Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email IJBLIN@MAIL.NDHU.EDU.TW _publ_contact_author_name 'Prof Ivan J. B. Lin' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_address ; Department of Chemistry National Dong Hwa University Shoufeng Hualien 974 TAIWAN ; _publ_section_title ; Organic-Inorganic Hybrids of Imidazole Complexes of Palladium(II), Copper(II), and Zinc(II). Crystals and Liquid Crystals. ; loop_ _publ_author_name 'Ivan J. B. Lin' 'Ling Mei Jing' 'Ching Kuan Lee' data_Pd(C12H25-im)2Cl2 _database_code_CSD 216100 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H56 Cl2 N4 Pd' _chemical_formula_weight 650.09 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 4.7995(5) _cell_length_b 44.832(5) _cell_length_c 7.7472(8) _cell_angle_alpha 90.00 _cell_angle_beta 94.345(2) _cell_angle_gamma 90.00 _cell_volume 1662.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2409 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 25 _exptl_crystal_description Columnar _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.299 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 688 _exptl_absorpt_coefficient_mu 0.743 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.83677 _exptl_absorpt_correction_T_max 0.97153 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10552 _diffrn_reflns_av_R_equivalents 0.0496 _diffrn_reflns_av_sigmaI/netI 0.1063 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -49 _diffrn_reflns_limit_k_max 59 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 0.91 _diffrn_reflns_theta_max 28.29 _reflns_number_total 3981 _reflns_number_gt 2283 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0478P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3981 _refine_ls_number_parameters 169 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1077 _refine_ls_R_factor_gt 0.0480 _refine_ls_wR_factor_ref 0.1159 _refine_ls_wR_factor_gt 0.0881 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _refine_ls_shift/su_max 0.001 _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 Pd1 Pd 0.5000 0.0000 0.0000 0.03328(15) Uani 1 2 d S . . Cl1 Cl 0.5113(3) 0.03834(2) 0.19988(14) 0.0478(3) Uani 1 1 d . . . N1 N 0.2223(7) 0.02326(7) -0.1559(4) 0.0337(9) Uani 1 1 d . . . N2 N -0.1112(8) 0.05444(7) -0.2399(5) 0.0422(10) Uani 1 1 d . . . C1 C 0.0363(9) 0.04261(9) -0.1039(5) 0.0361(10) Uani 1 1 d . . . C2 C 0.1869(11) 0.02284(10) -0.3353(6) 0.0457(12) Uani 1 1 d . . . C3 C -0.0182(11) 0.04228(10) -0.3862(6) 0.0482(13) Uani 1 1 d . . . C4 C -0.3174(10) 0.07900(10) -0.2309(6) 0.0494(13) Uani 1 1 d . . . C5 C -0.1797(10) 0.10877(10) -0.2446(6) 0.0430(12) Uani 1 1 d . . . C6 C -0.3827(10) 0.13526(10) -0.2381(6) 0.0461(12) Uani 1 1 d . . . C7 C -0.2367(12) 0.16507(10) -0.2437(6) 0.0495(13) Uani 1 1 d . . . C8 C -0.4263(11) 0.19207(10) -0.2377(6) 0.0504(13) Uani 1 1 d . . . C9 C -0.2693(12) 0.22152(10) -0.2431(6) 0.0541(14) Uani 1 1 d . . . C10 C -0.4524(11) 0.24880(10) -0.2383(6) 0.0524(14) Uani 1 1 d . . . C11 C -0.2949(12) 0.27814(11) -0.2416(7) 0.0571(15) Uani 1 1 d . . . C12 C -0.4766(12) 0.30563(10) -0.2392(6) 0.0573(14) Uani 1 1 d . . . C13 C -0.3213(12) 0.33505(11) -0.2389(7) 0.0597(16) Uani 1 1 d . . . C14 C -0.5036(13) 0.36238(11) -0.2402(7) 0.0668(16) Uani 1 1 d . . . C15 C -0.3510(17) 0.39133(13) -0.2362(8) 0.098(3) Uani 1 1 d . . . H1A H 0.0167 0.0465 0.0013 0.080 Uiso 1 1 d . . . H2A H 0.2865 0.0056 -0.4058 0.080 Uiso 1 1 d . . . H3A H -0.0921 0.0464 -0.5063 0.080 Uiso 1 1 d . . . H4A H -0.4693 0.0776 -0.3197 0.080 Uiso 1 1 d . . . H4B H -0.4046 0.0769 -0.0959 0.080 Uiso 1 1 d . . . H5A H -0.0182 0.1127 -0.1314 0.080 Uiso 1 1 d . . . H5B H -0.0429 0.1129 -0.3396 0.080 Uiso 1 1 d . . . H6A H -0.4628 0.1298 -0.1185 0.080 Uiso 1 1 d . . . H6B H -0.5170 0.1336 -0.3527 0.080 Uiso 1 1 d . . . H7A H -0.0760 0.1651 -0.1274 0.080 Uiso 1 1 d . . . H7B H -0.0907 0.1634 -0.3441 0.080 Uiso 1 1 d . . . H8A H -0.5828 0.1889 -0.3321 0.080 Uiso 1 1 d . . . H8B H -0.4757 0.1873 -0.1097 0.080 Uiso 1 1 d . . . H9A H -0.1589 0.2229 -0.3545 0.080 Uiso 1 1 d . . . H9B H -0.1109 0.2225 -0.1378 0.080 Uiso 1 1 d . . . H10A H -0.6126 0.2484 -0.3420 0.080 Uiso 1 1 d . . . H10B H -0.5823 0.2494 -0.1561 0.080 Uiso 1 1 d . . . H11A H -0.2121 0.2782 -0.3736 0.080 Uiso 1 1 d . . . H11B H -0.1189 0.2784 -0.1463 0.080 Uiso 1 1 d . . . H12A H -0.6027 0.3064 -0.3456 0.080 Uiso 1 1 d . . . H12B H -0.6067 0.3057 -0.1514 0.080 Uiso 1 1 d . . . H13A H -0.1791 0.3345 -0.3488 0.080 Uiso 1 1 d . . . H13B H -0.1440 0.3362 -0.1320 0.080 Uiso 1 1 d . . . H14A H -0.6229 0.3605 -0.1438 0.080 Uiso 1 1 d . . . H14B H -0.6746 0.3573 -0.3452 0.080 Uiso 1 1 d . . . H15A H -0.4383 0.4057 -0.2398 0.080 Uiso 1 1 d . . . H15B H -0.2548 0.3895 -0.3412 0.080 Uiso 1 1 d . . . H15C H -0.1890 0.3929 -0.1423 0.080 Uiso 1 1 d . . . 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 Pd1 0.0385(3) 0.0248(2) 0.0358(2) -0.0012(3) -0.00252(18) 0.0030(3) Cl1 0.0625(8) 0.0333(6) 0.0456(6) -0.0125(5) -0.0099(6) 0.0126(6) N1 0.040(2) 0.0226(18) 0.037(2) 0.0010(15) -0.0034(17) 0.0006(16) N2 0.046(3) 0.0210(19) 0.057(2) 0.0037(17) -0.011(2) 0.0006(16) C1 0.041(3) 0.023(2) 0.043(2) 0.0033(19) -0.002(2) -0.0013(19) C2 0.060(3) 0.033(3) 0.042(3) -0.006(2) -0.011(2) 0.004(2) C3 0.074(4) 0.024(2) 0.044(3) -0.001(2) -0.016(3) -0.001(2) C4 0.040(3) 0.028(2) 0.079(3) 0.007(2) -0.008(3) 0.006(2) C5 0.041(3) 0.027(3) 0.061(3) 0.003(2) 0.009(2) 0.000(2) C6 0.052(3) 0.026(2) 0.059(3) 0.004(2) -0.003(3) 0.004(2) C7 0.058(3) 0.028(3) 0.064(3) 0.000(3) 0.014(3) 0.000(2) C8 0.068(4) 0.025(2) 0.058(3) 0.000(2) -0.001(3) 0.004(2) C9 0.073(4) 0.025(3) 0.065(3) -0.002(3) 0.011(3) -0.004(3) C10 0.067(4) 0.029(3) 0.062(3) -0.003(2) 0.010(3) 0.000(2) C11 0.074(4) 0.030(3) 0.066(3) 0.001(3) 0.000(3) 0.002(3) C12 0.082(4) 0.031(3) 0.059(3) 0.002(2) 0.011(3) 0.000(3) C13 0.077(4) 0.032(3) 0.069(4) 0.000(3) 0.003(3) -0.004(3) C14 0.100(5) 0.031(3) 0.072(4) 0.003(3) 0.019(3) -0.007(3) C15 0.168(8) 0.033(4) 0.093(5) 0.006(3) 0.008(5) -0.005(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 Pd1 N1 2.019(3) . ? Pd1 N1 2.019(3) 3_655 ? Pd1 Cl1 2.3113(11) 3_655 ? Pd1 Cl1 2.3113(11) . ? N1 C1 1.329(5) . ? N1 C2 1.387(5) . ? N2 C1 1.334(5) . ? N2 C3 1.363(6) . ? N2 C4 1.486(5) . ? C2 C3 1.351(6) . ? C4 C5 1.497(6) . ? C5 C6 1.540(6) . ? C6 C7 1.511(6) . ? C7 C8 1.517(7) . ? C8 C9 1.522(7) . ? C9 C10 1.508(7) . ? C10 C11 1.518(7) . ? C11 C12 1.510(7) . ? C12 C13 1.515(7) . ? C13 C14 1.505(7) . ? C14 C15 1.490(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 N1 Pd1 N1 180.00(16) . 3_655 ? N1 Pd1 Cl1 90.13(10) . 3_655 ? N1 Pd1 Cl1 89.87(10) 3_655 3_655 ? N1 Pd1 Cl1 89.87(10) . . ? N1 Pd1 Cl1 90.13(10) 3_655 . ? Cl1 Pd1 Cl1 180.00(8) 3_655 . ? C1 N1 C2 106.2(4) . . ? C1 N1 Pd1 125.7(3) . . ? C2 N1 Pd1 128.1(3) . . ? C1 N2 C3 108.1(4) . . ? C1 N2 C4 125.0(4) . . ? C3 N2 C4 126.6(4) . . ? N1 C1 N2 110.4(4) . . ? C3 C2 N1 108.4(4) . . ? C2 C3 N2 107.0(4) . . ? N2 C4 C5 111.0(4) . . ? C4 C5 C6 113.7(4) . . ? C7 C6 C5 112.7(4) . . ? C6 C7 C8 115.1(4) . . ? C7 C8 C9 113.1(4) . . ? C10 C9 C8 114.3(5) . . ? C9 C10 C11 114.2(5) . . ? C12 C11 C10 114.7(5) . . ? C11 C12 C13 115.2(5) . . ? C14 C13 C12 115.0(5) . . ? C15 C14 C13 115.1(6) . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 0.370 _refine_diff_density_min -0.989 _refine_diff_density_rms 0.128 #====END data_Cu(C12H25-im)2Cl2 _database_code_CSD 216101 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H56 Cl2 Cu N4' _chemical_formula_weight 607.23 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' Cu Cu 0.3201 1.2651 '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 8.3007(10) _cell_length_b 10.732(2) _cell_length_c 19.3765(18) _cell_angle_alpha 77.929(10) _cell_angle_beta 89.330(8) _cell_angle_gamma 87.332(16) _cell_volume 1686.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 4.98 _cell_measurement_theta_max 12.65 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.9 _exptl_crystal_size_min 0.7 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.196 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 654 _exptl_absorpt_coefficient_mu 0.830 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6360 _exptl_absorpt_correction_T_max 0.8809 _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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 197 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6062 _diffrn_reflns_av_R_equivalents 0.0162 _diffrn_reflns_av_sigmaI/netI 0.0328 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.07 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5627 _reflns_number_gt 4673 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0500P)^2^+0.4000P] 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 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5627 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0499 _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.1052 _refine_ls_wR_factor_gt 0.0983 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.001 _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 Cu1 Cu 0.63496(3) 0.70152(3) 0.467080(14) 0.04053(11) Uani 1 1 d . . . Cl1 Cl 0.83886(8) 0.63988(8) 0.40073(4) 0.0687(2) Uani 1 1 d . . . Cl2 Cl 0.43152(7) 0.79789(6) 0.52064(4) 0.05503(18) Uani 1 1 d . . . N1 N 0.4762(2) 0.61223(18) 0.42120(10) 0.0436(5) Uani 1 1 d . . . N2 N 0.3770(3) 0.48305(19) 0.35995(11) 0.0478(5) Uani 1 1 d . . . N3 N 0.7945(2) 0.77677(18) 0.51998(10) 0.0436(5) Uani 1 1 d . . . N4 N 0.9072(2) 0.91169(19) 0.57379(10) 0.0470(5) Uani 1 1 d . . . C1 C 0.5103(3) 0.5234(2) 0.38450(13) 0.0489(6) Uani 1 1 d . . . H1A H 0.6142 0.4928 0.3768 0.059 Uiso 1 1 calc R . . C2 C 0.3106(3) 0.6268(3) 0.41988(15) 0.0546(6) Uani 1 1 d . . . H2A H 0.2502 0.6826 0.4419 0.066 Uiso 1 1 calc R . . C3 C 0.2494(3) 0.5490(3) 0.38223(15) 0.0580(7) Uani 1 1 d . . . H3A H 0.1410 0.5413 0.3731 0.070 Uiso 1 1 calc R . . C4 C 0.3712(4) 0.3852(2) 0.31726(13) 0.0548(6) Uani 1 1 d . . . H4A H 0.2766 0.3359 0.3306 0.066 Uiso 1 1 calc R . . H4B H 0.4654 0.3277 0.3277 0.066 Uiso 1 1 calc R . . C5 C 0.3657(4) 0.4393(2) 0.23936(14) 0.0542(6) Uani 1 1 d . . . H5A H 0.4577 0.4917 0.2258 0.065 Uiso 1 1 calc R . . H5B H 0.2685 0.4932 0.2281 0.065 Uiso 1 1 calc R . . C6 C 0.3683(4) 0.3335(2) 0.19787(14) 0.0573(7) Uani 1 1 d . . . H6A H 0.4638 0.2786 0.2113 0.069 Uiso 1 1 calc R . . H6B H 0.2753 0.2825 0.2118 0.069 Uiso 1 1 calc R . . C7 C 0.3672(4) 0.3760(2) 0.11877(14) 0.0598(7) Uani 1 1 d . . . H7A H 0.4578 0.4295 0.1044 0.072 Uiso 1 1 calc R . . H7B H 0.2692 0.4272 0.1046 0.072 Uiso 1 1 calc R . . C8 C 0.3772(4) 0.2663(2) 0.08068(14) 0.0591(7) Uani 1 1 d . . . H8A H 0.4746 0.2149 0.0958 0.071 Uiso 1 1 calc R . . H8B H 0.2863 0.2133 0.0954 0.071 Uiso 1 1 calc R . . C9 C 0.3781(4) 0.3022(3) 0.00137(14) 0.0614(7) Uani 1 1 d . . . H9A H 0.4681 0.3560 -0.0137 0.074 Uiso 1 1 calc R . . H9B H 0.2798 0.3521 -0.0142 0.074 Uiso 1 1 calc R . . C10 C 0.3909(4) 0.1896(3) -0.03433(14) 0.0617(7) Uani 1 1 d . . . H10A H 0.4884 0.1393 -0.0179 0.074 Uiso 1 1 calc R . . H10B H 0.3003 0.1365 -0.0193 0.074 Uiso 1 1 calc R . . C11 C 0.3940(4) 0.2219(3) -0.11369(14) 0.0620(7) Uani 1 1 d . . . H11A H 0.4853 0.2742 -0.1291 0.074 Uiso 1 1 calc R . . H11B H 0.2968 0.2723 -0.1304 0.074 Uiso 1 1 calc R . . C12 C 0.4059(4) 0.1064(3) -0.14717(15) 0.0664(8) Uani 1 1 d . . . H12A H 0.5033 0.0567 -0.1300 0.080 Uiso 1 1 calc R . . H12B H 0.3153 0.0541 -0.1308 0.080 Uiso 1 1 calc R . . C13 C 0.4085(4) 0.1315(3) -0.22623(15) 0.0678(8) Uani 1 1 d . . . H13A H 0.5006 0.1816 -0.2432 0.081 Uiso 1 1 calc R . . H13B H 0.3118 0.1816 -0.2441 0.081 Uiso 1 1 calc R . . C14 C 0.4177(5) 0.0105(3) -0.25534(17) 0.0825(10) Uani 1 1 d . . . H14A H 0.5149 -0.0387 -0.2374 0.099 Uiso 1 1 calc R . . H14B H 0.3265 -0.0399 -0.2373 0.099 Uiso 1 1 calc R . . C15 C 0.4184(5) 0.0296(4) -0.33290(19) 0.0957(12) Uani 1 1 d . . . H15A H 0.4247 -0.0518 -0.3462 0.144 Uiso 1 1 calc R . . H15B H 0.5099 0.0773 -0.3516 0.144 Uiso 1 1 calc R . . H15C H 0.3211 0.0757 -0.3514 0.144 Uiso 1 1 calc R . . C16 C 0.7740(3) 0.8855(2) 0.54208(12) 0.0440(5) Uani 1 1 d . . . H16A H 0.6796 0.9368 0.5363 0.053 Uiso 1 1 calc R . . C17 C 0.9503(3) 0.7325(3) 0.53911(13) 0.0500(6) Uani 1 1 d . . . H17A H 0.9998 0.6578 0.5303 0.060 Uiso 1 1 calc R . . C18 C 1.0189(3) 0.8144(3) 0.57243(13) 0.0532(6) Uani 1 1 d . . . H18A H 1.1226 0.8064 0.5910 0.064 Uiso 1 1 calc R . . C19 C 0.9222(3) 1.0211(2) 0.60742(13) 0.0538(6) Uani 1 1 d . . . H19A H 0.8359 1.0840 0.5909 0.065 Uiso 1 1 calc R . . H19B H 1.0238 1.0602 0.5935 0.065 Uiso 1 1 calc R . . C20 C 0.9148(4) 0.9827(3) 0.68727(13) 0.0569(7) Uani 1 1 d . . . H20A H 1.0080 0.9273 0.7042 0.068 Uiso 1 1 calc R . . H20B H 0.8190 0.9351 0.7010 0.068 Uiso 1 1 calc R . . C21 C 0.9113(4) 1.0978(2) 0.72179(13) 0.0570(7) Uani 1 1 d . . . H21A H 1.0050 1.1471 0.7063 0.068 Uiso 1 1 calc R . . H21B H 0.8161 1.1515 0.7059 0.068 Uiso 1 1 calc R . . C22 C 0.9101(4) 1.0632(3) 0.80133(14) 0.0606(7) Uani 1 1 d . . . H22A H 1.0078 1.0128 0.8172 0.073 Uiso 1 1 calc R . . H22B H 0.8193 1.0105 0.8167 0.073 Uiso 1 1 calc R . . C23 C 0.8989(4) 1.1775(3) 0.83618(14) 0.0616(7) Uani 1 1 d . . . H23A H 0.9896 1.2302 0.8206 0.074 Uiso 1 1 calc R . . H23B H 0.8012 1.2278 0.8201 0.074 Uiso 1 1 calc R . . C24 C 0.8975(4) 1.1449(3) 0.91581(14) 0.0609(7) Uani 1 1 d . . . H24A H 0.9954 1.0949 0.9319 0.073 Uiso 1 1 calc R . . H24B H 0.8072 1.0918 0.9313 0.073 Uiso 1 1 calc R . . C25 C 0.8855(4) 1.2584(3) 0.95069(14) 0.0619(7) Uani 1 1 d . . . H25A H 0.7874 1.3082 0.9346 0.074 Uiso 1 1 calc R . . H25B H 0.9756 1.3117 0.9349 0.074 Uiso 1 1 calc R . . C26 C 0.8846(4) 1.2270(2) 1.03044(14) 0.0592(7) Uani 1 1 d . . . H26A H 0.7943 1.1741 1.0465 0.071 Uiso 1 1 calc R . . H26B H 0.9826 1.1774 1.0468 0.071 Uiso 1 1 calc R . . C27 C 0.8725(4) 1.3423(2) 1.06382(14) 0.0618(7) Uani 1 1 d . . . H27A H 0.9618 1.3957 1.0470 0.074 Uiso 1 1 calc R . . H27B H 0.7737 1.3910 1.0478 0.074 Uiso 1 1 calc R . . C28 C 0.8738(4) 1.3135(3) 1.14340(14) 0.0605(7) Uani 1 1 d . . . H28A H 0.7844 1.2601 1.1603 0.073 Uiso 1 1 calc R . . H28B H 0.9726 1.2649 1.1595 0.073 Uiso 1 1 calc R . . C29 C 0.8615(5) 1.4294(3) 1.17597(16) 0.0747(9) Uani 1 1 d . . . H29A H 0.9504 1.4831 1.1587 0.090 Uiso 1 1 calc R . . H29B H 0.7623 1.4777 1.1601 0.090 Uiso 1 1 calc R . . C30 C 0.8639(5) 1.4011(4) 1.25536(18) 0.0939(12) Uani 1 1 d . . . H30A H 0.8553 1.4797 1.2717 0.141 Uiso 1 1 calc R . . H30B H 0.9631 1.3557 1.2718 0.141 Uiso 1 1 calc R . . H30C H 0.7747 1.3499 1.2732 0.141 Uiso 1 1 calc R . . 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 Cu1 0.03954(18) 0.04502(17) 0.03936(17) -0.01504(12) 0.00512(12) 0.00085(12) Cl1 0.0481(4) 0.0970(6) 0.0742(5) -0.0492(4) 0.0168(3) -0.0038(4) Cl2 0.0428(4) 0.0666(4) 0.0639(4) -0.0341(3) 0.0054(3) 0.0043(3) N1 0.0444(12) 0.0458(11) 0.0431(11) -0.0152(9) 0.0042(9) -0.0014(9) N2 0.0551(13) 0.0477(11) 0.0437(11) -0.0164(9) 0.0015(10) -0.0041(9) N3 0.0411(11) 0.0510(11) 0.0403(11) -0.0141(9) 0.0035(9) 0.0006(9) N4 0.0486(12) 0.0561(12) 0.0379(11) -0.0124(9) 0.0034(9) -0.0083(10) C1 0.0464(15) 0.0538(14) 0.0498(15) -0.0200(12) 0.0009(11) 0.0037(11) C2 0.0431(15) 0.0620(16) 0.0652(17) -0.0286(13) 0.0074(12) -0.0010(12) C3 0.0437(15) 0.0657(17) 0.0692(18) -0.0243(14) 0.0032(13) -0.0056(12) C4 0.0726(18) 0.0485(14) 0.0469(14) -0.0173(11) -0.0023(13) -0.0057(12) C5 0.0691(18) 0.0500(14) 0.0456(14) -0.0144(11) 0.0021(13) -0.0045(12) C6 0.0758(19) 0.0523(15) 0.0458(15) -0.0147(12) 0.0014(13) -0.0045(13) C7 0.081(2) 0.0525(15) 0.0460(15) -0.0115(12) 0.0032(14) -0.0039(14) C8 0.080(2) 0.0521(15) 0.0461(15) -0.0134(12) 0.0031(14) -0.0018(13) C9 0.083(2) 0.0545(15) 0.0464(15) -0.0111(12) 0.0029(14) -0.0016(14) C10 0.080(2) 0.0564(15) 0.0494(16) -0.0133(13) 0.0020(14) 0.0004(14) C11 0.080(2) 0.0571(16) 0.0499(16) -0.0153(13) -0.0009(14) 0.0026(14) C12 0.086(2) 0.0615(17) 0.0543(17) -0.0203(14) -0.0022(15) 0.0044(15) C13 0.084(2) 0.0689(18) 0.0518(17) -0.0184(14) -0.0063(15) 0.0117(16) C14 0.116(3) 0.072(2) 0.062(2) -0.0237(16) 0.0008(19) 0.0125(19) C15 0.130(3) 0.097(3) 0.067(2) -0.036(2) -0.004(2) 0.012(2) C16 0.0432(14) 0.0509(13) 0.0388(12) -0.0121(10) 0.0024(10) -0.0006(10) C17 0.0451(15) 0.0596(15) 0.0453(14) -0.0134(12) 0.0039(11) 0.0066(11) C18 0.0400(14) 0.0771(18) 0.0421(14) -0.0128(13) 0.0006(11) 0.0022(13) C19 0.0656(17) 0.0576(15) 0.0415(14) -0.0144(12) 0.0015(12) -0.0179(13) C20 0.0737(19) 0.0587(15) 0.0390(14) -0.0103(12) 0.0026(13) -0.0104(13) C21 0.0767(19) 0.0548(15) 0.0413(14) -0.0129(12) 0.0019(13) -0.0095(13) C22 0.078(2) 0.0595(16) 0.0466(15) -0.0153(12) 0.0015(14) -0.0053(14) C23 0.082(2) 0.0580(16) 0.0471(15) -0.0153(13) 0.0039(14) -0.0057(14) C24 0.083(2) 0.0562(16) 0.0449(15) -0.0143(12) 0.0015(14) -0.0001(14) C25 0.085(2) 0.0531(15) 0.0489(16) -0.0136(12) 0.0020(14) 0.0011(14) C26 0.079(2) 0.0530(15) 0.0460(15) -0.0127(12) 0.0013(14) -0.0008(14) C27 0.087(2) 0.0515(15) 0.0479(15) -0.0126(12) 0.0020(14) -0.0007(14) C28 0.077(2) 0.0571(16) 0.0479(15) -0.0126(12) 0.0042(14) -0.0014(14) C29 0.103(3) 0.0693(19) 0.0558(18) -0.0239(15) 0.0000(17) 0.0055(17) C30 0.114(3) 0.114(3) 0.064(2) -0.043(2) 0.004(2) 0.004(2) _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 Cu1 N3 1.984(2) . ? Cu1 N1 1.987(2) . ? Cu1 Cl1 2.2706(7) . ? Cu1 Cl2 2.2899(7) . ? N1 C1 1.323(3) . ? N1 C2 1.376(3) . ? N2 C1 1.335(3) . ? N2 C3 1.362(3) . ? N2 C4 1.469(3) . ? N3 C16 1.328(3) . ? N3 C17 1.384(3) . ? N4 C16 1.340(3) . ? N4 C18 1.369(3) . ? N4 C19 1.468(3) . ? C2 C3 1.339(4) . ? C4 C5 1.500(4) . ? C5 C6 1.522(3) . ? C6 C7 1.505(4) . ? C7 C8 1.513(3) . ? C8 C9 1.504(4) . ? C9 C10 1.512(4) . ? C10 C11 1.504(4) . ? C11 C12 1.514(4) . ? C12 C13 1.499(4) . ? C13 C14 1.518(4) . ? C14 C15 1.474(4) . ? C17 C18 1.344(4) . ? C19 C20 1.517(3) . ? C20 C21 1.522(3) . ? C21 C22 1.508(3) . ? C22 C23 1.517(4) . ? C23 C24 1.509(4) . ? C24 C25 1.511(4) . ? C25 C26 1.511(4) . ? C26 C27 1.510(4) . ? C27 C28 1.508(4) . ? C28 C29 1.507(4) . ? C29 C30 1.505(4) . ? 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 N3 Cu1 N1 174.79(8) . . ? N3 Cu1 Cl1 89.31(6) . . ? N1 Cu1 Cl1 91.34(6) . . ? N3 Cu1 Cl2 89.30(6) . . ? N1 Cu1 Cl2 90.94(6) . . ? Cl1 Cu1 Cl2 169.89(3) . . ? C1 N1 C2 104.8(2) . . ? C1 N1 Cu1 126.06(17) . . ? C2 N1 Cu1 129.15(17) . . ? C1 N2 C3 107.2(2) . . ? C1 N2 C4 125.8(2) . . ? C3 N2 C4 127.1(2) . . ? C16 N3 C17 105.4(2) . . ? C16 N3 Cu1 126.00(17) . . ? C17 N3 Cu1 128.53(16) . . ? C16 N4 C18 107.3(2) . . ? C16 N4 C19 125.0(2) . . ? C18 N4 C19 127.6(2) . . ? N1 C1 N2 111.5(2) . . ? C3 C2 N1 109.9(2) . . ? C2 C3 N2 106.6(2) . . ? N2 C4 C5 113.4(2) . . ? C4 C5 C6 111.0(2) . . ? C7 C6 C5 116.0(2) . . ? C6 C7 C8 113.4(2) . . ? C9 C8 C7 116.1(2) . . ? C8 C9 C10 114.2(2) . . ? C11 C10 C9 115.6(2) . . ? C10 C11 C12 113.8(2) . . ? C13 C12 C11 116.7(2) . . ? C12 C13 C14 113.2(3) . . ? C15 C14 C13 115.6(3) . . ? N3 C16 N4 111.1(2) . . ? C18 C17 N3 109.3(2) . . ? C17 C18 N4 106.9(2) . . ? N4 C19 C20 112.1(2) . . ? C19 C20 C21 112.0(2) . . ? C22 C21 C20 113.6(2) . . ? C21 C22 C23 113.9(2) . . ? C24 C23 C22 114.8(2) . . ? C23 C24 C25 114.9(2) . . ? C24 C25 C26 115.4(2) . . ? C27 C26 C25 114.2(2) . . ? C28 C27 C26 115.3(2) . . ? C29 C28 C27 114.7(2) . . ? C30 C29 C28 114.8(3) . . ? _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.949 _refine_diff_density_max 0.299 _refine_diff_density_min -0.326 _refine_diff_density_rms 0.079 data_001 _database_code_CSD 216102 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H80 Cl2 N4 Zn' _chemical_formula_weight 777.37 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' 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 8.221(3) _cell_length_b 11.8579(12) _cell_length_c 24.346(3) _cell_angle_alpha 82.486(7) _cell_angle_beta 81.457(12) _cell_angle_gamma 84.442(12) _cell_volume 2319.5(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 15 _cell_measurement_theta_min 5.11 _cell_measurement_theta_max 10.02 _exptl_crystal_description ? _exptl_crystal_colour colorless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.113 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 0.675 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9655 _exptl_absorpt_correction_T_max 0.9766 _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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6543 _diffrn_reflns_av_R_equivalents 0.0452 _diffrn_reflns_av_sigmaI/netI 0.1165 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 22.50 _reflns_number_total 6034 _reflns_number_gt 2990 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1500P)^2^+1.1000P] 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 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6034 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1709 _refine_ls_R_factor_gt 0.0749 _refine_ls_wR_factor_ref 0.2562 _refine_ls_wR_factor_gt 0.1840 _refine_ls_goodness_of_fit_ref 0.916 _refine_ls_restrained_S_all 0.916 _refine_ls_shift/su_max 0.100 _refine_ls_shift/su_mean 0.007 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 -1.26190(13) -0.25760(8) 1.51771(4) 0.0608(4) Uani 1 1 d . . . Cl1 Cl -1.4667(3) -0.1512(2) 1.56352(11) 0.0914(9) Uani 1 1 d . . . Cl2 Cl -1.1037(3) -0.38545(19) 1.56735(10) 0.0791(8) Uani 1 1 d . . . N1 N -1.4186(16) -0.4718(7) 1.4169(3) 0.085(3) Uani 1 1 d . . . N2 N -1.3688(9) -0.3427(6) 1.4680(3) 0.0626(19) Uani 1 1 d . . . N3 N -1.0180(9) 0.0031(5) 1.4172(3) 0.0572(18) Uani 1 1 d . . . N4 N -1.1094(9) -0.1481(6) 1.4708(3) 0.0632(19) Uani 1 1 d . . . C1 C -1.3122(14) -0.4360(8) 1.4452(4) 0.071(3) Uani 1 1 d . . . H1A H -1.2084 -0.4728 1.4486 0.086 Uiso 1 1 calc R . . C2 C -1.5246(14) -0.3155(11) 1.4514(4) 0.093(3) Uani 1 1 d . . . H2A H -1.5967 -0.2532 1.4605 0.112 Uiso 1 1 calc R . . C3 C -1.5511(16) -0.3924(14) 1.4212(5) 0.103(4) Uani 1 1 d . . . H3A H -1.6461 -0.3934 1.4048 0.123 Uiso 1 1 calc R . . C4 C -1.399(2) -0.5700(9) 1.3885(5) 0.134(5) Uani 1 1 d . . . H4A H -1.3556 -0.6328 1.4132 0.161 Uiso 1 1 calc R . . H4B H -1.5086 -0.5876 1.3836 0.161 Uiso 1 1 calc R . . C5 C -1.3031(19) -0.5701(9) 1.3376(5) 0.149(6) Uani 1 1 d . . . H5A H -1.3174 -0.6407 1.3234 0.179 Uiso 1 1 calc R . . H5B H -1.1892 -0.5738 1.3443 0.179 Uiso 1 1 calc R . . C6 C -1.3255(14) -0.4727(8) 1.2902(4) 0.096(3) Uani 1 1 d . . . H6A H -1.4278 -0.4789 1.2758 0.115 Uiso 1 1 calc R . . H6B H -1.3332 -0.4000 1.3050 0.115 Uiso 1 1 calc R . . C7 C -1.1839(12) -0.4764(7) 1.2431(3) 0.073(3) Uani 1 1 d . . . H7A H -1.0812 -0.4861 1.2589 0.087 Uiso 1 1 calc R . . H7B H -1.1896 -0.5426 1.2241 0.087 Uiso 1 1 calc R . . C8 C -1.1810(11) -0.3717(7) 1.2007(3) 0.064(2) Uani 1 1 d . . . H8A H -1.1859 -0.3049 1.2202 0.076 Uiso 1 1 calc R . . H8B H -1.2791 -0.3661 1.1824 0.076 Uiso 1 1 calc R . . C9 C -1.0308(11) -0.3697(7) 1.1561(3) 0.067(2) Uani 1 1 d . . . H9A H -0.9324 -0.3825 1.1744 0.080 Uiso 1 1 calc R . . H9B H -1.0315 -0.4325 1.1343 0.080 Uiso 1 1 calc R . . C10 C -1.0198(11) -0.2600(7) 1.1166(3) 0.072(3) Uani 1 1 d . . . H10A H -1.0221 -0.1970 1.1385 0.086 Uiso 1 1 calc R . . H10B H -1.1168 -0.2483 1.0976 0.086 Uiso 1 1 calc R . . C11 C -0.8674(12) -0.2562(7) 1.0727(3) 0.070(3) Uani 1 1 d . . . H11A H -0.8656 -0.3188 1.0506 0.084 Uiso 1 1 calc R . . H11B H -0.7704 -0.2686 1.0917 0.084 Uiso 1 1 calc R . . C12 C -0.8549(11) -0.1458(7) 1.0332(3) 0.063(2) Uani 1 1 d . . . H12A H -0.9503 -0.1343 1.0134 0.076 Uiso 1 1 calc R . . H12B H -0.8593 -0.0829 1.0553 0.076 Uiso 1 1 calc R . . C13 C -0.6996(11) -0.1421(7) 0.9905(3) 0.068(3) Uani 1 1 d . . . H13A H -0.6042 -0.1546 1.0103 0.082 Uiso 1 1 calc R . . H13B H -0.6960 -0.2044 0.9680 0.082 Uiso 1 1 calc R . . C14 C -0.6863(11) -0.0319(7) 0.9517(3) 0.064(2) Uani 1 1 d . . . H14A H -0.7822 -0.0192 0.9321 0.077 Uiso 1 1 calc R . . H14B H -0.6896 0.0303 0.9742 0.077 Uiso 1 1 calc R . . C15 C -0.5331(11) -0.0274(7) 0.9089(3) 0.063(2) Uani 1 1 d . . . H15A H -0.4370 -0.0396 0.9284 0.075 Uiso 1 1 calc R . . H15B H -0.5295 -0.0895 0.8864 0.075 Uiso 1 1 calc R . . C16 C -0.5221(11) 0.0829(7) 0.8706(3) 0.069(3) Uani 1 1 d . . . H16A H -0.5268 0.1450 0.8932 0.083 Uiso 1 1 calc R . . H16B H -0.6179 0.0948 0.8510 0.083 Uiso 1 1 calc R . . C17 C -0.3673(11) 0.0888(7) 0.8276(3) 0.068(3) Uani 1 1 d . . . H17A H -0.2719 0.0766 0.8474 0.082 Uiso 1 1 calc R . . H17B H -0.3628 0.0263 0.8052 0.082 Uiso 1 1 calc R . . C18 C -0.3528(11) 0.1976(7) 0.7887(4) 0.067(2) Uani 1 1 d . . . H18A H -0.3526 0.2598 0.8109 0.081 Uiso 1 1 calc R . . H18B H -0.4504 0.2114 0.7699 0.081 Uiso 1 1 calc R . . C19 C -0.2015(12) 0.2012(7) 0.7443(4) 0.077(3) Uani 1 1 d . . . H19A H -0.1038 0.1913 0.7630 0.093 Uiso 1 1 calc R . . H19B H -0.1986 0.1370 0.7231 0.093 Uiso 1 1 calc R . . C20 C -0.1932(13) 0.3080(8) 0.7043(4) 0.090(3) Uani 1 1 d . . . H20A H -0.1931 0.3721 0.7253 0.108 Uiso 1 1 calc R . . H20B H -0.2918 0.3189 0.6861 0.108 Uiso 1 1 calc R . . C21 C -0.0408(13) 0.3088(9) 0.6589(4) 0.101(4) Uani 1 1 d . . . H21A H -0.0444 0.3796 0.6349 0.151 Uiso 1 1 calc R . . H21B H -0.0409 0.2466 0.6373 0.151 Uiso 1 1 calc R . . H21C H 0.0577 0.3005 0.6764 0.151 Uiso 1 1 calc R . . C22 C -1.1490(12) -0.0535(7) 1.4401(3) 0.061(2) Uani 1 1 d . . . H22A H -1.2569 -0.0282 1.4348 0.074 Uiso 1 1 calc R . . C23 C -0.9361(12) -0.1515(7) 1.4682(4) 0.070(3) Uani 1 1 d . . . H23A H -0.8703 -0.2091 1.4859 0.084 Uiso 1 1 calc R . . C24 C -0.8819(12) -0.0581(8) 1.4361(4) 0.073(3) Uani 1 1 d . . . H24A H -0.7734 -0.0386 1.4281 0.088 Uiso 1 1 calc R . . C25 C -1.0202(11) 0.1130(6) 1.3828(3) 0.066(3) Uani 1 1 d . . . H25A H -1.0164 0.1727 1.4061 0.080 Uiso 1 1 calc R . . H25B H -1.1229 0.1264 1.3669 0.080 Uiso 1 1 calc R . . C26 C -0.8765(12) 0.1198(7) 1.3357(3) 0.069(3) Uani 1 1 d . . . H26A H -0.8796 0.0595 1.3126 0.083 Uiso 1 1 calc R . . H26B H -0.7739 0.1073 1.3516 0.083 Uiso 1 1 calc R . . C27 C -0.8790(11) 0.2341(6) 1.2990(3) 0.064(2) Uani 1 1 d . . . H27A H -0.8873 0.2953 1.3224 0.076 Uiso 1 1 calc R . . H27B H -0.9753 0.2432 1.2797 0.076 Uiso 1 1 calc R . . C28 C -0.7231(12) 0.2428(7) 1.2560(4) 0.074(3) Uani 1 1 d . . . H28A H -0.6276 0.2321 1.2758 0.089 Uiso 1 1 calc R . . H28B H -0.7159 0.1810 1.2330 0.089 Uiso 1 1 calc R . . C29 C -0.7158(11) 0.3536(6) 1.2184(4) 0.068(3) Uani 1 1 d . . . H29A H -0.7202 0.4152 1.2413 0.081 Uiso 1 1 calc R . . H29B H -0.8125 0.3652 1.1993 0.081 Uiso 1 1 calc R . . C30 C -0.5640(11) 0.3603(7) 1.1754(3) 0.069(3) Uani 1 1 d . . . H30A H -0.4680 0.3495 1.1949 0.083 Uiso 1 1 calc R . . H30B H -0.5589 0.2972 1.1534 0.083 Uiso 1 1 calc R . . C31 C -0.5516(11) 0.4690(7) 1.1358(3) 0.067(3) Uani 1 1 d . . . H31A H -0.5532 0.5320 1.1576 0.081 Uiso 1 1 calc R . . H31B H -0.6489 0.4810 1.1169 0.081 Uiso 1 1 calc R . . C32 C -0.3990(11) 0.4726(7) 1.0915(3) 0.066(2) Uani 1 1 d . . . H32A H -0.3015 0.4602 1.1102 0.079 Uiso 1 1 calc R . . H32B H -0.3977 0.4101 1.0693 0.079 Uiso 1 1 calc R . . C33 C -0.3888(10) 0.5825(6) 1.0526(3) 0.060(2) Uani 1 1 d . . . H33A H -0.3901 0.6452 1.0746 0.072 Uiso 1 1 calc R . . H33B H -0.4858 0.5949 1.0336 0.072 Uiso 1 1 calc R . . C34 C -0.2356(11) 0.5840(6) 1.0091(3) 0.068(3) Uani 1 1 d . . . H34A H -0.2347 0.5214 0.9871 0.081 Uiso 1 1 calc R . . H34B H -0.1389 0.5712 1.0282 0.081 Uiso 1 1 calc R . . C35 C -0.2233(11) 0.6953(7) 0.9695(3) 0.065(2) Uani 1 1 d . . . H35A H -0.2246 0.7579 0.9916 0.078 Uiso 1 1 calc R . . H35B H -0.3200 0.7081 0.9503 0.078 Uiso 1 1 calc R . . C36 C -0.0691(11) 0.6972(7) 0.9258(3) 0.062(2) Uani 1 1 d . . . H36A H 0.0278 0.6847 0.9448 0.074 Uiso 1 1 calc R . . H36B H -0.0677 0.6347 0.9036 0.074 Uiso 1 1 calc R . . C37 C -0.0590(11) 0.8073(6) 0.8872(3) 0.062(2) Uani 1 1 d . . . H37A H -0.0620 0.8696 0.9096 0.075 Uiso 1 1 calc R . . H37B H -0.1558 0.8193 0.8681 0.075 Uiso 1 1 calc R . . C38 C 0.0965(11) 0.8121(7) 0.8429(3) 0.067(2) Uani 1 1 d . . . H38A H 0.1935 0.7991 0.8619 0.081 Uiso 1 1 calc R . . H38B H 0.0987 0.7507 0.8200 0.081 Uiso 1 1 calc R . . C39 C 0.1062(11) 0.9231(7) 0.8052(3) 0.069(3) Uani 1 1 d . . . H39A H 0.1030 0.9844 0.8282 0.083 Uiso 1 1 calc R . . H39B H 0.0092 0.9358 0.7862 0.083 Uiso 1 1 calc R . . C40 C 0.2585(11) 0.9300(7) 0.7616(3) 0.067(2) Uani 1 1 d . . . H40A H 0.3559 0.9181 0.7804 0.080 Uiso 1 1 calc R . . H40B H 0.2623 0.8688 0.7385 0.080 Uiso 1 1 calc R . . C41 C 0.2641(12) 1.0425(8) 0.7242(4) 0.081(3) Uani 1 1 d . . . H41A H 0.2531 1.1038 0.7475 0.097 Uiso 1 1 calc R . . H41B H 0.1700 1.0520 0.7038 0.097 Uiso 1 1 calc R . . C42 C 0.4198(13) 1.0539(9) 0.6825(4) 0.098(3) Uani 1 1 d . . . H42A H 0.4139 1.1272 0.6606 0.147 Uiso 1 1 calc R . . H42B H 0.4304 0.9950 0.6584 0.147 Uiso 1 1 calc R . . H42C H 0.5138 1.0467 0.7023 0.147 Uiso 1 1 calc R . . 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 0.0708(8) 0.0474(6) 0.0580(7) 0.0025(4) 0.0043(5) -0.0061(5) Cl1 0.0898(19) 0.0648(15) 0.107(2) -0.0131(14) 0.0273(16) -0.0019(14) Cl2 0.0952(19) 0.0603(14) 0.0813(16) 0.0036(12) -0.0253(15) 0.0008(13) N1 0.164(10) 0.051(5) 0.047(5) 0.000(4) -0.021(6) -0.045(6) N2 0.070(6) 0.062(5) 0.049(4) 0.008(4) -0.004(4) -0.002(4) N3 0.072(5) 0.044(4) 0.049(4) 0.015(3) -0.001(4) -0.008(4) N4 0.074(6) 0.053(4) 0.056(4) 0.005(4) 0.001(4) -0.006(4) C1 0.100(8) 0.055(6) 0.059(6) -0.007(5) -0.006(6) -0.013(6) C2 0.075(8) 0.130(10) 0.072(7) -0.009(7) -0.023(6) 0.022(7) C3 0.090(9) 0.137(12) 0.082(9) 0.005(8) -0.019(7) -0.031(9) C4 0.255(18) 0.083(8) 0.080(8) 0.005(7) -0.054(10) -0.066(10) C5 0.234(16) 0.069(7) 0.101(9) -0.002(7) 0.090(10) 0.020(9) C6 0.129(10) 0.074(7) 0.072(7) 0.001(5) 0.018(7) -0.009(7) C7 0.091(7) 0.062(6) 0.056(5) 0.002(5) 0.014(5) -0.006(5) C8 0.076(6) 0.056(5) 0.053(5) -0.010(4) 0.009(5) 0.000(5) C9 0.081(7) 0.052(5) 0.057(5) 0.000(4) 0.011(5) 0.003(5) C10 0.080(7) 0.072(6) 0.055(5) -0.001(5) 0.009(5) 0.009(5) C11 0.090(7) 0.060(6) 0.058(5) -0.007(5) -0.011(5) -0.004(5) C12 0.073(6) 0.059(5) 0.054(5) -0.001(4) -0.004(5) -0.004(5) C13 0.079(7) 0.066(6) 0.052(5) -0.003(4) 0.011(5) -0.005(5) C14 0.075(6) 0.052(5) 0.061(5) 0.001(4) -0.006(5) -0.004(5) C15 0.069(6) 0.060(5) 0.055(5) -0.005(4) 0.004(5) -0.003(5) C16 0.085(7) 0.052(5) 0.063(6) -0.002(4) 0.013(5) -0.001(5) C17 0.082(7) 0.053(5) 0.064(6) -0.002(4) 0.011(5) -0.012(5) C18 0.069(6) 0.061(6) 0.068(6) -0.008(5) -0.002(5) -0.002(5) C19 0.095(8) 0.068(6) 0.067(6) -0.008(5) -0.005(6) -0.006(6) C20 0.106(9) 0.074(7) 0.080(7) 0.020(6) -0.008(7) -0.001(6) C21 0.087(8) 0.118(9) 0.082(7) 0.026(6) 0.002(7) -0.007(7) C22 0.073(6) 0.056(6) 0.045(5) 0.008(4) 0.006(5) 0.001(5) C23 0.068(7) 0.064(6) 0.068(6) 0.013(5) 0.002(5) 0.002(5) C24 0.071(7) 0.078(7) 0.065(6) 0.012(5) -0.005(5) -0.011(6) C25 0.081(7) 0.048(5) 0.063(6) 0.001(4) 0.009(5) -0.006(5) C26 0.085(7) 0.061(6) 0.056(5) 0.005(4) 0.004(5) -0.009(5) C27 0.082(7) 0.051(5) 0.051(5) 0.002(4) 0.008(5) -0.009(5) C28 0.093(7) 0.057(6) 0.065(6) -0.001(5) 0.007(6) -0.004(5) C29 0.076(6) 0.046(5) 0.070(6) 0.007(4) 0.018(5) -0.011(5) C30 0.090(7) 0.047(5) 0.060(5) 0.009(4) 0.006(5) 0.005(5) C31 0.075(6) 0.052(5) 0.068(6) 0.002(4) 0.001(5) 0.001(5) C32 0.077(6) 0.052(5) 0.061(5) 0.003(4) 0.007(5) -0.005(5) C33 0.071(6) 0.042(5) 0.061(5) 0.000(4) 0.006(5) -0.002(4) C34 0.085(7) 0.046(5) 0.064(6) 0.004(4) 0.006(5) -0.009(5) C35 0.075(6) 0.049(5) 0.064(5) -0.003(4) 0.007(5) 0.000(5) C36 0.069(6) 0.059(5) 0.053(5) -0.002(4) 0.008(5) -0.010(5) C37 0.080(6) 0.043(5) 0.060(5) 0.004(4) -0.008(5) 0.001(5) C38 0.075(7) 0.058(6) 0.064(6) -0.005(5) 0.006(5) -0.007(5) C39 0.085(7) 0.057(5) 0.061(6) -0.001(4) -0.001(5) -0.008(5) C40 0.071(6) 0.058(6) 0.063(6) 0.000(4) 0.006(5) 0.003(5) C41 0.096(8) 0.071(6) 0.066(6) 0.000(5) 0.013(6) -0.005(6) C42 0.119(9) 0.089(7) 0.078(7) 0.003(6) 0.016(7) -0.027(7) _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 N4 2.016(7) . ? Zn1 N2 2.015(8) . ? Zn1 Cl2 2.249(2) . ? Zn1 Cl1 2.251(3) . ? N1 C1 1.321(12) . ? N1 C3 1.371(14) . ? N1 C4 1.415(12) . ? N2 C1 1.317(10) . ? N2 C2 1.395(12) . ? N3 C22 1.336(10) . ? N3 C24 1.378(10) . ? N3 C25 1.454(9) . ? N4 C22 1.306(9) . ? N4 C23 1.414(11) . ? C2 C3 1.298(15) . ? C4 C5 1.366(14) . ? C5 C6 1.541(14) . ? C6 C7 1.509(12) . ? C7 C8 1.508(10) . ? C8 C9 1.518(10) . ? C9 C10 1.515(11) . ? C10 C11 1.521(11) . ? C11 C12 1.521(11) . ? C12 C13 1.523(11) . ? C13 C14 1.511(10) . ? C14 C15 1.511(11) . ? C15 C16 1.506(10) . ? C16 C17 1.525(11) . ? C17 C18 1.501(11) . ? C18 C19 1.522(11) . ? C19 C20 1.494(11) . ? C20 C21 1.542(13) . ? C23 C24 1.342(11) . ? C25 C26 1.519(11) . ? C26 C27 1.523(10) . ? C27 C28 1.532(11) . ? C28 C29 1.501(10) . ? C29 C30 1.507(11) . ? C30 C31 1.507(10) . ? C31 C32 1.528(11) . ? C32 C33 1.509(10) . ? C33 C34 1.520(11) . ? C34 C35 1.532(11) . ? C35 C36 1.530(11) . ? C36 C37 1.507(10) . ? C37 C38 1.546(11) . ? C38 C39 1.504(11) . ? C39 C40 1.519(11) . ? C40 C41 1.514(11) . ? C41 C42 1.516(12) . ? 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 N4 Zn1 N2 110.1(3) . . ? N4 Zn1 Cl2 106.7(2) . . ? N2 Zn1 Cl2 107.8(2) . . ? N4 Zn1 Cl1 106.8(2) . . ? N2 Zn1 Cl1 106.3(2) . . ? Cl2 Zn1 Cl1 119.02(11) . . ? C1 N1 C3 104.5(9) . . ? C1 N1 C4 127.6(12) . . ? C3 N1 C4 127.9(13) . . ? C1 N2 C2 104.6(9) . . ? C1 N2 Zn1 128.9(7) . . ? C2 N2 Zn1 126.4(8) . . ? C22 N3 C24 106.8(6) . . ? C22 N3 C25 126.5(8) . . ? C24 N3 C25 126.5(8) . . ? C22 N4 C23 104.6(7) . . ? C22 N4 Zn1 127.9(7) . . ? C23 N4 Zn1 127.2(6) . . ? N2 C1 N1 112.8(10) . . ? C3 C2 N2 108.0(11) . . ? C2 C3 N1 110.0(11) . . ? C5 C4 N1 120.2(10) . . ? C4 C5 C6 120.9(11) . . ? C7 C6 C5 111.6(9) . . ? C8 C7 C6 114.3(7) . . ? C7 C8 C9 114.7(7) . . ? C10 C9 C8 114.8(7) . . ? C9 C10 C11 115.1(7) . . ? C10 C11 C12 115.3(7) . . ? C13 C12 C11 114.8(7) . . ? C14 C13 C12 114.7(7) . . ? C15 C14 C13 115.2(7) . . ? C16 C15 C14 114.5(7) . . ? C15 C16 C17 114.9(7) . . ? C18 C17 C16 116.2(7) . . ? C17 C18 C19 116.0(7) . . ? C20 C19 C18 115.2(8) . . ? C19 C20 C21 114.4(8) . . ? N4 C22 N3 112.8(8) . . ? C24 C23 N4 108.9(8) . . ? C23 C24 N3 106.8(8) . . ? N3 C25 C26 112.5(7) . . ? C25 C26 C27 112.8(7) . . ? C26 C27 C28 111.4(7) . . ? C29 C28 C27 114.6(7) . . ? C28 C29 C30 114.3(7) . . ? C31 C30 C29 116.6(7) . . ? C30 C31 C32 115.6(7) . . ? C33 C32 C31 114.6(7) . . ? C32 C33 C34 113.5(7) . . ? C33 C34 C35 114.1(7) . . ? C34 C35 C36 114.3(7) . . ? C37 C36 C35 113.5(7) . . ? C36 C37 C38 114.7(7) . . ? C39 C38 C37 114.1(7) . . ? C38 C39 C40 115.0(7) . . ? C41 C40 C39 113.7(7) . . ? C40 C41 C42 114.6(8) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.473 _refine_diff_density_min -0.954 _refine_diff_density_rms 0.067