 
data_nol102m 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C35 H38 Cl N3 Pd' 
_chemical_formula_weight          642.53 
 
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' 
 'Cl'  'Cl'   0.1484   0.1585 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Pd'  'Pd'  -0.9988   1.0072 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            ? 
_symmetry_space_group_name_H-M    ? 
 
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' 
 '-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                    36.834(10) 
_cell_length_b                    12.576(3) 
_cell_length_c                    14.084(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  106.186(5) 
_cell_angle_gamma                 90.00 
_cell_volume                      6265(3) 
_cell_formula_units_Z             8 
_cell_measurement_temperature     150(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           ? 
_exptl_crystal_size_mid           ? 
_exptl_crystal_size_min           ? 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.362 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              2656 
_exptl_absorpt_coefficient_mu     0.705 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
_exptl_absorpt_process_details    ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       150(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   ? 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             11456 
_diffrn_reflns_av_R_equivalents   0.1431 
_diffrn_reflns_av_sigmaI/netI     0.1011 
_diffrn_reflns_limit_h_min        -41 
_diffrn_reflns_limit_h_max        40 
_diffrn_reflns_limit_k_min        -14 
_diffrn_reflns_limit_k_max        13 
_diffrn_reflns_limit_l_min        -11 
_diffrn_reflns_limit_l_max        11 
_diffrn_reflns_theta_min          3.46 
_diffrn_reflns_theta_max          23.47 
_reflns_number_total              3665 
_reflns_number_gt                 2893 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0764P)²+998.6046P] where P=(Fo²+2Fc²)/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          3665 
_refine_ls_number_parameters      373 
_refine_ls_number_restraints      620 
_refine_ls_R_factor_all           0.1041 
_refine_ls_R_factor_gt            0.0869 
_refine_ls_wR_factor_ref          0.1918 
_refine_ls_wR_factor_gt           0.1846 
_refine_ls_goodness_of_fit_ref    1.248 
_refine_ls_restrained_S_all       1.154 
_refine_ls_shift/su_max           0.388 
_refine_ls_shift/su_mean          0.005 
 
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 
Pd1 Pd 0.16654(4) 0.25454(12) 0.10079(13) 0.0150(6) Uani 1 1 d U . . 
Cl1 Cl 0.20786(14) 0.4003(4) 0.0868(4) 0.0215(14) Uani 1 1 d U . . 
N1 N 0.1649(5) 0.1858(14) -0.0459(14) 0.020(3) Uani 1 1 d U . . 
C1 C 0.1268(6) 0.1437(16) 0.1062(19) 0.023(3) Uani 1 1 d U . . 
N2 N 0.1294(5) 0.3580(14) 0.2454(15) 0.022(3) Uani 1 1 d U . . 
C2 C 0.1251(6) 0.0822(18) 0.1809(19) 0.026(4) Uani 1 1 d U . . 
H2 H 0.1441 0.0902 0.2418 0.031 Uiso 1 1 calc R . . 
N3 N 0.1896(4) 0.3495(13) 0.3123(14) 0.016(3) Uani 1 1 d U . . 
C3 C 0.0970(7) 0.006(2) 0.175(2) 0.035(4) Uani 1 1 d U . . 
H3 H 0.0978 -0.0367 0.2314 0.042 Uiso 1 1 calc R . . 
C4 C 0.0679(7) -0.008(2) 0.089(2) 0.038(5) Uani 1 1 d U . . 
H4 H 0.0484 -0.0583 0.0846 0.046 Uiso 1 1 calc R . . 
C5 C 0.0687(7) 0.0567(19) 0.010(2) 0.035(4) Uani 1 1 d U . . 
H5 H 0.0488 0.0495 -0.0496 0.042 Uiso 1 1 calc R . . 
C6 C 0.0968(6) 0.1309(18) 0.0112(19) 0.025(4) Uani 1 1 d U . . 
C7 C 0.0958(6) 0.1963(18) -0.0770(19) 0.026(3) Uani 1 1 d U . . 
C8 C 0.0605(6) 0.2327(19) -0.1359(19) 0.030(4) Uani 1 1 d U . . 
H8 H 0.0382 0.2111 -0.1201 0.036 Uiso 1 1 calc R . . 
C9 C 0.0575(6) 0.299(2) -0.216(2) 0.033(4) Uani 1 1 d U . . 
H9 H 0.0335 0.3235 -0.2546 0.039 Uiso 1 1 calc R . . 
C10 C 0.0891(6) 0.3294(19) -0.239(2) 0.031(4) Uani 1 1 d U . . 
H10 H 0.0864 0.3750 -0.2947 0.038 Uiso 1 1 calc R . . 
C11 C 0.1262(6) 0.2970(18) -0.1859(19) 0.025(4) Uani 1 1 d U . . 
H11 H 0.1482 0.3192 -0.2029 0.030 Uiso 1 1 calc R . . 
C12 C 0.1274(6) 0.2282(17) -0.1045(18) 0.022(3) Uani 1 1 d U . . 
C13 C 0.1976(6) 0.2274(18) -0.0843(19) 0.024(4) Uani 1 1 d U . . 
H13A H 0.2217 0.2016 -0.0413 0.037 Uiso 1 1 calc R . . 
H13B H 0.1975 0.3053 -0.0841 0.037 Uiso 1 1 calc R . . 
H13C H 0.1944 0.2016 -0.1518 0.037 Uiso 1 1 calc R . . 
C14 C 0.1666(6) 0.0718(16) -0.0525(18) 0.022(4) Uani 1 1 d U . . 
H14A H 0.1453 0.0403 -0.0338 0.033 Uiso 1 1 calc R . . 
H14B H 0.1904 0.0461 -0.0077 0.033 Uiso 1 1 calc R . . 
H14C H 0.1654 0.0513 -0.1205 0.033 Uiso 1 1 calc R . . 
C15 C 0.0662(6) 0.2805(19) 0.214(2) 0.032(4) Uani 1 1 d U . . 
C16 C 0.0296(6) 0.2714(19) 0.148(2) 0.033(4) Uani 1 1 d U . . 
H16 H 0.0118 0.2278 0.1675 0.040 Uiso 1 1 calc R . . 
C17 C 0.0182(7) 0.323(2) 0.058(2) 0.037(4) Uani 1 1 d U . . 
C18 C 0.0424(6) 0.3920(19) 0.030(2) 0.034(4) Uani 1 1 d U . . 
H18 H 0.0335 0.4319 -0.0294 0.040 Uiso 1 1 calc R . . 
C19 C 0.0807(6) 0.4045(19) 0.088(2) 0.030(4) Uani 1 1 d U . . 
C20 C 0.0905(6) 0.3473(18) 0.1778(19) 0.026(3) Uani 1 1 d U . . 
C21 C 0.0782(7) 0.225(2) 0.313(2) 0.034(5) Uani 1 1 d U . . 
H21A H 0.0732 0.2715 0.3637 0.052 Uiso 1 1 calc R . . 
H21B H 0.1053 0.2088 0.3296 0.052 Uiso 1 1 calc R . . 
H21C H 0.0639 0.1589 0.3096 0.052 Uiso 1 1 calc R . . 
C22 C -0.0221(6) 0.309(2) -0.005(2) 0.038(6) Uani 1 1 d U . . 
H22A H -0.0355 0.3775 -0.0099 0.057 Uiso 1 1 calc R . . 
H22B H -0.0348 0.2562 0.0250 0.057 Uiso 1 1 calc R . . 
H22C H -0.0221 0.2858 -0.0716 0.057 Uiso 1 1 calc R . . 
C23 C 0.1072(6) 0.4763(18) 0.054(2) 0.032(5) Uani 1 1 d U . . 
H23A H 0.0927 0.5342 0.0139 0.047 Uiso 1 1 calc R . . 
H23B H 0.1200 0.4354 0.0134 0.047 Uiso 1 1 calc R . . 
H23C H 0.1260 0.5061 0.1110 0.047 Uiso 1 1 calc R . . 
C24 C 0.1618(5) 0.3219(16) 0.2286(18) 0.017(3) Uani 1 1 d U . . 
C25 C 0.1371(6) 0.4136(17) 0.3326(18) 0.021(4) Uani 1 1 d U . . 
H25 H 0.1193 0.4483 0.3598 0.025 Uiso 1 1 calc R . . 
C26 C 0.1759(6) 0.4088(17) 0.3726(19) 0.024(4) Uani 1 1 d U . . 
H26 H 0.1901 0.4418 0.4321 0.028 Uiso 1 1 calc R . . 
C27 C 0.2312(5) 0.3302(15) 0.3336(16) 0.013(3) Uani 1 1 d U . . 
C28 C 0.2445(5) 0.2281(15) 0.3582(17) 0.017(3) Uani 1 1 d U . . 
C29 C 0.2858(5) 0.2131(16) 0.3856(17) 0.015(3) Uani 1 1 d U . . 
H29 H 0.2967 0.1450 0.4034 0.018 Uiso 1 1 calc R . . 
C30 C 0.3076(6) 0.2988(16) 0.3846(17) 0.017(3) Uani 1 1 d U . . 
C31 C 0.2937(5) 0.3997(16) 0.3577(16) 0.013(3) Uani 1 1 d U . . 
H31 H 0.311(5) 0.460(13) 0.352(14) 0.00(4) Uiso 1 1 d . . . 
C32 C 0.2537(5) 0.4189(15) 0.3317(16) 0.014(3) Uani 1 1 d U . . 
C33 C 0.2197(5) 0.1380(16) 0.3685(17) 0.016(4) Uani 1 1 d U . . 
H33A H 0.2002 0.1637 0.3982 0.024 Uiso 1 1 calc R . . 
H33B H 0.2349 0.0832 0.4111 0.024 Uiso 1 1 calc R . . 
H33C H 0.2076 0.1078 0.3032 0.024 Uiso 1 1 calc R . . 
C34 C 0.3504(6) 0.2816(17) 0.4125(19) 0.024(5) Uani 1 1 d U . . 
H34A H 0.3614 0.3009 0.4820 0.036 Uiso 1 1 calc R . . 
H34B H 0.3614 0.3262 0.3705 0.036 Uiso 1 1 calc R . . 
H34C H 0.3557 0.2067 0.4027 0.036 Uiso 1 1 calc R . . 
C35 C 0.2393(6) 0.5339(16) 0.3164(18) 0.022(5) Uani 1 1 d U . . 
H35A H 0.2168 0.5371 0.2596 0.032 Uiso 1 1 calc R . . 
H35B H 0.2591 0.5797 0.3042 0.032 Uiso 1 1 calc R . . 
H35C H 0.2329 0.5584 0.3758 0.032 Uiso 1 1 calc R . . 
 
 
_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 
Pd1 C1 2.04(2) . ? 
Pd1 C24 2.04(2) . ? 
Pd1 N1 2.225(19) . ? 
Pd1 Cl1 2.425(5) . ? 
N1 C14 1.44(3) . ? 
N1 C12 1.50(3) . ? 
N1 C13 1.54(3) . ? 
C1 C2 1.32(3) . ? 
C1 C6 1.49(3) . ? 
N2 C24 1.35(3) . ? 
N2 C25 1.37(3) . ? 
N2 C20 1.49(3) . ? 
C2 C3 1.40(3) . ? 
N3 C26 1.33(3) . ? 
N3 C24 1.37(3) . ? 
N3 C27 1.50(2) . ? 
C3 C4 1.39(4) . ? 
C4 C5 1.39(4) . ? 
C5 C6 1.39(3) . ? 
C6 C7 1.48(3) . ? 
C7 C12 1.38(3) . ? 
C7 C8 1.41(3) . ? 
C8 C9 1.39(4) . ? 
C9 C10 1.34(3) . ? 
C10 C11 1.42(3) . ? 
C11 C12 1.43(3) . ? 
C15 C16 1.41(3) . ? 
C15 C20 1.42(4) . ? 
C15 C21 1.51(4) . ? 
C16 C17 1.39(4) . ? 
C17 C18 1.38(4) . ? 
C17 C22 1.51(3) . ? 
C18 C19 1.43(3) . ? 
C19 C20 1.41(3) . ? 
C19 C23 1.51(3) . ? 
C25 C26 1.38(3) . ? 
C27 C28 1.38(3) . ? 
C27 C32 1.39(3) . ? 
C28 C29 1.48(3) . ? 
C28 C33 1.49(3) . ? 
C29 C30 1.35(3) . ? 
C30 C31 1.38(3) . ? 
C30 C34 1.53(3) . ? 
C31 C32 1.44(3) . ? 
C32 C35 1.53(3) . ? 
 
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 
C1 Pd1 C24 90.7(9) . . ? 
C1 Pd1 N1 86.3(9) . . ? 
C24 Pd1 N1 173.5(7) . . ? 
C1 Pd1 Cl1 173.5(6) . . ? 
C24 Pd1 Cl1 88.2(6) . . ? 
N1 Pd1 Cl1 94.2(5) . . ? 
C14 N1 C12 111.6(16) . . ? 
C14 N1 C13 105.3(17) . . ? 
C12 N1 C13 112.2(17) . . ? 
C14 N1 Pd1 117.2(15) . . ? 
C12 N1 Pd1 98.9(13) . . ? 
C13 N1 Pd1 111.9(13) . . ? 
C2 C1 C6 118(2) . . ? 
C2 C1 Pd1 128.7(17) . . ? 
C6 C1 Pd1 113.7(16) . . ? 
C24 N2 C25 110.8(17) . . ? 
C24 N2 C20 126.5(19) . . ? 
C25 N2 C20 122.5(17) . . ? 
C1 C2 C3 124(2) . . ? 
C26 N3 C24 111.2(17) . . ? 
C26 N3 C27 120.9(17) . . ? 
C24 N3 C27 127.6(18) . . ? 
C4 C3 C2 121(2) . . ? 
C5 C4 C3 117(2) . . ? 
C4 C5 C6 124(2) . . ? 
C5 C6 C7 121(2) . . ? 
C5 C6 C1 117(2) . . ? 
C7 C6 C1 122.1(19) . . ? 
C12 C7 C8 117(2) . . ? 
C12 C7 C6 125(2) . . ? 
C8 C7 C6 118(2) . . ? 
C9 C8 C7 122(2) . . ? 
C10 C9 C8 119(2) . . ? 
C9 C10 C11 124(3) . . ? 
C10 C11 C12 114(2) . . ? 
C7 C12 C11 124(2) . . ? 
C7 C12 N1 118(2) . . ? 
C11 C12 N1 118.3(18) . . ? 
C16 C15 C20 114(2) . . ? 
C16 C15 C21 123(2) . . ? 
C20 C15 C21 123(2) . . ? 
C17 C16 C15 123(2) . . ? 
C18 C17 C16 120(2) . . ? 
C18 C17 C22 121(2) . . ? 
C16 C17 C22 119(2) . . ? 
C17 C18 C19 121(2) . . ? 
C20 C19 C18 115(2) . . ? 
C20 C19 C23 125(2) . . ? 
C18 C19 C23 120(2) . . ? 
C19 C20 C15 126(2) . . ? 
C19 C20 N2 119(2) . . ? 
C15 C20 N2 115(2) . . ? 
N2 C24 N3 104.4(19) . . ? 
N2 C24 Pd1 126.1(15) . . ? 
N3 C24 Pd1 129.3(15) . . ? 
N2 C25 C26 105.8(19) . . ? 
N3 C26 C25 107(2) . . ? 
C28 C27 C32 125.3(18) . . ? 
C28 C27 N3 118.0(17) . . ? 
C32 C27 N3 116.5(16) . . ? 
C27 C28 C29 116.7(17) . . ? 
C27 C28 C33 123.3(17) . . ? 
C29 C28 C33 119.6(17) . . ? 
C30 C29 C28 118.1(18) . . ? 
C29 C30 C31 124.1(18) . . ? 
C29 C30 C34 117.3(18) . . ? 
C31 C30 C34 118.6(18) . . ? 
C30 C31 C32 120.1(18) . . ? 
C27 C32 C31 115.7(17) . . ? 
C27 C32 C35 124.9(17) . . ? 
C31 C32 C35 119.0(17) . . ? 
 
_diffrn_measured_fraction_theta_max    0.795 
_diffrn_reflns_theta_full              23.47 
_diffrn_measured_fraction_theta_full   0.795 
_refine_diff_density_max    3.594 
_refine_diff_density_min   -2.364 
_refine_diff_density_rms    0.246 

