# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2006 data_global _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Gregory Solan' _publ_contact_author_address ; Department of Chemistry University of Leicester George Porter Building 1A3 Leicester LE1 7RH UNITED KINGDOM ; _publ_contact_author_email GAS8@LE.AC.UK _publ_section_title ; Factors affecting imine coordination in [{Imino-terpyridine}MX2] (M = Fe, Co, Ni, Zn): Synthesis, structures, DFT calculations and ethylene oligomerisation studies ; loop_ _publ_author_name 'Gregory Solan' 'Rajinder K. Chaggar' 'Yohan D M Champouret' 'John Fawcett' 'Jean-Didier Marechal' ; F.Maseras ; 'Kuldip Singh' # Attachment '03112m.cif' data_03112m _database_code_depnum_ccdc_archive 'CCDC 615609' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C29 H30 Br2 N4 Ni) 3.5(C H Cl3)' _chemical_formula_sum 'C32.50 H33.50 Br2 Cl10.50 N4 Ni' _chemical_formula_weight 1070.89 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' Cl Cl 0.1484 0.1585 '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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c 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 33.824(8) _cell_length_b 10.759(3) _cell_length_c 23.446(6) _cell_angle_alpha 90.00 _cell_angle_beta 100.613(4) _cell_angle_gamma 90.00 _cell_volume 8386(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2193 _cell_measurement_theta_min 2.223 _cell_measurement_theta_max 24.585 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.696 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4264 _exptl_absorpt_coefficient_mu 3.068 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min o.517 _exptl_absorpt_correction_T_max 0.928 _exptl_absorpt_process_details ; absorption correction based on 4683 reflections(SADABS);Rint 0.0867 before correction and 0.0554 after. ; _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 '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 31356 _diffrn_reflns_av_R_equivalents 0.1464 _diffrn_reflns_av_sigmaI/netI 0.1803 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.22 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8219 _reflns_number_gt 2851 _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 '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^)+(0.1742P)^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 constrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8219 _refine_ls_number_parameters 454 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2232 _refine_ls_R_factor_gt 0.1088 _refine_ls_wR_factor_ref 0.3250 _refine_ls_wR_factor_gt 0.2653 _refine_ls_goodness_of_fit_ref 0.893 _refine_ls_restrained_S_all 0.893 _refine_ls_shift/su_max 0.002 _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 Ni1 Ni 0.16709(5) 0.67176(18) 0.10509(7) 0.0500(5) Uani 1 1 d . . . Br1 Br 0.15305(5) 0.84880(17) 0.02994(6) 0.0642(5) Uani 1 1 d . . . Br2 Br 0.18328(5) 0.51090(15) 0.18371(6) 0.0606(5) Uani 1 1 d . . . N1 N 0.1651(3) 0.7993(12) 0.1703(4) 0.053(3) Uani 1 1 d . . . N2 N 0.2234(3) 0.7238(12) 0.1216(4) 0.053(3) Uani 1 1 d . . . N3 N 0.1904(3) 0.5802(11) 0.0463(4) 0.049(3) Uani 1 1 d . . . N4 N 0.1170(3) 0.5543(12) 0.0639(4) 0.055(3) Uani 1 1 d . . . C1 C 0.1332(5) 0.8368(16) 0.1909(6) 0.064(4) Uani 1 1 d . . . H1 H 0.1074 0.8044 0.1747 0.077 Uiso 1 1 calc R . . C2 C 0.1369(5) 0.9240(15) 0.2363(6) 0.063(4) Uani 1 1 d . . . H2 H 0.1138 0.9544 0.2495 0.076 Uiso 1 1 calc R . . C3 C 0.1750(5) 0.9644(15) 0.2612(6) 0.062(4) Uani 1 1 d . . . H3 H 0.1783 1.0179 0.2939 0.075 Uiso 1 1 calc R . . C4 C 0.2077(5) 0.9284(14) 0.2394(6) 0.058(4) Uani 1 1 d . . . H4 H 0.2336 0.9609 0.2548 0.070 Uiso 1 1 calc R . . C5 C 0.2025(4) 0.8438(13) 0.1946(5) 0.044(3) Uani 1 1 d . . . C6 C 0.2357(4) 0.8033(13) 0.1661(5) 0.047(4) Uani 1 1 d . . . C7 C 0.2758(4) 0.8294(14) 0.1819(7) 0.059(4) Uani 1 1 d . . . H7 H 0.2854 0.8811 0.2143 0.071 Uiso 1 1 calc R . . C8 C 0.3020(5) 0.7794(15) 0.1497(6) 0.059(4) Uani 1 1 d . . . H8 H 0.3299 0.7965 0.1603 0.071 Uiso 1 1 calc R . . C9 C 0.2883(4) 0.7049(13) 0.1026(5) 0.049(3) Uani 1 1 d . . . H9 H 0.3061 0.6716 0.0795 0.058 Uiso 1 1 calc R . . C10 C 0.2485(4) 0.6814(13) 0.0907(5) 0.046(3) Uani 1 1 d . . . C11 C 0.2279(4) 0.6043(14) 0.0428(5) 0.050(4) Uani 1 1 d . . . C12 C 0.2431(5) 0.5556(15) -0.0032(6) 0.062(4) Uani 1 1 d . . . H12 H 0.2706 0.5664 -0.0057 0.075 Uiso 1 1 calc R . . C13 C 0.2175(5) 0.4910(14) -0.0453(6) 0.064(4) Uani 1 1 d . . . H13 H 0.2277 0.4592 -0.0775 0.077 Uiso 1 1 calc R . . C14 C 0.1789(5) 0.4711(14) -0.0428(6) 0.061(4) Uani 1 1 d . . . H14 H 0.1615 0.4292 -0.0732 0.073 Uiso 1 1 calc R . . C15 C 0.1654(4) 0.5132(14) 0.0050(6) 0.057(4) Uani 1 1 d . . . C16 C 0.1247(4) 0.4997(16) 0.0171(6) 0.062(4) Uani 1 1 d . . . C17 C 0.0956(4) 0.4219(16) -0.0244(7) 0.075(5) Uani 1 1 d . . . H17A H 0.1060 0.3371 -0.0250 0.112 Uiso 1 1 calc R . . H17B H 0.0922 0.4579 -0.0634 0.112 Uiso 1 1 calc R . . H17C H 0.0695 0.4201 -0.0117 0.112 Uiso 1 1 calc R . . C18 C 0.0809(5) 0.5297(18) 0.0821(6) 0.064(5) Uani 1 1 d . . . C19 C 0.0729(5) 0.4165(18) 0.1088(7) 0.067(5) Uani 1 1 d . . . C20 C 0.0387(6) 0.402(2) 0.1318(10) 0.120(9) Uani 1 1 d . . . H20 H 0.0336 0.3267 0.1502 0.145 Uiso 1 1 calc R . . C21 C 0.0112(7) 0.503(3) 0.1276(10) 0.122(10) Uani 1 1 d . . . H21 H -0.0120 0.4960 0.1450 0.147 Uiso 1 1 calc R . . C22 C 0.0171(5) 0.610(2) 0.0994(11) 0.102(8) Uani 1 1 d . . . H22 H -0.0028 0.6730 0.0947 0.122 Uiso 1 1 calc R . . C23 C 0.0508(6) 0.627(2) 0.0780(8) 0.081(6) Uani 1 1 d . . . C24 C 0.1019(5) 0.3063(18) 0.1130(7) 0.073(5) Uani 1 1 d . . . H24 H 0.1262 0.3315 0.0971 0.088 Uiso 1 1 calc R . . C25 C 0.1151(5) 0.2599(18) 0.1747(7) 0.087(6) Uani 1 1 d . . . H25A H 0.1332 0.3208 0.1970 0.130 Uiso 1 1 calc R . . H25B H 0.1292 0.1804 0.1742 0.130 Uiso 1 1 calc R . . H25C H 0.0914 0.2486 0.1928 0.130 Uiso 1 1 calc R . . C26 C 0.0818(6) 0.1956(19) 0.0781(9) 0.102(7) Uani 1 1 d . . . H26A H 0.0561 0.1774 0.0900 0.153 Uiso 1 1 calc R . . H26B H 0.0994 0.1228 0.0854 0.153 Uiso 1 1 calc R . . H26C H 0.0770 0.2158 0.0366 0.153 Uiso 1 1 calc R . . C27 C 0.0563(5) 0.7392(19) 0.0446(8) 0.084(6) Uani 1 1 d . . . H27 H 0.0859 0.7557 0.0505 0.101 Uiso 1 1 calc R . . C28 C 0.0417(6) 0.723(2) -0.0197(9) 0.128(9) Uani 1 1 d . . . H28A H 0.0601 0.6684 -0.0356 0.193 Uiso 1 1 calc R . . H28B H 0.0409 0.8047 -0.0388 0.193 Uiso 1 1 calc R . . H28C H 0.0147 0.6871 -0.0266 0.193 Uiso 1 1 calc R . . C29 C 0.0365(6) 0.8554(19) 0.0656(9) 0.119(8) Uani 1 1 d . . . H29A H 0.0099 0.8678 0.0414 0.178 Uiso 1 1 calc R . . H29B H 0.0534 0.9283 0.0626 0.178 Uiso 1 1 calc R . . H29C H 0.0337 0.8439 0.1061 0.178 Uiso 1 1 calc R . . C30 C 0.2760(5) 0.7360(19) 0.3712(8) 0.096(7) Uani 1 1 d . . . H30 H 0.2929 0.7991 0.3554 0.115 Uiso 1 1 calc R . . Cl1 Cl 0.24454(18) 0.6693(5) 0.31416(19) 0.0968(16) Uani 1 1 d . . . Cl2 Cl 0.30813(16) 0.6200(6) 0.4067(2) 0.113(2) Uani 1 1 d . . . Cl3 Cl 0.2482(2) 0.8117(5) 0.4154(2) 0.119(2) Uani 1 1 d . . . C31 C 0.1079(5) 0.989(2) 0.4112(6) 0.095(7) Uani 1 1 d . . . H31 H 0.1115 1.0307 0.4498 0.114 Uiso 1 1 calc R . . Cl4 Cl 0.10333(15) 1.1043(5) 0.3577(2) 0.0948(16) Uani 1 1 d . . . Cl5 Cl 0.14954(19) 0.8976(6) 0.4099(2) 0.116(2) Uani 1 1 d . . . Cl6 Cl 0.06425(19) 0.9018(8) 0.4027(3) 0.160(3) Uani 1 1 d . . . C32 C 0.0997(6) 0.5574(19) 0.2742(7) 0.089(6) Uani 1 1 d . . . H32 H 0.1054 0.5327 0.2354 0.107 Uiso 1 1 calc R . . Cl7 Cl 0.1398(2) 0.6215(8) 0.3110(2) 0.148(3) Uani 1 1 d . . . Cl8 Cl 0.0879(2) 0.4243(6) 0.3096(3) 0.130(2) Uani 1 1 d . . . Cl9 Cl 0.05827(17) 0.6538(6) 0.2635(3) 0.165(3) Uani 1 1 d . . . C33 C 0.01238(17) 0.0389(6) 0.2655(3) 0.35(7) Uani 0.50 1 d PR . . Cl10 Cl 0.02669(17) 0.0109(6) 0.2065(3) 0.133(5) Uani 0.50 1 d PR . . Cl11 Cl 0.00000(17) 0.1991(6) 0.2500(3) 0.121(6) Uani 0.50 2 d SPR . . 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 Ni1 0.0509(11) 0.0730(14) 0.0278(8) -0.0041(8) 0.0114(7) 0.0088(9) Br1 0.0640(10) 0.0894(13) 0.0394(8) 0.0076(8) 0.0104(7) 0.0181(9) Br2 0.0746(11) 0.0727(12) 0.0337(7) 0.0009(7) 0.0081(7) 0.0012(9) N1 0.034(6) 0.080(9) 0.042(6) 0.009(6) 0.001(5) 0.003(6) N2 0.054(7) 0.088(9) 0.022(5) 0.014(6) 0.017(5) 0.036(7) N3 0.048(7) 0.074(9) 0.024(5) 0.004(5) 0.006(5) 0.014(6) N4 0.055(7) 0.081(9) 0.036(6) -0.018(6) 0.023(5) 0.001(6) C1 0.058(9) 0.100(13) 0.039(8) -0.011(8) 0.018(7) 0.002(9) C2 0.069(11) 0.072(12) 0.060(9) -0.008(8) 0.037(8) 0.002(9) C3 0.069(11) 0.066(11) 0.059(9) -0.011(8) 0.032(8) 0.000(9) C4 0.066(10) 0.069(11) 0.039(8) 0.000(7) 0.009(7) 0.007(8) C5 0.054(8) 0.055(9) 0.021(6) 0.003(6) 0.004(5) -0.002(7) C6 0.061(9) 0.068(10) 0.018(6) 0.010(6) 0.020(6) 0.011(8) C7 0.050(9) 0.064(11) 0.064(9) 0.019(8) 0.011(7) -0.006(8) C8 0.053(9) 0.065(11) 0.061(10) 0.017(8) 0.013(8) 0.008(8) C9 0.055(9) 0.060(10) 0.031(7) 0.002(6) 0.009(6) 0.001(7) C10 0.043(8) 0.063(10) 0.028(6) 0.005(6) 0.000(6) 0.001(7) C11 0.055(9) 0.065(10) 0.033(7) 0.014(6) 0.020(6) 0.018(7) C12 0.077(11) 0.074(12) 0.034(7) 0.013(7) 0.004(7) 0.042(9) C13 0.090(12) 0.065(11) 0.044(8) 0.011(8) 0.032(8) 0.027(9) C14 0.079(11) 0.077(12) 0.034(7) -0.005(7) 0.031(7) 0.037(9) C15 0.061(9) 0.067(11) 0.044(8) 0.010(7) 0.015(7) 0.022(8) C16 0.045(8) 0.091(13) 0.047(8) -0.013(8) 0.001(7) 0.006(8) C17 0.059(10) 0.093(14) 0.068(10) -0.034(10) -0.001(8) -0.002(9) C18 0.055(10) 0.094(14) 0.041(8) -0.020(8) -0.001(7) 0.013(10) C19 0.055(10) 0.090(14) 0.057(10) -0.012(9) 0.011(8) 0.007(10) C20 0.062(13) 0.16(2) 0.15(2) -0.067(18) 0.054(13) -0.011(14) C21 0.087(16) 0.16(3) 0.14(2) -0.091(19) 0.069(15) -0.044(17) C22 0.051(11) 0.097(17) 0.17(2) -0.061(16) 0.050(13) -0.014(11) C23 0.072(13) 0.092(16) 0.077(12) -0.046(11) 0.008(10) -0.019(11) C24 0.063(10) 0.103(15) 0.057(10) -0.011(10) 0.019(8) -0.010(10) C25 0.100(14) 0.087(15) 0.072(12) 0.007(11) 0.013(10) -0.025(11) C26 0.086(14) 0.101(17) 0.124(17) -0.029(14) 0.032(12) -0.010(12) C27 0.052(10) 0.092(16) 0.105(15) -0.052(13) 0.006(10) 0.022(10) C28 0.126(19) 0.15(2) 0.104(17) -0.050(16) 0.010(14) 0.048(16) C29 0.109(17) 0.103(18) 0.14(2) -0.057(15) 0.008(14) 0.028(13) C30 0.053(10) 0.122(17) 0.106(15) 0.072(13) -0.001(9) -0.024(10) Cl1 0.156(5) 0.078(4) 0.058(3) 0.000(2) 0.024(3) 0.001(3) Cl2 0.090(4) 0.146(5) 0.103(4) 0.044(4) 0.014(3) -0.019(3) Cl3 0.192(6) 0.090(4) 0.095(4) -0.035(3) 0.075(4) -0.045(4) C31 0.063(11) 0.19(2) 0.029(8) 0.015(11) 0.000(7) -0.041(13) Cl4 0.114(4) 0.107(4) 0.068(3) -0.007(3) 0.026(3) -0.025(3) Cl5 0.138(5) 0.126(5) 0.087(4) -0.010(3) 0.024(3) -0.015(4) Cl6 0.126(5) 0.230(8) 0.109(5) 0.046(5) -0.017(4) -0.105(5) C32 0.103(15) 0.114(17) 0.052(10) 0.006(11) 0.020(10) 0.016(12) Cl7 0.161(6) 0.206(8) 0.066(3) 0.027(4) -0.007(3) -0.046(5) Cl8 0.161(6) 0.108(5) 0.138(5) 0.027(4) 0.074(4) 0.031(4) Cl9 0.116(5) 0.167(7) 0.206(8) 0.041(6) 0.011(5) 0.030(5) C33 0.13(5) 0.58(14) 0.26(7) 0.35(9) -0.15(5) -0.18(7) Cl10 0.076(7) 0.204(15) 0.119(9) -0.066(10) 0.017(6) 0.033(8) Cl11 0.162(16) 0.085(12) 0.106(12) 0.000 -0.002(11) 0.000 _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 Ni1 N2 1.953(12) . ? Ni1 N3 1.972(10) . ? Ni1 N1 2.064(12) . ? Ni1 N4 2.191(12) . ? Ni1 Br2 2.514(2) . ? Ni1 Br1 2.579(2) . ? N1 C1 1.325(16) . ? N1 C5 1.374(15) . ? N2 C10 1.297(15) . ? N2 C6 1.353(17) . ? N3 C11 1.313(16) . ? N3 C15 1.368(17) . ? N4 C16 1.313(16) . ? N4 C18 1.390(18) . ? C1 C2 1.407(19) . ? C1 H1 0.9500 . ? C2 C3 1.38(2) . ? C2 H2 0.9500 . ? C3 C4 1.357(18) . ? C3 H3 0.9500 . ? C4 C5 1.376(18) . ? C4 H4 0.9500 . ? C5 C6 1.474(17) . ? C6 C7 1.369(18) . ? C7 C8 1.373(19) . ? C7 H7 0.9500 . ? C8 C9 1.375(19) . ? C8 H8 0.9500 . ? C9 C10 1.349(17) . ? C9 H9 0.9500 . ? C10 C11 1.464(19) . ? C11 C12 1.381(17) . ? C12 C13 1.38(2) . ? C12 H12 0.9500 . ? C13 C14 1.33(2) . ? C13 H13 0.9500 . ? C14 C15 1.365(17) . ? C14 H14 0.9500 . ? C15 C16 1.462(19) . ? C16 C17 1.504(19) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.42(2) . ? C18 C23 1.45(2) . ? C19 C20 1.37(2) . ? C19 C24 1.53(2) . ? C20 C21 1.42(3) . ? C20 H20 0.9500 . ? C21 C22 1.36(3) . ? C21 H21 0.9500 . ? C22 C23 1.34(2) . ? C22 H22 0.9500 . ? C23 C27 1.47(3) . ? C24 C25 1.52(2) . ? C24 C26 1.53(2) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.51(2) . ? C27 C29 1.54(2) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 Cl1 1.706(19) . ? C30 Cl3 1.73(2) . ? C30 Cl2 1.760(18) . ? C30 H30 1.0000 . ? C31 Cl5 1.72(2) . ? C31 Cl6 1.728(16) . ? C31 Cl4 1.751(18) . ? C31 H31 1.0000 . ? C32 Cl7 1.62(2) . ? C32 Cl9 1.723(19) . ? C32 Cl8 1.74(2) . ? C32 H32 1.0000 . ? C33 C33 1.004(12) 2 ? C33 Cl10 1.5766 . ? C33 Cl10 1.607(12) 2 ? C33 Cl11 1.7950 . ? Cl10 C33 1.607(12) 2 ? Cl11 C33 1.795(3) 2 ? 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 N2 Ni1 N3 77.4(5) . . ? N2 Ni1 N1 79.9(4) . . ? N3 Ni1 N1 157.0(5) . . ? N2 Ni1 N4 154.1(4) . . ? N3 Ni1 N4 77.3(4) . . ? N1 Ni1 N4 125.6(4) . . ? N2 Ni1 Br2 88.8(3) . . ? N3 Ni1 Br2 96.2(3) . . ? N1 Ni1 Br2 87.0(3) . . ? N4 Ni1 Br2 88.4(3) . . ? N2 Ni1 Br1 88.5(3) . . ? N3 Ni1 Br1 86.5(3) . . ? N1 Ni1 Br1 89.3(3) . . ? N4 Ni1 Br1 95.4(3) . . ? Br2 Ni1 Br1 175.74(10) . . ? C1 N1 C5 119.5(13) . . ? C1 N1 Ni1 127.7(10) . . ? C5 N1 Ni1 112.8(8) . . ? C10 N2 C6 120.9(12) . . ? C10 N2 Ni1 120.1(10) . . ? C6 N2 Ni1 119.0(8) . . ? C11 N3 C15 122.6(11) . . ? C11 N3 Ni1 117.4(10) . . ? C15 N3 Ni1 118.9(9) . . ? C16 N4 C18 119.5(12) . . ? C16 N4 Ni1 111.7(9) . . ? C18 N4 Ni1 128.8(8) . . ? N1 C1 C2 121.0(14) . . ? N1 C1 H1 119.5 . . ? C2 C1 H1 119.5 . . ? C3 C2 C1 118.3(14) . . ? C3 C2 H2 120.8 . . ? C1 C2 H2 120.8 . . ? C4 C3 C2 120.8(15) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C3 C4 C5 118.5(15) . . ? C3 C4 H4 120.7 . . ? C5 C4 H4 120.7 . . ? N1 C5 C4 121.7(12) . . ? N1 C5 C6 115.3(11) . . ? C4 C5 C6 122.8(13) . . ? N2 C6 C7 119.1(12) . . ? N2 C6 C5 112.6(12) . . ? C7 C6 C5 128.1(13) . . ? C6 C7 C8 118.6(15) . . ? C6 C7 H7 120.7 . . ? C8 C7 H7 120.7 . . ? C7 C8 C9 121.0(15) . . ? C7 C8 H8 119.5 . . ? C9 C8 H8 119.5 . . ? C10 C9 C8 116.8(13) . . ? C10 C9 H9 121.6 . . ? C8 C9 H9 121.6 . . ? N2 C10 C9 123.4(13) . . ? N2 C10 C11 111.2(12) . . ? C9 C10 C11 125.5(13) . . ? N3 C11 C12 118.5(14) . . ? N3 C11 C10 113.1(11) . . ? C12 C11 C10 128.4(14) . . ? C13 C12 C11 118.4(15) . . ? C13 C12 H12 120.8 . . ? C11 C12 H12 120.8 . . ? C14 C13 C12 122.8(14) . . ? C14 C13 H13 118.6 . . ? C12 C13 H13 118.6 . . ? C13 C14 C15 117.5(15) . . ? C13 C14 H14 121.3 . . ? C15 C14 H14 121.3 . . ? C14 C15 N3 120.0(14) . . ? C14 C15 C16 126.5(15) . . ? N3 C15 C16 113.4(12) . . ? N4 C16 C15 117.1(13) . . ? N4 C16 C17 125.6(13) . . ? C15 C16 C17 117.3(13) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N4 C18 C19 123.3(15) . . ? N4 C18 C23 119.2(17) . . ? C19 C18 C23 117.4(16) . . ? C20 C19 C18 120.9(18) . . ? C20 C19 C24 117.6(19) . . ? C18 C19 C24 121.5(15) . . ? C19 C20 C21 118(2) . . ? C19 C20 H20 120.8 . . ? C21 C20 H20 120.8 . . ? C22 C21 C20 122(2) . . ? C22 C21 H21 119.1 . . ? C20 C21 H21 119.1 . . ? C23 C22 C21 121(2) . . ? C23 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? C22 C23 C18 121(2) . . ? C22 C23 C27 121(2) . . ? C18 C23 C27 118.0(17) . . ? C25 C24 C19 112.9(14) . . ? C25 C24 C26 106.1(16) . . ? C19 C24 C26 110.6(14) . . ? C25 C24 H24 109.0 . . ? C19 C24 H24 109.0 . . ? C26 C24 H24 109.0 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 C28 113.0(17) . . ? C23 C27 C29 112.9(17) . . ? C28 C27 C29 109.2(17) . . ? C23 C27 H27 107.1 . . ? C28 C27 H27 107.1 . . ? C29 C27 H27 107.1 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Cl1 C30 Cl3 109.8(9) . . ? Cl1 C30 Cl2 108.3(12) . . ? Cl3 C30 Cl2 114.0(10) . . ? Cl1 C30 H30 108.2 . . ? Cl3 C30 H30 108.2 . . ? Cl2 C30 H30 108.2 . . ? Cl5 C31 Cl6 112.0(13) . . ? Cl5 C31 Cl4 110.9(9) . . ? Cl6 C31 Cl4 109.9(9) . . ? Cl5 C31 H31 108.0 . . ? Cl6 C31 H31 108.0 . . ? Cl4 C31 H31 108.0 . . ? Cl7 C32 Cl9 113.6(13) . . ? Cl7 C32 Cl8 109.9(10) . . ? Cl9 C32 Cl8 108.3(11) . . ? Cl7 C32 H32 108.3 . . ? Cl9 C32 H32 108.3 . . ? Cl8 C32 H32 108.3 . . ? C33 C33 Cl10 73.3(7) 2 . ? C33 C33 Cl10 70.0(6) 2 2 ? Cl10 C33 Cl10 136.9(4) . 2 ? C33 C33 Cl11 73.8 2 . ? Cl10 C33 Cl11 95.9 . . ? Cl10 C33 Cl11 94.82(13) 2 . ? C33 Cl10 C33 36.7(5) . 2 ? C33 Cl11 C33 32.5(4) 2 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ni1 N1 C1 176.5(13) . . . . ? N3 Ni1 N1 C1 167.2(12) . . . . ? N4 Ni1 N1 C1 -8.3(14) . . . . ? Br2 Ni1 N1 C1 -94.2(12) . . . . ? Br1 Ni1 N1 C1 87.9(12) . . . . ? N2 Ni1 N1 C5 -5.8(9) . . . . ? N3 Ni1 N1 C5 -15.1(17) . . . . ? N4 Ni1 N1 C5 169.4(8) . . . . ? Br2 Ni1 N1 C5 83.6(8) . . . . ? Br1 Ni1 N1 C5 -94.4(8) . . . . ? N3 Ni1 N2 C10 0.2(10) . . . . ? N1 Ni1 N2 C10 -176.1(11) . . . . ? N4 Ni1 N2 C10 12.9(16) . . . . ? Br2 Ni1 N2 C10 96.8(10) . . . . ? Br1 Ni1 N2 C10 -86.5(10) . . . . ? N3 Ni1 N2 C6 -179.1(10) . . . . ? N1 Ni1 N2 C6 4.6(9) . . . . ? N4 Ni1 N2 C6 -166.4(10) . . . . ? Br2 Ni1 N2 C6 -82.5(9) . . . . ? Br1 Ni1 N2 C6 94.2(9) . . . . ? N2 Ni1 N3 C11 -5.9(9) . . . . ? N1 Ni1 N3 C11 3.5(17) . . . . ? N4 Ni1 N3 C11 179.8(10) . . . . ? Br2 Ni1 N3 C11 -93.2(9) . . . . ? Br1 Ni1 N3 C11 83.4(9) . . . . ? N2 Ni1 N3 C15 -174.2(11) . . . . ? N1 Ni1 N3 C15 -164.8(11) . . . . ? N4 Ni1 N3 C15 11.4(10) . . . . ? Br2 Ni1 N3 C15 98.4(10) . . . . ? Br1 Ni1 N3 C15 -85.0(10) . . . . ? N2 Ni1 N4 C16 -22.6(17) . . . . ? N3 Ni1 N4 C16 -9.9(10) . . . . ? N1 Ni1 N4 C16 168.3(10) . . . . ? Br2 Ni1 N4 C16 -106.6(10) . . . . ? Br1 Ni1 N4 C16 75.2(10) . . . . ? N2 Ni1 N4 C18 155.0(13) . . . . ? N3 Ni1 N4 C18 167.6(14) . . . . ? N1 Ni1 N4 C18 -14.2(16) . . . . ? Br2 Ni1 N4 C18 71.0(13) . . . . ? Br1 Ni1 N4 C18 -107.2(13) . . . . ? C5 N1 C1 C2 2(2) . . . . ? Ni1 N1 C1 C2 179.2(11) . . . . ? N1 C1 C2 C3 -4(2) . . . . ? C1 C2 C3 C4 5(2) . . . . ? C2 C3 C4 C5 -5(2) . . . . ? C1 N1 C5 C4 -1(2) . . . . ? Ni1 N1 C5 C4 -179.0(10) . . . . ? C1 N1 C5 C6 -176.0(13) . . . . ? Ni1 N1 C5 C6 6.1(14) . . . . ? C3 C4 C5 N1 2(2) . . . . ? C3 C4 C5 C6 177.0(13) . . . . ? C10 N2 C6 C7 -6.3(19) . . . . ? Ni1 N2 C6 C7 173.0(9) . . . . ? C10 N2 C6 C5 178.1(11) . . . . ? Ni1 N2 C6 C5 -2.6(14) . . . . ? N1 C5 C6 N2 -2.6(16) . . . . ? C4 C5 C6 N2 -177.4(12) . . . . ? N1 C5 C6 C7 -177.7(13) . . . . ? C4 C5 C6 C7 7(2) . . . . ? N2 C6 C7 C8 3.6(19) . . . . ? C5 C6 C7 C8 178.5(13) . . . . ? C6 C7 C8 C9 0(2) . . . . ? C7 C8 C9 C10 -2(2) . . . . ? C6 N2 C10 C9 5(2) . . . . ? Ni1 N2 C10 C9 -174.3(10) . . . . ? C6 N2 C10 C11 -176.1(11) . . . . ? Ni1 N2 C10 C11 4.7(15) . . . . ? C8 C9 C10 N2 -1(2) . . . . ? C8 C9 C10 C11 -179.8(13) . . . . ? C15 N3 C11 C12 -3(2) . . . . ? Ni1 N3 C11 C12 -170.6(10) . . . . ? C15 N3 C11 C10 177.8(12) . . . . ? Ni1 N3 C11 C10 9.9(15) . . . . ? N2 C10 C11 N3 -9.2(17) . . . . ? C9 C10 C11 N3 169.7(13) . . . . ? N2 C10 C11 C12 171.4(13) . . . . ? C9 C10 C11 C12 -10(2) . . . . ? N3 C11 C12 C13 4(2) . . . . ? C10 C11 C12 C13 -176.4(13) . . . . ? C11 C12 C13 C14 -2(2) . . . . ? C12 C13 C14 C15 -3(2) . . . . ? C13 C14 C15 N3 4(2) . . . . ? C13 C14 C15 C16 -178.9(14) . . . . ? C11 N3 C15 C14 -2(2) . . . . ? Ni1 N3 C15 C14 166.1(11) . . . . ? C11 N3 C15 C16 -178.8(13) . . . . ? Ni1 N3 C15 C16 -11.1(16) . . . . ? C18 N4 C16 C15 -170.5(14) . . . . ? Ni1 N4 C16 C15 7.3(17) . . . . ? C18 N4 C16 C17 8(2) . . . . ? Ni1 N4 C16 C17 -174.4(13) . . . . ? C14 C15 C16 N4 -175.5(15) . . . . ? N3 C15 C16 N4 2(2) . . . . ? C14 C15 C16 C17 6(2) . . . . ? N3 C15 C16 C17 -177.0(13) . . . . ? C16 N4 C18 C19 73.9(19) . . . . ? Ni1 N4 C18 C19 -103.5(16) . . . . ? C16 N4 C18 C23 -111.1(17) . . . . ? Ni1 N4 C18 C23 71.5(17) . . . . ? N4 C18 C19 C20 172.5(15) . . . . ? C23 C18 C19 C20 -3(2) . . . . ? N4 C18 C19 C24 -7(2) . . . . ? C23 C18 C19 C24 177.5(13) . . . . ? C18 C19 C20 C21 1(3) . . . . ? C24 C19 C20 C21 -179.2(17) . . . . ? C19 C20 C21 C22 3(3) . . . . ? C20 C21 C22 C23 -5(4) . . . . ? C21 C22 C23 C18 3(3) . . . . ? C21 C22 C23 C27 176.5(19) . . . . ? N4 C18 C23 C22 -174.6(15) . . . . ? C19 C18 C23 C22 1(2) . . . . ? N4 C18 C23 C27 12(2) . . . . ? C19 C18 C23 C27 -173.0(14) . . . . ? C20 C19 C24 C25 -55(2) . . . . ? C18 C19 C24 C25 125.2(16) . . . . ? C20 C19 C24 C26 64(2) . . . . ? C18 C19 C24 C26 -116.1(17) . . . . ? C22 C23 C27 C28 -91(2) . . . . ? C18 C23 C27 C28 82.8(19) . . . . ? C22 C23 C27 C29 34(2) . . . . ? C18 C23 C27 C29 -152.7(15) . . . . ? Cl10 C33 Cl10 C33 32.5(3) 2 . . 2 ? Cl11 C33 Cl10 C33 -71.06(16) . . . 2 ? Cl10 C33 Cl11 C33 70.7(8) . . . 2 ? Cl10 C33 Cl11 C33 -67.5(7) 2 . . 2 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.950 _refine_diff_density_min -1.183 _refine_diff_density_rms 0.202 # Attachment '04048.cif' data_04048 _database_code_depnum_ccdc_archive 'CCDC 615610' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C28 H28 Cl2 N4 Zn) (C H Cl3)' _chemical_formula_sum 'C29 H29 Cl5 N4 Zn' _chemical_formula_weight 676.18 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.3842(7) _cell_length_b 16.8912(11) _cell_length_c 17.4972(12) _cell_angle_alpha 90.00 _cell_angle_beta 96.1660(10) _cell_angle_gamma 90.00 _cell_volume 3051.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6420 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 25.22 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.472 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1384 _exptl_absorpt_coefficient_mu 1.269 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.784 _exptl_absorpt_correction_T_max 0.894 _exptl_absorpt_process_details ; absorption correction based on 10464 reflections (SADABS); Rint 0.036 before correction and 0.022 after. ; _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 '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 23670 _diffrn_reflns_av_R_equivalents 0.0366 _diffrn_reflns_av_sigmaI/netI 0.0421 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5986 _reflns_number_gt 4763 _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 '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^)+(0.0496P)^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 constrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5986 _refine_ls_number_parameters 374 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0471 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.0919 _refine_ls_wR_factor_gt 0.0884 _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_restrained_S_all 0.974 _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 Zn1 Zn 0.43755(3) 0.452569(15) 0.797350(15) 0.02309(9) Uani 1 1 d . . . Cl1 Cl 0.54626(6) 0.38865(3) 0.71204(3) 0.03119(16) Uani 1 1 d . . . Cl2 Cl 0.25168(6) 0.39737(4) 0.82721(4) 0.03511(17) Uani 1 1 d . . . N1 N 0.55535(18) 0.41309(11) 0.90198(11) 0.0256(4) Uani 1 1 d . . . N2 N 0.51278(18) 0.55580(10) 0.84834(11) 0.0222(4) Uani 1 1 d . . . N3 N 0.35284(18) 0.55067(10) 0.71999(11) 0.0228(4) Uani 1 1 d . . . N4 N 0.17627(19) 0.45619(11) 0.56116(11) 0.0269(5) Uani 1 1 d . . . C1 C 0.5681(3) 0.33816(14) 0.92647(15) 0.0327(6) Uani 1 1 d . . . H1 H 0.5235 0.2975 0.8968 0.039 Uiso 1 1 calc R . . C2 C 0.6436(2) 0.31795(15) 0.99313(15) 0.0358(6) Uani 1 1 d . . . H2 H 0.6519 0.2642 1.0089 0.043 Uiso 1 1 calc R . . C3 C 0.7066(2) 0.37672(15) 1.03636(15) 0.0332(6) Uani 1 1 d . . . H3 H 0.7589 0.3641 1.0827 0.040 Uiso 1 1 calc R . . C4 C 0.6935(2) 0.45455(14) 1.01215(14) 0.0289(6) Uani 1 1 d . . . H4 H 0.7355 0.4961 1.0417 0.035 Uiso 1 1 calc R . . C5 C 0.6178(2) 0.47040(13) 0.94383(13) 0.0235(5) Uani 1 1 d . . . C6 C 0.5979(2) 0.55129(13) 0.91179(13) 0.0241(5) Uani 1 1 d . . . C7 C 0.6617(2) 0.61799(15) 0.94249(15) 0.0323(6) Uani 1 1 d . . . H7 H 0.7202 0.6146 0.9880 0.039 Uiso 1 1 calc R . . C8 C 0.6380(3) 0.68966(15) 0.90534(15) 0.0358(6) Uani 1 1 d . . . H8 H 0.6833 0.7358 0.9241 0.043 Uiso 1 1 calc R . . C9 C 0.5492(2) 0.69435(14) 0.84130(14) 0.0319(6) Uani 1 1 d . . . H9 H 0.5317 0.7435 0.8160 0.038 Uiso 1 1 calc R . . C10 C 0.4854(2) 0.62577(13) 0.81426(13) 0.0235(5) Uani 1 1 d . . . C11 C 0.3852(2) 0.62345(13) 0.74773(13) 0.0235(5) Uani 1 1 d . . . C12 C 0.3262(2) 0.69150(14) 0.71611(14) 0.0292(6) Uani 1 1 d . . . H12 H 0.3491 0.7420 0.7372 0.035 Uiso 1 1 calc R . . C13 C 0.2337(3) 0.68464(14) 0.65356(14) 0.0329(6) Uani 1 1 d . . . H13 H 0.1912 0.7304 0.6316 0.040 Uiso 1 1 calc R . . C14 C 0.2037(2) 0.61058(14) 0.62337(14) 0.0294(6) Uani 1 1 d . . . H14 H 0.1415 0.6046 0.5798 0.035 Uiso 1 1 calc R . . C15 C 0.2660(2) 0.54492(13) 0.65778(13) 0.0235(5) Uani 1 1 d . . . C16 C 0.2398(2) 0.46430(13) 0.62637(14) 0.0244(5) Uani 1 1 d . . . H16 H 0.2706 0.4191 0.6551 0.029 Uiso 1 1 calc R . . C17 C 0.1490(2) 0.37909(13) 0.53016(13) 0.0250(5) Uani 1 1 d . . . C18 C 0.2135(2) 0.35666(14) 0.46627(14) 0.0274(5) Uani 1 1 d . . . C19 C 0.1784(2) 0.28532(15) 0.43053(14) 0.0319(6) Uani 1 1 d . . . H19 H 0.2200 0.2689 0.3874 0.038 Uiso 1 1 calc R . . C20 C 0.0842(2) 0.23795(15) 0.45657(14) 0.0351(6) Uani 1 1 d . . . H20 H 0.0612 0.1894 0.4313 0.042 Uiso 1 1 calc R . . C21 C 0.0235(2) 0.26094(15) 0.51919(14) 0.0323(6) Uani 1 1 d . . . H21 H -0.0412 0.2276 0.5365 0.039 Uiso 1 1 calc R . . C22 C 0.0539(2) 0.33138(14) 0.55778(14) 0.0280(6) Uani 1 1 d . . . C23 C 0.3197(3) 0.40772(15) 0.44075(15) 0.0364(6) Uani 1 1 d . . . H23 H 0.2979 0.4641 0.4511 0.044 Uiso 1 1 calc R . . C24 C 0.4504(3) 0.38898(18) 0.48722(18) 0.0476(8) Uani 1 1 d . . . H24A H 0.4449 0.4004 0.5417 0.071 Uiso 1 1 calc R . . H24B H 0.5183 0.4217 0.4685 0.071 Uiso 1 1 calc R . . H24C H 0.4711 0.3329 0.4811 0.071 Uiso 1 1 calc R . . C25 C 0.3347(3) 0.4003(2) 0.35520(17) 0.0587(9) Uani 1 1 d . . . H25A H 0.3612 0.3463 0.3440 0.088 Uiso 1 1 calc R . . H25B H 0.4006 0.4378 0.3416 0.088 Uiso 1 1 calc R . . H25C H 0.2518 0.4123 0.3252 0.088 Uiso 1 1 calc R . . C26 C -0.0194(2) 0.35556(15) 0.62437(14) 0.0326(6) Uani 1 1 d . . . H26 H 0.0257 0.4026 0.6495 0.039 Uiso 1 1 calc R . . C27 C -0.0200(5) 0.2919(2) 0.68399(19) 0.0934(15) Uani 1 1 d . . . H27A H -0.0589 0.3125 0.7286 0.140 Uiso 1 1 calc R . . H27B H 0.0690 0.2750 0.7000 0.140 Uiso 1 1 calc R . . H27C H -0.0707 0.2467 0.6624 0.140 Uiso 1 1 calc R . . C28 C -0.1541(4) 0.3805(3) 0.5956(2) 0.0978(17) Uani 1 1 d . . . H28A H -0.1995 0.3363 0.5683 0.147 Uiso 1 1 calc R . . H28B H -0.1506 0.4254 0.5604 0.147 Uiso 1 1 calc R . . H28C H -0.2004 0.3961 0.6391 0.147 Uiso 1 1 calc R . . C29 C 0.9706(3) 0.5015(2) 0.82452(19) 0.0578(9) Uani 1 1 d . . . H29 H 1.0393 0.4598 0.8271 0.069 Uiso 1 1 d R A . Cl3 Cl 0.82085(8) 0.45665(5) 0.79734(5) 0.0571(2) Uani 1 1 d . A . Cl4 Cl 0.9675(2) 0.55967(14) 0.90794(14) 0.0952(7) Uani 0.67 1 d P A 1 Cl5 Cl 1.0027(4) 0.5688(3) 0.7503(2) 0.0873(11) Uani 0.67 1 d P A 1 Cl4' Cl 0.9793(3) 0.5060(3) 0.9258(2) 0.0741(11) Uani 0.33 1 d P A 2 Cl5' Cl 1.0046(9) 0.5827(5) 0.7843(4) 0.106(3) Uani 0.33 1 d P A 2 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 0.02457(16) 0.01827(15) 0.02615(17) -0.00020(11) 0.00148(12) -0.00116(11) Cl1 0.0347(4) 0.0243(3) 0.0350(4) -0.0056(3) 0.0055(3) 0.0028(3) Cl2 0.0275(3) 0.0362(4) 0.0416(4) 0.0101(3) 0.0036(3) -0.0059(3) N1 0.0261(11) 0.0215(11) 0.0289(11) 0.0016(9) 0.0013(9) 0.0017(9) N2 0.0230(10) 0.0185(10) 0.0257(11) -0.0012(8) 0.0049(8) -0.0004(8) N3 0.0247(11) 0.0188(10) 0.0253(11) 0.0006(8) 0.0053(9) -0.0002(8) N4 0.0298(12) 0.0218(11) 0.0285(12) -0.0013(8) 0.0006(9) 0.0003(9) C1 0.0344(15) 0.0242(14) 0.0386(16) 0.0006(11) 0.0005(12) -0.0001(11) C2 0.0364(16) 0.0285(14) 0.0415(16) 0.0088(12) -0.0007(13) 0.0068(12) C3 0.0278(14) 0.0388(16) 0.0321(15) 0.0074(12) -0.0002(11) 0.0067(12) C4 0.0241(13) 0.0317(14) 0.0303(14) -0.0019(11) 0.0000(11) 0.0013(11) C5 0.0195(12) 0.0252(13) 0.0264(13) 0.0000(10) 0.0059(10) 0.0021(10) C6 0.0207(12) 0.0251(13) 0.0267(13) -0.0020(10) 0.0034(10) 0.0002(10) C7 0.0326(15) 0.0293(14) 0.0336(15) -0.0010(11) -0.0036(12) -0.0020(11) C8 0.0384(16) 0.0238(13) 0.0434(16) -0.0051(12) -0.0039(13) -0.0063(12) C9 0.0377(15) 0.0203(13) 0.0366(15) 0.0018(11) -0.0010(12) -0.0015(11) C10 0.0268(13) 0.0191(12) 0.0250(13) -0.0006(9) 0.0052(10) 0.0006(10) C11 0.0258(13) 0.0194(12) 0.0258(13) 0.0003(10) 0.0054(10) -0.0019(10) C12 0.0378(15) 0.0170(12) 0.0322(14) 0.0005(10) 0.0014(12) -0.0005(11) C13 0.0405(16) 0.0227(13) 0.0341(15) 0.0046(11) -0.0025(12) 0.0036(11) C14 0.0347(15) 0.0275(14) 0.0248(13) 0.0003(10) -0.0027(11) 0.0011(11) C15 0.0255(13) 0.0223(12) 0.0231(12) -0.0007(10) 0.0046(10) -0.0017(10) C16 0.0268(13) 0.0202(12) 0.0263(13) 0.0026(10) 0.0029(11) -0.0004(10) C17 0.0271(13) 0.0217(12) 0.0243(13) -0.0023(10) -0.0057(10) 0.0049(10) C18 0.0290(14) 0.0261(13) 0.0266(13) 0.0018(10) 0.0005(11) 0.0072(11) C19 0.0371(15) 0.0318(14) 0.0263(14) -0.0051(11) 0.0008(11) 0.0082(12) C20 0.0354(15) 0.0295(15) 0.0387(16) -0.0113(12) -0.0044(13) 0.0015(12) C21 0.0287(14) 0.0293(14) 0.0379(15) -0.0045(11) -0.0009(12) -0.0020(11) C22 0.0263(13) 0.0266(13) 0.0298(14) -0.0009(10) -0.0023(11) 0.0009(10) C23 0.0430(17) 0.0276(14) 0.0404(16) 0.0019(12) 0.0130(13) 0.0051(12) C24 0.0386(17) 0.0461(18) 0.059(2) -0.0017(15) 0.0098(15) -0.0011(14) C25 0.070(2) 0.067(2) 0.0428(19) 0.0113(16) 0.0210(17) -0.0008(18) C26 0.0358(15) 0.0317(14) 0.0312(14) -0.0042(11) 0.0073(12) -0.0065(12) C27 0.180(5) 0.060(2) 0.047(2) 0.0093(18) 0.044(3) 0.020(3) C28 0.065(3) 0.190(5) 0.040(2) -0.017(3) 0.0111(18) 0.063(3) C29 0.0315(17) 0.070(2) 0.074(2) -0.0095(19) 0.0116(15) 0.0009(16) Cl3 0.0435(5) 0.0616(5) 0.0690(6) -0.0181(4) 0.0182(4) -0.0105(4) Cl4 0.0560(11) 0.1362(19) 0.0931(16) -0.0509(15) 0.0067(10) -0.0281(14) Cl5 0.0660(17) 0.091(2) 0.113(3) 0.0118(17) 0.045(2) -0.0129(13) Cl4' 0.0345(15) 0.123(3) 0.064(2) -0.028(2) 0.0020(13) -0.010(2) Cl5' 0.084(4) 0.070(4) 0.157(7) 0.032(5) -0.016(5) -0.031(3) _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 N2 2.0729(18) . ? Zn1 N1 2.1935(19) . ? Zn1 Cl1 2.2429(6) . ? Zn1 Cl2 2.2548(7) . ? Zn1 N3 2.2574(18) . ? N1 C1 1.338(3) . ? N1 C5 1.339(3) . ? N2 C10 1.340(3) . ? N2 C6 1.345(3) . ? N3 C15 1.340(3) . ? N3 C11 1.351(3) . ? N4 C16 1.263(3) . ? N4 C17 1.427(3) . ? C1 C2 1.377(3) . ? C2 C3 1.371(4) . ? C3 C4 1.383(3) . ? C4 C5 1.384(3) . ? C5 C6 1.483(3) . ? C6 C7 1.385(3) . ? C7 C8 1.384(3) . ? C8 C9 1.375(3) . ? C9 C10 1.392(3) . ? C10 C11 1.476(3) . ? C11 C12 1.389(3) . ? C12 C13 1.381(3) . ? C13 C14 1.380(3) . ? C14 C15 1.388(3) . ? C15 C16 1.483(3) . ? C17 C22 1.401(3) . ? C17 C18 1.415(3) . ? C18 C19 1.388(3) . ? C18 C23 1.505(4) . ? C19 C20 1.378(4) . ? C20 C21 1.378(3) . ? C21 C22 1.388(3) . ? C22 C26 1.515(3) . ? C23 C25 1.526(4) . ? C23 C24 1.538(4) . ? C26 C28 1.495(4) . ? C26 C27 1.498(4) . ? C29 Cl5' 1.598(9) . ? C29 Cl3 1.749(3) . ? C29 Cl4 1.762(4) . ? C29 Cl4' 1.766(5) . ? C29 Cl5 1.783(6) . ? 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 N2 Zn1 N1 75.28(7) . . ? N2 Zn1 Cl1 119.87(5) . . ? N1 Zn1 Cl1 97.68(5) . . ? N2 Zn1 Cl2 122.72(5) . . ? N1 Zn1 Cl2 95.48(5) . . ? Cl1 Zn1 Cl2 117.37(3) . . ? N2 Zn1 N3 75.24(7) . . ? N1 Zn1 N3 150.47(7) . . ? Cl1 Zn1 N3 98.39(5) . . ? Cl2 Zn1 N3 98.88(5) . . ? C1 N1 C5 118.9(2) . . ? C1 N1 Zn1 125.59(16) . . ? C5 N1 Zn1 115.52(15) . . ? C10 N2 C6 120.41(19) . . ? C10 N2 Zn1 119.88(15) . . ? C6 N2 Zn1 119.44(15) . . ? C15 N3 C11 118.51(19) . . ? C15 N3 Zn1 128.22(15) . . ? C11 N3 Zn1 112.75(15) . . ? C16 N4 C17 120.4(2) . . ? N1 C1 C2 122.2(2) . . ? C3 C2 C1 118.9(2) . . ? C2 C3 C4 119.6(2) . . ? C3 C4 C5 118.4(2) . . ? N1 C5 C4 122.0(2) . . ? N1 C5 C6 114.8(2) . . ? C4 C5 C6 123.2(2) . . ? N2 C6 C7 121.2(2) . . ? N2 C6 C5 114.6(2) . . ? C7 C6 C5 124.1(2) . . ? C8 C7 C6 118.4(2) . . ? C9 C8 C7 120.2(2) . . ? C8 C9 C10 118.8(2) . . ? N2 C10 C9 120.8(2) . . ? N2 C10 C11 115.16(19) . . ? C9 C10 C11 124.0(2) . . ? N3 C11 C12 121.9(2) . . ? N3 C11 C10 115.76(19) . . ? C12 C11 C10 122.4(2) . . ? C13 C12 C11 119.0(2) . . ? C14 C13 C12 119.2(2) . . ? C13 C14 C15 118.9(2) . . ? N3 C15 C14 122.4(2) . . ? N3 C15 C16 116.6(2) . . ? C14 C15 C16 121.0(2) . . ? N4 C16 C15 119.5(2) . . ? C22 C17 C18 122.0(2) . . ? C22 C17 N4 120.8(2) . . ? C18 C17 N4 117.0(2) . . ? C19 C18 C17 117.7(2) . . ? C19 C18 C23 121.9(2) . . ? C17 C18 C23 120.3(2) . . ? C20 C19 C18 121.1(2) . . ? C21 C20 C19 120.1(2) . . ? C20 C21 C22 121.9(2) . . ? C21 C22 C17 117.2(2) . . ? C21 C22 C26 119.9(2) . . ? C17 C22 C26 122.8(2) . . ? C18 C23 C25 113.5(2) . . ? C18 C23 C24 111.0(2) . . ? C25 C23 C24 108.9(2) . . ? C28 C26 C27 111.3(3) . . ? C28 C26 C22 110.2(2) . . ? C27 C26 C22 112.5(2) . . ? Cl5' C29 Cl3 119.0(4) . . ? Cl5' C29 Cl4 84.9(3) . . ? Cl3 C29 Cl4 111.83(18) . . ? Cl5' C29 Cl4' 114.6(4) . . ? Cl3 C29 Cl4' 103.8(2) . . ? Cl4 C29 Cl4' 31.68(14) . . ? Cl5' C29 Cl5 20.8(3) . . ? Cl3 C29 Cl5 107.9(2) . . ? Cl4 C29 Cl5 105.6(2) . . ? Cl4' C29 Cl5 135.3(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.756 _refine_diff_density_min -0.554 _refine_diff_density_rms 0.068 # Attachment '04057.cif' data_04057 _database_code_depnum_ccdc_archive 'CCDC 615611' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C28 H28 Cl2 N4 Fe) (C2 H3 N)' _chemical_formula_sum 'C30 H31 Cl2 Fe N5' _chemical_formula_weight 588.35 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' Fe Fe 0.3463 0.8444 '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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.0666(12) _cell_length_b 17.260(2) _cell_length_c 16.987(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.542(2) _cell_angle_gamma 90.00 _cell_volume 2932.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5197 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 27.16 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.333 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 0.724 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.748 _exptl_absorpt_correction_T_max 0.894 _exptl_absorpt_process_details ; absorption correction based on 8788 reflections (SADABS); Rint 0.033 before correction and 0.026 after. ; _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 '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 20994 _diffrn_reflns_av_R_equivalents 0.0383 _diffrn_reflns_av_sigmaI/netI 0.0413 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5155 _reflns_number_gt 4281 _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 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; A molecule of lattice MeCN was modelled as disordered. 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^)+(0.0577P)^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 constrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5155 _refine_ls_number_parameters 367 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0497 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.1089 _refine_ls_wR_factor_gt 0.1039 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.002 _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 Fe1 Fe 0.93828(3) 0.546237(19) 0.79414(2) 0.02378(13) Uani 1 1 d . . . Cl1 Cl 0.74444(7) 0.60542(4) 0.81955(4) 0.0392(2) Uani 1 1 d . . . Cl2 Cl 1.06227(6) 0.61409(4) 0.71096(4) 0.03335(18) Uani 1 1 d . . . N1 N 1.0606(2) 0.58162(12) 0.90198(12) 0.0265(5) Uani 1 1 d . . . N2 N 1.01582(19) 0.44279(11) 0.84700(11) 0.0208(4) Uani 1 1 d . . . N3 N 0.85250(19) 0.45163(11) 0.71548(11) 0.0208(4) Uani 1 1 d . . . N4 N 0.6616(2) 0.55065(11) 0.55765(12) 0.0240(5) Uani 1 1 d . . . C1 C 1.0758(3) 0.65506(15) 0.92657(16) 0.0337(6) Uani 1 1 d . . . H1 H 1.0296 0.6948 0.8959 0.040 Uiso 1 1 calc R . . C2 C 1.1560(3) 0.67518(16) 0.99472(16) 0.0370(7) Uani 1 1 d . . . H2 H 1.1658 0.7279 1.0105 0.044 Uiso 1 1 calc R . . C3 C 1.2214(3) 0.61759(16) 1.03943(16) 0.0342(7) Uani 1 1 d . . . H3 H 1.2767 0.6301 1.0868 0.041 Uiso 1 1 calc R . . C4 C 1.2068(3) 0.54160(15) 1.01534(15) 0.0306(6) Uani 1 1 d . . . H4 H 1.2514 0.5011 1.0457 0.037 Uiso 1 1 calc R . . C5 C 1.1254(2) 0.52545(14) 0.94560(14) 0.0244(6) Uani 1 1 d . . . C6 C 1.1028(2) 0.44625(14) 0.91284(14) 0.0243(6) Uani 1 1 d . . . C7 C 1.1639(3) 0.38002(15) 0.94538(16) 0.0326(6) Uani 1 1 d . . . H7 H 1.2246 0.3827 0.9924 0.039 Uiso 1 1 calc R . . C8 C 1.1349(3) 0.31015(15) 0.90829(16) 0.0342(7) Uani 1 1 d . . . H8 H 1.1779 0.2643 0.9289 0.041 Uiso 1 1 calc R . . C9 C 1.0436(3) 0.30639(15) 0.84128(15) 0.0304(6) Uani 1 1 d . . . H9 H 1.0222 0.2583 0.8158 0.036 Uiso 1 1 calc R . . C10 C 0.9841(2) 0.37452(13) 0.81217(14) 0.0224(5) Uani 1 1 d . . . C11 C 0.8813(2) 0.37895(14) 0.74276(14) 0.0222(5) Uani 1 1 d . . . C12 C 0.8165(2) 0.31433(14) 0.70927(15) 0.0283(6) Uani 1 1 d . . . H12 H 0.8391 0.2640 0.7292 0.034 Uiso 1 1 calc R . . C13 C 0.7182(3) 0.32411(15) 0.64624(15) 0.0319(6) Uani 1 1 d . . . H13 H 0.6706 0.2806 0.6233 0.038 Uiso 1 1 calc R . . C14 C 0.6898(2) 0.39734(14) 0.61696(15) 0.0284(6) Uani 1 1 d . . . H14 H 0.6232 0.4049 0.5733 0.034 Uiso 1 1 calc R . . C15 C 0.7602(2) 0.46012(13) 0.65226(14) 0.0223(5) Uani 1 1 d . . . C16 C 0.7392(2) 0.53917(14) 0.62042(14) 0.0228(5) Uani 1 1 d . . . H16 H 0.7843 0.5816 0.6472 0.027 Uiso 1 1 calc R . . C17 C 0.6415(2) 0.62731(14) 0.52727(14) 0.0226(5) Uani 1 1 d . . . C18 C 0.5579(2) 0.67886(14) 0.56256(14) 0.0246(6) Uani 1 1 d . . . C19 C 0.5328(2) 0.75023(15) 0.52563(15) 0.0287(6) Uani 1 1 d . . . H19 H 0.4771 0.7865 0.5481 0.034 Uiso 1 1 calc R . . C20 C 0.5868(2) 0.76960(15) 0.45719(15) 0.0317(6) Uani 1 1 d . . . H20 H 0.5674 0.8185 0.4330 0.038 Uiso 1 1 calc R . . C21 C 0.6687(2) 0.71830(15) 0.42394(15) 0.0302(6) Uani 1 1 d . . . H21 H 0.7054 0.7323 0.3768 0.036 Uiso 1 1 calc R . . C22 C 0.6986(2) 0.64652(14) 0.45800(14) 0.0267(6) Uani 1 1 d . . . C23 C 0.4916(3) 0.65562(16) 0.63479(15) 0.0340(6) Uani 1 1 d . . . H23 H 0.5574 0.6240 0.6698 0.041 Uiso 1 1 calc R . . C24 C 0.4498(5) 0.7224(2) 0.6831(2) 0.0863(14) Uani 1 1 d . . . H24A H 0.5267 0.7564 0.6976 0.129 Uiso 1 1 calc R . . H24B H 0.4165 0.7027 0.7313 0.129 Uiso 1 1 calc R . . H24C H 0.3789 0.7518 0.6519 0.129 Uiso 1 1 calc R . . C25 C 0.3706(3) 0.6034(3) 0.6081(2) 0.0749(12) Uani 1 1 d . . . H25A H 0.3295 0.5861 0.6547 0.112 Uiso 1 1 calc R . . H25B H 0.4004 0.5582 0.5799 0.112 Uiso 1 1 calc R . . H25C H 0.3050 0.6327 0.5729 0.112 Uiso 1 1 calc R . . C26 C 0.7944(3) 0.59107(16) 0.42429(16) 0.0368(7) Uani 1 1 d . . . H26 H 0.7718 0.5375 0.4409 0.044 Uiso 1 1 calc R . . C27 C 0.7816(4) 0.5923(2) 0.33369(18) 0.0624(10) Uani 1 1 d . . . H27A H 0.6878 0.5843 0.3126 0.094 Uiso 1 1 calc R . . H27B H 0.8365 0.5509 0.3148 0.094 Uiso 1 1 calc R . . H27C H 0.8122 0.6425 0.3157 0.094 Uiso 1 1 calc R . . C28 C 0.9384(3) 0.6078(2) 0.4590(2) 0.0583(10) Uani 1 1 d . . . H28A H 0.9642 0.6596 0.4427 0.088 Uiso 1 1 calc R . . H28B H 0.9981 0.5691 0.4396 0.088 Uiso 1 1 calc R . . H28C H 0.9452 0.6053 0.5169 0.088 Uiso 1 1 calc R . . N5 N 0.3958(4) 0.5553(2) 0.8327(2) 0.0936(12) Uani 1 1 d . . . C29 C 0.4724(6) 0.4481(6) 0.9219(8) 0.167(6) Uani 0.67 1 d P A 1 H29A H 0.5417 0.4682 0.9619 0.251 Uiso 0.67 1 calc PR A 1 H29B H 0.5094 0.4057 0.8927 0.251 Uiso 0.67 1 calc PR A 1 H29C H 0.3970 0.4287 0.9480 0.251 Uiso 0.67 1 calc PR A 1 C30 C 0.4374(6) 0.4952(4) 0.8800(6) 0.077(2) Uani 0.67 1 d P A 1 C30' C 0.4791(19) 0.4741(9) 0.8297(10) 0.084(5) Uani 0.33 1 d P A 2 C29' C 0.527(2) 0.4213(8) 0.8264(13) 0.168(14) Uani 0.33 1 d P A 2 H29D H 0.5197 0.3919 0.8751 0.252 Uiso 0.33 1 calc PR A 2 H29E H 0.6211 0.4298 0.8201 0.252 Uiso 0.33 1 calc PR A 2 H29F H 0.4841 0.3921 0.7808 0.252 Uiso 0.33 1 calc PR A 2 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 Fe1 0.0267(2) 0.0176(2) 0.0261(2) -0.00009(14) -0.00094(16) 0.00111(14) Cl1 0.0343(4) 0.0487(5) 0.0342(4) -0.0091(3) 0.0024(3) 0.0146(3) Cl2 0.0337(4) 0.0269(4) 0.0402(4) 0.0053(3) 0.0076(3) -0.0029(3) N1 0.0276(11) 0.0235(12) 0.0281(12) -0.0012(9) 0.0023(9) -0.0028(9) N2 0.0210(11) 0.0200(11) 0.0214(11) 0.0018(8) 0.0021(9) -0.0009(8) N3 0.0210(10) 0.0203(11) 0.0217(11) -0.0002(8) 0.0047(9) -0.0002(8) N4 0.0258(11) 0.0242(12) 0.0223(11) 0.0016(9) 0.0043(9) 0.0006(9) C1 0.0378(16) 0.0255(15) 0.0366(16) -0.0023(12) -0.0004(13) -0.0021(12) C2 0.0404(17) 0.0300(16) 0.0406(17) -0.0076(13) 0.0048(14) -0.0095(13) C3 0.0312(15) 0.0418(17) 0.0286(15) -0.0046(13) -0.0008(12) -0.0114(13) C4 0.0270(14) 0.0363(16) 0.0276(14) 0.0037(12) -0.0003(11) -0.0047(12) C5 0.0205(13) 0.0270(14) 0.0259(14) 0.0005(11) 0.0037(11) -0.0033(11) C6 0.0209(13) 0.0270(14) 0.0250(13) 0.0030(11) 0.0028(11) -0.0003(10) C7 0.0297(15) 0.0320(16) 0.0340(15) 0.0036(12) -0.0055(12) 0.0020(12) C8 0.0347(16) 0.0256(15) 0.0400(16) 0.0056(12) -0.0063(13) 0.0065(12) C9 0.0369(15) 0.0215(14) 0.0321(15) -0.0005(11) 0.0014(12) 0.0021(11) C10 0.0239(13) 0.0205(13) 0.0232(13) 0.0022(10) 0.0041(10) -0.0006(10) C11 0.0237(13) 0.0207(13) 0.0231(13) -0.0007(10) 0.0065(10) -0.0012(10) C12 0.0347(15) 0.0187(13) 0.0310(15) 0.0012(11) 0.0021(12) -0.0008(11) C13 0.0363(16) 0.0235(14) 0.0342(15) -0.0025(12) -0.0038(13) -0.0060(11) C14 0.0292(14) 0.0272(14) 0.0276(14) -0.0008(11) -0.0021(11) -0.0017(11) C15 0.0234(13) 0.0233(13) 0.0206(13) -0.0005(10) 0.0039(10) 0.0006(10) C16 0.0215(13) 0.0223(13) 0.0247(13) -0.0021(10) 0.0033(11) 0.0004(10) C17 0.0238(13) 0.0218(13) 0.0211(13) 0.0004(10) -0.0024(10) -0.0040(10) C18 0.0239(13) 0.0250(14) 0.0239(13) -0.0003(11) -0.0019(11) -0.0009(10) C19 0.0260(14) 0.0261(14) 0.0326(15) 0.0003(11) -0.0029(11) 0.0022(11) C20 0.0314(14) 0.0284(15) 0.0327(15) 0.0084(12) -0.0075(12) -0.0043(12) C21 0.0324(15) 0.0325(15) 0.0251(14) 0.0054(12) 0.0013(11) -0.0078(12) C22 0.0273(14) 0.0261(14) 0.0262(14) 0.0001(11) 0.0014(11) -0.0042(11) C23 0.0375(16) 0.0386(16) 0.0265(14) 0.0020(12) 0.0068(12) 0.0115(13) C24 0.162(4) 0.056(2) 0.050(2) 0.0108(18) 0.051(3) 0.042(3) C25 0.055(2) 0.125(4) 0.047(2) 0.009(2) 0.0187(18) -0.029(2) C26 0.0471(18) 0.0311(16) 0.0352(16) 0.0004(12) 0.0173(14) -0.0004(13) C27 0.089(3) 0.063(2) 0.0393(19) -0.0020(17) 0.0264(18) 0.012(2) C28 0.0426(19) 0.058(2) 0.079(3) 0.0007(18) 0.0237(18) 0.0062(16) N5 0.080(3) 0.111(3) 0.088(3) 0.021(2) 0.004(2) -0.011(2) C29 0.024(3) 0.112(7) 0.368(17) 0.155(10) 0.037(6) 0.009(4) C30 0.024(3) 0.052(4) 0.156(8) 0.032(6) 0.020(4) 0.000(3) C30' 0.084(12) 0.053(10) 0.099(12) 0.005(8) -0.063(9) -0.018(9) C29' 0.19(2) 0.017(7) 0.25(3) -0.003(10) -0.19(2) 0.009(10) _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 Fe1 N2 2.1081(19) . ? Fe1 N1 2.175(2) . ? Fe1 N3 2.2214(19) . ? Fe1 Cl1 2.2868(8) . ? Fe1 Cl2 2.3081(7) . ? N1 C1 1.338(3) . ? N1 C5 1.343(3) . ? N2 C10 1.341(3) . ? N2 C6 1.341(3) . ? N3 C15 1.346(3) . ? N3 C11 1.357(3) . ? N4 C16 1.264(3) . ? N4 C17 1.426(3) . ? C1 C2 1.378(4) . ? C2 C3 1.373(4) . ? C3 C4 1.377(4) . ? C4 C5 1.390(3) . ? C5 C6 1.484(3) . ? C6 C7 1.383(3) . ? C7 C8 1.377(4) . ? C8 C9 1.380(3) . ? C9 C10 1.385(3) . ? C10 C11 1.479(3) . ? C11 C12 1.381(3) . ? C12 C13 1.383(3) . ? C13 C14 1.376(3) . ? C14 C15 1.393(3) . ? C15 C16 1.474(3) . ? C17 C18 1.405(3) . ? C17 C22 1.407(3) . ? C18 C19 1.392(3) . ? C18 C23 1.516(3) . ? C19 C20 1.380(3) . ? C20 C21 1.374(4) . ? C21 C22 1.386(3) . ? C22 C26 1.516(4) . ? C23 C24 1.503(4) . ? C23 C25 1.541(4) . ? C26 C28 1.529(4) . ? C26 C27 1.530(4) . ? N5 C30 1.349(8) . ? N5 C30' 1.64(2) . ? C29 C30 1.111(9) . ? C30' C29' 1.03(2) . ? 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 N2 Fe1 N1 74.48(8) . . ? N2 Fe1 N3 74.53(7) . . ? N1 Fe1 N3 148.97(8) . . ? N2 Fe1 Cl1 125.48(6) . . ? N1 Fe1 Cl1 97.41(6) . . ? N3 Fe1 Cl1 99.22(5) . . ? N2 Fe1 Cl2 119.39(6) . . ? N1 Fe1 Cl2 94.55(6) . . ? N3 Fe1 Cl2 101.84(5) . . ? Cl1 Fe1 Cl2 114.93(3) . . ? C1 N1 C5 118.7(2) . . ? C1 N1 Fe1 124.23(18) . . ? C5 N1 Fe1 117.04(16) . . ? C10 N2 C6 120.5(2) . . ? C10 N2 Fe1 119.90(15) . . ? C6 N2 Fe1 119.50(15) . . ? C15 N3 C11 118.3(2) . . ? C15 N3 Fe1 125.85(15) . . ? C11 N3 Fe1 114.89(15) . . ? C16 N4 C17 120.0(2) . . ? N1 C1 C2 122.4(3) . . ? C3 C2 C1 118.7(3) . . ? C2 C3 C4 119.8(3) . . ? C3 C4 C5 118.5(2) . . ? N1 C5 C4 121.8(2) . . ? N1 C5 C6 114.5(2) . . ? C4 C5 C6 123.7(2) . . ? N2 C6 C7 121.0(2) . . ? N2 C6 C5 114.3(2) . . ? C7 C6 C5 124.7(2) . . ? C8 C7 C6 118.7(2) . . ? C7 C8 C9 120.3(2) . . ? C8 C9 C10 118.3(2) . . ? N2 C10 C9 121.1(2) . . ? N2 C10 C11 114.6(2) . . ? C9 C10 C11 124.3(2) . . ? N3 C11 C12 122.2(2) . . ? N3 C11 C10 115.0(2) . . ? C12 C11 C10 122.7(2) . . ? C11 C12 C13 118.9(2) . . ? C14 C13 C12 119.5(2) . . ? C13 C14 C15 119.0(2) . . ? N3 C15 C14 122.0(2) . . ? N3 C15 C16 116.8(2) . . ? C14 C15 C16 121.2(2) . . ? N4 C16 C15 120.2(2) . . ? C18 C17 C22 122.0(2) . . ? C18 C17 N4 120.0(2) . . ? C22 C17 N4 117.8(2) . . ? C19 C18 C17 117.0(2) . . ? C19 C18 C23 121.7(2) . . ? C17 C18 C23 121.2(2) . . ? C20 C19 C18 121.7(2) . . ? C21 C20 C19 120.2(2) . . ? C20 C21 C22 121.1(2) . . ? C21 C22 C17 118.0(2) . . ? C21 C22 C26 121.6(2) . . ? C17 C22 C26 120.3(2) . . ? C24 C23 C18 114.5(2) . . ? C24 C23 C25 110.4(3) . . ? C18 C23 C25 108.9(2) . . ? C22 C26 C28 110.6(2) . . ? C22 C26 C27 112.7(2) . . ? C28 C26 C27 110.7(3) . . ? C30 N5 C30' 40.1(6) . . ? C29 C30 N5 176.7(14) . . ? C29' C30' N5 176.6(15) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.559 _refine_diff_density_min -0.312 _refine_diff_density_rms 0.058 # Attachment '04183.cif' data_04183 _database_code_depnum_ccdc_archive 'CCDC 615612' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C28 H28 Cl2 Co N4) (C2 H3 N)' _chemical_formula_sum 'C30 H31 Cl2 Co N5' _chemical_formula_weight 591.43 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' Co Co 0.3494 0.9721 '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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.089(3) _cell_length_b 17.124(5) _cell_length_c 16.991(5) _cell_angle_alpha 90.00 _cell_angle_beta 96.459(5) _cell_angle_gamma 90.00 _cell_volume 2916.8(15) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 949 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 27.70 _exptl_crystal_description green _exptl_crystal_colour block _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.347 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1228 _exptl_absorpt_coefficient_mu 0.799 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.817 _exptl_absorpt_correction_T_max 0.928 _exptl_absorpt_process_details ; absorption correction based on 13753 reflections(SADABS);Rint 0.033 before correction and 0.025 after. ; _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 '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 22391 _diffrn_reflns_av_R_equivalents 0.0285 _diffrn_reflns_av_sigmaI/netI 0.0291 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5730 _reflns_number_gt 4801 _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^)+(0.0586P)^2^+0.0331P] 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 constrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5730 _refine_ls_number_parameters 407 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0409 _refine_ls_R_factor_gt 0.0336 _refine_ls_wR_factor_ref 0.0947 _refine_ls_wR_factor_gt 0.0920 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.002 _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 Co1 Co 0.93764(2) 0.543232(14) 0.793045(14) 0.02135(9) Uani 1 1 d . . . Cl1 Cl 0.74467(5) 0.59807(3) 0.82167(3) 0.03763(15) Uani 1 1 d . . . Cl2 Cl 1.05955(5) 0.60918(3) 0.71003(3) 0.03195(13) Uani 1 1 d . . . N1 N 1.05523(16) 0.58412(9) 0.89848(9) 0.0262(4) Uani 1 1 d . . . N2 N 1.01234(15) 0.44338(8) 0.84501(9) 0.0214(3) Uani 1 1 d . . . N3 N 0.84907(15) 0.45154(8) 0.71365(9) 0.0208(3) Uani 1 1 d . . . N4 N 0.66085(16) 0.55126(9) 0.55582(9) 0.0247(4) Uani 1 1 d . . . C1 C 1.0694(2) 0.65829(12) 0.92179(13) 0.0339(5) Uani 1 1 d . . . H1 H 1.0228 0.6977 0.8906 0.041 Uiso 1 1 calc R . . C2 C 1.1496(2) 0.68002(13) 0.98984(13) 0.0370(5) Uani 1 1 d . . . H2 H 1.1582 0.7333 1.0050 0.044 Uiso 1 1 calc R . . C3 C 1.2166(2) 0.62244(13) 1.03493(12) 0.0351(5) Uani 1 1 d . . . H3 H 1.2721 0.6358 1.0819 0.042 Uiso 1 1 calc R . . C4 C 1.2029(2) 0.54560(12) 1.01179(12) 0.0302(5) Uani 1 1 d . . . H4 H 1.2482 0.5053 1.0425 0.036 Uiso 1 1 calc R . . C5 C 1.12132(18) 0.52813(11) 0.94237(11) 0.0247(4) Uani 1 1 d . . . C6 C 1.09948(18) 0.44797(11) 0.91090(11) 0.0241(4) Uani 1 1 d . . . C7 C 1.1606(2) 0.38127(12) 0.94451(12) 0.0316(5) Uani 1 1 d . . . H7 H 1.2214 0.3844 0.9914 0.038 Uiso 1 1 calc R . . C8 C 1.1309(2) 0.31039(12) 0.90822(13) 0.0348(5) Uani 1 1 d . . . H8 H 1.1736 0.2643 0.9294 0.042 Uiso 1 1 calc R . . C9 C 1.0396(2) 0.30582(11) 0.84123(12) 0.0296(4) Uani 1 1 d . . . H9 H 1.0182 0.2570 0.8164 0.035 Uiso 1 1 calc R . . C10 C 0.98029(18) 0.37415(10) 0.81128(11) 0.0221(4) Uani 1 1 d . . . C11 C 0.87771(18) 0.37846(10) 0.74152(11) 0.0219(4) Uani 1 1 d . . . C12 C 0.8131(2) 0.31291(11) 0.70854(12) 0.0282(4) Uani 1 1 d . . . H12 H 0.8355 0.2623 0.7288 0.034 Uiso 1 1 calc R . . C13 C 0.7149(2) 0.32269(11) 0.64543(12) 0.0326(5) Uani 1 1 d . . . H13 H 0.6673 0.2788 0.6228 0.039 Uiso 1 1 calc R . . C14 C 0.6867(2) 0.39635(11) 0.61565(12) 0.0287(4) Uani 1 1 d . . . H14 H 0.6202 0.4038 0.5721 0.034 Uiso 1 1 calc R . . C15 C 0.75741(19) 0.45966(10) 0.65046(11) 0.0226(4) Uani 1 1 d . . . C16 C 0.73675(18) 0.53967(11) 0.61903(11) 0.0235(4) Uani 1 1 d . . . H16 H 0.7806 0.5825 0.6464 0.028 Uiso 1 1 calc R . . C17 C 0.64097(18) 0.62872(11) 0.52620(11) 0.0226(4) Uani 1 1 d . . . C18 C 0.56047(18) 0.68157(11) 0.56257(11) 0.0255(4) Uani 1 1 d . A . C19 C 0.53605(19) 0.75381(12) 0.52637(12) 0.0297(4) Uani 1 1 d . . . H19 H 0.4820 0.7907 0.5497 0.036 Uiso 1 1 calc R . . C20 C 0.58836(19) 0.77319(12) 0.45737(12) 0.0303(4) Uani 1 1 d . . . H20 H 0.5694 0.8227 0.4336 0.036 Uiso 1 1 calc R . . C21 C 0.66806(19) 0.72081(12) 0.42284(12) 0.0304(5) Uani 1 1 d . . . H21 H 0.7045 0.7349 0.3757 0.036 Uiso 1 1 calc R . . C22 C 0.69556(19) 0.64807(11) 0.45599(11) 0.0269(4) Uani 1 1 d . . . C23 C 0.4964(2) 0.65937(13) 0.63613(12) 0.0353(5) Uani 1 1 d . . . H23 H 0.5591 0.6229 0.6673 0.029(5) Uiso 1 1 d R A . C24 C 0.5241(9) 0.7316(5) 0.6978(4) 0.075(2) Uani 0.50 1 d P A 1 H24A H 0.4706 0.7768 0.6782 0.112 Uiso 0.50 1 calc PR A 1 H24B H 0.6189 0.7454 0.7026 0.112 Uiso 0.50 1 calc PR A 1 H24C H 0.4995 0.7162 0.7497 0.112 Uiso 0.50 1 calc PR A 1 C24' C 0.4423(6) 0.7217(4) 0.6833(4) 0.0487(16) Uani 0.50 1 d P A 2 H24D H 0.3633 0.7446 0.6531 0.073 Uiso 0.50 1 calc PR A 2 H24E H 0.5101 0.7623 0.6952 0.073 Uiso 0.50 1 calc PR A 2 H24F H 0.4176 0.6997 0.7329 0.073 Uiso 0.50 1 calc PR A 2 C25 C 0.3557(7) 0.6480(6) 0.6171(5) 0.092(3) Uani 0.50 1 d P A 1 H25A H 0.3141 0.6409 0.6661 0.138 Uiso 0.50 1 calc PR A 1 H25B H 0.3399 0.6015 0.5838 0.138 Uiso 0.50 1 calc PR A 1 H25C H 0.3169 0.6937 0.5886 0.138 Uiso 0.50 1 calc PR A 1 C25' C 0.3771(7) 0.5989(3) 0.6096(4) 0.0433(15) Uani 0.50 1 d P A 2 H25D H 0.3364 0.5817 0.6563 0.065 Uiso 0.50 1 calc PR A 2 H25E H 0.4128 0.5536 0.5837 0.065 Uiso 0.50 1 calc PR A 2 H25F H 0.3096 0.6248 0.5724 0.065 Uiso 0.50 1 calc PR A 2 C26 C 0.7875(2) 0.59090(13) 0.42036(13) 0.0384(5) Uani 1 1 d . . . H26 H 0.7626 0.5370 0.4360 0.046 Uiso 1 1 calc R . . C27 C 0.7742(4) 0.59415(17) 0.33003(15) 0.0690(9) Uani 1 1 d . . . H27A H 0.6802 0.5881 0.3091 0.103 Uiso 1 1 calc R . . H27B H 0.8266 0.5519 0.3100 0.103 Uiso 1 1 calc R . . H27C H 0.8073 0.6445 0.3131 0.103 Uiso 1 1 calc R . . C28 C 0.9329(3) 0.60526(17) 0.45447(18) 0.0603(8) Uani 1 1 d . . . H28A H 0.9600 0.6578 0.4399 0.091 Uiso 1 1 calc R . . H28B H 0.9906 0.5665 0.4330 0.091 Uiso 1 1 calc R . . H28C H 0.9409 0.6007 0.5123 0.091 Uiso 1 1 calc R . . N5 N 0.3957(3) 0.5558(2) 0.83205(19) 0.0900(9) Uani 1 1 d . . . C29 C 0.4778(7) 0.4573(7) 0.9424(6) 0.070(3) Uani 0.40 1 d P B 1 H29A H 0.5507 0.4812 0.9772 0.106 Uiso 0.40 1 calc PR B 1 H29B H 0.5099 0.4097 0.9188 0.106 Uiso 0.40 1 calc PR B 1 H29C H 0.4044 0.4442 0.9733 0.106 Uiso 0.40 1 calc PR B 1 C30 C 0.443(2) 0.4982(15) 0.8956(9) 0.055(5) Uani 0.40 1 d P B 1 C29A C 0.4766(11) 0.4329(7) 0.8816(11) 0.108(6) Uani 0.40 1 d P B 2 H29D H 0.4024 0.3956 0.8771 0.162 Uiso 0.40 1 calc PR B 2 H29E H 0.5158 0.4361 0.9370 0.162 Uiso 0.40 1 calc PR B 2 H29F H 0.5446 0.4154 0.8486 0.162 Uiso 0.40 1 calc PR B 2 C29B C 0.5502(18) 0.4219(10) 0.8166(13) 0.076(5) Uani 0.20 1 d P B 3 H29G H 0.5290 0.4058 0.7613 0.115 Uiso 0.20 1 calc PR B 3 H29H H 0.5334 0.3783 0.8515 0.115 Uiso 0.20 1 calc PR B 3 H29I H 0.6444 0.4370 0.8260 0.115 Uiso 0.20 1 calc PR B 3 C30A C 0.440(2) 0.4902(12) 0.8618(10) 0.055(5) Uani 0.40 1 d P B 2 C30B C 0.487(2) 0.4720(11) 0.8291(16) 0.053(6) Uani 0.20 1 d P B 3 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 Co1 0.02213(15) 0.01780(15) 0.02371(15) 0.00076(10) 0.00071(10) 0.00113(9) Cl1 0.0302(3) 0.0480(3) 0.0344(3) -0.0083(2) 0.0023(2) 0.0128(2) Cl2 0.0324(3) 0.0271(3) 0.0372(3) 0.0057(2) 0.0075(2) -0.00318(19) N1 0.0265(9) 0.0242(9) 0.0274(9) -0.0004(7) 0.0009(7) -0.0024(7) N2 0.0216(8) 0.0199(8) 0.0225(8) 0.0017(6) 0.0025(6) -0.0015(6) N3 0.0206(8) 0.0203(8) 0.0217(8) 0.0009(6) 0.0039(6) 0.0001(6) N4 0.0261(9) 0.0243(9) 0.0234(9) 0.0018(6) 0.0021(7) 0.0003(7) C1 0.0392(12) 0.0257(11) 0.0358(12) -0.0024(9) 0.0001(9) -0.0041(9) C2 0.0413(13) 0.0311(12) 0.0378(13) -0.0069(9) 0.0012(10) -0.0109(10) C3 0.0315(11) 0.0421(13) 0.0308(11) -0.0059(10) -0.0006(9) -0.0142(10) C4 0.0256(10) 0.0373(12) 0.0268(11) 0.0032(9) -0.0011(8) -0.0049(8) C5 0.0202(9) 0.0276(10) 0.0264(10) 0.0000(8) 0.0027(8) -0.0043(8) C6 0.0201(9) 0.0263(10) 0.0256(10) 0.0030(8) 0.0019(8) -0.0010(7) C7 0.0294(11) 0.0301(11) 0.0332(11) 0.0049(9) -0.0055(9) 0.0018(8) C8 0.0351(12) 0.0274(11) 0.0400(12) 0.0067(9) -0.0045(9) 0.0054(9) C9 0.0321(11) 0.0218(10) 0.0340(11) -0.0008(8) 0.0001(9) 0.0017(8) C10 0.0224(9) 0.0205(9) 0.0237(10) 0.0017(7) 0.0043(7) 0.0004(7) C11 0.0225(9) 0.0203(9) 0.0234(10) 0.0004(7) 0.0049(8) 0.0006(7) C12 0.0338(11) 0.0194(10) 0.0308(11) 0.0023(8) 0.0010(9) -0.0008(8) C13 0.0369(12) 0.0242(11) 0.0347(12) -0.0042(9) -0.0045(9) -0.0065(9) C14 0.0293(11) 0.0287(11) 0.0269(10) -0.0020(8) -0.0018(8) -0.0025(8) C15 0.0236(10) 0.0229(10) 0.0217(9) 0.0007(7) 0.0040(7) 0.0019(7) C16 0.0221(10) 0.0239(10) 0.0244(10) -0.0022(8) 0.0027(8) 0.0001(7) C17 0.0220(9) 0.0230(10) 0.0214(9) -0.0003(7) -0.0032(7) -0.0010(7) C18 0.0214(10) 0.0296(11) 0.0244(10) -0.0001(8) -0.0025(8) -0.0001(8) C19 0.0256(10) 0.0286(11) 0.0333(11) -0.0003(8) -0.0033(8) 0.0040(8) C20 0.0298(11) 0.0254(10) 0.0328(11) 0.0085(9) -0.0083(8) -0.0036(8) C21 0.0336(11) 0.0322(11) 0.0247(10) 0.0059(9) 0.0001(8) -0.0069(9) C22 0.0285(10) 0.0273(10) 0.0243(10) -0.0008(8) 0.0008(8) -0.0044(8) C23 0.0366(12) 0.0441(13) 0.0262(11) 0.0070(9) 0.0079(9) 0.0137(10) C24 0.141(8) 0.057(4) 0.032(4) -0.001(3) 0.037(5) 0.005(6) C24' 0.066(4) 0.039(3) 0.045(4) -0.003(3) 0.022(3) 0.014(3) C25 0.041(4) 0.173(9) 0.063(5) 0.063(7) 0.014(3) -0.015(6) C25' 0.039(3) 0.055(4) 0.038(3) 0.004(3) 0.013(2) -0.009(3) C26 0.0490(14) 0.0344(12) 0.0349(12) 0.0025(9) 0.0177(10) 0.0028(10) C27 0.105(2) 0.0674(19) 0.0388(15) -0.0042(13) 0.0258(16) 0.0221(17) C28 0.0442(15) 0.0621(18) 0.079(2) 0.0070(15) 0.0258(14) 0.0118(13) N5 0.0698(19) 0.115(3) 0.083(2) 0.0193(19) -0.0006(16) -0.0155(18) C29 0.017(3) 0.080(7) 0.114(8) 0.067(7) 0.005(4) 0.006(4) C30 0.026(5) 0.064(8) 0.078(12) 0.002(10) 0.012(8) -0.013(5) C29A 0.067(7) 0.059(8) 0.183(15) 0.072(10) -0.055(10) -0.021(6) C29B 0.071(12) 0.035(9) 0.111(16) 0.000(9) -0.045(11) -0.010(9) C30A 0.034(7) 0.043(10) 0.084(16) 0.015(11) -0.012(10) -0.008(6) C30B 0.039(11) 0.029(10) 0.082(17) 0.004(9) -0.033(9) -0.001(8) _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 Co1 N2 2.0302(15) . ? Co1 N1 2.1514(16) . ? Co1 N3 2.1937(16) . ? Co1 Cl1 2.2630(7) . ? Co1 Cl2 2.2733(7) . ? N1 C1 1.333(2) . ? N1 C5 1.345(2) . ? N2 C10 1.340(2) . ? N2 C6 1.346(2) . ? N3 C15 1.343(2) . ? N3 C11 1.358(2) . ? N4 C16 1.263(2) . ? N4 C17 1.425(2) . ? C1 C2 1.386(3) . ? C2 C3 1.378(3) . ? C3 C4 1.376(3) . ? C4 C5 1.393(3) . ? C5 C6 1.481(3) . ? C6 C7 1.390(3) . ? C7 C8 1.379(3) . ? C8 C9 1.384(3) . ? C9 C10 1.385(3) . ? C10 C11 1.485(3) . ? C11 C12 1.385(3) . ? C12 C13 1.386(3) . ? C13 C14 1.377(3) . ? C14 C15 1.393(3) . ? C15 C16 1.477(3) . ? C17 C18 1.405(3) . ? C17 C22 1.409(3) . ? C18 C19 1.391(3) . ? C18 C23 1.519(3) . ? C19 C20 1.379(3) . ? C20 C21 1.379(3) . ? C21 C22 1.382(3) . ? C22 C26 1.520(3) . ? C23 C25 1.433(8) . ? C23 C24' 1.476(7) . ? C23 C25' 1.612(7) . ? C23 C24 1.624(8) . ? C26 C27 1.526(3) . ? C26 C28 1.535(4) . ? N5 C30A 1.29(2) . ? N5 C30 1.50(2) . ? N5 C30B 1.708(19) . ? C29 C30 1.09(3) . ? C29A C30A 1.09(3) . ? C29B C30B 1.10(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 N2 Co1 N1 76.64(6) . . ? N2 Co1 N3 76.71(6) . . ? N1 Co1 N3 153.29(6) . . ? N2 Co1 Cl1 122.84(5) . . ? N1 Co1 Cl1 95.34(5) . . ? N3 Co1 Cl1 97.38(4) . . ? N2 Co1 Cl2 119.20(5) . . ? N1 Co1 Cl2 93.95(5) . . ? N3 Co1 Cl2 100.68(5) . . ? Cl1 Co1 Cl2 117.76(3) . . ? C1 N1 C5 118.98(18) . . ? C1 N1 Co1 126.02(14) . . ? C5 N1 Co1 114.98(12) . . ? C10 N2 C6 120.73(15) . . ? C10 N2 Co1 119.94(12) . . ? C6 N2 Co1 119.23(12) . . ? C15 N3 C11 118.34(15) . . ? C15 N3 Co1 127.85(12) . . ? C11 N3 Co1 112.91(12) . . ? C16 N4 C17 119.64(16) . . ? N1 C1 C2 122.5(2) . . ? C3 C2 C1 118.4(2) . . ? C4 C3 C2 119.89(19) . . ? C3 C4 C5 118.56(19) . . ? N1 C5 C4 121.70(18) . . ? N1 C5 C6 114.61(16) . . ? C4 C5 C6 123.69(17) . . ? N2 C6 C7 120.79(17) . . ? N2 C6 C5 114.29(16) . . ? C7 C6 C5 124.92(18) . . ? C8 C7 C6 118.41(18) . . ? C7 C8 C9 120.57(19) . . ? C8 C9 C10 118.34(18) . . ? N2 C10 C9 121.10(17) . . ? N2 C10 C11 114.21(15) . . ? C9 C10 C11 124.68(17) . . ? N3 C11 C12 122.28(17) . . ? N3 C11 C10 115.22(15) . . ? C12 C11 C10 122.47(16) . . ? C11 C12 C13 118.58(17) . . ? C14 C13 C12 119.69(18) . . ? C13 C14 C15 118.84(18) . . ? N3 C15 C14 122.19(17) . . ? N3 C15 C16 116.21(16) . . ? C14 C15 C16 121.60(17) . . ? N4 C16 C15 120.06(17) . . ? C18 C17 C22 121.43(17) . . ? C18 C17 N4 120.65(16) . . ? C22 C17 N4 117.72(16) . . ? C19 C18 C17 117.44(18) . . ? C19 C18 C23 121.05(18) . . ? C17 C18 C23 121.43(17) . . ? C20 C19 C18 121.61(19) . . ? C21 C20 C19 120.16(18) . . ? C20 C21 C22 120.84(19) . . ? C21 C22 C17 118.52(18) . . ? C21 C22 C26 121.43(18) . . ? C17 C22 C26 119.99(17) . . ? C25 C23 C24' 78.7(5) . . ? C25 C23 C18 110.6(3) . . ? C24' C23 C18 118.9(3) . . ? C25 C23 C25' 32.9(4) . . ? C24' C23 C25' 107.9(4) . . ? C18 C23 C25' 107.7(3) . . ? C25 C23 C24 110.1(6) . . ? C24' C23 C24 31.4(3) . . ? C18 C23 C24 106.4(3) . . ? C25' C23 C24 137.6(4) . . ? C22 C26 C27 112.86(19) . . ? C22 C26 C28 110.25(19) . . ? C27 C26 C28 110.2(2) . . ? C30A N5 C30 22.9(11) . . ? C30A N5 C30B 28.0(9) . . ? C30 N5 C30B 48.9(13) . . ? C29 C30 N5 179(2) . . ? C29A C30A N5 175(2) . . ? C29B C30B N5 170(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.446 _refine_diff_density_min -0.269 _refine_diff_density_rms 0.057 # Attachment '06003.cif' data_06003 _database_code_depnum_ccdc_archive 'CCDC 615613' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H30 Cl2 N4 Zn' _chemical_formula_weight 570.84 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 10.2739(19) _cell_length_b 10.5553(19) _cell_length_c 12.623(2) _cell_angle_alpha 94.301(3) _cell_angle_beta 101.922(3) _cell_angle_gamma 96.325(3) _cell_volume 1324.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 789 _cell_measurement_theta_min 2.335 _cell_measurement_theta_max 24.184 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.431 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 592 _exptl_absorpt_coefficient_mu 1.155 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.595 _exptl_absorpt_correction_T_max 0.862 _exptl_absorpt_process_details ; absorption correction based on 5541 reflections(SADABS);Rint 0.0430 before correction and 0.0320 after. ; _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 '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 10435 _diffrn_reflns_av_R_equivalents 0.0362 _diffrn_reflns_av_sigmaI/netI 0.0577 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5134 _reflns_number_gt 4106 _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^)+(0.0499P)^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 constrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5134 _refine_ls_number_parameters 330 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0567 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.1055 _refine_ls_wR_factor_gt 0.1004 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _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 N1 N 0.7519(3) 0.9442(2) 0.5475(2) 0.0347(6) Uani 1 1 d . . . N2 N 0.5462(2) 0.7685(2) 0.52198(18) 0.0297(5) Uani 1 1 d . . . N3 N 0.5701(2) 0.6272(2) 0.69226(18) 0.0272(5) Uani 1 1 d . . . N4 N 0.6639(2) 0.5844(2) 0.96969(19) 0.0337(6) Uani 1 1 d . . . Cl1 Cl 0.87651(7) 0.68564(7) 0.60953(6) 0.03588(19) Uani 1 1 d . . . Cl2 Cl 0.71219(9) 0.92535(7) 0.79725(6) 0.0467(2) Uani 1 1 d . . . Zn1 Zn 0.71122(3) 0.79279(3) 0.65066(3) 0.03105(12) Uani 1 1 d . . . C1 C 0.8610(3) 1.0297(3) 0.5678(3) 0.0412(8) Uani 1 1 d . . . H1 H 0.9278 1.0260 0.6315 0.049 Uiso 1 1 calc R . . C2 C 0.8819(4) 1.1242(3) 0.5002(3) 0.0454(8) Uani 1 1 d . . . H2 H 0.9614 1.1837 0.5165 0.054 Uiso 1 1 calc R . . C3 C 0.7834(4) 1.1284(3) 0.4089(3) 0.0486(9) Uani 1 1 d . . . H3 H 0.7941 1.1922 0.3610 0.058 Uiso 1 1 calc R . . C4 C 0.6701(4) 1.0411(3) 0.3867(3) 0.0431(8) Uani 1 1 d . . . H4 H 0.6016 1.0439 0.3238 0.052 Uiso 1 1 calc R . . C5 C 0.6567(3) 0.9479(3) 0.4579(2) 0.0344(7) Uani 1 1 d . . . C6 C 0.5418(3) 0.8464(3) 0.4423(2) 0.0326(7) Uani 1 1 d . . . C7 C 0.4347(3) 0.8302(3) 0.3531(2) 0.0413(8) Uani 1 1 d . . . H7 H 0.4304 0.8872 0.2980 0.050 Uiso 1 1 calc R . . C8 C 0.3346(3) 0.7294(3) 0.3462(2) 0.0426(8) Uani 1 1 d . . . H8 H 0.2612 0.7159 0.2852 0.051 Uiso 1 1 calc R . . C9 C 0.3402(3) 0.6486(3) 0.4269(2) 0.0375(7) Uani 1 1 d . . . H9 H 0.2720 0.5786 0.4220 0.045 Uiso 1 1 calc R . . C10 C 0.4488(3) 0.6717(3) 0.5164(2) 0.0306(7) Uani 1 1 d . . . C11 C 0.4606(3) 0.5951(3) 0.6109(2) 0.0301(6) Uani 1 1 d . . . C12 C 0.3614(3) 0.4962(3) 0.6145(2) 0.0358(7) Uani 1 1 d . . . H12 H 0.2868 0.4742 0.5550 0.043 Uiso 1 1 calc R . . C13 C 0.3725(3) 0.4307(3) 0.7049(3) 0.0385(7) Uani 1 1 d . . . H13 H 0.3068 0.3612 0.7083 0.046 Uiso 1 1 calc R . . C14 C 0.4795(3) 0.4668(3) 0.7906(2) 0.0345(7) Uani 1 1 d . . . H14 H 0.4867 0.4247 0.8551 0.041 Uiso 1 1 calc R . . C15 C 0.5769(3) 0.5650(3) 0.7826(2) 0.0298(6) Uani 1 1 d . . . C16 C 0.6946(3) 0.5955(3) 0.8772(2) 0.0311(7) Uani 1 1 d . . . C17 C 0.8309(3) 0.6186(3) 0.8584(2) 0.0402(8) Uani 1 1 d . . . H17A H 0.8521 0.7093 0.8488 0.060 Uiso 1 1 calc R . . H17B H 0.8368 0.5658 0.7927 0.060 Uiso 1 1 calc R . . H17C H 0.8949 0.5961 0.9209 0.060 Uiso 1 1 calc R . . C18 C 0.7675(3) 0.5924(3) 1.0661(2) 0.0353(7) Uani 1 1 d . . . C19 C 0.8321(3) 0.7115(3) 1.1183(3) 0.0398(8) Uani 1 1 d . . . C20 C 0.9276(3) 0.7116(3) 1.2143(3) 0.0466(8) Uani 1 1 d . . . H20 H 0.9743 0.7908 1.2506 0.056 Uiso 1 1 calc R . . C21 C 0.9559(3) 0.5990(3) 1.2577(3) 0.0457(8) Uani 1 1 d . . . H21 H 1.0226 0.6015 1.3227 0.055 Uiso 1 1 calc R . . C22 C 0.8879(3) 0.4827(3) 1.2073(3) 0.0429(8) Uani 1 1 d . . . H22 H 0.9072 0.4060 1.2387 0.051 Uiso 1 1 calc R . . C23 C 0.7924(3) 0.4768(3) 1.1119(2) 0.0383(7) Uani 1 1 d . . . C24 C 0.7135(4) 0.3501(3) 1.0568(3) 0.0456(9) Uani 1 1 d . . . H24 H 0.6232 0.3694 1.0194 0.055 Uiso 1 1 calc R . . C25 C 0.7773(5) 0.2910(3) 0.9687(3) 0.0613(11) Uani 1 1 d . . . H25A H 0.7856 0.3522 0.9150 0.092 Uiso 1 1 calc R . . H25B H 0.7206 0.2125 0.9325 0.092 Uiso 1 1 calc R . . H25C H 0.8664 0.2705 1.0020 0.092 Uiso 1 1 calc R . . C26 C 0.6898(4) 0.2530(3) 1.1360(3) 0.0558(10) Uani 1 1 d . . . H26A H 0.6201 0.1838 1.0989 0.084 Uiso 1 1 calc R . . H26B H 0.6607 0.2952 1.1974 0.084 Uiso 1 1 calc R . . H26C H 0.7732 0.2174 1.1629 0.084 Uiso 1 1 calc R . . C27 C 0.7926(4) 0.8354(3) 1.0743(3) 0.0471(9) Uani 1 1 d . . . H27 H 0.7790 0.8221 0.9933 0.057 Uiso 1 1 calc R . . C28 C 0.6586(4) 0.8611(4) 1.0998(4) 0.0692(12) Uani 1 1 d . . . H28A H 0.6672 0.8715 1.1789 0.104 Uiso 1 1 calc R . . H28B H 0.5899 0.7889 1.0678 0.104 Uiso 1 1 calc R . . H28C H 0.6326 0.9396 1.0692 0.104 Uiso 1 1 calc R . . C29 C 0.8963(4) 0.9509(4) 1.1127(3) 0.0692(12) Uani 1 1 d . . . H29A H 0.8995 0.9773 1.1894 0.104 Uiso 1 1 calc R . . H29B H 0.8724 1.0212 1.0690 0.104 Uiso 1 1 calc R . . H29C H 0.9843 0.9294 1.1046 0.104 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 N1 0.0421(15) 0.0317(14) 0.0320(14) 0.0071(11) 0.0084(12) 0.0081(12) N2 0.0343(14) 0.0342(14) 0.0220(13) 0.0054(10) 0.0044(10) 0.0119(11) N3 0.0271(13) 0.0299(13) 0.0243(13) 0.0025(10) 0.0028(10) 0.0073(10) N4 0.0370(15) 0.0372(14) 0.0262(14) 0.0060(11) 0.0033(11) 0.0060(11) Cl1 0.0330(4) 0.0393(4) 0.0373(4) 0.0123(3) 0.0077(3) 0.0074(3) Cl2 0.0743(6) 0.0337(4) 0.0301(4) 0.0033(3) 0.0044(4) 0.0111(4) Zn1 0.0343(2) 0.0313(2) 0.0266(2) 0.00686(14) 0.00193(14) 0.00615(15) C1 0.049(2) 0.0360(18) 0.0413(19) 0.0093(15) 0.0112(16) 0.0104(15) C2 0.059(2) 0.0325(18) 0.050(2) 0.0090(16) 0.0238(18) 0.0067(16) C3 0.076(3) 0.0377(19) 0.040(2) 0.0134(16) 0.0240(19) 0.0119(18) C4 0.065(2) 0.0409(19) 0.0272(17) 0.0095(14) 0.0124(16) 0.0153(17) C5 0.0491(19) 0.0361(17) 0.0234(16) 0.0057(13) 0.0120(14) 0.0187(15) C6 0.0401(18) 0.0349(17) 0.0250(16) 0.0034(13) 0.0067(13) 0.0152(14) C7 0.051(2) 0.053(2) 0.0253(17) 0.0124(15) 0.0076(15) 0.0227(17) C8 0.0397(19) 0.059(2) 0.0274(17) 0.0032(15) -0.0026(14) 0.0161(16) C9 0.0347(17) 0.0486(19) 0.0283(17) 0.0020(14) 0.0028(13) 0.0095(14) C10 0.0300(16) 0.0365(17) 0.0257(15) 0.0014(13) 0.0027(12) 0.0130(13) C11 0.0296(16) 0.0343(16) 0.0274(16) 0.0018(13) 0.0054(12) 0.0112(13) C12 0.0314(17) 0.0431(18) 0.0301(17) -0.0009(14) 0.0040(13) 0.0008(14) C13 0.0363(18) 0.0388(18) 0.0399(19) 0.0015(15) 0.0110(15) -0.0008(14) C14 0.0394(18) 0.0362(17) 0.0299(16) 0.0083(14) 0.0097(14) 0.0052(14) C15 0.0337(16) 0.0284(15) 0.0294(16) 0.0039(12) 0.0091(13) 0.0084(13) C16 0.0414(18) 0.0251(15) 0.0280(16) 0.0094(12) 0.0049(13) 0.0097(13) C17 0.0425(19) 0.047(2) 0.0313(17) 0.0096(15) 0.0046(14) 0.0097(15) C18 0.0359(17) 0.0421(18) 0.0303(17) 0.0093(14) 0.0081(13) 0.0095(14) C19 0.0405(19) 0.0429(19) 0.0351(18) 0.0061(15) 0.0069(15) 0.0033(15) C20 0.044(2) 0.054(2) 0.0378(19) 0.0023(16) 0.0027(16) 0.0024(17) C21 0.0385(19) 0.058(2) 0.0388(19) 0.0075(17) 0.0013(15) 0.0107(17) C22 0.0405(19) 0.052(2) 0.0386(19) 0.0133(16) 0.0049(15) 0.0170(16) C23 0.0394(18) 0.0439(19) 0.0339(18) 0.0064(15) 0.0097(14) 0.0103(15) C24 0.050(2) 0.0416(19) 0.042(2) 0.0088(16) 0.0000(16) 0.0082(16) C25 0.098(3) 0.048(2) 0.041(2) 0.0039(17) 0.018(2) 0.015(2) C26 0.078(3) 0.040(2) 0.052(2) 0.0120(17) 0.015(2) 0.0143(19) C27 0.062(2) 0.0380(19) 0.039(2) 0.0070(15) 0.0043(17) 0.0066(17) C28 0.066(3) 0.044(2) 0.101(4) 0.014(2) 0.020(2) 0.015(2) C29 0.071(3) 0.048(2) 0.080(3) 0.017(2) -0.001(2) -0.005(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 N1 C1 1.327(4) . ? N1 C5 1.341(4) . ? N1 Zn1 2.193(2) . ? N2 C10 1.336(4) . ? N2 C6 1.343(3) . ? N2 Zn1 2.069(2) . ? N3 C11 1.350(3) . ? N3 C15 1.351(3) . ? N3 Zn1 2.308(2) . ? N4 C16 1.281(4) . ? N4 C18 1.432(4) . ? Cl1 Zn1 2.2654(9) . ? Cl2 Zn1 2.2322(9) . ? C1 C2 1.387(4) . ? C1 H1 0.9500 . ? C2 C3 1.375(5) . ? C2 H2 0.9500 . ? C3 C4 1.369(5) . ? C3 H3 0.9500 . ? C4 C5 1.395(4) . ? C4 H4 0.9500 . ? C5 C6 1.474(4) . ? C6 C7 1.388(4) . ? C7 C8 1.381(5) . ? C7 H7 0.9500 . ? C8 C9 1.373(4) . ? C8 H8 0.9500 . ? C9 C10 1.400(4) . ? C9 H9 0.9500 . ? C10 C11 1.482(4) . ? C11 C12 1.386(4) . ? C12 C13 1.370(4) . ? C12 H12 0.9500 . ? C13 C14 1.370(4) . ? C13 H13 0.9500 . ? C14 C15 1.384(4) . ? C14 H14 0.9500 . ? C15 C16 1.501(4) . ? C16 C17 1.465(4) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.402(4) . ? C18 C23 1.415(4) . ? C19 C20 1.392(4) . ? C19 C27 1.522(4) . ? C20 C21 1.380(5) . ? C20 H20 0.9500 . ? C21 C22 1.382(4) . ? C21 H21 0.9500 . ? C22 C23 1.380(4) . ? C22 H22 0.9500 . ? C23 C24 1.523(4) . ? C24 C26 1.519(4) . ? C24 C25 1.530(5) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C29 1.506(5) . ? C27 C28 1.525(5) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? 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 N1 C5 119.2(3) . . ? C1 N1 Zn1 125.2(2) . . ? C5 N1 Zn1 115.7(2) . . ? C10 N2 C6 120.9(2) . . ? C10 N2 Zn1 119.63(18) . . ? C6 N2 Zn1 119.4(2) . . ? C11 N3 C15 117.7(2) . . ? C11 N3 Zn1 110.82(18) . . ? C15 N3 Zn1 131.43(18) . . ? C16 N4 C18 120.0(3) . . ? N2 Zn1 N1 75.18(9) . . ? N2 Zn1 Cl2 119.32(7) . . ? N1 Zn1 Cl2 95.59(7) . . ? N2 Zn1 Cl1 110.85(7) . . ? N1 Zn1 Cl1 92.49(7) . . ? Cl2 Zn1 Cl1 129.60(3) . . ? N2 Zn1 N3 75.69(9) . . ? N1 Zn1 N3 150.70(9) . . ? Cl2 Zn1 N3 95.82(6) . . ? Cl1 Zn1 N3 100.75(6) . . ? N1 C1 C2 123.1(3) . . ? N1 C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? C3 C2 C1 117.6(3) . . ? C3 C2 H2 121.2 . . ? C1 C2 H2 121.2 . . ? C4 C3 C2 120.3(3) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 118.9(3) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? N1 C5 C4 121.0(3) . . ? N1 C5 C6 114.5(3) . . ? C4 C5 C6 124.5(3) . . ? N2 C6 C7 120.9(3) . . ? N2 C6 C5 115.2(3) . . ? C7 C6 C5 123.8(3) . . ? C8 C7 C6 118.5(3) . . ? C8 C7 H7 120.8 . . ? C6 C7 H7 120.8 . . ? C9 C8 C7 120.6(3) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C8 C9 C10 118.5(3) . . ? C8 C9 H9 120.8 . . ? C10 C9 H9 120.8 . . ? N2 C10 C9 120.7(3) . . ? N2 C10 C11 116.4(2) . . ? C9 C10 C11 122.9(3) . . ? N3 C11 C12 122.4(3) . . ? N3 C11 C10 117.1(3) . . ? C12 C11 C10 120.5(3) . . ? C13 C12 C11 119.1(3) . . ? C13 C12 H12 120.5 . . ? C11 C12 H12 120.5 . . ? C14 C13 C12 119.2(3) . . ? C14 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? C13 C14 C15 119.6(3) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? N3 C15 C14 122.0(3) . . ? N3 C15 C16 121.1(2) . . ? C14 C15 C16 116.8(3) . . ? N4 C16 C17 125.8(3) . . ? N4 C16 C15 113.6(3) . . ? C17 C16 C15 120.1(3) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C23 121.5(3) . . ? C19 C18 N4 120.9(3) . . ? C23 C18 N4 117.3(3) . . ? C20 C19 C18 117.5(3) . . ? C20 C19 C27 121.8(3) . . ? C18 C19 C27 120.7(3) . . ? C21 C20 C19 121.4(3) . . ? C21 C20 H20 119.3 . . ? C19 C20 H20 119.3 . . ? C20 C21 C22 120.4(3) . . ? C20 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? C23 C22 C21 120.7(3) . . ? C23 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? C22 C23 C18 118.4(3) . . ? C22 C23 C24 121.6(3) . . ? C18 C23 C24 120.1(3) . . ? C26 C24 C23 113.6(3) . . ? C26 C24 C25 110.3(3) . . ? C23 C24 C25 112.2(3) . . ? C26 C24 H24 106.8 . . ? C23 C24 H24 106.8 . . ? C25 C24 H24 106.8 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C29 C27 C19 114.8(3) . . ? C29 C27 C28 110.3(3) . . ? C19 C27 C28 110.0(3) . . ? C29 C27 H27 107.1 . . ? C19 C27 H27 107.1 . . ? C28 C27 H27 107.1 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C10 N2 Zn1 N1 177.8(2) . . . . ? C6 N2 Zn1 N1 1.2(2) . . . . ? C10 N2 Zn1 Cl2 -94.0(2) . . . . ? C6 N2 Zn1 Cl2 89.3(2) . . . . ? C10 N2 Zn1 Cl1 90.9(2) . . . . ? C6 N2 Zn1 Cl1 -85.8(2) . . . . ? C10 N2 Zn1 N3 -5.4(2) . . . . ? C6 N2 Zn1 N3 178.0(2) . . . . ? C1 N1 Zn1 N2 -179.8(3) . . . . ? C5 N1 Zn1 N2 0.4(2) . . . . ? C1 N1 Zn1 Cl2 61.3(2) . . . . ? C5 N1 Zn1 Cl2 -118.5(2) . . . . ? C1 N1 Zn1 Cl1 -68.9(2) . . . . ? C5 N1 Zn1 Cl1 111.3(2) . . . . ? C1 N1 Zn1 N3 173.8(2) . . . . ? C5 N1 Zn1 N3 -6.0(3) . . . . ? C11 N3 Zn1 N2 4.01(18) . . . . ? C15 N3 Zn1 N2 -172.7(3) . . . . ? C11 N3 Zn1 N1 10.4(3) . . . . ? C15 N3 Zn1 N1 -166.4(2) . . . . ? C11 N3 Zn1 Cl2 122.82(17) . . . . ? C15 N3 Zn1 Cl2 -53.9(2) . . . . ? C11 N3 Zn1 Cl1 -104.99(17) . . . . ? C15 N3 Zn1 Cl1 78.3(2) . . . . ? C5 N1 C1 C2 0.1(5) . . . . ? Zn1 N1 C1 C2 -179.7(2) . . . . ? N1 C1 C2 C3 0.5(5) . . . . ? C1 C2 C3 C4 -0.4(5) . . . . ? C2 C3 C4 C5 -0.2(5) . . . . ? C1 N1 C5 C4 -0.8(4) . . . . ? Zn1 N1 C5 C4 179.0(2) . . . . ? C1 N1 C5 C6 178.5(3) . . . . ? Zn1 N1 C5 C6 -1.7(3) . . . . ? C3 C4 C5 N1 0.9(5) . . . . ? C3 C4 C5 C6 -178.4(3) . . . . ? C10 N2 C6 C7 1.3(4) . . . . ? Zn1 N2 C6 C7 177.9(2) . . . . ? C10 N2 C6 C5 -179.1(2) . . . . ? Zn1 N2 C6 C5 -2.5(3) . . . . ? N1 C5 C6 N2 2.7(4) . . . . ? C4 C5 C6 N2 -178.0(3) . . . . ? N1 C5 C6 C7 -177.7(3) . . . . ? C4 C5 C6 C7 1.5(5) . . . . ? N2 C6 C7 C8 -2.1(4) . . . . ? C5 C6 C7 C8 178.3(3) . . . . ? C6 C7 C8 C9 1.1(5) . . . . ? C7 C8 C9 C10 0.7(5) . . . . ? C6 N2 C10 C9 0.5(4) . . . . ? Zn1 N2 C10 C9 -176.1(2) . . . . ? C6 N2 C10 C11 -177.5(2) . . . . ? Zn1 N2 C10 C11 5.9(3) . . . . ? C8 C9 C10 N2 -1.5(4) . . . . ? C8 C9 C10 C11 176.4(3) . . . . ? C15 N3 C11 C12 -4.2(4) . . . . ? Zn1 N3 C11 C12 178.5(2) . . . . ? C15 N3 C11 C10 174.8(2) . . . . ? Zn1 N3 C11 C10 -2.4(3) . . . . ? N2 C10 C11 N3 -1.8(4) . . . . ? C9 C10 C11 N3 -179.8(3) . . . . ? N2 C10 C11 C12 177.2(3) . . . . ? C9 C10 C11 C12 -0.7(4) . . . . ? N3 C11 C12 C13 1.8(4) . . . . ? C10 C11 C12 C13 -177.2(3) . . . . ? C11 C12 C13 C14 1.7(5) . . . . ? C12 C13 C14 C15 -2.6(5) . . . . ? C11 N3 C15 C14 3.3(4) . . . . ? Zn1 N3 C15 C14 179.9(2) . . . . ? C11 N3 C15 C16 -179.6(2) . . . . ? Zn1 N3 C15 C16 -3.0(4) . . . . ? C13 C14 C15 N3 0.1(4) . . . . ? C13 C14 C15 C16 -177.2(3) . . . . ? C18 N4 C16 C17 -1.1(5) . . . . ? C18 N4 C16 C15 171.1(2) . . . . ? N3 C15 C16 N4 146.3(3) . . . . ? C14 C15 C16 N4 -36.4(4) . . . . ? N3 C15 C16 C17 -41.0(4) . . . . ? C14 C15 C16 C17 136.3(3) . . . . ? C16 N4 C18 C19 80.7(4) . . . . ? C16 N4 C18 C23 -105.4(3) . . . . ? C23 C18 C19 C20 3.5(5) . . . . ? N4 C18 C19 C20 177.3(3) . . . . ? C23 C18 C19 C27 -173.1(3) . . . . ? N4 C18 C19 C27 0.6(5) . . . . ? C18 C19 C20 C21 -1.3(5) . . . . ? C27 C19 C20 C21 175.3(3) . . . . ? C19 C20 C21 C22 -1.0(5) . . . . ? C20 C21 C22 C23 1.1(5) . . . . ? C21 C22 C23 C18 1.1(5) . . . . ? C21 C22 C23 C24 -178.2(3) . . . . ? C19 C18 C23 C22 -3.5(5) . . . . ? N4 C18 C23 C22 -177.4(3) . . . . ? C19 C18 C23 C24 175.8(3) . . . . ? N4 C18 C23 C24 1.9(4) . . . . ? C22 C23 C24 C26 31.4(4) . . . . ? C18 C23 C24 C26 -147.9(3) . . . . ? C22 C23 C24 C25 -94.5(4) . . . . ? C18 C23 C24 C25 86.2(4) . . . . ? C20 C19 C27 C29 23.1(5) . . . . ? C18 C19 C27 C29 -160.4(3) . . . . ? C20 C19 C27 C28 -102.0(4) . . . . ? C18 C19 C27 C28 74.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.666 _refine_diff_density_min -0.281 _refine_diff_density_rms 0.074