# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Xu, Ruren' 'Li, Guanghua' 'Li, Yi' 'Song, Yu' 'Wang, Yu' 'Yu, Jihong' _publ_contact_author_name 'Prof Ruren Xu' _publ_contact_author_address ; State Key Lab. of Inorganic Synthesis & Preparative Chem. Jilin University College of Chemistry Changchun 130023 CHINA ; _publ_contact_author_phone '86 431 8922331 2479' _publ_contact_author_fax '86 431 5671974' _publ_contact_author_email 'rrxu@mail.jlu.edu.cn' _publ_requested_journal 'Chem. Commun.' _publ_requested_coeditor_name ? #============================================================================== # 2. TITLE AND AUTHOR LIST _publ_section_title ; Combinatorial Approach for the Hydrothermal Syntheses of Open-framework Zinc Phosphates ; data_p-1 _database_code_CSD 186431 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H30 N3 O24 P5 Zn6' _chemical_formula_weight 1099.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.984(2) _cell_length_b 12.354(3) _cell_length_c 12.834(3) _cell_angle_alpha 88.32(3) _cell_angle_beta 74.57(3) _cell_angle_gamma 75.81(3) _cell_volume 1478.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.470 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1092 _exptl_absorpt_coefficient_mu 5.163 _exptl_absorpt_correction_type None _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean '15X15 microns' _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 11032 _diffrn_reflns_av_R_equivalents 0.0205 _diffrn_reflns_av_sigmaI/netI 0.0459 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 27.45 _reflns_number_total 6712 _reflns_number_gt 5141 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXP-97' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0619P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6712 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0508 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.1011 _refine_ls_wR_factor_gt 0.0883 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.14229(6) -0.26149(5) 1.23476(4) 0.00955(12) Uani 1 1 d . . . Zn2 Zn -0.06753(6) -0.02401(5) 1.38030(4) 0.01053(13) Uani 1 1 d . . . Zn3 Zn -0.47358(6) -0.26107(5) 1.25653(4) 0.00875(12) Uani 1 1 d . . . Zn4 Zn -0.14691(6) -0.42805(5) 1.40013(4) 0.00960(12) Uani 1 1 d . . . Zn5 Zn -0.34002(6) 0.38926(5) 1.53622(4) 0.01085(13) Uani 1 1 d . . . Zn6 Zn -0.54126(6) -0.55773(5) 1.15085(4) 0.00969(12) Uani 1 1 d . . . P1 P -0.18800(13) -0.20473(10) 1.29361(9) 0.0092(2) Uani 1 1 d . . . P2 P -0.22059(13) 0.14054(10) 1.58569(9) 0.0085(2) Uani 1 1 d . . . P3 P -0.37041(14) -0.50720(11) 1.31305(10) 0.0115(2) Uani 1 1 d . . . P4 P -0.19950(13) 0.50232(10) 1.65057(9) 0.0079(2) Uani 1 1 d . . . P5 P 0.41204(13) -0.31490(10) 1.06067(9) 0.0086(2) Uani 1 1 d . . . O1 O 0.1084(4) -0.1436(3) 1.3495(2) 0.0125(7) Uani 1 1 d . . . O2 O -0.0428(4) -0.2597(3) 1.2163(3) 0.0167(8) Uani 1 1 d . . . O3 O 0.2729(4) -0.2231(3) 1.1058(2) 0.0122(7) Uani 1 1 d . . . O4 O 0.2172(4) -0.3871(3) 1.3138(3) 0.0141(7) Uani 1 1 d . . . O5 O -0.1972(4) -0.0819(3) 1.3215(3) 0.0149(7) Uani 1 1 d . . . O6 O -0.1678(4) 0.0282(3) 1.5237(3) 0.0140(7) Uani 1 1 d . . . O7 O -0.0055(4) 0.0944(3) 1.2824(3) 0.0210(8) Uani 1 1 d . . . O8 O -0.3052(4) -0.2035(3) 1.2373(3) 0.0141(7) Uani 1 1 d . . . O9 O -0.4818(3) -0.3929(3) 1.3470(3) 0.0124(7) Uani 1 1 d . . . O10 O -0.4720(4) -0.2996(3) 1.1121(2) 0.0138(7) Uani 1 1 d . . . O11 O -0.6345(4) -0.1479(3) 1.3358(3) 0.0139(7) Uani 1 1 d . . . O12 O -0.2100(4) -0.2680(3) 1.4002(3) 0.0150(7) Uani 1 1 d . . . O13 O -0.2198(4) -0.4868(3) 1.2920(3) 0.0169(8) Uani 1 1 d . . . O14 O 0.0482(4) -0.5167(3) 1.3647(3) 0.0130(7) Uani 1 1 d . . . O15 O -0.2234(4) 0.2358(3) 1.5077(2) 0.0131(7) Uani 1 1 d . . . O16 O -0.2391(3) 0.5128(3) 1.5395(2) 0.0119(7) Uani 1 1 d . . . O17 O -0.4009(4) 0.4155(3) 1.4053(3) 0.0185(8) Uani 1 1 d . . . O18 O -0.3807(4) -0.5537(3) 1.2083(3) 0.0158(7) Uani 1 1 d . . . O19 O -0.6945(3) -0.5952(3) 1.2709(3) 0.0129(7) Uani 1 1 d . . . O20 O -0.6238(4) -0.4282(3) 1.0822(2) 0.0138(7) Uani 1 1 d . . . O21 O -0.4670(3) -0.6963(3) 1.0621(2) 0.0107(7) Uani 1 1 d . . . O1W O 0.2936(5) 0.1604(4) 0.9814(3) 0.0405(12) Uani 1 1 d . . . O2W O -0.0462(5) -0.2574(4) 0.6073(4) 0.0374(11) Uani 1 1 d . . . O3W O 0.2338(5) 0.0087(4) 1.1376(3) 0.0334(10) Uani 1 1 d . . . C1 C 0.1516(9) 0.4683(9) 0.9702(7) 0.062(3) Uani 1 1 d . . . H1A H 0.1721 0.3952 0.9356 0.080 Uiso 1 1 calc . . . H1B H 0.2423 0.4861 0.9661 0.080 Uiso 1 1 calc . . . C2 C -0.0773(8) 0.5345(6) 0.9217(6) 0.0409(17) Uani 1 1 d . . . H2A H -0.1349 0.5908 0.8866 0.080 Uiso 1 1 calc . . . H2B H -0.0635 0.4628 0.8862 0.080 Uiso 1 1 calc . . . C3 C 0.0705(10) 0.6694(10) 0.9376(9) 0.097(4) Uani 1 1 d . . . H3A H 0.1692 0.6704 0.9257 0.146 Uiso 1 1 calc . . . H3B H 0.0213 0.6863 1.0126 0.146 Uiso 1 1 calc . . . H3C H 0.0266 0.7242 0.8942 0.146 Uiso 1 1 calc . . . C4 C 0.6247(6) 0.1863(5) 0.3050(4) 0.0231(12) Uani 1 1 d . . . H4A H 0.6221 0.2550 0.2662 0.080 Uiso 1 1 calc . . . H4B H 0.7120 0.1688 0.3285 0.080 Uiso 1 1 calc . . . C5 C 0.5005(7) 0.2068(7) 0.4025(6) 0.0440(19) Uani 1 1 d . . . H5A H 0.5260 0.1569 0.4578 0.080 Uiso 1 1 calc . . . H5B H 0.4840 0.2826 0.4299 0.080 Uiso 1 1 calc . . . C6 C 0.3779(7) 0.1053(6) 0.3137(6) 0.0371(16) Uani 1 1 d . . . H6A H 0.2909 0.1238 0.2898 0.080 Uiso 1 1 calc . . . H6B H 0.3786 0.0370 0.3531 0.080 Uiso 1 1 calc . . . C7 C 0.5002(7) 0.0826(5) 0.2179(4) 0.0260(13) Uani 1 1 d . . . H7A H 0.5164 0.0059 0.1931 0.080 Uiso 1 1 calc . . . H7B H 0.4745 0.1302 0.1613 0.080 Uiso 1 1 calc . . . C8 C 0.7535(6) 0.0845(5) 0.1327(5) 0.0280(13) Uani 1 1 d . . . H8A H 0.7556 0.0217 0.0895 0.042 Uiso 1 1 calc . . . H8B H 0.8418 0.0720 0.1531 0.042 Uiso 1 1 calc . . . H8C H 0.7419 0.1508 0.0917 0.042 Uiso 1 1 calc . . . N1 N 0.0617(7) 0.5589(5) 0.9076(4) 0.0376(14) Uani 1 1 d . . . H1 H 0.1079 0.5469 0.8359 0.080 Uiso 1 1 calc . . . N2 N 0.6329(7) 0.0983(7) 0.2305(6) 0.077(3) Uani 1 1 d . . . H2 H 0.6622 0.0365 0.2668 0.080 Uiso 1 1 calc . . . N3 N 0.3709(7) 0.1925(7) 0.3873(4) 0.060(2) Uani 1 1 d . . . H3D H 0.3254 0.2573 0.3648 0.080 Uiso 1 1 calc . . . H3E H 0.3155 0.1805 0.4523 0.080 Uiso 1 1 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0080(3) 0.0102(3) 0.0099(2) 0.0002(2) -0.0019(2) -0.0017(2) Zn2 0.0097(3) 0.0093(3) 0.0117(2) -0.0011(2) -0.0026(2) -0.0008(2) Zn3 0.0082(3) 0.0087(3) 0.0092(2) -0.00041(19) -0.0024(2) -0.0018(2) Zn4 0.0092(3) 0.0098(3) 0.0108(2) 0.0013(2) -0.0041(2) -0.0027(2) Zn5 0.0117(3) 0.0090(3) 0.0127(3) 0.0013(2) -0.0040(2) -0.0034(2) Zn6 0.0109(3) 0.0095(3) 0.0091(2) -0.00037(19) -0.0040(2) -0.0017(2) P1 0.0087(6) 0.0086(6) 0.0109(5) 0.0008(4) -0.0038(4) -0.0021(5) P2 0.0073(6) 0.0072(6) 0.0096(5) -0.0014(4) -0.0019(4) 0.0003(5) P3 0.0119(6) 0.0083(6) 0.0161(6) -0.0008(5) -0.0087(5) -0.0005(5) P4 0.0078(6) 0.0076(6) 0.0085(5) 0.0003(4) -0.0022(4) -0.0021(5) P5 0.0093(6) 0.0087(6) 0.0071(5) -0.0006(4) -0.0021(4) -0.0010(5) O1 0.0126(18) 0.0117(18) 0.0127(15) -0.0027(13) -0.0054(13) 0.0006(14) O2 0.0078(17) 0.026(2) 0.0169(17) -0.0035(15) -0.0041(14) -0.0032(16) O3 0.0121(17) 0.0101(18) 0.0111(15) 0.0024(13) -0.0002(13) -0.0003(14) O4 0.0184(19) 0.0109(18) 0.0136(15) 0.0032(13) -0.0045(14) -0.0046(15) O5 0.0154(18) 0.0083(18) 0.0241(18) 0.0022(14) -0.0103(15) -0.0036(15) O6 0.0155(18) 0.0093(18) 0.0145(16) -0.0036(13) -0.0006(13) -0.0011(15) O7 0.023(2) 0.014(2) 0.0269(19) 0.0075(15) -0.0066(16) -0.0063(17) O8 0.0108(18) 0.019(2) 0.0151(16) 0.0051(14) -0.0055(13) -0.0077(15) O9 0.0101(17) 0.0093(18) 0.0165(16) 0.0026(13) -0.0020(13) -0.0017(14) O10 0.0116(17) 0.018(2) 0.0116(15) -0.0026(13) -0.0042(13) -0.0022(15) O11 0.0082(17) 0.0104(18) 0.0176(16) -0.0024(13) 0.0034(13) 0.0007(14) O12 0.021(2) 0.0107(18) 0.0128(16) 0.0026(13) -0.0047(14) -0.0040(15) O13 0.0094(17) 0.022(2) 0.0202(17) -0.0072(15) -0.0072(14) -0.0004(15) O14 0.0098(17) 0.0138(18) 0.0159(16) -0.0011(13) -0.0040(13) -0.0031(14) O15 0.0135(18) 0.0117(18) 0.0123(15) 0.0017(13) -0.0029(13) -0.0001(15) O16 0.0115(17) 0.0154(19) 0.0111(15) 0.0021(13) -0.0052(13) -0.0052(15) O17 0.032(2) 0.0093(18) 0.0198(17) 0.0033(14) -0.0172(16) -0.0038(16) O18 0.0183(19) 0.0147(19) 0.0189(17) -0.0006(14) -0.0123(15) -0.0043(16) O19 0.0110(17) 0.0098(18) 0.0153(16) -0.0022(13) -0.0003(13) -0.0007(14) O20 0.0167(19) 0.0113(18) 0.0142(16) 0.0045(13) -0.0062(14) -0.0034(15) O21 0.0129(17) 0.0086(17) 0.0076(14) 0.0006(12) 0.0002(12) -0.0005(14) O1W 0.051(3) 0.045(3) 0.033(2) 0.019(2) -0.011(2) -0.028(3) O2W 0.032(3) 0.018(2) 0.052(3) -0.0027(19) 0.008(2) -0.008(2) O3W 0.043(3) 0.025(2) 0.024(2) -0.0009(17) 0.0070(18) -0.011(2) C1 0.044(5) 0.100(8) 0.051(5) 0.009(5) -0.018(4) -0.029(5) C2 0.056(5) 0.028(4) 0.047(4) -0.005(3) -0.040(4) 0.004(3) C3 0.047(6) 0.116(10) 0.118(9) -0.076(7) 0.015(5) -0.030(6) C4 0.034(3) 0.015(3) 0.026(3) 0.002(2) -0.014(2) -0.009(3) C5 0.023(3) 0.056(5) 0.052(4) -0.031(4) -0.001(3) -0.013(3) C6 0.023(3) 0.032(4) 0.058(4) -0.020(3) -0.016(3) -0.003(3) C7 0.035(3) 0.029(3) 0.020(3) 0.002(2) -0.012(2) -0.014(3) C8 0.025(3) 0.024(3) 0.032(3) 0.001(2) -0.009(2) 0.002(3) N1 0.071(4) 0.027(3) 0.017(2) 0.001(2) -0.004(2) -0.025(3) N2 0.031(4) 0.118(7) 0.077(5) -0.079(5) 0.012(3) -0.028(4) N3 0.052(4) 0.102(6) 0.032(3) -0.031(3) 0.012(3) -0.053(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O2 1.920(3) . ? Zn1 O4 1.934(3) . ? Zn1 O3 1.943(3) . ? Zn1 O1 2.006(3) . ? Zn2 O6 1.892(3) . ? Zn2 O5 1.940(3) . ? Zn2 O1 1.954(3) . ? Zn2 O7 2.006(3) . ? Zn3 O11 1.919(3) . ? Zn3 O10 1.922(3) . ? Zn3 O8 1.936(3) . ? Zn3 O9 1.977(3) . ? Zn4 O12 1.922(4) . ? Zn4 O14 1.927(3) . ? Zn4 O13 1.959(3) . ? Zn4 O16 1.989(3) 1_545 ? Zn5 O17 1.927(3) . ? Zn5 O15 1.953(4) . ? Zn5 O9 1.990(3) 2_458 ? Zn5 O16 2.031(3) . ? Zn5 P4 2.8723(14) . ? Zn6 O20 1.917(3) . ? Zn6 O18 1.946(3) . ? Zn6 O21 1.955(3) . ? Zn6 O19 1.995(3) . ? P1 O8 1.527(3) . ? P1 O2 1.529(4) . ? P1 O5 1.544(4) . ? P1 O12 1.547(3) . ? P2 O11 1.511(3) 2_458 ? P2 O15 1.522(3) . ? P2 O6 1.523(4) . ? P2 O1 1.570(3) 2_558 ? P3 O17 1.514(3) 1_545 ? P3 O18 1.516(3) . ? P3 O13 1.537(3) . ? P3 O9 1.559(4) . ? P4 O4 1.519(3) 2_558 ? P4 O14 1.524(3) 2_558 ? P4 O19 1.535(3) 2_458 ? P4 O16 1.572(3) . ? P5 O20 1.527(3) 1_655 ? P5 O10 1.527(3) 1_655 ? P5 O21 1.539(3) 2_547 ? P5 O3 1.546(4) . ? O1 P2 1.570(3) 2_558 ? O4 P4 1.519(3) 2_558 ? O9 Zn5 1.990(3) 2_458 ? O10 P5 1.527(3) 1_455 ? O11 P2 1.511(3) 2_458 ? O14 P4 1.524(3) 2_558 ? O16 Zn4 1.989(3) 1_565 ? O17 P3 1.514(3) 1_565 ? O19 P4 1.535(3) 2_458 ? O20 P5 1.527(3) 1_455 ? O21 P5 1.539(3) 2_547 ? C1 C2 1.392(10) 2_567 ? C1 N1 1.595(10) . ? C2 C1 1.392(10) 2_567 ? C2 N1 1.456(9) . ? C3 N1 1.459(11) . ? C4 N2 1.441(8) . ? C4 C5 1.486(8) . ? C5 N3 1.412(8) . ? C6 N3 1.430(8) . ? C6 C7 1.461(9) . ? C7 N2 1.435(8) . ? C8 N2 1.471(8) . ? 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_3 _geom_angle_publ_flag O2 Zn1 O4 113.55(15) . . ? O2 Zn1 O3 113.53(14) . . ? O4 Zn1 O3 117.55(15) . . ? O2 Zn1 O1 106.07(14) . . ? O4 Zn1 O1 96.60(14) . . ? O3 Zn1 O1 107.17(14) . . ? O6 Zn2 O5 106.96(15) . . ? O6 Zn2 O1 121.29(14) . . ? O5 Zn2 O1 104.26(14) . . ? O6 Zn2 O7 114.22(15) . . ? O5 Zn2 O7 107.51(15) . . ? O1 Zn2 O7 101.57(15) . . ? O11 Zn3 O10 117.05(15) . . ? O11 Zn3 O8 107.04(15) . . ? O10 Zn3 O8 104.23(14) . . ? O11 Zn3 O9 103.25(14) . . ? O10 Zn3 O9 109.31(14) . . ? O8 Zn3 O9 116.47(14) . . ? O12 Zn4 O14 127.00(15) . . ? O12 Zn4 O13 106.47(15) . . ? O14 Zn4 O13 101.00(14) . . ? O12 Zn4 O16 111.35(14) . 1_545 ? O14 Zn4 O16 103.85(14) . 1_545 ? O13 Zn4 O16 104.90(14) . 1_545 ? O17 Zn5 O15 100.75(15) . . ? O17 Zn5 O9 105.21(15) . 2_458 ? O15 Zn5 O9 109.72(14) . 2_458 ? O17 Zn5 O16 102.82(14) . . ? O15 Zn5 O16 118.16(14) . . ? O9 Zn5 O16 117.51(14) 2_458 . ? O17 Zn5 P4 134.55(11) . . ? O15 Zn5 P4 106.41(11) . . ? O9 Zn5 P4 99.05(10) 2_458 . ? O16 Zn5 P4 31.90(9) . . ? O20 Zn6 O18 118.43(15) . . ? O20 Zn6 O21 116.06(13) . . ? O18 Zn6 O21 101.82(15) . . ? O20 Zn6 O19 108.92(14) . . ? O18 Zn6 O19 107.85(14) . . ? O21 Zn6 O19 102.33(13) . . ? O8 P1 O2 108.60(19) . . ? O8 P1 O5 107.00(19) . . ? O2 P1 O5 111.2(2) . . ? O8 P1 O12 112.05(19) . . ? O2 P1 O12 109.9(2) . . ? O5 P1 O12 108.10(19) . . ? O11 P2 O15 112.2(2) 2_458 . ? O11 P2 O6 109.9(2) 2_458 . ? O15 P2 O6 110.49(19) . . ? O11 P2 O1 109.29(19) 2_458 2_558 ? O15 P2 O1 108.89(19) . 2_558 ? O6 P2 O1 105.88(19) . 2_558 ? O17 P3 O18 111.7(2) 1_545 . ? O17 P3 O13 112.2(2) 1_545 . ? O18 P3 O13 107.22(19) . . ? O17 P3 O9 107.0(2) 1_545 . ? O18 P3 O9 110.8(2) . . ? O13 P3 O9 107.88(19) . . ? O4 P4 O14 114.0(2) 2_558 2_558 ? O4 P4 O19 111.86(19) 2_558 2_458 ? O14 P4 O19 108.83(19) 2_558 2_458 ? O4 P4 O16 103.40(18) 2_558 . ? O14 P4 O16 110.14(18) 2_558 . ? O19 P4 O16 108.43(19) 2_458 . ? O4 P4 Zn5 61.89(13) 2_558 . ? O14 P4 Zn5 136.46(14) 2_558 . ? O19 P4 Zn5 112.42(14) 2_458 . ? O16 P4 Zn5 43.08(12) . . ? O20 P5 O10 113.05(19) 1_655 1_655 ? O20 P5 O21 109.15(19) 1_655 2_547 ? O10 P5 O21 107.55(19) 1_655 2_547 ? O20 P5 O3 107.89(19) 1_655 . ? O10 P5 O3 109.6(2) 1_655 . ? O21 P5 O3 109.53(18) 2_547 . ? P2 O1 Zn2 117.75(19) 2_558 . ? P2 O1 Zn1 122.6(2) 2_558 . ? Zn2 O1 Zn1 119.58(16) . . ? P1 O2 Zn1 126.4(2) . . ? P5 O3 Zn1 114.90(18) . . ? P4 O4 Zn1 142.4(2) 2_558 . ? P1 O5 Zn2 128.1(2) . . ? P2 O6 Zn2 136.3(2) . . ? P1 O8 Zn3 139.2(2) . . ? P3 O9 Zn3 121.56(19) . . ? P3 O9 Zn5 118.48(18) . 2_458 ? Zn3 O9 Zn5 118.38(17) . 2_458 ? P5 O10 Zn3 133.4(2) 1_455 . ? P2 O11 Zn3 138.3(2) 2_458 . ? P1 O12 Zn4 121.2(2) . . ? P3 O13 Zn4 124.9(2) . . ? P4 O14 Zn4 139.6(2) 2_558 . ? P2 O15 Zn5 127.5(2) . . ? P4 O16 Zn4 130.73(19) . 1_565 ? P4 O16 Zn5 105.02(17) . . ? Zn4 O16 Zn5 118.77(15) 1_565 . ? P3 O17 Zn5 133.1(2) 1_565 . ? P3 O18 Zn6 133.2(2) . . ? P4 O19 Zn6 119.87(19) 2_458 . ? P5 O20 Zn6 132.4(2) 1_455 . ? P5 O21 Zn6 116.78(19) 2_547 . ? C2 C1 N1 111.4(7) 2_567 . ? C1 C2 N1 113.2(6) 2_567 . ? N2 C4 C5 116.1(5) . . ? N3 C5 C4 115.8(5) . . ? N3 C6 C7 116.7(5) . . ? N2 C7 C6 116.7(5) . . ? C2 N1 C3 120.2(6) . . ? C2 N1 C1 107.9(5) . . ? C3 N1 C1 108.3(7) . . ? C7 N2 C4 117.4(6) . . ? C7 N2 C8 117.1(5) . . ? C4 N2 C8 114.2(6) . . ? C5 N3 C6 118.2(6) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O13 0.91 1.78 2.671(6) 164.2 2_557 N1 H1 O18 0.91 2.65 3.121(7) 112.9 2_557 N2 H2 O5 0.91 2.01 2.872(10) 156.4 1_654 N3 H3E O12 0.90 2.09 2.823(6) 138.1 2_557 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.552 _refine_diff_density_min -1.738 _refine_diff_density_rms 0.276 data_C _database_code_CSD 186432 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H16 N2 O17 P4 Zn5' _chemical_formula_weight 814.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 20.7940(9) _cell_length_b 5.2272(2) _cell_length_c 17.9628(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1952.46(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.772 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 6.471 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.1887 _exptl_absorpt_correction_T_max 0.3316 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean '15X15 microns' _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 8819 _diffrn_reflns_av_R_equivalents 0.0590 _diffrn_reflns_av_sigmaI/netI 0.0441 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 23.28 _reflns_number_total 2448 _reflns_number_gt 2233 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXP-97' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0576P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.394(19) _refine_ls_number_reflns 2448 _refine_ls_number_parameters 289 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0393 _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_ref 0.0851 _refine_ls_wR_factor_gt 0.0827 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.64889(5) 0.28434(19) 0.46652(6) 0.0149(3) Uani 1 1 d . . . Zn2 Zn 0.74644(4) 0.77233(19) 0.49751(7) 0.0146(3) Uani 1 1 d . . . Zn3 Zn 0.50064(4) 0.7263(2) 0.44990(7) 0.0166(3) Uani 1 1 d . . . Zn4 Zn 0.74987(4) 0.6133(2) 0.26270(7) 0.0169(3) Uani 1 1 d . . . Zn5 Zn 0.37115(5) 0.34858(19) 0.48363(6) 0.0148(3) Uani 1 1 d . . . P1 P 0.75730(11) 0.2635(4) 0.58705(15) 0.0128(5) Uani 1 1 d . . . P2 P 0.63930(10) 0.7698(5) 0.36921(14) 0.0118(5) Uani 1 1 d . . . P3 P 0.51169(12) 0.2511(5) 0.54428(16) 0.0153(6) Uani 1 1 d . . . P4 P 0.85888(11) 0.6484(5) 0.38579(14) 0.0129(5) Uani 1 1 d . . . O1 O 0.6809(3) 0.6248(12) 0.4290(3) 0.0152(14) Uani 1 1 d . . . O2 O 0.7198(3) 0.1221(11) 0.5220(3) 0.0145(14) Uani 1 1 d . . . O3 O 0.5764(3) 0.3651(15) 0.5252(4) 0.0272(17) Uani 1 1 d . . . O4 O 0.6494(3) 0.0603(12) 0.3794(3) 0.0183(15) Uani 1 1 d . . . O5 O 0.7428(3) 0.5471(12) 0.5799(4) 0.0200(15) Uani 1 1 d . . . O6 O 0.5699(3) 0.6905(14) 0.3783(4) 0.0235(16) Uani 1 1 d . . . O7 O 0.4634(3) 0.3998(11) 0.4928(4) 0.0194(15) Uani 1 1 d . . . O8 O 0.4304(3) 0.8071(14) 0.3806(4) 0.0231(16) Uani 1 1 d . . . O9 O 0.5067(4) 0.9669(15) 0.5276(5) 0.0342(19) Uani 1 1 d . . . O10 O 0.6620(3) 0.6946(12) 0.2915(4) 0.0161(15) Uani 1 1 d . . . O11 O 0.8269(3) 0.7309(13) 0.3131(4) 0.0212(16) Uani 1 1 d . . . O12 O 0.7519(3) 0.2373(13) 0.2952(5) 0.0247(18) Uani 1 1 d . . . O13 O 0.7683(3) 0.6632(13) 0.1605(4) 0.0208(16) Uani 1 1 d . . . O14 O 0.3320(3) 0.6841(12) 0.4517(4) 0.0193(15) Uani 1 1 d . . . O15 O 0.3418(3) 0.1312(12) 0.4021(4) 0.0200(16) Uani 1 1 d . . . O16 O 0.3287(3) 0.2950(13) 0.5764(4) 0.0218(16) Uani 1 1 d . . . O17 O 0.4955(3) 0.3022(14) 0.6236(5) 0.0250(18) Uani 1 1 d . . . C1 C -0.1152(6) 0.241(3) 0.1768(9) 0.047(4) Uani 1 1 d . . . H1A H -0.1450 0.1657 0.1423 0.080 Uiso 1 1 calc . . . H1B H -0.0848 0.3442 0.1501 0.080 Uiso 1 1 calc . . . H1C H -0.1382 0.3456 0.2117 0.080 Uiso 1 1 calc . . . C2 C -0.0315(5) 0.133(2) 0.2747(7) 0.038(3) Uani 1 1 d . . . H2A H -0.0539 0.2348 0.3117 0.080 Uiso 1 1 calc . . . H2B H -0.0128 -0.0129 0.2999 0.080 Uiso 1 1 calc . . . C3 C 0.0212(5) 0.290(2) 0.2419(8) 0.040(3) Uani 1 1 d . . . H3A H 0.0401 0.3943 0.2809 0.080 Uiso 1 1 calc . . . H3B H 0.0030 0.4050 0.2051 0.080 Uiso 1 1 calc . . . C4 C 0.1217(6) 0.302(3) 0.1664(7) 0.039(3) Uani 1 1 d . . . H4A H 0.1541 0.1979 0.1433 0.080 Uiso 1 1 calc . . . H4B H 0.1414 0.4143 0.2019 0.080 Uiso 1 1 calc . . . H4C H 0.1000 0.4007 0.1291 0.080 Uiso 1 1 calc . . . N1 N -0.0808(4) 0.0364(18) 0.2172(5) 0.033(2) Uani 1 1 d . . . H1A' H -0.0603 -0.0628 0.1838 0.080 Uiso 1 1 calc . . . H1B' H -0.1099 -0.0621 0.2408 0.080 Uiso 1 1 calc . . . N2 N 0.0740(4) 0.1325(16) 0.2054(6) 0.028(2) Uani 1 1 d . . . H2A' H 0.0944 0.0393 0.2403 0.080 Uiso 1 1 calc . . . H2B' H 0.0564 0.0238 0.1723 0.080 Uiso 1 1 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0126(5) 0.0148(6) 0.0174(7) 0.0000(5) -0.0009(4) -0.0002(4) Zn2 0.0131(6) 0.0146(6) 0.0163(7) -0.0004(5) -0.0008(4) -0.0013(4) Zn3 0.0125(6) 0.0184(6) 0.0189(7) -0.0009(5) 0.0009(4) -0.0024(5) Zn4 0.0127(5) 0.0241(6) 0.0139(6) 0.0015(5) -0.0001(4) 0.0003(5) Zn5 0.0119(5) 0.0158(5) 0.0168(6) -0.0006(5) -0.0011(4) -0.0002(5) P1 0.0140(13) 0.0138(12) 0.0105(14) -0.0004(11) 0.0010(10) 0.0003(10) P2 0.0069(11) 0.0136(13) 0.0148(14) 0.0022(10) -0.0016(10) 0.0005(9) P3 0.0130(12) 0.0139(13) 0.0189(15) -0.0005(11) -0.0020(11) 0.0001(10) P4 0.0104(12) 0.0154(13) 0.0130(14) 0.0002(10) -0.0004(9) 0.0001(10) O1 0.019(3) 0.015(3) 0.011(4) 0.008(3) -0.002(3) -0.001(3) O2 0.015(3) 0.012(3) 0.017(4) -0.004(3) -0.008(3) 0.004(3) O3 0.015(4) 0.039(4) 0.027(4) -0.004(3) 0.009(3) -0.007(3) O4 0.026(3) 0.017(4) 0.012(4) 0.002(3) 0.000(3) 0.004(3) O5 0.031(4) 0.014(3) 0.015(4) 0.003(3) 0.000(3) 0.004(3) O6 0.013(3) 0.037(4) 0.021(4) -0.005(3) -0.001(3) -0.003(3) O7 0.007(3) 0.022(3) 0.029(4) 0.011(3) -0.004(3) -0.004(3) O8 0.015(3) 0.033(4) 0.021(4) 0.003(3) 0.004(3) 0.002(3) O9 0.054(5) 0.016(4) 0.032(5) -0.002(3) -0.007(4) 0.004(3) O10 0.013(3) 0.022(4) 0.012(4) 0.000(3) 0.002(3) 0.000(3) O11 0.024(4) 0.027(4) 0.012(4) 0.009(3) -0.004(3) -0.011(3) O12 0.024(4) 0.024(4) 0.026(5) -0.001(3) 0.001(3) 0.003(3) O13 0.020(4) 0.021(4) 0.021(4) 0.003(3) 0.002(3) 0.005(3) O14 0.014(3) 0.018(3) 0.026(4) 0.006(3) 0.002(3) 0.004(3) O15 0.023(4) 0.013(4) 0.024(4) -0.002(3) -0.009(3) -0.003(3) O16 0.013(4) 0.032(4) 0.021(4) 0.000(3) -0.002(3) -0.010(3) O17 0.023(4) 0.030(4) 0.022(5) -0.007(3) -0.001(3) -0.002(3) C1 0.022(7) 0.061(10) 0.060(9) -0.009(7) -0.012(6) -0.008(6) C2 0.037(6) 0.045(7) 0.032(8) 0.005(6) 0.006(6) 0.003(6) C3 0.026(6) 0.049(8) 0.047(9) -0.022(6) 0.000(6) -0.011(5) C4 0.031(7) 0.032(7) 0.052(9) 0.000(6) 0.008(6) -0.008(6) N1 0.028(5) 0.036(6) 0.035(6) -0.009(5) 0.003(4) -0.001(4) N2 0.027(5) 0.025(5) 0.033(5) 0.002(5) -0.007(4) 0.003(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O3 1.887(6) . ? Zn1 O4 1.954(6) . ? Zn1 O2 1.972(6) . ? Zn1 O1 2.016(6) . ? Zn2 O5 1.893(7) . ? Zn2 O2 1.960(6) 1_565 ? Zn2 O14 1.973(6) 3_565 ? Zn2 O1 1.993(6) . ? Zn3 O9 1.883(8) . ? Zn3 O6 1.940(7) . ? Zn3 O8 1.965(7) . ? Zn3 O7 2.027(6) . ? Zn4 O13 1.893(7) . ? Zn4 O11 1.940(7) . ? Zn4 O10 1.946(6) . ? Zn4 O12 2.051(7) . ? Zn5 O16 1.907(6) . ? Zn5 O7 1.943(6) . ? Zn5 O15 1.952(6) . ? Zn5 O14 2.017(6) . ? P1 O13 1.516(7) 4_645 ? P1 O5 1.518(7) . ? P1 O16 1.527(7) 3 ? P1 O2 1.587(6) . ? P2 O6 1.511(6) . ? P2 O10 1.526(7) . ? P2 O4 1.544(7) 1_565 ? P2 O1 1.573(6) . ? P3 O17 1.488(9) . ? P3 O3 1.511(7) . ? P3 O9 1.519(8) 1_545 ? P3 O7 1.571(6) . ? P4 O8 1.508(6) 3_565 ? P4 O11 1.527(7) . ? P4 O15 1.532(7) 3 ? P4 O14 1.575(7) 3_565 ? O2 Zn2 1.960(6) 1_545 ? O4 P2 1.544(7) 1_545 ? O8 P4 1.508(6) 3_465 ? O9 P3 1.519(8) 1_565 ? O13 P1 1.516(7) 4_654 ? O14 P4 1.575(7) 3_465 ? O14 Zn2 1.973(6) 3_465 ? O15 P4 1.532(7) 3_455 ? O16 P1 1.527(7) 3_455 ? C1 N1 1.477(17) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.490(17) . ? C2 N1 1.540(15) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 N2 1.523(15) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 N2 1.501(14) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? 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_3 _geom_angle_publ_flag O3 Zn1 O4 125.8(3) . . ? O3 Zn1 O2 114.3(3) . . ? O4 Zn1 O2 98.2(2) . . ? O3 Zn1 O1 104.7(3) . . ? O4 Zn1 O1 105.0(3) . . ? O2 Zn1 O1 107.6(2) . . ? O5 Zn2 O2 113.1(3) . 1_565 ? O5 Zn2 O14 115.7(3) . 3_565 ? O2 Zn2 O14 103.9(3) 1_565 3_565 ? O5 Zn2 O1 102.4(3) . . ? O2 Zn2 O1 107.8(3) 1_565 . ? O14 Zn2 O1 113.8(3) 3_565 . ? O9 Zn3 O6 120.4(3) . . ? O9 Zn3 O8 112.1(3) . . ? O6 Zn3 O8 98.8(3) . . ? O9 Zn3 O7 107.8(3) . . ? O6 Zn3 O7 117.1(3) . . ? O8 Zn3 O7 97.9(3) . . ? O13 Zn4 O11 104.0(3) . . ? O13 Zn4 O10 114.7(3) . . ? O11 Zn4 O10 125.6(3) . . ? O13 Zn4 O12 113.8(3) . . ? O11 Zn4 O12 98.9(3) . . ? O10 Zn4 O12 98.8(3) . . ? O16 Zn5 O7 113.8(3) . . ? O16 Zn5 O15 115.2(3) . . ? O7 Zn5 O15 116.9(3) . . ? O16 Zn5 O14 100.9(3) . . ? O7 Zn5 O14 107.6(3) . . ? O15 Zn5 O14 99.6(3) . . ? O13 P1 O5 110.0(4) 4_645 . ? O13 P1 O16 112.4(4) 4_645 3 ? O5 P1 O16 112.2(4) . 3 ? O13 P1 O2 107.9(4) 4_645 . ? O5 P1 O2 107.2(4) . . ? O16 P1 O2 107.0(4) 3 . ? O6 P2 O10 108.9(4) . . ? O6 P2 O4 112.7(4) . 1_565 ? O10 P2 O4 108.7(4) . 1_565 ? O6 P2 O1 108.6(4) . . ? O10 P2 O1 109.3(4) . . ? O4 P2 O1 108.6(4) 1_565 . ? O17 P3 O3 110.4(4) . . ? O17 P3 O9 110.4(5) . 1_545 ? O3 P3 O9 113.7(4) . 1_545 ? O17 P3 O7 109.2(4) . . ? O3 P3 O7 103.9(4) . . ? O9 P3 O7 108.9(4) 1_545 . ? O8 P4 O11 109.5(4) 3_565 . ? O8 P4 O15 112.8(4) 3_565 3 ? O11 P4 O15 109.4(4) . 3 ? O8 P4 O14 108.1(4) 3_565 3_565 ? O11 P4 O14 109.3(4) . 3_565 ? O15 P4 O14 107.8(4) 3 3_565 ? P2 O1 Zn2 127.7(4) . . ? P2 O1 Zn1 118.2(3) . . ? Zn2 O1 Zn1 111.1(3) . . ? P1 O2 Zn2 117.5(3) . 1_545 ? P1 O2 Zn1 122.6(3) . . ? Zn2 O2 Zn1 119.9(3) 1_545 . ? P3 O3 Zn1 138.6(5) . . ? P2 O4 Zn1 133.2(4) 1_545 . ? P1 O5 Zn2 131.7(4) . . ? P2 O6 Zn3 139.0(5) . . ? P3 O7 Zn5 127.8(4) . . ? P3 O7 Zn3 113.3(3) . . ? Zn5 O7 Zn3 117.4(3) . . ? P4 O8 Zn3 136.6(4) 3_465 . ? P3 O9 Zn3 143.5(5) 1_565 . ? P2 O10 Zn4 126.1(4) . . ? P4 O11 Zn4 132.0(4) . . ? P1 O13 Zn4 145.1(4) 4_654 . ? P4 O14 Zn2 124.7(4) 3_465 3_465 ? P4 O14 Zn5 123.6(4) 3_465 . ? Zn2 O14 Zn5 110.2(3) 3_465 . ? P4 O15 Zn5 128.8(4) 3_455 . ? P1 O16 Zn5 126.1(4) 3_455 . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 N1 114.0(10) . . ? C3 C2 H2A 108.8 . . ? N1 C2 H2A 108.8 . . ? C3 C2 H2B 108.8 . . ? N1 C2 H2B 108.8 . . ? H2A C2 H2B 107.7 . . ? C2 C3 N2 113.8(10) . . ? C2 C3 H3A 108.8 . . ? N2 C3 H3A 108.8 . . ? C2 C3 H3B 108.8 . . ? N2 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? N2 C4 H4A 109.5 . . ? N2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C1 N1 C2 114.4(9) . . ? C1 N1 H1A 108.7 . . ? C2 N1 H1A 108.7 . . ? C1 N1 H1B 108.7 . . ? C2 N1 H1B 108.7 . . ? H1A N1 H1B 107.6 . . ? C4 N2 C3 111.0(9) . . ? C4 N2 H2A 109.4 . . ? C3 N2 H2A 109.4 . . ? C4 N2 H2B 109.4 . . ? C3 N2 H2B 109.4 . . ? H2A N2 H2B 108.0 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A O17 0.90 1.87 2.734(11) 161.1 4_544 N1 H1B O11 0.90 2.14 3.034(11) 170.7 1_445 N2 H2A O10 0.90 2.08 2.942(11) 161.0 3_455 N2 H2B O17 0.90 1.81 2.688(11) 165.1 4_544 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.28 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.455 _refine_diff_density_min -0.542 _refine_diff_density_rms 0.109