# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Gregory Solan' _publ_contact_author_email GAS8@LE.AC.UK _publ_section_title ; Solid and solution state flexibility of sterically congested bis(imino)bipyridine complexes of zinc(II) and nickel(II) ; loop_ _publ_author_name 'Gregory Solan' 'Mohamed J. Al-Khatib' 'Gerry A Griffith' 'Kalpana Patel' 'Kuldip Singh' # Attachment '2082.cif' data_2082 _database_code_depnum_ccdc_archive 'CCDC 692756' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H42 N4' _chemical_formula_weight 530.74 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P_-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.943(3) _cell_length_b 9.685(3) _cell_length_c 18.211(5) _cell_angle_alpha 90.00(2) _cell_angle_beta 80.88(2) _cell_angle_gamma 88.617(18) _cell_volume 1556.7(8) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 44 _cell_measurement_theta_min 5.32 _cell_measurement_theta_max 12.96 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.132 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 572 _exptl_absorpt_coefficient_mu 0.067 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 213 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 6642 _diffrn_reflns_av_R_equivalents 0.0445 _diffrn_reflns_av_sigmaI/netI 0.0515 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5497 _reflns_number_gt 3618 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XSCANS (Fait, 1991)' _computing_cell_refinement 'XSCANS (Fait, 1991)' _computing_data_reduction 'XSCANS (Fait, 1991)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0560P)^2^+0.6655P] 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 5497 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0963 _refine_ls_R_factor_gt 0.0567 _refine_ls_wR_factor_ref 0.1457 _refine_ls_wR_factor_gt 0.1265 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.000 _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 0.8809(2) 0.66610(19) 0.28658(10) 0.0316(5) Uani 1 1 d . . . N2 N 0.9419(2) 0.91424(18) 0.42176(10) 0.0304(4) Uani 1 1 d . . . C1 C 0.4200(3) 0.5791(3) 0.29365(17) 0.0570(8) Uani 1 1 d . . . H1B H 0.3536 0.5896 0.3410 0.085 Uiso 1 1 calc R . . H1C H 0.4575 0.4843 0.2878 0.085 Uiso 1 1 calc R . . H1D H 0.3641 0.6022 0.2536 0.085 Uiso 1 1 calc R . . C2 C 0.4954(4) 0.8243(3) 0.30639(18) 0.0647(9) Uani 1 1 d . . . H2B H 0.5811 0.8842 0.3054 0.097 Uiso 1 1 calc R . . H2C H 0.4324 0.8299 0.3549 0.097 Uiso 1 1 calc R . . H2D H 0.4366 0.8532 0.2685 0.097 Uiso 1 1 calc R . . C3 C 0.5527(3) 0.6752(2) 0.29126(14) 0.0400(6) Uani 1 1 d . . . H3A H 0.6085 0.6477 0.3320 0.048 Uiso 1 1 calc R . . C4 C 0.6631(3) 0.6646(2) 0.21912(13) 0.0334(6) Uani 1 1 d . . . C5 C 0.6122(3) 0.6562(2) 0.15076(14) 0.0418(6) Uani 1 1 d . . . H5A H 0.5075 0.6588 0.1496 0.050 Uiso 1 1 calc R . . C6 C 0.7109(3) 0.6442(3) 0.08510(14) 0.0460(7) Uani 1 1 d . . . H6A H 0.6734 0.6408 0.0397 0.055 Uiso 1 1 calc R . . C7 C 0.8648(3) 0.6371(3) 0.08553(13) 0.0416(6) Uani 1 1 d . . . H7A H 0.9315 0.6266 0.0404 0.050 Uiso 1 1 calc R . . C8 C 0.9231(3) 0.6452(2) 0.15213(12) 0.0335(6) Uani 1 1 d . . . C9 C 1.1533(3) 0.7884(3) 0.14298(16) 0.0544(7) Uani 1 1 d . . . H9A H 1.0966 0.8495 0.1801 0.082 Uiso 1 1 calc R . . H9B H 1.1430 0.8215 0.0937 0.082 Uiso 1 1 calc R . . H9C H 1.2594 0.7869 0.1486 0.082 Uiso 1 1 calc R . . C10 C 1.1807(3) 0.5444(3) 0.09589(16) 0.0550(8) Uani 1 1 d . . . H10A H 1.1403 0.4525 0.1032 0.082 Uiso 1 1 calc R . . H10B H 1.2866 0.5421 0.1019 0.082 Uiso 1 1 calc R . . H10C H 1.1715 0.5760 0.0462 0.082 Uiso 1 1 calc R . . C11 C 1.0921(3) 0.6431(2) 0.15321(13) 0.0373(6) Uani 1 1 d . . . H11A H 1.1083 0.6110 0.2030 0.045 Uiso 1 1 calc R . . C12 C 0.8196(3) 0.6622(2) 0.21835(12) 0.0303(5) Uani 1 1 d . . . C13 C 0.8869(3) 0.7805(2) 0.31955(12) 0.0321(5) Uani 1 1 d . . . H13A H 0.8472 0.8610 0.3002 0.039 Uiso 1 1 calc R . . C14 C 0.9555(3) 0.7894(2) 0.38805(12) 0.0298(5) Uani 1 1 d . . . C15 C 1.0321(3) 0.6782(2) 0.41404(13) 0.0384(6) Uani 1 1 d . . . H15A H 1.0368 0.5919 0.3901 0.046 Uiso 1 1 calc R . . C16 C 1.1011(3) 0.6967(3) 0.47559(14) 0.0440(7) Uani 1 1 d . . . H16B H 1.1541 0.6230 0.4942 0.053 Uiso 1 1 calc R . . C17 C 1.0918(3) 0.8248(2) 0.50973(13) 0.0376(6) Uani 1 1 d . . . H17A H 1.1404 0.8400 0.5511 0.045 Uiso 1 1 calc R . . C18 C 1.0094(3) 0.9307(2) 0.48193(12) 0.0297(5) Uani 1 1 d . . . N1A N 0.2465(2) 0.83007(19) 0.72012(10) 0.0332(5) Uani 1 1 d . . . N2A N 0.3931(2) 0.58616(18) 0.57983(10) 0.0304(4) Uani 1 1 d . . . C1A C 0.4038(4) 0.9645(4) 0.9098(2) 0.0794(11) Uani 1 1 d . . . H1AB H 0.5128 0.9615 0.9082 0.119 Uiso 1 1 calc R . . H1AC H 0.3543 0.9444 0.9598 0.119 Uiso 1 1 calc R . . H1AD H 0.3720 1.0558 0.8955 0.119 Uiso 1 1 calc R . . C2A C 0.4204(4) 0.7166(3) 0.8726(2) 0.0852(12) Uani 1 1 d . . . H2AB H 0.5284 0.7203 0.8736 0.128 Uiso 1 1 calc R . . H2AC H 0.4023 0.6526 0.8342 0.128 Uiso 1 1 calc R . . H2AD H 0.3690 0.6857 0.9205 0.128 Uiso 1 1 calc R . . C3A C 0.3608(3) 0.8582(3) 0.85632(14) 0.0428(6) Uani 1 1 d . . . H3AA H 0.4109 0.8837 0.8059 0.051 Uiso 1 1 calc R . . C4A C 0.1922(3) 0.8548(2) 0.85432(13) 0.0370(6) Uani 1 1 d . . . C5A C 0.0864(3) 0.8645(3) 0.91891(14) 0.0459(7) Uani 1 1 d . . . H5AA H 0.1202 0.8765 0.9648 0.055 Uiso 1 1 calc R . . C6A C -0.0664(3) 0.8571(3) 0.91745(14) 0.0481(7) Uani 1 1 d . . . H6AA H -0.1359 0.8624 0.9619 0.058 Uiso 1 1 calc R . . C7A C -0.1171(3) 0.8418(2) 0.85013(14) 0.0405(6) Uani 1 1 d . . . H7AA H -0.2218 0.8383 0.8495 0.049 Uiso 1 1 calc R . . C8A C -0.0177(3) 0.8315(2) 0.78344(13) 0.0339(6) Uani 1 1 d . . . C9A C -0.2081(3) 0.9207(3) 0.70442(16) 0.0509(7) Uani 1 1 d . . . H9AA H -0.2424 0.9083 0.6570 0.076 Uiso 1 1 calc R . . H9AB H -0.1732 1.0141 0.7080 0.076 Uiso 1 1 calc R . . H9AC H -0.2913 0.9048 0.7444 0.076 Uiso 1 1 calc R . . C10A C -0.1283(4) 0.6715(3) 0.69835(18) 0.0654(9) Uani 1 1 d . . . H10D H -0.0449 0.6070 0.7014 0.098 Uiso 1 1 calc R . . H10E H -0.1584 0.6648 0.6496 0.098 Uiso 1 1 calc R . . H10F H -0.2134 0.6496 0.7362 0.098 Uiso 1 1 calc R . . C11A C -0.0785(3) 0.8182(2) 0.71060(14) 0.0396(6) Uani 1 1 d . . . H11B H 0.0053 0.8387 0.6699 0.048 Uiso 1 1 calc R . . C12A C 0.1378(3) 0.8351(2) 0.78655(12) 0.0320(5) Uani 1 1 d . . . C13A C 0.2729(3) 0.7174(2) 0.68433(12) 0.0331(5) Uani 1 1 d . . . H13B H 0.2193 0.6385 0.7016 0.040 Uiso 1 1 calc R . . C14A C 0.3865(3) 0.7079(2) 0.61586(12) 0.0304(5) Uani 1 1 d . . . C15A C 0.4804(3) 0.8154(3) 0.59184(13) 0.0406(6) Uani 1 1 d . . . H15B H 0.4709 0.9001 0.6176 0.049 Uiso 1 1 calc R . . C16A C 0.5883(3) 0.7964(3) 0.52962(14) 0.0465(7) Uani 1 1 d . . . H16A H 0.6538 0.8679 0.5122 0.056 Uiso 1 1 calc R . . C17A C 0.5989(3) 0.6698(3) 0.49299(13) 0.0393(6) Uani 1 1 d . . . H17B H 0.6733 0.6534 0.4511 0.047 Uiso 1 1 calc R . . C18A C 0.4985(3) 0.5686(2) 0.51911(12) 0.0301(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0379(12) 0.0315(10) 0.0274(10) -0.0059(8) -0.0112(9) -0.0006(9) N2 0.0333(11) 0.0344(11) 0.0250(10) -0.0050(8) -0.0093(8) -0.0021(9) C1 0.0477(18) 0.0630(19) 0.0629(19) -0.0023(15) -0.0165(15) -0.0045(14) C2 0.063(2) 0.0505(18) 0.076(2) -0.0213(16) 0.0012(17) 0.0146(15) C3 0.0382(14) 0.0410(14) 0.0433(15) -0.0058(11) -0.0147(12) 0.0047(11) C4 0.0432(15) 0.0243(12) 0.0360(13) -0.0052(10) -0.0170(11) 0.0057(10) C5 0.0455(16) 0.0393(14) 0.0459(16) -0.0084(11) -0.0247(13) 0.0053(12) C6 0.0599(19) 0.0485(16) 0.0354(14) -0.0074(12) -0.0257(14) 0.0017(13) C7 0.0540(17) 0.0436(15) 0.0293(13) -0.0066(11) -0.0140(12) 0.0023(13) C8 0.0455(15) 0.0249(12) 0.0322(13) -0.0050(10) -0.0127(11) 0.0012(10) C9 0.0585(19) 0.0450(16) 0.0626(19) -0.0051(14) -0.0176(15) -0.0075(14) C10 0.0525(18) 0.0525(17) 0.0595(18) -0.0190(14) -0.0090(15) 0.0074(14) C11 0.0447(15) 0.0375(14) 0.0312(13) -0.0049(10) -0.0111(11) 0.0003(11) C12 0.0423(14) 0.0224(11) 0.0299(12) -0.0057(9) -0.0170(11) 0.0020(10) C13 0.0362(14) 0.0335(13) 0.0287(12) -0.0040(10) -0.0111(10) -0.0013(10) C14 0.0300(13) 0.0349(13) 0.0246(11) -0.0050(10) -0.0047(10) -0.0020(10) C15 0.0439(15) 0.0362(14) 0.0368(14) -0.0118(11) -0.0129(12) 0.0081(11) C16 0.0534(17) 0.0408(15) 0.0417(15) -0.0089(12) -0.0222(13) 0.0134(12) C17 0.0423(15) 0.0450(15) 0.0289(12) -0.0089(11) -0.0168(11) 0.0061(12) C18 0.0298(12) 0.0385(13) 0.0217(11) -0.0057(9) -0.0063(9) -0.0028(10) N1A 0.0346(11) 0.0338(11) 0.0293(10) -0.0065(8) 0.0001(9) 0.0051(9) N2A 0.0321(11) 0.0337(11) 0.0248(10) -0.0052(8) -0.0039(8) 0.0058(8) C1A 0.073(2) 0.074(2) 0.095(3) -0.033(2) -0.023(2) -0.0060(19) C2A 0.059(2) 0.059(2) 0.138(4) 0.002(2) -0.019(2) 0.0142(17) C3A 0.0478(16) 0.0458(15) 0.0346(14) -0.0065(11) -0.0062(12) 0.0008(12) C4A 0.0451(15) 0.0322(13) 0.0319(13) -0.0063(10) -0.0005(11) 0.0010(11) C5A 0.0575(19) 0.0476(16) 0.0300(14) -0.0069(11) 0.0006(13) 0.0043(13) C6A 0.0560(19) 0.0451(16) 0.0363(15) -0.0065(12) 0.0130(13) 0.0053(13) C7A 0.0388(15) 0.0339(14) 0.0447(15) -0.0046(11) 0.0056(12) 0.0007(11) C8A 0.0366(14) 0.0251(12) 0.0369(13) -0.0054(10) 0.0034(11) 0.0019(10) C9A 0.0450(16) 0.0512(17) 0.0574(18) -0.0009(13) -0.0123(14) 0.0074(13) C10A 0.076(2) 0.0468(17) 0.079(2) -0.0205(16) -0.0292(18) 0.0004(16) C11A 0.0375(14) 0.0384(14) 0.0422(14) -0.0064(11) -0.0043(12) 0.0025(11) C12A 0.0398(14) 0.0229(11) 0.0298(12) -0.0051(9) 0.0050(11) 0.0031(10) C13A 0.0366(14) 0.0301(13) 0.0313(13) -0.0034(10) -0.0017(11) 0.0020(10) C14A 0.0322(13) 0.0339(13) 0.0253(12) -0.0058(10) -0.0062(10) 0.0067(10) C15A 0.0425(15) 0.0399(14) 0.0367(14) -0.0123(11) 0.0017(12) -0.0014(12) C16A 0.0477(16) 0.0477(16) 0.0410(15) -0.0122(12) 0.0039(12) -0.0144(13) C17A 0.0365(14) 0.0496(16) 0.0295(13) -0.0126(11) 0.0023(11) -0.0034(12) C18A 0.0294(12) 0.0376(13) 0.0236(11) -0.0047(9) -0.0057(10) 0.0039(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 N1 C13 1.267(3) . ? N1 C12 1.436(3) . ? N2 C18 1.343(3) . ? N2 C14 1.350(3) . ? C1 C3 1.521(4) . ? C1 H1B 0.9700 . ? C1 H1C 0.9700 . ? C1 H1D 0.9700 . ? C2 C3 1.530(3) . ? C2 H2B 0.9700 . ? C2 H2C 0.9700 . ? C2 H2D 0.9700 . ? C3 C4 1.515(3) . ? C3 H3A 0.9900 . ? C4 C5 1.395(3) . ? C4 C12 1.397(3) . ? C5 C6 1.372(4) . ? C5 H5A 0.9400 . ? C6 C7 1.378(4) . ? C6 H6A 0.9400 . ? C7 C8 1.397(3) . ? C7 H7A 0.9400 . ? C8 C12 1.406(3) . ? C8 C11 1.513(3) . ? C9 C11 1.523(3) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 C11 1.527(3) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C11 H11A 0.9900 . ? C13 C14 1.478(3) . ? C13 H13A 0.9400 . ? C14 C15 1.386(3) . ? C15 C16 1.376(3) . ? C15 H15A 0.9400 . ? C16 C17 1.382(3) . ? C16 H16B 0.9400 . ? C17 C18 1.390(3) . ? C17 H17A 0.9400 . ? C18 C18 1.490(4) 2_776 ? N1A C13A 1.269(3) . ? N1A C12A 1.427(3) . ? N2A C18A 1.342(3) . ? N2A C14A 1.345(3) . ? C1A C3A 1.514(4) . ? C1A H1AB 0.9700 . ? C1A H1AC 0.9700 . ? C1A H1AD 0.9700 . ? C2A C3A 1.506(4) . ? C2A H2AB 0.9700 . ? C2A H2AC 0.9700 . ? C2A H2AD 0.9700 . ? C3A C4A 1.516(4) . ? C3A H3AA 0.9900 . ? C4A C5A 1.389(3) . ? C4A C12A 1.411(3) . ? C5A C6A 1.375(4) . ? C5A H5AA 0.9400 . ? C6A C7A 1.382(4) . ? C6A H6AA 0.9400 . ? C7A C8A 1.389(3) . ? C7A H7AA 0.9400 . ? C8A C12A 1.401(3) . ? C8A C11A 1.518(3) . ? C9A C11A 1.526(3) . ? C9A H9AA 0.9700 . ? C9A H9AB 0.9700 . ? C9A H9AC 0.9700 . ? C10A C11A 1.525(3) . ? C10A H10D 0.9700 . ? C10A H10E 0.9700 . ? C10A H10F 0.9700 . ? C11A H11B 0.9900 . ? C13A C14A 1.480(3) . ? C13A H13B 0.9400 . ? C14A C15A 1.381(3) . ? C15A C16A 1.376(3) . ? C15A H15B 0.9400 . ? C16A C17A 1.390(3) . ? C16A H16A 0.9400 . ? C17A C18A 1.378(3) . ? C17A H17B 0.9400 . ? C18A C18A 1.498(4) 2_666 ? 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 C13 N1 C12 119.48(19) . . ? C18 N2 C14 117.84(19) . . ? C3 C1 H1B 109.5 . . ? C3 C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C1 H1D 109.5 . . ? H1B C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? C3 C2 H2B 109.5 . . ? C3 C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C3 C2 H2D 109.5 . . ? H2B C2 H2D 109.5 . . ? H2C C2 H2D 109.5 . . ? C4 C3 C1 112.9(2) . . ? C4 C3 C2 111.0(2) . . ? C1 C3 C2 110.3(2) . . ? C4 C3 H3A 107.4 . . ? C1 C3 H3A 107.4 . . ? C2 C3 H3A 107.4 . . ? C5 C4 C12 117.3(2) . . ? C5 C4 C3 121.2(2) . . ? C12 C4 C3 121.5(2) . . ? C6 C5 C4 121.8(2) . . ? C6 C5 H5A 119.1 . . ? C4 C5 H5A 119.1 . . ? C5 C6 C7 120.1(2) . . ? C5 C6 H6A 120.0 . . ? C7 C6 H6A 120.0 . . ? C6 C7 C8 120.9(2) . . ? C6 C7 H7A 119.5 . . ? C8 C7 H7A 119.5 . . ? C7 C8 C12 117.8(2) . . ? C7 C8 C11 121.5(2) . . ? C12 C8 C11 120.7(2) . . ? C11 C9 H9A 109.5 . . ? C11 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C11 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 H10A 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C11 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 C9 110.4(2) . . ? C8 C11 C10 113.29(19) . . ? C9 C11 C10 110.5(2) . . ? C8 C11 H11A 107.5 . . ? C9 C11 H11A 107.5 . . ? C10 C11 H11A 107.5 . . ? C4 C12 C8 122.0(2) . . ? C4 C12 N1 120.7(2) . . ? C8 C12 N1 117.2(2) . . ? N1 C13 C14 120.9(2) . . ? N1 C13 H13A 119.5 . . ? C14 C13 H13A 119.5 . . ? N2 C14 C15 122.8(2) . . ? N2 C14 C13 115.2(2) . . ? C15 C14 C13 122.0(2) . . ? C16 C15 C14 118.7(2) . . ? C16 C15 H15A 120.7 . . ? C14 C15 H15A 120.7 . . ? C15 C16 C17 119.3(2) . . ? C15 C16 H16B 120.3 . . ? C17 C16 H16B 120.3 . . ? C16 C17 C18 118.9(2) . . ? C16 C17 H17A 120.6 . . ? C18 C17 H17A 120.6 . . ? N2 C18 C17 122.4(2) . . ? N2 C18 C18 116.3(2) . 2_776 ? C17 C18 C18 121.3(2) . 2_776 ? C13A N1A C12A 119.8(2) . . ? C18A N2A C14A 117.9(2) . . ? C3A C1A H1AB 109.5 . . ? C3A C1A H1AC 109.5 . . ? H1AB C1A H1AC 109.5 . . ? C3A C1A H1AD 109.5 . . ? H1AB C1A H1AD 109.5 . . ? H1AC C1A H1AD 109.5 . . ? C3A C2A H2AB 109.5 . . ? C3A C2A H2AC 109.5 . . ? H2AB C2A H2AC 109.5 . . ? C3A C2A H2AD 109.5 . . ? H2AB C2A H2AD 109.5 . . ? H2AC C2A H2AD 109.5 . . ? C2A C3A C1A 111.0(3) . . ? C2A C3A C4A 110.3(2) . . ? C1A C3A C4A 113.7(2) . . ? C2A C3A H3AA 107.1 . . ? C1A C3A H3AA 107.1 . . ? C4A C3A H3AA 107.1 . . ? C5A C4A C12A 117.7(2) . . ? C5A C4A C3A 121.5(2) . . ? C12A C4A C3A 120.7(2) . . ? C6A C5A C4A 121.6(2) . . ? C6A C5A H5AA 119.2 . . ? C4A C5A H5AA 119.2 . . ? C5A C6A C7A 119.5(2) . . ? C5A C6A H6AA 120.2 . . ? C7A C6A H6AA 120.2 . . ? C6A C7A C8A 121.9(3) . . ? C6A C7A H7AA 119.1 . . ? C8A C7A H7AA 119.1 . . ? C7A C8A C12A 117.6(2) . . ? C7A C8A C11A 120.1(2) . . ? C12A C8A C11A 122.3(2) . . ? C11A C9A H9AA 109.5 . . ? C11A C9A H9AB 109.5 . . ? H9AA C9A H9AB 109.5 . . ? C11A C9A H9AC 109.5 . . ? H9AA C9A H9AC 109.5 . . ? H9AB C9A H9AC 109.5 . . ? C11A C10A H10D 109.5 . . ? C11A C10A H10E 109.5 . . ? H10D C10A H10E 109.5 . . ? C11A C10A H10F 109.5 . . ? H10D C10A H10F 109.5 . . ? H10E C10A H10F 109.5 . . ? C8A C11A C10A 111.7(2) . . ? C8A C11A C9A 112.7(2) . . ? C10A C11A C9A 109.8(2) . . ? C8A C11A H11B 107.4 . . ? C10A C11A H11B 107.4 . . ? C9A C11A H11B 107.4 . . ? C8A C12A C4A 121.6(2) . . ? C8A C12A N1A 120.7(2) . . ? C4A C12A N1A 117.5(2) . . ? N1A C13A C14A 121.3(2) . . ? N1A C13A H13B 119.4 . . ? C14A C13A H13B 119.4 . . ? N2A C14A C15A 122.8(2) . . ? N2A C14A C13A 115.0(2) . . ? C15A C14A C13A 122.3(2) . . ? C16A C15A C14A 118.9(2) . . ? C16A C15A H15B 120.6 . . ? C14A C15A H15B 120.6 . . ? C15A C16A C17A 118.9(2) . . ? C15A C16A H16A 120.5 . . ? C17A C16A H16A 120.5 . . ? C18A C17A C16A 118.9(2) . . ? C18A C17A H17B 120.6 . . ? C16A C17A H17B 120.6 . . ? N2A C18A C17A 122.6(2) . . ? N2A C18A C18A 116.0(3) . 2_666 ? C17A C18A C18A 121.4(3) . 2_666 ? 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 C1 C3 C4 C5 42.4(3) . . . . ? C2 C3 C4 C5 -82.1(3) . . . . ? C1 C3 C4 C12 -137.3(2) . . . . ? C2 C3 C4 C12 98.2(3) . . . . ? C12 C4 C5 C6 0.8(4) . . . . ? C3 C4 C5 C6 -178.9(2) . . . . ? C4 C5 C6 C7 1.4(4) . . . . ? C5 C6 C7 C8 -1.5(4) . . . . ? C6 C7 C8 C12 -0.6(3) . . . . ? C6 C7 C8 C11 -177.6(2) . . . . ? C7 C8 C11 C9 86.4(3) . . . . ? C12 C8 C11 C9 -90.6(3) . . . . ? C7 C8 C11 C10 -38.2(3) . . . . ? C12 C8 C11 C10 144.9(2) . . . . ? C5 C4 C12 C8 -3.0(3) . . . . ? C3 C4 C12 C8 176.6(2) . . . . ? C5 C4 C12 N1 -178.0(2) . . . . ? C3 C4 C12 N1 1.6(3) . . . . ? C7 C8 C12 C4 2.9(3) . . . . ? C11 C8 C12 C4 180.0(2) . . . . ? C7 C8 C12 N1 178.1(2) . . . . ? C11 C8 C12 N1 -4.9(3) . . . . ? C13 N1 C12 C4 -79.9(3) . . . . ? C13 N1 C12 C8 104.9(2) . . . . ? C12 N1 C13 C14 -177.2(2) . . . . ? C18 N2 C14 C15 1.6(3) . . . . ? C18 N2 C14 C13 -176.4(2) . . . . ? N1 C13 C14 N2 -173.9(2) . . . . ? N1 C13 C14 C15 8.1(4) . . . . ? N2 C14 C15 C16 -1.9(4) . . . . ? C13 C14 C15 C16 176.0(2) . . . . ? C14 C15 C16 C17 0.2(4) . . . . ? C15 C16 C17 C18 1.6(4) . . . . ? C14 N2 C18 C17 0.3(3) . . . . ? C14 N2 C18 C18 -179.4(2) . . . 2_776 ? C16 C17 C18 N2 -1.9(4) . . . . ? C16 C17 C18 C18 177.7(3) . . . 2_776 ? C2A C3A C4A C5A 83.7(3) . . . . ? C1A C3A C4A C5A -41.8(4) . . . . ? C2A C3A C4A C12A -93.4(3) . . . . ? C1A C3A C4A C12A 141.1(3) . . . . ? C12A C4A C5A C6A -0.8(4) . . . . ? C3A C4A C5A C6A -178.0(2) . . . . ? C4A C5A C6A C7A -1.1(4) . . . . ? C5A C6A C7A C8A 1.0(4) . . . . ? C6A C7A C8A C12A 0.9(3) . . . . ? C6A C7A C8A C11A -178.6(2) . . . . ? C7A C8A C11A C10A -78.1(3) . . . . ? C12A C8A C11A C10A 102.4(3) . . . . ? C7A C8A C11A C9A 46.1(3) . . . . ? C12A C8A C11A C9A -133.3(2) . . . . ? C7A C8A C12A C4A -2.8(3) . . . . ? C11A C8A C12A C4A 176.7(2) . . . . ? C7A C8A C12A N1A -177.7(2) . . . . ? C11A C8A C12A N1A 1.7(3) . . . . ? C5A C4A C12A C8A 2.7(3) . . . . ? C3A C4A C12A C8A 180.0(2) . . . . ? C5A C4A C12A N1A 177.8(2) . . . . ? C3A C4A C12A N1A -4.9(3) . . . . ? C13A N1A C12A C8A -73.5(3) . . . . ? C13A N1A C12A C4A 111.4(3) . . . . ? C12A N1A C13A C14A -179.1(2) . . . . ? C18A N2A C14A C15A 1.7(3) . . . . ? C18A N2A C14A C13A -177.06(19) . . . . ? N1A C13A C14A N2A -174.1(2) . . . . ? N1A C13A C14A C15A 7.1(4) . . . . ? N2A C14A C15A C16A -1.9(4) . . . . ? C13A C14A C15A C16A 176.9(2) . . . . ? C14A C15A C16A C17A 0.1(4) . . . . ? C15A C16A C17A C18A 1.6(4) . . . . ? C14A N2A C18A C17A 0.1(3) . . . . ? C14A N2A C18A C18A 179.9(2) . . . 2_666 ? C16A C17A C18A N2A -1.8(4) . . . . ? C16A C17A C18A C18A 178.4(3) . . . 2_666 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.312 _refine_diff_density_min -0.214 _refine_diff_density_rms 0.039 # Attachment '08030.cif' data_08030 _database_code_depnum_ccdc_archive 'CCDC 692757' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C36 H42 Cl2 N4 Zn)0.5(C H2 Cl2)2(H2 O)' _chemical_formula_sum 'C36.50 H47 Cl3 N4 O2 Zn' _chemical_formula_weight 745.50 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 13.701(3) _cell_length_b 16.571(3) _cell_length_c 33.355(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7573(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 738 _cell_measurement_theta_min 2.282 _cell_measurement_theta_max 23.403 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.308 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3128 _exptl_absorpt_coefficient_mu 0.897 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.372 _exptl_absorpt_correction_T_max 0.928 _exptl_absorpt_process_details ; absorption correction based on 7161 reflections(SADABS);Rint 0.0806 before correction and 0.0730 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 59507 _diffrn_reflns_av_R_equivalents 0.1839 _diffrn_reflns_av_sigmaI/netI 0.2232 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.22 _diffrn_reflns_theta_max 26.00 _reflns_number_total 14881 _reflns_number_gt 6420 _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 ; Disordered CH2Cl2 and H2O were omitted using the SQUEEZE option of PLATON. The solvent accessible voids are 1087.7\%A3 with an estimated 287e/cell to be added. Four solvent CH2Cl2 molecules and sixteen H2O molecules/unit cell accounting for 296e were included in the formula, FWt, (000) and density calculations. PLATON Reference: Spek, A.L. (1990), Acta Cryst. A46, C-34. 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^)+(0.0493P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.065(18) _refine_ls_number_reflns 14881 _refine_ls_number_parameters 781 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1749 _refine_ls_R_factor_gt 0.0788 _refine_ls_wR_factor_ref 0.1710 _refine_ls_wR_factor_gt 0.1404 _refine_ls_goodness_of_fit_ref 0.886 _refine_ls_restrained_S_all 0.886 _refine_ls_shift/su_max 0.000 _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 0.79502(8) 0.56430(6) 0.37254(3) 0.0543(3) Uani 1 1 d . . . Cl1 Cl 0.6559(2) 0.62828(17) 0.35922(7) 0.0751(8) Uani 1 1 d . . . Cl2 Cl 0.8585(2) 0.47808(16) 0.32849(7) 0.0841(10) Uani 1 1 d . . . N1 N 0.8921(5) 0.6717(4) 0.3646(2) 0.046(2) Uani 1 1 d . . . N2 N 0.8571(5) 0.5845(4) 0.42801(18) 0.0395(18) Uani 1 1 d . . . N3 N 0.7389(5) 0.4670(4) 0.41190(19) 0.0448(19) Uani 1 1 d . . . N4 N 0.6011(6) 0.3474(5) 0.3425(2) 0.052(2) Uani 1 1 d . . . C1 C 0.8998(8) 0.7167(6) 0.3250(3) 0.056(3) Uani 1 1 d . . . C2 C 0.8433(9) 0.7816(6) 0.3178(3) 0.065(3) Uani 1 1 d . . . C3 C 0.8397(10) 0.8132(7) 0.2785(4) 0.092(4) Uani 1 1 d . . . H3 H 0.7990 0.8578 0.2721 0.110 Uiso 1 1 calc R . . C4 C 0.8980(10) 0.7768(9) 0.2493(3) 0.092(5) Uani 1 1 d . . . H4 H 0.8949 0.7972 0.2227 0.111 Uiso 1 1 calc R . . C5 C 0.9585(8) 0.7143(8) 0.2567(3) 0.077(4) Uani 1 1 d . . . H5 H 0.9972 0.6929 0.2356 0.092 Uiso 1 1 calc R . . C6 C 0.9647(7) 0.6801(6) 0.2959(3) 0.055(3) Uani 1 1 d . . . C7 C 1.0371(7) 0.6152(6) 0.3066(3) 0.056(3) Uani 1 1 d . . . H7 H 1.0073 0.5803 0.3278 0.068 Uiso 1 1 calc R . . C8 C 1.1298(6) 0.6512(6) 0.3233(3) 0.065(3) Uani 1 1 d . . . H8A H 1.1619 0.6837 0.3026 0.098 Uiso 1 1 calc R . . H8B H 1.1737 0.6078 0.3319 0.098 Uiso 1 1 calc R . . H8C H 1.1140 0.6856 0.3463 0.098 Uiso 1 1 calc R . . C9 C 1.0618(8) 0.5624(7) 0.2711(3) 0.092(4) Uani 1 1 d . . . H9A H 1.0022 0.5368 0.2610 0.138 Uiso 1 1 calc R . . H9B H 1.1082 0.5206 0.2794 0.138 Uiso 1 1 calc R . . H9C H 1.0911 0.5954 0.2499 0.138 Uiso 1 1 calc R . . C10 C 0.7831(9) 0.8227(6) 0.3503(3) 0.074(3) Uani 1 1 d . . . H10 H 0.7793 0.7855 0.3739 0.089 Uiso 1 1 calc R . . C11 C 0.8332(10) 0.8994(6) 0.3636(3) 0.113(5) Uani 1 1 d . . . H11A H 0.9004 0.8873 0.3716 0.170 Uiso 1 1 calc R . . H11B H 0.7978 0.9227 0.3864 0.170 Uiso 1 1 calc R . . H11C H 0.8337 0.9381 0.3414 0.170 Uiso 1 1 calc R . . C12 C 0.6772(9) 0.8459(7) 0.3378(3) 0.110(5) Uani 1 1 d . . . H12A H 0.6424 0.8680 0.3610 0.166 Uiso 1 1 calc R . . H12B H 0.6429 0.7978 0.3281 0.166 Uiso 1 1 calc R . . H12C H 0.6795 0.8864 0.3165 0.166 Uiso 1 1 calc R . . C13 C 0.9289(6) 0.7001(5) 0.3957(2) 0.034(2) Uani 1 1 d . . . H13 H 0.9638 0.7496 0.3960 0.040 Uiso 1 1 calc R . . C14 C 0.9140(6) 0.6504(5) 0.4325(2) 0.030(2) Uiso 1 1 d . . . C15 C 0.9480(6) 0.6729(5) 0.4712(2) 0.046(3) Uani 1 1 d . . . H15 H 0.9852 0.7206 0.4751 0.055 Uiso 1 1 calc R . . C16 C 0.9245(6) 0.6225(5) 0.5027(2) 0.036(2) Uani 1 1 d . . . H16 H 0.9467 0.6358 0.5289 0.043 Uiso 1 1 calc R . . C17 C 0.8724(5) 0.5567(5) 0.4976(2) 0.040(2) Uani 1 1 d . . . H17 H 0.8561 0.5240 0.5200 0.048 Uiso 1 1 calc R . . C18 C 0.8399(7) 0.5337(6) 0.4581(2) 0.044(2) Uani 1 1 d . . . C19 C 0.7846(6) 0.4654(6) 0.4483(2) 0.053(3) Uani 1 1 d . . . C20 C 0.7745(7) 0.3961(6) 0.4727(3) 0.059(3) Uani 1 1 d . . . H20 H 0.8100 0.3926 0.4971 0.071 Uiso 1 1 calc R . . C21 C 0.7148(7) 0.3346(7) 0.4617(3) 0.072(3) Uani 1 1 d . . . H21 H 0.7058 0.2902 0.4794 0.087 Uiso 1 1 calc R . . C22 C 0.6667(8) 0.3357(6) 0.4252(3) 0.071(3) Uani 1 1 d . . . H22 H 0.6240 0.2935 0.4172 0.085 Uiso 1 1 calc R . . C23 C 0.6851(7) 0.4041(6) 0.4003(3) 0.056(3) Uani 1 1 d . . . C24 C 0.6474(8) 0.4029(6) 0.3581(3) 0.064(3) Uani 1 1 d . . . H24 H 0.6604 0.4489 0.3419 0.077 Uiso 1 1 calc R . . C25 C 0.5861(8) 0.3497(8) 0.3002(3) 0.073(4) Uani 1 1 d . . . C26 C 0.6388(8) 0.2930(7) 0.2797(3) 0.068(3) Uani 1 1 d . . . C27 C 0.6286(8) 0.2937(9) 0.2361(3) 0.105(5) Uani 1 1 d . . . H27 H 0.6662 0.2583 0.2199 0.126 Uiso 1 1 calc R . . C28 C 0.5642(9) 0.3461(9) 0.2192(4) 0.097(5) Uani 1 1 d . . . H28 H 0.5570 0.3467 0.1909 0.117 Uiso 1 1 calc R . . C29 C 0.5102(10) 0.3974(8) 0.2417(4) 0.097(5) Uani 1 1 d . . . H29 H 0.4664 0.4331 0.2286 0.116 Uiso 1 1 calc R . . C30 C 0.5162(8) 0.3998(7) 0.2837(3) 0.073(4) Uani 1 1 d . . . C31 C 0.4505(9) 0.4560(7) 0.3057(3) 0.084(4) Uani 1 1 d . . . H31 H 0.4666 0.4504 0.3348 0.101 Uiso 1 1 calc R . . C32 C 0.3416(9) 0.4325(8) 0.3010(4) 0.130(5) Uani 1 1 d . . . H32A H 0.3033 0.4577 0.3224 0.194 Uiso 1 1 calc R . . H32B H 0.3349 0.3737 0.3026 0.194 Uiso 1 1 calc R . . H32C H 0.3176 0.4513 0.2749 0.194 Uiso 1 1 calc R . . C33 C 0.4559(11) 0.5408(7) 0.2963(4) 0.139(6) Uani 1 1 d . . . H33A H 0.5245 0.5568 0.2936 0.208 Uiso 1 1 calc R . . H33B H 0.4255 0.5720 0.3179 0.208 Uiso 1 1 calc R . . H33C H 0.4215 0.5512 0.2711 0.208 Uiso 1 1 calc R . . C34 C 0.7050(9) 0.2349(7) 0.3004(3) 0.084(4) Uani 1 1 d . . . H34 H 0.6897 0.2359 0.3297 0.101 Uiso 1 1 calc R . . C35 C 0.8151(9) 0.2607(7) 0.2947(3) 0.100(4) Uani 1 1 d . . . H35A H 0.8340 0.2535 0.2666 0.150 Uiso 1 1 calc R . . H35B H 0.8567 0.2272 0.3118 0.150 Uiso 1 1 calc R . . H35C H 0.8228 0.3175 0.3022 0.150 Uiso 1 1 calc R . . C36 C 0.6956(10) 0.1470(7) 0.2856(3) 0.115(5) Uani 1 1 d . . . H36A H 0.6300 0.1268 0.2916 0.172 Uiso 1 1 calc R . . H36B H 0.7441 0.1133 0.2992 0.172 Uiso 1 1 calc R . . H36C H 0.7067 0.1451 0.2566 0.172 Uiso 1 1 calc R . . Zn1A Zn 0.16332(7) 0.96500(6) 0.87860(3) 0.0446(3) Uani 1 1 d . . . Cl1A Cl 0.26755(18) 0.92087(15) 0.92579(6) 0.0616(7) Uani 1 1 d . . . Cl2A Cl 0.06684(18) 1.07070(15) 0.89183(6) 0.0570(7) Uani 1 1 d . . . N1A N 0.0653(5) 0.8587(4) 0.88577(18) 0.0396(19) Uani 1 1 d . . . N2A N 0.1563(5) 0.9117(4) 0.82272(17) 0.0341(17) Uani 1 1 d . . . N3A N 0.2706(5) 1.0328(4) 0.84157(17) 0.0358(17) Uani 1 1 d . . . N4A N 0.3772(5) 1.1671(4) 0.9124(2) 0.0425(19) Uani 1 1 d . . . C1A C 0.0321(7) 0.8261(6) 0.9246(3) 0.046(2) Uani 1 1 d . . . C2A C 0.0837(9) 0.7618(7) 0.9411(3) 0.068(3) Uani 1 1 d . . . C3A C 0.0605(10) 0.7384(7) 0.9811(3) 0.082(4) Uani 1 1 d . . . H3A H 0.0929 0.6945 0.9937 0.099 Uiso 1 1 calc R . . C4A C -0.0097(9) 0.7814(8) 1.0006(3) 0.080(4) Uani 1 1 d . . . H4A H -0.0250 0.7666 1.0274 0.096 Uiso 1 1 calc R . . C5A C -0.0594(8) 0.8446(7) 0.9839(3) 0.068(3) Uani 1 1 d . . . H5A H -0.1059 0.8731 0.9996 0.082 Uiso 1 1 calc R . . C6A C -0.0432(7) 0.8678(7) 0.9445(3) 0.063(3) Uani 1 1 d . . . C7A C -0.1059(7) 0.9263(6) 0.9239(3) 0.065(3) Uani 1 1 d . . . H7A H -0.0650 0.9529 0.9029 0.078 Uiso 1 1 calc R . . C8A C -0.1891(7) 0.8890(6) 0.9033(3) 0.074(3) Uani 1 1 d . . . H8A1 H -0.1662 0.8612 0.8792 0.112 Uiso 1 1 calc R . . H8A2 H -0.2363 0.9308 0.8958 0.112 Uiso 1 1 calc R . . H8A3 H -0.2205 0.8500 0.9213 0.112 Uiso 1 1 calc R . . C9A C -0.1412(9) 0.9954(6) 0.9538(3) 0.106(4) Uani 1 1 d . . . H9A1 H -0.1820 0.9717 0.9748 0.159 Uiso 1 1 calc R . . H9A2 H -0.1791 1.0356 0.9389 0.159 Uiso 1 1 calc R . . H9A3 H -0.0843 1.0214 0.9660 0.159 Uiso 1 1 calc R . . C10A C 0.1598(8) 0.7121(6) 0.9192(3) 0.059(3) Uani 1 1 d . . . H10A H 0.1775 0.7403 0.8937 0.071 Uiso 1 1 calc R . . C11A C 0.1211(10) 0.6306(7) 0.9093(4) 0.118(5) Uani 1 1 d . . . H11D H 0.1033 0.6024 0.9340 0.178 Uiso 1 1 calc R . . H11E H 0.1712 0.5996 0.8950 0.178 Uiso 1 1 calc R . . H11F H 0.0632 0.6361 0.8922 0.178 Uiso 1 1 calc R . . C12A C 0.2500(8) 0.7029(7) 0.9442(3) 0.093(4) Uani 1 1 d . . . H12D H 0.2794 0.7560 0.9487 0.139 Uiso 1 1 calc R . . H12E H 0.2967 0.6680 0.9303 0.139 Uiso 1 1 calc R . . H12F H 0.2328 0.6786 0.9701 0.139 Uiso 1 1 calc R . . C13A C 0.0531(6) 0.8171(6) 0.8543(3) 0.047(3) Uani 1 1 d . . . H13A H 0.0159 0.7687 0.8542 0.057 Uiso 1 1 calc R . . C14A C 0.1008(6) 0.8490(5) 0.8175(2) 0.037(2) Uani 1 1 d . . . C15A C 0.0932(7) 0.8102(5) 0.7801(3) 0.051(3) Uani 1 1 d . . . H15A H 0.0518 0.7648 0.7764 0.061 Uiso 1 1 calc R . . C16A C 0.1492(8) 0.8414(6) 0.7489(3) 0.059(3) Uani 1 1 d . . . H16A H 0.1462 0.8170 0.7232 0.070 Uiso 1 1 calc R . . C17A C 0.2067(7) 0.9049(5) 0.7548(2) 0.049(3) Uani 1 1 d . . . H17A H 0.2453 0.9252 0.7334 0.059 Uiso 1 1 calc R . . C18A C 0.2101(6) 0.9418(4) 0.7925(2) 0.0314(19) Uani 1 1 d . . . C19A C 0.2736(6) 1.0085(5) 0.8025(2) 0.037(2) Uani 1 1 d . . . C20A C 0.3361(7) 1.0467(6) 0.7759(3) 0.058(3) Uani 1 1 d . . . H20A H 0.3348 1.0310 0.7485 0.070 Uiso 1 1 calc R . . C21A C 0.4001(8) 1.1063(6) 0.7875(3) 0.071(3) Uani 1 1 d . . . H21A H 0.4449 1.1298 0.7691 0.085 Uiso 1 1 calc R . . C22A C 0.3956(7) 1.1311(6) 0.8286(3) 0.056(3) Uani 1 1 d . . . H22A H 0.4358 1.1735 0.8384 0.067 Uiso 1 1 calc R . . C23A C 0.3298(7) 1.0907(5) 0.8539(2) 0.041(2) Uani 1 1 d . . . C24A C 0.3191(6) 1.1183(4) 0.8972(2) 0.033(2) Uiso 1 1 d . . . H24A H 0.2669 1.0979 0.9130 0.040 Uiso 1 1 calc R . . C25A C 0.3606(7) 1.1853(5) 0.9543(3) 0.041(2) Uani 1 1 d . . . C26A C 0.3078(7) 1.2538(6) 0.9630(3) 0.053(3) Uani 1 1 d . . . C27A C 0.2985(7) 1.2769(6) 1.0049(3) 0.070(3) Uani 1 1 d . . . H27A H 0.2648 1.3249 1.0119 0.084 Uiso 1 1 calc R . . C28A C 0.3388(9) 1.2290(7) 1.0343(3) 0.072(3) Uani 1 1 d . . . H28A H 0.3329 1.2440 1.0617 0.087 Uiso 1 1 calc R . . C29A C 0.3864(8) 1.1609(7) 1.0243(3) 0.067(3) Uani 1 1 d . . . H29A H 0.4118 1.1281 1.0451 0.081 Uiso 1 1 calc R . . C30A C 0.4006(6) 1.1358(5) 0.9840(3) 0.041(2) Uani 1 1 d . . . C31A C 0.4611(7) 1.0617(7) 0.9738(3) 0.063(3) Uani 1 1 d . . . H31A H 0.4338 1.0386 0.9485 0.075 Uiso 1 1 calc R . . C32A C 0.5621(9) 1.0845(7) 0.9656(4) 0.120(5) Uani 1 1 d . . . H32D H 0.5950 1.0982 0.9907 0.180 Uiso 1 1 calc R . . H32E H 0.5631 1.1313 0.9476 0.180 Uiso 1 1 calc R . . H32F H 0.5960 1.0392 0.9528 0.180 Uiso 1 1 calc R . . C33A C 0.4622(10) 0.9968(8) 1.0034(4) 0.139(6) Uani 1 1 d . . . H33D H 0.5048 0.9532 0.9940 0.208 Uiso 1 1 calc R . . H33E H 0.3958 0.9761 1.0071 0.208 Uiso 1 1 calc R . . H33F H 0.4868 1.0176 1.0290 0.208 Uiso 1 1 calc R . . C34A C 0.2687(9) 1.3087(6) 0.9304(3) 0.075(3) Uani 1 1 d . . . H34A H 0.3034 1.2943 0.9050 0.090 Uiso 1 1 calc R . . C35A C 0.1594(9) 1.2912(6) 0.9237(3) 0.092(4) Uani 1 1 d . . . H35D H 0.1510 1.2347 0.9157 0.137 Uiso 1 1 calc R . . H35E H 0.1343 1.3265 0.9025 0.137 Uiso 1 1 calc R . . H35F H 0.1235 1.3012 0.9486 0.137 Uiso 1 1 calc R . . C36A C 0.2854(9) 1.3985(6) 0.9375(3) 0.088(4) Uani 1 1 d . . . H36D H 0.2424 1.4172 0.9591 0.132 Uiso 1 1 calc R . . H36E H 0.2709 1.4284 0.9129 0.132 Uiso 1 1 calc R . . H36F H 0.3536 1.4075 0.9452 0.132 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0727(8) 0.0677(8) 0.0226(5) 0.0086(5) -0.0095(5) -0.0213(7) Cl1 0.0731(19) 0.106(2) 0.0462(15) 0.0238(14) -0.0174(14) -0.0165(18) Cl2 0.136(3) 0.082(2) 0.0341(14) -0.0081(13) 0.0167(15) -0.043(2) N1 0.059(5) 0.046(5) 0.033(5) 0.000(4) -0.008(4) -0.017(4) N2 0.038(4) 0.052(5) 0.029(4) 0.010(3) -0.009(3) -0.008(4) N3 0.046(5) 0.052(5) 0.036(4) 0.010(4) -0.020(3) -0.019(4) N4 0.062(6) 0.076(6) 0.018(4) 0.003(4) -0.007(4) -0.010(5) C1 0.077(8) 0.067(8) 0.023(5) 0.010(5) -0.016(5) -0.028(6) C2 0.116(9) 0.053(7) 0.026(5) 0.003(5) -0.011(6) 0.029(7) C3 0.115(11) 0.091(9) 0.070(9) 0.028(7) -0.045(9) -0.037(9) C4 0.113(12) 0.131(13) 0.033(7) 0.020(8) -0.017(7) -0.025(10) C5 0.070(9) 0.130(12) 0.031(6) 0.027(7) -0.002(6) -0.028(8) C6 0.058(7) 0.077(8) 0.028(6) 0.000(5) 0.006(5) -0.013(6) C7 0.056(7) 0.057(7) 0.057(7) -0.018(5) 0.021(5) -0.019(6) C8 0.040(6) 0.096(9) 0.060(7) -0.014(6) 0.012(5) 0.000(6) C9 0.086(8) 0.115(10) 0.075(8) -0.031(7) 0.030(6) -0.005(8) C10 0.108(10) 0.045(7) 0.070(8) 0.003(6) -0.002(7) -0.002(7) C11 0.173(13) 0.078(9) 0.089(10) -0.035(7) -0.010(9) 0.034(10) C12 0.134(13) 0.100(10) 0.097(10) 0.008(7) -0.037(9) 0.049(10) C13 0.046(6) 0.026(5) 0.029(5) -0.008(4) -0.001(4) -0.005(4) C15 0.067(7) 0.032(6) 0.038(6) -0.008(4) -0.003(5) -0.032(5) C16 0.038(5) 0.039(6) 0.031(5) -0.011(4) -0.004(4) -0.011(5) C17 0.042(5) 0.059(6) 0.019(4) 0.001(4) -0.003(4) -0.021(5) C18 0.056(6) 0.057(6) 0.018(4) -0.004(4) 0.006(4) -0.018(6) C19 0.046(6) 0.079(8) 0.033(5) 0.002(5) 0.005(5) 0.005(6) C20 0.071(7) 0.072(8) 0.034(6) 0.018(5) 0.001(5) -0.026(6) C21 0.078(8) 0.107(9) 0.033(6) 0.020(6) -0.011(5) -0.055(7) C22 0.098(9) 0.076(8) 0.040(6) 0.001(5) -0.022(6) -0.042(7) C23 0.061(7) 0.063(7) 0.044(6) 0.006(5) -0.015(5) -0.012(6) C24 0.095(9) 0.066(8) 0.033(6) 0.007(5) -0.010(6) -0.003(7) C25 0.069(8) 0.126(11) 0.024(6) 0.006(6) -0.012(6) -0.036(8) C26 0.071(8) 0.102(10) 0.032(6) -0.002(6) 0.004(6) 0.003(7) C27 0.063(9) 0.223(17) 0.030(7) -0.017(8) 0.015(6) -0.020(10) C28 0.059(9) 0.196(17) 0.037(8) 0.040(9) -0.009(6) -0.025(10) C29 0.094(11) 0.139(13) 0.058(9) 0.018(8) -0.001(7) -0.053(9) C30 0.072(9) 0.103(10) 0.045(7) 0.003(7) -0.015(6) 0.012(7) C31 0.101(10) 0.086(10) 0.066(8) 0.013(7) -0.037(7) -0.022(9) C32 0.100(10) 0.174(14) 0.115(11) -0.023(10) -0.032(9) -0.021(11) C33 0.189(15) 0.046(9) 0.181(15) 0.048(9) -0.072(12) -0.001(10) C34 0.085(9) 0.095(10) 0.071(8) -0.020(7) -0.003(7) -0.010(9) C35 0.125(13) 0.094(10) 0.081(9) -0.019(7) -0.017(8) -0.008(9) C36 0.155(14) 0.114(11) 0.074(9) -0.009(8) 0.003(9) 0.004(11) Zn1A 0.0581(6) 0.0524(6) 0.0233(5) -0.0064(5) 0.0049(5) -0.0121(6) Cl1A 0.0666(17) 0.0822(19) 0.0360(14) 0.0071(13) -0.0059(12) -0.0104(15) Cl2A 0.0752(18) 0.0572(16) 0.0387(13) -0.0080(12) 0.0064(12) -0.0065(15) N1A 0.049(5) 0.058(5) 0.012(4) -0.012(3) 0.007(3) 0.006(4) N2A 0.044(4) 0.024(4) 0.035(4) -0.003(3) -0.007(3) -0.019(4) N3A 0.045(4) 0.035(4) 0.028(4) -0.002(3) -0.003(3) 0.000(4) N4A 0.042(5) 0.042(5) 0.044(5) 0.002(4) -0.012(4) -0.018(4) C1A 0.060(7) 0.046(7) 0.031(5) 0.001(5) -0.009(5) -0.024(5) C2A 0.102(10) 0.060(8) 0.043(7) 0.004(6) -0.004(7) -0.021(7) C3A 0.141(12) 0.075(9) 0.032(7) 0.021(6) -0.007(7) -0.034(9) C4A 0.117(12) 0.097(11) 0.025(6) -0.011(7) 0.012(7) -0.030(9) C5A 0.084(9) 0.090(9) 0.031(6) -0.013(6) 0.019(6) -0.040(8) C6A 0.049(7) 0.093(9) 0.048(7) 0.000(6) 0.012(5) -0.021(7) C7A 0.055(7) 0.071(8) 0.068(7) 0.014(6) 0.010(6) 0.020(6) C8A 0.070(8) 0.072(7) 0.081(8) -0.034(6) -0.031(6) 0.008(6) C9A 0.109(10) 0.089(10) 0.121(11) -0.054(8) 0.008(8) -0.004(8) C10A 0.079(8) 0.061(7) 0.038(6) 0.009(5) 0.002(6) -0.017(7) C11A 0.140(13) 0.098(11) 0.117(11) -0.034(8) -0.036(9) -0.022(10) C12A 0.098(10) 0.099(10) 0.080(9) -0.013(7) -0.029(8) 0.033(8) C13A 0.025(5) 0.055(7) 0.062(7) 0.018(5) 0.004(5) 0.004(5) C14A 0.061(6) 0.031(5) 0.020(5) -0.004(4) -0.007(4) 0.002(5) C15A 0.086(8) 0.031(6) 0.036(6) -0.016(4) -0.004(5) -0.040(5) C16A 0.091(8) 0.059(7) 0.026(5) -0.003(5) -0.002(5) -0.021(7) C17A 0.071(7) 0.049(6) 0.027(5) -0.008(4) 0.009(5) -0.011(6) C18A 0.029(5) 0.023(5) 0.043(5) 0.002(4) 0.016(4) 0.001(4) C19A 0.039(5) 0.042(6) 0.032(5) -0.001(4) 0.021(4) -0.015(4) C20A 0.068(7) 0.057(7) 0.050(6) 0.007(5) 0.003(6) 0.017(6) C21A 0.097(9) 0.076(8) 0.038(7) 0.008(6) 0.017(6) -0.022(7) C22A 0.061(7) 0.058(7) 0.047(6) -0.006(5) -0.002(5) -0.027(6) C23A 0.072(7) 0.018(5) 0.033(5) 0.007(4) 0.005(5) 0.008(5) C25A 0.051(6) 0.042(6) 0.031(5) 0.000(4) -0.001(4) -0.013(5) C26A 0.050(7) 0.076(8) 0.032(6) 0.002(5) 0.004(5) 0.004(6) C27A 0.068(8) 0.086(8) 0.057(7) -0.014(6) 0.013(6) 0.007(7) C28A 0.097(9) 0.094(10) 0.026(6) -0.007(6) -0.003(6) -0.017(8) C29A 0.076(8) 0.086(9) 0.040(7) 0.001(6) -0.004(6) -0.026(7) C30A 0.046(6) 0.039(6) 0.039(6) -0.001(5) 0.001(5) -0.012(5) C31A 0.054(7) 0.079(9) 0.055(7) 0.020(6) -0.008(5) -0.006(7) C32A 0.096(11) 0.073(10) 0.191(15) 0.009(9) 0.041(10) 0.020(8) C33A 0.141(13) 0.151(14) 0.124(12) 0.068(11) 0.021(10) -0.021(11) C34A 0.124(11) 0.062(8) 0.040(6) -0.001(5) 0.000(7) 0.027(8) C35A 0.116(10) 0.069(8) 0.090(9) -0.011(6) -0.051(8) 0.031(8) C36A 0.103(9) 0.058(8) 0.103(9) -0.004(6) 0.012(8) 0.018(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N2 2.064(6) . ? Zn1 N3 2.216(7) . ? Zn1 Cl1 2.226(3) . ? Zn1 Cl2 2.226(3) . ? Zn1 N1 2.237(7) . ? N1 C13 1.248(9) . ? N1 C1 1.519(10) . ? N2 C18 1.332(9) . ? N2 C14 1.350(9) . ? N3 C23 1.334(10) . ? N3 C19 1.366(9) . ? N4 C24 1.232(10) . ? N4 C25 1.429(11) . ? C1 C2 1.346(12) . ? C1 C6 1.449(13) . ? C2 C3 1.411(12) . ? C2 C10 1.525(13) . ? C3 C4 1.396(15) . ? C3 H3 0.9500 . ? C4 C5 1.349(16) . ? C4 H4 0.9500 . ? C5 C6 1.430(12) . ? C5 H5 0.9500 . ? C6 C7 1.506(12) . ? C7 C9 1.510(11) . ? C7 C8 1.510(11) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.510(13) . ? C10 C12 1.559(14) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.490(10) . ? C13 H13 0.9500 . ? C14 C15 1.421(10) . ? C15 C16 1.382(10) . ? C15 H15 0.9500 . ? C16 C17 1.315(10) . ? C16 H16 0.9500 . ? C17 C18 1.440(9) . ? C17 H17 0.9500 . ? C18 C19 1.401(11) . ? C19 C20 1.415(11) . ? C20 C21 1.357(11) . ? C20 H20 0.9500 . ? C21 C22 1.386(11) . ? C21 H21 0.9500 . ? C22 C23 1.428(11) . ? C22 H22 0.9500 . ? C23 C24 1.500(11) . ? C24 H24 0.9500 . ? C25 C26 1.367(14) . ? C25 C30 1.381(14) . ? C26 C27 1.461(13) . ? C26 C34 1.491(14) . ? C27 C28 1.360(16) . ? C27 H27 0.9500 . ? C28 C29 1.355(16) . ? C28 H28 0.9500 . ? C29 C30 1.404(13) . ? C29 H29 0.9500 . ? C30 C31 1.489(14) . ? C31 C33 1.442(13) . ? C31 C32 1.551(14) . ? C31 H31 1.0000 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C36 1.542(13) . ? C34 C35 1.579(14) . ? C34 H34 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? Zn1A N2A 2.065(6) . ? Zn1A N3A 2.225(6) . ? Zn1A N1A 2.228(7) . ? Zn1A Cl2A 2.238(3) . ? Zn1A Cl1A 2.247(2) . ? N1A C13A 1.267(10) . ? N1A C1A 1.474(10) . ? N2A C14A 1.300(9) . ? N2A C18A 1.343(8) . ? N3A C23A 1.323(10) . ? N3A C19A 1.365(9) . ? N4A C24A 1.243(9) . ? N4A C25A 1.446(10) . ? C1A C2A 1.392(13) . ? C1A C6A 1.409(13) . ? C2A C3A 1.425(12) . ? C2A C10A 1.517(14) . ? C3A C4A 1.363(14) . ? C3A H3A 0.9500 . ? C4A C5A 1.368(14) . ? C4A H4A 0.9500 . ? C5A C6A 1.389(12) . ? C5A H5A 0.9500 . ? C6A C7A 1.465(13) . ? C7A C8A 1.468(12) . ? C7A C9A 1.593(12) . ? C7A H7A 1.0000 . ? C8A H8A1 0.9800 . ? C8A H8A2 0.9800 . ? C8A H8A3 0.9800 . ? C9A H9A1 0.9800 . ? C9A H9A2 0.9800 . ? C9A H9A3 0.9800 . ? C10A C11A 1.488(12) . ? C10A C12A 1.498(13) . ? C10A H10A 1.0000 . ? C11A H11D 0.9800 . ? C11A H11E 0.9800 . ? C11A H11F 0.9800 . ? C12A H12D 0.9800 . ? C12A H12E 0.9800 . ? C12A H12F 0.9800 . ? C13A C14A 1.487(11) . ? C13A H13A 0.9500 . ? C14A C15A 1.407(10) . ? C15A C16A 1.392(11) . ? C15A H15A 0.9500 . ? C16A C17A 1.329(11) . ? C16A H16A 0.9500 . ? C17A C18A 1.401(10) . ? C17A H17A 0.9500 . ? C18A C19A 1.445(10) . ? C19A C20A 1.385(11) . ? C20A C21A 1.376(12) . ? C20A H20A 0.9500 . ? C21A C22A 1.433(11) . ? C21A H21A 0.9500 . ? C22A C23A 1.405(11) . ? C22A H22A 0.9500 . ? C23A C24A 1.522(10) . ? C24A H24A 0.9500 . ? C25A C26A 1.378(11) . ? C25A C30A 1.397(11) . ? C26A C27A 1.454(11) . ? C26A C34A 1.515(12) . ? C27A C28A 1.378(12) . ? C27A H27A 0.9500 . ? C28A C29A 1.346(13) . ? C28A H28A 0.9500 . ? C29A C30A 1.421(12) . ? C29A H29A 0.9500 . ? C30A C31A 1.519(12) . ? C31A C33A 1.459(13) . ? C31A C32A 1.461(13) . ? C31A H31A 1.0000 . ? C32A H32D 0.9800 . ? C32A H32E 0.9800 . ? C32A H32F 0.9800 . ? C33A H33D 0.9800 . ? C33A H33E 0.9800 . ? C33A H33F 0.9800 . ? C34A C36A 1.523(12) . ? C34A C35A 1.541(14) . ? C34A H34A 1.0000 . ? C35A H35D 0.9800 . ? C35A H35E 0.9800 . ? C35A H35F 0.9800 . ? C36A H36D 0.9800 . ? C36A H36E 0.9800 . ? C36A H36F 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 N2 Zn1 N3 74.3(2) . . ? N2 Zn1 Cl1 117.0(2) . . ? N3 Zn1 Cl1 99.65(19) . . ? N2 Zn1 Cl2 122.3(2) . . ? N3 Zn1 Cl2 93.4(2) . . ? Cl1 Zn1 Cl2 120.56(11) . . ? N2 Zn1 N1 74.5(3) . . ? N3 Zn1 N1 148.8(2) . . ? Cl1 Zn1 N1 96.10(19) . . ? Cl2 Zn1 N1 101.5(2) . . ? C13 N1 C1 120.6(7) . . ? C13 N1 Zn1 116.2(6) . . ? C1 N1 Zn1 122.4(5) . . ? C18 N2 C14 122.0(7) . . ? C18 N2 Zn1 120.1(6) . . ? C14 N2 Zn1 117.9(5) . . ? C23 N3 C19 119.7(8) . . ? C23 N3 Zn1 126.0(6) . . ? C19 N3 Zn1 112.4(6) . . ? C24 N4 C25 118.0(9) . . ? C2 C1 C6 124.5(9) . . ? C2 C1 N1 120.6(9) . . ? C6 C1 N1 114.7(9) . . ? C1 C2 C3 118.9(10) . . ? C1 C2 C10 122.6(9) . . ? C3 C2 C10 118.5(10) . . ? C4 C3 C2 117.9(12) . . ? C4 C3 H3 121.1 . . ? C2 C3 H3 121.1 . . ? C5 C4 C3 123.7(12) . . ? C5 C4 H4 118.1 . . ? C3 C4 H4 118.1 . . ? C4 C5 C6 120.5(12) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C5 C6 C1 114.3(10) . . ? C5 C6 C7 122.5(10) . . ? C1 C6 C7 123.1(9) . . ? C6 C7 C9 112.2(9) . . ? C6 C7 C8 111.0(8) . . ? C9 C7 C8 109.3(8) . . ? C6 C7 H7 108.1 . . ? C9 C7 H7 108.1 . . ? C8 C7 H7 108.1 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C2 109.8(10) . . ? C11 C10 C12 107.1(10) . . ? C2 C10 C12 115.0(9) . . ? C11 C10 H10 108.2 . . ? C2 C10 H10 108.2 . . ? C12 C10 H10 108.2 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 C14 114.9(7) . . ? N1 C13 H13 122.5 . . ? C14 C13 H13 122.5 . . ? N2 C14 C15 120.1(7) . . ? N2 C14 C13 115.8(7) . . ? C15 C14 C13 123.8(7) . . ? C16 C15 C14 117.2(7) . . ? C16 C15 H15 121.4 . . ? C14 C15 H15 121.4 . . ? C17 C16 C15 121.9(8) . . ? C17 C16 H16 119.0 . . ? C15 C16 H16 119.0 . . ? C16 C17 C18 120.4(8) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? N2 C18 C19 115.4(7) . . ? N2 C18 C17 117.9(8) . . ? C19 C18 C17 126.5(8) . . ? N3 C19 C18 116.1(8) . . ? N3 C19 C20 118.9(9) . . ? C18 C19 C20 124.9(8) . . ? C21 C20 C19 120.8(9) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C20 C21 C22 120.9(9) . . ? C20 C21 H21 119.5 . . ? C22 C21 H21 119.5 . . ? C21 C22 C23 116.0(9) . . ? C21 C22 H22 122.0 . . ? C23 C22 H22 122.0 . . ? N3 C23 C22 123.3(8) . . ? N3 C23 C24 118.2(9) . . ? C22 C23 C24 118.4(9) . . ? N4 C24 C23 125.6(9) . . ? N4 C24 H24 117.2 . . ? C23 C24 H24 117.2 . . ? C26 C25 C30 125.5(11) . . ? C26 C25 N4 113.5(11) . . ? C30 C25 N4 120.6(11) . . ? C25 C26 C27 116.1(11) . . ? C25 C26 C34 122.4(11) . . ? C27 C26 C34 121.5(11) . . ? C28 C27 C26 118.8(12) . . ? C28 C27 H27 120.6 . . ? C26 C27 H27 120.6 . . ? C29 C28 C27 121.6(13) . . ? C29 C28 H28 119.2 . . ? C27 C28 H28 119.2 . . ? C28 C29 C30 122.6(14) . . ? C28 C29 H29 118.7 . . ? C30 C29 H29 118.7 . . ? C25 C30 C29 114.9(12) . . ? C25 C30 C31 126.8(11) . . ? C29 C30 C31 118.3(11) . . ? C33 C31 C30 118.1(12) . . ? C33 C31 C32 105.7(11) . . ? C30 C31 C32 112.0(10) . . ? C33 C31 H31 106.8 . . ? C30 C31 H31 106.8 . . ? C32 C31 H31 106.8 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C26 C34 C36 114.3(10) . . ? C26 C34 C35 110.5(10) . . ? C36 C34 C35 107.4(11) . . ? C26 C34 H34 108.2 . . ? C36 C34 H34 108.2 . . ? C35 C34 H34 108.2 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N2A Zn1A N3A 75.2(2) . . ? N2A Zn1A N1A 74.4(2) . . ? N3A Zn1A N1A 149.0(2) . . ? N2A Zn1A Cl2A 119.02(19) . . ? N3A Zn1A Cl2A 95.98(18) . . ? N1A Zn1A Cl2A 104.00(18) . . ? N2A Zn1A Cl1A 121.5(2) . . ? N3A Zn1A Cl1A 97.67(17) . . ? N1A Zn1A Cl1A 92.89(18) . . ? Cl2A Zn1A Cl1A 119.46(9) . . ? C13A N1A C1A 119.2(8) . . ? C13A N1A Zn1A 114.9(6) . . ? C1A N1A Zn1A 124.7(5) . . ? C14A N2A C18A 121.2(7) . . ? C14A N2A Zn1A 119.3(5) . . ? C18A N2A Zn1A 119.5(5) . . ? C23A N3A C19A 119.6(7) . . ? C23A N3A Zn1A 126.8(5) . . ? C19A N3A Zn1A 113.6(5) . . ? C24A N4A C25A 115.3(7) . . ? C2A C1A C6A 124.1(10) . . ? C2A C1A N1A 118.1(9) . . ? C6A C1A N1A 117.4(9) . . ? C1A C2A C3A 117.8(11) . . ? C1A C2A C10A 125.1(9) . . ? C3A C2A C10A 117.1(11) . . ? C4A C3A C2A 117.6(12) . . ? C4A C3A H3A 121.2 . . ? C2A C3A H3A 121.2 . . ? C3A C4A C5A 123.8(11) . . ? C3A C4A H4A 118.1 . . ? C5A C4A H4A 118.1 . . ? C4A C5A C6A 121.3(11) . . ? C4A C5A H5A 119.4 . . ? C6A C5A H5A 119.4 . . ? C5A C6A C1A 115.3(11) . . ? C5A C6A C7A 122.2(10) . . ? C1A C6A C7A 122.2(9) . . ? C6A C7A C8A 113.2(9) . . ? C6A C7A C9A 111.2(9) . . ? C8A C7A C9A 111.0(8) . . ? C6A C7A H7A 107.0 . . ? C8A C7A H7A 107.0 . . ? C9A C7A H7A 107.0 . . ? C7A C8A H8A1 109.5 . . ? C7A C8A H8A2 109.5 . . ? H8A1 C8A H8A2 109.5 . . ? C7A C8A H8A3 109.5 . . ? H8A1 C8A H8A3 109.5 . . ? H8A2 C8A H8A3 109.5 . . ? C7A C9A H9A1 109.5 . . ? C7A C9A H9A2 109.5 . . ? H9A1 C9A H9A2 109.5 . . ? C7A C9A H9A3 109.5 . . ? H9A1 C9A H9A3 109.5 . . ? H9A2 C9A H9A3 109.5 . . ? C11A C10A C12A 109.1(9) . . ? C11A C10A C2A 110.8(9) . . ? C12A C10A C2A 110.7(8) . . ? C11A C10A H10A 108.7 . . ? C12A C10A H10A 108.7 . . ? C2A C10A H10A 108.7 . . ? C10A C11A H11D 109.5 . . ? C10A C11A H11E 109.5 . . ? H11D C11A H11E 109.5 . . ? C10A C11A H11F 109.5 . . ? H11D C11A H11F 109.5 . . ? H11E C11A H11F 109.5 . . ? C10A C12A H12D 109.5 . . ? C10A C12A H12E 109.5 . . ? H12D C12A H12E 109.5 . . ? C10A C12A H12F 109.5 . . ? H12D C12A H12F 109.5 . . ? H12E C12A H12F 109.5 . . ? N1A C13A C14A 115.6(8) . . ? N1A C13A H13A 122.2 . . ? C14A C13A H13A 122.2 . . ? N2A C14A C15A 121.8(8) . . ? N2A C14A C13A 115.6(7) . . ? C15A C14A C13A 122.4(8) . . ? C16A C15A C14A 116.9(8) . . ? C16A C15A H15A 121.6 . . ? C14A C15A H15A 121.6 . . ? C17A C16A C15A 120.8(8) . . ? C17A C16A H16A 119.6 . . ? C15A C16A H16A 119.6 . . ? C16A C17A C18A 119.8(8) . . ? C16A C17A H17A 120.1 . . ? C18A C17A H17A 120.1 . . ? N2A C18A C17A 119.6(8) . . ? N2A C18A C19A 116.2(7) . . ? C17A C18A C19A 124.1(7) . . ? N3A C19A C20A 119.6(8) . . ? N3A C19A C18A 115.3(7) . . ? C20A C19A C18A 125.1(8) . . ? C21A C20A C19A 122.9(9) . . ? C21A C20A H20A 118.6 . . ? C19A C20A H20A 118.6 . . ? C20A C21A C22A 116.5(9) . . ? C20A C21A H21A 121.7 . . ? C22A C21A H21A 121.7 . . ? C23A C22A C21A 117.9(9) . . ? C23A C22A H22A 121.1 . . ? C21A C22A H22A 121.1 . . ? N3A C23A C22A 123.4(8) . . ? N3A C23A C24A 117.0(8) . . ? C22A C23A C24A 119.3(8) . . ? N4A C24A C23A 121.3(8) . . ? N4A C24A H24A 119.3 . . ? C23A C24A H24A 119.3 . . ? C26A C25A C30A 122.7(8) . . ? C26A C25A N4A 117.2(8) . . ? C30A C25A N4A 120.0(8) . . ? C25A C26A C27A 117.7(8) . . ? C25A C26A C34A 122.0(8) . . ? C27A C26A C34A 120.0(9) . . ? C28A C27A C26A 119.9(10) . . ? C28A C27A H27A 120.0 . . ? C26A C27A H27A 120.0 . . ? C29A C28A C27A 119.9(10) . . ? C29A C28A H28A 120.1 . . ? C27A C28A H28A 120.1 . . ? C28A C29A C30A 123.3(10) . . ? C28A C29A H29A 118.4 . . ? C30A C29A H29A 118.4 . . ? C25A C30A C29A 116.4(9) . . ? C25A C30A C31A 122.0(8) . . ? C29A C30A C31A 121.5(9) . . ? C33A C31A C32A 107.9(10) . . ? C33A C31A C30A 116.8(9) . . ? C32A C31A C30A 110.5(9) . . ? C33A C31A H31A 107.1 . . ? C32A C31A H31A 107.1 . . ? C30A C31A H31A 107.1 . . ? C31A C32A H32D 109.5 . . ? C31A C32A H32E 109.5 . . ? H32D C32A H32E 109.5 . . ? C31A C32A H32F 109.5 . . ? H32D C32A H32F 109.5 . . ? H32E C32A H32F 109.5 . . ? C31A C33A H33D 109.5 . . ? C31A C33A H33E 109.5 . . ? H33D C33A H33E 109.5 . . ? C31A C33A H33F 109.5 . . ? H33D C33A H33F 109.5 . . ? H33E C33A H33F 109.5 . . ? C26A C34A C36A 114.9(9) . . ? C26A C34A C35A 109.5(9) . . ? C36A C34A C35A 110.7(9) . . ? C26A C34A H34A 107.1 . . ? C36A C34A H34A 107.1 . . ? C35A C34A H34A 107.1 . . ? C34A C35A H35D 109.5 . . ? C34A C35A H35E 109.5 . . ? H35D C35A H35E 109.5 . . ? C34A C35A H35F 109.5 . . ? H35D C35A H35F 109.5 . . ? H35E C35A H35F 109.5 . . ? C34A C36A H36D 109.5 . . ? C34A C36A H36E 109.5 . . ? H36D C36A H36E 109.5 . . ? C34A C36A H36F 109.5 . . ? H36D C36A H36F 109.5 . . ? H36E C36A H36F 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 N2 Zn1 N1 C13 -7.7(6) . . . . ? N3 Zn1 N1 C13 -11.4(9) . . . . ? Cl1 Zn1 N1 C13 108.7(6) . . . . ? Cl2 Zn1 N1 C13 -128.4(6) . . . . ? N2 Zn1 N1 C1 -177.6(8) . . . . ? N3 Zn1 N1 C1 178.7(7) . . . . ? Cl1 Zn1 N1 C1 -61.2(7) . . . . ? Cl2 Zn1 N1 C1 61.7(7) . . . . ? N3 Zn1 N2 C18 2.4(6) . . . . ? Cl1 Zn1 N2 C18 95.4(6) . . . . ? Cl2 Zn1 N2 C18 -81.6(7) . . . . ? N1 Zn1 N2 C18 -175.6(7) . . . . ? N3 Zn1 N2 C14 -177.1(6) . . . . ? Cl1 Zn1 N2 C14 -84.1(6) . . . . ? Cl2 Zn1 N2 C14 98.9(6) . . . . ? N1 Zn1 N2 C14 4.9(6) . . . . ? N2 Zn1 N3 C23 -173.3(8) . . . . ? Cl1 Zn1 N3 C23 71.2(7) . . . . ? Cl2 Zn1 N3 C23 -50.6(7) . . . . ? N1 Zn1 N3 C23 -169.6(6) . . . . ? N2 Zn1 N3 C19 -8.9(6) . . . . ? Cl1 Zn1 N3 C19 -124.4(6) . . . . ? Cl2 Zn1 N3 C19 113.8(6) . . . . ? N1 Zn1 N3 C19 -5.2(9) . . . . ? C13 N1 C1 C2 -76.2(12) . . . . ? Zn1 N1 C1 C2 93.3(10) . . . . ? C13 N1 C1 C6 109.0(9) . . . . ? Zn1 N1 C1 C6 -81.5(9) . . . . ? C6 C1 C2 C3 5.3(16) . . . . ? N1 C1 C2 C3 -168.9(9) . . . . ? C6 C1 C2 C10 -174.3(9) . . . . ? N1 C1 C2 C10 11.5(15) . . . . ? C1 C2 C3 C4 -2.0(17) . . . . ? C10 C2 C3 C4 177.6(10) . . . . ? C2 C3 C4 C5 -1.2(19) . . . . ? C3 C4 C5 C6 1.2(19) . . . . ? C4 C5 C6 C1 1.7(15) . . . . ? C4 C5 C6 C7 -174.6(10) . . . . ? C2 C1 C6 C5 -5.1(15) . . . . ? N1 C1 C6 C5 169.4(8) . . . . ? C2 C1 C6 C7 171.2(9) . . . . ? N1 C1 C6 C7 -14.3(13) . . . . ? C5 C6 C7 C9 -29.8(13) . . . . ? C1 C6 C7 C9 154.2(9) . . . . ? C5 C6 C7 C8 92.8(11) . . . . ? C1 C6 C7 C8 -83.2(11) . . . . ? C1 C2 C10 C11 102.7(12) . . . . ? C3 C2 C10 C11 -76.9(13) . . . . ? C1 C2 C10 C12 -136.4(11) . . . . ? C3 C2 C10 C12 44.0(14) . . . . ? C1 N1 C13 C14 178.8(8) . . . . ? Zn1 N1 C13 C14 8.7(9) . . . . ? C18 N2 C14 C15 -7.7(12) . . . . ? Zn1 N2 C14 C15 171.8(6) . . . . ? C18 N2 C14 C13 178.2(7) . . . . ? Zn1 N2 C14 C13 -2.3(9) . . . . ? N1 C13 C14 N2 -4.6(11) . . . . ? N1 C13 C14 C15 -178.4(8) . . . . ? N2 C14 C15 C16 3.3(12) . . . . ? C13 C14 C15 C16 177.0(8) . . . . ? C14 C15 C16 C17 -0.5(13) . . . . ? C15 C16 C17 C18 1.7(13) . . . . ? C14 N2 C18 C19 -176.1(8) . . . . ? Zn1 N2 C18 C19 4.4(11) . . . . ? C14 N2 C18 C17 8.7(12) . . . . ? Zn1 N2 C18 C17 -170.8(6) . . . . ? C16 C17 C18 N2 -5.6(13) . . . . ? C16 C17 C18 C19 179.7(9) . . . . ? C23 N3 C19 C18 179.8(8) . . . . ? Zn1 N3 C19 C18 14.3(10) . . . . ? C23 N3 C19 C20 0.7(13) . . . . ? Zn1 N3 C19 C20 -164.8(7) . . . . ? N2 C18 C19 N3 -12.7(12) . . . . ? C17 C18 C19 N3 162.0(8) . . . . ? N2 C18 C19 C20 166.2(8) . . . . ? C17 C18 C19 C20 -19.0(15) . . . . ? N3 C19 C20 C21 -4.9(14) . . . . ? C18 C19 C20 C21 176.2(9) . . . . ? C19 C20 C21 C22 4.0(16) . . . . ? C20 C21 C22 C23 0.8(16) . . . . ? C19 N3 C23 C22 4.3(14) . . . . ? Zn1 N3 C23 C22 167.7(8) . . . . ? C19 N3 C23 C24 -171.7(8) . . . . ? Zn1 N3 C23 C24 -8.3(12) . . . . ? C21 C22 C23 N3 -5.1(16) . . . . ? C21 C22 C23 C24 170.9(9) . . . . ? C25 N4 C24 C23 -168.9(10) . . . . ? N3 C23 C24 N4 176.3(10) . . . . ? C22 C23 C24 N4 0.0(16) . . . . ? C24 N4 C25 C26 109.0(12) . . . . ? C24 N4 C25 C30 -77.6(13) . . . . ? C30 C25 C26 C27 8.6(17) . . . . ? N4 C25 C26 C27 -178.4(9) . . . . ? C30 C25 C26 C34 -172.9(11) . . . . ? N4 C25 C26 C34 0.0(15) . . . . ? C25 C26 C27 C28 -4.1(17) . . . . ? C34 C26 C27 C28 177.5(11) . . . . ? C26 C27 C28 C29 0(2) . . . . ? C27 C28 C29 C30 0(2) . . . . ? C26 C25 C30 C29 -8.6(17) . . . . ? N4 C25 C30 C29 178.9(9) . . . . ? C26 C25 C30 C31 173.1(11) . . . . ? N4 C25 C30 C31 0.6(18) . . . . ? C28 C29 C30 C25 4.2(17) . . . . ? C28 C29 C30 C31 -177.4(12) . . . . ? C25 C30 C31 C33 120.1(13) . . . . ? C29 C30 C31 C33 -58.1(15) . . . . ? C25 C30 C31 C32 -116.7(13) . . . . ? C29 C30 C31 C32 65.1(14) . . . . ? C25 C26 C34 C36 135.0(12) . . . . ? C27 C26 C34 C36 -46.7(15) . . . . ? C25 C26 C34 C35 -103.8(12) . . . . ? C27 C26 C34 C35 74.5(13) . . . . ? N2A Zn1A N1A C13A 1.0(6) . . . . ? N3A Zn1A N1A C13A -10.9(9) . . . . ? Cl2A Zn1A N1A C13A 117.7(6) . . . . ? Cl1A Zn1A N1A C13A -121.0(6) . . . . ? N2A Zn1A N1A C1A 168.3(7) . . . . ? N3A Zn1A N1A C1A 156.5(6) . . . . ? Cl2A Zn1A N1A C1A -75.0(7) . . . . ? Cl1A Zn1A N1A C1A 46.4(7) . . . . ? N3A Zn1A N2A C14A 176.1(6) . . . . ? N1A Zn1A N2A C14A 2.4(6) . . . . ? Cl2A Zn1A N2A C14A -95.2(6) . . . . ? Cl1A Zn1A N2A C14A 86.1(6) . . . . ? N3A Zn1A N2A C18A -3.0(6) . . . . ? N1A Zn1A N2A C18A -176.7(6) . . . . ? Cl2A Zn1A N2A C18A 85.7(6) . . . . ? Cl1A Zn1A N2A C18A -93.1(6) . . . . ? N2A Zn1A N3A C23A -175.9(7) . . . . ? N1A Zn1A N3A C23A -164.1(6) . . . . ? Cl2A Zn1A N3A C23A 65.6(6) . . . . ? Cl1A Zn1A N3A C23A -55.3(6) . . . . ? N2A Zn1A N3A C19A 2.7(5) . . . . ? N1A Zn1A N3A C19A 14.5(8) . . . . ? Cl2A Zn1A N3A C19A -115.8(5) . . . . ? Cl1A Zn1A N3A C19A 123.4(5) . . . . ? C13A N1A C1A C2A 71.0(11) . . . . ? Zn1A N1A C1A C2A -95.8(9) . . . . ? C13A N1A C1A C6A -115.7(9) . . . . ? Zn1A N1A C1A C6A 77.5(9) . . . . ? C6A C1A C2A C3A -1.9(15) . . . . ? N1A C1A C2A C3A 170.9(8) . . . . ? C6A C1A C2A C10A 175.2(9) . . . . ? N1A C1A C2A C10A -12.0(14) . . . . ? C1A C2A C3A C4A -0.9(15) . . . . ? C10A C2A C3A C4A -178.3(10) . . . . ? C2A C3A C4A C5A 0.8(17) . . . . ? C3A C4A C5A C6A 2.1(18) . . . . ? C4A C5A C6A C1A -4.6(15) . . . . ? C4A C5A C6A C7A 170.1(10) . . . . ? C2A C1A C6A C5A 4.6(14) . . . . ? N1A C1A C6A C5A -168.3(8) . . . . ? C2A C1A C6A C7A -170.1(9) . . . . ? N1A C1A C6A C7A 17.1(13) . . . . ? C5A C6A C7A C8A -89.3(12) . . . . ? C1A C6A C7A C8A 85.0(12) . . . . ? C5A C6A C7A C9A 36.5(13) . . . . ? C1A C6A C7A C9A -149.2(9) . . . . ? C1A C2A C10A C11A -106.7(11) . . . . ? C3A C2A C10A C11A 70.4(12) . . . . ? C1A C2A C10A C12A 132.1(10) . . . . ? C3A C2A C10A C12A -50.8(13) . . . . ? C1A N1A C13A C14A -171.8(7) . . . . ? Zn1A N1A C13A C14A -3.7(10) . . . . ? C18A N2A C14A C15A -0.8(12) . . . . ? Zn1A N2A C14A C15A -179.9(7) . . . . ? C18A N2A C14A C13A 174.1(7) . . . . ? Zn1A N2A C14A C13A -5.1(9) . . . . ? N1A C13A C14A N2A 5.8(11) . . . . ? N1A C13A C14A C15A -179.4(8) . . . . ? N2A C14A C15A C16A 0.9(13) . . . . ? C13A C14A C15A C16A -173.6(8) . . . . ? C14A C15A C16A C17A 0.0(14) . . . . ? C15A C16A C17A C18A -0.9(15) . . . . ? C14A N2A C18A C17A -0.2(12) . . . . ? Zn1A N2A C18A C17A 179.0(6) . . . . ? C14A N2A C18A C19A -176.3(7) . . . . ? Zn1A N2A C18A C19A 2.9(9) . . . . ? C16A C17A C18A N2A 1.1(13) . . . . ? C16A C17A C18A C19A 176.8(8) . . . . ? C23A N3A C19A C20A -2.3(11) . . . . ? Zn1A N3A C19A C20A 178.9(6) . . . . ? C23A N3A C19A C18A 176.6(7) . . . . ? Zn1A N3A C19A C18A -2.2(8) . . . . ? N2A C18A C19A N3A -0.3(10) . . . . ? C17A C18A C19A N3A -176.1(8) . . . . ? N2A C18A C19A C20A 178.6(8) . . . . ? C17A C18A C19A C20A 2.7(13) . . . . ? N3A C19A C20A C21A 3.4(13) . . . . ? C18A C19A C20A C21A -175.4(9) . . . . ? C19A C20A C21A C22A -3.4(14) . . . . ? C20A C21A C22A C23A 2.5(14) . . . . ? C19A N3A C23A C22A 1.7(12) . . . . ? Zn1A N3A C23A C22A -179.8(6) . . . . ? C19A N3A C23A C24A 176.8(6) . . . . ? Zn1A N3A C23A C24A -4.6(10) . . . . ? C21A C22A C23A N3A -1.8(14) . . . . ? C21A C22A C23A C24A -176.8(8) . . . . ? C25A N4A C24A C23A -177.5(7) . . . . ? N3A C23A C24A N4A 173.4(7) . . . . ? C22A C23A C24A N4A -11.2(12) . . . . ? C24A N4A C25A C26A -96.4(9) . . . . ? C24A N4A C25A C30A 85.9(10) . . . . ? C30A C25A C26A C27A 3.4(14) . . . . ? N4A C25A C26A C27A -174.3(8) . . . . ? C30A C25A C26A C34A 177.3(9) . . . . ? N4A C25A C26A C34A -0.3(13) . . . . ? C25A C26A C27A C28A -2.4(15) . . . . ? C34A C26A C27A C28A -176.5(10) . . . . ? C26A C27A C28A C29A -0.1(17) . . . . ? C27A C28A C29A C30A 1.9(17) . . . . ? C26A C25A C30A C29A -1.7(13) . . . . ? N4A C25A C30A C29A 175.8(8) . . . . ? C26A C25A C30A C31A -178.3(8) . . . . ? N4A C25A C30A C31A -0.7(12) . . . . ? C28A C29A C30A C25A -1.0(15) . . . . ? C28A C29A C30A C31A 175.5(10) . . . . ? C25A C30A C31A C33A -153.4(10) . . . . ? C29A C30A C31A C33A 30.3(14) . . . . ? C25A C30A C31A C32A 82.8(11) . . . . ? C29A C30A C31A C32A -93.6(11) . . . . ? C25A C26A C34A C36A -134.1(10) . . . . ? C27A C26A C34A C36A 39.7(14) . . . . ? C25A C26A C34A C35A 100.6(11) . . . . ? C27A C26A C34A C35A -85.6(11) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.577 _refine_diff_density_min -0.686 _refine_diff_density_rms 0.077 # Attachment '08028.cif' data_08028 _database_code_depnum_ccdc_archive 'CCDC 692758' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H44 Cl2 N4 Ni O' _chemical_formula_weight 678.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 13.5748(17) _cell_length_b 16.500(2) _cell_length_c 32.768(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7339.4(16) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1015 _cell_measurement_theta_min 2.307 _cell_measurement_theta_max 23.335 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.228 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2864 _exptl_absorpt_coefficient_mu 0.706 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.363 _exptl_absorpt_correction_T_max 0.928 _exptl_absorpt_process_details ; absorption correction based on 11338 reflections(SADABS);Rint 0.0694 before correction and 0.0675 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 57619 _diffrn_reflns_av_R_equivalents 0.1161 _diffrn_reflns_av_sigmaI/netI 0.1260 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.24 _diffrn_reflns_theta_max 26.00 _reflns_number_total 14424 _reflns_number_gt 9441 _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 ; Disordered H2O was omitted using the SQUEEZE option of PLATON.The solvent accessible voids are 812.4 \%A3 with an estimated 60e/cell to be added.Eight solvent H2O molecules/unit cell accounting for 64e were included in the formula, FWt, (000) and density calculations. PLATON Reference: Spek, A.L. (1990), Acta Cryst. A46, C-34. 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^)+(0.0265P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.046(13) _refine_ls_number_reflns 14424 _refine_ls_number_parameters 791 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0954 _refine_ls_R_factor_gt 0.0597 _refine_ls_wR_factor_ref 0.1053 _refine_ls_wR_factor_gt 0.0954 _refine_ls_goodness_of_fit_ref 0.883 _refine_ls_restrained_S_all 0.883 _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 0.67914(4) 0.96687(3) 0.126422(17) 0.03342(16) Uani 1 1 d . . . Cl1 Cl 0.57315(9) 1.06992(7) 0.11468(4) 0.0436(3) Uani 1 1 d . . . Cl2 Cl 0.80221(10) 0.91687(8) 0.08780(4) 0.0482(4) Uani 1 1 d . . . N1 N 0.5825(3) 0.8650(2) 0.11457(10) 0.0299(9) Uani 1 1 d . . . N2 N 0.6646(3) 0.9190(2) 0.18071(10) 0.0307(9) Uani 1 1 d . . . N3 N 0.7754(3) 1.0410(2) 0.16122(11) 0.0338(9) Uani 1 1 d . . . N4 N 0.8824(3) 1.1740(2) 0.08818(12) 0.0367(10) Uani 1 1 d . . . C1 C 0.5574(4) 0.8324(3) 0.07478(14) 0.0345(12) Uani 1 1 d . . . C2 C 0.6132(4) 0.7687(3) 0.05907(14) 0.0396(13) Uani 1 1 d . . . C3 C 0.5956(5) 0.7468(4) 0.01800(17) 0.0573(17) Uani 1 1 d . . . H3 H 0.6307 0.7028 0.0062 0.069 Uiso 1 1 calc R . . C4 C 0.5281(5) 0.7889(4) -0.00498(19) 0.070(2) Uani 1 1 d . . . H4 H 0.5206 0.7763 -0.0331 0.084 Uiso 1 1 calc R . . C5 C 0.4720(5) 0.8482(4) 0.01189(17) 0.0620(19) Uani 1 1 d . . . H5 H 0.4236 0.8743 -0.0045 0.074 Uiso 1 1 calc R . . C6 C 0.4831(4) 0.8721(3) 0.05281(15) 0.0414(14) Uani 1 1 d . . . C7 C 0.4132(4) 0.9300(3) 0.07258(16) 0.0533(15) Uani 1 1 d . . . H7 H 0.4489 0.9565 0.0957 0.064 Uiso 1 1 calc R . . C8 C 0.3251(4) 0.8843(3) 0.09065(17) 0.0704(18) Uani 1 1 d . . . H8A H 0.2908 0.8548 0.0689 0.106 Uiso 1 1 calc R . . H8B H 0.2797 0.9230 0.1033 0.106 Uiso 1 1 calc R . . H8C H 0.3484 0.8458 0.1113 0.106 Uiso 1 1 calc R . . C9 C 0.3755(4) 0.9979(3) 0.04415(18) 0.079(2) Uani 1 1 d . . . H9A H 0.4316 1.0286 0.0335 0.119 Uiso 1 1 calc R . . H9B H 0.3321 1.0343 0.0595 0.119 Uiso 1 1 calc R . . H9C H 0.3387 0.9738 0.0214 0.119 Uiso 1 1 calc R . . C10 C 0.6863(4) 0.7183(3) 0.08363(16) 0.0503(15) Uani 1 1 d . . . H10 H 0.6998 0.7478 0.1097 0.060 Uiso 1 1 calc R . . C11 C 0.7851(4) 0.7044(3) 0.06230(16) 0.0640(18) Uani 1 1 d . . . H11A H 0.7739 0.6776 0.0360 0.096 Uiso 1 1 calc R . . H11B H 0.8270 0.6700 0.0794 0.096 Uiso 1 1 calc R . . H11C H 0.8177 0.7566 0.0578 0.096 Uiso 1 1 calc R . . C12 C 0.6404(5) 0.6364(3) 0.09461(19) 0.079(2) Uani 1 1 d . . . H12A H 0.5781 0.6453 0.1091 0.118 Uiso 1 1 calc R . . H12B H 0.6857 0.6061 0.1122 0.118 Uiso 1 1 calc R . . H12C H 0.6279 0.6055 0.0696 0.118 Uiso 1 1 calc R . . C13 C 0.5653(3) 0.8243(3) 0.14688(13) 0.0297(11) Uani 1 1 d . . . H13 H 0.5261 0.7766 0.1461 0.036 Uiso 1 1 calc R . . C14 C 0.6081(3) 0.8537(3) 0.18544(13) 0.0300(12) Uani 1 1 d . . . C15 C 0.5981(3) 0.8163(3) 0.22314(14) 0.0349(12) Uani 1 1 d . . . H15 H 0.5581 0.7694 0.2263 0.042 Uiso 1 1 calc R . . C16 C 0.6479(4) 0.8492(3) 0.25602(14) 0.0401(14) Uani 1 1 d . . . H16 H 0.6414 0.8255 0.2823 0.048 Uiso 1 1 calc R . . C17 C 0.7065(3) 0.9156(3) 0.25083(13) 0.0375(13) Uani 1 1 d . . . H17 H 0.7421 0.9376 0.2732 0.045 Uiso 1 1 calc R . . C18 C 0.7135(3) 0.9506(3) 0.21245(13) 0.0277(10) Uani 1 1 d . . . C19 C 0.7775(3) 1.0200(3) 0.20144(13) 0.0303(11) Uani 1 1 d . . . C20 C 0.8363(3) 1.0614(3) 0.22934(14) 0.0374(12) Uani 1 1 d . . . H20 H 0.8356 1.0472 0.2574 0.045 Uiso 1 1 calc R . . C21 C 0.8952(4) 1.1228(3) 0.21552(16) 0.0476(15) Uani 1 1 d . . . H21 H 0.9362 1.1517 0.2340 0.057 Uiso 1 1 calc R . . C22 C 0.8949(4) 1.1427(3) 0.17456(16) 0.0433(14) Uani 1 1 d . . . H22 H 0.9368 1.1844 0.1646 0.052 Uiso 1 1 calc R . . C23 C 0.8329(3) 1.1014(3) 0.14803(14) 0.0326(12) Uani 1 1 d . . . C24 C 0.8254(4) 1.1223(3) 0.10445(14) 0.0385(13) Uani 1 1 d . . . H24 H 0.7768 1.0965 0.0881 0.046 Uiso 1 1 calc R . . C25 C 0.8666(4) 1.1916(3) 0.04593(15) 0.0370(13) Uani 1 1 d . . . C26 C 0.8148(4) 1.2639(3) 0.03678(15) 0.0445(14) Uani 1 1 d . . . C27 C 0.8059(4) 1.2847(3) -0.00446(16) 0.0540(15) Uani 1 1 d . . . H27 H 0.7726 1.3332 -0.0117 0.065 Uiso 1 1 calc R . . C28 C 0.8441(4) 1.2366(4) -0.03447(18) 0.0607(18) Uani 1 1 d . . . H28 H 0.8354 1.2514 -0.0623 0.073 Uiso 1 1 calc R . . C29 C 0.8947(4) 1.1673(4) -0.02503(17) 0.0519(16) Uani 1 1 d . . . H29 H 0.9218 1.1356 -0.0465 0.062 Uiso 1 1 calc R . . C30 C 0.9075(4) 1.1422(3) 0.01528(16) 0.0432(14) Uani 1 1 d . . . C31 C 0.9692(4) 1.0687(3) 0.02590(17) 0.0542(16) Uani 1 1 d . . . H31 H 0.9336 1.0370 0.0473 0.065 Uiso 1 1 calc R . . C32 C 1.0674(5) 1.0945(4) 0.04298(19) 0.084(2) Uani 1 1 d . . . H32A H 1.1058 1.1213 0.0216 0.126 Uiso 1 1 calc R . . H32B H 1.1032 1.0467 0.0528 0.126 Uiso 1 1 calc R . . H32C H 1.0569 1.1322 0.0657 0.126 Uiso 1 1 calc R . . C33 C 0.9901(5) 1.0126(4) -0.0099(2) 0.099(3) Uani 1 1 d . . . H33A H 0.9282 0.9994 -0.0237 0.148 Uiso 1 1 calc R . . H33B H 1.0208 0.9627 0.0001 0.148 Uiso 1 1 calc R . . H33C H 1.0347 1.0396 -0.0291 0.148 Uiso 1 1 calc R . . C34 C 0.7728(4) 1.3163(3) 0.07060(17) 0.0525(15) Uani 1 1 d . . . H34 H 0.8104 1.3037 0.0960 0.063 Uiso 1 1 calc R . . C35 C 0.6651(4) 1.2960(3) 0.07879(18) 0.0699(18) Uani 1 1 d . . . H35A H 0.6269 1.3030 0.0537 0.105 Uiso 1 1 calc R . . H35B H 0.6393 1.3322 0.0999 0.105 Uiso 1 1 calc R . . H35C H 0.6599 1.2397 0.0880 0.105 Uiso 1 1 calc R . . C36 C 0.7852(4) 1.4070(3) 0.06220(18) 0.0744(19) Uani 1 1 d . . . H36A H 0.7459 1.4222 0.0383 0.112 Uiso 1 1 calc R . . H36B H 0.8548 1.4189 0.0569 0.112 Uiso 1 1 calc R . . H36C H 0.7629 1.4381 0.0860 0.112 Uiso 1 1 calc R . . Ni1A Ni 0.20141(4) 0.45095(4) 0.122758(16) 0.03464(16) Uani 1 1 d . . . Cl1A Cl 0.34273(9) 0.38378(8) 0.13441(4) 0.0489(4) Uani 1 1 d . . . Cl2A Cl 0.12428(10) 0.54525(9) 0.16093(4) 0.0568(4) Uani 1 1 d . . . N1A N 0.1092(3) 0.3458(2) 0.13626(11) 0.0315(10) Uani 1 1 d . . . N2A N 0.1491(3) 0.4230(2) 0.06894(10) 0.0283(9) Uani 1 1 d . . . N3A N 0.2670(3) 0.5410(2) 0.08558(10) 0.0317(9) Uani 1 1 d . . . N4A N 0.4042(3) 0.6621(2) 0.15511(11) 0.0329(10) Uani 1 1 d . . . C1A C 0.1026(4) 0.3043(3) 0.17504(14) 0.0344(12) Uani 1 1 d . . . C2A C 0.0418(4) 0.3400(3) 0.20512(15) 0.0402(14) Uani 1 1 d . . . C3A C 0.0465(4) 0.3088(4) 0.24402(16) 0.0564(18) Uani 1 1 d . . . H3A H 0.0072 0.3325 0.2648 0.068 Uiso 1 1 calc R . . C4A C 0.1066(5) 0.2442(4) 0.25378(17) 0.0619(19) Uani 1 1 d . . . H4A H 0.1105 0.2252 0.2811 0.074 Uiso 1 1 calc R . . C5A C 0.1611(4) 0.2076(4) 0.22339(17) 0.0566(16) Uani 1 1 d . . . H5A H 0.1997 0.1613 0.2299 0.068 Uiso 1 1 calc R . . C6A C 0.1610(4) 0.2370(3) 0.18299(15) 0.0396(13) Uani 1 1 d . . . C7A C 0.2187(4) 0.1901(3) 0.15149(16) 0.0473(14) Uani 1 1 d . . . H7A H 0.2176 0.2216 0.1254 0.057 Uiso 1 1 calc R . . C8A C 0.1679(5) 0.1071(3) 0.14363(18) 0.078(2) Uani 1 1 d . . . H8A1 H 0.1683 0.0750 0.1688 0.117 Uiso 1 1 calc R . . H8A2 H 0.2037 0.0778 0.1223 0.117 Uiso 1 1 calc R . . H8A3 H 0.0998 0.1161 0.1349 0.117 Uiso 1 1 calc R . . C9A C 0.3255(4) 0.1740(3) 0.16264(17) 0.0645(17) Uani 1 1 d . . . H9A1 H 0.3602 0.2257 0.1661 0.097 Uiso 1 1 calc R . . H9A2 H 0.3570 0.1427 0.1408 0.097 Uiso 1 1 calc R . . H9A3 H 0.3284 0.1433 0.1882 0.097 Uiso 1 1 calc R . . C10A C -0.0334(4) 0.4038(3) 0.19369(16) 0.0452(14) Uani 1 1 d . . . H10A H -0.0056 0.4370 0.1709 0.054 Uiso 1 1 calc R . . C11A C -0.1281(4) 0.3635(3) 0.17841(16) 0.0572(16) Uani 1 1 d . . . H11D H -0.1127 0.3278 0.1554 0.086 Uiso 1 1 calc R . . H11E H -0.1747 0.4053 0.1695 0.086 Uiso 1 1 calc R . . H11F H -0.1575 0.3317 0.2005 0.086 Uiso 1 1 calc R . . C12A C -0.0608(4) 0.4608(4) 0.22820(17) 0.076(2) Uani 1 1 d . . . H12D H -0.0959 0.4306 0.2494 0.113 Uiso 1 1 calc R . . H12E H -0.1034 0.5040 0.2177 0.113 Uiso 1 1 calc R . . H12F H -0.0009 0.4847 0.2398 0.113 Uiso 1 1 calc R . . C13A C 0.0748(3) 0.3148(3) 0.10404(13) 0.0302(12) Uani 1 1 d . . . H13A H 0.0383 0.2657 0.1051 0.036 Uiso 1 1 calc R . . C14A C 0.0921(3) 0.3559(3) 0.06490(13) 0.0265(11) Uani 1 1 d . . . C15A C 0.0622(3) 0.3298(3) 0.02725(13) 0.0346(13) Uani 1 1 d . . . H15A H 0.0252 0.2813 0.0245 0.041 Uiso 1 1 calc R . . C16A C 0.0867(4) 0.3756(3) -0.00706(14) 0.0378(13) Uani 1 1 d . . . H16A H 0.0645 0.3594 -0.0333 0.045 Uiso 1 1 calc R . . C17A C 0.1435(3) 0.4444(3) -0.00268(13) 0.0309(11) Uani 1 1 d . . . H17A H 0.1616 0.4758 -0.0258 0.037 Uiso 1 1 calc R . . C18A C 0.1737(3) 0.4672(3) 0.03622(12) 0.0302(11) Uani 1 1 d . . . C19A C 0.2369(3) 0.5382(3) 0.04616(13) 0.0321(11) Uani 1 1 d . . . C20A C 0.2618(4) 0.5968(3) 0.01805(15) 0.0418(14) Uani 1 1 d . . . H20A H 0.2368 0.5948 -0.0090 0.050 Uiso 1 1 calc R . . C21A C 0.3236(4) 0.6581(3) 0.03010(14) 0.0462(14) Uani 1 1 d . . . H21A H 0.3422 0.6987 0.0111 0.055 Uiso 1 1 calc R . . C22A C 0.3590(3) 0.6613(3) 0.06960(14) 0.0390(13) Uani 1 1 d . . . H22A H 0.4028 0.7030 0.0780 0.047 Uiso 1 1 calc R . . C23A C 0.3281(3) 0.6011(3) 0.09685(13) 0.0317(12) Uani 1 1 d . . . C24A C 0.3548(3) 0.6049(3) 0.14046(14) 0.0338(12) Uani 1 1 d . . . H24A H 0.3337 0.5625 0.1580 0.041 Uiso 1 1 calc R . . C25A C 0.4145(4) 0.6629(3) 0.19865(14) 0.0388(13) Uani 1 1 d . . . C26A C 0.3582(4) 0.7213(4) 0.21951(15) 0.0461(15) Uani 1 1 d . . . C27A C 0.3651(4) 0.7229(4) 0.26174(17) 0.0575(17) Uani 1 1 d . . . H27A H 0.3286 0.7618 0.2768 0.069 Uiso 1 1 calc R . . C28A C 0.4251(4) 0.6682(4) 0.28215(16) 0.0626(19) Uani 1 1 d . . . H28A H 0.4266 0.6677 0.3111 0.075 Uiso 1 1 calc R . . C29A C 0.4816(4) 0.6152(4) 0.26065(17) 0.0567(17) Uani 1 1 d . . . H29A H 0.5241 0.5796 0.2752 0.068 Uiso 1 1 calc R . . C30A C 0.4797(4) 0.6110(3) 0.21854(15) 0.0420(14) Uani 1 1 d . . . C31A C 0.5521(4) 0.5569(3) 0.19579(16) 0.0518(15) Uani 1 1 d . . . H31A H 0.5410 0.5661 0.1660 0.062 Uiso 1 1 calc R . . C32A C 0.6598(4) 0.5798(4) 0.20466(18) 0.078(2) Uani 1 1 d . . . H32D H 0.6697 0.6375 0.1990 0.117 Uiso 1 1 calc R . . H32E H 0.7035 0.5476 0.1873 0.117 Uiso 1 1 calc R . . H32F H 0.6747 0.5688 0.2334 0.117 Uiso 1 1 calc R . . C33A C 0.5348(5) 0.4672(4) 0.20380(19) 0.084(2) Uani 1 1 d . . . H33D H 0.5421 0.4562 0.2330 0.126 Uiso 1 1 calc R . . H33E H 0.5829 0.4351 0.1884 0.126 Uiso 1 1 calc R . . H33F H 0.4680 0.4525 0.1951 0.126 Uiso 1 1 calc R . . C34A C 0.2938(4) 0.7813(3) 0.19648(15) 0.0467(14) Uani 1 1 d . . . H34A H 0.3120 0.7775 0.1670 0.056 Uiso 1 1 calc R . . C35A C 0.1851(4) 0.7590(3) 0.20001(17) 0.0665(18) Uani 1 1 d . . . H35D H 0.1635 0.7661 0.2283 0.100 Uiso 1 1 calc R . . H35E H 0.1759 0.7024 0.1918 0.100 Uiso 1 1 calc R . . H35F H 0.1462 0.7943 0.1821 0.100 Uiso 1 1 calc R . . C36A C 0.3106(4) 0.8689(3) 0.20970(17) 0.0683(18) Uani 1 1 d . . . H36D H 0.2966 0.8743 0.2389 0.102 Uiso 1 1 calc R . . H36E H 0.2669 0.9048 0.1942 0.102 Uiso 1 1 calc R . . H36F H 0.3793 0.8840 0.2045 0.102 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 Ni1 0.0395(4) 0.0365(4) 0.0243(3) 0.0037(3) -0.0033(3) -0.0108(3) Cl1 0.0456(8) 0.0416(8) 0.0436(8) -0.0009(6) -0.0096(6) -0.0038(6) Cl2 0.0485(9) 0.0540(8) 0.0422(7) -0.0066(7) 0.0073(7) -0.0125(7) N1 0.035(2) 0.035(2) 0.019(2) 0.0073(18) -0.0030(17) -0.007(2) N2 0.035(2) 0.034(2) 0.023(2) -0.0017(18) -0.0015(18) -0.007(2) N3 0.036(2) 0.033(2) 0.032(2) -0.001(2) -0.0039(18) -0.008(2) N4 0.035(3) 0.031(2) 0.044(3) 0.007(2) -0.001(2) -0.011(2) C1 0.038(3) 0.037(3) 0.029(3) 0.004(2) 0.001(2) -0.016(3) C2 0.044(3) 0.044(3) 0.030(3) -0.003(3) 0.010(2) -0.026(3) C3 0.067(4) 0.066(4) 0.039(4) -0.016(3) 0.009(3) -0.027(4) C4 0.079(5) 0.094(6) 0.036(4) -0.006(4) -0.003(4) -0.046(4) C5 0.063(4) 0.084(5) 0.039(4) 0.016(4) -0.010(3) -0.035(4) C6 0.046(3) 0.047(4) 0.031(3) 0.011(3) -0.006(3) -0.027(3) C7 0.058(4) 0.044(4) 0.058(4) 0.003(3) -0.021(3) -0.021(3) C8 0.072(5) 0.066(4) 0.074(4) 0.011(4) 0.010(4) 0.006(4) C9 0.055(4) 0.080(5) 0.103(5) 0.052(4) -0.016(4) -0.012(4) C10 0.059(4) 0.045(3) 0.047(3) -0.008(3) 0.019(3) -0.006(3) C11 0.059(4) 0.069(4) 0.064(4) -0.009(3) 0.022(3) -0.004(3) C12 0.083(5) 0.065(4) 0.088(5) 0.008(4) 0.035(4) -0.007(4) C13 0.027(3) 0.035(3) 0.027(3) 0.002(2) -0.003(2) -0.007(2) C14 0.034(3) 0.035(3) 0.021(3) -0.006(2) 0.002(2) -0.003(2) C15 0.036(3) 0.038(3) 0.031(3) 0.002(2) 0.001(2) -0.006(3) C16 0.050(3) 0.049(4) 0.021(3) 0.002(3) 0.007(2) -0.012(3) C17 0.036(3) 0.052(3) 0.025(3) -0.002(2) -0.005(2) 0.000(3) C18 0.024(3) 0.032(3) 0.027(2) -0.005(2) -0.0004(19) 0.001(2) C19 0.027(3) 0.031(3) 0.033(3) -0.002(2) -0.003(2) 0.003(2) C20 0.046(3) 0.033(3) 0.033(3) -0.005(2) -0.010(2) 0.000(3) C21 0.046(4) 0.046(4) 0.051(4) -0.003(3) -0.018(3) -0.011(3) C22 0.036(3) 0.035(3) 0.059(4) 0.004(3) -0.008(3) -0.015(3) C23 0.029(3) 0.028(3) 0.041(3) -0.003(2) -0.001(2) -0.009(2) C24 0.034(3) 0.043(3) 0.039(3) -0.008(3) -0.008(2) -0.004(3) C25 0.036(3) 0.041(3) 0.034(3) 0.006(3) -0.004(2) -0.014(3) C26 0.043(3) 0.052(4) 0.039(3) 0.003(3) -0.003(3) -0.018(3) C27 0.047(4) 0.063(4) 0.052(4) 0.018(3) -0.012(3) -0.005(3) C28 0.047(4) 0.091(5) 0.044(4) -0.001(4) -0.001(3) -0.015(4) C29 0.045(4) 0.068(4) 0.043(4) -0.014(3) 0.003(3) -0.014(3) C30 0.036(3) 0.048(4) 0.046(3) -0.003(3) 0.001(3) -0.016(3) C31 0.058(4) 0.049(4) 0.055(4) 0.002(3) 0.014(3) -0.012(3) C32 0.088(6) 0.072(5) 0.093(5) -0.009(4) -0.026(4) 0.012(4) C33 0.071(5) 0.081(5) 0.144(7) -0.057(5) 0.008(5) 0.001(4) C34 0.066(4) 0.044(4) 0.048(4) 0.007(3) -0.010(3) -0.002(3) C35 0.074(5) 0.061(4) 0.075(5) -0.001(3) 0.020(4) -0.002(4) C36 0.079(5) 0.058(4) 0.087(5) 0.001(4) -0.002(4) -0.003(4) Ni1A 0.0421(4) 0.0389(4) 0.0229(3) 0.0023(3) -0.0025(3) -0.0128(3) Cl1A 0.0434(8) 0.0629(9) 0.0404(8) 0.0123(7) -0.0052(6) -0.0050(7) Cl2A 0.0761(10) 0.0485(9) 0.0458(8) -0.0106(7) 0.0195(7) -0.0191(8) N1A 0.030(2) 0.041(2) 0.023(2) -0.0023(19) 0.0045(17) -0.005(2) N2A 0.030(2) 0.028(2) 0.027(2) -0.0007(18) -0.0030(17) -0.0030(18) N3A 0.039(2) 0.037(2) 0.019(2) 0.0042(19) -0.0019(17) -0.018(2) N4A 0.030(2) 0.035(3) 0.034(2) 0.000(2) -0.0040(19) -0.009(2) C1A 0.040(3) 0.037(3) 0.027(3) 0.002(2) -0.008(2) -0.014(3) C2A 0.037(3) 0.053(4) 0.031(3) -0.007(3) -0.002(2) -0.027(3) C3A 0.051(4) 0.088(5) 0.030(3) -0.015(3) 0.007(3) -0.033(4) C4A 0.066(5) 0.089(5) 0.030(3) 0.015(4) -0.011(3) -0.025(4) C5A 0.050(4) 0.063(4) 0.057(4) 0.021(3) -0.012(3) -0.014(3) C6A 0.042(3) 0.043(3) 0.034(3) 0.001(3) -0.009(3) -0.013(3) C7A 0.049(4) 0.042(3) 0.051(3) 0.002(3) -0.012(3) 0.008(3) C8A 0.084(5) 0.057(4) 0.093(5) -0.017(4) -0.010(4) -0.005(4) C9A 0.061(4) 0.060(4) 0.073(4) 0.001(3) -0.014(4) 0.016(4) C10A 0.038(3) 0.049(4) 0.049(3) -0.012(3) 0.012(3) -0.005(3) C11A 0.057(4) 0.059(4) 0.056(4) -0.007(3) -0.007(3) 0.006(3) C12A 0.053(4) 0.079(5) 0.095(5) -0.040(4) 0.019(4) -0.010(4) C13A 0.034(3) 0.030(3) 0.028(3) 0.003(2) 0.000(2) -0.005(2) C14A 0.023(3) 0.025(3) 0.032(3) -0.005(2) -0.002(2) -0.004(2) C15A 0.039(3) 0.036(3) 0.029(3) -0.007(2) -0.002(2) -0.010(3) C16A 0.042(3) 0.048(3) 0.024(3) 0.000(3) -0.008(2) -0.004(3) C17A 0.028(3) 0.042(3) 0.023(3) 0.006(2) 0.000(2) -0.006(2) C18A 0.035(3) 0.036(3) 0.020(2) 0.005(2) 0.003(2) -0.001(3) C19A 0.034(3) 0.037(3) 0.025(3) 0.007(2) -0.001(2) -0.004(3) C20A 0.045(3) 0.044(3) 0.036(3) 0.007(3) -0.005(2) -0.009(3) C21A 0.061(4) 0.046(3) 0.032(3) 0.016(3) 0.003(3) -0.014(3) C22A 0.046(3) 0.040(3) 0.031(3) 0.007(3) -0.002(2) -0.022(3) C23A 0.033(3) 0.034(3) 0.028(3) 0.003(2) 0.001(2) 0.000(2) C24A 0.029(3) 0.038(3) 0.035(3) 0.006(2) -0.003(2) -0.010(2) C25A 0.044(3) 0.045(3) 0.027(3) -0.001(3) 0.001(2) -0.027(3) C26A 0.043(3) 0.069(4) 0.026(3) -0.002(3) 0.001(2) -0.011(3) C27A 0.051(4) 0.084(5) 0.038(4) -0.014(3) 0.005(3) -0.027(4) C28A 0.061(4) 0.106(6) 0.020(3) 0.012(4) -0.005(3) -0.030(4) C29A 0.058(4) 0.065(4) 0.048(4) 0.009(3) -0.013(3) -0.022(4) C30A 0.049(4) 0.046(3) 0.031(3) 0.010(3) -0.009(3) -0.019(3) C31A 0.055(4) 0.047(4) 0.053(4) 0.013(3) -0.019(3) -0.012(3) C32A 0.054(4) 0.086(5) 0.096(5) -0.020(4) -0.008(4) -0.007(4) C33A 0.087(5) 0.063(5) 0.101(5) 0.024(4) -0.033(4) -0.009(4) C34A 0.045(4) 0.058(4) 0.037(3) -0.011(3) 0.001(3) 0.004(3) C35A 0.046(4) 0.071(4) 0.082(4) -0.026(4) -0.004(3) 0.005(4) C36A 0.066(4) 0.065(4) 0.073(4) -0.015(3) 0.004(4) -0.024(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N2 1.956(3) . ? Ni1 N3 2.122(4) . ? Ni1 N1 2.167(4) . ? Ni1 Cl2 2.2523(14) . ? Ni1 Cl1 2.2603(14) . ? N1 C13 1.276(5) . ? N1 C1 1.451(5) . ? N2 C14 1.332(5) . ? N2 C18 1.339(5) . ? N3 C23 1.339(5) . ? N3 C19 1.363(5) . ? N4 C24 1.269(5) . ? N4 C25 1.431(6) . ? C1 C2 1.395(6) . ? C1 C6 1.401(6) . ? C2 C3 1.414(6) . ? C2 C10 1.524(7) . ? C3 C4 1.375(8) . ? C3 H3 0.9500 . ? C4 C5 1.358(8) . ? C4 H4 0.9500 . ? C5 C6 1.406(7) . ? C5 H5 0.9500 . ? C6 C7 1.494(7) . ? C7 C8 1.534(7) . ? C7 C9 1.544(7) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.529(6) . ? C10 C12 1.531(7) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.473(6) . ? C13 H13 0.9500 . ? C14 C15 1.388(6) . ? C15 C16 1.384(6) . ? C15 H15 0.9500 . ? C16 C17 1.364(6) . ? C16 H16 0.9500 . ? C17 C18 1.387(6) . ? C17 H17 0.9500 . ? C18 C19 1.483(6) . ? C19 C20 1.393(6) . ? C20 C21 1.368(6) . ? C20 H20 0.9500 . ? C21 C22 1.382(6) . ? C21 H21 0.9500 . ? C22 C23 1.388(6) . ? C22 H22 0.9500 . ? C23 C24 1.473(6) . ? C24 H24 0.9500 . ? C25 C30 1.407(7) . ? C25 C26 1.418(7) . ? C26 C27 1.399(6) . ? C26 C34 1.517(7) . ? C27 C28 1.366(7) . ? C27 H27 0.9500 . ? C28 C29 1.369(7) . ? C28 H28 0.9500 . ? C29 C30 1.395(7) . ? C29 H29 0.9500 . ? C30 C31 1.514(7) . ? C31 C32 1.507(7) . ? C31 C33 1.520(7) . ? C31 H31 1.0000 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.523(7) . ? C34 C36 1.531(7) . ? C34 H34 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? Ni1A N2A 1.956(3) . ? Ni1A N3A 2.118(3) . ? Ni1A N1A 2.184(4) . ? Ni1A Cl1A 2.2482(14) . ? Ni1A Cl2A 2.2542(15) . ? N1A C13A 1.263(5) . ? N1A C1A 1.446(5) . ? N2A C18A 1.339(5) . ? N2A C14A 1.357(5) . ? N3A C23A 1.345(5) . ? N3A C19A 1.356(5) . ? N4A C24A 1.253(5) . ? N4A C25A 1.434(5) . ? C1A C6A 1.390(6) . ? C1A C2A 1.414(7) . ? C2A C3A 1.376(7) . ? C2A C10A 1.514(7) . ? C3A C4A 1.380(8) . ? C3A H3A 0.9500 . ? C4A C5A 1.380(7) . ? C4A H4A 0.9500 . ? C5A C6A 1.410(6) . ? C5A H5A 0.9500 . ? C6A C7A 1.509(7) . ? C7A C9A 1.519(7) . ? C7A C8A 1.555(7) . ? C7A H7A 1.0000 . ? C8A H8A1 0.9800 . ? C8A H8A2 0.9800 . ? C8A H8A3 0.9800 . ? C9A H9A1 0.9800 . ? C9A H9A2 0.9800 . ? C9A H9A3 0.9800 . ? C10A C12A 1.517(6) . ? C10A C11A 1.531(6) . ? C10A H10A 1.0000 . ? C11A H11D 0.9800 . ? C11A H11E 0.9800 . ? C11A H11F 0.9800 . ? C12A H12D 0.9800 . ? C12A H12E 0.9800 . ? C12A H12F 0.9800 . ? C13A C14A 1.470(6) . ? C13A H13A 0.9500 . ? C14A C15A 1.368(6) . ? C15A C16A 1.394(6) . ? C15A H15A 0.9500 . ? C16A C17A 1.381(6) . ? C16A H16A 0.9500 . ? C17A C18A 1.390(5) . ? C17A H17A 0.9500 . ? C18A C19A 1.488(6) . ? C19A C20A 1.377(6) . ? C20A C21A 1.373(6) . ? C20A H20A 0.9500 . ? C21A C22A 1.382(6) . ? C21A H21A 0.9500 . ? C22A C23A 1.399(6) . ? C22A H22A 0.9500 . ? C23A C24A 1.475(6) . ? C24A H24A 0.9500 . ? C25A C30A 1.394(7) . ? C25A C26A 1.408(7) . ? C26A C27A 1.387(7) . ? C26A C34A 1.520(7) . ? C27A C28A 1.388(7) . ? C27A H27A 0.9500 . ? C28A C29A 1.360(8) . ? C28A H28A 0.9500 . ? C29A C30A 1.382(7) . ? C29A H29A 0.9500 . ? C30A C31A 1.522(7) . ? C31A C33A 1.522(7) . ? C31A C32A 1.537(7) . ? C31A H31A 1.0000 . ? C32A H32D 0.9800 . ? C32A H32E 0.9800 . ? C32A H32F 0.9800 . ? C33A H33D 0.9800 . ? C33A H33E 0.9800 . ? C33A H33F 0.9800 . ? C34A C35A 1.524(7) . ? C34A C36A 1.527(6) . ? C34A H34A 1.0000 . ? C35A H35D 0.9800 . ? C35A H35E 0.9800 . ? C35A H35F 0.9800 . ? C36A H36D 0.9800 . ? C36A H36E 0.9800 . ? C36A H36F 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 N2 Ni1 N3 78.81(15) . . ? N2 Ni1 N1 77.82(14) . . ? N3 Ni1 N1 156.34(14) . . ? N2 Ni1 Cl2 115.96(11) . . ? N3 Ni1 Cl2 93.23(11) . . ? N1 Ni1 Cl2 93.68(10) . . ? N2 Ni1 Cl1 113.23(11) . . ? N3 Ni1 Cl1 92.86(11) . . ? N1 Ni1 Cl1 99.64(10) . . ? Cl2 Ni1 Cl1 130.69(5) . . ? C13 N1 C1 120.5(4) . . ? C13 N1 Ni1 111.8(3) . . ? C1 N1 Ni1 126.2(3) . . ? C14 N2 C18 120.7(4) . . ? C14 N2 Ni1 119.4(3) . . ? C18 N2 Ni1 120.0(3) . . ? C23 N3 C19 119.3(4) . . ? C23 N3 Ni1 128.0(3) . . ? C19 N3 Ni1 112.8(3) . . ? C24 N4 C25 116.8(4) . . ? C2 C1 C6 123.7(5) . . ? C2 C1 N1 118.9(4) . . ? C6 C1 N1 117.2(5) . . ? C1 C2 C3 116.8(5) . . ? C1 C2 C10 124.8(4) . . ? C3 C2 C10 118.3(5) . . ? C4 C3 C2 120.4(6) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C5 C4 C3 121.0(6) . . ? C5 C4 H4 119.5 . . ? C3 C4 H4 119.5 . . ? C4 C5 C6 122.0(6) . . ? C4 C5 H5 119.0 . . ? C6 C5 H5 119.0 . . ? C1 C6 C5 115.8(6) . . ? C1 C6 C7 122.2(5) . . ? C5 C6 C7 121.6(5) . . ? C6 C7 C8 110.4(4) . . ? C6 C7 C9 114.4(5) . . ? C8 C7 C9 109.3(5) . . ? C6 C7 H7 107.5 . . ? C8 C7 H7 107.5 . . ? C9 C7 H7 107.5 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C2 C10 C11 114.3(4) . . ? C2 C10 C12 109.9(5) . . ? C11 C10 C12 109.4(4) . . ? C2 C10 H10 107.7 . . ? C11 C10 H10 107.7 . . ? C12 C10 H10 107.7 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 C14 117.8(4) . . ? N1 C13 H13 121.1 . . ? C14 C13 H13 121.1 . . ? N2 C14 C15 121.3(4) . . ? N2 C14 C13 113.2(4) . . ? C15 C14 C13 125.3(4) . . ? C16 C15 C14 118.1(5) . . ? C16 C15 H15 121.0 . . ? C14 C15 H15 121.0 . . ? C17 C16 C15 120.2(4) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C16 C17 C18 119.1(4) . . ? C16 C17 H17 120.4 . . ? C18 C17 H17 120.4 . . ? N2 C18 C17 120.6(4) . . ? N2 C18 C19 113.7(4) . . ? C17 C18 C19 125.6(4) . . ? N3 C19 C20 121.5(4) . . ? N3 C19 C18 114.8(4) . . ? C20 C19 C18 123.7(4) . . ? C21 C20 C19 118.7(5) . . ? C21 C20 H20 120.6 . . ? C19 C20 H20 120.6 . . ? C20 C21 C22 119.7(5) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C21 C22 C23 119.6(5) . . ? C21 C22 H22 120.2 . . ? C23 C22 H22 120.2 . . ? N3 C23 C22 121.1(5) . . ? N3 C23 C24 116.6(4) . . ? C22 C23 C24 122.3(5) . . ? N4 C24 C23 121.5(5) . . ? N4 C24 H24 119.3 . . ? C23 C24 H24 119.3 . . ? C30 C25 C26 122.2(5) . . ? C30 C25 N4 120.9(5) . . ? C26 C25 N4 116.7(5) . . ? C27 C26 C25 116.9(5) . . ? C27 C26 C34 122.3(5) . . ? C25 C26 C34 120.8(4) . . ? C28 C27 C26 121.4(6) . . ? C28 C27 H27 119.3 . . ? C26 C27 H27 119.3 . . ? C27 C28 C29 120.9(6) . . ? C27 C28 H28 119.6 . . ? C29 C28 H28 119.6 . . ? C28 C29 C30 121.6(6) . . ? C28 C29 H29 119.2 . . ? C30 C29 H29 119.2 . . ? C29 C30 C25 117.0(5) . . ? C29 C30 C31 121.6(5) . . ? C25 C30 C31 121.2(5) . . ? C32 C31 C30 110.4(5) . . ? C32 C31 C33 107.1(5) . . ? C30 C31 C33 114.4(5) . . ? C32 C31 H31 108.3 . . ? C30 C31 H31 108.3 . . ? C33 C31 H31 108.3 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C26 C34 C35 111.3(5) . . ? C26 C34 C36 112.6(5) . . ? C35 C34 C36 110.7(5) . . ? C26 C34 H34 107.3 . . ? C35 C34 H34 107.3 . . ? C36 C34 H34 107.3 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N2A Ni1A N3A 78.43(14) . . ? N2A Ni1A N1A 77.73(14) . . ? N3A Ni1A N1A 156.16(14) . . ? N2A Ni1A Cl1A 110.31(11) . . ? N3A Ni1A Cl1A 94.85(11) . . ? N1A Ni1A Cl1A 93.63(10) . . ? N2A Ni1A Cl2A 119.60(11) . . ? N3A Ni1A Cl2A 91.73(11) . . ? N1A Ni1A Cl2A 99.76(10) . . ? Cl1A Ni1A Cl2A 129.97(6) . . ? C13A N1A C1A 121.3(4) . . ? C13A N1A Ni1A 111.4(3) . . ? C1A N1A Ni1A 126.1(3) . . ? C18A N2A C14A 120.6(4) . . ? C18A N2A Ni1A 120.2(3) . . ? C14A N2A Ni1A 119.1(3) . . ? C23A N3A C19A 118.2(4) . . ? C23A N3A Ni1A 128.3(3) . . ? C19A N3A Ni1A 113.4(3) . . ? C24A N4A C25A 116.1(4) . . ? C6A C1A C2A 122.3(5) . . ? C6A C1A N1A 120.5(5) . . ? C2A C1A N1A 116.9(5) . . ? C3A C2A C1A 117.6(5) . . ? C3A C2A C10A 121.4(5) . . ? C1A C2A C10A 120.7(4) . . ? C2A C3A C4A 122.1(6) . . ? C2A C3A H3A 118.9 . . ? C4A C3A H3A 118.9 . . ? C3A C4A C5A 119.2(5) . . ? C3A C4A H4A 120.4 . . ? C5A C4A H4A 120.4 . . ? C4A C5A C6A 121.7(6) . . ? C4A C5A H5A 119.1 . . ? C6A C5A H5A 119.1 . . ? C1A C6A C5A 116.9(5) . . ? C1A C6A C7A 125.3(5) . . ? C5A C6A C7A 117.7(5) . . ? C6A C7A C9A 114.9(4) . . ? C6A C7A C8A 109.6(4) . . ? C9A C7A C8A 108.0(4) . . ? C6A C7A H7A 108.1 . . ? C9A C7A H7A 108.1 . . ? C8A C7A H7A 108.1 . . ? C7A C8A H8A1 109.5 . . ? C7A C8A H8A2 109.5 . . ? H8A1 C8A H8A2 109.5 . . ? C7A C8A H8A3 109.5 . . ? H8A1 C8A H8A3 109.5 . . ? H8A2 C8A H8A3 109.5 . . ? C7A C9A H9A1 109.5 . . ? C7A C9A H9A2 109.5 . . ? H9A1 C9A H9A2 109.5 . . ? C7A C9A H9A3 109.5 . . ? H9A1 C9A H9A3 109.5 . . ? H9A2 C9A H9A3 109.5 . . ? C2A C10A C12A 114.3(5) . . ? C2A C10A C11A 110.2(4) . . ? C12A C10A C11A 107.9(4) . . ? C2A C10A H10A 108.1 . . ? C12A C10A H10A 108.1 . . ? C11A C10A H10A 108.1 . . ? C10A C11A H11D 109.5 . . ? C10A C11A H11E 109.5 . . ? H11D C11A H11E 109.5 . . ? C10A C11A H11F 109.5 . . ? H11D C11A H11F 109.5 . . ? H11E C11A H11F 109.5 . . ? C10A C12A H12D 109.5 . . ? C10A C12A H12E 109.5 . . ? H12D C12A H12E 109.5 . . ? C10A C12A H12F 109.5 . . ? H12D C12A H12F 109.5 . . ? H12E C12A H12F 109.5 . . ? N1A C13A C14A 118.9(4) . . ? N1A C13A H13A 120.6 . . ? C14A C13A H13A 120.6 . . ? N2A C14A C15A 120.9(4) . . ? N2A C14A C13A 112.5(4) . . ? C15A C14A C13A 126.5(4) . . ? C14A C15A C16A 119.1(5) . . ? C14A C15A H15A 120.5 . . ? C16A C15A H15A 120.5 . . ? C17A C16A C15A 119.7(4) . . ? C17A C16A H16A 120.2 . . ? C15A C16A H16A 120.2 . . ? C16A C17A C18A 118.8(4) . . ? C16A C17A H17A 120.6 . . ? C18A C17A H17A 120.6 . . ? N2A C18A C17A 120.9(4) . . ? N2A C18A C19A 113.4(4) . . ? C17A C18A C19A 125.7(4) . . ? N3A C19A C20A 122.6(4) . . ? N3A C19A C18A 114.2(4) . . ? C20A C19A C18A 123.2(4) . . ? C21A C20A C19A 118.3(5) . . ? C21A C20A H20A 120.8 . . ? C19A C20A H20A 120.8 . . ? C20A C21A C22A 120.7(5) . . ? C20A C21A H21A 119.6 . . ? C22A C21A H21A 119.6 . . ? C21A C22A C23A 117.8(4) . . ? C21A C22A H22A 121.1 . . ? C23A C22A H22A 121.1 . . ? N3A C23A C22A 122.2(4) . . ? N3A C23A C24A 116.6(4) . . ? C22A C23A C24A 121.0(4) . . ? N4A C24A C23A 122.3(4) . . ? N4A C24A H24A 118.9 . . ? C23A C24A H24A 118.9 . . ? C30A C25A C26A 122.6(5) . . ? C30A C25A N4A 121.5(5) . . ? C26A C25A N4A 115.9(5) . . ? C27A C26A C25A 117.4(5) . . ? C27A C26A C34A 121.5(5) . . ? C25A C26A C34A 121.1(4) . . ? C26A C27A C28A 120.6(6) . . ? C26A C27A H27A 119.7 . . ? C28A C27A H27A 119.7 . . ? C29A C28A C27A 120.0(5) . . ? C29A C28A H28A 120.0 . . ? C27A C28A H28A 120.0 . . ? C28A C29A C30A 122.6(6) . . ? C28A C29A H29A 118.7 . . ? C30A C29A H29A 118.7 . . ? C29A C30A C25A 116.6(6) . . ? C29A C30A C31A 120.4(5) . . ? C25A C30A C31A 122.8(5) . . ? C30A C31A C33A 112.6(5) . . ? C30A C31A C32A 112.2(5) . . ? C33A C31A C32A 110.7(5) . . ? C30A C31A H31A 107.0 . . ? C33A C31A H31A 107.0 . . ? C32A C31A H31A 107.0 . . ? C31A C32A H32D 109.5 . . ? C31A C32A H32E 109.5 . . ? H32D C32A H32E 109.5 . . ? C31A C32A H32F 109.5 . . ? H32D C32A H32F 109.5 . . ? H32E C32A H32F 109.5 . . ? C31A C33A H33D 109.5 . . ? C31A C33A H33E 109.5 . . ? H33D C33A H33E 109.5 . . ? C31A C33A H33F 109.5 . . ? H33D C33A H33F 109.5 . . ? H33E C33A H33F 109.5 . . ? C26A C34A C35A 111.2(5) . . ? C26A C34A C36A 112.9(5) . . ? C35A C34A C36A 110.6(5) . . ? C26A C34A H34A 107.3 . . ? C35A C34A H34A 107.3 . . ? C36A C34A H34A 107.3 . . ? C34A C35A H35D 109.5 . . ? C34A C35A H35E 109.5 . . ? H35D C35A H35E 109.5 . . ? C34A C35A H35F 109.5 . . ? H35D C35A H35F 109.5 . . ? H35E C35A H35F 109.5 . . ? C34A C36A H36D 109.5 . . ? C34A C36A H36E 109.5 . . ? H36D C36A H36E 109.5 . . ? C34A C36A H36F 109.5 . . ? H36D C36A H36F 109.5 . . ? H36E C36A H36F 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 N2 Ni1 N1 C13 -1.2(3) . . . . ? N3 Ni1 N1 C13 7.9(6) . . . . ? Cl2 Ni1 N1 C13 114.6(3) . . . . ? Cl1 Ni1 N1 C13 -113.1(3) . . . . ? N2 Ni1 N1 C1 -167.0(4) . . . . ? N3 Ni1 N1 C1 -157.9(4) . . . . ? Cl2 Ni1 N1 C1 -51.2(4) . . . . ? Cl1 Ni1 N1 C1 81.1(4) . . . . ? N3 Ni1 N2 C14 -176.8(4) . . . . ? N1 Ni1 N2 C14 -0.5(3) . . . . ? Cl2 Ni1 N2 C14 -88.7(3) . . . . ? Cl1 Ni1 N2 C14 94.9(3) . . . . ? N3 Ni1 N2 C18 1.3(3) . . . . ? N1 Ni1 N2 C18 177.7(4) . . . . ? Cl2 Ni1 N2 C18 89.5(3) . . . . ? Cl1 Ni1 N2 C18 -87.0(3) . . . . ? N2 Ni1 N3 C23 177.3(4) . . . . ? N1 Ni1 N3 C23 168.3(4) . . . . ? Cl2 Ni1 N3 C23 61.5(4) . . . . ? Cl1 Ni1 N3 C23 -69.6(4) . . . . ? N2 Ni1 N3 C19 -0.8(3) . . . . ? N1 Ni1 N3 C19 -9.8(5) . . . . ? Cl2 Ni1 N3 C19 -116.6(3) . . . . ? Cl1 Ni1 N3 C19 112.3(3) . . . . ? C13 N1 C1 C2 -71.8(6) . . . . ? Ni1 N1 C1 C2 92.9(5) . . . . ? C13 N1 C1 C6 113.8(5) . . . . ? Ni1 N1 C1 C6 -81.5(5) . . . . ? C6 C1 C2 C3 3.1(7) . . . . ? N1 C1 C2 C3 -171.0(4) . . . . ? C6 C1 C2 C10 -172.9(4) . . . . ? N1 C1 C2 C10 13.0(7) . . . . ? C1 C2 C3 C4 1.7(8) . . . . ? C10 C2 C3 C4 178.0(5) . . . . ? C2 C3 C4 C5 -4.8(9) . . . . ? C3 C4 C5 C6 3.1(9) . . . . ? C2 C1 C6 C5 -4.7(7) . . . . ? N1 C1 C6 C5 169.5(4) . . . . ? C2 C1 C6 C7 169.2(4) . . . . ? N1 C1 C6 C7 -16.7(7) . . . . ? C4 C5 C6 C1 1.5(8) . . . . ? C4 C5 C6 C7 -172.4(5) . . . . ? C1 C6 C7 C8 -86.2(6) . . . . ? C5 C6 C7 C8 87.3(6) . . . . ? C1 C6 C7 C9 150.1(5) . . . . ? C5 C6 C7 C9 -36.4(7) . . . . ? C1 C2 C10 C11 -134.4(5) . . . . ? C3 C2 C10 C11 49.6(6) . . . . ? C1 C2 C10 C12 102.2(6) . . . . ? C3 C2 C10 C12 -73.8(6) . . . . ? C1 N1 C13 C14 169.3(4) . . . . ? Ni1 N1 C13 C14 2.6(5) . . . . ? C18 N2 C14 C15 -0.2(7) . . . . ? Ni1 N2 C14 C15 178.0(4) . . . . ? C18 N2 C14 C13 -176.2(4) . . . . ? Ni1 N2 C14 C13 1.9(5) . . . . ? N1 C13 C14 N2 -3.1(6) . . . . ? N1 C13 C14 C15 -178.9(5) . . . . ? N2 C14 C15 C16 0.6(7) . . . . ? C13 C14 C15 C16 176.2(4) . . . . ? C14 C15 C16 C17 -1.3(7) . . . . ? C15 C16 C17 C18 1.5(7) . . . . ? C14 N2 C18 C17 0.4(7) . . . . ? Ni1 N2 C18 C17 -177.8(3) . . . . ? C14 N2 C18 C19 176.6(4) . . . . ? Ni1 N2 C18 C19 -1.6(5) . . . . ? C16 C17 C18 N2 -1.0(7) . . . . ? C16 C17 C18 C19 -176.8(4) . . . . ? C23 N3 C19 C20 1.6(7) . . . . ? Ni1 N3 C19 C20 179.9(3) . . . . ? C23 N3 C19 C18 -178.1(4) . . . . ? Ni1 N3 C19 C18 0.3(5) . . . . ? N2 C18 C19 N3 0.8(6) . . . . ? C17 C18 C19 N3 176.8(4) . . . . ? N2 C18 C19 C20 -178.9(4) . . . . ? C17 C18 C19 C20 -2.9(7) . . . . ? N3 C19 C20 C21 -1.9(7) . . . . ? C18 C19 C20 C21 177.7(4) . . . . ? C19 C20 C21 C22 0.3(7) . . . . ? C20 C21 C22 C23 1.6(8) . . . . ? C19 N3 C23 C22 0.4(7) . . . . ? Ni1 N3 C23 C22 -177.6(3) . . . . ? C19 N3 C23 C24 -178.6(4) . . . . ? Ni1 N3 C23 C24 3.3(6) . . . . ? C21 C22 C23 N3 -2.0(8) . . . . ? C21 C22 C23 C24 177.0(5) . . . . ? C25 N4 C24 C23 -178.1(4) . . . . ? N3 C23 C24 N4 -174.1(4) . . . . ? C22 C23 C24 N4 6.9(8) . . . . ? C24 N4 C25 C30 -84.0(6) . . . . ? C24 N4 C25 C26 100.8(5) . . . . ? C30 C25 C26 C27 -0.1(7) . . . . ? N4 C25 C26 C27 175.1(4) . . . . ? C30 C25 C26 C34 -179.1(5) . . . . ? N4 C25 C26 C34 -4.0(7) . . . . ? C25 C26 C27 C28 1.1(8) . . . . ? C34 C26 C27 C28 -179.9(5) . . . . ? C26 C27 C28 C29 -1.7(9) . . . . ? C27 C28 C29 C30 1.4(9) . . . . ? C28 C29 C30 C25 -0.4(8) . . . . ? C28 C29 C30 C31 -175.9(5) . . . . ? C26 C25 C30 C29 -0.2(8) . . . . ? N4 C25 C30 C29 -175.2(4) . . . . ? C26 C25 C30 C31 175.3(5) . . . . ? N4 C25 C30 C31 0.3(7) . . . . ? C29 C30 C31 C32 104.2(6) . . . . ? C25 C30 C31 C32 -71.1(7) . . . . ? C29 C30 C31 C33 -16.6(8) . . . . ? C25 C30 C31 C33 168.1(5) . . . . ? C27 C26 C34 C35 86.2(6) . . . . ? C25 C26 C34 C35 -94.8(6) . . . . ? C27 C26 C34 C36 -38.8(7) . . . . ? C25 C26 C34 C36 140.2(5) . . . . ? N2A Ni1A N1A C13A 5.4(3) . . . . ? N3A Ni1A N1A C13A 6.1(6) . . . . ? Cl1A Ni1A N1A C13A -104.6(3) . . . . ? Cl2A Ni1A N1A C13A 123.8(3) . . . . ? N2A Ni1A N1A C1A 172.9(4) . . . . ? N3A Ni1A N1A C1A 173.6(4) . . . . ? Cl1A Ni1A N1A C1A 62.9(4) . . . . ? Cl2A Ni1A N1A C1A -68.7(4) . . . . ? N3A Ni1A N2A C18A -0.2(3) . . . . ? N1A Ni1A N2A C18A 179.5(4) . . . . ? Cl1A Ni1A N2A C18A -91.1(3) . . . . ? Cl2A Ni1A N2A C18A 85.2(3) . . . . ? N3A Ni1A N2A C14A 176.1(3) . . . . ? N1A Ni1A N2A C14A -4.2(3) . . . . ? Cl1A Ni1A N2A C14A 85.2(3) . . . . ? Cl2A Ni1A N2A C14A -98.5(3) . . . . ? N2A Ni1A N3A C23A 179.8(4) . . . . ? N1A Ni1A N3A C23A 179.1(3) . . . . ? Cl1A Ni1A N3A C23A -70.5(4) . . . . ? Cl2A Ni1A N3A C23A 59.9(4) . . . . ? N2A Ni1A N3A C19A 4.0(3) . . . . ? N1A Ni1A N3A C19A 3.3(6) . . . . ? Cl1A Ni1A N3A C19A 113.8(3) . . . . ? Cl2A Ni1A N3A C19A -115.9(3) . . . . ? C13A N1A C1A C6A 72.6(6) . . . . ? Ni1A N1A C1A C6A -93.8(5) . . . . ? C13A N1A C1A C2A -113.2(5) . . . . ? Ni1A N1A C1A C2A 80.4(5) . . . . ? C6A C1A C2A C3A 4.1(7) . . . . ? N1A C1A C2A C3A -170.0(4) . . . . ? C6A C1A C2A C10A -169.5(4) . . . . ? N1A C1A C2A C10A 16.4(6) . . . . ? C1A C2A C3A C4A -1.2(8) . . . . ? C10A C2A C3A C4A 172.4(5) . . . . ? C2A C3A C4A C5A -2.5(9) . . . . ? C3A C4A C5A C6A 3.4(8) . . . . ? C2A C1A C6A C5A -3.2(7) . . . . ? N1A C1A C6A C5A 170.7(4) . . . . ? C2A C1A C6A C7A 172.7(5) . . . . ? N1A C1A C6A C7A -13.4(7) . . . . ? C4A C5A C6A C1A -0.6(8) . . . . ? C4A C5A C6A C7A -176.8(5) . . . . ? C1A C6A C7A C9A 131.1(5) . . . . ? C5A C6A C7A C9A -53.1(7) . . . . ? C1A C6A C7A C8A -107.2(6) . . . . ? C5A C6A C7A C8A 68.7(6) . . . . ? C3A C2A C10A C12A 31.6(7) . . . . ? C1A C2A C10A C12A -155.0(5) . . . . ? C3A C2A C10A C11A -90.0(6) . . . . ? C1A C2A C10A C11A 83.3(6) . . . . ? C1A N1A C13A C14A -174.1(4) . . . . ? Ni1A N1A C13A C14A -5.8(5) . . . . ? C18A N2A C14A C15A 2.8(7) . . . . ? Ni1A N2A C14A C15A -173.5(3) . . . . ? C18A N2A C14A C13A 178.8(4) . . . . ? Ni1A N2A C14A C13A 2.5(5) . . . . ? N1A C13A C14A N2A 2.7(6) . . . . ? N1A C13A C14A C15A 178.4(5) . . . . ? N2A C14A C15A C16A -3.3(7) . . . . ? C13A C14A C15A C16A -178.6(5) . . . . ? C14A C15A C16A C17A 2.3(7) . . . . ? C15A C16A C17A C18A -0.9(7) . . . . ? C14A N2A C18A C17A -1.4(6) . . . . ? Ni1A N2A C18A C17A 174.9(3) . . . . ? C14A N2A C18A C19A -179.6(4) . . . . ? Ni1A N2A C18A C19A -3.3(5) . . . . ? C16A C17A C18A N2A 0.4(7) . . . . ? C16A C17A C18A C19A 178.4(4) . . . . ? C23A N3A C19A C20A -3.9(7) . . . . ? Ni1A N3A C19A C20A 172.4(4) . . . . ? C23A N3A C19A C18A 177.0(4) . . . . ? Ni1A N3A C19A C18A -6.7(5) . . . . ? N2A C18A C19A N3A 6.6(6) . . . . ? C17A C18A C19A N3A -171.4(4) . . . . ? N2A C18A C19A C20A -172.4(4) . . . . ? C17A C18A C19A C20A 9.5(8) . . . . ? N3A C19A C20A C21A 3.4(7) . . . . ? C18A C19A C20A C21A -177.6(4) . . . . ? C19A C20A C21A C22A -0.7(8) . . . . ? C20A C21A C22A C23A -1.3(8) . . . . ? C19A N3A C23A C22A 1.7(7) . . . . ? Ni1A N3A C23A C22A -173.9(3) . . . . ? C19A N3A C23A C24A 176.6(4) . . . . ? Ni1A N3A C23A C24A 1.0(6) . . . . ? C21A C22A C23A N3A 0.8(7) . . . . ? C21A C22A C23A C24A -173.9(5) . . . . ? C25A N4A C24A C23A 172.8(4) . . . . ? N3A C23A C24A N4A -173.8(4) . . . . ? C22A C23A C24A N4A 1.2(7) . . . . ? C24A N4A C25A C30A 76.9(6) . . . . ? C24A N4A C25A C26A -105.8(5) . . . . ? C30A C25A C26A C27A -3.7(8) . . . . ? N4A C25A C26A C27A 179.0(4) . . . . ? C30A C25A C26A C34A 175.2(5) . . . . ? N4A C25A C26A C34A -2.1(7) . . . . ? C25A C26A C27A C28A -0.5(8) . . . . ? C34A C26A C27A C28A -179.4(5) . . . . ? C26A C27A C28A C29A 3.5(8) . . . . ? C27A C28A C29A C30A -2.5(9) . . . . ? C28A C29A C30A C25A -1.5(8) . . . . ? C28A C29A C30A C31A 173.5(5) . . . . ? C26A C25A C30A C29A 4.7(8) . . . . ? N4A C25A C30A C29A -178.2(4) . . . . ? C26A C25A C30A C31A -170.2(5) . . . . ? N4A C25A C30A C31A 6.9(7) . . . . ? C29A C30A C31A C33A 66.7(7) . . . . ? C25A C30A C31A C33A -118.6(5) . . . . ? C29A C30A C31A C32A -59.1(7) . . . . ? C25A C30A C31A C32A 115.7(6) . . . . ? C27A C26A C34A C35A -75.9(6) . . . . ? C25A C26A C34A C35A 105.2(6) . . . . ? C27A C26A C34A C36A 49.1(7) . . . . ? C25A C26A C34A C36A -129.7(5) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.726 _refine_diff_density_min -0.708 _refine_diff_density_rms 0.065 # Attachment '08024.cif' data_08024 _database_code_depnum_ccdc_archive 'CCDC 692759' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C24 H25 Cl2 N3 O Zn)(C H Cl3)(C H2 Cl2)' _chemical_formula_sum 'C26 H28 Cl7 N3 O Zn' _chemical_formula_weight 712.03 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I-4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 20.148(5) _cell_length_b 20.148(5) _cell_length_c 15.683(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6366(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 826 _cell_measurement_theta_min 2.598 _cell_measurement_theta_max 23.459 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.486 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2896 _exptl_absorpt_coefficient_mu 1.384 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.355 _exptl_absorpt_correction_T_max 0.928 _exptl_absorpt_process_details ; absorption correction based on 4271 reflections(SADABS);Rint 0.0830 before correction and 0.0720 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 24706 _diffrn_reflns_av_R_equivalents 0.1569 _diffrn_reflns_av_sigmaI/netI 0.1953 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6227 _reflns_number_gt 3211 _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 ; Disordered CHCl3 and CH2Cl2 are omitted using the SQUEEZE option of PLATON. The solvent accessible voids are 2045.9 \%A3 with an estimated 794e/cell to be added.Eight solvent CHCl3 and eight CH2Cl2 molecules/unit cell accounting for 800e were included in the formula, FWt, (000) and density calculations. PLATON Reference: Spek, A.L. (1990), Acta Cryst. A46,C-34. 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^)+(0.0333P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.08(2) _refine_ls_number_reflns 6227 _refine_ls_number_parameters 284 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1238 _refine_ls_R_factor_gt 0.0651 _refine_ls_wR_factor_ref 0.1190 _refine_ls_wR_factor_gt 0.1035 _refine_ls_goodness_of_fit_ref 0.809 _refine_ls_restrained_S_all 0.809 _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 0.22708(4) 0.17256(4) 0.00788(5) 0.0350(2) Uani 1 1 d . . . Cl1 Cl 0.14381(9) 0.19624(9) 0.09662(12) 0.0459(5) Uani 1 1 d . . . Cl2 Cl 0.32954(9) 0.20181(9) 0.04832(12) 0.0468(5) Uani 1 1 d . . . O1 O 0.2452(4) 0.3977(3) 0.0490(4) 0.121(3) Uani 1 1 d . . . N1 N 0.2339(2) 0.0607(3) 0.0294(4) 0.0377(16) Uani 1 1 d . . . N2 N 0.2153(2) 0.1309(3) -0.1116(4) 0.0313(14) Uani 1 1 d . . . N3 N 0.2170(3) 0.2598(3) -0.0846(4) 0.0376(15) Uani 1 1 d . . . C1 C 0.2481(3) 0.0232(3) 0.1083(5) 0.0361(18) Uani 1 1 d . . . C2 C 0.1942(3) 0.0103(3) 0.1604(5) 0.0364(19) Uani 1 1 d . . . C3 C 0.2084(4) -0.0229(3) 0.2376(5) 0.045(2) Uani 1 1 d . . . H3 H 0.1732 -0.0351 0.2748 0.054 Uiso 1 1 calc R . . C4 C 0.2741(4) -0.0381(3) 0.2595(6) 0.052(2) Uani 1 1 d . . . H4 H 0.2844 -0.0572 0.3133 0.062 Uiso 1 1 calc R . . C5 C 0.3242(4) -0.0243(4) 0.1999(6) 0.062(3) Uani 1 1 d . . . H5 H 0.3682 -0.0385 0.2123 0.074 Uiso 1 1 calc R . . C6 C 0.3132(4) 0.0084(3) 0.1250(5) 0.043(2) Uani 1 1 d . . . C7 C 0.3703(3) 0.0230(4) 0.0643(5) 0.053(2) Uani 1 1 d . . . H7 H 0.3531 0.0538 0.0194 0.064 Uiso 1 1 calc R . . C8 C 0.3920(4) -0.0420(4) 0.0188(6) 0.077(3) Uani 1 1 d . . . H8A H 0.4307 -0.0332 -0.0172 0.116 Uiso 1 1 calc R . . H8B H 0.3554 -0.0584 -0.0167 0.116 Uiso 1 1 calc R . . H8C H 0.4034 -0.0756 0.0616 0.116 Uiso 1 1 calc R . . C9 C 0.4280(3) 0.0586(4) 0.1094(5) 0.065(3) Uani 1 1 d . . . H9A H 0.4140 0.1033 0.1259 0.098 Uiso 1 1 calc R . . H9B H 0.4660 0.0615 0.0706 0.098 Uiso 1 1 calc R . . H9C H 0.4407 0.0335 0.1604 0.098 Uiso 1 1 calc R . . C10 C 0.1229(3) 0.0232(4) 0.1389(5) 0.049(2) Uani 1 1 d . . . H10 H 0.1227 0.0594 0.0952 0.059 Uiso 1 1 calc R . . C11 C 0.0943(3) -0.0378(3) 0.0958(5) 0.054(2) Uani 1 1 d . . . H11A H 0.0897 -0.0736 0.1377 0.081 Uiso 1 1 calc R . . H11B H 0.1241 -0.0522 0.0500 0.081 Uiso 1 1 calc R . . H11C H 0.0506 -0.0271 0.0719 0.081 Uiso 1 1 calc R . . C12 C 0.0806(3) 0.0470(3) 0.2116(5) 0.051(2) Uani 1 1 d . . . H12A H 0.0691 0.0093 0.2483 0.076 Uiso 1 1 calc R . . H12B H 0.0398 0.0670 0.1892 0.076 Uiso 1 1 calc R . . H12C H 0.1051 0.0800 0.2448 0.076 Uiso 1 1 calc R . . C13 C 0.2265(3) 0.0294(3) -0.0414(5) 0.0372(19) Uani 1 1 d . . . H13 H 0.2286 -0.0177 -0.0414 0.045 Uiso 1 1 calc R . . C14 C 0.2152(3) 0.0638(4) -0.1215(5) 0.0392(19) Uani 1 1 d . . . C15 C 0.2057(4) 0.0332(4) -0.1989(5) 0.043(2) Uani 1 1 d . . . H15 H 0.2060 -0.0138 -0.2038 0.052 Uiso 1 1 calc R . . C16 C 0.1959(4) 0.0728(4) -0.2689(5) 0.057(2) Uani 1 1 d . . . H16 H 0.1890 0.0530 -0.3231 0.068 Uiso 1 1 calc R . . C17 C 0.1957(4) 0.1403(4) -0.2619(5) 0.059(2) Uani 1 1 d . . . H17 H 0.1889 0.1677 -0.3104 0.070 Uiso 1 1 calc R . . C18 C 0.2061(3) 0.1681(4) -0.1806(5) 0.0421(19) Uani 1 1 d . . . C19 C 0.2118(3) 0.2428(4) -0.1646(5) 0.0392(18) Uani 1 1 d . . . C20 C 0.2137(3) 0.2870(4) -0.2333(5) 0.045(2) Uani 1 1 d . . . H20 H 0.2110 0.2721 -0.2907 0.054 Uiso 1 1 calc R . . C21 C 0.2199(4) 0.3544(4) -0.2127(5) 0.054(2) Uani 1 1 d . . . H21 H 0.2199 0.3868 -0.2566 0.065 Uiso 1 1 calc R . . C22 C 0.2258(4) 0.3731(4) -0.1307(6) 0.061(3) Uani 1 1 d . . . H22 H 0.2320 0.4185 -0.1163 0.073 Uiso 1 1 calc R . . C23 C 0.2228(4) 0.3253(4) -0.0682(5) 0.045(2) Uani 1 1 d . . . C24 C 0.2301(4) 0.3434(4) 0.0238(5) 0.063(3) Uani 1 1 d . . . H24 H 0.2223 0.3098 0.0651 0.076 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0374(5) 0.0394(5) 0.0280(4) -0.0021(4) -0.0033(4) 0.0011(4) Cl1 0.0397(11) 0.0429(11) 0.0550(13) -0.0036(10) 0.0033(10) 0.0017(9) Cl2 0.0453(12) 0.0462(12) 0.0490(12) -0.0046(10) -0.0032(10) -0.0045(10) O1 0.255(10) 0.034(4) 0.072(5) -0.012(4) -0.005(5) -0.032(5) N1 0.015(3) 0.044(4) 0.054(5) 0.003(3) -0.004(3) 0.005(3) N2 0.021(3) 0.027(3) 0.046(4) -0.002(3) 0.003(3) 0.002(3) N3 0.028(3) 0.060(4) 0.024(4) -0.005(3) 0.011(3) -0.001(3) C1 0.023(4) 0.029(4) 0.057(5) -0.012(4) -0.006(4) 0.008(3) C2 0.027(4) 0.036(4) 0.046(5) -0.010(4) -0.001(4) -0.005(3) C3 0.057(5) 0.036(4) 0.042(5) 0.006(4) 0.000(4) -0.008(4) C4 0.059(5) 0.038(5) 0.059(6) 0.009(4) -0.008(5) 0.011(4) C5 0.050(6) 0.043(5) 0.092(8) -0.002(5) -0.014(6) 0.007(4) C6 0.066(6) 0.017(4) 0.047(5) -0.009(4) -0.008(4) 0.002(4) C7 0.028(4) 0.067(6) 0.065(6) -0.029(5) -0.002(4) -0.001(4) C8 0.052(5) 0.075(6) 0.105(9) -0.018(6) 0.022(6) 0.015(5) C9 0.040(5) 0.066(6) 0.091(7) -0.006(5) -0.007(5) 0.011(4) C10 0.037(5) 0.049(5) 0.062(6) 0.010(4) -0.003(4) -0.007(4) C11 0.025(4) 0.057(5) 0.081(7) -0.019(5) 0.005(4) 0.001(4) C12 0.027(4) 0.051(5) 0.074(6) -0.016(5) -0.002(4) -0.006(4) C13 0.036(4) 0.027(4) 0.049(5) -0.011(4) 0.009(4) -0.003(4) C14 0.024(4) 0.054(5) 0.040(5) -0.011(4) -0.005(4) 0.011(4) C15 0.049(5) 0.040(5) 0.041(5) -0.012(4) -0.003(4) 0.011(4) C16 0.069(6) 0.059(6) 0.042(5) -0.023(5) -0.010(5) -0.006(5) C17 0.072(6) 0.073(7) 0.030(5) -0.010(5) 0.008(5) -0.010(5) C18 0.040(5) 0.051(5) 0.035(4) 0.001(5) -0.006(4) 0.006(4) C19 0.036(4) 0.042(5) 0.040(5) 0.008(4) 0.013(4) -0.001(4) C20 0.039(5) 0.055(5) 0.040(5) 0.019(4) -0.017(4) 0.004(4) C21 0.060(6) 0.046(6) 0.055(6) 0.038(5) 0.008(5) -0.008(4) C22 0.069(7) 0.048(6) 0.064(7) -0.013(5) -0.014(6) -0.005(5) C23 0.066(5) 0.034(5) 0.036(5) 0.014(4) -0.007(4) -0.012(4) C24 0.099(7) 0.046(5) 0.045(6) 0.009(4) 0.014(5) 0.015(5) _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 2.067(6) . ? Zn1 Cl1 2.231(2) . ? Zn1 Cl2 2.239(2) . ? Zn1 N1 2.283(5) . ? Zn1 N3 2.288(6) . ? O1 C24 1.201(9) . ? N1 C13 1.285(8) . ? N1 C1 1.478(9) . ? N2 C18 1.329(8) . ? N2 C14 1.360(8) . ? N3 C19 1.304(8) . ? N3 C23 1.350(8) . ? C1 C6 1.371(9) . ? C1 C2 1.384(9) . ? C2 C3 1.412(9) . ? C2 C10 1.499(9) . ? C3 C4 1.401(10) . ? C3 H3 0.9500 . ? C4 C5 1.405(10) . ? C4 H4 0.9500 . ? C5 C6 1.365(10) . ? C5 H5 0.9500 . ? C6 C7 1.523(10) . ? C7 C9 1.537(9) . ? C7 C8 1.555(9) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C12 1.503(10) . ? C10 C11 1.517(9) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.453(9) . ? C13 H13 0.9500 . ? C14 C15 1.375(9) . ? C15 C16 1.372(10) . ? C15 H15 0.9500 . ? C16 C17 1.363(10) . ? C16 H16 0.9500 . ? C17 C18 1.408(9) . ? C17 H17 0.9500 . ? C18 C19 1.531(10) . ? C19 C20 1.397(9) . ? C20 C21 1.401(10) . ? C20 H20 0.9500 . ? C21 C22 1.346(10) . ? C21 H21 0.9500 . ? C22 C23 1.376(10) . ? C22 H22 0.9500 . ? C23 C24 1.495(10) . ? C24 H24 0.9500 . ? 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 Cl1 124.48(15) . . ? N2 Zn1 Cl2 118.00(15) . . ? Cl1 Zn1 Cl2 117.41(8) . . ? N2 Zn1 N1 74.9(2) . . ? Cl1 Zn1 N1 99.45(15) . . ? Cl2 Zn1 N1 99.36(14) . . ? N2 Zn1 N3 74.2(2) . . ? Cl1 Zn1 N3 99.46(14) . . ? Cl2 Zn1 N3 93.40(15) . . ? N1 Zn1 N3 149.0(2) . . ? C13 N1 C1 119.7(6) . . ? C13 N1 Zn1 110.5(4) . . ? C1 N1 Zn1 129.8(5) . . ? C18 N2 C14 117.8(6) . . ? C18 N2 Zn1 121.7(5) . . ? C14 N2 Zn1 120.5(5) . . ? C19 N3 C23 116.6(7) . . ? C19 N3 Zn1 114.5(5) . . ? C23 N3 Zn1 128.5(5) . . ? C6 C1 C2 126.6(7) . . ? C6 C1 N1 117.2(7) . . ? C2 C1 N1 116.1(6) . . ? C1 C2 C3 115.9(7) . . ? C1 C2 C10 125.9(7) . . ? C3 C2 C10 118.0(7) . . ? C4 C3 C2 120.3(7) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 118.2(8) . . ? C3 C4 H4 120.9 . . ? C5 C4 H4 120.9 . . ? C6 C5 C4 123.5(8) . . ? C6 C5 H5 118.3 . . ? C4 C5 H5 118.3 . . ? C5 C6 C1 115.2(8) . . ? C5 C6 C7 120.6(8) . . ? C1 C6 C7 124.1(7) . . ? C6 C7 C9 111.9(7) . . ? C6 C7 C8 109.6(6) . . ? C9 C7 C8 113.1(6) . . ? C6 C7 H7 107.3 . . ? C9 C7 H7 107.3 . . ? C8 C7 H7 107.3 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C2 C10 C12 115.4(6) . . ? C2 C10 C11 108.9(6) . . ? C12 C10 C11 112.3(6) . . ? C2 C10 H10 106.6 . . ? C12 C10 H10 106.6 . . ? C11 C10 H10 106.6 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 C14 122.1(6) . . ? N1 C13 H13 119.0 . . ? C14 C13 H13 119.0 . . ? N2 C14 C15 123.2(7) . . ? N2 C14 C13 112.0(6) . . ? C15 C14 C13 124.7(7) . . ? C16 C15 C14 117.6(7) . . ? C16 C15 H15 121.2 . . ? C14 C15 H15 121.2 . . ? C17 C16 C15 121.1(8) . . ? C17 C16 H16 119.5 . . ? C15 C16 H16 119.5 . . ? C16 C17 C18 118.0(8) . . ? C16 C17 H17 121.0 . . ? C18 C17 H17 121.0 . . ? N2 C18 C17 122.3(7) . . ? N2 C18 C19 114.2(6) . . ? C17 C18 C19 123.4(7) . . ? N3 C19 C20 124.9(7) . . ? N3 C19 C18 114.9(7) . . ? C20 C19 C18 120.1(7) . . ? C19 C20 C21 116.2(7) . . ? C19 C20 H20 121.9 . . ? C21 C20 H20 121.9 . . ? C22 C21 C20 120.0(7) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C21 C22 C23 118.7(8) . . ? C21 C22 H22 120.7 . . ? C23 C22 H22 120.7 . . ? N3 C23 C22 123.5(7) . . ? N3 C23 C24 115.6(7) . . ? C22 C23 C24 120.8(7) . . ? O1 C24 C23 124.3(7) . . ? O1 C24 H24 117.8 . . ? C23 C24 H24 117.8 . . ? 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 Zn1 N1 C13 -0.6(5) . . . . ? Cl1 Zn1 N1 C13 122.7(5) . . . . ? Cl2 Zn1 N1 C13 -117.2(5) . . . . ? N3 Zn1 N1 C13 -4.2(7) . . . . ? N2 Zn1 N1 C1 176.1(5) . . . . ? Cl1 Zn1 N1 C1 -60.6(5) . . . . ? Cl2 Zn1 N1 C1 59.4(5) . . . . ? N3 Zn1 N1 C1 172.5(4) . . . . ? Cl1 Zn1 N2 C18 88.7(5) . . . . ? Cl2 Zn1 N2 C18 -87.3(5) . . . . ? N1 Zn1 N2 C18 179.9(5) . . . . ? N3 Zn1 N2 C18 -2.0(5) . . . . ? Cl1 Zn1 N2 C14 -89.6(5) . . . . ? Cl2 Zn1 N2 C14 94.4(5) . . . . ? N1 Zn1 N2 C14 1.6(5) . . . . ? N3 Zn1 N2 C14 179.7(5) . . . . ? N2 Zn1 N3 C19 -2.7(5) . . . . ? Cl1 Zn1 N3 C19 -126.0(5) . . . . ? Cl2 Zn1 N3 C19 115.5(5) . . . . ? N1 Zn1 N3 C19 0.9(7) . . . . ? N2 Zn1 N3 C23 -174.9(6) . . . . ? Cl1 Zn1 N3 C23 61.7(6) . . . . ? Cl2 Zn1 N3 C23 -56.8(6) . . . . ? N1 Zn1 N3 C23 -171.3(5) . . . . ? C13 N1 C1 C6 85.7(8) . . . . ? Zn1 N1 C1 C6 -90.8(7) . . . . ? C13 N1 C1 C2 -98.1(8) . . . . ? Zn1 N1 C1 C2 85.5(7) . . . . ? C6 C1 C2 C3 -1.5(11) . . . . ? N1 C1 C2 C3 -177.3(6) . . . . ? C6 C1 C2 C10 -176.1(7) . . . . ? N1 C1 C2 C10 8.1(10) . . . . ? C1 C2 C3 C4 2.9(10) . . . . ? C10 C2 C3 C4 178.0(7) . . . . ? C2 C3 C4 C5 -5.1(11) . . . . ? C3 C4 C5 C6 6.0(12) . . . . ? C4 C5 C6 C1 -4.5(11) . . . . ? C4 C5 C6 C7 178.5(7) . . . . ? C2 C1 C6 C5 2.2(11) . . . . ? N1 C1 C6 C5 177.9(6) . . . . ? C2 C1 C6 C7 179.1(6) . . . . ? N1 C1 C6 C7 -5.2(10) . . . . ? C5 C6 C7 C9 -52.6(9) . . . . ? C1 C6 C7 C9 130.6(8) . . . . ? C5 C6 C7 C8 73.6(9) . . . . ? C1 C6 C7 C8 -103.1(8) . . . . ? C1 C2 C10 C12 -142.8(7) . . . . ? C3 C2 C10 C12 42.7(9) . . . . ? C1 C2 C10 C11 89.9(9) . . . . ? C3 C2 C10 C11 -84.7(8) . . . . ? C1 N1 C13 C14 -177.5(6) . . . . ? Zn1 N1 C13 C14 -0.4(8) . . . . ? C18 N2 C14 C15 -0.2(10) . . . . ? Zn1 N2 C14 C15 178.1(5) . . . . ? C18 N2 C14 C13 179.4(6) . . . . ? Zn1 N2 C14 C13 -2.3(7) . . . . ? N1 C13 C14 N2 1.7(10) . . . . ? N1 C13 C14 C15 -178.7(7) . . . . ? N2 C14 C15 C16 -0.2(11) . . . . ? C13 C14 C15 C16 -179.7(7) . . . . ? C14 C15 C16 C17 0.3(12) . . . . ? C15 C16 C17 C18 0.0(13) . . . . ? C14 N2 C18 C17 0.6(10) . . . . ? Zn1 N2 C18 C17 -177.8(5) . . . . ? C14 N2 C18 C19 -176.0(5) . . . . ? Zn1 N2 C18 C19 5.7(8) . . . . ? C16 C17 C18 N2 -0.5(12) . . . . ? C16 C17 C18 C19 175.7(7) . . . . ? C23 N3 C19 C20 1.9(10) . . . . ? Zn1 N3 C19 C20 -171.3(5) . . . . ? C23 N3 C19 C18 179.4(6) . . . . ? Zn1 N3 C19 C18 6.2(7) . . . . ? N2 C18 C19 N3 -7.8(9) . . . . ? C17 C18 C19 N3 175.7(7) . . . . ? N2 C18 C19 C20 169.8(6) . . . . ? C17 C18 C19 C20 -6.7(11) . . . . ? N3 C19 C20 C21 -1.8(11) . . . . ? C18 C19 C20 C21 -179.2(6) . . . . ? C19 C20 C21 C22 2.2(11) . . . . ? C20 C21 C22 C23 -2.7(12) . . . . ? C19 N3 C23 C22 -2.4(11) . . . . ? Zn1 N3 C23 C22 169.7(6) . . . . ? C19 N3 C23 C24 -178.7(7) . . . . ? Zn1 N3 C23 C24 -6.6(10) . . . . ? C21 C22 C23 N3 2.9(13) . . . . ? C21 C22 C23 C24 179.0(8) . . . . ? N3 C23 C24 O1 168.9(8) . . . . ? C22 C23 C24 O1 -7.5(15) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.482 _refine_diff_density_min -0.420 _refine_diff_density_rms 0.070 # Attachment '08015.cif' data_08015 _database_code_depnum_ccdc_archive 'CCDC 692760' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C38 H46 Cl4 N4 Zn2)2(C H Cl3)2(C4 H10 O)' _chemical_formula_sum 'C48 H68 Cl10 N4 O2 Zn2' _chemical_formula_weight 1218.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 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 24.436(8) _cell_length_b 14.694(5) _cell_length_c 16.839(6) _cell_angle_alpha 90.00 _cell_angle_beta 112.374(6) _cell_angle_gamma 90.00 _cell_volume 5591(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 757 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 23.268 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.447 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2520 _exptl_absorpt_coefficient_mu 1.376 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.572 _exptl_absorpt_correction_T_max 0.928 _exptl_absorpt_process_details ; absorption correction based on 2159 reflections(SADABS);Rint 0.0893 before correction and 0.0534 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 19671 _diffrn_reflns_av_R_equivalents 0.1937 _diffrn_reflns_av_sigmaI/netI 0.2868 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 24.99 _reflns_number_total 4910 _reflns_number_gt 1641 _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^)+(0.0916P)^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 4910 _refine_ls_number_parameters 222 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2068 _refine_ls_R_factor_gt 0.0808 _refine_ls_wR_factor_ref 0.2126 _refine_ls_wR_factor_gt 0.1782 _refine_ls_goodness_of_fit_ref 0.774 _refine_ls_restrained_S_all 0.774 _refine_ls_shift/su_max 0.000 _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 0.10051(5) 0.93517(8) 0.35911(6) 0.0499(4) Uani 1 1 d . . . Cl1 Cl 0.15336(12) 1.03175(18) 0.45932(14) 0.0661(9) Uani 1 1 d . . . Cl2 Cl 0.04183(12) 0.84415(19) 0.39091(14) 0.0672(8) Uani 1 1 d . . . N2 N 0.0646(3) 1.0069(5) 0.2460(4) 0.048(2) Uani 1 1 d . . . N1 N 0.1516(3) 0.8910(5) 0.2941(4) 0.049(2) Uani 1 1 d . . . C1 C 0.1946(5) 0.8196(8) 0.3278(6) 0.054(3) Uani 1 1 d . . . C2 C 0.2550(6) 0.8479(10) 0.3710(7) 0.071(4) Uani 1 1 d . . . C3 C 0.2943(5) 0.7763(9) 0.4099(6) 0.065(3) Uani 1 1 d . . . H3 H 0.3350 0.7905 0.4392 0.078 Uiso 1 1 calc R . . C4 C 0.2785(5) 0.6938(9) 0.4080(7) 0.072(3) Uani 1 1 d . . . H4 H 0.3068 0.6496 0.4395 0.087 Uiso 1 1 calc R . . C5 C 0.2166(7) 0.6646(8) 0.3574(8) 0.089(4) Uani 1 1 d . . . H5 H 0.2055 0.6022 0.3508 0.106 Uiso 1 1 calc R . . C6 C 0.1764(5) 0.7322(8) 0.3211(6) 0.061(3) Uani 1 1 d . . . C7 C 0.1105(5) 0.7042(10) 0.2712(7) 0.092(4) Uani 1 1 d . . . H7 H 0.0859 0.7574 0.2743 0.111 Uiso 1 1 calc R . . C8 C 0.0888(7) 0.6255(10) 0.3039(11) 0.163(8) Uani 1 1 d . . . H8A H 0.1120 0.5716 0.3025 0.245 Uiso 1 1 calc R . . H8B H 0.0471 0.6150 0.2680 0.245 Uiso 1 1 calc R . . H8C H 0.0928 0.6374 0.3631 0.245 Uiso 1 1 calc R . . C9 C 0.1030(6) 0.6953(12) 0.1720(8) 0.170(8) Uani 1 1 d . . . H9A H 0.1258 0.6429 0.1655 0.255 Uiso 1 1 calc R . . H9B H 0.1175 0.7508 0.1544 0.255 Uiso 1 1 calc R . . H9C H 0.0611 0.6867 0.1359 0.255 Uiso 1 1 calc R . . C10 C 0.2785(6) 0.9433(9) 0.3785(8) 0.096(4) Uani 1 1 d . . . H10 H 0.2445 0.9839 0.3460 0.115 Uiso 1 1 calc R . . C11 C 0.3055(6) 0.9789(10) 0.4709(8) 0.129(5) Uani 1 1 d . . . H11A H 0.2757 0.9767 0.4967 0.193 Uiso 1 1 calc R . . H11B H 0.3187 1.0418 0.4706 0.193 Uiso 1 1 calc R . . H11C H 0.3394 0.9409 0.5044 0.193 Uiso 1 1 calc R . . C12 C 0.3231(6) 0.9484(11) 0.3340(9) 0.138(6) Uani 1 1 d . . . H12A H 0.3543 0.9030 0.3593 0.207 Uiso 1 1 calc R . . H12B H 0.3408 1.0093 0.3419 0.207 Uiso 1 1 calc R . . H12C H 0.3027 0.9361 0.2725 0.207 Uiso 1 1 calc R . . C13 C 0.1432(4) 0.9328(7) 0.2234(5) 0.059(3) Uani 1 1 d . . . C14 C 0.1790(5) 0.9171(9) 0.1682(6) 0.099(5) Uani 1 1 d . . . H14A H 0.2015 0.8605 0.1858 0.148 Uiso 1 1 calc R . . H14B H 0.2063 0.9681 0.1753 0.148 Uiso 1 1 calc R . . H14C H 0.1522 0.9126 0.1078 0.148 Uiso 1 1 calc R . . C15 C 0.0937(4) 0.9963(6) 0.1933(6) 0.045(2) Uani 1 1 d . . . C16 C 0.0775(4) 1.0412(7) 0.1135(5) 0.059(3) Uani 1 1 d . . . H16 H 0.0984 1.0328 0.0767 0.070 Uiso 1 1 calc R . . C17 C 0.0290(4) 1.0980(7) 0.0927(5) 0.053(3) Uani 1 1 d . . . H17 H 0.0171 1.1318 0.0408 0.064 Uiso 1 1 calc R . . C18 C -0.0031(4) 1.1076(6) 0.1457(6) 0.051(3) Uani 1 1 d . . . H18 H -0.0373 1.1452 0.1296 0.061 Uiso 1 1 calc R . . C19 C 0.0168(4) 1.0608(7) 0.2215(5) 0.045(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0596(8) 0.0696(8) 0.0231(5) 0.0040(6) 0.0187(5) 0.0026(7) Cl1 0.075(2) 0.088(2) 0.0328(13) -0.0070(13) 0.0184(14) -0.0088(16) Cl2 0.088(2) 0.081(2) 0.0443(15) 0.0018(14) 0.0381(15) -0.0115(17) N2 0.054(5) 0.068(6) 0.036(4) 0.003(4) 0.034(4) 0.014(5) N1 0.058(5) 0.058(5) 0.028(4) 0.002(4) 0.013(4) 0.012(5) C1 0.067(9) 0.061(9) 0.035(6) 0.002(5) 0.021(6) 0.033(7) C2 0.067(9) 0.104(11) 0.062(7) 0.026(8) 0.046(7) 0.041(9) C3 0.060(9) 0.086(10) 0.062(7) -0.025(7) 0.038(7) -0.043(9) C4 0.045(8) 0.078(10) 0.081(9) 0.005(7) 0.010(7) -0.004(7) C5 0.133(13) 0.054(8) 0.096(9) -0.006(8) 0.063(10) 0.009(9) C6 0.101(10) 0.035(7) 0.051(6) 0.018(5) 0.032(7) 0.047(7) C7 0.037(8) 0.135(13) 0.068(8) -0.036(8) -0.020(6) 0.003(8) C8 0.132(14) 0.084(11) 0.219(18) 0.034(12) 0.006(13) -0.054(11) C9 0.094(11) 0.230(19) 0.108(12) -0.112(12) -0.048(9) 0.039(11) C10 0.089(10) 0.069(10) 0.111(11) 0.003(9) 0.019(9) -0.006(9) C11 0.089(10) 0.176(16) 0.093(11) -0.020(10) 0.002(9) -0.011(10) C12 0.111(11) 0.169(15) 0.156(13) 0.044(12) 0.074(11) -0.025(11) C13 0.078(8) 0.070(7) 0.037(5) 0.019(6) 0.032(6) 0.007(7) C14 0.077(8) 0.176(14) 0.047(6) 0.050(8) 0.027(6) 0.065(9) C15 0.038(6) 0.055(7) 0.041(6) -0.008(5) 0.013(5) 0.001(5) C16 0.042(6) 0.108(9) 0.022(5) 0.022(5) 0.008(5) 0.012(6) C17 0.057(7) 0.075(8) 0.024(5) 0.012(5) 0.011(5) 0.005(6) C18 0.049(6) 0.069(7) 0.048(6) 0.015(5) 0.033(5) 0.007(5) C19 0.050(6) 0.060(6) 0.027(5) -0.002(5) 0.015(4) -0.001(6) _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 N1 2.055(7) . ? Zn1 N2 2.057(7) . ? Zn1 Cl2 2.172(3) . ? Zn1 Cl1 2.207(3) . ? N2 C15 1.341(10) . ? N2 C19 1.341(10) . ? N1 C13 1.285(10) . ? N1 C1 1.439(11) . ? C1 C6 1.349(13) . ? C1 C2 1.437(15) . ? C2 C3 1.405(14) . ? C2 C10 1.502(16) . ? C3 C4 1.270(13) . ? C3 H3 0.9500 . ? C4 C5 1.488(15) . ? C4 H4 0.9500 . ? C5 C6 1.366(13) . ? C5 H5 0.9500 . ? C6 C7 1.561(15) . ? C7 C8 1.465(16) . ? C7 C9 1.615(16) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.532(15) . ? C10 C12 1.543(15) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C15 1.457(12) . ? C13 C14 1.516(12) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.412(11) . ? C16 C17 1.381(12) . ? C16 H16 0.9500 . ? C17 C18 1.402(11) . ? C17 H17 0.9500 . ? C18 C19 1.366(11) . ? C18 H18 0.9500 . ? C19 C19 1.482(15) 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 N1 Zn1 N2 78.5(3) . . ? N1 Zn1 Cl2 122.0(2) . . ? N2 Zn1 Cl2 117.1(2) . . ? N1 Zn1 Cl1 108.2(2) . . ? N2 Zn1 Cl1 107.3(2) . . ? Cl2 Zn1 Cl1 117.17(10) . . ? C15 N2 C19 118.9(7) . . ? C15 N2 Zn1 114.0(6) . . ? C19 N2 Zn1 127.1(5) . . ? C13 N1 C1 123.3(8) . . ? C13 N1 Zn1 115.3(7) . . ? C1 N1 Zn1 121.4(5) . . ? C6 C1 C2 124.0(11) . . ? C6 C1 N1 119.6(11) . . ? C2 C1 N1 116.4(11) . . ? C3 C2 C1 114.0(12) . . ? C3 C2 C10 119.2(12) . . ? C1 C2 C10 126.7(11) . . ? C4 C3 C2 123.7(12) . . ? C4 C3 H3 118.1 . . ? C2 C3 H3 118.1 . . ? C3 C4 C5 121.5(12) . . ? C3 C4 H4 119.2 . . ? C5 C4 H4 119.2 . . ? C6 C5 C4 116.6(11) . . ? C6 C5 H5 121.7 . . ? C4 C5 H5 121.7 . . ? C1 C6 C5 119.8(12) . . ? C1 C6 C7 122.3(10) . . ? C5 C6 C7 117.8(12) . . ? C8 C7 C6 116.9(11) . . ? C8 C7 C9 114.2(12) . . ? C6 C7 C9 105.4(10) . . ? C8 C7 H7 106.5 . . ? C6 C7 H7 106.5 . . ? C9 C7 H7 106.5 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C2 C10 C11 114.0(11) . . ? C2 C10 C12 108.8(11) . . ? C11 C10 C12 111.5(11) . . ? C2 C10 H10 107.4 . . ? C11 C10 H10 107.4 . . ? C12 C10 H10 107.4 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 C15 116.6(8) . . ? N1 C13 C14 124.7(10) . . ? C15 C13 C14 118.7(8) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N2 C15 C16 123.3(9) . . ? N2 C15 C13 115.0(8) . . ? C16 C15 C13 121.6(8) . . ? C17 C16 C15 115.2(8) . . ? C17 C16 H16 122.4 . . ? C15 C16 H16 122.4 . . ? C16 C17 C18 122.3(8) . . ? C16 C17 H17 118.9 . . ? C18 C17 H17 118.9 . . ? C19 C18 C17 117.2(9) . . ? C19 C18 H18 121.4 . . ? C17 C18 H18 121.4 . . ? N2 C19 C18 123.0(8) . . ? N2 C19 C19 115.6(7) . 2 ? C18 C19 C19 121.2(9) . 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 N1 Zn1 N2 C15 -5.3(6) . . . . ? Cl2 Zn1 N2 C15 -125.5(6) . . . . ? Cl1 Zn1 N2 C15 100.4(6) . . . . ? N1 Zn1 N2 C19 174.5(8) . . . . ? Cl2 Zn1 N2 C19 54.4(8) . . . . ? Cl1 Zn1 N2 C19 -79.8(8) . . . . ? N2 Zn1 N1 C13 7.4(7) . . . . ? Cl2 Zn1 N1 C13 122.2(7) . . . . ? Cl1 Zn1 N1 C13 -97.2(7) . . . . ? N2 Zn1 N1 C1 -174.0(8) . . . . ? Cl2 Zn1 N1 C1 -59.2(8) . . . . ? Cl1 Zn1 N1 C1 81.3(8) . . . . ? C13 N1 C1 C6 -103.9(11) . . . . ? Zn1 N1 C1 C6 77.6(10) . . . . ? C13 N1 C1 C2 79.1(11) . . . . ? Zn1 N1 C1 C2 -99.3(9) . . . . ? C6 C1 C2 C3 -2.7(13) . . . . ? N1 C1 C2 C3 174.1(7) . . . . ? C6 C1 C2 C10 178.0(10) . . . . ? N1 C1 C2 C10 -5.2(14) . . . . ? C1 C2 C3 C4 -0.4(15) . . . . ? C10 C2 C3 C4 179.0(11) . . . . ? C2 C3 C4 C5 5.1(17) . . . . ? C3 C4 C5 C6 -6.9(16) . . . . ? C2 C1 C6 C5 0.6(15) . . . . ? N1 C1 C6 C5 -176.1(8) . . . . ? C2 C1 C6 C7 -178.2(9) . . . . ? N1 C1 C6 C7 5.2(14) . . . . ? C4 C5 C6 C1 3.9(14) . . . . ? C4 C5 C6 C7 -177.2(9) . . . . ? C1 C6 C7 C8 -147.1(12) . . . . ? C5 C6 C7 C8 34.1(16) . . . . ? C1 C6 C7 C9 84.8(13) . . . . ? C5 C6 C7 C9 -94.0(12) . . . . ? C3 C2 C10 C11 -62.3(14) . . . . ? C1 C2 C10 C11 117.0(12) . . . . ? C3 C2 C10 C12 62.8(13) . . . . ? C1 C2 C10 C12 -118.0(12) . . . . ? C1 N1 C13 C15 173.4(9) . . . . ? Zn1 N1 C13 C15 -8.1(11) . . . . ? C1 N1 C13 C14 -3.5(16) . . . . ? Zn1 N1 C13 C14 175.0(9) . . . . ? C19 N2 C15 C16 1.8(14) . . . . ? Zn1 N2 C15 C16 -178.3(7) . . . . ? C19 N2 C15 C13 -177.0(8) . . . . ? Zn1 N2 C15 C13 2.9(10) . . . . ? N1 C13 C15 N2 3.4(13) . . . . ? C14 C13 C15 N2 -179.5(9) . . . . ? N1 C13 C15 C16 -175.4(9) . . . . ? C14 C13 C15 C16 1.7(14) . . . . ? N2 C15 C16 C17 0.2(14) . . . . ? C13 C15 C16 C17 178.9(9) . . . . ? C15 C16 C17 C18 -2.4(14) . . . . ? C16 C17 C18 C19 2.5(14) . . . . ? C15 N2 C19 C18 -1.7(14) . . . . ? Zn1 N2 C19 C18 178.4(7) . . . . ? C15 N2 C19 C19 173.3(8) . . . 2 ? Zn1 N2 C19 C19 -6.5(11) . . . 2 ? C17 C18 C19 N2 -0.4(14) . . . . ? C17 C18 C19 C19 -175.1(7) . . . 2 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.914 _refine_diff_density_min -0.569 _refine_diff_density_rms 0.117 # Attachment '08018.cif' data_08018 _database_code_depnum_ccdc_archive 'CCDC 692761' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ' C38 H46 Cl2 N4 Ni, 3(C H Cl3) ' _chemical_formula_sum 'C41 H49 Cl11 N4 Ni' _chemical_formula_weight 1046.50 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' Ni Ni 0.3393 1.1124 '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 10.8776(17) _cell_length_b 14.496(2) _cell_length_c 17.156(3) _cell_angle_alpha 65.944(3) _cell_angle_beta 88.962(3) _cell_angle_gamma 77.909(3) _cell_volume 2408.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 837 _cell_measurement_theta_min 2.427 _cell_measurement_theta_max 20.176 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.443 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1076 _exptl_absorpt_coefficient_mu 1.047 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.780 _exptl_absorpt_correction_T_max 0.928 _exptl_absorpt_process_details ; absorption correction based on 6971 reflections(SADABS);Rint 0.0492 before correction and 0.0293 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 19018 _diffrn_reflns_av_R_equivalents 0.0779 _diffrn_reflns_av_sigmaI/netI 0.1612 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9350 _reflns_number_gt 4830 _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^)+(0.0385P)^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 9350 _refine_ls_number_parameters 524 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1402 _refine_ls_R_factor_gt 0.0665 _refine_ls_wR_factor_ref 0.1371 _refine_ls_wR_factor_gt 0.1164 _refine_ls_goodness_of_fit_ref 0.886 _refine_ls_restrained_S_all 0.886 _refine_ls_shift/su_max 0.000 _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 0.71033(6) 0.08288(5) 0.29606(4) 0.02328(18) Uani 1 1 d . . . Cl1 Cl 0.90124(12) -0.04551(10) 0.31146(8) 0.0292(3) Uani 1 1 d . . . Cl2 Cl 0.51883(12) 0.20450(10) 0.29199(8) 0.0316(3) Uani 1 1 d . . . N1 N 0.6299(4) 0.0481(3) 0.1946(2) 0.0213(10) Uani 1 1 d . . . N2 N 0.6200(4) -0.0280(3) 0.3613(3) 0.0249(10) Uani 1 1 d . . . N3 N 0.7565(4) 0.0572(3) 0.4164(2) 0.0234(10) Uani 1 1 d . . . N4 N 0.8179(4) 0.2032(3) 0.2811(2) 0.0230(10) Uani 1 1 d . . . C1 C 0.6545(5) 0.0801(4) 0.1050(3) 0.0262(13) Uani 1 1 d . . . C2 C 0.7313(5) 0.0082(4) 0.0786(3) 0.0312(14) Uani 1 1 d . . . C3 C 0.7546(5) 0.0441(5) -0.0078(3) 0.0357(15) Uani 1 1 d . . . H3 H 0.8073 -0.0018 -0.0275 0.043 Uiso 1 1 calc R . . C4 C 0.7042(5) 0.1426(5) -0.0645(3) 0.0399(16) Uani 1 1 d . . . H4 H 0.7206 0.1641 -0.1231 0.048 Uiso 1 1 calc R . . C5 C 0.6297(5) 0.2113(4) -0.0376(3) 0.0341(14) Uani 1 1 d . . . H5 H 0.5956 0.2802 -0.0777 0.041 Uiso 1 1 calc R . . C6 C 0.6038(5) 0.1807(4) 0.0482(3) 0.0277(13) Uani 1 1 d . . . C7 C 0.5180(6) 0.2552(4) 0.0765(3) 0.0399(16) Uani 1 1 d . . . H7 H 0.5378 0.2300 0.1394 0.048 Uiso 1 1 calc R . . C8 C 0.5360(6) 0.3659(4) 0.0349(4) 0.0497(18) Uani 1 1 d . . . H8A H 0.6255 0.3658 0.0408 0.074 Uiso 1 1 calc R . . H8B H 0.4868 0.4067 0.0630 0.074 Uiso 1 1 calc R . . H8C H 0.5074 0.3964 -0.0260 0.074 Uiso 1 1 calc R . . C9 C 0.3815(6) 0.2538(5) 0.0639(5) 0.070(2) Uani 1 1 d . . . H9A H 0.3625 0.2652 0.0046 0.105 Uiso 1 1 calc R . . H9B H 0.3274 0.3088 0.0760 0.105 Uiso 1 1 calc R . . H9C H 0.3659 0.1865 0.1029 0.105 Uiso 1 1 calc R . . C10 C 0.7913(5) -0.1027(4) 0.1373(4) 0.0402(15) Uani 1 1 d . . . H10 H 0.7661 -0.1151 0.1965 0.048 Uiso 1 1 calc R . . C11 C 0.9352(5) -0.1227(5) 0.1396(4) 0.0464(17) Uani 1 1 d . . . H11A H 0.9617 -0.1051 0.0813 0.070 Uiso 1 1 calc R . . H11B H 0.9710 -0.1960 0.1752 0.070 Uiso 1 1 calc R . . H11C H 0.9650 -0.0799 0.1637 0.070 Uiso 1 1 calc R . . C12 C 0.7456(6) -0.1791(5) 0.1109(4) 0.0507(18) Uani 1 1 d . . . H12A H 0.6533 -0.1650 0.1081 0.076 Uiso 1 1 calc R . . H12B H 0.7798 -0.2500 0.1530 0.076 Uiso 1 1 calc R . . H12C H 0.7743 -0.1715 0.0545 0.076 Uiso 1 1 calc R . . C13 C 0.5532(5) -0.0110(4) 0.2240(3) 0.0277(13) Uani 1 1 d . . . C14 C 0.4711(5) -0.0436(4) 0.1742(3) 0.0372(15) Uani 1 1 d . . . H14A H 0.4785 -0.0063 0.1128 0.056 Uiso 1 1 calc R . . H14B H 0.3831 -0.0274 0.1871 0.056 Uiso 1 1 calc R . . H14C H 0.4985 -0.1183 0.1906 0.056 Uiso 1 1 calc R . . C15 C 0.5429(5) -0.0559(4) 0.3197(3) 0.0255(13) Uani 1 1 d . . . C16 C 0.4689(5) -0.1233(4) 0.3639(3) 0.0323(14) Uani 1 1 d . . . H16 H 0.4123 -0.1421 0.3344 0.039 Uiso 1 1 calc R . . C17 C 0.4784(5) -0.1636(4) 0.4529(4) 0.0403(16) Uani 1 1 d . . . H17 H 0.4291 -0.2115 0.4847 0.048 Uiso 1 1 calc R . . C18 C 0.5590(5) -0.1345(4) 0.4952(3) 0.0331(14) Uani 1 1 d . . . H18 H 0.5667 -0.1624 0.5560 0.040 Uiso 1 1 calc R . . C19 C 0.6284(5) -0.0636(4) 0.4471(3) 0.0287(13) Uani 1 1 d . . . C20 C 0.7138(5) -0.0176(4) 0.4788(3) 0.0267(13) Uani 1 1 d . . . C21 C 0.7497(5) -0.0446(4) 0.5646(3) 0.0361(15) Uani 1 1 d . . . H21 H 0.7192 -0.0967 0.6099 0.043 Uiso 1 1 calc R . . C22 C 0.8315(5) 0.0078(5) 0.5803(3) 0.0399(16) Uani 1 1 d . . . H22 H 0.8583 -0.0092 0.6378 0.048 Uiso 1 1 calc R . . C23 C 0.8757(5) 0.0843(4) 0.5148(3) 0.0326(14) Uani 1 1 d . . . H23 H 0.9322 0.1196 0.5267 0.039 Uiso 1 1 calc R . . C24 C 0.8357(5) 0.1078(4) 0.4319(3) 0.0287(13) Uani 1 1 d . . . C25 C 0.8663(5) 0.1913(4) 0.3534(3) 0.0253(12) Uani 1 1 d . . . C26 C 0.9519(5) 0.2530(4) 0.3673(3) 0.0364(15) Uani 1 1 d . . . H26A H 0.9693 0.3034 0.3118 0.055 Uiso 1 1 calc R . . H26B H 1.0312 0.2063 0.3978 0.055 Uiso 1 1 calc R . . H26C H 0.9111 0.2895 0.4012 0.055 Uiso 1 1 calc R . . C27 C 0.8282(5) 0.2951(4) 0.2053(3) 0.0268(13) Uani 1 1 d . . . C28 C 0.7672(5) 0.3938(4) 0.1990(3) 0.0301(14) Uani 1 1 d . . . C29 C 0.7742(5) 0.4795(5) 0.1243(4) 0.0386(15) Uani 1 1 d . . . H29 H 0.7324 0.5467 0.1185 0.046 Uiso 1 1 calc R . . C30 C 0.8412(6) 0.4683(5) 0.0582(4) 0.0445(17) Uani 1 1 d . . . H30 H 0.8470 0.5277 0.0080 0.053 Uiso 1 1 calc R . . C31 C 0.8989(5) 0.3717(5) 0.0653(3) 0.0393(16) Uani 1 1 d . . . H31 H 0.9431 0.3651 0.0189 0.047 Uiso 1 1 calc R . . C32 C 0.8951(5) 0.2826(4) 0.1382(3) 0.0304(14) Uani 1 1 d . . . C33 C 0.9623(6) 0.1786(5) 0.1453(4) 0.0424(16) Uani 1 1 d . . . H33 H 0.9165 0.1266 0.1845 0.051 Uiso 1 1 calc R . . C34 C 1.0962(6) 0.1517(5) 0.1857(4) 0.0577(19) Uani 1 1 d . . . H34A H 1.1446 0.1995 0.1473 0.087 Uiso 1 1 calc R . . H34B H 1.1367 0.0806 0.1951 0.087 Uiso 1 1 calc R . . H34C H 1.0931 0.1577 0.2406 0.087 Uiso 1 1 calc R . . C35 C 0.9662(6) 0.1686(5) 0.0600(4) 0.0574(19) Uani 1 1 d . . . H35A H 0.8807 0.1912 0.0322 0.086 Uiso 1 1 calc R . . H35B H 1.0002 0.0961 0.0701 0.086 Uiso 1 1 calc R . . H35C H 1.0201 0.2120 0.0229 0.086 Uiso 1 1 calc R . . C36 C 0.6884(5) 0.4132(4) 0.2673(3) 0.0330(14) Uani 1 1 d . . . H36 H 0.6924 0.3455 0.3175 0.040 Uiso 1 1 calc R . . C37 C 0.5513(5) 0.4604(5) 0.2312(4) 0.0480(17) Uani 1 1 d . . . H37A H 0.5445 0.5310 0.1873 0.072 Uiso 1 1 calc R . . H37B H 0.4981 0.4625 0.2775 0.072 Uiso 1 1 calc R . . H37C H 0.5234 0.4182 0.2058 0.072 Uiso 1 1 calc R . . C38 C 0.7356(6) 0.4861(5) 0.2973(4) 0.0517(18) Uani 1 1 d . . . H38A H 0.8255 0.4593 0.3157 0.078 Uiso 1 1 calc R . . H38B H 0.6886 0.4907 0.3453 0.078 Uiso 1 1 calc R . . H38C H 0.7229 0.5550 0.2501 0.078 Uiso 1 1 calc R . . C39 C 0.2392(6) 0.4359(5) 0.2266(4) 0.059(2) Uani 1 1 d . . . H39 H 0.3233 0.3984 0.2185 0.071 Uiso 1 1 calc R . . Cl3 Cl 0.22514(17) 0.40216(15) 0.33540(11) 0.0655(5) Uani 1 1 d . . . Cl4 Cl 0.22882(19) 0.57048(17) 0.17289(13) 0.0847(7) Uani 1 1 d . . . Cl5 Cl 0.1216(2) 0.4031(2) 0.18214(13) 0.0992(8) Uani 1 1 d . . . C40 C 0.2824(6) 0.6554(5) 0.3609(4) 0.065(2) Uani 1 1 d . . . H40 H 0.2371 0.6129 0.3432 0.078 Uiso 1 1 calc R . . Cl6 Cl 0.3137(3) 0.5961(2) 0.46931(16) 0.1566(13) Uani 1 1 d . . . Cl7 Cl 0.42419(18) 0.66240(16) 0.30941(14) 0.0814(7) Uani 1 1 d . . . Cl8 Cl 0.18637(16) 0.77840(14) 0.32982(13) 0.0658(5) Uani 1 1 d . . . C41 C 0.8881(5) 0.6957(5) 0.3783(4) 0.0431(16) Uani 1 1 d . . . H41 H 0.9016 0.7669 0.3435 0.052 Uiso 1 1 calc R . . Cl9 Cl 0.72684(16) 0.69815(14) 0.36763(12) 0.0636(5) Uani 1 1 d . . . Cl10 Cl 0.97562(15) 0.61096(13) 0.33837(12) 0.0590(5) Uani 1 1 d . . . Cl11 Cl 0.9365(2) 0.66056(18) 0.48383(11) 0.0931(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0257(4) 0.0271(4) 0.0183(4) -0.0099(3) 0.0044(3) -0.0076(3) Cl1 0.0294(8) 0.0307(8) 0.0275(7) -0.0134(7) 0.0035(6) -0.0038(7) Cl2 0.0339(8) 0.0338(9) 0.0244(7) -0.0114(7) 0.0063(6) -0.0032(7) N1 0.018(2) 0.025(3) 0.020(2) -0.009(2) 0.0041(19) -0.005(2) N2 0.033(3) 0.019(3) 0.019(2) -0.006(2) 0.007(2) -0.004(2) N3 0.030(3) 0.023(3) 0.015(2) -0.009(2) 0.0053(19) 0.000(2) N4 0.021(2) 0.030(3) 0.017(2) -0.010(2) 0.0015(19) -0.004(2) C1 0.026(3) 0.037(3) 0.023(3) -0.017(3) 0.000(2) -0.012(3) C2 0.039(4) 0.036(4) 0.025(3) -0.018(3) 0.006(3) -0.012(3) C3 0.035(4) 0.047(4) 0.032(3) -0.025(3) 0.007(3) -0.006(3) C4 0.047(4) 0.056(4) 0.018(3) -0.014(3) 0.001(3) -0.016(4) C5 0.045(4) 0.032(3) 0.019(3) -0.004(3) 0.000(3) -0.011(3) C6 0.028(3) 0.032(3) 0.027(3) -0.014(3) 0.001(2) -0.007(3) C7 0.058(4) 0.037(4) 0.017(3) -0.009(3) -0.001(3) 0.003(3) C8 0.059(4) 0.042(4) 0.048(4) -0.020(3) -0.012(3) -0.007(4) C9 0.052(5) 0.035(4) 0.109(6) -0.019(4) 0.037(4) -0.008(4) C10 0.048(4) 0.043(4) 0.031(3) -0.019(3) 0.012(3) -0.003(3) C11 0.056(4) 0.050(4) 0.036(4) -0.026(3) 0.001(3) 0.001(3) C12 0.065(5) 0.043(4) 0.051(4) -0.027(4) 0.014(4) -0.011(4) C13 0.032(3) 0.025(3) 0.026(3) -0.015(3) 0.000(3) 0.003(3) C14 0.041(4) 0.044(4) 0.035(3) -0.019(3) 0.006(3) -0.019(3) C15 0.023(3) 0.025(3) 0.027(3) -0.010(3) 0.006(2) -0.006(3) C16 0.029(3) 0.033(4) 0.038(4) -0.017(3) 0.012(3) -0.009(3) C17 0.042(4) 0.028(4) 0.046(4) -0.007(3) 0.022(3) -0.015(3) C18 0.034(3) 0.029(3) 0.026(3) -0.005(3) 0.013(3) -0.001(3) C19 0.033(3) 0.020(3) 0.023(3) -0.003(3) 0.010(3) 0.002(3) C20 0.030(3) 0.023(3) 0.025(3) -0.011(3) 0.003(3) 0.002(3) C21 0.048(4) 0.033(4) 0.019(3) -0.007(3) 0.001(3) 0.001(3) C22 0.052(4) 0.044(4) 0.020(3) -0.016(3) -0.010(3) 0.005(3) C23 0.038(4) 0.035(4) 0.024(3) -0.015(3) -0.002(3) 0.000(3) C24 0.029(3) 0.032(3) 0.032(3) -0.024(3) -0.004(3) 0.004(3) C25 0.025(3) 0.022(3) 0.028(3) -0.012(3) 0.004(2) 0.000(3) C26 0.034(3) 0.040(4) 0.035(3) -0.017(3) -0.009(3) -0.005(3) C27 0.027(3) 0.033(3) 0.025(3) -0.012(3) 0.003(2) -0.015(3) C28 0.025(3) 0.034(4) 0.031(3) -0.010(3) 0.003(3) -0.014(3) C29 0.043(4) 0.031(4) 0.039(4) -0.010(3) 0.002(3) -0.011(3) C30 0.049(4) 0.038(4) 0.042(4) -0.006(3) 0.009(3) -0.023(3) C31 0.037(4) 0.055(4) 0.028(3) -0.014(3) 0.016(3) -0.024(3) C32 0.030(3) 0.039(4) 0.026(3) -0.014(3) 0.008(3) -0.014(3) C33 0.055(4) 0.043(4) 0.034(4) -0.016(3) 0.020(3) -0.022(3) C34 0.067(5) 0.060(5) 0.043(4) -0.025(4) 0.008(4) 0.000(4) C35 0.060(5) 0.075(5) 0.058(5) -0.047(4) 0.017(4) -0.020(4) C36 0.040(4) 0.028(3) 0.031(3) -0.012(3) 0.001(3) -0.007(3) C37 0.047(4) 0.049(4) 0.048(4) -0.024(3) 0.011(3) -0.003(3) C38 0.059(5) 0.046(4) 0.050(4) -0.023(4) 0.001(3) -0.006(4) C39 0.053(4) 0.089(6) 0.053(4) -0.036(4) 0.021(4) -0.041(4) Cl3 0.0699(13) 0.0818(14) 0.0502(11) -0.0325(10) 0.0128(9) -0.0178(11) Cl4 0.0836(15) 0.0919(17) 0.0691(14) -0.0148(12) 0.0000(11) -0.0376(13) Cl5 0.0957(17) 0.176(2) 0.0723(14) -0.0669(16) 0.0365(12) -0.0956(17) C40 0.044(4) 0.062(5) 0.084(6) -0.024(4) -0.002(4) -0.016(4) Cl6 0.145(3) 0.167(3) 0.0755(18) 0.0203(18) 0.0008(17) -0.010(2) Cl7 0.0574(13) 0.0838(15) 0.1305(19) -0.0717(15) 0.0244(12) -0.0170(11) Cl8 0.0439(11) 0.0638(13) 0.1013(15) -0.0460(12) 0.0068(10) -0.0113(10) C41 0.053(4) 0.040(4) 0.044(4) -0.020(3) 0.005(3) -0.018(3) Cl9 0.0455(11) 0.0604(12) 0.0898(14) -0.0371(11) 0.0163(10) -0.0101(9) Cl10 0.0453(10) 0.0538(11) 0.0898(14) -0.0419(11) 0.0077(10) -0.0102(9) Cl11 0.134(2) 0.1153(19) 0.0395(11) -0.0260(12) 0.0024(12) -0.0595(16) _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 1.989(4) . ? Ni1 N3 1.997(4) . ? Ni1 N4 2.226(4) . ? Ni1 N1 2.238(4) . ? Ni1 Cl2 2.4121(15) . ? Ni1 Cl1 2.4178(15) . ? N1 C13 1.271(6) . ? N1 C1 1.451(6) . ? N2 C15 1.332(6) . ? N2 C19 1.344(6) . ? N3 C24 1.335(6) . ? N3 C20 1.336(6) . ? N4 C25 1.288(6) . ? N4 C27 1.457(6) . ? C1 C6 1.381(7) . ? C1 C2 1.412(7) . ? C2 C3 1.395(7) . ? C2 C10 1.513(7) . ? C3 C4 1.358(7) . ? C3 H3 0.9500 . ? C4 C5 1.373(7) . ? C4 H4 0.9500 . ? C5 C6 1.395(7) . ? C5 H5 0.9500 . ? C6 C7 1.503(7) . ? C7 C9 1.510(8) . ? C7 C8 1.522(7) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C12 1.527(7) . ? C10 C11 1.529(7) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.511(7) . ? C13 C15 1.512(7) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.372(7) . ? C16 C17 1.391(7) . ? C16 H16 0.9500 . ? C17 C18 1.379(7) . ? C17 H17 0.9500 . ? C18 C19 1.386(7) . ? C18 H18 0.9500 . ? C19 C20 1.475(7) . ? C20 C21 1.399(7) . ? C21 C22 1.378(7) . ? C21 H21 0.9500 . ? C22 C23 1.382(7) . ? C22 H22 0.9500 . ? C23 C24 1.376(6) . ? C23 H23 0.9500 . ? C24 C25 1.488(7) . ? C25 C26 1.501(7) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C32 1.404(7) . ? C27 C28 1.407(7) . ? C28 C29 1.390(7) . ? C28 C36 1.522(7) . ? C29 C30 1.383(7) . ? C29 H29 0.9500 . ? C30 C31 1.365(8) . ? C30 H30 0.9500 . ? C31 C32 1.392(7) . ? C31 H31 0.9500 . ? C32 C33 1.488(8) . ? C33 C34 1.526(8) . ? C33 C35 1.528(7) . ? C33 H33 1.0000 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C38 1.524(7) . ? C36 C37 1.528(7) . ? C36 H36 1.0000 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 Cl3 1.739(6) . ? C39 Cl5 1.740(6) . ? C39 Cl4 1.764(7) . ? C39 H39 1.0000 . ? C40 Cl6 1.706(7) . ? C40 Cl8 1.738(7) . ? C40 Cl7 1.764(7) . ? C40 H40 1.0000 . ? C41 Cl11 1.728(6) . ? C41 Cl10 1.748(6) . ? C41 Cl9 1.758(6) . ? C41 H41 1.0000 . ? 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 78.76(17) . . ? N2 Ni1 N4 154.62(16) . . ? N3 Ni1 N4 76.34(16) . . ? N2 Ni1 N1 76.43(16) . . ? N3 Ni1 N1 154.73(16) . . ? N4 Ni1 N1 128.76(15) . . ? N2 Ni1 Cl2 86.63(12) . . ? N3 Ni1 Cl2 90.97(12) . . ? N4 Ni1 Cl2 88.92(11) . . ? N1 Ni1 Cl2 92.32(11) . . ? N2 Ni1 Cl1 90.64(12) . . ? N3 Ni1 Cl1 85.30(12) . . ? N4 Ni1 Cl1 92.17(11) . . ? N1 Ni1 Cl1 90.21(11) . . ? Cl2 Ni1 Cl1 175.75(5) . . ? C13 N1 C1 118.1(4) . . ? C13 N1 Ni1 111.7(3) . . ? C1 N1 Ni1 130.2(3) . . ? C15 N2 C19 122.1(5) . . ? C15 N2 Ni1 119.8(3) . . ? C19 N2 Ni1 117.6(4) . . ? C24 N3 C20 122.6(5) . . ? C24 N3 Ni1 119.9(4) . . ? C20 N3 Ni1 117.2(3) . . ? C25 N4 C27 118.2(4) . . ? C25 N4 Ni1 112.0(3) . . ? C27 N4 Ni1 129.5(3) . . ? C6 C1 C2 121.9(5) . . ? C6 C1 N1 118.9(5) . . ? C2 C1 N1 119.2(5) . . ? C3 C2 C1 116.7(5) . . ? C3 C2 C10 118.4(5) . . ? C1 C2 C10 124.8(5) . . ? C4 C3 C2 122.0(5) . . ? C4 C3 H3 119.0 . . ? C2 C3 H3 119.0 . . ? C3 C4 C5 120.4(5) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C4 C5 C6 120.6(5) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C1 C6 C5 118.5(5) . . ? C1 C6 C7 121.3(5) . . ? C5 C6 C7 120.2(5) . . ? C6 C7 C9 111.2(5) . . ? C6 C7 C8 114.6(5) . . ? C9 C7 C8 110.0(5) . . ? C6 C7 H7 106.9 . . ? C9 C7 H7 106.9 . . ? C8 C7 H7 106.9 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C2 C10 C12 111.5(5) . . ? C2 C10 C11 111.5(5) . . ? C12 C10 C11 109.6(5) . . ? C2 C10 H10 108.1 . . ? C12 C10 H10 108.1 . . ? C11 C10 H10 108.1 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 C14 127.4(5) . . ? N1 C13 C15 117.3(5) . . ? C14 C13 C15 115.3(5) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N2 C15 C16 120.5(5) . . ? N2 C15 C13 113.3(5) . . ? C16 C15 C13 126.1(5) . . ? C15 C16 C17 118.6(5) . . ? C15 C16 H16 120.7 . . ? C17 C16 H16 120.7 . . ? C18 C17 C16 120.3(5) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C17 C18 C19 118.5(5) . . ? C17 C18 H18 120.8 . . ? C19 C18 H18 120.8 . . ? N2 C19 C18 119.9(5) . . ? N2 C19 C20 112.8(5) . . ? C18 C19 C20 127.3(5) . . ? N3 C20 C21 120.2(5) . . ? N3 C20 C19 113.4(4) . . ? C21 C20 C19 126.4(5) . . ? C22 C21 C20 117.0(5) . . ? C22 C21 H21 121.5 . . ? C20 C21 H21 121.5 . . ? C21 C22 C23 122.0(5) . . ? C21 C22 H22 119.0 . . ? C23 C22 H22 119.0 . . ? C24 C23 C22 118.1(5) . . ? C24 C23 H23 120.9 . . ? C22 C23 H23 120.9 . . ? N3 C24 C23 120.1(5) . . ? N3 C24 C25 113.6(4) . . ? C23 C24 C25 126.2(5) . . ? N4 C25 C24 117.4(5) . . ? N4 C25 C26 126.7(5) . . ? C24 C25 C26 115.9(5) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C32 C27 C28 121.3(5) . . ? C32 C27 N4 118.9(5) . . ? C28 C27 N4 119.8(5) . . ? C29 C28 C27 118.3(5) . . ? C29 C28 C36 117.3(5) . . ? C27 C28 C36 124.3(5) . . ? C30 C29 C28 120.9(6) . . ? C30 C29 H29 119.5 . . ? C28 C29 H29 119.5 . . ? C31 C30 C29 119.8(6) . . ? C31 C30 H30 120.1 . . ? C29 C30 H30 120.1 . . ? C30 C31 C32 122.3(6) . . ? C30 C31 H31 118.9 . . ? C32 C31 H31 118.9 . . ? C31 C32 C27 117.4(5) . . ? C31 C32 C33 121.1(5) . . ? C27 C32 C33 121.5(5) . . ? C32 C33 C34 110.2(5) . . ? C32 C33 C35 113.6(5) . . ? C34 C33 C35 109.8(5) . . ? C32 C33 H33 107.7 . . ? C34 C33 H33 107.7 . . ? C35 C33 H33 107.7 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C28 C36 C38 111.9(5) . . ? C28 C36 C37 109.3(4) . . ? C38 C36 C37 109.0(5) . . ? C28 C36 H36 108.8 . . ? C38 C36 H36 108.8 . . ? C37 C36 H36 108.8 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? Cl3 C39 Cl5 111.3(3) . . ? Cl3 C39 Cl4 109.8(4) . . ? Cl5 C39 Cl4 109.0(4) . . ? Cl3 C39 H39 108.9 . . ? Cl5 C39 H39 108.9 . . ? Cl4 C39 H39 108.9 . . ? Cl6 C40 Cl8 111.1(4) . . ? Cl6 C40 Cl7 110.3(4) . . ? Cl8 C40 Cl7 110.4(4) . . ? Cl6 C40 H40 108.3 . . ? Cl8 C40 H40 108.3 . . ? Cl7 C40 H40 108.3 . . ? Cl11 C41 Cl10 111.1(3) . . ? Cl11 C41 Cl9 110.7(3) . . ? Cl10 C41 Cl9 109.6(3) . . ? Cl11 C41 H41 108.4 . . ? Cl10 C41 H41 108.4 . . ? Cl9 C41 H41 108.4 . . ? 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 C13 9.6(3) . . . . ? N3 Ni1 N1 C13 20.9(6) . . . . ? N4 Ni1 N1 C13 -166.8(3) . . . . ? Cl2 Ni1 N1 C13 -76.3(3) . . . . ? Cl1 Ni1 N1 C13 100.2(3) . . . . ? N2 Ni1 N1 C1 -168.7(4) . . . . ? N3 Ni1 N1 C1 -157.5(4) . . . . ? N4 Ni1 N1 C1 14.8(5) . . . . ? Cl2 Ni1 N1 C1 105.3(4) . . . . ? Cl1 Ni1 N1 C1 -78.1(4) . . . . ? N3 Ni1 N2 C15 173.7(4) . . . . ? N4 Ni1 N2 C15 162.4(4) . . . . ? N1 Ni1 N2 C15 -11.1(4) . . . . ? Cl2 Ni1 N2 C15 82.1(4) . . . . ? Cl1 Ni1 N2 C15 -101.2(4) . . . . ? N3 Ni1 N2 C19 1.4(4) . . . . ? N4 Ni1 N2 C19 -10.0(6) . . . . ? N1 Ni1 N2 C19 176.5(4) . . . . ? Cl2 Ni1 N2 C19 -90.3(4) . . . . ? Cl1 Ni1 N2 C19 86.5(4) . . . . ? N2 Ni1 N3 C24 176.7(4) . . . . ? N4 Ni1 N3 C24 -8.3(4) . . . . ? N1 Ni1 N3 C24 165.5(3) . . . . ? Cl2 Ni1 N3 C24 -97.0(4) . . . . ? Cl1 Ni1 N3 C24 85.1(4) . . . . ? N2 Ni1 N3 C20 2.3(4) . . . . ? N4 Ni1 N3 C20 177.3(4) . . . . ? N1 Ni1 N3 C20 -8.9(6) . . . . ? Cl2 Ni1 N3 C20 88.6(3) . . . . ? Cl1 Ni1 N3 C20 -89.3(3) . . . . ? N2 Ni1 N4 C25 18.0(6) . . . . ? N3 Ni1 N4 C25 6.5(3) . . . . ? N1 Ni1 N4 C25 -170.1(3) . . . . ? Cl2 Ni1 N4 C25 97.8(3) . . . . ? Cl1 Ni1 N4 C25 -78.1(3) . . . . ? N2 Ni1 N4 C27 -154.9(4) . . . . ? N3 Ni1 N4 C27 -166.3(4) . . . . ? N1 Ni1 N4 C27 17.1(5) . . . . ? Cl2 Ni1 N4 C27 -75.1(4) . . . . ? Cl1 Ni1 N4 C27 109.1(4) . . . . ? C13 N1 C1 C6 106.6(6) . . . . ? Ni1 N1 C1 C6 -75.1(6) . . . . ? C13 N1 C1 C2 -74.5(6) . . . . ? Ni1 N1 C1 C2 103.8(5) . . . . ? C6 C1 C2 C3 0.6(8) . . . . ? N1 C1 C2 C3 -178.3(5) . . . . ? C6 C1 C2 C10 179.2(5) . . . . ? N1 C1 C2 C10 0.3(8) . . . . ? C1 C2 C3 C4 -1.3(8) . . . . ? C10 C2 C3 C4 180.0(5) . . . . ? C2 C3 C4 C5 1.3(9) . . . . ? C3 C4 C5 C6 -0.6(9) . . . . ? C2 C1 C6 C5 0.1(8) . . . . ? N1 C1 C6 C5 179.0(4) . . . . ? C2 C1 C6 C7 177.5(5) . . . . ? N1 C1 C6 C7 -3.6(7) . . . . ? C4 C5 C6 C1 -0.1(8) . . . . ? C4 C5 C6 C7 -177.6(5) . . . . ? C1 C6 C7 C9 -92.3(6) . . . . ? C5 C6 C7 C9 85.1(7) . . . . ? C1 C6 C7 C8 142.3(5) . . . . ? C5 C6 C7 C8 -40.3(7) . . . . ? C3 C2 C10 C12 -62.2(7) . . . . ? C1 C2 C10 C12 119.2(6) . . . . ? C3 C2 C10 C11 60.6(7) . . . . ? C1 C2 C10 C11 -118.0(6) . . . . ? C1 N1 C13 C14 -7.6(8) . . . . ? Ni1 N1 C13 C14 173.8(4) . . . . ? C1 N1 C13 C15 171.4(4) . . . . ? Ni1 N1 C13 C15 -7.2(5) . . . . ? C19 N2 C15 C16 -0.3(8) . . . . ? Ni1 N2 C15 C16 -172.3(4) . . . . ? C19 N2 C15 C13 -177.2(4) . . . . ? Ni1 N2 C15 C13 10.8(6) . . . . ? N1 C13 C15 N2 -1.3(7) . . . . ? C14 C13 C15 N2 177.8(4) . . . . ? N1 C13 C15 C16 -178.0(5) . . . . ? C14 C13 C15 C16 1.2(8) . . . . ? N2 C15 C16 C17 -1.5(8) . . . . ? C13 C15 C16 C17 174.9(5) . . . . ? C15 C16 C17 C18 1.3(8) . . . . ? C16 C17 C18 C19 0.8(8) . . . . ? C15 N2 C19 C18 2.5(7) . . . . ? Ni1 N2 C19 C18 174.6(4) . . . . ? C15 N2 C19 C20 -176.5(4) . . . . ? Ni1 N2 C19 C20 -4.3(6) . . . . ? C17 C18 C19 N2 -2.6(8) . . . . ? C17 C18 C19 C20 176.2(5) . . . . ? C24 N3 C20 C21 1.3(7) . . . . ? Ni1 N3 C20 C21 175.5(4) . . . . ? C24 N3 C20 C19 -179.3(4) . . . . ? Ni1 N3 C20 C19 -5.1(5) . . . . ? N2 C19 C20 N3 6.0(6) . . . . ? C18 C19 C20 N3 -172.8(5) . . . . ? N2 C19 C20 C21 -174.6(5) . . . . ? C18 C19 C20 C21 6.5(9) . . . . ? N3 C20 C21 C22 -1.2(8) . . . . ? C19 C20 C21 C22 179.5(5) . . . . ? C20 C21 C22 C23 0.5(8) . . . . ? C21 C22 C23 C24 0.1(8) . . . . ? C20 N3 C24 C23 -0.6(7) . . . . ? Ni1 N3 C24 C23 -174.7(4) . . . . ? C20 N3 C24 C25 -177.2(4) . . . . ? Ni1 N3 C24 C25 8.7(6) . . . . ? C22 C23 C24 N3 0.0(8) . . . . ? C22 C23 C24 C25 176.1(5) . . . . ? C27 N4 C25 C24 169.5(4) . . . . ? Ni1 N4 C25 C24 -4.2(5) . . . . ? C27 N4 C25 C26 -10.9(7) . . . . ? Ni1 N4 C25 C26 175.4(4) . . . . ? N3 C24 C25 N4 -2.2(7) . . . . ? C23 C24 C25 N4 -178.5(5) . . . . ? N3 C24 C25 C26 178.2(4) . . . . ? C23 C24 C25 C26 1.8(7) . . . . ? C25 N4 C27 C32 117.9(5) . . . . ? Ni1 N4 C27 C32 -69.7(6) . . . . ? C25 N4 C27 C28 -64.6(6) . . . . ? Ni1 N4 C27 C28 107.8(5) . . . . ? C32 C27 C28 C29 0.3(8) . . . . ? N4 C27 C28 C29 -177.2(4) . . . . ? C32 C27 C28 C36 177.3(5) . . . . ? N4 C27 C28 C36 -0.1(7) . . . . ? C27 C28 C29 C30 -1.1(8) . . . . ? C36 C28 C29 C30 -178.3(5) . . . . ? C28 C29 C30 C31 1.6(9) . . . . ? C29 C30 C31 C32 -1.3(9) . . . . ? C30 C31 C32 C27 0.5(8) . . . . ? C30 C31 C32 C33 -178.0(5) . . . . ? C28 C27 C32 C31 0.0(8) . . . . ? N4 C27 C32 C31 177.5(4) . . . . ? C28 C27 C32 C33 178.5(5) . . . . ? N4 C27 C32 C33 -4.0(7) . . . . ? C31 C32 C33 C34 90.3(6) . . . . ? C27 C32 C33 C34 -88.1(6) . . . . ? C31 C32 C33 C35 -33.4(8) . . . . ? C27 C32 C33 C35 148.2(5) . . . . ? C29 C28 C36 C38 -59.0(6) . . . . ? C27 C28 C36 C38 124.0(6) . . . . ? C29 C28 C36 C37 61.9(6) . . . . ? C27 C28 C36 C37 -115.1(6) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.681 _refine_diff_density_min -0.519 _refine_diff_density_rms 0.086