003(4) -0.027(5) C(21) 0.027(4) 0.078(7) 0.052(6) 0.000(5) -0.013(4) -0.007(5) C(22) 0.027(5) 0.069(7) 0.048(6) 0.011(5) 0.008(4) 0.004(5) C(23) 0.045(5) 0.030(4) 0.039(5) 0.008(4) 0.003(4) -0.004(4) C(24) 0.067(6) 0.038(5) 0.030(5) 0.015(5) -0.003(5) 0.008(4) C(25) 0.074(6) 0.029(4) 0.037(5) 0.003(5) 0.010(5) 0.010(4) C(26) 0.038(5) 0.036(5) 0.059(6) 0.004(4) 0.001(5) 0.002(4) C(27) 0.044(5) 0.027(5) 0.023(4) -0.001(4) 0.002(4) -0.004(3) C(28) 0.056(5) 0.028(4) 0.015(4) 0.005(4) -0.007(4) 0.002(4) C(29) 0.041(4) 0.040(4) 0.039(4) 0.002(4) -0.007(4) -0.010(5) C(30) 0.057(5) 0.043(5) 0.047(5) 0.011(5) -0.011(5) 0.007(5) C(31) 0.091(7) 0.021(4) 0.040(5) 0.003(5) -0.008(6) 0.015(5) C(32) 0.057(5) 0.030(4) 0.022(4) -0.021(4) -0.003(4) 0.019(4) C(33) 0.068(6) 0.082(8) 0.069(7) -0.003(6) 0.029(5) -0.029(6) C(34) 0.039(5) 0.038(5) 0.047(6) -0.006(5) 0.000(4) -0.004(4) #--------------------------------------------------------------------------- #-- _computing_data_collection 'CRYSTALCLEAR' _computing_cell_refinement 'CRYSTALCLEAR' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL97' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #--------------------------------------------------------------------------- #-- _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu(1) N(1) 2.037(6) . . yes Cu(1) N(2) 2.030(6) . . yes Cu(1) N(3) 2.046(7) . . yes Cu(1) N(4) 1.883(7) . . yes Cu(2) N(5) 2.086(6) . . yes Cu(2) N(6) 2.061(6) . . yes Cu(2) N(7) 2.032(5) . . yes Cu(2) N(8) 1.920(6) . . yes S(1) C(1) 1.776(8) . . yes S(1) C(15) 1.77(1) . . yes S(2) C(5) 1.784(7) . . yes S(2) C(6) 1.773(8) . . yes S(3) C(10) 1.767(7) . . yes S(3) C(11) 1.810(10) . . yes S(4) C(18) 1.774(8) . . yes S(4) C(32) 1.774(7) . . yes S(5) C(22) 1.779(9) . . yes S(5) C(23) 1.786(7) . . yes S(6) C(27) 1.769(7) . . yes S(6) C(28) 1.797(6) . . yes P(1) F(1) 1.564(6) . . yes P(1) F(2) 1.61(1) . . yes P(1) F(3) 1.53(1) . . yes P(1) F(4) 1.63(1) . . yes P(1) F(5) 1.66(1) . . yes P(1) F(6) 1.553(7) . . yes P(1) F(13) 1.54(2) . . yes P(1) F(14) 1.45(2) . . yes P(1) F(15) 1.59(2) . . yes P(1) F(16) 1.69(2) . . yes P(2) F(7) 1.474(8) . . yes P(2) F(8) 1.59(1) . . yes P(2) F(9) 1.530(9) . . yes P(2) F(10) 1.524(7) . . yes P(2) F(11) 1.556(6) . . yes P(2) F(12) 1.512(9) . . yes F(2) F(13) 1.03(3) . . yes F(2) F(16) 1.47(2) . . yes F(3) F(15) 1.09(3) . . yes F(3) F(16) 1.33(2) . . yes F(4) F(14) 1.24(3) . . yes F(4) F(15) 1.44(2) . . yes F(5) F(13) 1.32(2) . . yes F(5) F(14) 1.25(2) . . yes N(1) C(1) 1.35(1) . . yes N(1) C(5) 1.37(1) . . yes N(2) C(6) 1.356(9) . . yes N(2) C(10) 1.33(1) . . yes N(3) C(11) 1.30(1) . . yes N(3) C(15) 1.37(1) . . yes N(4) C(17) 1.12(1) . . yes N(5) C(18) 1.35(1) . . yes N(5) C(22) 1.35(1) . . yes N(6) C(23) 1.333(10) . . yes N(6) C(27) 1.335(10) . . yes N(7) C(28) 1.354(9) . . yes N(7) C(32) 1.364(8) . . yes N(8) C(34) 1.11(1) . . yes C(1) C(2) 1.39(1) . . yes C(2) C(3) 1.40(1) . . yes C(3) C(4) 1.35(1) . . yes C(4) C(5) 1.39(1) . . yes C(6) C(7) 1.39(1) . . yes C(7) C(8) 1.39(1) . . yes C(8) C(9) 1.37(1) . . yes C(9) C(10) 1.38(1) . . yes C(11) C(12) 1.36(1) . . yes C(12) C(13) 1.36(2) . . yes C(13) C(14) 1.38(1) . . yes C(14) C(15) 1.40(1) . . yes C(16) C(17) 1.45(1) . . yes C(18) C(19) 1.39(1) . . yes C(19) C(20) 1.36(1) . . yes C(20) C(21) 1.42(1) . . yes C(21) C(22) 1.38(1) . . yes C(23) C(24) 1.38(1) . . yes C(24) C(25) 1.39(1) . . yes C(25) C(26) 1.38(1) . . yes C(26) C(27) 1.39(1) . . yes C(28) C(29) 1.368(10) . . yes C(29) C(30) 1.386(10) . . yes C(30) C(31) 1.35(1) . . yes C(31) C(32) 1.36(1) . . yes C(33) C(34) 1.45(1) . . yes #--------------------------------------------------------------------------- #-- loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(1) Cu(1) N(2) 94.1(2) . . . yes N(1) Cu(1) N(3) 93.3(3) . . . yes N(1) Cu(1) N(4) 122.3(3) . . . yes N(2) Cu(1) N(3) 92.7(3) . . . yes N(2) Cu(1) N(4) 130.5(3) . . . yes N(3) Cu(1) N(4) 114.9(3) . . . yes N(5) Cu(2) N(6) 93.5(2) . . . yes N(5) Cu(2) N(7) 92.8(2) . . . yes N(5) Cu(2) N(8) 112.2(3) . . . yes N(6) Cu(2) N(7) 93.6(2) . . . yes N(6) Cu(2) N(8) 120.8(3) . . . yes N(7) Cu(2) N(8) 134.3(3) . . . yes C(1) S(1) C(15) 102.2(4) . . . yes C(5) S(2) C(6) 100.1(3) . . . yes C(10) S(3) C(11) 100.8(4) . . . yes C(18) S(4) C(32) 101.3(3) . . . yes C(22) S(5) C(23) 100.7(3) . . . yes C(27) S(6) C(28) 100.3(3) . . . yes F(1) P(1) F(2) 100.5(5) . . . yes F(1) P(1) F(3) 92.8(6) . . . yes F(1) P(1) F(4) 80.5(5) . . . yes F(1) P(1) F(5) 84.1(5) . . . yes F(1) P(1) F(6) 177.1(3) . . . yes F(1) P(1) F(13) 85.2(8) . . . yes F(1) P(1) F(14) 99.8(8) . . . yes F(1) P(1) F(15) 94.9(7) . . . yes F(1) P(1) F(16) 81.4(6) . . . yes F(2) P(1) F(3) 96.5(7) . . . yes F(2) P(1) F(4) 171.2(6) . . . yes F(2) P(1) F(5) 84.9(6) . . . yes F(2) P(1) F(6) 79.3(5) . . . yes F(2) P(1) F(13) 38.2(10) . . . yes F(2) P(1) F(14) 124(1) . . . yes F(2) P(1) F(15) 135.2(9) . . . yes F(2) P(1) F(16) 52.9(8) . . . yes F(3) P(1) F(4) 92.2(7) . . . yes F(3) P(1) F(5) 176.8(7) . . . yes F(3) P(1) F(6) 90.1(6) . . . yes F(3) P(1) F(13) 132.3(10) . . . yes F(3) P(1) F(14) 133(1) . . . yes F(3) P(1) F(15) 40.6(10) . . . yes F(3) P(1) F(16) 48.7(9) . . . yes F(4) P(1) F(5) 86.6(6) . . . yes F(4) P(1) F(6) 99.2(5) . . . yes F(4) P(1) F(13) 133.9(10) . . . yes F(4) P(1) F(14) 47(1) . . . yes F(4) P(1) F(15) 52.9(9) . . . yes F(4) P(1) F(16) 135.6(8) . . . yes F(5) P(1) F(6) 93.0(5) . . . yes F(5) P(1) F(13) 48.3(9) . . . yes F(5) P(1) F(14) 46.7(10) . . . yes F(5) P(1) F(15) 138.8(9) . . . yes F(5) P(1) F(16) 131.2(8) . . . yes F(6) P(1) F(13) 93.0(8) . . . yes F(6) P(1) F(14) 78.1(9) . . . yes F(6) P(1) F(15) 87.2(8) . . . yes F(6) P(1) F(16) 100.6(6) . . . yes F(13) P(1) F(14) 93(1) . . . yes F(13) P(1) F(15) 172(1) . . . yes F(13) P(1) F(16) 84(1) . . . yes F(14) P(1) F(15) 93(1) . . . yes F(14) P(1) F(16) 177(1) . . . yes F(15) P(1) F(16) 88(1) . . . yes F(7) P(2) F(8) 81.5(6) . . . yes F(7) P(2) F(9) 93.4(8) . . . yes F(7) P(2) F(10) 98.1(7) . . . yes F(7) P(2) F(11) 92.1(5) . . . yes F(7) P(2) F(12) 163.9(5) . . . yes F(8) P(2) F(9) 89.6(6) . . . yes F(8) P(2) F(10) 94.3(5) . . . yes F(8) P(2) F(11) 172.4(5) . . . yes F(8) P(2) F(12) 83.6(5) . . . yes F(9) P(2) F(10) 168.3(7) . . . yes F(9) P(2) F(11) 86.6(5) . . . yes F(9) P(2) F(12) 80.4(6) . . . yes F(10) P(2) F(11) 90.7(4) . . . yes F(10) P(2) F(12) 89.1(5) . . . yes F(11) P(2) F(12) 102.3(4) . . . yes P(1) F(2) F(13) 67(1) . . . yes P(1) F(2) F(16) 66.3(8) . . . yes F(13) F(2) F(16) 118(1) . . . yes P(1) F(3) F(15) 72(1) . . . yes P(1) F(3) F(16) 71.8(9) . . . yes F(15) F(3) F(16) 143(1) . . . yes P(1) F(4) F(14) 58.6(9) . . . yes P(1) F(4) F(15) 62.2(8) . . . yes F(14) F(4) F(15) 111(1) . . . yes P(1) F(5) F(13) 60(1) . . . yes P(1) F(5) F(14) 57.5(9) . . . yes F(13) F(5) F(14) 116(1) . . . yes P(1) F(13) F(2) 74(1) . . . yes P(1) F(13) F(5) 70(1) . . . yes F(2) F(13) F(5) 140(2) . . . yes P(1) F(14) F(4) 74(1) . . . yes P(1) F(14) F(5) 75(1) . . . yes F(4) F(14) F(5) 129(1) . . . yes P(1) F(15) F(3) 66(1) . . . yes P(1) F(15) F(4) 64.9(9) . . . yes F(3) F(15) F(4) 128(1) . . . yes P(1) F(16) F(2) 60.8(7) . . . yes P(1) F(16) F(3) 59.6(8) . . . yes F(2) F(16) F(3) 113(1) . . . yes Cu(1) N(1) C(1) 122.9(5) . . . yes Cu(1) N(1) C(5) 121.1(5) . . . yes C(1) N(1) C(5) 115.5(6) . . . yes Cu(1) N(2) C(6) 119.3(5) . . . yes Cu(1) N(2) C(10) 122.1(5) . . . yes C(6) N(2) C(10) 117.4(6) . . . yes Cu(1) N(3) C(11) 122.6(6) . . . yes Cu(1) N(3) C(15) 120.3(6) . . . yes C(11) N(3) C(15) 116.7(7) . . . yes Cu(1) N(4) C(17) 172.2(7) . . . yes Cu(2) N(5) C(18) 121.0(5) . . . yes Cu(2) N(5) C(22) 119.6(5) . . . yes C(18) N(5) C(22) 118.5(7) . . . yes Cu(2) N(6) C(23) 120.4(5) . . . yes Cu(2) N(6) C(27) 119.9(5) . . . yes C(23) N(6) C(27) 118.7(6) . . . yes Cu(2) N(7) C(28) 120.7(4) . . . yes Cu(2) N(7) C(32) 123.3(4) . . . yes C(28) N(7) C(32) 115.2(5) . . . yes Cu(2) N(8) C(34) 166.5(7) . . . yes S(1) C(1) N(1) 116.6(6) . . . yes S(1) C(1) C(2) 118.2(7) . . . yes N(1) C(1) C(2) 125.2(7) . . . yes C(1) C(2) C(3) 115.1(8) . . . yes C(2) C(3) C(4) 122.4(8) . . . yes C(3) C(4) C(5) 117.5(7) . . . yes S(2) C(5) N(1) 116.3(5) . . . yes S(2) C(5) C(4) 120.0(6) . . . yes N(1) C(5) C(4) 123.7(6) . . . yes S(2) C(6) N(2) 118.5(6) . . . yes S(2) C(6) C(7) 117.8(5) . . . yes N(2) C(6) C(7) 123.6(7) . . . yes C(6) C(7) C(8) 117.8(7) . . . yes C(7) C(8) C(9) 118.3(8) . . . yes C(8) C(9) C(10) 120.8(8) . . . yes S(3) C(10) N(2) 117.8(6) . . . yes S(3) C(10) C(9) 120.3(7) . . . yes N(2) C(10) C(9) 121.9(7) . . . yes S(3) C(11) N(3) 117.7(6) . . . yes S(3) C(11) C(12) 115.9(8) . . . yes N(3) C(11) C(12) 126.3(9) . . . yes C(11) C(12) C(13) 117(1) . . . yes C(12) C(13) C(14) 120.2(10) . . . yes C(13) C(14) C(15) 118.4(9) . . . yes S(1) C(15) N(3) 118.5(6) . . . yes S(1) C(15) C(14) 120.4(7) . . . yes N(3) C(15) C(14) 121.1(9) . . . yes N(4) C(17) C(16) 171.8(9) . . . yes S(4) C(18) N(5) 117.7(5) . . . yes S(4) C(18) C(19) 120.4(6) . . . yes N(5) C(18) C(19) 121.8(7) . . . yes C(18) C(19) C(20) 119.8(8) . . . yes C(19) C(20) C(21) 119.2(8) . . . yes C(20) C(21) C(22) 117.9(7) . . . yes S(5) C(22) N(5) 118.7(6) . . . yes S(5) C(22) C(21) 118.7(7) . . . yes N(5) C(22) C(21) 122.7(8) . . . yes S(5) C(23) N(6) 118.6(5) . . . yes S(5) C(23) C(24) 117.5(6) . . . yes N(6) C(23) C(24) 123.9(7) . . . yes C(23) C(24) C(25) 116.6(7) . . . yes C(24) C(25) C(26) 120.3(8) . . . yes C(25) C(26) C(27) 118.5(7) . . . yes S(6) C(27) N(6) 118.7(5) . . . yes S(6) C(27) C(26) 119.5(6) . . . yes N(6) C(27) C(26) 121.8(6) . . . yes S(6) C(28) N(7) 117.7(5) . . . yes S(6) C(28) C(29) 118.1(5) . . . yes N(7) C(28) C(29) 124.1(6) . . . yes C(28) C(29) C(30) 117.8(7) . . . yes C(29) C(30) C(31) 119.6(7) . . . yes C(30) C(31) C(32) 119.8(7) . . . yes S(4) C(32) N(7) 115.7(5) . . . yes S(4) C(32) C(31) 120.8(5) . . . yes N(7) C(32) C(31) 123.3(6) . . . yes N(8) C(34) C(33) 176.7(9) . . . yes #--------------------------------------------------------------------------- #-- loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cu(1) N(1) C(1) S(1) 8.4(9) . . . . yes Cu(1) N(1) C(1) C(2) -170.6(6) . . . . yes Cu(1) N(1) C(5) S(2) -7.1(7) . . . . yes Cu(1) N(1) C(5) C(4) 173.5(5) . . . . yes Cu(1) N(2) C(6) S(2) 12.2(8) . . . . yes Cu(1) N(2) C(6) C(7) -170.7(6) . . . . yes Cu(1) N(2) C(10) S(3) -10.9(8) . . . . yes Cu(1) N(2) C(10) C(9) 171.6(6) . . . . yes Cu(1) N(3) C(11) S(3) 5.8(9) . . . . yes Cu(1) N(3) C(11) C(12) -176.2(7) . . . . yes Cu(1) N(3) C(15) S(1) -6.2(8) . . . . yes Cu(1) N(3) C(15) C(14) 175.6(6) . . . . yes Cu(1) N(4) C(17) C(16) 155(4) . . . . yes Cu(2) N(5) C(18) S(4) -9.6(8) . . . . yes Cu(2) N(5) C(18) C(19) 172.2(5) . . . . yes Cu(2) N(5) C(22) S(5) 8.1(8) . . . . yes Cu(2) N(5) C(22) C(21) -172.6(6) . . . . yes Cu(2) N(6) C(23) S(5) -10.5(7) . . . . yes Cu(2) N(6) C(23) C(24) 169.1(5) . . . . yes Cu(2) N(6) C(27) S(6) 10.9(7) . . . . yes Cu(2) N(6) C(27) C(26) -171.0(5) . . . . yes Cu(2) N(7) C(28) S(6) -6.5(8) . . . . yes Cu(2) N(7) C(28) C(29) 176.3(6) . . . . yes Cu(2) N(7) C(32) S(4) 11.5(8) . . . . yes Cu(2) N(7) C(32) C(31) -174.2(6) . . . . yes Cu(2) N(8) C(34) C(33) 66(16) . . . . yes S(1) C(1) N(1) C(5) -179.6(5) . . . . yes S(1) C(1) C(2) C(3) 174.4(6) . . . . yes S(1) C(15) N(3) C(11) -179.0(6) . . . . yes S(1) C(15) C(14) C(13) -178.3(7) . . . . yes S(2) C(5) N(1) C(1) -179.2(5) . . . . yes S(2) C(5) C(4) C(3) -177.7(6) . . . . yes S(2) C(6) N(2) C(10) 179.9(5) . . . . yes S(2) C(6) C(7) C(8) 175.7(6) . . . . yes S(3) C(10) N(2) C(6) -178.2(5) . . . . yes S(3) C(10) C(9) C(8) -178.5(7) . . . . yes S(3) C(11) N(3) C(15) 178.4(6) . . . . yes S(3) C(11) C(12) C(13) 179.5(7) . . . . yes S(4) C(18) N(5) C(22) -178.5(5) . . . . yes S(4) C(18) C(19) C(20) -177.7(6) . . . . yes S(4) C(32) N(7) C(28) -179.0(5) . . . . yes S(4) C(32) C(31) C(30) 175.3(7) . . . . yes S(5) C(22) N(5) C(18) 177.2(5) . . . . yes S(5) C(22) C(21) C(20) 179.4(6) . . . . yes S(5) C(23) N(6) C(27) -179.0(5) . . . . yes S(5) C(23) C(24) C(25) -176.9(6) . . . . yes S(6) C(27) N(6) C(23) 179.5(5) . . . . yes S(6) C(27) C(26) C(25) 178.1(6) . . . . yes S(6) C(28) N(7) C(32) -176.3(5) . . . . yes S(6) C(28) C(29) C(30) 178.0(6) . . . . yes P(1) F(2) F(13) F(5) 30(2) . . . . yes P(1) F(2) F(16) F(3) -29(1) . . . . yes P(1) F(3) F(15) F(4) 20(1) . . . . yes P(1) F(3) F(16) F(2) 29(1) . . . . yes P(1) F(4) F(14) F(5) 55(1) . . . . yes P(1) F(4) F(15) F(3) -20(1) . . . . yes P(1) F(5) F(13) F(2) -31(2) . . . . yes P(1) F(5) F(14) F(4) -54(1) . . . . yes P(1) F(13) F(2) F(16) 43(1) . . . . yes P(1) F(13) F(5) F(14) 17(1) . . . . yes P(1) F(14) F(4) F(15) 34(1) . . . . yes P(1) F(14) F(5) F(13) -17(1) . . . . yes P(1) F(15) F(3) F(16) -15(2) . . . . yes P(1) F(15) F(4) F(14) -33(1) . . . . yes P(1) F(16) F(2) F(13) -43(1) . . . . yes P(1) F(16) F(3) F(15) 15(2) . . . . yes F(1) P(1) F(2) F(13) 68(1) . . . . yes F(1) P(1) F(2) F(16) -70.8(8) . . . . yes F(1) P(1) F(3) F(15) -94(1) . . . . yes F(1) P(1) F(3) F(16) 76.0(10) . . . . yes F(1) P(1) F(4) F(14) -112(1) . . . . yes F(1) P(1) F(4) F(15) 103.6(10) . . . . yes F(1) P(1) F(5) F(13) -88(1) . . . . yes F(1) P(1) F(5) F(14) 109(1) . . . . yes F(1) P(1) F(13) F(2) -113(1) . . . . yes F(1) P(1) F(13) F(5) 86.4(9) . . . . yes F(1) P(1) F(14) F(4) 67.2(10) . . . . yes F(1) P(1) F(14) F(5) -72(1) . . . . yes F(1) P(1) F(15) F(3) 88(1) . . . . yes F(1) P(1) F(15) F(4) -74.3(8) . . . . yes F(1) P(1) F(16) F(2) 110.1(8) . . . . yes F(1) P(1) F(16) F(3) -101.4(9) . . . . yes F(2) P(1) F(3) F(15) 164(1) . . . . yes F(2) P(1) F(3) F(16) -24(1) . . . . yes F(2) P(1) F(4) F(14) -15(4) . . . . yes F(2) P(1) F(4) F(15) -159(4) . . . . yes F(2) P(1) F(5) F(13) 12(1) . . . . yes F(2) P(1) F(5) F(14) -149(1) . . . . yes F(2) P(1) F(13) F(5) -159(1) . . . . yes F(2) P(1) F(14) F(4) 177.1(9) . . . . yes F(2) P(1) F(14) F(5) 37(1) . . . . yes F(2) P(1) F(15) F(3) -21(1) . . . . yes F(2) P(1) F(15) F(4) 175.6(8) . . . . yes F(2) P(1) F(16) F(3) 148(1) . . . . yes F(2) F(13) P(1) F(3) -24(1) . . . . yes F(2) F(13) P(1) F(4) 174.4(9) . . . . yes F(2) F(13) P(1) F(5) 159(1) . . . . yes F(2) F(13) P(1) F(6) 68(1) . . . . yes F(2) F(13) P(1) F(14) 146(1) . . . . yes F(2) F(13) P(1) F(15) -22(9) . . . . yes F(2) F(13) P(1) F(16) -31(1) . . . . yes F(2) F(13) F(5) F(14) -14(3) . . . . yes F(2) F(16) P(1) F(3) -148(1) . . . . yes F(2) F(16) P(1) F(4) 177.1(9) . . . . yes F(2) F(16) P(1) F(5) 35(1) . . . . yes F(2) F(16) P(1) F(6) -67.8(8) . . . . yes F(2) F(16) P(1) F(13) 24(1) . . . . yes F(2) F(16) P(1) F(14) -7(19) . . . . yes F(2) F(16) P(1) F(15) -154(1) . . . . yes F(2) F(16) F(3) F(15) 45(3) . . . . yes F(3) P(1) F(2) F(13) 162(1) . . . . yes F(3) P(1) F(2) F(16) 23.3(10) . . . . yes F(3) P(1) F(4) F(14) 154(1) . . . . yes F(3) P(1) F(4) F(15) 11(1) . . . . yes F(3) P(1) F(5) F(13) -102(14) . . . . yes F(3) P(1) F(5) F(14) 95(14) . . . . yes F(3) P(1) F(13) F(5) 175.8(10) . . . . yes F(3) P(1) F(14) F(4) -36(1) . . . . yes F(3) P(1) F(14) F(5) -175.6(9) . . . . yes F(3) P(1) F(15) F(4) -162(1) . . . . yes F(3) F(15) P(1) F(4) 162(1) . . . . yes F(3) F(15) P(1) F(5) 175(1) . . . . yes F(3) F(15) P(1) F(6) -93(1) . . . . yes F(3) F(15) P(1) F(13) -1(9) . . . . yes F(3) F(15) P(1) F(14) -171(1) . . . . yes F(3) F(15) P(1) F(16) 7(1) . . . . yes F(3) F(15) F(4) F(14) -53(2) . . . . yes F(3) F(16) P(1) F(4) -34(1) . . . . yes F(3) F(16) P(1) F(5) -175.7(9) . . . . yes F(3) F(16) P(1) F(6) 80.7(10) . . . . yes F(3) F(16) P(1) F(13) 172(1) . . . . yes F(3) F(16) P(1) F(14) 141(18) . . . . yes F(3) F(16) P(1) F(15) -6(1) . . . . yes F(3) F(16) F(2) F(13) -73(2) . . . . yes F(4) P(1) F(2) F(13) -27(4) . . . . yes F(4) P(1) F(2) F(16) -166(3) . . . . yes F(4) P(1) F(3) F(15) -13(1) . . . . yes F(4) P(1) F(3) F(16) 156(1) . . . . yes F(4) P(1) F(5) F(13) -169(1) . . . . yes F(4) P(1) F(5) F(14) 28(1) . . . . yes F(4) P(1) F(13) F(5) 14(1) . . . . yes F(4) P(1) F(14) F(5) -139(1) . . . . yes F(4) F(14) P(1) F(5) 139(1) . . . . yes F(4) F(14) P(1) F(6) -114(1) . . . . yes F(4) F(14) P(1) F(13) 152(1) . . . . yes F(4) F(14) P(1) F(15) -28(1) . . . . yes F(4) F(14) P(1) F(16) -176(18) . . . . yes F(4) F(14) F(5) F(13) -72(2) . . . . yes F(4) F(15) P(1) F(5) 12(1) . . . . yes F(4) F(15) P(1) F(6) 103.8(8) . . . . yes F(4) F(15) P(1) F(13) -164(8) . . . . yes F(4) F(15) P(1) F(14) 25(1) . . . . yes F(4) F(15) P(1) F(16) -155.6(10) . . . . yes F(4) F(15) F(3) F(16) 4(4) . . . . yes F(5) P(1) F(2) F(13) -14(1) . . . . yes F(5) P(1) F(2) F(16) -153.8(9) . . . . yes F(5) P(1) F(3) F(15) -80(14) . . . . yes F(5) P(1) F(3) F(16) 89(14) . . . . yes F(5) P(1) F(4) F(14) -28(1) . . . . yes F(5) P(1) F(4) F(15) -171(1) . . . . yes F(5) F(13) P(1) F(6) -91.4(9) . . . . yes F(5) F(13) P(1) F(14) -13(1) . . . . yes F(5) F(13) P(1) F(15) 177(8) . . . . yes F(5) F(13) P(1) F(16) 168(1) . . . . yes F(5) F(13) F(2) F(16) 73(3) . . . . yes F(5) F(14) P(1) F(6) 105(1) . . . . yes F(5) F(14) P(1) F(13) 13(1) . . . . yes F(5) F(14) P(1) F(15) -167(1) . . . . yes F(5) F(14) P(1) F(16) 44(19) . . . . yes F(5) F(14) F(4) F(15) 89(2) . . . . yes F(6) P(1) F(2) F(13) -109(1) . . . . yes F(6) P(1) F(2) F(16) 112.1(8) . . . . yes F(6) P(1) F(3) F(15) 85(1) . . . . yes F(6) P(1) F(3) F(16) -104.1(10) . . . . yes F(6) P(1) F(4) F(14) 64(1) . . . . yes F(6) P(1) F(4) F(15) -79.3(10) . . . . yes F(6) P(1) F(5) F(13) 91(1) . . . . yes F(6) P(1) F(5) F(14) -70(1) . . . . yes F(13) P(1) F(2) F(16) -138(1) . . . . yes F(13) P(1) F(3) F(15) 179(1) . . . . yes F(13) P(1) F(3) F(16) -9(1) . . . . yes F(13) P(1) F(4) F(14) -39(1) . . . . yes F(13) P(1) F(4) F(15) 177(1) . . . . yes F(13) P(1) F(5) F(14) -161(1) . . . . yes F(13) F(2) P(1) F(14) -41(1) . . . . yes F(13) F(2) P(1) F(15) 176(1) . . . . yes F(13) F(2) P(1) F(16) 138(1) . . . . yes F(13) F(5) P(1) F(14) 161(1) . . . . yes F(13) F(5) P(1) F(15) -179(1) . . . . yes F(13) F(5) P(1) F(16) -15(1) . . . . yes F(14) P(1) F(2) F(16) 179(1) . . . . yes F(14) P(1) F(3) F(15) 12(1) . . . . yes F(14) P(1) F(3) F(16) -177(1) . . . . yes F(14) P(1) F(4) F(15) -143(1) . . . . yes F(14) F(4) P(1) F(15) 143(1) . . . . yes F(14) F(4) P(1) F(16) 179(1) . . . . yes F(14) F(5) P(1) F(15) 18(1) . . . . yes F(14) F(5) P(1) F(16) -177(1) . . . . yes F(15) P(1) F(2) F(16) 37(1) . . . . yes F(15) P(1) F(3) F(16) 170(1) . . . . yes F(15) F(3) P(1) F(16) -170(1) . . . . yes F(15) F(4) P(1) F(16) 36(1) . . . . yes N(1) Cu(1) N(2) C(6) 37.2(6) . . . . yes N(1) Cu(1) N(2) C(10) -129.9(6) . . . . yes N(1) Cu(1) N(3) C(11) 133.3(6) . . . . yes N(1) Cu(1) N(3) C(15) -39.1(6) . . . . yes N(1) Cu(1) N(4) C(17) 84(5) . . . . yes N(1) C(1) S(1) C(15) -59.8(7) . . . . yes N(1) C(1) C(2) C(3) -6(1) . . . . yes N(1) C(5) S(2) C(6) 60.6(6) . . . . yes N(1) C(5) C(4) C(3) 1(1) . . . . yes N(2) Cu(1) N(1) C(1) 131.4(6) . . . . yes N(2) Cu(1) N(1) C(5) -40.2(6) . . . . yes N(2) Cu(1) N(3) C(11) 39.1(6) . . . . yes N(2) Cu(1) N(3) C(15) -133.3(6) . . . . yes N(2) Cu(1) N(4) C(17) -145(5) . . . . yes N(2) C(6) S(2) C(5) -64.8(6) . . . . yes N(2) C(6) C(7) C(8) -1(1) . . . . yes N(2) C(10) S(3) C(11) 60.9(7) . . . . yes N(2) C(10) C(9) C(8) -1(1) . . . . yes N(3) Cu(1) N(1) C(1) 38.4(6) . . . . yes N(3) Cu(1) N(1) C(5) -133.2(6) . . . . yes N(3) Cu(1) N(2) C(6) 130.7(6) . . . . yes N(3) Cu(1) N(2) C(10) -36.4(6) . . . . yes N(3) Cu(1) N(4) C(17) -27(5) . . . . yes N(3) C(11) S(3) C(10) -58.1(7) . . . . yes N(3) C(11) C(12) C(13) 1(1) . . . . yes N(3) C(15) S(1) C(1) 58.8(7) . . . . yes N(3) C(15) C(14) C(13) 0(1) . . . . yes N(4) Cu(1) N(1) C(1) -83.9(7) . . . . yes N(4) Cu(1) N(1) C(5) 104.5(6) . . . . yes N(4) Cu(1) N(2) C(6) -102.8(6) . . . . yes N(4) Cu(1) N(2) C(10) 90.1(6) . . . . yes N(4) Cu(1) N(3) C(11) -98.6(7) . . . . yes N(4) Cu(1) N(3) C(15) 89.0(6) . . . . yes N(5) Cu(2) N(6) C(23) -37.3(6) . . . . yes N(5) Cu(2) N(6) C(27) 131.1(5) . . . . yes N(5) Cu(2) N(7) C(28) -133.7(5) . . . . yes N(5) Cu(2) N(7) C(32) 35.3(6) . . . . yes N(5) Cu(2) N(8) C(34) 11(2) . . . . yes N(5) C(18) S(4) C(32) 62.2(6) . . . . yes N(5) C(18) C(19) C(20) 0(1) . . . . yes N(5) C(22) S(5) C(23) -60.7(7) . . . . yes N(5) C(22) C(21) C(20) 0(1) . . . . yes N(6) Cu(2) N(5) C(18) -130.2(6) . . . . yes N(6) Cu(2) N(5) C(22) 38.6(6) . . . . yes N(6) Cu(2) N(7) C(28) -40.0(6) . . . . yes N(6) Cu(2) N(7) C(32) 129.0(6) . . . . yes N(6) Cu(2) N(8) C(34) -97(2) . . . . yes N(6) C(23) S(5) C(22) 62.6(6) . . . . yes N(6) C(23) C(24) C(25) 3(1) . . . . yes N(6) C(27) S(6) C(28) -62.5(6) . . . . yes N(6) C(27) C(26) C(25) 0(1) . . . . yes N(7) Cu(2) N(5) C(18) -36.4(6) . . . . yes N(7) Cu(2) N(5) C(22) 132.4(6) . . . . yes N(7) Cu(2) N(6) C(23) -130.4(5) . . . . yes N(7) Cu(2) N(6) C(27) 38.1(5) . . . . yes N(7) Cu(2) N(8) C(34) 129(2) . . . . yes N(7) C(28) S(6) C(27) 59.9(6) . . . . yes N(7) C(28) C(29) C(30) -4(1) . . . . yes N(7) C(32) S(4) C(18) -63.2(6) . . . . yes N(7) C(32) C(31) C(30) 1(1) . . . . yes N(8) Cu(2) N(5) C(18) 104.4(6) . . . . yes N(8) Cu(2) N(5) C(22) -86.8(6) . . . . yes N(8) Cu(2) N(6) C(23) 81.2(6) . . . . yes N(8) Cu(2) N(6) C(27) -110.4(5) . . . . yes N(8) Cu(2) N(7) C(28) 101.2(6) . . . . yes N(8) Cu(2) N(7) C(32) -89.9(6) . . . . yes C(1) S(1) C(15) C(14) -122.9(7) . . . . yes C(1) N(1) C(5) C(4) 1(1) . . . . yes C(1) C(2) C(3) C(4) 9(1) . . . . yes C(2) C(1) S(1) C(15) 119.3(7) . . . . yes C(2) C(1) N(1) C(5) 1(1) . . . . yes C(2) C(3) C(4) C(5) -7(1) . . . . yes C(4) C(5) S(2) C(6) -119.9(6) . . . . yes C(5) S(2) C(6) C(7) 118.0(6) . . . . yes C(6) N(2) C(10) C(9) 4(1) . . . . yes C(6) C(7) C(8) C(9) 4(1) . . . . yes C(7) C(6) N(2) C(10) -3(1) . . . . yes C(7) C(8) C(9) C(10) -3(1) . . . . yes C(9) C(10) S(3) C(11) -121.6(7) . . . . yes C(10) S(3) C(11) C(12) 123.7(7) . . . . yes C(11) N(3) C(15) C(14) 2(1) . . . . yes C(11) C(12) C(13) C(14) 1(1) . . . . yes C(12) C(11) N(3) C(15) -3(1) . . . . yes C(12) C(13) C(14) C(15) -2(1) . . . . yes C(18) S(4) C(32) C(31) 122.4(7) . . . . yes C(18) N(5) C(22) C(21) -3(1) . . . . yes C(18) C(19) C(20) C(21) -4(1) . . . . yes C(19) C(18) S(4) C(32) -119.5(6) . . . . yes C(19) C(18) N(5) C(22) 3(1) . . . . yes C(19) C(20) C(21) C(22) 3(1) . . . . yes C(21) C(22) S(5) C(23) 120.0(6) . . . . yes C(22) S(5) C(23) C(24) -117.0(6) . . . . yes C(23) N(6) C(27) C(26) -2.4(10) . . . . yes C(23) C(24) C(25) C(26) -5(1) . . . . yes C(24) C(23) N(6) C(27) 0(1) . . . . yes C(24) C(25) C(26) C(27) 4(1) . . . . yes C(26) C(27) S(6) C(28) 119.3(6) . . . . yes C(27) S(6) C(28) C(29) -122.8(6) . . . . yes C(28) N(7) C(32) C(31) -4(1) . . . . yes C(28) C(29) C(30) C(31) 0(1) . . . . yes C(29) C(28) N(7) C(32) 6(1) . . . . yes C(29) C(30) C(31) C(32) 0(1) . . . . yes C(29) C(30) C(31) C(32) 0(1) . . . . yes #--------------------------------------------------------------------------- #-- loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag S(1) F(15) 3.54(2) . 3_555 ? S(3) F(8) 3.054(10) . 3_564 ? S(3) C(20) 3.541(8) . 4_465 ? S(4) C(11) 3.392(9) . 2_664 ? S(4) N(3) 3.506(7) . 2_664 ? S(4) C(10) 3.542(8) . 2_664 ? S(4) C(12) 3.567(9) . 2_664 ? S(5) F(3) 3.04(1) . 4_555 ? S(5) F(15) 3.17(2) . 4_555 ? S(6) F(6) 3.006(7) . 3_554 ? F(1) C(14) 3.21(1) . 3_554 ? F(1) C(19) 3.323(9) . 4_465 ? F(1) C(20) 3.46(1) . 4_465 ? F(2) C(16) 3.17(1) . 3_555 ? F(2) C(29) 3.53(1) . 3_555 ? F(3) C(33) 3.55(2) . 2_655 ? F(4) C(19) 3.27(2) . 4_465 ? F(4) C(2) 3.39(1) . 3_554 ? F(5) C(29) 2.94(1) . 3_555 ? F(5) C(20) 3.11(1) . 4_465 ? F(5) C(30) 3.23(1) . 3_555 ? F(5) C(19) 3.27(1) . 4_465 ? F(6) C(24) 3.12(1) . 4_455 ? F(6) C(29) 3.196(10) . 3_555 ? F(6) C(28) 3.289(10) . 3_555 ? F(7) C(16) 3.22(1) . 3_555 ? F(7) C(34) 3.43(2) . 2_655 ? F(7) C(33) 3.52(2) . 2_655 ? F(8) C(13) 3.24(2) . 1_545 ? F(8) C(12) 3.47(1) . 1_545 ? F(8) C(21) 3.50(1) . 2_655 ? F(8) C(22) 3.55(1) . 2_655 ? F(9) C(21) 3.09(1) . 4_455 ? F(9) C(12) 3.17(2) . 1_545 ? F(10) C(33) 3.35(1) . 4_456 ? F(10) C(9) 3.43(1) . 3_545 ? F(10) C(16) 3.57(1) . 3_555 ? F(10) C(34) 3.59(1) . 4_456 ? F(11) C(4) 3.240(10) . 4_455 ? F(11) C(3) 3.34(1) . 4_455 ? F(11) C(16) 3.382(10) . 3_555 ? F(12) C(9) 3.22(1) . 3_545 ? F(12) C(4) 3.30(1) . 4_455 ? F(12) C(3) 3.40(1) . 4_455 ? F(12) C(30) 3.42(1) . 3_545 ? F(12) C(10) 3.44(1) . 3_545 ? F(13) C(29) 3.13(2) . 3_555 ? F(14) C(7) 3.22(2) . 4_465 ? F(14) C(19) 3.30(2) . 4_465 ? F(14) C(8) 3.38(2) . 4_465 ? F(14) C(29) 3.44(3) . 3_555 ? F(15) C(24) 3.32(2) . 4_455 ? F(15) C(23) 3.33(2) . 4_455 ? F(15) C(2) 3.58(2) . 3_554 ? F(16) C(33) 3.06(2) . 2_655 ? N(6) C(2) 3.598(10) . 2_654 ? C(3) C(27) 3.58(1) . 2_655 ? C(13) C(19) 3.46(1) . 2_665 ? C(14) C(19) 3.54(1) . 2_665 ? #----- #------------------------------------------------------------------------------ data_[Cu(py3s3)]2(PF6)2 _database_code_CSD 183864 #--------------------------------------------------------------------------- #-- # CHEMICAL DATA _chemical_formula_sum 'C17 H13 Cl2 Cu F6 N3 P S3 ' _chemical_formula_moiety '?' _chemical_formula_weight 634.91 _chemical_melting_point ? #--------------------------------------------------------------------------- #-- # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 13.6779(6) _cell_length_b 20.4121(9) _cell_length_c 8.5003(4) _cell_angle_alpha 90 _cell_angle_beta 102.049(2) _cell_angle_gamma 90 _cell_volume 2321.0(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 20671 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 296.2 #--------------------------------------------------------------------------- #-- _exptl_crystal_description 'prism' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.150 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.817 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.570 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.546 _exptl_absorpt_correction_T_max 0.790 #--------------------------------------------------------------------------- #-- # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.00 _diffrn_reflns_number 10353 _diffrn_reflns_av_R_equivalents 0.015 _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 0.9985 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.9985 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 #--------------------------------------------------------------------------- #-- # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 5319 _reflns_number_gt 4258 _reflns_threshold_expression F^2^3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0567 _refine_ls_wR_factor_ref 0.0954 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 4258 _refine_ls_number_parameters 298 _refine_ls_goodness_of_fit_ref 1.848 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00203|Fo|^2^]' _refine_ls_shift/su_max 0.0003 _refine_diff_density_max 1.56 _refine_diff_density_min -1.04 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Cu' 'Cu' 0.320 1.265 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Cl' 'Cl' 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'P' 'P' 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'F' 'F' 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #--------------------------------------------------------------------------- #-- # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu(1) Cu 0.47005(4) -0.43731(2) 0.58920(6) 0.0340(1) Uani 1.00 d . . . Cl(1) Cl 0.4625(3) 0.0458(2) 0.1831(5) 0.162(1) Uani 1.00 d . . . Cl(2) Cl 0.6766(2) 0.0310(1) 0.4525(3) 0.1110(8) Uani 1.00 d . . . S(1) S 0.26038(8) -0.36170(7) 0.4804(2) 0.0490(3) Uani 1.00 d . . . S(2) S 0.62472(8) -0.35612(6) 0.8583(1) 0.0453(3) Uani 1.00 d . . . S(3) S 0.56756(8) -0.47496(5) 0.2840(1) 0.0358(3) Uani 1.00 d . . . P(1) P 0.5613(1) -0.23148(6) 0.2928(2) 0.0473(3) Uani 1.00 d . . . F(1) F 0.561(1) -0.1822(3) 0.1573(9) 0.241(5) Uani 1.00 d . . . F(2) F 0.5443(9) -0.2808(3) 0.4121(8) 0.220(4) Uani 1.00 d . . . F(3) F 0.5332(4) -0.1731(2) 0.3991(5) 0.111(2) Uani 1.00 d . . . F(4) F 0.5916(3) -0.2888(2) 0.1857(5) 0.084(1) Uani 1.00 d . . . F(5) F 0.4556(5) -0.2384(5) 0.206(1) 0.233(4) Uani 1.00 d . . . F(6) F 0.6665(5) -0.2203(6) 0.357(1) 0.256(5) Uani 1.00 d . . . N(1) N 0.4405(3) -0.3468(2) 0.6755(4) 0.0350(8) Uani 1.00 d . . . N(2) N 0.6129(2) -0.4141(2) 0.5710(4) 0.0334(8) Uani 1.00 d . . . N(3) N 0.4053(3) -0.4168(2) 0.3555(4) 0.0345(8) Uani 1.00 d . . . C(1) C 0.3566(3) -0.3149(2) 0.6053(5) 0.039(1) Uani 1.00 d . . . C(2) C 0.3430(4) -0.2488(2) 0.6286(6) 0.051(1) Uani 1.00 d . . . C(3) C 0.4193(5) -0.2145(2) 0.7257(7) 0.060(2) Uani 1.00 d . . . C(4) C 0.5084(4) -0.2455(2) 0.7953(6) 0.052(1) Uani 1.00 d . . . C(5) C 0.5149(3) -0.3119(2) 0.7666(5) 0.0361(10) Uani 1.00 d . . . C(6) C 0.6711(3) -0.3769(2) 0.6820(5) 0.0376(10) Uani 1.00 d . . . C(7) C 0.7649(3) -0.3546(3) 0.6703(6) 0.050(1) Uani 1.00 d . . . C(8) C 0.7970(4) -0.3694(3) 0.5306(7) 0.063(2) Uani 1.00 d . . . C(9) C 0.7349(4) -0.4038(3) 0.4092(6) 0.050(1) Uani 1.00 d . . . C(10) C 0.6451(3) -0.4257(2) 0.4355(5) 0.0343(9) Uani 1.00 d . . . C(11) C 0.4540(3) -0.4282(2) 0.2376(5) 0.0359(10) Uani 1.00 d . . . C(12) C 0.4203(4) -0.4068(3) 0.0814(5) 0.048(1) Uani 1.00 d . . . C(13) C 0.3329(4) -0.3717(3) 0.0452(6) 0.057(1) Uani 1.00 d . . . C(14) C 0.2820(4) -0.3580(3) 0.1665(6) 0.054(1) Uani 1.00 d . . . C(15) C 0.3214(3) -0.3801(2) 0.3195(5) 0.040(1) Uani 1.00 d . . . C(16) C 0.5158(9) -0.0271(5) 0.264(1) 0.128(4) Uani 1.00 d . . . C(17) C 0.6222(9) -0.0278(4) 0.308(2) 0.138(4) Uani 1.00 d . . . H(1) H 0.2824 -0.2278 0.5783 0.0602 Uiso 1.00 calc . . . H(2) H 0.4117 -0.1689 0.7431 0.0716 Uiso 1.00 calc . . . H(3) H 0.5616 -0.2226 0.8597 0.0626 Uiso 1.00 calc . . . H(4) H 0.8060 -0.3301 0.7547 0.0604 Uiso 1.00 calc . . . H(5) H 0.8623 -0.3560 0.5183 0.0744 Uiso 1.00 calc . . . H(6) H 0.7544 -0.4121 0.3085 0.0604 Uiso 1.00 calc . . . H(7) H 0.4573 -0.4165 0.0008 0.0565 Uiso 1.00 calc . . . H(8) H 0.3075 -0.3566 -0.0609 0.0667 Uiso 1.00 calc . . . H(9) H 0.2221 -0.3334 0.1446 0.0658 Uiso 1.00 calc . . . H(10) H 0.4963 -0.0609 0.1927 0.1603 Uiso 1.00 calc . . . H(11) H 0.4935 -0.0348 0.3631 0.1603 Uiso 1.00 calc . . . H(12) H 0.6419 -0.0689 0.3452 0.1865 Uiso 1.00 calc . . . H(13) H 0.6440 -0.0178 0.2109 0.1865 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cu(1) 0.0360(3) 0.0301(3) 0.0358(3) -0.0007(2) 0.0073(2) 0.0008(2) Cl(1) 0.159(3) 0.090(2) 0.203(4) 0.026(2) -0.039(3) 0.007(2) Cl(2) 0.120(2) 0.116(2) 0.095(1) -0.043(2) 0.017(1) -0.005(1) S(1) 0.0297(5) 0.0638(7) 0.0518(6) 0.0046(5) 0.0047(4) -0.0050(5) S(2) 0.0378(6) 0.0593(7) 0.0354(5) 0.0012(5) 0.0000(4) -0.0078(5) S(3) 0.0427(6) 0.0324(5) 0.0344(5) -0.0005(4) 0.0128(4) -0.0027(4) P(1) 0.0528(7) 0.0424(6) 0.0477(6) -0.0027(5) 0.0131(5) 0.0003(5) F(1) 0.56(2) 0.074(4) 0.139(5) 0.015(7) 0.196(9) 0.011(4) F(2) 0.46(2) 0.101(4) 0.161(6) 0.106(6) 0.221(9) 0.065(4) F(3) 0.192(6) 0.060(2) 0.104(3) 0.006(3) 0.087(4) -0.011(2) F(4) 0.106(3) 0.069(2) 0.082(2) 0.011(2) 0.028(2) -0.020(2) F(5) 0.102(4) 0.177(8) 0.36(1) 0.072(5) -0.078(6) -0.092(9) F(6) 0.071(3) 0.33(1) 0.34(1) -0.032(5) -0.002(5) -0.25(1) N(1) 0.039(2) 0.035(2) 0.031(2) 0.000(1) 0.008(1) -0.005(1) N(2) 0.031(2) 0.033(2) 0.036(2) -0.001(1) 0.007(1) 0.001(1) N(3) 0.036(2) 0.033(2) 0.033(2) -0.002(1) 0.004(1) 0.001(1) C(1) 0.040(2) 0.039(2) 0.040(2) 0.007(2) 0.012(2) -0.001(2) C(2) 0.059(3) 0.044(2) 0.054(3) 0.015(2) 0.016(2) 0.002(2) C(3) 0.083(4) 0.038(2) 0.058(3) 0.011(2) 0.016(3) -0.008(2) C(4) 0.065(3) 0.042(2) 0.051(3) -0.004(2) 0.017(2) -0.011(2) C(5) 0.039(2) 0.037(2) 0.034(2) 0.000(2) 0.010(2) -0.003(2) C(6) 0.033(2) 0.039(2) 0.040(2) 0.004(2) 0.005(2) -0.004(2) C(7) 0.033(2) 0.061(3) 0.053(3) -0.009(2) 0.003(2) -0.005(2) C(8) 0.036(3) 0.087(4) 0.070(3) -0.011(3) 0.019(2) -0.012(3) C(9) 0.040(2) 0.058(3) 0.058(3) -0.008(2) 0.022(2) -0.003(2) C(10) 0.036(2) 0.029(2) 0.038(2) 0.001(1) 0.008(2) 0.001(1) C(11) 0.041(2) 0.034(2) 0.032(2) -0.006(2) 0.007(2) -0.001(1) C(12) 0.049(3) 0.053(3) 0.039(2) -0.006(2) 0.004(2) 0.004(2) C(13) 0.058(3) 0.073(3) 0.036(2) 0.001(3) -0.004(2) 0.007(2) C(14) 0.042(3) 0.064(3) 0.050(3) 0.008(2) -0.005(2) 0.001(2) C(15) 0.033(2) 0.042(2) 0.040(2) -0.001(2) -0.001(2) -0.001(2) C(16) 0.142(9) 0.067(5) 0.149(9) 0.002(5) -0.026(8) -0.004(5) C(17) 0.109(7) 0.058(4) 0.23(1) -0.005(5) -0.008(8) -0.029(6) #--------------------------------------------------------------------------- #-- _computing_data_collection 'PROCESS-AUTO' _computing_cell_refinement 'PROCESS-AUTO' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #--------------------------------------------------------------------------- #-- _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu(1) S(3) 2.206(1) . 3_646 yes Cu(1) N(1) 2.058(4) . . yes Cu(1) N(2) 2.048(4) . . yes Cu(1) N(3) 2.042(3) . . yes Cl(1) C(16) 1.73(1) . . yes Cl(2) C(17) 1.77(1) . . yes S(1) C(1) 1.786(4) . . yes S(1) C(15) 1.785(5) . . yes S(2) C(5) 1.786(4) . . yes S(2) C(6) 1.795(5) . . yes S(3) C(10) 1.796(4) . . yes S(3) C(11) 1.796(4) . . yes P(1) F(1) 1.529(8) . . yes P(1) F(2) 1.481(8) . . yes P(1) F(3) 1.591(5) . . yes P(1) F(4) 1.589(4) . . yes P(1) F(5) 1.487(7) . . yes P(1) F(6) 1.447(7) . . yes N(1) C(1) 1.346(5) . . yes N(1) C(5) 1.347(5) . . yes N(2) C(6) 1.337(5) . . yes N(2) C(10) 1.337(6) . . yes N(3) C(11) 1.334(6) . . yes N(3) C(15) 1.350(5) . . yes C(1) C(2) 1.382(7) . . yes C(2) C(3) 1.380(7) . . yes C(3) C(4) 1.391(8) . . yes C(4) C(5) 1.382(6) . . yes C(6) C(7) 1.384(7) . . yes C(7) C(8) 1.382(9) . . yes C(8) C(9) 1.383(8) . . yes C(9) C(10) 1.369(7) . . yes C(11) C(12) 1.382(6) . . yes C(12) C(13) 1.373(8) . . yes C(13) C(14) 1.387(8) . . yes C(14) C(15) 1.376(7) . . yes C(16) C(17) 1.42(2) . . yes #--------------------------------------------------------------------------- #-- loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S(3) Cu(1) N(1) 118.1(1) 3_646 . . yes S(3) Cu(1) N(2) 123.27(10) 3_646 . . yes S(3) Cu(1) N(3) 122.9(1) 3_646 . . yes N(1) Cu(1) N(2) 94.6(1) . . . yes N(1) Cu(1) N(3) 94.9(1) . . . yes N(2) Cu(1) N(3) 96.1(1) . . . yes C(1) S(1) C(15) 99.4(2) . . . yes C(5) S(2) C(6) 99.6(2) . . . yes Cu(1) S(3) C(10) 105.5(1) 3_646 . . yes Cu(1) S(3) C(11) 105.1(1) 3_646 . . yes C(10) S(3) C(11) 102.4(2) . . . yes F(1) P(1) F(2) 170.9(7) . . . yes F(1) P(1) F(3) 88.5(4) . . . yes F(1) P(1) F(4) 90.6(4) . . . yes F(1) P(1) F(5) 80.9(7) . . . yes F(1) P(1) F(6) 91.5(7) . . . yes F(2) P(1) F(3) 91.6(4) . . . yes F(2) P(1) F(4) 89.4(3) . . . yes F(2) P(1) F(5) 90.0(6) . . . yes F(2) P(1) F(6) 97.6(6) . . . yes F(3) P(1) F(4) 178.6(3) . . . yes F(3) P(1) F(5) 91.7(5) . . . yes F(3) P(1) F(6) 90.3(5) . . . yes F(4) P(1) F(5) 89.3(5) . . . yes F(4) P(1) F(6) 88.6(5) . . . yes F(5) P(1) F(6) 172.1(7) . . . yes Cu(1) N(1) C(1) 119.3(3) . . . yes Cu(1) N(1) C(5) 119.9(3) . . . yes C(1) N(1) C(5) 118.0(4) . . . yes Cu(1) N(2) C(6) 121.0(3) . . . yes Cu(1) N(2) C(10) 121.0(3) . . . yes C(6) N(2) C(10) 117.0(4) . . . yes Cu(1) N(3) C(11) 120.8(3) . . . yes Cu(1) N(3) C(15) 120.7(3) . . . yes C(11) N(3) C(15) 117.4(3) . . . yes S(1) C(1) N(1) 117.3(3) . . . yes S(1) C(1) C(2) 120.2(3) . . . yes N(1) C(1) C(2) 122.5(4) . . . yes C(1) C(2) C(3) 118.2(5) . . . yes C(2) C(3) C(4) 120.6(5) . . . yes C(3) C(4) C(5) 117.0(4) . . . yes S(2) C(5) N(1) 116.6(3) . . . yes S(2) C(5) C(4) 119.8(3) . . . yes N(1) C(5) C(4) 123.5(4) . . . yes S(2) C(6) N(2) 117.5(3) . . . yes S(2) C(6) C(7) 118.5(3) . . . yes N(2) C(6) C(7) 124.0(4) . . . yes C(6) C(7) C(8) 117.1(5) . . . yes C(7) C(8) C(9) 119.8(5) . . . yes C(8) C(9) C(10) 118.4(5) . . . yes S(3) C(10) N(2) 117.8(3) . . . yes S(3) C(10) C(9) 118.8(4) . . . yes N(2) C(10) C(9) 123.4(4) . . . yes S(3) C(11) N(3) 118.2(3) . . . yes S(3) C(11) C(12) 118.5(4) . . . yes N(3) C(11) C(12) 123.3(4) . . . yes C(11) C(12) C(13) 118.7(5) . . . yes C(12) C(13) C(14) 119.1(5) . . . yes C(13) C(14) C(15) 118.6(5) . . . yes S(1) C(15) N(3) 117.0(3) . . . yes S(1) C(15) C(14) 120.1(4) . . . yes N(3) C(15) C(14) 122.9(5) . . . yes Cl(1) C(16) C(17) 115.8(8) . . . yes Cl(2) C(17) C(16) 115.8(9) . . . yes #--------------------------------------------------------------------------- #-- loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cu(1) S(3) C(10) N(2) 49.6(3) . 3_646 3_646 3_646 yes Cu(1) S(3) C(10) C(9) -128.5(3) . 3_646 3_646 3_646 yes Cu(1) S(3) C(11) N(3) -49.5(3) . 3_646 3_646 3_646 yes Cu(1) S(3) C(11) C(12) 129.3(3) . 3_646 3_646 3_646 yes Cu(1) N(1) C(1) S(1) 17.0(5) . . . . yes Cu(1) N(1) C(1) C(2) -163.9(4) . . . . yes Cu(1) N(1) C(5) S(2) -19.2(4) . . . . yes Cu(1) N(1) C(5) C(4) 163.1(4) . . . . yes Cu(1) N(2) C(6) S(2) 7.0(4) . . . . yes Cu(1) N(2) C(6) C(7) -174.2(4) . . . . yes Cu(1) N(2) C(10) S(3) -10.6(4) . . . . yes Cu(1) N(2) C(10) C(9) 171.4(3) . . . . yes Cu(1) N(3) C(11) S(3) 10.9(4) . . . . yes Cu(1) N(3) C(11) C(12) -170.4(3) . . . . yes Cu(1) N(3) C(15) S(1) -9.3(5) . . . . yes Cu(1) N(3) C(15) C(14) 171.5(4) . . . . yes Cl(1) C(16) C(17) Cl(2) 59(1) . . . . yes S(1) C(1) N(1) C(5) 178.2(3) . . . . yes S(1) C(1) C(2) C(3) -179.9(4) . . . . yes S(1) C(15) N(3) C(11) -176.9(3) . . . . yes S(1) C(15) C(14) C(13) 178.2(4) . . . . yes S(2) C(5) N(1) C(1) 179.8(3) . . . . yes S(2) C(5) C(4) C(3) -177.4(4) . . . . yes S(2) C(6) N(2) C(10) 175.8(3) . . . . yes S(2) C(6) C(7) C(8) -177.7(4) . . . . yes S(3) Cu(1) N(2) C(6) 89.9(3) . 3_646 3_646 3_646 yes S(3) Cu(1) N(2) C(10) -101.7(3) . 3_646 3_646 3_646 yes S(3) Cu(1) N(3) C(11) 102.1(3) . 3_646 3_646 3_646 yes S(3) Cu(1) N(3) C(15) -90.8(3) . 3_646 3_646 3_646 yes S(3) C(10) N(2) C(6) -179.4(3) . . . . yes S(3) C(10) C(9) C(8) -176.0(4) . . . . yes S(3) C(11) N(3) C(15) 178.4(3) . . . . yes S(3) C(11) C(12) C(13) 179.2(4) . . . . yes N(1) Cu(1) S(3) C(10) 126.1(2) . . 3_646 3_646 yes N(1) Cu(1) S(3) C(11) -126.1(2) . . 3_646 3_646 yes N(1) Cu(1) N(2) C(6) 38.3(3) . . . . yes N(1) Cu(1) N(2) C(10) -130.1(3) . . . . yes N(1) Cu(1) N(3) C(11) 129.7(3) . . . . yes N(1) Cu(1) N(3) C(15) -37.5(3) . . . . yes N(1) C(1) S(1) C(15) -68.0(4) . . . . yes N(1) C(1) C(2) C(3) 1.0(8) . . . . yes N(1) C(5) S(2) C(6) 68.5(4) . . . . yes N(1) C(5) C(4) C(3) 0.3(8) . . . . yes N(2) Cu(1) S(3) C(10) -116.5(2) . . 3_646 3_646 yes N(2) Cu(1) S(3) C(11) -8.7(2) . . 3_646 3_646 yes N(2) Cu(1) N(1) C(1) 129.5(3) . . . . yes N(2) Cu(1) N(1) C(5) -31.3(3) . . . . yes N(2) Cu(1) N(3) C(11) 34.5(3) . . . . yes N(2) Cu(1) N(3) C(15) -132.7(3) . . . . yes N(2) C(6) S(2) C(5) -61.3(4) . . . . yes N(2) C(6) C(7) C(8) 3.4(7) . . . . yes N(2) C(10) S(3) C(11) 60.1(3) . . . . yes N(2) C(10) C(9) C(8) 2.0(7) . . . . yes N(3) Cu(1) S(3) C(10) 8.7(2) . . 3_646 3_646 yes N(3) Cu(1) S(3) C(11) 116.4(2) . . 3_646 3_646 yes N(3) Cu(1) N(1) C(1) 33.0(3) . . . . yes N(3) Cu(1) N(1) C(5) -127.9(3) . . . . yes N(3) Cu(1) N(2) C(6) 133.7(3) . . . . yes N(3) Cu(1) N(2) C(10) -34.6(3) . . . . yes N(3) C(11) S(3) C(10) -60.5(4) . . . . yes N(3) C(11) C(12) C(13) 0.5(7) . . . . yes N(3) C(15) S(1) C(1) 63.0(4) . . . . yes N(3) C(15) C(14) C(13) -2.6(8) . . . . yes C(1) S(1) C(15) C(14) -117.8(4) . . . . yes C(1) N(1) C(5) C(4) 2.0(7) . . . . yes C(1) C(2) C(3) C(4) 1.4(9) . . . . yes C(2) C(1) S(1) C(15) 112.9(4) . . . . yes C(2) C(1) N(1) C(5) -2.7(7) . . . . yes C(2) C(3) C(4) C(5) -2.0(9) . . . . yes C(4) C(5) S(2) C(6) -113.6(4) . . . . yes C(5) S(2) C(6) C(7) 119.8(4) . . . . yes C(6) N(2) C(10) C(9) 2.6(6) . . . . yes C(6) C(7) C(8) C(9) 1.4(8) . . . . yes C(7) C(6) N(2) C(10) -5.4(6) . . . . yes C(7) C(8) C(9) C(10) -3.9(9) . . . . yes C(9) C(10) S(3) C(11) -121.8(4) . . . . yes C(10) S(3) C(11) C(12) 120.7(4) . . . . yes C(11) N(3) C(15) C(14) 3.9(6) . . . . yes C(11) C(12) C(13) C(14) 0.9(8) . . . . yes C(12) C(11) N(3) C(15) -2.9(6) . . . . yes C(12) C(13) C(14) C(15) 0.1(8) . . . . yes C(12) C(13) C(14) C(15) 0.1(8) . . . . yes #--------------------------------------------------------------------------- #-- loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag S(1) F(1) 3.49(1) . 4_445 ? S(2) F(4) 3.220(5) . 1_556 ? F(1) C(4) 3.276(9) . 1_554 ? F(1) C(16) 3.39(1) . . ? F(1) C(17) 3.44(1) . . ? F(2) N(2) 3.095(7) . . ? F(2) C(5) 3.186(9) . . ? F(2) N(1) 3.19(1) . . ? F(2) C(6) 3.234(8) . . ? F(2) C(10) 3.253(9) . . ? F(2) N(3) 3.343(9) . . ? F(2) C(1) 3.40(1) . . ? F(2) C(11) 3.466(8) . . ? F(2) C(4) 3.469(10) . . ? F(3) C(16) 3.19(1) . . ? F(3) C(17) 3.36(1) . . ? F(3) C(3) 3.557(8) . . ? F(4) C(12) 3.348(7) . . ? F(4) C(9) 3.377(6) . . ? F(4) C(4) 3.393(6) . 1_554 ? F(4) C(11) 3.490(6) . . ? F(4) C(10) 3.494(6) . . ? F(4) C(5) 3.529(6) . 1_554 ? F(5) C(7) 3.189(10) . 4_444 ? F(5) C(8) 3.23(1) . 4_444 ? F(5) C(13) 3.33(1) . . ? F(5) C(14) 3.37(1) . . ? F(5) C(12) 3.60(1) . . ? F(6) C(13) 3.12(1) . 4_545 ? F(6) C(14) 3.20(1) . 4_545 ? F(6) C(2) 3.46(1) . 4_544 ? #------------------------------------------------------------------------------ data_py4s4-cu-cubr2 _database_code_CSD 183865 #--------------------------------------------------------------------------- #-- # CHEMICAL DATA _chemical_formula_sum 'C22 H16 Br4 Cl4 Cu3 N4 S4 ' _chemical_formula_moiety '?' _chemical_formula_weight 1116.70 _chemical_melting_point ? #--------------------------------------------------------------------------- #-- # CRYSTAL DATA _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P42/nmc' #(origin at -1) _symmetry_Int_Tables_number 137 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,y,z x,1/2-y,z 1/2-x,1/2-y,z y,x,1/2+z 1/2-y,x,1/2+z y,1/2-x,1/2+z 1/2-y,1/2-x,1/2+z -x,-y,-z 1/2+x,-y,-z -x,1/2+y,-z 1/2+x,1/2+y,-z -y,-x,1/2-z 1/2+y,-x,1/2-z -y,1/2+x,1/2-z 1/2+y,1/2+x,1/2-z _cell_length_a 13.3084(7) _cell_length_b 13.3084(7) _cell_length_c 9.2055(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1630.4(1) _cell_formula_units_Z 2 _cell_measurement_reflns_used 21506 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 296.2 #--------------------------------------------------------------------------- #-- _exptl_crystal_description 'needle' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 2.275 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 7.463 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.265 _exptl_absorpt_correction_T_max 0.474 #--------------------------------------------------------------------------- #-- # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.00 _diffrn_reflns_number 14971 _diffrn_reflns_av_R_equivalents 0.060 _diffrn_reflns_theta_max 27.47 _diffrn_measured_fraction_theta_max 0.9961 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.9961 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 #--------------------------------------------------------------------------- #-- # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ 3.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 1019 _reflns_number_gt 641 _reflns_threshold_expression F^2^3.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0581 _refine_ls_wR_factor_ref 0.1483 _refine_ls_hydrogen_treatment ? _refine_ls_number_reflns 641 _refine_ls_number_parameters 65 _refine_ls_goodness_of_fit_ref 1.977 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.06000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0004 _refine_diff_density_max 0.92 _refine_diff_density_min -0.92 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Cu' 'Cu' 0.320 1.265 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Br' 'Br' -0.290 2.459 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Cl' 'Cl' 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #--------------------------------------------------------------------------- #-- # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br(1) Br 0.2500 -0.07951(10) 0.8912(2) 0.0526(4) Uani 1.00 d S . . Cu(1) Cu 0.2500 -0.2500 1.2500 0.0320(4) Uani 1.00 d S . . Cu(2) Cu 0.2014(4) -0.2500 0.8779(5) 0.090(1) Uani 0.50 d SP . . Cl(1) Cl -0.1399(4) -0.2500 1.3961(6) 0.100(2) Uani 1.00 d S . . S(1) S 0.0568(2) -0.2500 1.0354(3) 0.0409(8) Uani 1.00 d S . . N(1) N 0.1433(4) -0.1433 1.2500 0.034(1) Uani 1.00 d S . . C(1) C 0.0640(5) -0.1482(6) 1.1595(8) 0.033(2) Uani 1.00 d . . . C(2) C -0.0099(6) -0.0757(6) 1.1552(9) 0.045(2) Uani 1.00 d . . . C(3) C -0.0037(6) 0.0037 1.2500 0.049(2) Uani 1.00 d S . . C(4) C -0.2500 -0.2500 1.288(3) 0.19(2) Uani 1.00 d S . . H(1) H -0.058(6) -0.083(6) 1.095(8) 0.04(2) Uiso 1.00 calc . . . H(2) H -0.049(6) 0.0494 1.2500 0.04(2) Uiso 1.00 calc S . . H(3) H -0.2500 -0.1917 1.2325 0.2331 Uiso 1.00 calc S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Br(1) 0.0386(7) 0.0580(8) 0.061(1) 0.0000 0.0000 0.0130(7) Cu(1) 0.0266(7) 0.0266 0.043(2) 0.0000 0.0000 0.0000 Cu(2) 0.137(4) 0.064(2) 0.068(2) 0.0000 0.032(3) 0.0000 Cl(1) 0.085(3) 0.120(4) 0.097(4) 0.0000 0.013(3) 0.0000 S(1) 0.047(2) 0.041(1) 0.035(2) 0.0000 -0.005(1) 0.0000 N(1) 0.031(2) 0.0306 0.039(5) 0.000(3) -0.0025 -0.003(3) C(1) 0.030(3) 0.036(3) 0.034(4) 0.001(3) 0.005(3) 0.010(3) C(2) 0.036(4) 0.053(5) 0.045(6) 0.013(4) -0.005(4) 0.006(4) C(3) 0.040(3) 0.0403 0.067(8) 0.016(5) 0.0073 0.007(4) C(4) 0.09(2) 0.41(7) 0.06(2) 0.0000 0.0000 0.0000 #--------------------------------------------------------------------------- #-- _computing_data_collection 'PROCESS-AUTO' _computing_cell_refinement 'PROCESS-AUTO' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #--------------------------------------------------------------------------- #-- _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br(1) Cu(2) 2.362(2) . . yes Br(1) Cu(2) 2.362(2) . 2_555 yes Br(1) Cu(2) 2.961(5) . 13_556 yes Cu(1) N(1) 2.009(8) . . yes Cu(1) N(1) 2.009(8) . 2_555 yes Cu(1) N(1) 2.009(8) . 3_545 yes Cu(1) N(1) 2.009(8) . 4_545 yes Cu(1) C(1) 2.943(7) . . yes Cu(1) C(1) 2.943(7) . 2_555 yes Cu(1) C(1) 2.943(7) . 3_545 yes Cu(1) C(1) 2.943(7) . 4_545 yes Cu(1) C(1) 2.943(7) . 15_547 yes Cu(1) C(1) 2.943(7) . 16_547 yes Cu(1) C(1) 2.943(7) . 13_557 yes Cu(1) C(1) 2.943(7) . 14_557 yes Cu(2) Cu(2) 1.29(1) . 2_555 yes Cu(2) Cu(2) 2.527(8) . 15_546 yes Cu(2) Cu(2) 2.527(8) . 13_556 yes Cu(2) S(1) 2.409(6) . . yes Cl(1) Cl(1) 2.93(1) . 2_455 yes Cl(1) C(4) 1.77(2) . . yes S(1) N(1) 2.691(3) . . yes S(1) N(1) 2.691(3) . 3_545 yes S(1) C(1) 1.775(8) . . yes S(1) C(1) 1.775(8) . 3_545 yes S(1) C(2) 2.718(8) . . yes S(1) C(2) 2.718(8) . 3_545 yes N(1) N(1) 2.84(1) . 2_555 yes N(1) N(1) 2.84(1) . 3_545 yes N(1) C(1) 1.346(8) . . yes N(1) C(1) 1.346(8) . 13_557 yes N(1) C(2) 2.39(1) . . yes N(1) C(2) 2.39(1) . 13_557 yes N(1) C(3) 2.77(1) . . yes C(1) C(1) 2.71(2) . 3_545 yes C(1) C(1) 2.30(2) . 13_557 yes C(1) C(2) 1.378(10) . . yes C(1) C(2) 2.71(1) . 13_557 yes C(1) C(3) 2.36(1) . . yes C(2) C(2) 2.37(2) . 13_557 yes C(2) C(3) 1.373(10) . . yes #--------------------------------------------------------------------------- loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Br(1) Cu(2) Cu(2) Br(1) 173.8(2) . . 2_555 3_545 yes Br(1) Cu(2) Cu(2) Cu(2) -108.4(2) . . 2_555 15_546 yes Br(1) Cu(2) Cu(2) Cu(2) -77.7(1) . . 2_555 13_556 yes Br(1) Cu(2) Cu(2) S(1) 86.9(1) . . 2_555 2_555 yes Br(1) Cu(2) Cu(2) Br(1) -93.82(7) . . 15_546 13_556 yes Br(1) Cu(2) Cu(2) Br(1) 52.9(3) . . 15_546 14_556 yes Br(1) Cu(2) Cu(2) Cu(2) 69.4(2) . . 15_546 2_555 yes Br(1) Cu(2) Cu(2) Cu(2) -16.5(1) . . 15_546 13_556 yes Br(1) Cu(2) Cu(2) S(1) 177.8(1) . . 15_546 15_546 yes Br(1) Cu(2) Cu(2) Br(1) -119.5(2) . . 13_556 13_556 yes Br(1) Cu(2) Cu(2) Br(1) 93.82(7) . . 13_556 14_556 yes Br(1) Cu(2) Cu(2) Cu(2) 77.28(7) . . 13_556 2_555 yes Br(1) Cu(2) Cu(2) Cu(2) 163.3(1) . . 13_556 15_546 yes Br(1) Cu(2) Cu(2) S(1) -31.1(4) . . 13_556 13_556 yes Br(1) Cu(2) S(1) N(1) -45.9(2) . . . . yes Br(1) Cu(2) S(1) N(1) -109.9(2) . . . 3_545 yes Br(1) Cu(2) S(1) C(1) -23.5(3) . . . . yes Br(1) Cu(2) S(1) C(1) -132.3(3) . . . 3_545 yes Br(1) Cu(2) S(1) C(2) 3.6(3) . . . . yes Br(1) Cu(2) S(1) C(2) -159.4(2) . . . 3_545 yes Br(1) Cu(2) Br(1) Cu(2) 11.1(4) . 2_555 3_545 . yes Br(1) Cu(2) Cu(2) Cu(2) 108.4(2) . 2_555 . 15_546 yes Br(1) Cu(2) Cu(2) Cu(2) 77.7(1) . 2_555 . 13_556 yes Br(1) Cu(2) Cu(2) S(1) -86.9(1) . 2_555 . . yes Br(1) Cu(2) Cu(2) Br(1) -52.9(3) . 2_555 15_546 13_556 yes Br(1) Cu(2) Cu(2) Br(1) 93.82(7) . 2_555 15_546 14_556 yes Br(1) Cu(2) Cu(2) Cu(2) -69.4(2) . 2_555 15_546 . yes Br(1) Cu(2) Cu(2) Cu(2) 16.5(1) . 2_555 15_546 13_556 yes Br(1) Cu(2) Cu(2) S(1) -177.8(1) . 2_555 15_546 15_546 yes Br(1) Cu(2) Cu(2) Br(1) -93.82(7) . 2_555 13_556 13_556 yes Br(1) Cu(2) Cu(2) Br(1) 119.5(2) . 2_555 13_556 14_556 yes Br(1) Cu(2) Cu(2) Cu(2) -77.28(7) . 2_555 13_556 . yes Br(1) Cu(2) Cu(2) Cu(2) -163.3(1) . 2_555 13_556 15_546 yes Br(1) Cu(2) Cu(2) S(1) 31.1(4) . 2_555 13_556 13_556 yes Br(1) Cu(2) S(1) C(1) 23.5(3) . 2_555 2_555 2_555 yes Br(1) Cu(2) S(1) C(1) 132.3(3) . 2_555 2_555 4_545 yes Br(1) Cu(2) Br(1) Cu(2) -121.6(1) . 13_556 13_556 15_546 yes Br(1) Cu(2) Br(1) Cu(2) 121.6(1) . 13_556 14_556 15_546 yes Br(1) Cu(2) Cu(2) Cu(2) -77.28(7) . 13_556 . 2_555 yes Br(1) Cu(2) Cu(2) Cu(2) -163.3(1) . 13_556 . 15_546 yes Br(1) Cu(2) Cu(2) S(1) 88.4(2) . 13_556 . . yes Br(1) Cu(2) Cu(2) Br(1) 146.7(3) . 13_556 2_555 3_545 yes Br(1) Cu(2) Cu(2) Cu(2) 77.28(7) . 13_556 2_555 . yes Br(1) Cu(2) Cu(2) Cu(2) 163.3(1) . 13_556 2_555 15_546 yes Br(1) Cu(2) Cu(2) S(1) -88.4(2) . 13_556 2_555 2_555 yes Br(1) Cu(2) Cu(2) Br(1) 93.1(1) . 13_556 15_546 13_556 yes Br(1) Cu(2) Cu(2) Br(1) -93.1(1) . 13_556 15_546 14_556 yes Br(1) Cu(2) Cu(2) Cu(2) 15.3(1) . 13_556 15_546 . yes Br(1) Cu(2) Cu(2) Cu(2) -15.3(1) . 13_556 15_546 2_555 yes Br(1) Cu(2) Cu(2) S(1) 180.0 . 13_556 15_546 15_546 yes Cu(1) N(1) N(1) C(1) 85.5(7) . . 2_555 2_555 yes Cu(1) N(1) N(1) C(1) -141.7(3) . . 2_555 14_557 yes Cu(1) N(1) N(1) C(1) -141.7(3) . . 3_545 3_545 yes Cu(1) N(1) N(1) C(1) 85.5(7) . . 3_545 15_547 yes Cu(1) N(1) C(1) C(1) 30.9(2) . . . 3_545 yes Cu(1) N(1) C(1) C(1) 180.0 . . . 13_557 yes Cu(1) N(1) C(1) C(2) -179.1(6) . . . . yes Cu(1) N(1) C(1) C(2) 179.6(3) . . . 13_557 yes Cu(1) N(1) C(1) C(3) 180.0 . . . . yes Cu(1) N(1) C(1) S(1) -1.7(6) . . 13_557 13_557 yes Cu(1) N(1) C(1) C(2) -179.1(6) . . 13_557 13_557 yes Cu(1) N(1) C(2) C(2) -180.0 . . . 13_557 yes Cu(1) N(1) C(2) C(3) -180.0 . . . . yes Cu(1) N(1) C(2) C(1) 1.6(10) . . 13_557 13_557 yes Cu(1) N(1) C(2) C(3) -180.0 . . 13_557 . yes Cu(1) N(1) C(1) S(1) 1.7(6) . 2_555 2_555 2_555 yes Cu(1) N(1) C(1) C(2) 179.1(6) . 2_555 2_555 2_555 yes Cu(1) N(1) C(1) S(1) 1.7(6) . 2_555 14_557 13_557 yes Cu(1) N(1) C(1) C(2) 179.1(6) . 2_555 14_557 14_557 yes Cu(1) N(1) C(1) S(1) 1.7(6) . 3_545 3_545 . yes Cu(1) N(1) C(1) C(2) 179.1(6) . 3_545 3_545 3_545 yes Cu(1) N(1) C(1) S(1) 1.7(6) . 3_545 15_547 15_547 yes Cu(1) N(1) C(1) C(2) 179.1(6) . 3_545 15_547 15_547 yes Cu(1) N(1) C(1) S(1) -1.7(6) . 4_545 4_545 2_555 yes Cu(1) N(1) C(1) C(2) -179.1(6) . 4_545 4_545 4_545 yes Cu(1) N(1) C(1) S(1) -1.7(6) . 4_545 16_547 15_547 yes Cu(1) N(1) C(1) C(2) -179.1(6) . 4_545 16_547 16_547 yes Cu(1) C(1) C(1) S(1) -113.3(4) . . 3_545 . yes Cu(1) C(1) C(1) N(1) 19.7(2) . . 3_545 3_545 yes Cu(1) C(1) C(1) C(2) 163.7(8) . . 3_545 3_545 yes Cu(1) C(1) C(1) S(1) -2(1) . . 13_557 13_557 yes Cu(1) C(1) C(1) N(1) 0.0 . . 13_557 . yes Cu(1) C(1) C(1) C(2) -179.2(5) . . 13_557 13_557 yes Cu(1) C(1) C(2) C(2) -2(1) . . . 13_557 yes Cu(1) C(1) C(2) C(3) -3(1) . . . . yes Cu(1) C(1) C(2) C(1) 0.7(4) . . 13_557 13_557 yes Cu(1) C(1) C(2) C(3) 179.4(4) . . 13_557 . yes Cu(1) C(1) S(1) Cu(2) 60.5(2) . 2_555 2_555 2_555 yes Cu(1) C(1) S(1) C(1) -55.2(3) . 2_555 2_555 4_545 yes Cu(1) C(1) N(1) C(1) -180.0 . 2_555 2_555 14_557 yes Cu(1) C(1) C(2) C(3) 3(1) . 2_555 2_555 14_557 yes Cu(1) C(1) S(1) N(1) -33.7(2) . 3_545 . . yes Cu(1) C(1) S(1) N(1) 1.0(3) . 3_545 . 3_545 yes Cu(1) C(1) S(1) C(1) -55.2(3) . 3_545 . . yes Cu(1) C(1) S(1) C(2) -78.4(3) . 3_545 . . yes Cu(1) C(1) S(1) C(2) 178.5(7) . 3_545 . 3_545 yes Cu(1) C(1) N(1) C(1) -180.0 . 3_545 3_545 15_547 yes Cu(1) C(1) C(2) C(3) 3(1) . 3_545 3_545 3_545 yes Cu(1) C(1) S(1) Cu(2) -60.5(2) . 4_545 2_555 2_555 yes Cu(1) C(1) S(1) C(1) 55.2(3) . 4_545 2_555 2_555 yes Cu(1) C(1) N(1) C(1) 180.0 . 4_545 4_545 16_547 yes Cu(1) C(1) S(1) Cu(2) 60.5(2) . 15_547 15_547 15_547 yes Cu(1) C(1) S(1) C(1) -55.2(3) . 15_547 15_547 16_547 yes Cu(1) C(1) N(1) C(1) -180.0 . 15_547 3_545 3_545 yes Cu(1) C(1) C(2) C(3) 3(1) . 15_547 15_547 15_547 yes Cu(1) C(1) S(1) Cu(2) -60.5(2) . 16_547 15_547 15_547 yes Cu(1) C(1) S(1) C(1) 55.2(3) . 16_547 15_547 15_547 yes Cu(1) C(1) N(1) C(1) 180.0 . 16_547 4_545 4_545 yes Cu(1) C(1) S(1) Cu(2) -60.5(2) . 13_557 13_557 13_557 yes Cu(1) C(1) S(1) C(1) 55.2(3) . 13_557 13_557 14_557 yes Cu(1) C(1) N(1) N(1) -30.9(2) . 13_557 . 2_555 yes Cu(1) C(1) N(1) N(1) 55.6(5) . 13_557 . 3_545 yes Cu(1) C(1) N(1) C(1) 180.0 . 13_557 . . yes Cu(1) C(1) N(1) C(2) -179.6(3) . 13_557 . . yes Cu(1) C(1) N(1) C(2) 179.1(6) . 13_557 . 13_557 yes Cu(1) C(1) N(1) C(3) 180.0000(1) . 13_557 . . yes Cu(1) C(1) C(2) C(3) -3(1) . 13_557 13_557 . yes Cu(1) C(1) S(1) Cu(2) 60.5(2) . 14_557 13_557 13_557 yes Cu(1) C(1) S(1) C(1) -55.2(3) . 14_557 13_557 13_557 yes Cu(1) C(1) N(1) C(1) -180.0 . 14_557 2_555 2_555 yes Cu(1) C(1) C(2) C(3) 3(1) . 14_557 14_557 2_555 yes Cu(2) Cu(2) Cu(2) Cu(2) 85.98(7) . 2_555 15_546 13_556 yes Cu(2) Cu(2) Cu(2) S(1) -108.3(3) . 2_555 15_546 15_546 yes Cu(2) Cu(2) Cu(2) Cu(2) -85.98(7) . 2_555 13_556 15_546 yes Cu(2) Cu(2) Cu(2) S(1) 108.3(3) . 2_555 13_556 13_556 yes Cu(2) Cu(2) S(1) C(1) -54.4(3) . 2_555 2_555 2_555 yes Cu(2) Cu(2) S(1) C(1) 54.4(3) . 2_555 2_555 4_545 yes Cu(2) Cu(2) Cu(2) Cu(2) -85.98(7) . 15_546 2_555 13_556 yes Cu(2) Cu(2) Cu(2) S(1) 165.7(2) . 15_546 2_555 2_555 yes Cu(2) Cu(2) Cu(2) Cu(2) 30.7(3) . 15_546 13_556 2_555 yes Cu(2) Cu(2) Cu(2) S(1) -164.7(1) . 15_546 13_556 13_556 yes Cu(2) Cu(2) Cu(2) Cu(2) 85.98(7) . 13_556 2_555 15_546 yes Cu(2) Cu(2) Cu(2) S(1) -165.7(2) . 13_556 2_555 2_555 yes Cu(2) Cu(2) Cu(2) Cu(2) -30.7(3) . 13_556 15_546 2_555 yes Cu(2) Cu(2) Cu(2) S(1) 164.7(1) . 13_556 15_546 15_546 yes Cu(2) S(1) N(1) N(1) -20.7(1) . . . 2_555 yes Cu(2) S(1) N(1) N(1) -93.6(1) . . . 3_545 yes Cu(2) S(1) N(1) C(1) 125.6(5) . . . . yes Cu(2) S(1) N(1) C(1) 122.4(6) . . . 13_557 yes Cu(2) S(1) N(1) C(2) 124.2(2) . . . . yes Cu(2) S(1) N(1) C(2) 124.1(2) . . . 13_557 yes Cu(2) S(1) N(1) C(3) 124.19(8) . . . . yes Cu(2) S(1) N(1) C(1) -125.6(5) . . 3_545 3_545 yes Cu(2) S(1) N(1) C(1) -122.4(6) . . 3_545 15_547 yes Cu(2) S(1) C(1) C(1) -115.7(3) . . . 3_545 yes Cu(2) S(1) C(1) C(1) -57(1) . . . 13_557 yes Cu(2) S(1) C(1) C(2) 118.0(6) . . . . yes Cu(2) S(1) C(1) C(2) 48(18) . . . 13_557 yes Cu(2) S(1) C(1) C(3) 117.3(6) . . . . yes Cu(2) S(1) C(1) N(1) 59.5(5) . . 3_545 3_545 yes Cu(2) S(1) C(1) C(2) -118.0(6) . . 3_545 3_545 yes Cu(2) S(1) C(2) C(2) -72.3(7) . . . 13_557 yes Cu(2) S(1) C(2) C(3) -72(1) . . . . yes Cu(2) S(1) C(2) C(1) 73.7(7) . . 3_545 3_545 yes Cu(2) S(1) C(2) C(3) 72(1) . . 3_545 3_545 yes S(1) N(1) N(1) C(1) 31.2(6) . . 2_555 2_555 yes S(1) N(1) N(1) C(1) 164.0(4) . . 2_555 14_557 yes S(1) N(1) N(1) C(1) -21.5(3) . . 3_545 3_545 yes S(1) N(1) N(1) C(1) -154.3(7) . . 3_545 15_547 yes S(1) N(1) C(1) C(1) 32.5(4) . . . 3_545 yes S(1) N(1) C(1) C(1) -178.3(6) . . . 13_557 yes S(1) N(1) C(1) C(2) -177(1) . . . . yes S(1) N(1) C(1) C(2) -178.8(5) . . . 13_557 yes S(1) N(1) C(1) C(3) -178.3(6) . . . . yes S(1) N(1) C(1) C(2) 3(1) . . 13_557 13_557 yes S(1) N(1) C(2) C(2) -179.9(4) . . . 13_557 yes S(1) N(1) C(2) C(3) -179.9(4) . . . . yes S(1) N(1) C(2) C(1) -178.3(7) . . 13_557 13_557 yes S(1) N(1) C(2) C(3) 0.1(5) . . 13_557 . yes S(1) N(1) Cu(1) N(1) 47.38(6) . 3_545 . . yes S(1) N(1) Cu(1) N(1) -132.62(6) . 3_545 . 4_545 yes S(1) N(1) Cu(1) C(1) 30.3(2) . 3_545 . . yes S(1) N(1) Cu(1) C(1) -86.2(3) . 3_545 . 2_555 yes S(1) N(1) Cu(1) C(1) 1.0(3) . 3_545 . 3_545 yes S(1) N(1) Cu(1) C(1) -115.5(2) . 3_545 . 4_545 yes S(1) N(1) Cu(1) C(1) -179.0(3) . 3_545 . 15_547 yes S(1) N(1) Cu(1) C(1) -149.7(2) . 3_545 . 16_547 yes S(1) N(1) Cu(1) C(1) 64.5(2) . 3_545 . 13_557 yes S(1) N(1) Cu(1) C(1) 93.8(3) . 3_545 . 14_557 yes S(1) N(1) C(1) C(2) 177(1) . 3_545 3_545 3_545 yes S(1) N(1) C(1) C(2) -3(1) . 3_545 15_547 15_547 yes S(1) C(1) C(1) N(1) 133.0(6) . . 3_545 3_545 yes S(1) C(1) C(1) C(2) -82.9(8) . . 3_545 3_545 yes S(1) C(1) C(1) S(1) -5(2) . . 13_557 13_557 yes S(1) C(1) C(1) N(1) -2(1) . . 13_557 . yes S(1) C(1) C(1) C(2) 177.9(8) . . 13_557 13_557 yes S(1) C(1) C(2) C(2) -178.8(4) . . . 13_557 yes S(1) C(1) C(2) C(3) -179.2(5) . . . . yes S(1) C(1) C(2) C(1) -108(18) . . 13_557 13_557 yes S(1) C(1) C(2) C(3) 70(18) . . 13_557 . yes S(1) C(1) N(1) C(1) -178.3(6) . 3_545 3_545 15_547 yes S(1) C(1) C(2) C(3) 179.2(5) . 3_545 3_545 3_545 yes S(1) C(2) C(2) C(1) 0.6(9) . . 13_557 13_557 yes S(1) C(2) C(2) C(3) 179.9(5) . . 13_557 . yes S(1) C(2) C(1) N(1) -177(1) . 3_545 3_545 3_545 yes N(1) N(1) Cu(1) C(1) 17.1(2) . 2_555 . . yes N(1) N(1) Cu(1) C(1) 133.6(3) . 2_555 . 2_555 yes N(1) N(1) Cu(1) C(1) 46.4(3) . 2_555 . 3_545 yes N(1) N(1) Cu(1) C(1) 162.9(2) . 2_555 . 4_545 yes N(1) N(1) Cu(1) C(1) -133.6(3) . 2_555 . 15_547 yes N(1) N(1) Cu(1) C(1) -162.9(2) . 2_555 . 16_547 yes N(1) N(1) Cu(1) C(1) -17.1(2) . 2_555 . 13_557 yes N(1) N(1) Cu(1) C(1) -46.4(3) . 2_555 . 14_557 yes N(1) N(1) C(1) C(2) 123.5(7) . 2_555 2_555 2_555 yes N(1) N(1) C(1) C(2) -150.1(7) . 2_555 14_557 14_557 yes N(1) N(1) Cu(1) C(1) -17.1(2) . 3_545 . . yes N(1) N(1) Cu(1) C(1) -133.6(3) . 3_545 . 2_555 yes N(1) N(1) Cu(1) C(1) -46.4(3) . 3_545 . 3_545 yes N(1) N(1) Cu(1) C(1) -162.9(2) . 3_545 . 4_545 yes N(1) N(1) Cu(1) C(1) 133.6(3) . 3_545 . 15_547 yes N(1) N(1) Cu(1) C(1) 162.9(2) . 3_545 . 16_547 yes N(1) N(1) Cu(1) C(1) 17.1(2) . 3_545 . 13_557 yes N(1) N(1) Cu(1) C(1) 46.4(3) . 3_545 . 14_557 yes N(1) N(1) C(1) C(2) -150.1(7) . 3_545 3_545 3_545 yes N(1) N(1) C(1) C(2) 123.5(7) . 3_545 15_547 15_547 yes N(1) C(1) C(1) N(1) 0.0 . . 3_545 3_545 yes N(1) C(1) C(1) C(2) 144.0(9) . . 3_545 3_545 yes N(1) C(1) C(1) C(2) -179.2(5) . . 13_557 13_557 yes N(1) C(1) C(2) C(2) -1.4(8) . . . 13_557 yes N(1) C(1) C(2) C(3) -1(1) . . . . yes N(1) C(1) C(2) C(1) 0.4(3) . . 13_557 13_557 yes N(1) C(1) C(2) C(3) 179.1(5) . . 13_557 . yes N(1) C(1) S(1) C(1) 56.2(6) . 13_557 13_557 14_557 yes N(1) C(1) C(2) C(3) -1(1) . 13_557 13_557 . yes N(1) C(2) C(2) C(1) 0.7(5) . . 13_557 13_557 yes N(1) C(2) C(2) C(3) 180.0 . . 13_557 . yes C(1) C(1) S(1) C(2) -23.2(3) . 3_545 . . yes C(1) C(1) S(1) C(2) -126.2(6) . 3_545 . 3_545 yes C(1) C(1) C(2) C(3) -133.9(5) . 3_545 3_545 3_545 yes C(1) C(1) N(1) C(2) 0.4(3) . 13_557 . . yes C(1) C(1) N(1) C(2) -0.9(6) . 13_557 . 13_557 yes C(1) C(1) N(1) C(3) 0.0 . 13_557 . . yes C(1) C(1) C(2) C(3) -1.3(8) . 13_557 13_557 . yes C(1) C(2) C(2) C(1) 1.5(9) . . 13_557 13_557 yes C(1) C(2) C(2) C(3) -179.3(5) . . 13_557 . yes C(1) C(2) C(2) C(3) -179.3(5) . . 13_557 . yes #--------------------------------------------------------------------------- #-- loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Br(1) Cu(2) 2.961(5) . 13_556 ? Cu(1) C(1) 2.943(7) . . ? Cu(1) C(1) 2.943(7) . 2_555 ? Cu(1) C(1) 2.943(7) . 3_545 ? Cu(1) C(1) 2.943(7) . 4_545 ? Cu(1) C(1) 2.943(7) . 15_547 ? Cu(1) C(1) 2.943(7) . 16_547 ? Cu(1) C(1) 2.943(7) . 13_557 ? Cu(1) C(1) 2.943(7) . 14_557 ? Cu(2) Cu(2) 2.527(8) . 15_546 ? Cu(2) Cu(2) 2.527(8) . 13_556 ? Cl(1) Cl(1) 2.93(1) . 2_455 ? S(1) N(1) 2.691(3) . . ? S(1) N(1) 2.691(3) . 3_545 ? S(1) C(2) 2.718(8) . . ? S(1) C(2) 2.718(8) . 3_545 ? N(1) N(1) 2.84(1) . 2_555 ? N(1) N(1) 2.84(1) . 3_545 ? N(1) C(3) 2.77(1) . . ? C(1) C(1) 2.71(2) . 3_545 ? C(1) C(2) 2.71(1) . 13_557 ? Cu(1) C(1) 2.943(7) . 14_557 ? Cu(1) C(1) 2.943(7) . 15_547 ? Cu(1) C(1) 2.943(7) . 16_547 ? N(1) C(1) 3.084(8) . 14_557 ? #------------------------------------------------------------------------------ data_Py4S4 _database_code_CSD 183866 #--------------------------------------------------------------------------- #-- # CHEMICAL DATA _chemical_formula_sum 'C20 H12 N4 S4 ' _chemical_formula_moiety 'C20 H12 N4 S4 ' _chemical_formula_weight 436.58 _chemical_melting_point ? #--------------------------------------------------------------------------- #-- # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 8.680(2) _cell_length_b 9.7776(5) _cell_length_c 11.5637(7) _cell_angle_alpha 97.695(4) _cell_angle_beta 97.170(10) _cell_angle_gamma 90.681(9) _cell_volume 964.5(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 29.6 _cell_measurement_theta_max 30.0 _cell_measurement_temperature 296.2 #--------------------------------------------------------------------------- #-- _exptl_crystal_description 'plate' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.050 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.503 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 4.637 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.756 _exptl_absorpt_correction_T_max 0.999 #--------------------------------------------------------------------------- #-- # EXPERIMENTAL DATA _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 3079 _diffrn_reflns_av_R_equivalents 0.024 _diffrn_reflns_theta_max 60.06 _diffrn_measured_fraction_theta_max 1.0046 _diffrn_reflns_theta_full 60.06 _diffrn_measured_fraction_theta_full 1.0046 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 1.33 #--------------------------------------------------------------------------- #-- # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 2863 _reflns_number_gt 2657 _reflns_threshold_expression F^2^2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0960 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 2863 _refine_ls_number_parameters 301 _refine_ls_goodness_of_fit_ref 1.572 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0009 _refine_diff_density_max 0.15 _refine_diff_density_min -0.31 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.018 0.009 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'N' 'N' 0.031 0.018 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.333 0.557 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #--------------------------------------------------------------------------- #-- # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S(1) S -1.19327(6) -0.65391(6) -0.93490(5) 0.0617(2) Uani 1.00 d . . . S(2) S -0.94467(6) -0.80879(6) -0.53922(4) 0.0547(2) Uani 1.00 d . . . S(3) S -0.34787(6) -0.75126(7) -0.59809(5) 0.0619(2) Uani 1.00 d . . . S(4) S -0.65528(6) -0.88880(6) -1.01927(5) 0.0602(2) Uani 1.00 d . . . N(1) N -1.0447(2) -0.7085(2) -0.7322(1) 0.0452(4) Uani 1.00 d . . . N(2) N -0.6405(2) -0.7790(2) -0.5516(1) 0.0473(4) Uani 1.00 d . . . N(3) N -0.5197(2) -0.7953(2) -0.8071(1) 0.0470(4) Uani 1.00 d . . . N(4) N -0.9321(2) -0.7755(2) -0.9909(1) 0.0461(4) Uani 1.00 d . . . C(1) C -1.0624(2) -0.6116(2) -0.8037(2) 0.0480(5) Uani 1.00 d . . . C(2) C -0.9892(3) -0.4834(2) -0.7778(2) 0.0609(7) Uani 1.00 d . . . C(3) C -0.8943(3) -0.4539(2) -0.6731(2) 0.0656(7) Uani 1.00 d . . . C(4) C -0.8727(3) -0.5512(2) -0.5986(2) 0.0563(6) Uani 1.00 d . . . C(5) C -0.9504(2) -0.6778(2) -0.6323(2) 0.0455(5) Uani 1.00 d . . . C(6) C -0.7450(2) -0.8123(2) -0.4841(2) 0.0475(5) Uani 1.00 d . . . C(7) C -0.7065(3) -0.8605(3) -0.3777(2) 0.0654(7) Uani 1.00 d . . . C(8) C -0.5517(3) -0.8790(3) -0.3414(2) 0.0677(7) Uani 1.00 d . . . C(9) C -0.4424(3) -0.8454(2) -0.4082(2) 0.0589(6) Uani 1.00 d . . . C(10) C -0.4921(2) -0.7939(2) -0.5124(2) 0.0484(5) Uani 1.00 d . . . C(11) C -0.4628(2) -0.6965(2) -0.7212(2) 0.0497(5) Uani 1.00 d . . . C(12) C -0.4815(3) -0.5574(2) -0.7256(2) 0.0597(6) Uani 1.00 d . . . C(13) C -0.5644(3) -0.5181(2) -0.8249(2) 0.0641(7) Uani 1.00 d . . . C(14) C -0.6240(2) -0.6171(2) -0.9144(2) 0.0565(6) Uani 1.00 d . . . C(15) C -0.5988(2) -0.7540(2) -0.9019(2) 0.0458(5) Uani 1.00 d . . . C(16) C -0.8569(2) -0.8688(2) -1.0555(2) 0.0467(5) Uani 1.00 d . . . C(17) C -0.9287(3) -0.9601(2) -1.1496(2) 0.0571(6) Uani 1.00 d . . . C(18) C -1.0862(3) -0.9532(3) -1.1771(2) 0.0651(7) Uani 1.00 d . . . C(19) C -1.1680(3) -0.8588(2) -1.1117(2) 0.0616(7) Uani 1.00 d . . . C(20) C -1.0858(2) -0.7732(2) -1.0192(2) 0.0471(5) Uani 1.00 d . . . H(1) H -1.011(3) -0.426(3) -0.831(2) 0.072(7) Uiso 1.00 calc . . . H(2) H -0.846(3) -0.369(3) -0.655(2) 0.085(8) Uiso 1.00 calc . . . H(3) H -0.809(3) -0.534(2) -0.532(2) 0.069(7) Uiso 1.00 calc . . . H(4) H -0.783(4) -0.880(3) -0.331(3) 0.096(9) Uiso 1.00 calc . . . H(5) H -0.522(3) -0.909(3) -0.270(3) 0.084(8) Uiso 1.00 calc . . . H(6) H -0.333(3) -0.860(2) -0.389(2) 0.065(6) Uiso 1.00 calc . . . H(7) H -0.434(3) -0.492(3) -0.660(2) 0.084(8) Uiso 1.00 calc . . . H(8) H -0.581(3) -0.428(3) -0.831(2) 0.085(8) Uiso 1.00 calc . . . H(9) H -0.679(3) -0.594(2) -0.983(2) 0.061(6) Uiso 1.00 calc . . . H(10) H -0.865(3) -1.026(2) -1.191(2) 0.058(6) Uiso 1.00 calc . . . H(11) H -1.139(3) -1.012(3) -1.235(2) 0.078(7) Uiso 1.00 calc . . . H(12) H -1.280(3) -0.854(3) -1.122(2) 0.073(7) Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 S(1) 0.0462(3) 0.0874(4) 0.0540(3) 0.0186(3) 0.0034(2) 0.0198(3) S(2) 0.0454(3) 0.0715(3) 0.0519(3) 0.0004(2) 0.0087(2) 0.0232(2) S(3) 0.0397(3) 0.0928(4) 0.0567(3) 0.0011(2) 0.0013(2) 0.0277(3) S(4) 0.0517(3) 0.0715(4) 0.0565(3) 0.0118(3) 0.0116(2) 0.0005(3) N(1) 0.0406(8) 0.0503(9) 0.0460(9) 0.0030(6) 0.0080(7) 0.0094(7) N(2) 0.0438(9) 0.0596(10) 0.0404(8) 0.0030(7) 0.0047(7) 0.0141(7) N(3) 0.0387(8) 0.0557(9) 0.0502(9) 0.0038(7) 0.0096(7) 0.0168(7) N(4) 0.0443(9) 0.0556(9) 0.0394(8) 0.0027(7) 0.0040(7) 0.0110(7) C(1) 0.0425(10) 0.057(1) 0.048(1) 0.0104(8) 0.0139(8) 0.0130(9) C(2) 0.067(1) 0.055(1) 0.067(1) 0.008(1) 0.018(1) 0.022(1) C(3) 0.069(1) 0.049(1) 0.079(2) -0.005(1) 0.015(1) 0.006(1) C(4) 0.056(1) 0.056(1) 0.054(1) -0.0011(9) 0.007(1) -0.0007(10) C(5) 0.0428(10) 0.053(1) 0.0432(10) 0.0052(8) 0.0123(8) 0.0075(8) C(6) 0.047(1) 0.057(1) 0.0395(10) 0.0026(8) 0.0060(8) 0.0106(8) C(7) 0.065(1) 0.091(2) 0.043(1) -0.006(1) 0.007(1) 0.022(1) C(8) 0.072(2) 0.089(2) 0.044(1) -0.004(1) -0.005(1) 0.026(1) C(9) 0.056(1) 0.070(1) 0.049(1) -0.001(1) -0.0076(10) 0.0171(10) C(10) 0.047(1) 0.055(1) 0.0425(10) 0.0003(8) 0.0006(8) 0.0096(8) C(11) 0.0365(9) 0.066(1) 0.051(1) 0.0022(8) 0.0095(8) 0.0195(9) C(12) 0.055(1) 0.059(1) 0.064(1) -0.0010(10) 0.004(1) 0.008(1) C(13) 0.062(1) 0.052(1) 0.080(2) 0.007(1) 0.005(1) 0.019(1) C(14) 0.049(1) 0.065(1) 0.059(1) 0.0056(9) 0.0038(10) 0.024(1) C(15) 0.0368(9) 0.057(1) 0.048(1) 0.0049(8) 0.0113(8) 0.0150(9) C(16) 0.052(1) 0.053(1) 0.0385(9) 0.0005(8) 0.0083(8) 0.0158(8) C(17) 0.076(2) 0.055(1) 0.041(1) -0.001(1) 0.008(1) 0.0093(9) C(18) 0.077(2) 0.068(1) 0.046(1) -0.013(1) -0.010(1) 0.007(1) C(19) 0.057(1) 0.074(1) 0.053(1) -0.009(1) -0.009(1) 0.022(1) C(20) 0.047(1) 0.057(1) 0.0410(10) 0.0008(8) 0.0014(8) 0.0224(8) #--------------------------------------------------------------------------- _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #--------------------------------------------------------------------------- _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag S(1) C(1) 1.776(2) . . yes S(1) C(20) 1.769(2) . . yes S(2) C(5) 1.777(2) . . yes S(2) C(6) 1.773(2) . . yes S(3) C(10) 1.770(2) . . yes S(3) C(11) 1.781(2) . . yes S(4) C(15) 1.777(2) . . yes S(4) C(16) 1.768(2) . . yes N(1) C(1) 1.337(3) . . yes N(1) C(5) 1.327(2) . . yes N(2) C(6) 1.333(3) . . yes N(2) C(10) 1.327(2) . . yes N(3) C(11) 1.332(2) . . yes N(3) C(15) 1.332(3) . . yes N(4) C(16) 1.330(2) . . yes N(4) C(20) 1.334(2) . . yes C(1) C(2) 1.377(3) . . yes C(2) C(3) 1.371(3) . . yes C(2) H(1) 0.893 . . no C(3) C(4) 1.366(4) . . yes C(3) H(2) 0.912 . . no C(4) C(5) 1.387(3) . . yes C(4) H(3) 0.889 . . no C(6) C(7) 1.379(3) . . yes C(7) C(8) 1.378(4) . . yes C(7) H(4) 0.941 . . no C(8) C(9) 1.360(4) . . yes C(8) H(5) 0.920 . . no C(9) C(10) 1.389(3) . . yes C(9) H(6) 0.964 . . no C(11) C(12) 1.379(3) . . yes C(12) C(13) 1.379(3) . . yes C(12) H(7) 0.964 . . no C(13) C(14) 1.364(3) . . yes C(13) H(8) 0.909 . . no C(14) C(15) 1.382(3) . . yes C(14) H(9) 0.930 . . no C(16) C(17) 1.388(3) . . yes C(17) C(18) 1.369(4) . . yes C(17) H(10) 0.967 . . no C(18) C(19) 1.375(3) . . yes C(18) H(11) 0.892 . . no C(19) C(20) 1.382(3) . . yes C(19) H(12) 0.970 . . no #--------------------------------------------------------------------------- #-- loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(1) S(1) C(20) 101.74(9) . . . yes C(5) S(2) C(6) 103.21(9) . . . yes C(10) S(3) C(11) 101.57(9) . . . yes C(15) S(4) C(16) 104.40(9) . . . yes C(1) N(1) C(5) 117.2(2) . . . yes C(6) N(2) C(10) 116.9(2) . . . yes C(11) N(3) C(15) 116.5(2) . . . yes C(16) N(4) C(20) 116.7(1) . . . yes S(1) C(1) N(1) 116.2(1) . . . yes S(1) C(1) C(2) 120.5(2) . . . yes N(1) C(1) C(2) 123.3(2) . . . yes C(1) C(2) C(3) 118.2(2) . . . yes C(1) C(2) H(1) 115.9 . . . no C(3) C(2) H(1) 125.9 . . . no C(2) C(3) C(4) 120.0(2) . . . yes C(2) C(3) H(2) 118.8 . . . no C(4) C(3) H(2) 121.2 . . . no C(3) C(4) C(5) 117.9(2) . . . yes C(3) C(4) H(3) 120.8 . . . no C(5) C(4) H(3) 121.3 . . . no S(2) C(5) N(1) 113.7(1) . . . yes S(2) C(5) C(4) 122.6(1) . . . yes N(1) C(5) C(4) 123.5(2) . . . yes S(2) C(6) N(2) 118.3(1) . . . yes S(2) C(6) C(7) 117.9(2) . . . yes N(2) C(6) C(7) 123.6(2) . . . yes C(6) C(7) C(8) 118.0(2) . . . yes C(6) C(7) H(4) 121.5 . . . no C(8) C(7) H(4) 120.5 . . . no C(7) C(8) C(9) 119.7(2) . . . yes C(7) C(8) H(5) 120.3 . . . no C(9) C(8) H(5) 119.9 . . . no C(8) C(9) C(10) 118.1(2) . . . yes C(8) C(9) H(6) 123.5 . . . no C(10) C(9) H(6) 118.3 . . . no S(3) C(10) N(2) 119.0(1) . . . yes S(3) C(10) C(9) 117.3(2) . . . yes N(2) C(10) C(9) 123.6(2) . . . yes S(3) C(11) N(3) 116.5(2) . . . yes S(3) C(11) C(12) 119.5(1) . . . yes N(3) C(11) C(12) 124.0(2) . . . yes C(11) C(12) C(13) 118.0(2) . . . yes C(11) C(12) H(7) 118.7 . . . no C(13) C(12) H(7) 123.2 . . . no C(12) C(13) C(14) 119.3(2) . . . yes C(12) C(13) H(8) 120.9 . . . no C(14) C(13) H(8) 119.8 . . . no C(13) C(14) C(15) 118.5(2) . . . yes C(13) C(14) H(9) 121.2 . . . no C(15) C(14) H(9) 120.3 . . . no S(4) C(15) N(3) 114.4(1) . . . yes S(4) C(15) C(14) 121.6(2) . . . yes N(3) C(15) C(14) 123.7(2) . . . yes S(4) C(16) N(4) 120.4(1) . . . yes S(4) C(16) C(17) 115.7(2) . . . yes N(4) C(16) C(17) 123.9(2) . . . yes C(16) C(17) C(18) 117.8(2) . . . yes C(16) C(17) H(10) 118.1 . . . no C(18) C(17) H(10) 124.1 . . . no C(17) C(18) C(19) 120.0(2) . . . yes C(17) C(18) H(11) 121.4 . . . no C(19) C(18) H(11) 118.6 . . . no C(18) C(19) C(20) 117.8(2) . . . yes C(18) C(19) H(12) 123.7 . . . no C(20) C(19) H(12) 118.3 . . . no S(1) C(20) N(4) 118.9(1) . . . yes S(1) C(20) C(19) 117.1(2) . . . yes N(4) C(20) C(19) 123.9(2) . . . yes #--------------------------------------------------------------------------- #-- loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S(1) C(1) N(1) C(5) -178.4(1) . . . . yes S(1) C(1) C(2) C(3) 177.3(2) . . . . yes S(1) C(20) N(4) C(16) 178.7(1) . . . . yes S(1) C(20) C(19) C(18) -179.2(2) . . . . yes S(2) C(5) N(1) C(1) 176.1(1) . . . . yes S(2) C(5) C(4) C(3) -175.1(2) . . . . yes S(2) C(6) N(2) C(10) -174.4(1) . . . . yes S(2) C(6) C(7) C(8) 172.3(2) . . . . yes S(3) C(10) N(2) C(6) -180.0(1) . . . . yes S(3) C(10) C(9) C(8) -179.8(2) . . . . yes S(3) C(11) N(3) C(15) -176.6(1) . . . . yes S(3) C(11) C(12) C(13) 176.6(2) . . . . yes S(4) C(15) N(3) C(11) 174.1(1) . . . . yes S(4) C(15) C(14) C(13) -173.7(2) . . . . yes S(4) C(16) N(4) C(20) -175.6(2) . . . . yes S(4) C(16) C(17) C(18) 176.8(2) . . . . yes N(1) C(1) S(1) C(20) -73.3(2) . . . . yes N(1) C(1) C(2) C(3) -0.4(3) . . . . yes N(1) C(5) S(2) C(6) 139.2(1) . . . . yes N(1) C(5) C(4) C(3) -0.4(3) . . . . yes N(2) C(6) S(2) C(5) -30.2(2) . . . . yes N(2) C(6) C(7) C(8) -2.1(3) . . . . yes N(2) C(10) S(3) C(11) 0.1(2) . . . . yes N(2) C(10) C(9) C(8) -1.7(3) . . . . yes N(3) C(11) S(3) C(10) -84.2(2) . . . . yes N(3) C(11) C(12) C(13) 0.1(3) . . . . yes N(3) C(15) S(4) C(16) 128.2(1) . . . . yes N(3) C(15) C(14) C(13) 0.2(3) . . . . yes N(4) C(16) S(4) C(15) -5.7(2) . . . . yes N(4) C(16) C(17) C(18) 0.1(3) . . . . yes N(4) C(20) S(1) C(1) -19.2(2) . . . . yes N(4) C(20) C(19) C(18) 1.0(4) . . . . yes C(1) S(1) C(20) C(19) 161.0(2) . . . . yes C(1) N(1) C(5) C(4) 1.0(3) . . . . yes C(1) C(2) C(3) C(4) 0.9(4) . . . . yes C(2) C(1) S(1) C(20) 108.8(2) . . . . yes C(2) C(1) N(1) C(5) -0.6(3) . . . . yes C(2) C(3) C(4) C(5) -0.6(4) . . . . yes C(4) C(5) S(2) C(6) -45.6(2) . . . . yes C(5) S(2) C(6) C(7) 155.1(2) . . . . yes C(6) N(2) C(10) C(9) 1.9(3) . . . . yes C(6) C(7) C(8) C(9) 2.2(4) . . . . yes C(7) C(6) N(2) C(10) 0.0(3) . . . . yes C(7) C(8) C(9) C(10) -0.5(3) . . . . yes C(9) C(10) S(3) C(11) 178.3(2) . . . . yes C(10) S(3) C(11) C(12) 99.0(2) . . . . yes C(11) N(3) C(15) C(14) -0.2(3) . . . . yes C(11) C(12) C(13) C(14) -0.1(4) . . . . yes C(12) C(11) N(3) C(15) 0.0(3) . . . . yes C(12) C(13) C(14) C(15) 0.0(4) . . . . yes C(14) C(15) S(4) C(16) -57.4(2) . . . . yes C(15) S(4) C(16) C(17) 177.5(2) . . . . yes C(16) N(4) C(20) C(19) -1.5(3) . . . . yes C(16) C(17) C(18) C(19) -0.5(4) . . . . yes C(17) C(16) N(4) C(20) 0.9(3) . . . . yes C(17) C(18) C(19) C(20) 0.0(4) . . . . yes C(17) C(18) C(19) C(20) 0.0(4) . . . . yes #--------------------------------------------------------------------------- #-- loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag S(2) S(3) 3.547(1) . 1_455 ? S(3) N(1) 3.266(2) . 1_655 ? S(3) C(5) 3.596(2) . 1_655 ? S(4) C(19) 3.497(3) . 2_333 ? S(4) S(4) 3.506(1) . 2_433 ? N(1) C(17) 3.337(3) . 2_333 ? N(1) C(18) 3.576(3) . 2_333 ? N(4) C(18) 3.486(3) . 2_333 ? N(4) C(17) 3.510(3) . 2_333 ? C(4) C(4) 3.433(5) . 2_344 ? C(8) C(10) 3.460(3) . 2_434 ? C(9) C(9) 3.511(4) . 2_434 ? C(9) C(10) 3.544(3) . 2_434 ? C(16) C(18) 3.475(3) . 2_333 ? C(16) C(19) 3.489(3) . 2_333 ? C(17) C(20) 3.455(3) . 2_333 ? #---- End Included Message -----