# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Mir Wais Hosseini' _publ_contact_author_email HOSSEINI@CHIMIE.U-STRASBG.FR _publ_section_title ; Molecular tectonics: formation and structural studies on a 2-D directional coordination network based on a non-centric metacyclophane based tecton and zinc cation ; loop_ _publ_author_name 'Mir Wais Hosseini' 'Jerome Ehrhart' 'Nathalie Kyritsakas-Gruber' 'Jean-Marc Planeix' # Attachment '_11-CoBr2_n.cif' data_e1460c _database_code_depnum_ccdc_archive 'CCDC 744810' #TrackingRef '_11-CoBr2_n.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H68 Br2 Co N4 S2' _chemical_formula_sum 'C62 H68 Br2 Co N4 S2' _chemical_formula_weight 1152.07 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' Br Br -0.2901 2.4595 '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' S S 0.1246 0.1234 '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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.0135(18) _cell_length_b 14.0197(13) _cell_length_c 32.858(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.339(3) _cell_angle_gamma 90.00 _cell_volume 7370.7(13) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2371 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 21.32 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.038 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2388 _exptl_absorpt_coefficient_mu 1.406 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9204 _exptl_absorpt_correction_T_max 0.9459 _exptl_absorpt_process_details sadabs _exptl_special_details ; Owing to large disorder of the solvent present in the cavities of this structure, the SQUEEZE command has been applied. Because of the floppiness of one ring the rigid group refinement was used and the thermal parameters of these atoms were constrainded ; _diffrn_ambient_temperature 173(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 58445 _diffrn_reflns_av_R_equivalents 0.0685 _diffrn_reflns_av_sigmaI/netI 0.1039 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 27.58 _reflns_number_total 17006 _reflns_number_gt 8815 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17006 _refine_ls_number_parameters 600 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1446 _refine_ls_R_factor_gt 0.0970 _refine_ls_wR_factor_ref 0.2766 _refine_ls_wR_factor_gt 0.2566 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0.020 _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 C39 C 0.7452(5) 0.3637(6) 0.48623(18) 0.1005(19) Uani 1 1 d G . . C40 C 0.6627(5) 0.3464(5) 0.4737(2) 0.1005(19) Uani 1 1 d G . . H40 H 0.6295 0.3038 0.4887 0.121 Uiso 1 1 calc R . . C41 C 0.6286(4) 0.3913(6) 0.4391(2) 0.1005(19) Uani 1 1 d GD . . H41 H 0.5721 0.3795 0.4306 0.121 Uiso 1 1 calc R . . C42 C 0.6770(4) 0.4536(5) 0.41716(18) 0.1005(19) Uani 1 1 d GD . . C43 C 0.7596(4) 0.4709(5) 0.4297(2) 0.1005(19) Uani 1 1 d GD . . H43 H 0.7927 0.5135 0.4147 0.121 Uiso 1 1 calc R . . C44 C 0.7937(4) 0.4260(6) 0.4642(2) 0.1005(19) Uani 1 1 d G . . H44 H 0.8501 0.4379 0.4728 0.121 Uiso 1 1 calc R . . Co1 Co 1.01565(6) -0.44047(7) 0.65311(2) 0.0300(2) Uani 1 1 d . . . Br1 Br 1.06957(7) -0.59567(7) 0.64837(3) 0.0640(3) Uani 1 1 d . . . Br2 Br 0.91244(5) -0.42443(7) 0.70188(2) 0.0503(3) Uani 1 1 d . . . C1 C 0.5472(4) 0.0698(5) 0.6566(2) 0.0334(15) Uani 1 1 d . . . C2 C 0.4695(4) 0.0962(5) 0.6374(2) 0.0349(16) Uani 1 1 d . . . C3 C 0.4402(4) 0.0422(5) 0.6037(2) 0.0332(15) Uani 1 1 d . . . C4 C 0.4862(4) -0.0311(5) 0.5878(2) 0.0318(15) Uani 1 1 d . . . C5 C 0.5645(4) -0.0534(5) 0.60640(19) 0.0275(13) Uani 1 1 d . . . C6 C 0.5926(4) -0.0054(5) 0.64239(18) 0.0294(14) Uani 1 1 d . . . C7 C 0.4174(4) 0.1782(6) 0.6530(2) 0.0457(19) Uani 1 1 d . . . H7A H 0.3848 0.2068 0.6302 0.069 Uiso 1 1 calc R . . H7B H 0.4545 0.2265 0.6656 0.069 Uiso 1 1 calc R . . H7C H 0.3794 0.1542 0.6733 0.069 Uiso 1 1 calc R . . C8 C 0.3537(4) 0.0635(6) 0.5852(2) 0.0386(17) Uani 1 1 d . . . C9 C 0.2847(4) 0.0346(6) 0.6046(2) 0.0461(19) Uani 1 1 d . . . H9 H 0.2911 -0.0014 0.6290 0.055 Uiso 1 1 calc R . . C10 C 0.2032(4) 0.0576(6) 0.5888(2) 0.0460(19) Uani 1 1 d . . . H10 H 0.1553 0.0372 0.6026 0.055 Uiso 1 1 calc R . . C11 C 0.1945(4) 0.1093(6) 0.5536(2) 0.0375(16) Uani 1 1 d . . . S1 S 0.09297(12) 0.14064(17) 0.53338(6) 0.0469(5) Uani 1 1 d . . . C12 C 0.2648(5) 0.1367(7) 0.5332(2) 0.048(2) Uani 1 1 d . . . H12 H 0.2593 0.1698 0.5080 0.058 Uiso 1 1 calc R . . C13 C 0.3423(5) 0.1152(7) 0.5501(2) 0.049(2) Uani 1 1 d . . . H13 H 0.3902 0.1371 0.5368 0.059 Uiso 1 1 calc R . . C14 C 0.0645(5) 0.2347(7) 0.5661(3) 0.059(2) Uani 1 1 d . . . H14A H 0.0631 0.2110 0.5941 0.088 Uiso 1 1 calc R . . H14B H 0.0092 0.2588 0.5574 0.088 Uiso 1 1 calc R . . H14C H 0.1056 0.2864 0.5647 0.088 Uiso 1 1 calc R . . C15 C 0.4505(4) -0.0900(6) 0.5520(2) 0.0417(18) Uani 1 1 d . . . H15A H 0.3907 -0.0766 0.5480 0.062 Uiso 1 1 calc R . . H15B H 0.4586 -0.1580 0.5577 0.062 Uiso 1 1 calc R . . H15C H 0.4794 -0.0730 0.5272 0.062 Uiso 1 1 calc R . . C16 C 0.6688(4) -0.0406(5) 0.66573(19) 0.0308(14) Uani 1 1 d . . . H16A H 0.7173 -0.0025 0.6585 0.046 Uiso 1 1 calc R . . H16B H 0.6785 -0.1077 0.6590 0.046 Uiso 1 1 calc R . . H16C H 0.6605 -0.0347 0.6950 0.046 Uiso 1 1 calc R . . C17 C 0.6154(4) -0.1358(5) 0.5890(2) 0.0336(15) Uani 1 1 d . . . H17A H 0.5913 -0.1505 0.5615 0.040 Uiso 1 1 calc R . . H17B H 0.6068 -0.1926 0.6062 0.040 Uiso 1 1 calc R . . C18 C 0.7103(4) -0.1220(5) 0.58539(18) 0.0284(14) Uani 1 1 d . . . C19 C 0.7644(4) -0.1932(5) 0.60080(19) 0.0305(14) Uani 1 1 d . . . C20 C 0.8524(4) -0.1790(5) 0.59706(19) 0.0311(14) Uani 1 1 d . . . C21 C 0.8832(4) -0.1001(5) 0.57720(19) 0.0305(14) Uani 1 1 d . . . C22 C 0.8280(4) -0.0301(5) 0.56083(17) 0.0278(14) Uani 1 1 d . . . C23 C 0.7410(4) -0.0439(5) 0.56434(17) 0.0253(13) Uani 1 1 d . . . C24 C 0.7337(5) -0.2826(6) 0.6210(2) 0.0469(19) Uani 1 1 d . . . H24A H 0.7293 -0.2712 0.6503 0.070 Uiso 1 1 calc R . . H24B H 0.7732 -0.3347 0.6168 0.070 Uiso 1 1 calc R . . H24C H 0.6787 -0.2999 0.6091 0.070 Uiso 1 1 calc R . . C25 C 0.9113(4) -0.2545(5) 0.61443(19) 0.0316(15) Uani 1 1 d . . . H25A H 0.9649 -0.2242 0.6232 0.038 Uiso 1 1 calc R . . H25B H 0.8868 -0.2834 0.6387 0.038 Uiso 1 1 calc R . . N1 N 0.9272(3) -0.3292(4) 0.58483(15) 0.0327(13) Uani 1 1 d . . . N2 N 0.9657(4) -0.4106(4) 0.59693(16) 0.0358(14) Uani 1 1 d . . . C26 C 0.9697(6) -0.4632(6) 0.5633(2) 0.055(2) Uani 1 1 d . . . H26 H 0.9924 -0.5257 0.5622 0.066 Uiso 1 1 calc R . . C27 C 0.9350(7) -0.4125(8) 0.5292(2) 0.073(3) Uani 1 1 d . . . H27 H 0.9317 -0.4326 0.5016 0.088 Uiso 1 1 calc R . . C28 C 0.9075(5) -0.3284(7) 0.5450(2) 0.053(2) Uani 1 1 d . . . H28 H 0.8795 -0.2787 0.5303 0.063 Uiso 1 1 calc R . . C29 C 0.9781(4) -0.0898(6) 0.5727(2) 0.0425(18) Uani 1 1 d . . . H29A H 1.0057 -0.0819 0.5996 0.064 Uiso 1 1 calc R . . H29B H 0.9893 -0.0338 0.5559 0.064 Uiso 1 1 calc R . . H29C H 0.9997 -0.1470 0.5596 0.064 Uiso 1 1 calc R . . C30 C 0.6802(4) 0.0271(6) 0.5436(2) 0.0380(16) Uani 1 1 d . . . H30A H 0.6249 -0.0023 0.5401 0.057 Uiso 1 1 calc R . . H30B H 0.7006 0.0448 0.5169 0.057 Uiso 1 1 calc R . . H30C H 0.6764 0.0844 0.5606 0.057 Uiso 1 1 calc R . . C31 C 0.8609(4) 0.0525(5) 0.53622(19) 0.0323(15) Uani 1 1 d . . . H31A H 0.9227 0.0514 0.5391 0.039 Uiso 1 1 calc R . . H31B H 0.8457 0.0403 0.5072 0.039 Uiso 1 1 calc R . . C32 C 0.8324(4) 0.1528(5) 0.54611(18) 0.0298(14) Uani 1 1 d . . . C33 C 0.8030(4) 0.2134(6) 0.51442(19) 0.0371(16) Uani 1 1 d . . . C34 C 0.7773(4) 0.3038(6) 0.5225(2) 0.0381(16) Uani 1 1 d . . . C35 C 0.7781(5) 0.3403(5) 0.5632(2) 0.0431(18) Uani 1 1 d . . . C36 C 0.8093(4) 0.2803(6) 0.5953(2) 0.0370(16) Uani 1 1 d . . . C37 C 0.8380(4) 0.1890(5) 0.58613(19) 0.0284(14) Uani 1 1 d . . . C38 C 0.7997(5) 0.1782(7) 0.4703(2) 0.050(2) Uani 1 1 d . . . H38A H 0.7818 0.2305 0.4522 0.074 Uiso 1 1 calc R . . H38B H 0.7598 0.1254 0.4674 0.074 Uiso 1 1 calc R . . H38C H 0.8552 0.1562 0.4631 0.074 Uiso 1 1 calc R . . S2 S 0.6292(2) 0.5135(2) 0.37239(8) 0.1005(19) Uani 1 1 d D . . C45 C 0.7142(7) 0.5875(7) 0.3659(3) 0.1005(19) Uani 1 1 d D . . H45A H 0.7218 0.6294 0.3896 0.121 Uiso 1 1 calc R . . H45B H 0.7044 0.6262 0.3413 0.121 Uiso 1 1 calc R . . H45C H 0.7645 0.5487 0.3630 0.121 Uiso 1 1 calc R . . C46 C 0.7503(7) 0.4417(6) 0.5708(3) 0.063(2) Uani 1 1 d . . . H46A H 0.7326 0.4716 0.5449 0.094 Uiso 1 1 calc R . . H46B H 0.7968 0.4779 0.5834 0.094 Uiso 1 1 calc R . . H46C H 0.7034 0.4412 0.5891 0.094 Uiso 1 1 calc R . . C47 C 0.8801(4) 0.1289(5) 0.6198(2) 0.0360(16) Uani 1 1 d . . . H47A H 0.9051 0.1710 0.6408 0.054 Uiso 1 1 calc R . . H47B H 0.9237 0.0894 0.6083 0.054 Uiso 1 1 calc R . . H47C H 0.8384 0.0878 0.6320 0.054 Uiso 1 1 calc R . . C48 C 0.8135(5) 0.3182(5) 0.6393(2) 0.0423(17) Uani 1 1 d . . . H48A H 0.7821 0.3790 0.6396 0.051 Uiso 1 1 calc R . . H48B H 0.8726 0.3332 0.6466 0.051 Uiso 1 1 calc R . . C49 C 0.7800(4) 0.2534(5) 0.67347(19) 0.0340(15) Uani 1 1 d . . . C50 C 0.8303(4) 0.2316(6) 0.7074(2) 0.0376(17) Uani 1 1 d . . . C51 C 0.7998(5) 0.1692(6) 0.73640(19) 0.0395(18) Uani 1 1 d . . . C52 C 0.7169(4) 0.1346(5) 0.73295(18) 0.0345(16) Uani 1 1 d . . . C53 C 0.6654(4) 0.1594(5) 0.69945(19) 0.0331(15) Uani 1 1 d . . . C54 C 0.6972(4) 0.2195(5) 0.66969(19) 0.0331(15) Uani 1 1 d . . . C55 C 0.9151(5) 0.2763(7) 0.7150(2) 0.053(2) Uani 1 1 d . . . H55A H 0.9324 0.2688 0.7438 0.079 Uiso 1 1 calc R . . H55B H 0.9123 0.3443 0.7082 0.079 Uiso 1 1 calc R . . H55C H 0.9558 0.2449 0.6980 0.079 Uiso 1 1 calc R . . C56 C 0.8576(5) 0.1323(6) 0.7704(2) 0.0441(19) Uani 1 1 d . . . H56A H 0.8439 0.0648 0.7760 0.053 Uiso 1 1 calc R . . H56B H 0.9160 0.1349 0.7617 0.053 Uiso 1 1 calc R . . N3 N 0.8503(4) 0.1886(5) 0.80795(16) 0.0362(14) Uani 1 1 d . . . N4 N 0.8948(3) 0.1598(4) 0.84238(15) 0.0310(12) Uani 1 1 d . . . C57 C 0.8696(5) 0.2180(6) 0.8725(2) 0.0428(18) Uani 1 1 d . . . H57 H 0.8893 0.2148 0.9001 0.051 Uiso 1 1 calc R . . C58 C 0.8110(5) 0.2826(7) 0.8572(2) 0.056(2) Uani 1 1 d . . . H58 H 0.7838 0.3315 0.8716 0.068 Uiso 1 1 calc R . . C59 C 0.8008(6) 0.2604(7) 0.8168(3) 0.058(2) Uani 1 1 d . . . H59 H 0.7637 0.2918 0.7979 0.070 Uiso 1 1 calc R . . C60 C 0.6856(6) 0.0729(7) 0.7672(2) 0.050(2) Uani 1 1 d . . . H60A H 0.6244 0.0694 0.7651 0.075 Uiso 1 1 calc R . . H60B H 0.7031 0.1010 0.7935 0.075 Uiso 1 1 calc R . . H60C H 0.7091 0.0086 0.7652 0.075 Uiso 1 1 calc R . . C61 C 0.6395(5) 0.2529(6) 0.6342(2) 0.0415(17) Uani 1 1 d . . . H61A H 0.6405 0.2061 0.6121 0.062 Uiso 1 1 calc R . . H61B H 0.6588 0.3148 0.6244 0.062 Uiso 1 1 calc R . . H61C H 0.5824 0.2592 0.6435 0.062 Uiso 1 1 calc R . . C62 C 0.5760(4) 0.1233(6) 0.69583(19) 0.0377(17) Uani 1 1 d . . . H62A H 0.5385 0.1787 0.6989 0.045 Uiso 1 1 calc R . . H62B H 0.5674 0.0803 0.7192 0.045 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 C39 0.133(5) 0.096(4) 0.073(3) 0.010(3) 0.005(3) 0.044(4) C40 0.133(5) 0.096(4) 0.073(3) 0.010(3) 0.005(3) 0.044(4) C41 0.133(5) 0.096(4) 0.073(3) 0.010(3) 0.005(3) 0.044(4) C42 0.133(5) 0.096(4) 0.073(3) 0.010(3) 0.005(3) 0.044(4) C43 0.133(5) 0.096(4) 0.073(3) 0.010(3) 0.005(3) 0.044(4) C44 0.133(5) 0.096(4) 0.073(3) 0.010(3) 0.005(3) 0.044(4) Co1 0.0334(5) 0.0320(5) 0.0241(4) 0.0015(4) -0.0029(3) 0.0051(4) Br1 0.0870(7) 0.0421(5) 0.0636(6) 0.0088(4) 0.0108(5) 0.0255(5) Br2 0.0462(5) 0.0618(6) 0.0438(4) 0.0098(4) 0.0134(3) 0.0048(4) C1 0.030(3) 0.040(4) 0.031(3) 0.001(3) -0.001(3) -0.003(3) C2 0.025(3) 0.043(4) 0.037(4) -0.002(3) -0.002(3) 0.002(3) C3 0.020(3) 0.042(4) 0.037(3) 0.001(3) -0.002(3) 0.005(3) C4 0.023(3) 0.037(4) 0.034(3) -0.004(3) -0.005(3) -0.001(3) C5 0.021(3) 0.027(3) 0.034(3) 0.003(3) 0.004(2) 0.003(3) C6 0.022(3) 0.043(4) 0.024(3) 0.007(3) 0.001(2) -0.004(3) C7 0.027(4) 0.055(5) 0.054(4) -0.015(4) -0.002(3) 0.008(3) C8 0.029(4) 0.048(5) 0.039(4) -0.003(3) -0.005(3) 0.012(3) C9 0.032(4) 0.058(5) 0.048(4) 0.019(4) -0.008(3) 0.000(3) C10 0.026(4) 0.057(5) 0.055(5) 0.013(4) -0.006(3) -0.003(3) C11 0.034(4) 0.045(5) 0.033(3) 0.004(3) 0.000(3) 0.011(3) S1 0.0327(10) 0.0628(14) 0.0446(10) -0.0047(9) -0.0075(8) 0.0145(9) C12 0.041(4) 0.068(6) 0.036(4) 0.015(4) 0.007(3) 0.014(4) C13 0.031(4) 0.073(6) 0.043(4) 0.020(4) 0.011(3) 0.009(4) C14 0.042(5) 0.070(6) 0.065(5) -0.010(5) 0.000(4) 0.013(4) C15 0.025(3) 0.053(5) 0.046(4) -0.003(4) -0.010(3) 0.007(3) C16 0.025(3) 0.037(4) 0.031(3) 0.000(3) -0.003(3) 0.002(3) C17 0.025(3) 0.033(4) 0.042(4) -0.001(3) -0.006(3) 0.000(3) C18 0.024(3) 0.036(4) 0.025(3) -0.002(3) -0.002(2) 0.006(3) C19 0.029(3) 0.031(4) 0.031(3) -0.001(3) 0.000(3) 0.004(3) C20 0.026(3) 0.034(4) 0.033(3) 0.000(3) -0.007(3) 0.009(3) C21 0.020(3) 0.042(4) 0.030(3) -0.002(3) -0.003(3) 0.011(3) C22 0.031(3) 0.038(4) 0.015(3) -0.001(2) -0.001(2) 0.009(3) C23 0.024(3) 0.033(4) 0.018(3) 0.002(2) -0.002(2) 0.011(3) C24 0.047(4) 0.039(5) 0.055(5) 0.013(4) 0.009(4) 0.005(4) C25 0.036(4) 0.031(4) 0.027(3) -0.004(3) -0.003(3) 0.015(3) N1 0.038(3) 0.037(3) 0.022(2) -0.003(2) -0.008(2) 0.014(3) N2 0.044(3) 0.037(3) 0.027(3) -0.008(2) -0.002(2) 0.016(3) C26 0.086(6) 0.050(5) 0.028(4) -0.010(3) -0.005(4) 0.029(5) C27 0.113(9) 0.073(7) 0.032(4) -0.014(4) -0.019(5) 0.033(6) C28 0.068(6) 0.067(6) 0.022(3) -0.003(3) -0.010(3) 0.031(5) C29 0.025(4) 0.057(5) 0.045(4) 0.007(4) 0.001(3) 0.012(3) C30 0.035(4) 0.043(4) 0.036(4) 0.005(3) -0.005(3) 0.013(3) C31 0.029(3) 0.043(4) 0.025(3) 0.009(3) 0.003(3) 0.011(3) C32 0.024(3) 0.040(4) 0.026(3) 0.011(3) -0.003(2) 0.002(3) C33 0.039(4) 0.045(5) 0.027(3) 0.016(3) 0.002(3) -0.002(3) C34 0.037(4) 0.040(4) 0.037(4) 0.009(3) 0.000(3) 0.006(3) C35 0.041(4) 0.033(4) 0.056(4) 0.017(3) 0.003(3) 0.005(3) C36 0.036(4) 0.045(5) 0.030(3) 0.007(3) -0.003(3) -0.010(3) C37 0.023(3) 0.032(4) 0.030(3) 0.006(3) 0.002(2) 0.000(3) C38 0.045(4) 0.068(6) 0.036(4) 0.015(4) 0.002(3) 0.009(4) S2 0.133(5) 0.096(4) 0.073(3) 0.010(3) 0.005(3) 0.044(4) C45 0.133(5) 0.096(4) 0.073(3) 0.010(3) 0.005(3) 0.044(4) C46 0.082(7) 0.039(5) 0.068(6) 0.019(4) 0.007(5) 0.008(5) C47 0.038(4) 0.038(4) 0.032(3) 0.006(3) -0.005(3) 0.002(3) C48 0.052(5) 0.029(4) 0.045(4) -0.002(3) -0.009(3) -0.011(3) C49 0.039(4) 0.037(4) 0.025(3) -0.007(3) -0.007(3) -0.006(3) C50 0.030(4) 0.047(5) 0.036(4) -0.012(3) -0.002(3) -0.006(3) C51 0.050(4) 0.047(5) 0.020(3) -0.017(3) -0.013(3) 0.009(4) C52 0.039(4) 0.041(4) 0.023(3) -0.006(3) -0.003(3) 0.013(3) C53 0.036(4) 0.035(4) 0.028(3) -0.005(3) -0.001(3) 0.006(3) C54 0.036(4) 0.036(4) 0.027(3) 0.001(3) -0.009(3) 0.004(3) C55 0.051(5) 0.064(6) 0.041(4) -0.013(4) -0.016(4) -0.001(4) C56 0.046(4) 0.052(5) 0.033(4) -0.021(3) -0.016(3) 0.018(4) N3 0.037(3) 0.043(4) 0.028(3) -0.018(3) -0.009(2) 0.012(3) N4 0.025(3) 0.040(3) 0.028(3) -0.016(2) -0.004(2) -0.004(2) C57 0.042(4) 0.061(5) 0.026(3) -0.013(3) 0.004(3) -0.004(4) C58 0.056(5) 0.066(6) 0.046(4) -0.025(4) -0.004(4) 0.019(4) C59 0.067(6) 0.060(6) 0.047(4) -0.013(4) -0.015(4) 0.025(5) C60 0.062(5) 0.066(6) 0.020(3) -0.002(3) -0.002(3) 0.007(4) C61 0.036(4) 0.042(5) 0.046(4) 0.010(3) -0.014(3) 0.004(3) C62 0.033(4) 0.055(5) 0.025(3) -0.003(3) 0.000(3) 0.009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C39 C40 1.3900 . ? C39 C44 1.3900 . ? C39 C34 1.530(8) . ? C40 C41 1.3900 . ? C40 H40 0.9500 . ? C41 C42 1.3900 . ? C41 H41 0.9500 . ? C42 C43 1.3900 . ? C42 S2 1.834(4) . ? C43 C44 1.3900 . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? Co1 N4 2.008(6) 2_746 ? Co1 N2 2.026(5) . ? Co1 Br1 2.3485(13) . ? Co1 Br2 2.3591(12) . ? C1 C6 1.374(10) . ? C1 C2 1.421(10) . ? C1 C62 1.545(9) . ? C2 C3 1.405(10) . ? C2 C7 1.522(10) . ? C3 C4 1.380(10) . ? C3 C8 1.520(9) . ? C4 C5 1.407(9) . ? C4 C15 1.530(10) . ? C5 C6 1.418(9) . ? C5 C17 1.536(9) . ? C6 C16 1.499(9) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.359(11) . ? C8 C13 1.368(10) . ? C9 C10 1.422(10) . ? C9 H9 0.9500 . ? C10 C11 1.368(10) . ? C10 H10 0.9500 . ? C11 C12 1.387(11) . ? C11 S1 1.786(7) . ? S1 C14 1.772(9) . ? C12 C13 1.373(10) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.542(9) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C23 1.394(9) . ? C18 C19 1.402(9) . ? C19 C20 1.432(9) . ? C19 C24 1.511(10) . ? C20 C21 1.386(10) . ? C20 C25 1.514(9) . ? C21 C22 1.412(9) . ? C21 C29 1.539(9) . ? C22 C23 1.416(9) . ? C22 C31 1.520(9) . ? C23 C30 1.533(9) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 N1 1.459(8) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? N1 C28 1.335(8) . ? N1 N2 1.349(8) . ? N2 C26 1.333(9) . ? C26 C27 1.420(12) . ? C26 H26 0.9500 . ? C27 C28 1.368(12) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.517(10) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.409(9) . ? C32 C37 1.409(9) . ? C33 C34 1.362(11) . ? C33 C38 1.529(10) . ? C34 C35 1.431(11) . ? C35 C36 1.426(10) . ? C35 C46 1.513(12) . ? C36 C37 1.397(10) . ? C36 C48 1.538(10) . ? C37 C47 1.526(9) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? S2 C45 1.732(8) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 C49 1.555(10) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.382(9) . ? C49 C54 1.410(10) . ? C50 C51 1.397(11) . ? C50 C55 1.507(11) . ? C51 C52 1.414(11) . ? C51 C56 1.512(9) . ? C52 C53 1.392(9) . ? C52 C60 1.522(11) . ? C53 C54 1.403(10) . ? C53 C62 1.517(10) . ? C54 C61 1.530(9) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 N3 1.474(8) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? N3 C59 1.320(10) . ? N3 N4 1.373(7) . ? N4 C57 1.356(9) . ? N4 Co1 2.008(6) 2_756 ? C57 C58 1.384(11) . ? C57 H57 0.9500 . ? C58 C59 1.367(11) . ? C58 H58 0.9500 . ? C59 H59 0.9500 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? 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 C40 C39 C44 120.0 . . ? C40 C39 C34 114.9(6) . . ? C44 C39 C34 124.9(6) . . ? C39 C40 C41 120.0 . . ? C39 C40 H40 120.0 . . ? C41 C40 H40 120.0 . . ? C42 C41 C40 120.0 . . ? C42 C41 H41 120.0 . . ? C40 C41 H41 120.0 . . ? C43 C42 C41 120.0 . . ? C43 C42 S2 121.3(4) . . ? C41 C42 S2 118.7(4) . . ? C42 C43 C44 120.0 . . ? C42 C43 H43 120.0 . . ? C44 C43 H43 120.0 . . ? C43 C44 C39 120.0 . . ? C43 C44 H44 120.0 . . ? C39 C44 H44 120.0 . . ? N4 Co1 N2 100.2(2) 2_746 . ? N4 Co1 Br1 112.95(16) 2_746 . ? N2 Co1 Br1 105.29(16) . . ? N4 Co1 Br2 113.63(17) 2_746 . ? N2 Co1 Br2 109.73(17) . . ? Br1 Co1 Br2 113.77(5) . . ? C6 C1 C2 121.0(6) . . ? C6 C1 C62 120.7(6) . . ? C2 C1 C62 118.1(6) . . ? C3 C2 C1 117.9(6) . . ? C3 C2 C7 120.2(6) . . ? C1 C2 C7 121.9(6) . . ? C4 C3 C2 122.2(6) . . ? C4 C3 C8 119.1(6) . . ? C2 C3 C8 118.6(6) . . ? C3 C4 C5 118.8(6) . . ? C3 C4 C15 120.3(6) . . ? C5 C4 C15 120.8(6) . . ? C4 C5 C6 120.2(6) . . ? C4 C5 C17 118.8(6) . . ? C6 C5 C17 120.9(5) . . ? C1 C6 C5 119.6(6) . . ? C1 C6 C16 120.7(6) . . ? C5 C6 C16 119.6(6) . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C13 118.0(6) . . ? C9 C8 C3 119.9(7) . . ? C13 C8 C3 122.0(7) . . ? C8 C9 C10 121.0(7) . . ? C8 C9 H9 119.5 . . ? C10 C9 H9 119.5 . . ? C11 C10 C9 119.2(7) . . ? C11 C10 H10 120.4 . . ? C9 C10 H10 120.4 . . ? C10 C11 C12 120.0(7) . . ? C10 C11 S1 120.3(6) . . ? C12 C11 S1 119.7(5) . . ? C14 S1 C11 102.1(4) . . ? C13 C12 C11 118.8(7) . . ? C13 C12 H12 120.6 . . ? C11 C12 H12 120.6 . . ? C8 C13 C12 123.0(7) . . ? C8 C13 H13 118.5 . . ? C12 C13 H13 118.5 . . ? S1 C14 H14A 109.5 . . ? S1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? S1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C4 C15 H15A 109.5 . . ? C4 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C4 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C6 C16 H16A 109.5 . . ? C6 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C6 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C5 C17 C18 118.3(6) . . ? C5 C17 H17A 107.8 . . ? C18 C17 H17A 107.7 . . ? C5 C17 H17B 107.7 . . ? C18 C17 H17B 107.7 . . ? H17A C17 H17B 107.1 . . ? C23 C18 C19 120.8(6) . . ? C23 C18 C17 120.3(6) . . ? C19 C18 C17 118.7(6) . . ? C18 C19 C20 117.7(6) . . ? C18 C19 C24 122.8(6) . . ? C20 C19 C24 119.5(6) . . ? C21 C20 C19 121.5(6) . . ? C21 C20 C25 120.5(6) . . ? C19 C20 C25 118.1(6) . . ? C20 C21 C22 120.3(6) . . ? C20 C21 C29 119.5(6) . . ? C22 C21 C29 120.2(6) . . ? C21 C22 C23 118.5(6) . . ? C21 C22 C31 120.5(6) . . ? C23 C22 C31 120.7(5) . . ? C18 C23 C22 121.0(5) . . ? C18 C23 C30 120.0(6) . . ? C22 C23 C30 119.0(6) . . ? C19 C24 H24A 109.5 . . ? C19 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C19 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N1 C25 C20 112.0(5) . . ? N1 C25 H25A 109.2 . . ? C20 C25 H25A 109.2 . . ? N1 C25 H25B 109.2 . . ? C20 C25 H25B 109.2 . . ? H25A C25 H25B 107.9 . . ? C28 N1 N2 112.5(6) . . ? C28 N1 C25 127.4(6) . . ? N2 N1 C25 120.1(5) . . ? C26 N2 N1 105.1(5) . . ? C26 N2 Co1 127.7(5) . . ? N1 N2 Co1 127.0(4) . . ? N2 C26 C27 110.3(7) . . ? N2 C26 H26 124.8 . . ? C27 C26 H26 124.9 . . ? C28 C27 C26 104.7(7) . . ? C28 C27 H27 127.6 . . ? C26 C27 H27 127.6 . . ? N1 C28 C27 107.3(7) . . ? N1 C28 H28 126.3 . . ? C27 C28 H28 126.4 . . ? C21 C29 H29A 109.5 . . ? C21 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C21 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C23 C30 H30A 109.5 . . ? C23 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C23 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 C22 118.6(5) . . ? C32 C31 H31A 107.7 . . ? C22 C31 H31A 107.7 . . ? C32 C31 H31B 107.7 . . ? C22 C31 H31B 107.7 . . ? H31A C31 H31B 107.1 . . ? C33 C32 C37 118.6(6) . . ? C33 C32 C31 119.6(6) . . ? C37 C32 C31 121.7(5) . . ? C34 C33 C32 120.7(6) . . ? C34 C33 C38 119.0(6) . . ? C32 C33 C38 120.2(7) . . ? C33 C34 C35 121.6(6) . . ? C33 C34 C39 117.0(7) . . ? C35 C34 C39 121.4(7) . . ? C36 C35 C34 118.1(7) . . ? C36 C35 C46 121.8(7) . . ? C34 C35 C46 120.0(7) . . ? C37 C36 C35 119.2(6) . . ? C37 C36 C48 121.2(6) . . ? C35 C36 C48 119.6(7) . . ? C36 C37 C32 121.5(6) . . ? C36 C37 C47 119.2(6) . . ? C32 C37 C47 119.2(6) . . ? C33 C38 H38A 109.5 . . ? C33 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C33 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C45 S2 C42 93.9(4) . . ? S2 C45 H45A 109.4 . . ? S2 C45 H45B 109.9 . . ? H45A C45 H45B 109.5 . . ? S2 C45 H45C 109.2 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C35 C46 H46A 109.5 . . ? C35 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C35 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C37 C47 H47A 109.5 . . ? C37 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C37 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C36 C48 C49 118.3(6) . . ? C36 C48 H48A 107.7 . . ? C49 C48 H48A 107.7 . . ? C36 C48 H48B 107.8 . . ? C49 C48 H48B 107.7 . . ? H48A C48 H48B 107.1 . . ? C50 C49 C54 120.8(6) . . ? C50 C49 C48 120.3(6) . . ? C54 C49 C48 118.9(6) . . ? C49 C50 C51 118.7(6) . . ? C49 C50 C55 122.3(7) . . ? C51 C50 C55 118.9(6) . . ? C50 C51 C52 120.9(6) . . ? C50 C51 C56 119.9(7) . . ? C52 C51 C56 119.1(7) . . ? C53 C52 C51 120.2(7) . . ? C53 C52 C60 121.6(7) . . ? C51 C52 C60 118.2(6) . . ? C52 C53 C54 118.7(6) . . ? C52 C53 C62 120.4(6) . . ? C54 C53 C62 120.9(6) . . ? C53 C54 C49 120.6(6) . . ? C53 C54 C61 119.3(6) . . ? C49 C54 C61 120.0(6) . . ? C50 C55 H55A 109.5 . . ? C50 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C50 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? N3 C56 C51 111.6(6) . . ? N3 C56 H56A 109.3 . . ? C51 C56 H56A 109.3 . . ? N3 C56 H56B 109.3 . . ? C51 C56 H56B 109.3 . . ? H56A C56 H56B 108.0 . . ? C59 N3 N4 109.8(5) . . ? C59 N3 C56 131.4(6) . . ? N4 N3 C56 118.4(5) . . ? C57 N4 N3 105.3(6) . . ? C57 N4 Co1 126.9(5) . 2_756 ? N3 N4 Co1 127.7(4) . 2_756 ? N4 C57 C58 110.4(6) . . ? N4 C57 H57 124.8 . . ? C58 C57 H57 124.8 . . ? C59 C58 C57 104.8(7) . . ? C59 C58 H58 127.6 . . ? C57 C58 H58 127.6 . . ? N3 C59 C58 109.8(7) . . ? N3 C59 H59 125.1 . . ? C58 C59 H59 125.1 . . ? C52 C60 H60A 109.5 . . ? C52 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C52 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C54 C61 H61A 109.5 . . ? C54 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C54 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C53 C62 C1 118.4(5) . . ? C53 C62 H62A 107.7 . . ? C1 C62 H62A 107.7 . . ? C53 C62 H62B 107.7 . . ? C1 C62 H62B 107.7 . . ? H62A C62 H62B 107.1 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.305 _refine_diff_density_min -1.295 _refine_diff_density_rms 0.170 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.498 -0.014 -0.007 2796.6 201.7 _platon_squeeze_details ; ; # Attachment '_11-CoCl2_n.cif' data_e1579a _database_code_depnum_ccdc_archive 'CCDC 744811' #TrackingRef '_11-CoCl2_n.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H68 Cl2 Co N4 S2' _chemical_formula_sum 'C62 H68 Cl2 Co N4 S2' _chemical_formula_weight 1063.15 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' Co Co 0.3494 0.9721 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.8582(6) _cell_length_b 13.8304(6) _cell_length_c 32.7069(12) _cell_angle_alpha 90.00 _cell_angle_beta 91.618(2) _cell_angle_gamma 90.00 _cell_volume 7170.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8261 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 27.25 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 0.985 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2244 _exptl_absorpt_coefficient_mu 0.405 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9761 _exptl_absorpt_correction_T_max 0.9840 _exptl_absorpt_process_details sadabs _exptl_special_details ; Owing to large disorder of the solvent present in the cavities of this structure, the SQUEEZE command has been applied Because of the flopiness of one ring we used the same thermal parameters for these atoms ; _diffrn_ambient_temperature 173(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45269 _diffrn_reflns_av_R_equivalents 0.0439 _diffrn_reflns_av_sigmaI/netI 0.0656 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 27.57 _reflns_number_total 16440 _reflns_number_gt 9347 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16440 _refine_ls_number_parameters 630 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1480 _refine_ls_R_factor_gt 0.1026 _refine_ls_wR_factor_ref 0.340 _refine_ls_wR_factor_gt 0.3039 _refine_ls_goodness_of_fit_ref 1.263 _refine_ls_restrained_S_all 1.267 _refine_ls_shift/su_max 0.021 _refine_ls_shift/su_mean 0.005 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C53 C 0.7421(4) 0.3687(4) 0.48447(15) 0.065(2) Uani 1 1 d G . . C54 C 0.6598(4) 0.3574(5) 0.4696(2) 0.109(4) Uani 1 1 d G . . H54 H 0.6220 0.3160 0.4833 0.130 Uiso 1 1 calc R . . C55 C 0.6326(4) 0.4065(7) 0.4345(2) 0.109(4) Uani 1 1 d G . . H55 H 0.5764 0.3988 0.4243 0.130 Uiso 1 1 calc R . . C56 C 0.6879(6) 0.4670(6) 0.41442(17) 0.109(4) Uani 1 1 d GD . . C57 C 0.7702(5) 0.4783(4) 0.42932(18) 0.109(4) Uani 1 1 d G . . H57 H 0.8080 0.5196 0.4156 0.130 Uiso 1 1 calc R . . C58 C 0.7974(4) 0.4291(4) 0.46435(17) 0.075(3) Uani 1 1 d G . . H58 H 0.8537 0.4369 0.4745 0.090 Uiso 1 1 calc R . . Co1 Co 1.01677(5) -0.44249(5) 0.65472(2) 0.0292(2) Uani 1 1 d . . . Cl1 Cl 0.91765(11) -0.42169(13) 0.70052(5) 0.0497(4) Uani 1 1 d . . . Cl2 Cl 1.06939(15) -0.59061(13) 0.65056(6) 0.0656(6) Uani 1 1 d . . . C1 C 0.8266(3) -0.0325(4) 0.55981(16) 0.0268(11) Uani 1 1 d . . . C2 C 0.8833(3) -0.1018(4) 0.57626(16) 0.0298(11) Uani 1 1 d . . . C3 C 0.8507(3) -0.1816(4) 0.59647(16) 0.0283(11) Uani 1 1 d . . . C4 C 0.7644(3) -0.1954(4) 0.60079(16) 0.0288(11) Uani 1 1 d . . . C5 C 0.7086(3) -0.1245(4) 0.58539(16) 0.0255(10) Uani 1 1 d . . . C6 C 0.7402(3) -0.0451(4) 0.56356(15) 0.0260(11) Uani 1 1 d . . . C7 C 0.9776(3) -0.0935(4) 0.5706(2) 0.0368(13) Uani 1 1 d . . . H7A H 1.0025 -0.0537 0.5926 0.055 Uiso 1 1 calc R . . H7B H 0.9881 -0.0635 0.5441 0.055 Uiso 1 1 calc R . . H7C H 1.0030 -0.1581 0.5715 0.055 Uiso 1 1 calc R . . C8 C 0.9110(3) -0.2551(4) 0.61476(15) 0.0282(11) Uani 1 1 d . . . H8A H 0.9649 -0.2230 0.6225 0.034 Uiso 1 1 calc R . . H8B H 0.8869 -0.2825 0.6398 0.034 Uiso 1 1 calc R . . N1 N 0.9271(3) -0.3329(3) 0.58593(13) 0.0285(10) Uani 1 1 d . . . N2 N 0.9677(3) -0.4152(3) 0.59809(15) 0.0345(11) Uani 1 1 d . . . C9 C 0.9727(4) -0.4691(5) 0.56523(19) 0.0493(17) Uani 1 1 d . . . H9 H 0.9979 -0.5314 0.5647 0.059 Uiso 1 1 calc R . . C10 C 0.9362(5) -0.4232(5) 0.5311(2) 0.058(2) Uani 1 1 d . . . H10 H 0.9316 -0.4470 0.5039 0.069 Uiso 1 1 calc R . . C11 C 0.9087(5) -0.3365(5) 0.54546(17) 0.0496(18) Uani 1 1 d . . . H11 H 0.8813 -0.2873 0.5297 0.060 Uiso 1 1 calc R . . C12 C 0.7331(4) -0.2842(4) 0.6215(2) 0.0389(14) Uani 1 1 d . . . H12A H 0.7761 -0.3351 0.6204 0.058 Uiso 1 1 calc R . . H12B H 0.6811 -0.3065 0.6076 0.058 Uiso 1 1 calc R . . H12C H 0.7217 -0.2694 0.6501 0.058 Uiso 1 1 calc R . . C13 C 0.6792(3) 0.0241(4) 0.54312(17) 0.0322(12) Uani 1 1 d . . . H13A H 0.6679 0.0778 0.5617 0.048 Uiso 1 1 calc R . . H13B H 0.6263 -0.0097 0.5363 0.048 Uiso 1 1 calc R . . H13C H 0.7036 0.0492 0.5181 0.048 Uiso 1 1 calc R . . C14 C 0.6137(3) -0.1370(4) 0.58966(18) 0.0292(11) Uani 1 1 d . . . H14A H 0.5892 -0.1518 0.5622 0.035 Uiso 1 1 calc R . . H14B H 0.6046 -0.1945 0.6070 0.035 Uiso 1 1 calc R . . C15 C 0.5636(3) -0.0542(4) 0.60721(17) 0.0269(11) Uani 1 1 d . . . C16 C 0.4857(3) -0.0316(4) 0.58879(18) 0.0319(12) Uani 1 1 d . . . C17 C 0.4374(3) 0.0452(4) 0.60515(18) 0.0318(12) Uani 1 1 d . . . C18 C 0.4682(3) 0.0970(4) 0.63914(18) 0.0334(12) Uani 1 1 d . . . C19 C 0.5454(3) 0.0725(4) 0.65786(17) 0.0297(11) Uani 1 1 d . . . C20 C 0.5920(3) -0.0062(4) 0.64269(16) 0.0269(11) Uani 1 1 d . . . C21 C 0.4510(4) -0.0897(5) 0.5532(2) 0.0445(15) Uani 1 1 d . . . H21A H 0.4879 -0.0825 0.5299 0.067 Uiso 1 1 calc R . . H21B H 0.3943 -0.0665 0.5456 0.067 Uiso 1 1 calc R . . H21C H 0.4481 -0.1581 0.5610 0.067 Uiso 1 1 calc R . . C22 C 0.3519(4) 0.0670(4) 0.58668(19) 0.0361(13) Uani 1 1 d . . . C23 C 0.2807(4) 0.0395(5) 0.6062(2) 0.0461(16) Uani 1 1 d . . . H23 H 0.2856 0.0025 0.6306 0.055 Uiso 1 1 calc R . . C24 C 0.2011(4) 0.0651(5) 0.5908(2) 0.0469(16) Uani 1 1 d . . . H24 H 0.1523 0.0462 0.6049 0.056 Uiso 1 1 calc R . . C25 C 0.1927(4) 0.1172(4) 0.55540(18) 0.0375(13) Uani 1 1 d . . . C26 C 0.2636(5) 0.1418(6) 0.5348(2) 0.059(2) Uani 1 1 d . . . H26 H 0.2589 0.1761 0.5097 0.070 Uiso 1 1 calc R . . C27 C 0.3413(4) 0.1166(6) 0.5507(3) 0.062(2) Uani 1 1 d . . . H27 H 0.3900 0.1343 0.5362 0.075 Uiso 1 1 calc R . . S1 S 0.09144(10) 0.14995(13) 0.53510(5) 0.0479(4) Uani 1 1 d . . . C28 C 0.0634(5) 0.2472(6) 0.5679(2) 0.0584(19) Uani 1 1 d . . . H28A H 0.0662 0.2252 0.5964 0.088 Uiso 1 1 calc R . . H28B H 0.0060 0.2687 0.5609 0.088 Uiso 1 1 calc R . . H28C H 0.1028 0.3010 0.5645 0.088 Uiso 1 1 calc R . . C29 C 0.4157(4) 0.1788(5) 0.6555(2) 0.0495(17) Uani 1 1 d . . . H29A H 0.3614 0.1812 0.6405 0.074 Uiso 1 1 calc R . . H29B H 0.4456 0.2401 0.6520 0.074 Uiso 1 1 calc R . . H29C H 0.4061 0.1681 0.6846 0.074 Uiso 1 1 calc R . . C30 C 0.6694(3) -0.0403(4) 0.66566(18) 0.0333(12) Uani 1 1 d . . . H30A H 0.6772 -0.1096 0.6609 0.050 Uiso 1 1 calc R . . H30B H 0.6631 -0.0285 0.6950 0.050 Uiso 1 1 calc R . . H30C H 0.7187 -0.0049 0.6561 0.050 Uiso 1 1 calc R . . C31 C 0.5754(4) 0.1268(4) 0.69667(18) 0.0360(13) Uani 1 1 d . . . H31A H 0.5387 0.1841 0.6997 0.043 Uiso 1 1 calc R . . H31B H 0.5658 0.0842 0.7204 0.043 Uiso 1 1 calc R . . C32 C 0.6657(4) 0.1609(4) 0.69955(18) 0.0348(12) Uani 1 1 d . . . C33 C 0.7194(4) 0.1371(4) 0.73311(16) 0.0348(13) Uani 1 1 d . . . C34 C 0.8019(4) 0.1722(4) 0.73520(17) 0.0369(13) Uani 1 1 d . . . C35 C 0.8323(4) 0.2353(5) 0.70578(18) 0.0384(14) Uani 1 1 d . . . C36 C 0.7811(4) 0.2579(4) 0.67112(18) 0.0337(12) Uani 1 1 d . . . C37 C 0.6981(3) 0.2231(4) 0.66871(18) 0.0319(12) Uani 1 1 d . . . C38 C 0.6877(5) 0.0750(5) 0.7672(2) 0.0518(17) Uani 1 1 d . . . H38A H 0.6890 0.0069 0.7589 0.078 Uiso 1 1 calc R . . H38B H 0.6296 0.0934 0.7731 0.078 Uiso 1 1 calc R . . H38C H 0.7237 0.0841 0.7917 0.078 Uiso 1 1 calc R . . C39 C 0.8610(4) 0.1380(5) 0.76874(17) 0.0408(15) Uani 1 1 d . . . H39A H 0.8505 0.0684 0.7737 0.049 Uiso 1 1 calc R . . H39B H 0.9197 0.1447 0.7596 0.049 Uiso 1 1 calc R . . N3 N 0.8526(3) 0.1906(4) 0.80714(14) 0.0353(11) Uani 1 1 d . . . N4 N 0.8940(3) 0.1596(3) 0.84172(13) 0.0301(10) Uani 1 1 d . . . C40 C 0.8678(4) 0.2177(5) 0.87108(18) 0.0387(14) Uani 1 1 d . . . H40 H 0.8856 0.2129 0.8990 0.046 Uiso 1 1 calc R . . C41 C 0.8119(5) 0.2856(6) 0.8561(2) 0.0546(19) Uani 1 1 d . . . H41 H 0.7850 0.3354 0.8709 0.065 Uiso 1 1 calc R . . C42 C 0.8032(5) 0.2660(6) 0.8151(2) 0.058(2) Uani 1 1 d . . . H42 H 0.7684 0.2999 0.7958 0.070 Uiso 1 1 calc R . . C43 C 0.9174(4) 0.2818(6) 0.7125(2) 0.059(2) Uani 1 1 d . . . H43A H 0.9360 0.2735 0.7411 0.088 Uiso 1 1 calc R . . H43B H 0.9134 0.3509 0.7061 0.088 Uiso 1 1 calc R . . H43C H 0.9582 0.2512 0.6946 0.088 Uiso 1 1 calc R . . C44 C 0.6393(4) 0.2557(5) 0.6343(2) 0.0425(15) Uani 1 1 d . . . H44A H 0.6582 0.3183 0.6240 0.064 Uiso 1 1 calc R . . H44B H 0.5820 0.2620 0.6445 0.064 Uiso 1 1 calc R . . H44C H 0.6396 0.2078 0.6122 0.064 Uiso 1 1 calc R . . C45 C 0.8142(4) 0.3204(4) 0.63749(18) 0.0382(13) Uani 1 1 d . . . H45A H 0.8743 0.3341 0.6441 0.046 Uiso 1 1 calc R . . H45B H 0.7839 0.3829 0.6383 0.046 Uiso 1 1 calc R . . C46 C 0.8084(4) 0.2835(4) 0.59383(19) 0.0360(13) Uani 1 1 d . . . C47 C 0.7769(4) 0.3425(4) 0.5620(2) 0.0437(15) Uani 1 1 d . . . C48 C 0.7752(4) 0.3074(4) 0.5212(2) 0.0409(14) Uani 1 1 d . . . C49 C 0.8004(3) 0.2132(4) 0.51241(17) 0.0316(12) Uani 1 1 d . . . C50 C 0.8311(3) 0.1545(4) 0.54436(17) 0.0307(12) Uani 1 1 d . . . C51 C 0.8378(3) 0.1905(4) 0.58449(17) 0.0300(11) Uani 1 1 d . . . C52 C 0.7489(6) 0.4461(5) 0.5706(3) 0.067(2) Uani 1 1 d . . . H52A H 0.6969 0.4449 0.5861 0.101 Uiso 1 1 calc R . . H52B H 0.7385 0.4802 0.5447 0.101 Uiso 1 1 calc R . . H52C H 0.7932 0.4796 0.5866 0.101 Uiso 1 1 calc R . . S2 S 0.6367(2) 0.5261(2) 0.37052(8) 0.109(4) Uani 1 1 d D . . C59 C 0.7135(6) 0.6071(6) 0.3612(3) 0.109(4) Uani 1 1 d D . . H59A H 0.7372 0.6315 0.3872 0.130 Uiso 1 1 calc R . . H59B H 0.6898 0.6611 0.3452 0.130 Uiso 1 1 calc R . . H59C H 0.7581 0.5758 0.3458 0.130 Uiso 1 1 calc R . . C60 C 0.7965(4) 0.1776(5) 0.46936(19) 0.0467(16) Uani 1 1 d . . . H60A H 0.7690 0.2263 0.4518 0.070 Uiso 1 1 calc R . . H60B H 0.7642 0.1173 0.4679 0.070 Uiso 1 1 calc R . . H60C H 0.8539 0.1659 0.4601 0.070 Uiso 1 1 calc R . . C61 C 0.8822(4) 0.1292(4) 0.61747(18) 0.0355(12) Uani 1 1 d . . . H61A H 0.8410 0.0866 0.6301 0.053 Uiso 1 1 calc R . . H61B H 0.9078 0.1716 0.6384 0.053 Uiso 1 1 calc R . . H61C H 0.9262 0.0900 0.6051 0.053 Uiso 1 1 calc R . . C62 C 0.8604(3) 0.0519(4) 0.53474(17) 0.0318(12) Uani 1 1 d . . . H62A H 0.8459 0.0389 0.5056 0.038 Uiso 1 1 calc R . . H62B H 0.9227 0.0509 0.5376 0.038 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 C53 0.087(6) 0.054(5) 0.055(5) 0.016(4) -0.018(4) 0.005(4) C54 0.107(9) 0.092(8) 0.124(10) 0.037(7) -0.047(7) 0.004(6) C55 0.107(9) 0.092(8) 0.124(10) 0.037(7) -0.047(7) 0.004(6) C56 0.107(9) 0.092(8) 0.124(10) 0.037(7) -0.047(7) 0.004(6) C57 0.107(9) 0.092(8) 0.124(10) 0.037(7) -0.047(7) 0.004(6) C58 0.141(9) 0.044(4) 0.039(4) 0.010(3) 0.001(5) 0.022(5) Co1 0.0343(4) 0.0280(4) 0.0251(4) 0.0021(3) -0.0044(3) 0.0058(3) Cl1 0.0479(9) 0.0598(10) 0.0421(9) 0.0113(8) 0.0123(7) 0.0057(7) Cl2 0.1004(16) 0.0411(9) 0.0553(11) 0.0079(8) 0.0042(10) 0.0321(9) C1 0.025(3) 0.031(3) 0.023(2) 0.002(2) -0.005(2) 0.009(2) C2 0.025(3) 0.038(3) 0.026(3) -0.004(2) -0.005(2) 0.010(2) C3 0.025(3) 0.035(3) 0.024(3) -0.002(2) -0.003(2) 0.011(2) C4 0.031(3) 0.031(3) 0.024(3) 0.001(2) -0.003(2) 0.010(2) C5 0.024(2) 0.024(2) 0.029(3) -0.001(2) -0.002(2) 0.0037(18) C6 0.024(2) 0.032(3) 0.021(2) 0.004(2) -0.0046(19) 0.0085(19) C7 0.026(3) 0.040(3) 0.044(3) 0.001(3) -0.001(2) 0.010(2) C8 0.033(3) 0.032(3) 0.020(2) -0.003(2) -0.005(2) 0.017(2) N1 0.036(2) 0.027(2) 0.021(2) -0.0030(17) -0.0084(18) 0.0112(18) N2 0.043(3) 0.029(2) 0.032(3) -0.0067(19) -0.006(2) 0.0144(19) C9 0.063(4) 0.054(4) 0.029(3) -0.018(3) -0.012(3) 0.030(3) C10 0.085(6) 0.057(4) 0.030(3) -0.017(3) -0.016(3) 0.033(4) C11 0.068(5) 0.061(4) 0.019(3) -0.002(3) -0.012(3) 0.031(3) C12 0.039(3) 0.033(3) 0.044(3) 0.008(3) 0.006(3) 0.008(2) C13 0.025(3) 0.038(3) 0.033(3) 0.011(2) -0.007(2) 0.008(2) C14 0.024(3) 0.026(3) 0.037(3) 0.002(2) 0.001(2) 0.0050(19) C15 0.021(2) 0.028(3) 0.032(3) 0.004(2) 0.001(2) 0.0029(19) C16 0.021(2) 0.036(3) 0.038(3) 0.007(2) -0.003(2) 0.001(2) C17 0.020(2) 0.037(3) 0.039(3) 0.006(2) -0.002(2) 0.002(2) C18 0.026(3) 0.035(3) 0.040(3) -0.001(2) -0.003(2) 0.007(2) C19 0.024(2) 0.033(3) 0.032(3) 0.002(2) -0.001(2) 0.003(2) C20 0.022(2) 0.027(3) 0.031(3) 0.007(2) -0.003(2) 0.0034(19) C21 0.033(3) 0.057(4) 0.044(4) -0.007(3) -0.009(3) 0.007(3) C22 0.032(3) 0.041(3) 0.035(3) 0.002(3) -0.004(2) 0.013(2) C23 0.032(3) 0.051(4) 0.055(4) 0.018(3) -0.005(3) -0.002(3) C24 0.027(3) 0.053(4) 0.060(4) 0.008(3) -0.008(3) -0.003(3) C25 0.033(3) 0.045(3) 0.035(3) 0.000(3) -0.004(2) 0.015(2) C26 0.050(4) 0.075(5) 0.051(4) 0.017(4) 0.004(3) 0.024(4) C27 0.034(4) 0.089(6) 0.065(5) 0.029(4) 0.011(3) 0.020(4) S1 0.0367(8) 0.0563(10) 0.0499(10) -0.0083(8) -0.0136(7) 0.0194(7) C28 0.051(4) 0.060(5) 0.064(5) -0.011(4) 0.003(4) 0.019(3) C29 0.028(3) 0.043(4) 0.076(5) -0.015(3) -0.009(3) 0.010(2) C30 0.028(3) 0.038(3) 0.034(3) 0.003(2) -0.003(2) 0.004(2) C31 0.035(3) 0.040(3) 0.033(3) -0.004(2) -0.003(2) 0.006(2) C32 0.039(3) 0.034(3) 0.031(3) 0.000(2) -0.004(2) 0.007(2) C33 0.045(3) 0.039(3) 0.020(3) -0.005(2) -0.007(2) 0.007(2) C34 0.044(3) 0.042(3) 0.025(3) -0.012(2) -0.014(2) 0.010(2) C35 0.033(3) 0.053(4) 0.029(3) -0.014(3) -0.007(2) -0.004(2) C36 0.037(3) 0.028(3) 0.035(3) -0.006(2) -0.008(2) 0.001(2) C37 0.035(3) 0.025(3) 0.036(3) -0.003(2) -0.006(2) 0.003(2) C38 0.071(5) 0.054(4) 0.029(3) 0.000(3) -0.009(3) -0.004(3) C39 0.047(4) 0.052(4) 0.023(3) -0.013(3) -0.010(2) 0.016(3) N3 0.035(3) 0.044(3) 0.026(2) -0.011(2) -0.007(2) 0.005(2) N4 0.026(2) 0.041(3) 0.022(2) -0.0039(19) -0.0005(18) -0.0053(18) C40 0.042(3) 0.048(3) 0.027(3) -0.014(3) 0.000(2) -0.005(3) C41 0.056(4) 0.064(5) 0.044(4) -0.026(3) -0.007(3) 0.021(3) C42 0.064(5) 0.061(5) 0.049(4) -0.015(4) -0.010(4) 0.031(4) C43 0.048(4) 0.085(6) 0.043(4) -0.013(4) -0.010(3) -0.014(4) C44 0.042(3) 0.036(3) 0.048(4) 0.010(3) -0.012(3) -0.002(2) C45 0.043(3) 0.033(3) 0.039(3) -0.004(2) -0.005(3) -0.008(2) C46 0.033(3) 0.030(3) 0.044(3) 0.007(2) -0.007(3) -0.005(2) C47 0.044(3) 0.029(3) 0.057(4) 0.017(3) -0.012(3) -0.004(2) C48 0.044(3) 0.034(3) 0.045(4) 0.008(3) -0.010(3) -0.005(2) C49 0.024(3) 0.037(3) 0.033(3) 0.012(2) -0.002(2) 0.000(2) C50 0.023(3) 0.038(3) 0.031(3) 0.012(2) -0.006(2) -0.003(2) C51 0.028(3) 0.031(3) 0.031(3) 0.009(2) -0.007(2) -0.004(2) C52 0.085(6) 0.033(4) 0.082(6) 0.016(4) -0.016(5) -0.007(3) S2 0.107(9) 0.092(8) 0.124(10) 0.037(7) -0.047(7) 0.004(6) C59 0.107(9) 0.092(8) 0.124(10) 0.037(7) -0.047(7) 0.004(6) C60 0.046(4) 0.056(4) 0.037(3) 0.021(3) -0.007(3) -0.009(3) C61 0.037(3) 0.037(3) 0.032(3) 0.005(2) -0.008(2) 0.005(2) C62 0.024(3) 0.042(3) 0.030(3) 0.010(2) -0.002(2) 0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C53 C54 1.3900 . ? C53 C58 1.3900 . ? C53 C48 1.549(7) . ? C54 C55 1.3900 . ? C54 H54 0.9500 . ? C55 C56 1.3900 . ? C55 H55 0.9500 . ? C56 C57 1.3900 . ? C56 S2 1.823(4) . ? C57 C58 1.3900 . ? C57 H57 0.9500 . ? C58 H58 0.9500 . ? Co1 N4 1.999(5) 2_746 ? Co1 N2 2.024(5) . ? Co1 Cl2 2.2176(18) . ? Co1 Cl1 2.2206(17) . ? C1 C6 1.391(7) . ? C1 C2 1.411(7) . ? C1 C62 1.531(7) . ? C2 C3 1.393(8) . ? C2 C7 1.515(8) . ? C3 C4 1.394(7) . ? C3 C8 1.507(7) . ? C4 C5 1.403(7) . ? C4 C12 1.495(8) . ? C5 C6 1.409(7) . ? C5 C14 1.526(7) . ? C6 C13 1.504(7) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 N1 1.457(6) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? N1 C11 1.348(7) . ? N1 N2 1.362(6) . ? N2 C9 1.312(7) . ? C9 C10 1.396(9) . ? C9 H9 0.9500 . ? C10 C11 1.365(9) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.516(7) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.395(7) . ? C15 C20 1.400(8) . ? C16 C17 1.423(8) . ? C16 C21 1.505(9) . ? C17 C18 1.398(8) . ? C17 C22 1.500(8) . ? C18 C19 1.395(8) . ? C18 C29 1.510(8) . ? C19 C20 1.414(7) . ? C19 C31 1.539(8) . ? C20 C30 1.497(7) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.367(9) . ? C22 C27 1.367(9) . ? C23 C24 1.391(9) . ? C23 H23 0.9500 . ? C24 C25 1.366(9) . ? C24 H24 0.9500 . ? C25 C26 1.369(10) . ? C25 S1 1.779(6) . ? C26 C27 1.370(10) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? S1 C28 1.785(7) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.507(8) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.409(8) . ? C32 C37 1.432(8) . ? C33 C34 1.396(9) . ? C33 C38 1.505(9) . ? C34 C35 1.395(9) . ? C34 C39 1.499(8) . ? C35 C36 1.411(8) . ? C35 C43 1.506(9) . ? C36 C37 1.401(8) . ? C36 C45 1.505(8) . ? C37 C44 1.509(8) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 N3 1.461(7) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? N3 C42 1.333(8) . ? N3 N4 1.361(6) . ? N4 C40 1.328(7) . ? N4 Co1 1.999(5) 2_756 ? C40 C41 1.373(9) . ? C40 H40 0.9500 . ? C41 C42 1.372(10) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C46 1.517(9) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C51 1.406(8) . ? C46 C47 1.404(8) . ? C47 C48 1.419(10) . ? C47 C52 1.529(10) . ? C48 C49 1.395(8) . ? C49 C50 1.400(7) . ? C49 C60 1.491(9) . ? C50 C51 1.405(8) . ? C50 C62 1.529(8) . ? C51 C61 1.528(7) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? S2 C59 1.689(8) . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? 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 C54 C53 C58 120.0 . . ? C54 C53 C48 120.3(4) . . ? C58 C53 C48 119.4(4) . . ? C55 C54 C53 120.0 . . ? C55 C54 H54 120.0 . . ? C53 C54 H54 120.0 . . ? C56 C55 C54 120.0 . . ? C56 C55 H55 120.0 . . ? C54 C55 H55 120.0 . . ? C55 C56 C57 120.0 . . ? C55 C56 S2 111.7(5) . . ? C57 C56 S2 128.2(5) . . ? C58 C57 C56 120.0 . . ? C58 C57 H57 120.0 . . ? C56 C57 H57 120.0 . . ? C57 C58 C53 120.0 . . ? C57 C58 H58 120.0 . . ? C53 C58 H58 120.0 . . ? N4 Co1 N2 100.08(19) 2_746 . ? N4 Co1 Cl2 112.90(14) 2_746 . ? N2 Co1 Cl2 104.58(14) . . ? N4 Co1 Cl1 112.47(14) 2_746 . ? N2 Co1 Cl1 109.38(15) . . ? Cl2 Co1 Cl1 115.83(8) . . ? C6 C1 C2 120.0(5) . . ? C6 C1 C62 120.3(4) . . ? C2 C1 C62 119.6(5) . . ? C3 C2 C1 118.6(5) . . ? C3 C2 C7 119.8(5) . . ? C1 C2 C7 121.5(5) . . ? C2 C3 C4 122.3(5) . . ? C2 C3 C8 118.9(5) . . ? C4 C3 C8 118.8(5) . . ? C3 C4 C5 118.6(5) . . ? C3 C4 C12 119.8(5) . . ? C5 C4 C12 121.6(5) . . ? C4 C5 C6 119.8(5) . . ? C4 C5 C14 120.1(5) . . ? C6 C5 C14 120.0(4) . . ? C1 C6 C5 120.5(4) . . ? C1 C6 C13 120.2(5) . . ? C5 C6 C13 119.2(5) . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 C3 111.2(4) . . ? N1 C8 H8A 109.4 . . ? C3 C8 H8A 109.4 . . ? N1 C8 H8B 109.4 . . ? C3 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? C11 N1 N2 110.1(5) . . ? C11 N1 C8 128.7(5) . . ? N2 N1 C8 121.2(4) . . ? C9 N2 N1 105.9(5) . . ? C9 N2 Co1 127.8(4) . . ? N1 N2 Co1 126.1(3) . . ? N2 C9 C10 111.3(6) . . ? N2 C9 H9 124.3 . . ? C10 C9 H9 124.3 . . ? C11 C10 C9 104.7(5) . . ? C11 C10 H10 127.6 . . ? C9 C10 H10 127.6 . . ? N1 C11 C10 107.9(5) . . ? N1 C11 H11 126.0 . . ? C10 C11 H11 126.0 . . ? C4 C12 H12A 109.5 . . ? C4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C6 C13 H13A 109.5 . . ? C6 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C6 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C5 118.6(4) . . ? C15 C14 H14A 107.7 . . ? C5 C14 H14A 107.7 . . ? C15 C14 H14B 107.7 . . ? C5 C14 H14B 107.7 . . ? H14A C14 H14B 107.1 . . ? C16 C15 C20 120.9(5) . . ? C16 C15 C14 118.2(5) . . ? C20 C15 C14 120.8(5) . . ? C15 C16 C17 118.9(5) . . ? C15 C16 C21 121.0(5) . . ? C17 C16 C21 120.1(5) . . ? C18 C17 C16 120.2(5) . . ? C18 C17 C22 120.6(5) . . ? C16 C17 C22 119.2(5) . . ? C19 C18 C17 120.4(5) . . ? C19 C18 C29 120.8(5) . . ? C17 C18 C29 118.8(5) . . ? C18 C19 C20 119.6(5) . . ? C18 C19 C31 119.4(5) . . ? C20 C19 C31 120.8(5) . . ? C15 C20 C19 119.7(5) . . ? C15 C20 C30 120.5(5) . . ? C19 C20 C30 119.7(5) . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C27 117.3(6) . . ? C23 C22 C17 120.4(5) . . ? C27 C22 C17 122.3(6) . . ? C22 C23 C24 120.9(6) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.6 . . ? C25 C24 C23 120.5(6) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C24 C25 C26 119.0(6) . . ? C24 C25 S1 121.1(5) . . ? C26 C25 S1 119.9(5) . . ? C25 C26 C27 119.6(7) . . ? C25 C26 H26 120.2 . . ? C27 C26 H26 120.2 . . ? C26 C27 C22 122.7(7) . . ? C26 C27 H27 118.6 . . ? C22 C27 H27 118.6 . . ? C25 S1 C28 101.8(3) . . ? S1 C28 H28A 109.5 . . ? S1 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? S1 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C18 C29 H29A 109.5 . . ? C18 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C18 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C20 C30 H30A 109.5 . . ? C20 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C20 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 C19 118.4(5) . . ? C32 C31 H31A 107.7 . . ? C19 C31 H31A 107.7 . . ? C32 C31 H31B 107.7 . . ? C19 C31 H31B 107.7 . . ? H31A C31 H31B 107.1 . . ? C33 C32 C37 117.9(5) . . ? C33 C32 C31 121.9(5) . . ? C37 C32 C31 120.2(5) . . ? C34 C33 C32 120.2(5) . . ? C34 C33 C38 119.7(5) . . ? C32 C33 C38 120.2(6) . . ? C33 C34 C35 121.7(5) . . ? C33 C34 C39 119.5(6) . . ? C35 C34 C39 118.8(6) . . ? C34 C35 C36 119.4(5) . . ? C34 C35 C43 119.5(6) . . ? C36 C35 C43 121.0(6) . . ? C37 C36 C35 119.2(5) . . ? C37 C36 C45 120.1(5) . . ? C35 C36 C45 120.7(5) . . ? C36 C37 C32 121.5(5) . . ? C36 C37 C44 120.0(5) . . ? C32 C37 C44 118.5(5) . . ? C33 C38 H38A 109.5 . . ? C33 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C33 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N3 C39 C34 113.7(5) . . ? N3 C39 H39A 108.8 . . ? C34 C39 H39A 108.8 . . ? N3 C39 H39B 108.8 . . ? C34 C39 H39B 108.8 . . ? H39A C39 H39B 107.7 . . ? C42 N3 N4 110.9(5) . . ? C42 N3 C39 128.7(5) . . ? N4 N3 C39 120.2(5) . . ? C40 N4 N3 104.8(5) . . ? C40 N4 Co1 128.4(4) . 2_756 ? N3 N4 Co1 126.5(3) . 2_756 ? N4 C40 C41 111.7(6) . . ? N4 C40 H40 124.2 . . ? C41 C40 H40 124.2 . . ? C42 C41 C40 105.0(6) . . ? C42 C41 H41 127.5 . . ? C40 C41 H41 127.5 . . ? N3 C42 C41 107.7(6) . . ? N3 C42 H42 126.2 . . ? C41 C42 H42 126.2 . . ? C35 C43 H43A 109.5 . . ? C35 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C35 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C37 C44 H44A 109.5 . . ? C37 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C37 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C36 C45 C46 118.8(5) . . ? C36 C45 H45A 107.6 . . ? C46 C45 H45A 107.6 . . ? C36 C45 H45B 107.6 . . ? C46 C45 H45B 107.6 . . ? H45A C45 H45B 107.0 . . ? C51 C46 C47 118.9(6) . . ? C51 C46 C45 120.1(5) . . ? C47 C46 C45 120.9(6) . . ? C46 C47 C48 119.8(6) . . ? C46 C47 C52 120.4(7) . . ? C48 C47 C52 119.7(6) . . ? C49 C48 C47 121.0(5) . . ? C49 C48 C53 116.4(6) . . ? C47 C48 C53 122.6(5) . . ? C48 C49 C50 118.9(6) . . ? C48 C49 C60 119.9(5) . . ? C50 C49 C60 121.2(5) . . ? C49 C50 C51 120.5(5) . . ? C49 C50 C62 119.1(5) . . ? C51 C50 C62 120.4(5) . . ? C46 C51 C50 120.7(5) . . ? C46 C51 C61 120.2(5) . . ? C50 C51 C61 119.0(5) . . ? C47 C52 H52A 109.5 . . ? C47 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C47 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C59 S2 C56 97.6(5) . . ? S2 C59 H59A 109.5 . . ? S2 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? S2 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C49 C60 H60A 109.5 . . ? C49 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C49 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C51 C61 H61A 109.5 . . ? C51 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C51 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C1 C62 C50 118.9(4) . . ? C1 C62 H62A 107.6 . . ? C50 C62 H62A 107.6 . . ? C1 C62 H62B 107.6 . . ? C50 C62 H62B 107.6 . . ? H62A C62 H62B 107.0 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.57 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.572 _refine_diff_density_min -1.987 _refine_diff_density_rms 0.168 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.499 -0.016 -0.005 2662.4 323.4 _platon_squeeze_details ; ; # Attachment '12_ZnCl2.cif' data_e1499d _database_code_depnum_ccdc_archive 'CCDC 744812' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '8(C29 H31 Cl2 N3 Zn), 2(C H4 O), 2(H2 O)' _chemical_formula_sum 'C234 H260 Cl16 N24 O4 Zn8' _chemical_formula_weight 4562.82 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' H H 0.0000 0.0000 '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 _symmetry_space_group_name_Hall '-C 2yc' 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 12.6081(13) _cell_length_b 32.110(4) _cell_length_c 13.8506(15) _cell_angle_alpha 90.00 _cell_angle_beta 94.815(4) _cell_angle_gamma 90.00 _cell_volume 5587.6(11) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9970 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 27.62 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.356 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2376 _exptl_absorpt_coefficient_mu 1.095 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8798 _exptl_absorpt_correction_T_max 0.9079 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 42137 _diffrn_reflns_av_R_equivalents 0.0471 _diffrn_reflns_av_sigmaI/netI 0.0411 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 27.71 _reflns_number_total 6425 _reflns_number_gt 4616 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1108P)^2^+14.1681P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6425 _refine_ls_number_parameters 336 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1311 _refine_ls_R_factor_gt 0.0910 _refine_ls_wR_factor_ref 0.2921 _refine_ls_wR_factor_gt 0.3180 _refine_ls_goodness_of_fit_ref 1.254 _refine_ls_restrained_S_all 1.254 _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 Zn2 Zn 0.27749(9) 0.54767(3) 1.01561(9) 0.0419(4) Uani 1 1 d . . 4 Cl1 Cl 0.1208(2) 0.57310(9) 1.0431(3) 0.0775(12) Uani 1 1 d . . 4 Cl2 Cl 0.4154(3) 0.55057(14) 1.1232(4) 0.1001(16) Uani 1 1 d . . 4 C1 C 0.2966(6) 0.7541(2) 0.8587(5) 0.0214(14) Uani 1 1 d . . 4 C2 C 0.2706(6) 0.7132(2) 0.8831(5) 0.0245(15) Uani 1 1 d . . 4 C3 C 0.3423(7) 0.6900(2) 0.9424(6) 0.0268(16) Uani 1 1 d . . 4 C4 C 0.4400(6) 0.7071(2) 0.9801(6) 0.0253(15) Uani 1 1 d . . 4 C5 C 0.4639(6) 0.7486(2) 0.9588(5) 0.0205(14) Uani 1 1 d . . 4 C6 C 0.3915(6) 0.7720(2) 0.9000(5) 0.0193(14) Uani 1 1 d . . 4 C7 C 0.1650(7) 0.6947(3) 0.8456(7) 0.038(2) Uani 1 1 d . . 4 H7A H 0.1690 0.6853 0.7787 0.057 Uiso 1 1 calc R . 4 H7B H 0.1091 0.7158 0.8476 0.057 Uiso 1 1 calc R . 4 H7C H 0.1484 0.6710 0.8862 0.057 Uiso 1 1 calc R . 4 C8 C 0.3153(8) 0.6452(2) 0.9648(6) 0.0345(19) Uani 1 1 d . . 4 H8A H 0.3584 0.6361 1.0241 0.041 Uiso 1 1 calc R . 4 H8B H 0.2393 0.6432 0.9772 0.041 Uiso 1 1 calc R . 4 N1 N 0.3362(7) 0.6174(2) 0.8838(6) 0.0390(18) Uani 1 1 d . . 4 N2 N 0.3219(8) 0.5761(2) 0.8928(7) 0.050(2) Uani 1 1 d . . 4 C9 C 0.3625(11) 0.6264(4) 0.7950(8) 0.059(3) Uani 1 1 d . . 4 H9 H 0.3761 0.6534 0.7708 0.070 Uiso 1 1 calc R . 4 C10 C 0.3665(13) 0.5900(4) 0.7448(9) 0.071(4) Uani 1 1 d . . 4 H10 H 0.3828 0.5865 0.6796 0.085 Uiso 1 1 calc R . 4 C11 C 0.3423(12) 0.5598(4) 0.8077(10) 0.068(4) Uani 1 1 d . . 4 H11 H 0.3402 0.5308 0.7933 0.081 Uiso 1 1 calc R . 4 C12 C 0.5161(8) 0.6815(3) 1.0450(8) 0.048(3) Uani 1 1 d . . 4 H12A H 0.5862 0.6815 1.0193 0.071 Uiso 1 1 calc R . 4 H12B H 0.4897 0.6528 1.0476 0.071 Uiso 1 1 calc R . 4 H12C H 0.5221 0.6934 1.1103 0.071 Uiso 1 1 calc R . 4 C13 C 0.4110(6) 0.8176(2) 0.8841(6) 0.0250(15) Uani 1 1 d . . 4 H13A H 0.4466 0.8297 0.9431 0.037 Uiso 1 1 calc R . 4 H13B H 0.3428 0.8317 0.8683 0.037 Uiso 1 1 calc R . 4 H13C H 0.4561 0.8210 0.8304 0.037 Uiso 1 1 calc R . 4 C14 C 0.5657(6) 0.7683(2) 1.0059(5) 0.0227(14) Uani 1 1 d . . 4 H14A H 0.5458 0.7866 1.0590 0.027 Uiso 1 1 calc R . 4 H14B H 0.6104 0.7456 1.0360 0.027 Uiso 1 1 calc R . 4 C15 C 0.6346(6) 0.7937(2) 0.9422(5) 0.0212(14) Uani 1 1 d . . 4 C16 C 0.6595(6) 0.8352(2) 0.9659(5) 0.0234(15) Uani 1 1 d . A 4 C17 C 0.7165(6) 0.8585(2) 0.9028(6) 0.0232(15) Uani 1 1 d . . 4 C18 C 0.2472(6) 0.8414(2) 0.6809(6) 0.0243(15) Uani 1 1 d . . 4 C19 C 0.2678(5) 0.7992(2) 0.7015(5) 0.0220(14) Uani 1 1 d . . 4 C20 C 0.3260(5) 0.7755(2) 0.6389(5) 0.0196(14) Uani 1 1 d . . 4 C21 C 0.6282(7) 0.8546(3) 1.0591(6) 0.0315(18) Uani 1 1 d . A 4 H21A H 0.6325 0.8336 1.1106 0.047 Uiso 1 1 calc R A 4 H21B H 0.5552 0.8652 1.0493 0.047 Uiso 1 1 calc R A 4 H21C H 0.6767 0.8777 1.0777 0.047 Uiso 1 1 calc R A 4 C22 C 0.7340(6) 0.9038(2) 0.9254(6) 0.0272(16) Uani 1 1 d . . 4 C23 C 0.8310(8) 0.9198(3) 0.9577(9) 0.046(2) Uani 1 1 d . . 4 H23 H 0.8920 0.9023 0.9636 0.055 Uiso 1 1 calc R . 4 C24 C 0.8400(8) 0.9613(3) 0.9816(9) 0.047(3) Uani 1 1 d . . 4 H24 H 0.9078 0.9717 1.0056 0.057 Uiso 1 1 calc R . 4 N3 N 0.7596(6) 0.9874(2) 0.9728(6) 0.0374(17) Uani 1 1 d . . 4 C25 C 0.6660(8) 0.9723(3) 0.9403(9) 0.048(3) Uani 1 1 d . . 4 H25 H 0.6069 0.9907 0.9338 0.058 Uiso 1 1 calc R . 4 C26 C 0.6500(7) 0.9312(3) 0.9152(8) 0.043(2) Uani 1 1 d . . 4 H26 H 0.5814 0.9218 0.8911 0.052 Uiso 1 1 calc R . 4 C27 C 0.1844(7) 0.8684(3) 0.7449(6) 0.0349(19) Uani 1 1 d . B 4 H27A H 0.1140 0.8561 0.7501 0.052 Uiso 1 1 calc R B 4 H27B H 0.1762 0.8963 0.7167 0.052 Uiso 1 1 calc R B 4 H27C H 0.2222 0.8703 0.8095 0.052 Uiso 1 1 calc R B 4 C28 C 0.3420(6) 0.7296(2) 0.6563(6) 0.0260(16) Uani 1 1 d . C 4 H28A H 0.3475 0.7154 0.5943 0.039 Uiso 1 1 calc R C 4 H28B H 0.2813 0.7184 0.6877 0.039 Uiso 1 1 calc R C 4 H28C H 0.4075 0.7252 0.6982 0.039 Uiso 1 1 calc R C 4 C29 C 0.2229(6) 0.7792(3) 0.7892(5) 0.0251(15) Uani 1 1 d . . 4 H29A H 0.1918 0.8017 0.8268 0.030 Uiso 1 1 calc R . 4 H29B H 0.1636 0.7608 0.7649 0.030 Uiso 1 1 calc R . 4 C31 C 0.5000 0.0432(11) 0.7500 0.060(9) Uani 0.50 2 d SP . . O1 O 0.4159(19) 0.0195(9) 0.8048(15) 0.113(10) Uani 0.50 1 d P . . 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 Zn2 0.0409(7) 0.0210(5) 0.0653(8) -0.0034(5) 0.0132(5) -0.0040(4) Cl1 0.0459(16) 0.0390(14) 0.152(4) -0.0125(17) 0.0321(19) -0.0008(12) Cl2 0.068(2) 0.100(3) 0.130(4) -0.062(3) -0.004(2) 0.012(2) C1 0.021(3) 0.024(3) 0.020(3) 0.000(3) 0.011(3) 0.001(3) C2 0.023(4) 0.026(4) 0.026(4) -0.003(3) 0.009(3) -0.007(3) C3 0.034(4) 0.019(3) 0.030(4) 0.001(3) 0.014(3) -0.006(3) C4 0.027(4) 0.020(3) 0.029(4) 0.005(3) 0.009(3) 0.004(3) C5 0.021(3) 0.020(3) 0.023(3) 0.000(3) 0.011(3) -0.001(3) C6 0.021(3) 0.018(3) 0.021(3) 0.000(2) 0.009(3) -0.001(3) C7 0.037(5) 0.040(5) 0.038(5) -0.001(4) 0.007(4) -0.016(4) C8 0.049(5) 0.022(4) 0.034(4) -0.001(3) 0.013(4) -0.011(4) N1 0.053(5) 0.022(3) 0.044(4) -0.001(3) 0.014(4) -0.007(3) N2 0.068(6) 0.023(4) 0.062(5) -0.007(4) 0.021(5) -0.009(4) C9 0.093(9) 0.039(6) 0.048(6) 0.000(5) 0.026(6) 0.002(6) C10 0.111(12) 0.054(7) 0.052(7) -0.013(6) 0.031(7) 0.001(7) C11 0.098(10) 0.039(6) 0.069(8) -0.019(6) 0.023(7) -0.007(6) C12 0.042(5) 0.032(5) 0.068(7) 0.027(5) -0.004(5) -0.001(4) C13 0.025(4) 0.018(3) 0.032(4) 0.002(3) 0.001(3) -0.003(3) C14 0.022(4) 0.024(4) 0.022(3) 0.001(3) 0.006(3) -0.001(3) C15 0.018(3) 0.020(3) 0.026(3) 0.002(3) 0.000(3) -0.002(3) C16 0.023(4) 0.020(3) 0.028(4) -0.003(3) 0.001(3) 0.000(3) C17 0.018(3) 0.020(3) 0.032(4) -0.001(3) 0.002(3) -0.001(3) C18 0.018(3) 0.025(4) 0.030(4) -0.002(3) 0.000(3) 0.003(3) C19 0.014(3) 0.025(4) 0.027(4) 0.001(3) 0.000(3) 0.002(3) C20 0.018(3) 0.019(3) 0.022(3) 0.001(3) 0.004(3) 0.000(3) C21 0.038(5) 0.028(4) 0.029(4) -0.009(3) 0.010(3) -0.005(3) C22 0.028(4) 0.019(4) 0.035(4) -0.002(3) 0.005(3) -0.007(3) C23 0.031(5) 0.025(4) 0.079(7) -0.014(4) -0.004(5) 0.003(4) C24 0.031(5) 0.029(5) 0.082(8) -0.012(5) 0.001(5) -0.007(4) N3 0.036(4) 0.020(3) 0.057(5) -0.002(3) 0.008(3) -0.001(3) C25 0.036(5) 0.027(4) 0.080(8) 0.001(5) -0.002(5) 0.004(4) C26 0.029(5) 0.027(4) 0.072(7) -0.005(4) -0.005(4) -0.003(3) C27 0.041(5) 0.031(4) 0.034(4) -0.003(3) 0.012(4) 0.014(4) C28 0.028(4) 0.020(3) 0.031(4) -0.001(3) 0.011(3) 0.002(3) C29 0.017(3) 0.034(4) 0.025(4) 0.002(3) 0.008(3) 0.002(3) C31 0.09(3) 0.06(2) 0.026(13) 0.000 0.014(15) 0.000 O1 0.094(16) 0.17(2) 0.069(13) 0.063(15) -0.046(11) -0.047(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 Zn2 N3 2.029(7) 3_445 ? Zn2 N2 2.050(9) . ? Zn2 Cl2 2.196(5) . ? Zn2 Cl1 2.200(3) . ? C1 C2 1.400(10) . ? C1 C6 1.406(10) . ? C1 C29 1.514(10) . ? C2 C3 1.386(12) . ? C2 C7 1.511(11) . ? C3 C4 1.408(11) . ? C3 C8 1.518(10) . ? C4 C5 1.404(10) . ? C4 C12 1.504(11) . ? C5 C6 1.391(10) . ? C5 C14 1.526(10) . ? C6 C13 1.504(9) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 N1 1.474(11) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? N1 C9 1.333(13) . ? N1 N2 1.345(10) . ? N2 C11 1.335(15) . ? C9 C10 1.363(16) . ? C9 H9 0.9500 . ? C10 C11 1.356(18) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.525(10) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C20 1.393(10) 2_656 ? C15 C16 1.402(10) . ? C16 C17 1.396(11) . ? C16 C21 1.516(10) . ? C17 C18 1.394(11) 2_656 ? C17 C22 1.499(10) . ? C18 C17 1.394(11) 2_656 ? C18 C19 1.405(10) . ? C18 C27 1.510(10) . ? C19 C20 1.408(10) . ? C19 C29 1.524(10) . ? C20 C15 1.393(10) 2_656 ? C20 C28 1.502(10) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.367(12) . ? C22 C26 1.375(12) . ? C23 C24 1.378(12) . ? C23 H23 0.9500 . ? C24 N3 1.313(12) . ? C24 H24 0.9500 . ? N3 C25 1.320(13) . ? N3 Zn2 2.029(7) 3 ? C25 C26 1.376(13) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C31 O1 1.56(3) . ? C31 O1 1.56(3) 2_656 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Zn2 N2 102.4(3) 3_445 . ? N3 Zn2 Cl2 107.5(3) 3_445 . ? N2 Zn2 Cl2 106.8(3) . . ? N3 Zn2 Cl1 109.0(2) 3_445 . ? N2 Zn2 Cl1 106.8(3) . . ? Cl2 Zn2 Cl1 122.57(17) . . ? C2 C1 C6 119.6(7) . . ? C2 C1 C29 120.7(7) . . ? C6 C1 C29 119.8(6) . . ? C3 C2 C1 119.5(7) . . ? C3 C2 C7 120.3(7) . . ? C1 C2 C7 120.2(7) . . ? C2 C3 C4 121.2(7) . . ? C2 C3 C8 119.0(7) . . ? C4 C3 C8 119.8(7) . . ? C5 C4 C3 119.2(7) . . ? C5 C4 C12 120.5(7) . . ? C3 C4 C12 120.3(7) . . ? C6 C5 C4 119.6(7) . . ? C6 C5 C14 120.9(6) . . ? C4 C5 C14 119.4(7) . . ? C5 C6 C1 120.8(6) . . ? C5 C6 C13 120.3(6) . . ? C1 C6 C13 118.9(6) . . ? N1 C8 C3 111.1(7) . . ? N1 C8 H8A 109.4 . . ? C3 C8 H8A 109.4 . . ? N1 C8 H8B 109.4 . . ? C3 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? C9 N1 N2 110.1(8) . . ? C9 N1 C8 130.3(8) . . ? N2 N1 C8 119.4(7) . . ? C11 N2 N1 105.6(9) . . ? C11 N2 Zn2 130.0(7) . . ? N1 N2 Zn2 124.4(6) . . ? N1 C9 C10 107.9(10) . . ? N1 C9 H9 126.0 . . ? C10 C9 H9 126.0 . . ? C11 C10 C9 105.4(11) . . ? C11 C10 H10 127.3 . . ? C9 C10 H10 127.3 . . ? N2 C11 C10 110.8(10) . . ? N2 C11 H11 124.6 . . ? C10 C11 H11 124.6 . . ? C15 C14 C5 118.2(6) . . ? C15 C14 H14A 107.8 . . ? C5 C14 H14A 107.8 . . ? C15 C14 H14B 107.8 . . ? C5 C14 H14B 107.8 . . ? H14A C14 H14B 107.1 . . ? C20 C15 C16 119.9(7) 2_656 . ? C20 C15 C14 120.1(6) 2_656 . ? C16 C15 C14 120.0(7) . . ? C17 C16 C15 118.8(7) . . ? C17 C16 C21 119.7(7) . . ? C15 C16 C21 121.5(7) . . ? C18 C17 C16 122.1(7) 2_656 . ? C18 C17 C22 120.1(7) 2_656 . ? C16 C17 C22 117.7(7) . . ? C17 C18 C19 118.7(7) 2_656 . ? C17 C18 C27 119.2(7) 2_656 . ? C19 C18 C27 122.0(7) . . ? C18 C19 C20 119.7(7) . . ? C18 C19 C29 119.6(7) . . ? C20 C19 C29 120.7(6) . . ? C15 C20 C19 120.6(6) 2_656 . ? C15 C20 C28 119.2(6) 2_656 . ? C19 C20 C28 120.1(6) . . ? C23 C22 C26 117.0(7) . . ? C23 C22 C17 122.9(7) . . ? C26 C22 C17 120.1(7) . . ? C22 C23 C24 119.7(9) . . ? C22 C23 H23 120.2 . . ? C24 C23 H23 120.2 . . ? N3 C24 C23 123.3(9) . . ? N3 C24 H24 118.3 . . ? C23 C24 H24 118.3 . . ? C24 N3 C25 117.2(8) . . ? C24 N3 Zn2 121.0(6) . 3 ? C25 N3 Zn2 121.6(6) . 3 ? N3 C25 C26 123.2(9) . . ? N3 C25 H25 118.4 . . ? C26 C25 H25 118.4 . . ? C22 C26 C25 119.5(8) . . ? C22 C26 H26 120.2 . . ? C25 C26 H26 120.2 . . ? C1 C29 C19 118.8(6) . . ? C1 C29 H29A 107.6 . . ? C19 C29 H29A 107.6 . . ? C1 C29 H29B 107.6 . . ? C19 C29 H29B 107.6 . . ? H29A C29 H29B 107.0 . . ? O1 C31 O1 121(3) . 2_656 ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 27.71 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.473 _refine_diff_density_min -0.635 _refine_diff_density_rms 0.187 # Attachment '7_CoBr2.cif' data_e1436a _database_code_depnum_ccdc_archive 'CCDC 744813' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H54 Br4 Co N4, C H Cl3' _chemical_formula_sum 'C49 H55 Br4 Cl3 Co N4' _chemical_formula_weight 1184.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.5480(2) _cell_length_b 14.7042(3) _cell_length_c 15.2422(3) _cell_angle_alpha 92.5061(9) _cell_angle_beta 92.9050(8) _cell_angle_gamma 110.0702(10) _cell_volume 2422.73(8) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9241 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 27.55 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.624 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1190 _exptl_absorpt_coefficient_mu 3.857 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6547 _exptl_absorpt_correction_T_max 0.7478 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 38997 _diffrn_reflns_av_R_equivalents 0.0399 _diffrn_reflns_av_sigmaI/netI 0.0577 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 27.55 _reflns_number_total 11105 _reflns_number_gt 7946 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0533P)^2^+7.6566P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11105 _refine_ls_number_parameters 556 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0854 _refine_ls_R_factor_gt 0.0542 _refine_ls_wR_factor_ref 0.1349 _refine_ls_wR_factor_gt 0.1209 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.026 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.56254(6) 0.29420(5) 0.57823(4) 0.02677(15) Uani 1 1 d . . . Br1 Br 0.45141(4) 0.21762(4) 0.44125(3) 0.03171(13) Uani 1 1 d . . . Br2 Br 0.46610(6) 0.30407(5) 0.71076(4) 0.04441(16) Uani 1 1 d . . . C1 C 0.7675(4) 0.4000(3) 0.1853(3) 0.0232(9) Uani 1 1 d . . . C2 C 0.7274(4) 0.4531(3) 0.2482(3) 0.0241(10) Uani 1 1 d . . . C3 C 0.8156(4) 0.5197(3) 0.3080(3) 0.0235(10) Uani 1 1 d . . . C4 C 0.9407(4) 0.5286(3) 0.3098(3) 0.0253(10) Uani 1 1 d . . . C5 C 0.9805(4) 0.4788(3) 0.2435(3) 0.0239(10) Uani 1 1 d . . . C6 C 0.8936(4) 0.4182(3) 0.1791(3) 0.0237(10) Uani 1 1 d . . . C7 C 0.5923(4) 0.4416(4) 0.2510(4) 0.0340(12) Uani 1 1 d . . . H7A H 0.5456 0.3763 0.2681 0.051 Uiso 1 1 calc R . . H7B H 0.5601 0.4511 0.1927 0.051 Uiso 1 1 calc R . . H7C H 0.5836 0.4899 0.2941 0.051 Uiso 1 1 calc R . . C8 C 0.7763(4) 0.5862(3) 0.3689(3) 0.0276(10) Uani 1 1 d . . . H8A H 0.8492 0.6443 0.3876 0.033 Uiso 1 1 calc R . . H8B H 0.7154 0.6081 0.3363 0.033 Uiso 1 1 calc R . . N1 N 0.7215(3) 0.5395(3) 0.4476(3) 0.0253(8) Uani 1 1 d . . . C9 C 0.7037(4) 0.4484(4) 0.4676(3) 0.0305(11) Uani 1 1 d . . . H9 H 0.7262 0.4029 0.4325 0.037 Uiso 1 1 calc R . . N2 N 0.6501(4) 0.4300(3) 0.5433(3) 0.0297(9) Uani 1 1 d . . . C10 C 0.6345(4) 0.5140(4) 0.5727(3) 0.0315(11) Uani 1 1 d . . . H10 H 0.5992 0.5230 0.6259 0.038 Uiso 1 1 calc R . . C11 C 0.6771(4) 0.5822(4) 0.5143(3) 0.0307(11) Uani 1 1 d . . . H11 H 0.6766 0.6467 0.5183 0.037 Uiso 1 1 calc R . . C12 C 1.0305(5) 0.5941(4) 0.3822(4) 0.0369(12) Uani 1 1 d . . . H12A H 1.0601 0.6610 0.3643 0.055 Uiso 1 1 calc R . . H12B H 1.1008 0.5721 0.3921 0.055 Uiso 1 1 calc R . . H12C H 0.9882 0.5914 0.4367 0.055 Uiso 1 1 calc R . . C13 C 0.9360(5) 0.3762(4) 0.0995(3) 0.0323(11) Uani 1 1 d . . . H13A H 0.9413 0.3129 0.1122 0.049 Uiso 1 1 calc R . . H13B H 1.0174 0.4202 0.0859 0.049 Uiso 1 1 calc R . . H13C H 0.8766 0.3683 0.0490 0.049 Uiso 1 1 calc R . . C14 C 1.1179(4) 0.4985(3) 0.2368(4) 0.0289(11) Uani 1 1 d . . . H14A H 1.1619 0.5357 0.2915 0.035 Uiso 1 1 calc R . . H14B H 1.1451 0.5410 0.1877 0.035 Uiso 1 1 calc R . . C15 C 1.1612(4) 0.4119(3) 0.2226(3) 0.0259(10) Uani 1 1 d . . . C16 C 1.2371(4) 0.4110(4) 0.1539(3) 0.0288(11) Uani 1 1 d . . . C17 C 1.2735(4) 0.3301(3) 0.1432(3) 0.0262(10) Uani 1 1 d . . . Br3 Br 1.36349(4) 0.32197(4) 0.04134(3) 0.03421(13) Uani 1 1 d . . . C18 C 1.2467(4) 0.2552(3) 0.1992(3) 0.0227(9) Uani 1 1 d . . . C19 C 1.1695(4) 0.2568(3) 0.2670(3) 0.0221(9) Uani 1 1 d . . . C20 C 1.1290(4) 0.3362(3) 0.2797(3) 0.0225(9) Uani 1 1 d . . . C21 C 1.2812(5) 0.4945(4) 0.0951(4) 0.0485(15) Uani 1 1 d . . . H21A H 1.3481 0.4875 0.0614 0.073 Uiso 1 1 calc R . . H21B H 1.3117 0.5558 0.1313 0.073 Uiso 1 1 calc R . . H21C H 1.2125 0.4942 0.0545 0.073 Uiso 1 1 calc R . . C22 C 1.3004(5) 0.1754(4) 0.1887(3) 0.0303(11) Uani 1 1 d . . . H22A H 1.3668 0.1943 0.1483 0.045 Uiso 1 1 calc R . . H22B H 1.2356 0.1155 0.1648 0.045 Uiso 1 1 calc R . . H22C H 1.3337 0.1646 0.2462 0.045 Uiso 1 1 calc R . . C23 C 1.0552(4) 0.3421(3) 0.3567(3) 0.0271(10) Uani 1 1 d . . . H23A H 0.9669 0.3158 0.3381 0.041 Uiso 1 1 calc R . . H23B H 1.0775 0.4100 0.3786 0.041 Uiso 1 1 calc R . . H23C H 1.0730 0.3043 0.4036 0.041 Uiso 1 1 calc R . . C24 C 1.1363(4) 0.1740(3) 0.3281(3) 0.0246(10) Uani 1 1 d . . . H24A H 1.1853 0.1986 0.3848 0.029 Uiso 1 1 calc R . . H24B H 1.1644 0.1228 0.3026 0.029 Uiso 1 1 calc R . . C25 C 1.0019(4) 0.1262(3) 0.3484(3) 0.0222(9) Uani 1 1 d . . . C26 C 0.9691(4) 0.1135(3) 0.4357(3) 0.0211(9) Uani 1 1 d . . . C27 C 0.8455(4) 0.0616(3) 0.4517(3) 0.0229(9) Uani 1 1 d . . . C28 C 0.7531(4) 0.0294(3) 0.3827(3) 0.0221(9) Uani 1 1 d . . . C29 C 0.7858(4) 0.0448(3) 0.2958(3) 0.0224(9) Uani 1 1 d . . . C30 C 0.9103(4) 0.0887(3) 0.2789(3) 0.0203(9) Uani 1 1 d . . . C31 C 1.0616(4) 0.1536(4) 0.5143(3) 0.0286(10) Uani 1 1 d . . . H31A H 1.0833 0.1007 0.5392 0.043 Uiso 1 1 calc R . . H31B H 1.0250 0.1832 0.5589 0.043 Uiso 1 1 calc R . . H31C H 1.1361 0.2026 0.4955 0.043 Uiso 1 1 calc R . . C32 C 0.8130(4) 0.0397(3) 0.5451(3) 0.0244(10) Uani 1 1 d . . . H32A H 0.7479 -0.0250 0.5450 0.029 Uiso 1 1 calc R . . H32B H 0.8867 0.0378 0.5799 0.029 Uiso 1 1 calc R . . N3 N 0.7688(3) 0.1130(3) 0.5875(2) 0.0240(8) Uani 1 1 d . . . C33 C 0.7102(4) 0.1663(3) 0.5474(3) 0.0259(10) Uani 1 1 d . . . H33 H 0.6977 0.1671 0.4854 0.031 Uiso 1 1 calc R . . N4 N 0.6724(3) 0.2174(3) 0.6054(2) 0.0261(9) Uani 1 1 d . . . C34 C 0.7074(5) 0.1947(4) 0.6864(3) 0.0341(12) Uani 1 1 d . . . H34 H 0.6922 0.2200 0.7414 0.041 Uiso 1 1 calc R . . C35 C 0.7668(5) 0.1305(4) 0.6758(3) 0.0354(12) Uani 1 1 d . . . H35 H 0.8006 0.1030 0.7212 0.042 Uiso 1 1 calc R . . C36 C 0.6195(4) -0.0222(4) 0.4000(3) 0.0287(11) Uani 1 1 d . . . H36A H 0.6119 -0.0267 0.4636 0.043 Uiso 1 1 calc R . . H36B H 0.5910 -0.0877 0.3710 0.043 Uiso 1 1 calc R . . H36C H 0.5691 0.0141 0.3768 0.043 Uiso 1 1 calc R . . C37 C 0.9486(4) 0.0923(4) 0.1852(3) 0.0296(11) Uani 1 1 d . . . H37A H 0.8877 0.0396 0.1483 0.044 Uiso 1 1 calc R . . H37B H 1.0298 0.0851 0.1840 0.044 Uiso 1 1 calc R . . H37C H 0.9532 0.1548 0.1626 0.044 Uiso 1 1 calc R . . C38 C 0.6854(4) 0.0080(3) 0.2213(3) 0.0260(10) Uani 1 1 d . . . H38A H 0.6047 -0.0097 0.2477 0.031 Uiso 1 1 calc R . . H38B H 0.6914 -0.0526 0.1943 0.031 Uiso 1 1 calc R . . C39 C 0.6828(4) 0.0738(3) 0.1471(3) 0.0225(9) Uani 1 1 d . . . C40 C 0.6749(4) 0.0380(3) 0.0592(3) 0.0249(10) Uani 1 1 d . . . C41 C 0.6656(4) 0.0983(3) -0.0059(3) 0.0232(9) Uani 1 1 d . . . Br4 Br 0.65032(5) 0.04978(4) -0.12586(3) 0.03442(13) Uani 1 1 d . . . C42 C 0.6656(4) 0.1928(3) 0.0104(3) 0.0262(10) Uani 1 1 d . . . C43 C 0.6754(4) 0.2281(3) 0.0987(3) 0.0225(9) Uani 1 1 d . . . C44 C 0.6789(4) 0.1668(3) 0.1665(3) 0.0228(9) Uani 1 1 d . . . C45 C 0.6735(5) -0.0629(4) 0.0343(3) 0.0371(12) Uani 1 1 d . . . H45A H 0.7529 -0.0590 0.0117 0.056 Uiso 1 1 calc R . . H45B H 0.6068 -0.0940 -0.0112 0.056 Uiso 1 1 calc R . . H45C H 0.6598 -0.1012 0.0863 0.056 Uiso 1 1 calc R . . C46 C 0.6523(6) 0.2523(4) -0.0652(3) 0.0393(13) Uani 1 1 d . . . H46A H 0.7338 0.2857 -0.0865 0.059 Uiso 1 1 calc R . . H46B H 0.6163 0.3003 -0.0451 0.059 Uiso 1 1 calc R . . H46C H 0.5982 0.2095 -0.1129 0.059 Uiso 1 1 calc R . . C47 C 0.6712(5) 0.1998(4) 0.2605(3) 0.0286(10) Uani 1 1 d . . . H47A H 0.7548 0.2307 0.2885 0.043 Uiso 1 1 calc R . . H47B H 0.6262 0.1437 0.2928 0.043 Uiso 1 1 calc R . . H47C H 0.6277 0.2465 0.2614 0.043 Uiso 1 1 calc R . . C48 C 0.6709(4) 0.3284(3) 0.1195(3) 0.0276(10) Uani 1 1 d . . . H48A H 0.5887 0.3199 0.1412 0.033 Uiso 1 1 calc R . . H48B H 0.6748 0.3601 0.0632 0.033 Uiso 1 1 calc R . . C49 C 0.9069(7) 0.7758(6) 0.1208(5) 0.071(2) Uani 1 1 d . . . H49 H 0.8207 0.7485 0.0929 0.086 Uiso 1 1 calc R . . Cl1 Cl 0.9591(3) 0.6795(2) 0.13647(16) 0.108 Uani 1 1 d . . . Cl2 Cl 0.9018(3) 0.8367(2) 0.22061(16) 0.1120(9) Uani 1 1 d . . . Cl3 Cl 0.9960(3) 0.8546(2) 0.05056(18) 0.1109(9) 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 Co1 0.0288(3) 0.0293(4) 0.0252(3) -0.0003(3) 0.0006(3) 0.0144(3) Br1 0.0334(3) 0.0313(3) 0.0300(3) -0.0001(2) -0.0061(2) 0.0121(2) Br2 0.0552(3) 0.0557(4) 0.0370(3) 0.0061(3) 0.0146(3) 0.0360(3) C1 0.025(2) 0.018(2) 0.026(2) 0.0025(19) -0.0021(18) 0.0070(18) C2 0.025(2) 0.019(2) 0.030(3) 0.0027(19) 0.0017(19) 0.0098(18) C3 0.027(2) 0.018(2) 0.027(3) -0.0027(19) 0.0021(19) 0.0096(19) C4 0.024(2) 0.017(2) 0.033(3) -0.0032(19) -0.0015(19) 0.0063(18) C5 0.022(2) 0.018(2) 0.031(3) 0.0002(19) -0.0003(19) 0.0065(18) C6 0.028(2) 0.017(2) 0.026(3) 0.0002(18) 0.0012(19) 0.0090(18) C7 0.022(2) 0.037(3) 0.042(3) -0.013(2) -0.004(2) 0.012(2) C8 0.031(2) 0.020(2) 0.033(3) -0.002(2) 0.003(2) 0.010(2) N1 0.0232(18) 0.020(2) 0.032(2) -0.0074(17) -0.0015(16) 0.0085(16) C9 0.036(3) 0.025(3) 0.035(3) 0.000(2) 0.005(2) 0.015(2) N2 0.032(2) 0.029(2) 0.030(2) -0.0050(18) -0.0001(18) 0.0141(18) C10 0.028(2) 0.035(3) 0.032(3) -0.012(2) 0.000(2) 0.013(2) C11 0.026(2) 0.027(3) 0.039(3) -0.011(2) 0.001(2) 0.010(2) C12 0.031(3) 0.030(3) 0.045(3) -0.012(2) -0.007(2) 0.008(2) C13 0.032(2) 0.034(3) 0.031(3) -0.003(2) 0.003(2) 0.012(2) C14 0.023(2) 0.020(2) 0.044(3) 0.002(2) 0.004(2) 0.0071(19) C15 0.020(2) 0.023(2) 0.032(3) -0.002(2) -0.0024(19) 0.0057(18) C16 0.024(2) 0.030(3) 0.031(3) 0.007(2) 0.002(2) 0.009(2) C17 0.016(2) 0.031(3) 0.029(3) 0.001(2) 0.0006(18) 0.0062(19) Br3 0.0293(2) 0.0477(3) 0.0280(3) 0.0028(2) 0.0052(2) 0.0160(2) C18 0.020(2) 0.023(2) 0.025(2) -0.0016(19) -0.0014(18) 0.0078(18) C19 0.020(2) 0.023(2) 0.022(2) -0.0018(18) -0.0030(17) 0.0075(18) C20 0.019(2) 0.022(2) 0.024(2) -0.0012(19) -0.0021(17) 0.0047(18) C21 0.047(3) 0.042(3) 0.064(4) 0.021(3) 0.027(3) 0.020(3) C22 0.034(3) 0.034(3) 0.028(3) 0.001(2) 0.008(2) 0.018(2) C23 0.029(2) 0.026(3) 0.028(3) -0.005(2) -0.001(2) 0.013(2) C24 0.025(2) 0.027(2) 0.025(2) 0.000(2) 0.0005(18) 0.015(2) C25 0.026(2) 0.019(2) 0.024(2) 0.0003(18) -0.0006(18) 0.0113(18) C26 0.028(2) 0.016(2) 0.022(2) -0.0007(18) -0.0020(18) 0.0123(18) C27 0.030(2) 0.019(2) 0.024(2) 0.0003(18) 0.0001(19) 0.0144(19) C28 0.027(2) 0.019(2) 0.021(2) 0.0003(18) -0.0009(18) 0.0102(18) C29 0.027(2) 0.020(2) 0.023(2) 0.0015(18) -0.0011(18) 0.0109(19) C30 0.030(2) 0.015(2) 0.018(2) 0.0004(17) 0.0017(18) 0.0100(18) C31 0.031(2) 0.029(3) 0.025(3) -0.002(2) -0.005(2) 0.011(2) C32 0.031(2) 0.025(2) 0.021(2) 0.0054(19) 0.0031(19) 0.014(2) N3 0.0274(19) 0.029(2) 0.019(2) 0.0032(16) 0.0016(15) 0.0131(17) C33 0.033(2) 0.027(3) 0.020(2) 0.0032(19) 0.0005(19) 0.013(2) N4 0.0257(19) 0.033(2) 0.023(2) 0.0003(17) 0.0015(16) 0.0139(17) C34 0.043(3) 0.054(3) 0.014(2) 0.000(2) 0.002(2) 0.030(3) C35 0.046(3) 0.056(4) 0.014(2) 0.007(2) 0.003(2) 0.030(3) C36 0.029(2) 0.029(3) 0.025(3) 0.005(2) 0.0015(19) 0.005(2) C37 0.028(2) 0.037(3) 0.019(2) -0.005(2) -0.0015(19) 0.007(2) C38 0.031(2) 0.020(2) 0.023(2) 0.0008(19) -0.0028(19) 0.0045(19) C39 0.021(2) 0.024(2) 0.020(2) -0.0016(19) -0.0026(17) 0.0068(18) C40 0.026(2) 0.025(2) 0.022(2) -0.0042(19) -0.0053(18) 0.0083(19) C41 0.024(2) 0.030(3) 0.013(2) -0.0031(18) 0.0010(17) 0.0068(19) Br4 0.0486(3) 0.0375(3) 0.0185(2) -0.0047(2) -0.0016(2) 0.0180(2) C42 0.029(2) 0.026(2) 0.023(3) 0.002(2) 0.0009(19) 0.010(2) C43 0.022(2) 0.024(2) 0.020(2) -0.0023(18) -0.0007(17) 0.0072(18) C44 0.023(2) 0.025(2) 0.020(2) -0.0002(19) -0.0013(18) 0.0078(19) C45 0.061(3) 0.033(3) 0.021(3) -0.004(2) 0.001(2) 0.022(3) C46 0.068(4) 0.033(3) 0.021(3) 0.005(2) 0.001(2) 0.022(3) C47 0.039(3) 0.032(3) 0.018(2) -0.001(2) 0.003(2) 0.017(2) C48 0.028(2) 0.027(3) 0.029(3) -0.007(2) -0.005(2) 0.013(2) C49 0.066(4) 0.067(5) 0.070(5) 0.017(4) -0.022(4) 0.011(4) Cl1 0.150 0.139 0.070 0.017 0.018 0.092 Cl2 0.128(2) 0.160(3) 0.0793(16) 0.0230(16) 0.0218(15) 0.087(2) Cl3 0.1132(19) 0.112(2) 0.1072(19) 0.0408(16) 0.0469(16) 0.0296(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 Co1 N4 2.007(4) . ? Co1 N2 2.014(4) . ? Co1 Br2 2.3781(8) . ? Co1 Br1 2.4094(8) . ? C1 C6 1.396(6) . ? C1 C2 1.404(6) . ? C1 C48 1.531(6) . ? C2 C3 1.404(6) . ? C2 C7 1.514(6) . ? C3 C4 1.405(6) . ? C3 C8 1.514(6) . ? C4 C5 1.407(6) . ? C4 C12 1.525(7) . ? C5 C6 1.406(6) . ? C5 C14 1.521(6) . ? C6 C13 1.515(6) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 N1 1.470(6) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? N1 C9 1.335(6) . ? N1 C11 1.381(6) . ? C9 N2 1.332(6) . ? C9 H9 0.9500 . ? N2 C10 1.368(6) . ? C10 C11 1.351(7) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.530(6) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.402(7) . ? C15 C20 1.404(6) . ? C16 C17 1.397(7) . ? C16 C21 1.510(7) . ? C17 C18 1.383(6) . ? C17 Br3 1.933(5) . ? C18 C19 1.404(6) . ? C18 C22 1.509(6) . ? C19 C20 1.408(6) . ? C19 C24 1.520(6) . ? C20 C23 1.501(6) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.523(6) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.403(6) . ? C25 C30 1.408(6) . ? C26 C27 1.408(6) . ? C26 C31 1.517(6) . ? C27 C28 1.401(6) . ? C27 C32 1.512(6) . ? C28 C29 1.403(6) . ? C28 C36 1.510(6) . ? C29 C30 1.401(6) . ? C29 C38 1.520(6) . ? C30 C37 1.515(6) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 N3 1.478(6) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? N3 C33 1.345(6) . ? N3 C35 1.362(6) . ? C33 N4 1.320(6) . ? C33 H33 0.9500 . ? N4 C34 1.371(6) . ? C34 C35 1.352(7) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C39 1.525(6) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C44 1.403(6) . ? C39 C40 1.405(6) . ? C40 C41 1.383(6) . ? C40 C45 1.510(7) . ? C41 C42 1.400(7) . ? C41 Br4 1.911(4) . ? C42 C43 1.406(6) . ? C42 C46 1.510(7) . ? C43 C44 1.409(6) . ? C43 C48 1.513(6) . ? C44 C47 1.510(6) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 Cl3 1.718(8) . ? C49 Cl1 1.738(8) . ? C49 Cl2 1.745(9) . ? C49 H49 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 N4 Co1 N2 115.16(16) . . ? N4 Co1 Br2 105.14(11) . . ? N2 Co1 Br2 108.33(12) . . ? N4 Co1 Br1 103.74(11) . . ? N2 Co1 Br1 101.12(12) . . ? Br2 Co1 Br1 123.86(3) . . ? C6 C1 C2 120.1(4) . . ? C6 C1 C48 121.2(4) . . ? C2 C1 C48 118.5(4) . . ? C3 C2 C1 118.8(4) . . ? C3 C2 C7 119.8(4) . . ? C1 C2 C7 121.3(4) . . ? C2 C3 C4 121.1(4) . . ? C2 C3 C8 119.5(4) . . ? C4 C3 C8 119.3(4) . . ? C3 C4 C5 119.2(4) . . ? C3 C4 C12 119.0(4) . . ? C5 C4 C12 121.8(4) . . ? C6 C5 C4 119.4(4) . . ? C6 C5 C14 120.4(4) . . ? C4 C5 C14 119.9(4) . . ? C1 C6 C5 120.5(4) . . ? C1 C6 C13 119.1(4) . . ? C5 C6 C13 120.3(4) . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 C3 113.0(4) . . ? N1 C8 H8A 109.0 . . ? C3 C8 H8A 109.0 . . ? N1 C8 H8B 109.0 . . ? C3 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? C9 N1 C11 107.3(4) . . ? C9 N1 C8 126.9(4) . . ? C11 N1 C8 125.9(4) . . ? N2 C9 N1 110.8(4) . . ? N2 C9 H9 124.6 . . ? N1 C9 H9 124.6 . . ? C9 N2 C10 106.2(4) . . ? C9 N2 Co1 122.7(3) . . ? C10 N2 Co1 128.2(3) . . ? C11 C10 N2 109.4(4) . . ? C11 C10 H10 125.3 . . ? N2 C10 H10 125.3 . . ? C10 C11 N1 106.4(4) . . ? C10 C11 H11 126.8 . . ? N1 C11 H11 126.8 . . ? C4 C12 H12A 109.5 . . ? C4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C6 C13 H13A 109.5 . . ? C6 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C6 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C5 C14 C15 118.5(4) . . ? C5 C14 H14A 107.7 . . ? C15 C14 H14A 107.7 . . ? C5 C14 H14B 107.7 . . ? C15 C14 H14B 107.7 . . ? H14A C14 H14B 107.1 . . ? C16 C15 C20 120.5(4) . . ? C16 C15 C14 119.2(4) . . ? C20 C15 C14 120.2(4) . . ? C17 C16 C15 117.0(4) . . ? C17 C16 C21 120.9(4) . . ? C15 C16 C21 122.1(4) . . ? C18 C17 C16 124.3(4) . . ? C18 C17 Br3 118.5(3) . . ? C16 C17 Br3 117.2(3) . . ? C17 C18 C19 117.6(4) . . ? C17 C18 C22 121.2(4) . . ? C19 C18 C22 121.2(4) . . ? C18 C19 C20 120.0(4) . . ? C18 C19 C24 118.6(4) . . ? C20 C19 C24 121.3(4) . . ? C15 C20 C19 120.3(4) . . ? C15 C20 C23 119.6(4) . . ? C19 C20 C23 120.0(4) . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C18 C22 H22A 109.5 . . ? C18 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C18 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C19 C24 C25 119.0(4) . . ? C19 C24 H24A 107.6 . . ? C25 C24 H24A 107.6 . . ? C19 C24 H24B 107.6 . . ? C25 C24 H24B 107.6 . . ? H24A C24 H24B 107.0 . . ? C26 C25 C30 119.4(4) . . ? C26 C25 C24 120.8(4) . . ? C30 C25 C24 119.6(4) . . ? C25 C26 C27 119.2(4) . . ? C25 C26 C31 122.7(4) . . ? C27 C26 C31 118.1(4) . . ? C28 C27 C26 121.3(4) . . ? C28 C27 C32 119.7(4) . . ? C26 C27 C32 119.0(4) . . ? C27 C28 C29 119.2(4) . . ? C27 C28 C36 121.4(4) . . ? C29 C28 C36 119.4(4) . . ? C30 C29 C28 119.8(4) . . ? C30 C29 C38 121.3(4) . . ? C28 C29 C38 118.9(4) . . ? C29 C30 C25 120.8(4) . . ? C29 C30 C37 120.2(4) . . ? C25 C30 C37 119.0(4) . . ? C26 C31 H31A 109.5 . . ? C26 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C26 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N3 C32 C27 112.1(4) . . ? N3 C32 H32A 109.2 . . ? C27 C32 H32A 109.2 . . ? N3 C32 H32B 109.2 . . ? C27 C32 H32B 109.2 . . ? H32A C32 H32B 107.9 . . ? C33 N3 C35 106.9(4) . . ? C33 N3 C32 126.9(4) . . ? C35 N3 C32 125.8(4) . . ? N4 C33 N3 111.2(4) . . ? N4 C33 H33 124.4 . . ? N3 C33 H33 124.4 . . ? C33 N4 C34 105.8(4) . . ? C33 N4 Co1 125.8(3) . . ? C34 N4 Co1 127.7(3) . . ? C35 C34 N4 109.2(4) . . ? C35 C34 H34 125.4 . . ? N4 C34 H34 125.4 . . ? C34 C35 N3 106.9(4) . . ? C34 C35 H35 126.5 . . ? N3 C35 H35 126.5 . . ? C28 C36 H36A 109.5 . . ? C28 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C28 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C30 C37 H37A 109.5 . . ? C30 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C30 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C29 C38 C39 119.1(4) . . ? C29 C38 H38A 107.5 . . ? C39 C38 H38A 107.5 . . ? C29 C38 H38B 107.5 . . ? C39 C38 H38B 107.5 . . ? H38A C38 H38B 107.0 . . ? C44 C39 C40 120.2(4) . . ? C44 C39 C38 120.1(4) . . ? C40 C39 C38 119.5(4) . . ? C41 C40 C39 117.5(4) . . ? C41 C40 C45 119.9(4) . . ? C39 C40 C45 122.6(4) . . ? C40 C41 C42 124.2(4) . . ? C40 C41 Br4 118.2(3) . . ? C42 C41 Br4 117.6(3) . . ? C41 C42 C43 117.6(4) . . ? C41 C42 C46 120.2(4) . . ? C43 C42 C46 122.1(4) . . ? C42 C43 C44 119.5(4) . . ? C42 C43 C48 119.5(4) . . ? C44 C43 C48 120.8(4) . . ? C39 C44 C43 120.8(4) . . ? C39 C44 C47 119.8(4) . . ? C43 C44 C47 119.3(4) . . ? C40 C45 H45A 109.5 . . ? C40 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C40 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C42 C46 H46A 109.5 . . ? C42 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C42 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C44 C47 H47A 109.5 . . ? C44 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C44 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C43 C48 C1 120.4(4) . . ? C43 C48 H48A 107.2 . . ? C1 C48 H48A 107.2 . . ? C43 C48 H48B 107.2 . . ? C1 C48 H48B 107.2 . . ? H48A C48 H48B 106.9 . . ? Cl3 C49 Cl1 111.1(5) . . ? Cl3 C49 Cl2 110.7(4) . . ? Cl1 C49 Cl2 111.6(4) . . ? Cl3 C49 H49 107.8 . . ? Cl1 C49 H49 107.8 . . ? Cl2 C49 H49 107.8 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.104 _refine_diff_density_min -2.228 _refine_diff_density_rms 0.116 # Attachment '7-CoCl2.cif' data_e1489a _database_code_depnum_ccdc_archive 'CCDC 744814' #TrackingRef '7-CoCl2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C48 H54 Br2 Cl2 Co N4), 5(H2 O)' _chemical_formula_sum 'C96 H118 Br4 Cl4 Co2 N8 O5' _chemical_formula_weight 2043.28 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.8253(9) _cell_length_b 14.3000(11) _cell_length_c 15.6345(12) _cell_angle_alpha 92.834(4) _cell_angle_beta 99.430(3) _cell_angle_gamma 107.919(4) _cell_volume 2467.5(3) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9251 _cell_measurement_theta_min 2.66 _cell_measurement_theta_max 26.62 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.375 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1052 _exptl_absorpt_coefficient_mu 2.117 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7560 _exptl_absorpt_correction_T_max 0.8162 _exptl_absorpt_process_details sadabs _exptl_special_details ; There is a disorder with the molecules water, therefore we can't see their hydrogene and we fixed their thermal parameters ; _diffrn_ambient_temperature 173(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 33489 _diffrn_reflns_av_R_equivalents 0.0485 _diffrn_reflns_av_sigmaI/netI 0.0673 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10866 _reflns_number_gt 6978 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1460P)^2^+8.8207P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10866 _refine_ls_number_parameters 538 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1285 _refine_ls_R_factor_gt 0.0820 _refine_ls_wR_factor_ref 0.2717 _refine_ls_wR_factor_gt 0.2357 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.56605(8) 0.29474(7) 0.57105(6) 0.0382(3) Uani 1 1 d . . . Cl1 Cl 0.44142(18) 0.21111(14) 0.44744(13) 0.0486(5) Uani 1 1 d . . . Cl2 Cl 0.5031(2) 0.32045(18) 0.69488(14) 0.0608(6) Uani 1 1 d . . . C1 C 0.7406(6) 0.4014(5) 0.1877(4) 0.0315(13) Uani 1 1 d . . . C2 C 0.7055(6) 0.4548(5) 0.2507(5) 0.0364(15) Uani 1 1 d . . . C3 C 0.7940(6) 0.5216(5) 0.3141(4) 0.0330(14) Uani 1 1 d . . . C4 C 0.9168(5) 0.5309(4) 0.3203(4) 0.0290(13) Uani 1 1 d . . . C5 C 0.9521(5) 0.4802(4) 0.2549(4) 0.0284(13) Uani 1 1 d . . . C6 C 0.8633(6) 0.4192(5) 0.1865(4) 0.0317(13) Uani 1 1 d . . . C7 C 0.5721(7) 0.4408(6) 0.2492(6) 0.054(2) Uani 1 1 d . . . H7A H 0.5281 0.3704 0.2491 0.080 Uiso 1 1 calc R . . H7B H 0.5386 0.4650 0.1965 0.080 Uiso 1 1 calc R . . H7C H 0.5638 0.4780 0.3008 0.080 Uiso 1 1 calc R . . C8 C 0.7587(6) 0.5877(5) 0.3741(5) 0.0378(15) Uani 1 1 d . . . H8A H 0.8300 0.6466 0.3963 0.045 Uiso 1 1 calc R . . H8B H 0.6956 0.6105 0.3403 0.045 Uiso 1 1 calc R . . N1 N 0.7123(5) 0.5409(4) 0.4495(4) 0.0369(13) Uani 1 1 d . . . C9 C 0.6925(7) 0.4467(5) 0.4654(5) 0.0421(17) Uani 1 1 d . . . H9 H 0.7084 0.3986 0.4294 0.050 Uiso 1 1 calc R . . N2 N 0.6480(5) 0.4289(5) 0.5372(4) 0.0420(14) Uani 1 1 d . . . C10 C 0.6398(6) 0.5175(5) 0.5693(5) 0.0431(17) Uani 1 1 d . . . H10 H 0.6116 0.5283 0.6212 0.052 Uiso 1 1 calc R . . C11 C 0.6783(6) 0.5868(5) 0.5152(5) 0.0416(17) Uani 1 1 d . . . H11 H 0.6811 0.6540 0.5215 0.050 Uiso 1 1 calc R . . C12 C 1.0101(6) 0.5968(5) 0.3950(5) 0.0396(16) Uani 1 1 d . . . H12A H 1.0526 0.6593 0.3744 0.059 Uiso 1 1 calc R . . H12B H 1.0684 0.5636 0.4171 0.059 Uiso 1 1 calc R . . H12C H 0.9696 0.6101 0.4419 0.059 Uiso 1 1 calc R . . C13 C 0.9027(7) 0.3798(6) 0.1090(4) 0.0395(16) Uani 1 1 d . . . H13A H 0.9042 0.3125 0.1164 0.059 Uiso 1 1 calc R . . H13B H 0.9837 0.4223 0.1047 0.059 Uiso 1 1 calc R . . H13C H 0.8455 0.3788 0.0557 0.059 Uiso 1 1 calc R . . C14 C 1.0862(6) 0.4971(5) 0.2543(4) 0.0326(14) Uani 1 1 d . . . H14A H 1.1088 0.5394 0.2076 0.039 Uiso 1 1 calc R . . H14B H 1.1332 0.5353 0.3103 0.039 Uiso 1 1 calc R . . C15 C 1.1274(5) 0.4078(5) 0.2417(4) 0.0316(13) Uani 1 1 d . . . C16 C 1.1963(6) 0.4026(5) 0.1760(5) 0.0361(15) Uani 1 1 d . . . C17 C 1.2303(5) 0.3190(5) 0.1669(4) 0.0359(15) Uani 1 1 d . . . Br1 Br 1.30887(7) 0.30514(7) 0.07036(5) 0.0513(2) Uani 1 1 d . . . C18 C 1.2094(6) 0.2427(5) 0.2200(4) 0.0353(15) Uani 1 1 d . . . C19 C 1.1402(6) 0.2484(5) 0.2840(4) 0.0314(13) Uani 1 1 d . . . C20 C 1.1003(5) 0.3310(5) 0.2947(4) 0.0296(13) Uani 1 1 d . . . C21 C 1.2335(8) 0.4865(6) 0.1206(6) 0.0515(19) Uani 1 1 d . . . H21A H 1.2718 0.5488 0.1584 0.077 Uiso 1 1 calc R . . H21B H 1.1618 0.4903 0.0814 0.077 Uiso 1 1 calc R . . H21C H 1.2909 0.4747 0.0862 0.077 Uiso 1 1 calc R . . C22 C 1.2623(7) 0.1603(6) 0.2095(5) 0.0469(18) Uani 1 1 d . . . H22A H 1.3313 0.1826 0.1798 0.070 Uiso 1 1 calc R . . H22B H 1.2006 0.1029 0.1747 0.070 Uiso 1 1 calc R . . H22C H 1.2895 0.1421 0.2670 0.070 Uiso 1 1 calc R . . C23 C 1.0350(6) 0.3395(5) 0.3687(4) 0.0343(14) Uani 1 1 d . . . H23A H 0.9475 0.3178 0.3463 0.052 Uiso 1 1 calc R . . H23B H 1.0617 0.4084 0.3943 0.052 Uiso 1 1 calc R . . H23C H 1.0533 0.2978 0.4133 0.052 Uiso 1 1 calc R . . C24 C 1.1114(6) 0.1658(5) 0.3425(4) 0.0355(14) Uani 1 1 d . . . H24A H 1.1608 0.1920 0.4012 0.043 Uiso 1 1 calc R . . H24B H 1.1400 0.1128 0.3202 0.043 Uiso 1 1 calc R . . C25 C 0.9810(6) 0.1175(4) 0.3538(4) 0.0283(13) Uani 1 1 d . . . C26 C 0.9516(6) 0.1063(4) 0.4364(4) 0.0303(13) Uani 1 1 d . . . C27 C 0.8334(6) 0.0536(4) 0.4433(4) 0.0317(14) Uani 1 1 d . . . C28 C 0.7403(6) 0.0204(5) 0.3706(4) 0.0331(14) Uani 1 1 d . . . C29 C 0.7688(6) 0.0365(4) 0.2879(4) 0.0302(13) Uani 1 1 d . . . C30 C 0.8901(6) 0.0793(5) 0.2789(4) 0.0312(13) Uani 1 1 d . . . C31 C 1.0457(7) 0.1483(5) 0.5193(4) 0.0388(16) Uani 1 1 d . . . H31A H 1.0708 0.0950 0.5449 0.058 Uiso 1 1 calc R . . H31B H 1.0108 0.1789 0.5611 0.058 Uiso 1 1 calc R . . H31C H 1.1162 0.1982 0.5053 0.058 Uiso 1 1 calc R . . C32 C 0.8064(6) 0.0294(5) 0.5331(4) 0.0355(15) Uani 1 1 d . . . H32A H 0.7416 -0.0351 0.5269 0.043 Uiso 1 1 calc R . . H32B H 0.8797 0.0230 0.5698 0.043 Uiso 1 1 calc R . . N3 N 0.7684(5) 0.1047(4) 0.5778(3) 0.0342(12) Uani 1 1 d . . . C33 C 0.7046(6) 0.1590(5) 0.5407(4) 0.0375(15) Uani 1 1 d . . . H33 H 0.6807 0.1573 0.4795 0.045 Uiso 1 1 calc R . . N4 N 0.6782(5) 0.2158(5) 0.5989(4) 0.0375(13) Uani 1 1 d . . . C34 C 0.7262(8) 0.1944(6) 0.6786(5) 0.0490(19) Uani 1 1 d . . . H34 H 0.7206 0.2221 0.7336 0.059 Uiso 1 1 calc R . . C35 C 0.7834(8) 0.1267(7) 0.6655(5) 0.052(2) Uani 1 1 d . . . H35 H 0.8259 0.1000 0.7095 0.063 Uiso 1 1 calc R . . C36 C 0.6108(7) -0.0326(6) 0.3797(5) 0.0441(17) Uani 1 1 d . . . H36A H 0.6059 -0.0328 0.4417 0.066 Uiso 1 1 calc R . . H36B H 0.5857 -0.1009 0.3525 0.066 Uiso 1 1 calc R . . H36C H 0.5574 0.0016 0.3509 0.066 Uiso 1 1 calc R . . C37 C 0.9233(7) 0.0800(5) 0.1906(4) 0.0403(16) Uani 1 1 d . . . H37A H 0.8636 0.0253 0.1512 0.060 Uiso 1 1 calc R . . H37B H 1.0036 0.0725 0.1951 0.060 Uiso 1 1 calc R . . H37C H 0.9244 0.1428 0.1677 0.060 Uiso 1 1 calc R . . C38 C 0.6685(6) 0.0007(5) 0.2064(4) 0.0360(15) Uani 1 1 d . . . H38A H 0.6752 -0.0607 0.1790 0.043 Uiso 1 1 calc R . . H38B H 0.5898 -0.0171 0.2260 0.043 Uiso 1 1 calc R . . C39 C 0.6644(5) 0.0699(5) 0.1364(4) 0.0305(13) Uani 1 1 d . . . C40 C 0.6638(6) 0.0377(5) 0.0488(4) 0.0342(14) Uani 1 1 d . . . C41 C 0.6583(6) 0.1035(5) -0.0125(4) 0.0309(13) Uani 1 1 d . . . Br2 Br 0.66397(7) 0.06200(6) -0.12995(5) 0.0466(2) Uani 1 1 d . . . C42 C 0.6500(6) 0.1967(5) 0.0053(4) 0.0351(14) Uani 1 1 d . . . C43 C 0.6530(5) 0.2289(5) 0.0928(4) 0.0310(13) Uani 1 1 d . . . C44 C 0.6567(5) 0.1639(5) 0.1564(4) 0.0302(13) Uani 1 1 d . . . C45 C 0.6653(7) -0.0650(5) 0.0214(5) 0.0426(17) Uani 1 1 d . . . H45A H 0.7462 -0.0614 0.0116 0.064 Uiso 1 1 calc R . . H45B H 0.6061 -0.0924 -0.0326 0.064 Uiso 1 1 calc R . . H45C H 0.6444 -0.1077 0.0675 0.064 Uiso 1 1 calc R . . C46 C 0.6377(9) 0.2601(6) -0.0687(5) 0.052(2) Uani 1 1 d . . . H46A H 0.7161 0.2868 -0.0865 0.078 Uiso 1 1 calc R . . H46B H 0.6112 0.3146 -0.0490 0.078 Uiso 1 1 calc R . . H46C H 0.5779 0.2196 -0.1183 0.078 Uiso 1 1 calc R . . C47 C 0.6456(7) 0.1941(5) 0.2482(5) 0.0394(15) Uani 1 1 d . . . H47A H 0.7265 0.2263 0.2833 0.059 Uiso 1 1 calc R . . H47B H 0.6042 0.1353 0.2744 0.059 Uiso 1 1 calc R . . H47C H 0.5989 0.2402 0.2462 0.059 Uiso 1 1 calc R . . C48 C 0.6445(6) 0.3306(5) 0.1161(5) 0.0362(15) Uani 1 1 d . . . H48A H 0.5649 0.3210 0.1330 0.043 Uiso 1 1 calc R . . H48B H 0.6440 0.3643 0.0623 0.043 Uiso 1 1 calc R . . O1 O 0.0000 0.0000 0.0000 0.0729(13) Uani 1 2 d S . . O2 O 0.9785(6) 0.3105(6) 0.9130(4) 0.0729(13) Uani 1 1 d . . . O3 O 0.8441(6) 0.8048(6) 0.2408(4) 0.0729(13) 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 Co1 0.0374(5) 0.0422(5) 0.0371(5) -0.0033(4) 0.0029(4) 0.0192(4) Cl1 0.0512(10) 0.0424(9) 0.0455(11) -0.0029(8) -0.0082(8) 0.0156(8) Cl2 0.0759(14) 0.0742(14) 0.0500(12) 0.0024(10) 0.0211(11) 0.0454(12) C1 0.034(3) 0.028(3) 0.034(4) 0.000(3) -0.001(3) 0.016(3) C2 0.033(3) 0.033(3) 0.044(4) -0.004(3) -0.003(3) 0.018(3) C3 0.040(3) 0.024(3) 0.037(4) -0.005(3) 0.002(3) 0.018(3) C4 0.030(3) 0.020(3) 0.035(4) 0.001(2) 0.002(3) 0.008(2) C5 0.028(3) 0.023(3) 0.031(3) -0.001(2) -0.001(2) 0.009(2) C6 0.035(3) 0.027(3) 0.031(3) -0.001(2) -0.001(3) 0.012(3) C7 0.040(4) 0.056(5) 0.064(6) -0.018(4) 0.000(4) 0.025(4) C8 0.041(4) 0.030(3) 0.044(4) -0.008(3) 0.003(3) 0.017(3) N1 0.030(3) 0.031(3) 0.047(4) -0.014(2) -0.004(2) 0.014(2) C9 0.044(4) 0.033(4) 0.048(4) -0.008(3) 0.006(3) 0.014(3) N2 0.039(3) 0.046(3) 0.041(4) -0.010(3) 0.002(3) 0.019(3) C10 0.032(3) 0.041(4) 0.052(5) -0.019(3) 0.000(3) 0.012(3) C11 0.026(3) 0.038(4) 0.054(5) -0.019(3) -0.002(3) 0.009(3) C12 0.044(4) 0.032(3) 0.039(4) -0.009(3) 0.002(3) 0.013(3) C13 0.041(4) 0.046(4) 0.026(3) -0.008(3) 0.001(3) 0.011(3) C14 0.032(3) 0.026(3) 0.037(4) 0.000(3) 0.003(3) 0.008(3) C15 0.026(3) 0.033(3) 0.032(3) -0.004(3) -0.001(3) 0.008(3) C16 0.032(3) 0.036(3) 0.038(4) -0.002(3) 0.003(3) 0.009(3) C17 0.023(3) 0.046(4) 0.035(4) -0.011(3) 0.002(3) 0.009(3) Br1 0.0406(4) 0.0693(5) 0.0426(5) -0.0117(4) 0.0066(3) 0.0191(4) C18 0.029(3) 0.038(4) 0.036(4) -0.011(3) -0.004(3) 0.014(3) C19 0.029(3) 0.034(3) 0.027(3) -0.005(3) -0.002(2) 0.010(3) C20 0.029(3) 0.028(3) 0.029(3) -0.006(2) -0.004(2) 0.010(3) C21 0.053(5) 0.048(4) 0.057(5) 0.013(4) 0.021(4) 0.015(4) C22 0.041(4) 0.053(5) 0.050(5) -0.008(4) 0.004(3) 0.024(4) C23 0.041(4) 0.032(3) 0.033(4) 0.002(3) 0.004(3) 0.018(3) C24 0.038(3) 0.038(4) 0.030(3) -0.002(3) -0.004(3) 0.018(3) C25 0.034(3) 0.019(3) 0.030(3) -0.002(2) -0.004(3) 0.013(3) C26 0.039(3) 0.022(3) 0.032(3) 0.001(2) -0.001(3) 0.017(3) C27 0.044(4) 0.021(3) 0.033(4) 0.003(2) 0.002(3) 0.017(3) C28 0.039(3) 0.026(3) 0.031(3) 0.000(2) 0.000(3) 0.010(3) C29 0.032(3) 0.024(3) 0.032(3) 0.001(2) 0.001(3) 0.008(3) C30 0.035(3) 0.024(3) 0.033(3) 0.001(2) 0.001(3) 0.010(3) C31 0.050(4) 0.034(3) 0.032(4) -0.006(3) -0.005(3) 0.019(3) C32 0.046(4) 0.032(3) 0.032(4) 0.004(3) 0.003(3) 0.019(3) N3 0.041(3) 0.039(3) 0.027(3) 0.004(2) 0.003(2) 0.021(3) C33 0.045(4) 0.047(4) 0.027(3) 0.002(3) 0.005(3) 0.026(3) N4 0.038(3) 0.047(3) 0.031(3) 0.001(2) 0.005(2) 0.020(3) C34 0.070(5) 0.060(5) 0.026(4) 0.007(3) 0.009(4) 0.034(4) C35 0.073(6) 0.065(5) 0.031(4) 0.011(4) 0.006(4) 0.041(5) C36 0.048(4) 0.043(4) 0.037(4) 0.007(3) 0.006(3) 0.008(3) C37 0.041(4) 0.043(4) 0.031(4) -0.008(3) 0.003(3) 0.010(3) C38 0.039(4) 0.030(3) 0.032(4) -0.001(3) -0.001(3) 0.007(3) C39 0.024(3) 0.033(3) 0.028(3) -0.001(2) -0.002(2) 0.004(3) C40 0.031(3) 0.032(3) 0.034(4) -0.011(3) -0.004(3) 0.010(3) C41 0.033(3) 0.037(3) 0.018(3) -0.006(2) -0.005(2) 0.011(3) Br2 0.0562(5) 0.0554(5) 0.0268(4) -0.0085(3) -0.0003(3) 0.0219(4) C42 0.036(3) 0.035(3) 0.026(3) -0.001(3) -0.004(3) 0.006(3) C43 0.028(3) 0.032(3) 0.031(3) -0.005(3) 0.000(3) 0.012(3) C44 0.028(3) 0.032(3) 0.024(3) -0.006(2) -0.002(2) 0.007(3) C45 0.057(4) 0.032(3) 0.036(4) -0.009(3) -0.005(3) 0.017(3) C46 0.078(6) 0.045(4) 0.031(4) 0.005(3) -0.002(4) 0.024(4) C47 0.043(4) 0.040(4) 0.035(4) -0.003(3) 0.007(3) 0.014(3) C48 0.035(3) 0.034(3) 0.039(4) -0.005(3) -0.003(3) 0.016(3) O1 0.076(3) 0.132(4) 0.0319(19) 0.011(2) 0.0215(19) 0.058(3) O2 0.076(3) 0.132(4) 0.0319(19) 0.011(2) 0.0215(19) 0.058(3) O3 0.076(3) 0.132(4) 0.0319(19) 0.011(2) 0.0215(19) 0.058(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N4 2.001(6) . ? Co1 N2 2.006(7) . ? Co1 Cl2 2.238(2) . ? Co1 Cl1 2.256(2) . ? C1 C6 1.397(9) . ? C1 C2 1.408(9) . ? C1 C48 1.527(9) . ? C2 C3 1.393(9) . ? C2 C7 1.524(10) . ? C3 C4 1.403(9) . ? C3 C8 1.493(9) . ? C4 C5 1.413(9) . ? C4 C12 1.516(9) . ? C5 C6 1.408(9) . ? C5 C14 1.531(9) . ? C6 C13 1.511(9) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 N1 1.484(10) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? N1 C9 1.338(9) . ? N1 C11 1.371(9) . ? C9 N2 1.319(10) . ? C9 H9 0.9500 . ? N2 C10 1.377(9) . ? C10 C11 1.356(12) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.516(9) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C20 1.399(9) . ? C15 C16 1.423(10) . ? C16 C17 1.383(10) . ? C16 C21 1.511(10) . ? C17 C18 1.390(10) . ? C17 Br1 1.929(7) . ? C18 C19 1.406(9) . ? C18 C22 1.508(10) . ? C19 C20 1.413(9) . ? C19 C24 1.520(9) . ? C20 C23 1.511(9) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.527(9) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.396(9) . ? C25 C30 1.410(8) . ? C26 C27 1.394(9) . ? C26 C31 1.524(9) . ? C27 C28 1.395(9) . ? C27 C32 1.523(9) . ? C28 C29 1.401(9) . ? C28 C36 1.519(10) . ? C29 C30 1.409(9) . ? C29 C38 1.535(9) . ? C30 C37 1.496(9) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 N3 1.475(8) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? N3 C33 1.330(8) . ? N3 C35 1.362(9) . ? C33 N4 1.327(9) . ? C33 H33 0.9500 . ? N4 C34 1.371(9) . ? C34 C35 1.365(11) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C39 1.517(9) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C44 1.398(9) . ? C39 C40 1.421(9) . ? C40 C41 1.383(9) . ? C40 C45 1.516(9) . ? C41 C42 1.385(9) . ? C41 Br2 1.919(6) . ? C42 C43 1.412(9) . ? C42 C46 1.521(10) . ? C43 C44 1.399(9) . ? C43 C48 1.519(9) . ? C44 C47 1.517(9) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Co1 N2 113.2(2) . . ? N4 Co1 Cl2 106.01(18) . . ? N2 Co1 Cl2 106.28(19) . . ? N4 Co1 Cl1 103.14(18) . . ? N2 Co1 Cl1 104.60(18) . . ? Cl2 Co1 Cl1 123.83(9) . . ? C6 C1 C2 119.9(6) . . ? C6 C1 C48 120.1(6) . . ? C2 C1 C48 119.8(6) . . ? C3 C2 C1 119.4(6) . . ? C3 C2 C7 120.2(6) . . ? C1 C2 C7 120.4(6) . . ? C2 C3 C4 121.1(6) . . ? C2 C3 C8 119.7(6) . . ? C4 C3 C8 119.2(6) . . ? C3 C4 C5 119.1(6) . . ? C3 C4 C12 120.1(6) . . ? C5 C4 C12 120.8(6) . . ? C6 C5 C4 119.5(6) . . ? C6 C5 C14 119.9(6) . . ? C4 C5 C14 120.5(5) . . ? C1 C6 C5 120.2(6) . . ? C1 C6 C13 120.5(6) . . ? C5 C6 C13 119.1(6) . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 C3 114.4(5) . . ? N1 C8 H8A 108.7 . . ? C3 C8 H8A 108.7 . . ? N1 C8 H8B 108.7 . . ? C3 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? C9 N1 C11 107.1(6) . . ? C9 N1 C8 127.2(6) . . ? C11 N1 C8 125.7(6) . . ? N2 C9 N1 111.7(6) . . ? N2 C9 H9 124.2 . . ? N1 C9 H9 124.2 . . ? C9 N2 C10 105.5(7) . . ? C9 N2 Co1 125.7(5) . . ? C10 N2 Co1 126.6(5) . . ? C11 C10 N2 109.3(7) . . ? C11 C10 H10 125.3 . . ? N2 C10 H10 125.3 . . ? C10 C11 N1 106.4(6) . . ? C10 C11 H11 126.8 . . ? N1 C11 H11 126.8 . . ? C4 C12 H12A 109.5 . . ? C4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C6 C13 H13A 109.5 . . ? C6 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C6 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C5 118.5(5) . . ? C15 C14 H14A 107.7 . . ? C5 C14 H14A 107.7 . . ? C15 C14 H14B 107.7 . . ? C5 C14 H14B 107.7 . . ? H14A C14 H14B 107.1 . . ? C20 C15 C16 119.6(6) . . ? C20 C15 C14 120.8(6) . . ? C16 C15 C14 119.7(6) . . ? C17 C16 C15 117.1(6) . . ? C17 C16 C21 121.7(7) . . ? C15 C16 C21 121.2(7) . . ? C16 C17 C18 125.3(6) . . ? C16 C17 Br1 117.3(6) . . ? C18 C17 Br1 117.4(5) . . ? C17 C18 C19 116.7(6) . . ? C17 C18 C22 120.4(6) . . ? C19 C18 C22 122.9(7) . . ? C18 C19 C20 120.3(6) . . ? C18 C19 C24 119.1(6) . . ? C20 C19 C24 120.6(6) . . ? C15 C20 C19 120.9(6) . . ? C15 C20 C23 119.7(6) . . ? C19 C20 C23 119.2(6) . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C18 C22 H22A 109.5 . . ? C18 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C18 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C19 C24 C25 119.8(5) . . ? C19 C24 H24A 107.4 . . ? C25 C24 H24A 107.4 . . ? C19 C24 H24B 107.4 . . ? C25 C24 H24B 107.4 . . ? H24A C24 H24B 106.9 . . ? C26 C25 C30 119.7(6) . . ? C26 C25 C24 121.3(5) . . ? C30 C25 C24 118.9(6) . . ? C27 C26 C25 119.2(6) . . ? C27 C26 C31 119.0(6) . . ? C25 C26 C31 121.8(6) . . ? C26 C27 C28 122.1(6) . . ? C26 C27 C32 118.7(6) . . ? C28 C27 C32 119.2(6) . . ? C27 C28 C29 118.4(6) . . ? C27 C28 C36 121.4(6) . . ? C29 C28 C36 120.2(6) . . ? C28 C29 C30 120.2(6) . . ? C28 C29 C38 119.8(6) . . ? C30 C29 C38 119.9(6) . . ? C29 C30 C25 119.8(6) . . ? C29 C30 C37 120.2(6) . . ? C25 C30 C37 119.9(6) . . ? C26 C31 H31A 109.5 . . ? C26 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C26 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N3 C32 C27 113.3(5) . . ? N3 C32 H32A 108.9 . . ? C27 C32 H32A 108.9 . . ? N3 C32 H32B 108.9 . . ? C27 C32 H32B 108.9 . . ? H32A C32 H32B 107.7 . . ? C33 N3 C35 106.4(6) . . ? C33 N3 C32 126.8(6) . . ? C35 N3 C32 126.6(6) . . ? N4 C33 N3 112.4(6) . . ? N4 C33 H33 123.8 . . ? N3 C33 H33 123.8 . . ? C33 N4 C34 105.3(6) . . ? C33 N4 Co1 124.9(5) . . ? C34 N4 Co1 129.0(5) . . ? C35 C34 N4 108.6(7) . . ? C35 C34 H34 125.7 . . ? N4 C34 H34 125.7 . . ? N3 C35 C34 107.3(6) . . ? N3 C35 H35 126.3 . . ? C34 C35 H35 126.3 . . ? C28 C36 H36A 109.5 . . ? C28 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C28 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C30 C37 H37A 109.5 . . ? C30 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C30 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C39 C38 C29 118.5(5) . . ? C39 C38 H38A 107.7 . . ? C29 C38 H38A 107.7 . . ? C39 C38 H38B 107.7 . . ? C29 C38 H38B 107.7 . . ? H38A C38 H38B 107.1 . . ? C44 C39 C40 119.5(6) . . ? C44 C39 C38 120.7(6) . . ? C40 C39 C38 119.8(6) . . ? C41 C40 C39 117.2(6) . . ? C41 C40 C45 120.3(6) . . ? C39 C40 C45 122.5(6) . . ? C40 C41 C42 124.5(6) . . ? C40 C41 Br2 117.2(5) . . ? C42 C41 Br2 118.3(5) . . ? C41 C42 C43 117.9(6) . . ? C41 C42 C46 119.5(6) . . ? C43 C42 C46 122.6(6) . . ? C44 C43 C42 119.1(6) . . ? C44 C43 C48 120.7(6) . . ? C42 C43 C48 120.1(6) . . ? C39 C44 C43 121.6(6) . . ? C39 C44 C47 119.2(6) . . ? C43 C44 C47 119.1(6) . . ? C40 C45 H45A 109.5 . . ? C40 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C40 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C42 C46 H46A 109.5 . . ? C42 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C42 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C44 C47 H47A 109.5 . . ? C44 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C44 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C43 C48 C1 119.4(5) . . ? C43 C48 H48A 107.5 . . ? C1 C48 H48A 107.5 . . ? C43 C48 H48B 107.5 . . ? C1 C48 H48B 107.5 . . ? H48A C48 H48B 107.0 . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 1.139 _refine_diff_density_min -0.652 _refine_diff_density_rms 0.171 # Attachment '7_CuCl2.cif' data_e1434a _database_code_depnum_ccdc_archive 'CCDC 744815' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H54 Br4 Cu N4, C H Cl3' _chemical_formula_sum 'C49 H55 Br4 Cl3 Cu N4' _chemical_formula_weight 1189.50 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.4322(3) _cell_length_b 14.6136(3) _cell_length_c 15.3801(4) _cell_angle_alpha 91.8790(10) _cell_angle_beta 93.1620(10) _cell_angle_gamma 109.7170(10) _cell_volume 2411.54(10) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7145 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 21.09 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.638 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1194 _exptl_absorpt_coefficient_mu 3.972 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5516 _exptl_absorpt_correction_T_max 0.7163 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 35032 _diffrn_reflns_av_R_equivalents 0.0453 _diffrn_reflns_av_sigmaI/netI 0.0644 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 27.55 _reflns_number_total 11055 _reflns_number_gt 7834 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0475P)^2^+7.0438P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11055 _refine_ls_number_parameters 556 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0868 _refine_ls_R_factor_gt 0.0539 _refine_ls_wR_factor_ref 0.1300 _refine_ls_wR_factor_gt 0.1131 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.59099(6) 0.30418(4) 0.57364(4) 0.02630(15) Uani 1 1 d . . . Br1 Br 0.48030(5) 0.22471(3) 0.43879(3) 0.02925(13) Uani 1 1 d . . . Br2 Br 0.53119(6) 0.33600(4) 0.71360(4) 0.04147(16) Uani 1 1 d . . . C1 C 0.7590(5) 0.4000(3) 0.1796(3) 0.0230(10) Uani 1 1 d . . . C2 C 0.7175(4) 0.4548(3) 0.2397(3) 0.0236(10) Uani 1 1 d . . . C3 C 0.8057(5) 0.5240(3) 0.2966(3) 0.0253(10) Uani 1 1 d . . . C4 C 0.9321(5) 0.5337(3) 0.2997(3) 0.0273(11) Uani 1 1 d . . . C5 C 0.9734(4) 0.4821(3) 0.2363(3) 0.0253(10) Uani 1 1 d . . . C6 C 0.8874(5) 0.4190(3) 0.1734(3) 0.0260(11) Uani 1 1 d . . . C7 C 0.5813(5) 0.4410(4) 0.2415(4) 0.0329(12) Uani 1 1 d . . . H7A H 0.5375 0.3776 0.2645 0.049 Uiso 1 1 calc R . . H7B H 0.5467 0.4434 0.1822 0.049 Uiso 1 1 calc R . . H7C H 0.5708 0.4928 0.2789 0.049 Uiso 1 1 calc R . . C8 C 0.7640(5) 0.5905(3) 0.3548(3) 0.0282(11) Uani 1 1 d . . . H8A H 0.8359 0.6503 0.3711 0.034 Uiso 1 1 calc R . . H8B H 0.7000 0.6098 0.3218 0.034 Uiso 1 1 calc R . . N1 N 0.7120(4) 0.5455(3) 0.4351(3) 0.0252(9) Uani 1 1 d . . . C9 C 0.6903(5) 0.4533(3) 0.4549(3) 0.0295(11) Uani 1 1 d . . . H9 H 0.7066 0.4062 0.4182 0.035 Uiso 1 1 calc R . . N2 N 0.6437(4) 0.4356(3) 0.5313(3) 0.0277(9) Uani 1 1 d . . . C10 C 0.6327(5) 0.5211(4) 0.5621(3) 0.0297(11) Uani 1 1 d . . . H10 H 0.6011 0.5309 0.6162 0.036 Uiso 1 1 calc R . . C11 C 0.6738(4) 0.5891(3) 0.5033(3) 0.0282(11) Uani 1 1 d . . . H11 H 0.6759 0.6546 0.5080 0.034 Uiso 1 1 calc R . . C12 C 1.0223(5) 0.6020(4) 0.3695(4) 0.0389(14) Uani 1 1 d . . . H12A H 1.0646 0.6647 0.3449 0.058 Uiso 1 1 calc R . . H12B H 1.0841 0.5732 0.3899 0.058 Uiso 1 1 calc R . . H12C H 0.9760 0.6120 0.4186 0.058 Uiso 1 1 calc R . . C13 C 0.9301(5) 0.3760(4) 0.0956(3) 0.0306(11) Uani 1 1 d . . . H13A H 0.9469 0.3171 0.1119 0.046 Uiso 1 1 calc R . . H13B H 1.0063 0.4236 0.0766 0.046 Uiso 1 1 calc R . . H13C H 0.8648 0.3594 0.0479 0.046 Uiso 1 1 calc R . . C14 C 1.1133(5) 0.5009(3) 0.2312(4) 0.0302(12) Uani 1 1 d . . . H14A H 1.1418 0.5439 0.1825 0.036 Uiso 1 1 calc R . . H14B H 1.1567 0.5379 0.2855 0.036 Uiso 1 1 calc R . . C15 C 1.1570(4) 0.4142(3) 0.2185(3) 0.0268(11) Uani 1 1 d . . . C16 C 1.2297(5) 0.4102(3) 0.1486(3) 0.0284(11) Uani 1 1 d . . . C17 C 1.2689(4) 0.3302(3) 0.1415(3) 0.0252(10) Uani 1 1 d . . . Br3 Br 1.35366(5) 0.31738(4) 0.03888(3) 0.03453(14) Uani 1 1 d . . . C18 C 1.2464(4) 0.2569(3) 0.2000(3) 0.0233(10) Uani 1 1 d . . . C19 C 1.1715(4) 0.2617(3) 0.2686(3) 0.0225(10) Uani 1 1 d . . . C20 C 1.1292(4) 0.3408(3) 0.2785(3) 0.0236(10) Uani 1 1 d . . . C21 C 1.2685(6) 0.4901(4) 0.0850(4) 0.0454(15) Uani 1 1 d . . . H21A H 1.3464 0.4910 0.0608 0.068 Uiso 1 1 calc R . . H21B H 1.2810 0.5530 0.1153 0.068 Uiso 1 1 calc R . . H21C H 1.2033 0.4780 0.0376 0.068 Uiso 1 1 calc R . . C22 C 1.3033(5) 0.1777(3) 0.1936(3) 0.0300(11) Uani 1 1 d . . . H22A H 1.3664 0.1939 0.1506 0.045 Uiso 1 1 calc R . . H22B H 1.2381 0.1156 0.1754 0.045 Uiso 1 1 calc R . . H22C H 1.3423 0.1722 0.2506 0.045 Uiso 1 1 calc R . . C23 C 1.0561(5) 0.3489(4) 0.3558(3) 0.0297(11) Uani 1 1 d . . . H23A H 0.9668 0.3239 0.3382 0.045 Uiso 1 1 calc R . . H23B H 1.0802 0.4173 0.3765 0.045 Uiso 1 1 calc R . . H23C H 1.0740 0.3108 0.4027 0.045 Uiso 1 1 calc R . . C24 C 1.1408(4) 0.1811(3) 0.3329(3) 0.0254(10) Uani 1 1 d . . . H24A H 1.1864 0.2093 0.3894 0.031 Uiso 1 1 calc R . . H24B H 1.1750 0.1312 0.3119 0.031 Uiso 1 1 calc R . . C25 C 1.0044(4) 0.1289(3) 0.3502(3) 0.0198(9) Uani 1 1 d . . . C26 C 0.9679(4) 0.1133(3) 0.4360(3) 0.0209(10) Uani 1 1 d . . . C27 C 0.8439(5) 0.0566(3) 0.4495(3) 0.0233(10) Uani 1 1 d . . . C28 C 0.7542(4) 0.0236(3) 0.3802(3) 0.0227(10) Uani 1 1 d . . . C29 C 0.7890(4) 0.0427(3) 0.2943(3) 0.0222(10) Uani 1 1 d . . . C30 C 0.9150(4) 0.0901(3) 0.2794(3) 0.0214(10) Uani 1 1 d . . . C31 C 1.0585(5) 0.1566(4) 0.5149(3) 0.0291(11) Uani 1 1 d . . . H31A H 1.0933 0.1080 0.5360 0.044 Uiso 1 1 calc R . . H31B H 1.0145 0.1760 0.5611 0.044 Uiso 1 1 calc R . . H31C H 1.1260 0.2138 0.4982 0.044 Uiso 1 1 calc R . . C32 C 0.8108(5) 0.0299(3) 0.5418(3) 0.0242(10) Uani 1 1 d . . . H32A H 0.7480 -0.0363 0.5403 0.029 Uiso 1 1 calc R . . H32B H 0.8861 0.0292 0.5764 0.029 Uiso 1 1 calc R . . N3 N 0.7609(4) 0.0997(3) 0.5842(2) 0.0233(9) Uani 1 1 d . . . C33 C 0.7055(5) 0.1556(3) 0.5455(3) 0.0246(10) Uani 1 1 d . . . H33 H 0.6963 0.1596 0.4842 0.030 Uiso 1 1 calc R . . N4 N 0.6646(4) 0.2049(3) 0.6030(3) 0.0261(9) Uani 1 1 d . . . C34 C 0.6961(5) 0.1785(4) 0.6834(3) 0.0336(12) Uani 1 1 d . . . H34 H 0.6798 0.2024 0.7379 0.040 Uiso 1 1 calc R . . C35 C 0.7542(5) 0.1126(4) 0.6720(3) 0.0328(12) Uani 1 1 d . . . H35 H 0.7846 0.0812 0.7165 0.039 Uiso 1 1 calc R . . C36 C 0.6201(5) -0.0332(4) 0.3957(3) 0.0327(12) Uani 1 1 d . . . H36A H 0.6125 -0.0433 0.4581 0.049 Uiso 1 1 calc R . . H36B H 0.5943 -0.0964 0.3632 0.049 Uiso 1 1 calc R . . H36C H 0.5668 0.0034 0.3759 0.049 Uiso 1 1 calc R . . C37 C 0.9548(5) 0.0958(3) 0.1874(3) 0.0271(11) Uani 1 1 d . . . H37A H 0.8960 0.0420 0.1507 0.041 Uiso 1 1 calc R . . H37B H 1.0383 0.0911 0.1870 0.041 Uiso 1 1 calc R . . H37C H 0.9561 0.1579 0.1645 0.041 Uiso 1 1 calc R . . C38 C 0.6894(5) 0.0064(3) 0.2196(3) 0.0254(11) Uani 1 1 d . . . H38A H 0.6074 -0.0121 0.2450 0.030 Uiso 1 1 calc R . . H38B H 0.6969 -0.0540 0.1933 0.030 Uiso 1 1 calc R . . C39 C 0.6864(4) 0.0726(3) 0.1458(3) 0.0216(10) Uani 1 1 d . . . C40 C 0.6790(4) 0.0369(3) 0.0596(3) 0.0241(10) Uani 1 1 d . . . C41 C 0.6656(4) 0.0975(3) -0.0058(3) 0.0222(10) Uani 1 1 d . . . Br4 Br 0.64834(5) 0.04711(4) -0.12456(3) 0.03292(14) Uani 1 1 d . . . C42 C 0.6608(5) 0.1905(3) 0.0092(3) 0.0258(10) Uani 1 1 d . . . C43 C 0.6717(4) 0.2258(3) 0.0963(3) 0.0229(10) Uani 1 1 d . . . C44 C 0.6791(4) 0.1651(3) 0.1638(3) 0.0215(10) Uani 1 1 d . . . C45 C 0.6843(5) -0.0626(3) 0.0351(3) 0.0323(12) Uani 1 1 d . . . H45A H 0.7529 -0.0558 -0.0025 0.048 Uiso 1 1 calc R . . H45B H 0.6055 -0.1024 0.0039 0.048 Uiso 1 1 calc R . . H45C H 0.6979 -0.0942 0.0881 0.048 Uiso 1 1 calc R . . C46 C 0.6422(6) 0.2481(4) -0.0664(3) 0.0383(14) Uani 1 1 d . . . H46A H 0.7212 0.2763 -0.0935 0.057 Uiso 1 1 calc R . . H46B H 0.6136 0.3005 -0.0455 0.057 Uiso 1 1 calc R . . H46C H 0.5797 0.2052 -0.1094 0.057 Uiso 1 1 calc R . . C47 C 0.6724(5) 0.1987(4) 0.2572(3) 0.0298(11) Uani 1 1 d . . . H47A H 0.7568 0.2324 0.2835 0.045 Uiso 1 1 calc R . . H47B H 0.6313 0.1421 0.2907 0.045 Uiso 1 1 calc R . . H47C H 0.6247 0.2432 0.2579 0.045 Uiso 1 1 calc R . . C48 C 0.6630(5) 0.3266(3) 0.1163(3) 0.0259(11) Uani 1 1 d . . . H48A H 0.6640 0.3579 0.0601 0.031 Uiso 1 1 calc R . . H48B H 0.5802 0.3164 0.1386 0.031 Uiso 1 1 calc R . . C49 C 0.9212(9) 0.7825(6) 0.1190(5) 0.081(3) Uani 1 1 d . . . H49 H 0.8344 0.7507 0.0924 0.097 Uiso 1 1 calc R . . Cl1 Cl 0.9838(3) 0.6917(2) 0.12993(16) 0.108 Uani 1 1 d . . . Cl2 Cl 0.9085(3) 0.8354(2) 0.21696(16) 0.1070(9) Uani 1 1 d . . . Cl3 Cl 0.9990(2) 0.86689(19) 0.04660(17) 0.0948(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 Cu1 0.0305(4) 0.0288(3) 0.0229(3) -0.0003(2) 0.0003(3) 0.0149(3) Br1 0.0337(3) 0.0300(2) 0.0249(3) 0.00014(19) -0.0035(2) 0.0129(2) Br2 0.0563(4) 0.0540(3) 0.0274(3) 0.0008(2) 0.0075(3) 0.0357(3) C1 0.026(3) 0.020(2) 0.025(3) 0.0025(18) -0.002(2) 0.0118(19) C2 0.023(3) 0.021(2) 0.028(3) 0.0037(18) 0.000(2) 0.0106(19) C3 0.026(3) 0.020(2) 0.029(3) 0.0007(18) 0.003(2) 0.0072(19) C4 0.028(3) 0.021(2) 0.031(3) -0.0013(19) 0.001(2) 0.006(2) C5 0.023(3) 0.019(2) 0.036(3) 0.0051(19) 0.005(2) 0.0079(19) C6 0.032(3) 0.019(2) 0.029(3) 0.0014(18) 0.004(2) 0.010(2) C7 0.026(3) 0.030(3) 0.041(3) -0.008(2) -0.002(2) 0.010(2) C8 0.031(3) 0.020(2) 0.034(3) -0.0012(19) 0.003(2) 0.009(2) N1 0.024(2) 0.0224(19) 0.031(2) -0.0035(16) -0.0033(18) 0.0118(17) C9 0.035(3) 0.021(2) 0.036(3) -0.003(2) 0.003(2) 0.014(2) N2 0.029(2) 0.029(2) 0.028(2) -0.0007(17) 0.0010(19) 0.0142(18) C10 0.027(3) 0.033(3) 0.028(3) -0.012(2) 0.000(2) 0.010(2) C11 0.023(3) 0.025(2) 0.037(3) -0.013(2) 0.000(2) 0.010(2) C12 0.033(3) 0.030(3) 0.050(4) -0.013(2) -0.007(3) 0.009(2) C13 0.027(3) 0.033(3) 0.032(3) -0.003(2) 0.004(2) 0.012(2) C14 0.023(3) 0.021(2) 0.046(3) 0.000(2) 0.003(2) 0.007(2) C15 0.016(2) 0.021(2) 0.040(3) 0.000(2) 0.000(2) 0.0024(18) C16 0.025(3) 0.022(2) 0.035(3) 0.004(2) 0.006(2) 0.0037(19) C17 0.016(2) 0.031(2) 0.028(3) -0.003(2) 0.002(2) 0.0069(19) Br3 0.0313(3) 0.0448(3) 0.0297(3) 0.0020(2) 0.0055(2) 0.0154(2) C18 0.017(2) 0.023(2) 0.028(3) -0.0017(19) -0.001(2) 0.0058(18) C19 0.013(2) 0.025(2) 0.026(3) -0.0033(18) -0.0039(19) 0.0035(18) C20 0.015(2) 0.022(2) 0.030(3) -0.0045(19) -0.003(2) 0.0026(18) C21 0.044(4) 0.033(3) 0.066(4) 0.019(3) 0.020(3) 0.017(3) C22 0.032(3) 0.027(2) 0.034(3) -0.001(2) 0.004(2) 0.015(2) C23 0.029(3) 0.029(2) 0.034(3) -0.001(2) 0.005(2) 0.015(2) C24 0.025(3) 0.026(2) 0.027(3) -0.0027(19) -0.003(2) 0.011(2) C25 0.020(2) 0.019(2) 0.022(2) -0.0024(17) -0.0018(19) 0.0095(18) C26 0.025(3) 0.020(2) 0.021(2) -0.0007(17) -0.0017(19) 0.0127(19) C27 0.031(3) 0.020(2) 0.023(2) 0.0028(18) 0.003(2) 0.0124(19) C28 0.026(3) 0.019(2) 0.022(2) 0.0032(17) 0.002(2) 0.0074(19) C29 0.028(3) 0.015(2) 0.023(2) 0.0006(17) 0.000(2) 0.0066(18) C30 0.026(3) 0.0157(19) 0.022(2) 0.0033(17) 0.0034(19) 0.0072(18) C31 0.032(3) 0.033(3) 0.024(3) -0.002(2) -0.002(2) 0.013(2) C32 0.030(3) 0.025(2) 0.021(2) 0.0050(18) 0.004(2) 0.015(2) N3 0.026(2) 0.032(2) 0.016(2) 0.0049(16) 0.0028(16) 0.0143(17) C33 0.034(3) 0.025(2) 0.019(2) 0.0035(18) 0.002(2) 0.015(2) N4 0.028(2) 0.032(2) 0.021(2) 0.0046(17) 0.0005(17) 0.0145(18) C34 0.044(3) 0.045(3) 0.019(3) 0.001(2) 0.002(2) 0.023(3) C35 0.044(3) 0.048(3) 0.015(2) 0.008(2) 0.001(2) 0.026(3) C36 0.031(3) 0.031(3) 0.030(3) 0.010(2) -0.001(2) 0.003(2) C37 0.025(3) 0.029(2) 0.024(3) -0.0022(19) 0.003(2) 0.005(2) C38 0.028(3) 0.023(2) 0.020(2) 0.0017(18) -0.004(2) 0.0024(19) C39 0.020(2) 0.024(2) 0.021(2) -0.0008(18) -0.0006(19) 0.0074(18) C40 0.022(3) 0.023(2) 0.026(3) -0.0002(19) 0.000(2) 0.0074(19) C41 0.026(3) 0.025(2) 0.014(2) -0.0009(17) -0.0010(19) 0.0071(19) Br4 0.0458(3) 0.0359(3) 0.0187(3) -0.00382(19) -0.0013(2) 0.0170(2) C42 0.028(3) 0.026(2) 0.024(3) 0.0022(19) 0.002(2) 0.009(2) C43 0.020(3) 0.024(2) 0.024(3) -0.0014(18) 0.001(2) 0.0064(19) C44 0.018(2) 0.025(2) 0.019(2) -0.0043(18) -0.0018(19) 0.0046(18) C45 0.048(3) 0.025(2) 0.024(3) -0.0014(19) -0.003(2) 0.013(2) C46 0.067(4) 0.031(3) 0.022(3) 0.004(2) 0.006(3) 0.022(3) C47 0.040(3) 0.030(2) 0.022(3) -0.003(2) 0.002(2) 0.015(2) C48 0.027(3) 0.025(2) 0.028(3) -0.0063(19) -0.005(2) 0.014(2) C49 0.098(7) 0.088(6) 0.060(5) 0.019(4) -0.010(5) 0.036(5) Cl1 0.150 0.139 0.070 0.017 0.018 0.092 Cl2 0.150(3) 0.135(2) 0.0696(15) 0.0157(14) 0.0207(15) 0.089(2) Cl3 0.0839(16) 0.1071(18) 0.1016(18) 0.0469(14) 0.0354(14) 0.0349(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N2 1.954(4) . ? Cu1 N4 1.961(4) . ? Cu1 Br2 2.3724(8) . ? Cu1 Br1 2.4108(8) . ? C1 C2 1.407(7) . ? C1 C6 1.408(7) . ? C1 C48 1.524(6) . ? C2 C3 1.401(6) . ? C2 C7 1.503(7) . ? C3 C4 1.402(7) . ? C3 C8 1.508(7) . ? C4 C5 1.408(7) . ? C4 C12 1.525(7) . ? C5 C6 1.406(7) . ? C5 C14 1.535(7) . ? C6 C13 1.512(7) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 N1 1.477(6) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? N1 C9 1.333(6) . ? N1 C11 1.375(6) . ? C9 N2 1.313(6) . ? C9 H9 0.9500 . ? N2 C10 1.370(6) . ? C10 C11 1.348(7) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.522(6) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C20 1.404(7) . ? C15 C16 1.406(7) . ? C16 C17 1.390(7) . ? C16 C21 1.513(7) . ? C17 C18 1.387(7) . ? C17 Br3 1.932(5) . ? C18 C19 1.410(7) . ? C18 C22 1.510(6) . ? C19 C20 1.402(6) . ? C19 C24 1.525(6) . ? C20 C23 1.514(7) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.530(6) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.407(6) . ? C25 C30 1.413(6) . ? C26 C27 1.411(7) . ? C26 C31 1.521(6) . ? C27 C28 1.390(7) . ? C27 C32 1.518(6) . ? C28 C29 1.410(6) . ? C28 C36 1.513(7) . ? C29 C30 1.407(6) . ? C29 C38 1.520(6) . ? C30 C37 1.508(6) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 N3 1.476(6) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? N3 C33 1.327(6) . ? N3 C35 1.366(6) . ? C33 N4 1.323(6) . ? C33 H33 0.9500 . ? N4 C34 1.372(6) . ? C34 C35 1.354(7) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C39 1.522(6) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.397(6) . ? C39 C44 1.402(6) . ? C40 C41 1.397(6) . ? C40 C45 1.511(6) . ? C41 C42 1.391(6) . ? C41 Br4 1.921(4) . ? C42 C43 1.405(7) . ? C42 C46 1.504(7) . ? C43 C44 1.404(6) . ? C43 C48 1.532(6) . ? C44 C47 1.517(6) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 Cl2 1.707(9) . ? C49 Cl1 1.715(9) . ? C49 Cl3 1.735(8) . ? C49 H49 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 Cu1 N4 138.45(17) . . ? N2 Cu1 Br2 99.88(12) . . ? N4 Cu1 Br2 99.04(12) . . ? N2 Cu1 Br1 95.56(12) . . ? N4 Cu1 Br1 96.81(12) . . ? Br2 Cu1 Br1 134.70(3) . . ? C2 C1 C6 120.2(4) . . ? C2 C1 C48 118.5(4) . . ? C6 C1 C48 121.0(4) . . ? C3 C2 C1 118.8(4) . . ? C3 C2 C7 120.6(4) . . ? C1 C2 C7 120.6(4) . . ? C2 C3 C4 121.3(4) . . ? C2 C3 C8 119.3(4) . . ? C4 C3 C8 119.4(4) . . ? C3 C4 C5 119.0(4) . . ? C3 C4 C12 119.4(4) . . ? C5 C4 C12 121.6(5) . . ? C6 C5 C4 120.0(5) . . ? C6 C5 C14 119.8(4) . . ? C4 C5 C14 120.0(4) . . ? C5 C6 C1 119.6(4) . . ? C5 C6 C13 121.3(5) . . ? C1 C6 C13 118.9(4) . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 C3 113.3(4) . . ? N1 C8 H8A 108.9 . . ? C3 C8 H8A 108.9 . . ? N1 C8 H8B 108.9 . . ? C3 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? C9 N1 C11 106.3(4) . . ? C9 N1 C8 126.5(4) . . ? C11 N1 C8 127.2(4) . . ? N2 C9 N1 112.0(4) . . ? N2 C9 H9 124.0 . . ? N1 C9 H9 124.0 . . ? C9 N2 C10 105.8(4) . . ? C9 N2 Cu1 121.1(3) . . ? C10 N2 Cu1 132.8(4) . . ? C11 C10 N2 109.0(4) . . ? C11 C10 H10 125.5 . . ? N2 C10 H10 125.5 . . ? C10 C11 N1 106.9(4) . . ? C10 C11 H11 126.6 . . ? N1 C11 H11 126.6 . . ? C4 C12 H12A 109.5 . . ? C4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C6 C13 H13A 109.5 . . ? C6 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C6 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C5 118.7(4) . . ? C15 C14 H14A 107.7 . . ? C5 C14 H14A 107.7 . . ? C15 C14 H14B 107.7 . . ? C5 C14 H14B 107.7 . . ? H14A C14 H14B 107.1 . . ? C20 C15 C16 120.3(4) . . ? C20 C15 C14 120.0(5) . . ? C16 C15 C14 119.6(4) . . ? C17 C16 C15 117.0(4) . . ? C17 C16 C21 120.5(5) . . ? C15 C16 C21 122.5(5) . . ? C18 C17 C16 125.0(5) . . ? C18 C17 Br3 117.9(4) . . ? C16 C17 Br3 117.0(4) . . ? C17 C18 C19 116.8(4) . . ? C17 C18 C22 122.2(4) . . ? C19 C18 C22 120.9(4) . . ? C20 C19 C18 120.3(4) . . ? C20 C19 C24 120.9(4) . . ? C18 C19 C24 118.7(4) . . ? C19 C20 C15 120.5(4) . . ? C19 C20 C23 120.0(4) . . ? C15 C20 C23 119.5(4) . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C18 C22 H22A 109.5 . . ? C18 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C18 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C19 C24 C25 118.8(4) . . ? C19 C24 H24A 107.6 . . ? C25 C24 H24A 107.6 . . ? C19 C24 H24B 107.6 . . ? C25 C24 H24B 107.6 . . ? H24A C24 H24B 107.0 . . ? C26 C25 C30 119.3(4) . . ? C26 C25 C24 120.9(4) . . ? C30 C25 C24 119.7(4) . . ? C25 C26 C27 119.4(4) . . ? C25 C26 C31 121.7(4) . . ? C27 C26 C31 118.9(4) . . ? C28 C27 C26 121.2(4) . . ? C28 C27 C32 120.4(4) . . ? C26 C27 C32 118.4(4) . . ? C27 C28 C29 119.5(4) . . ? C27 C28 C36 120.8(4) . . ? C29 C28 C36 119.7(4) . . ? C30 C29 C28 119.7(4) . . ? C30 C29 C38 121.6(4) . . ? C28 C29 C38 118.6(4) . . ? C29 C30 C25 120.4(4) . . ? C29 C30 C37 119.4(4) . . ? C25 C30 C37 120.1(4) . . ? C26 C31 H31A 109.5 . . ? C26 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C26 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N3 C32 C27 111.4(4) . . ? N3 C32 H32A 109.3 . . ? C27 C32 H32A 109.3 . . ? N3 C32 H32B 109.3 . . ? C27 C32 H32B 109.3 . . ? H32A C32 H32B 108.0 . . ? C33 N3 C35 106.9(4) . . ? C33 N3 C32 127.3(4) . . ? C35 N3 C32 125.6(4) . . ? N4 C33 N3 111.6(4) . . ? N4 C33 H33 124.2 . . ? N3 C33 H33 124.2 . . ? C33 N4 C34 105.8(4) . . ? C33 N4 Cu1 124.5(3) . . ? C34 N4 Cu1 129.3(3) . . ? C35 C34 N4 108.6(4) . . ? C35 C34 H34 125.7 . . ? N4 C34 H34 125.7 . . ? C34 C35 N3 107.1(4) . . ? C34 C35 H35 126.5 . . ? N3 C35 H35 126.5 . . ? C28 C36 H36A 109.5 . . ? C28 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C28 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C30 C37 H37A 109.5 . . ? C30 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C30 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C29 C38 C39 119.5(4) . . ? C29 C38 H38A 107.4 . . ? C39 C38 H38A 107.4 . . ? C29 C38 H38B 107.4 . . ? C39 C38 H38B 107.4 . . ? H38A C38 H38B 107.0 . . ? C40 C39 C44 120.2(4) . . ? C40 C39 C38 119.2(4) . . ? C44 C39 C38 120.3(4) . . ? C39 C40 C41 117.0(4) . . ? C39 C40 C45 123.2(4) . . ? C41 C40 C45 119.8(4) . . ? C42 C41 C40 124.7(4) . . ? C42 C41 Br4 117.9(3) . . ? C40 C41 Br4 117.4(3) . . ? C41 C42 C43 117.2(4) . . ? C41 C42 C46 120.0(4) . . ? C43 C42 C46 122.7(4) . . ? C44 C43 C42 119.6(4) . . ? C44 C43 C48 120.9(4) . . ? C42 C43 C48 119.2(4) . . ? C39 C44 C43 121.1(4) . . ? C39 C44 C47 119.8(4) . . ? C43 C44 C47 119.1(4) . . ? C40 C45 H45A 109.5 . . ? C40 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C40 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C42 C46 H46A 109.5 . . ? C42 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C42 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C44 C47 H47A 109.5 . . ? C44 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C44 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C1 C48 C43 120.6(4) . . ? C1 C48 H48A 107.2 . . ? C43 C48 H48A 107.2 . . ? C1 C48 H48B 107.2 . . ? C43 C48 H48B 107.2 . . ? H48A C48 H48B 106.8 . . ? Cl2 C49 Cl1 112.5(4) . . ? Cl2 C49 Cl3 112.7(5) . . ? Cl1 C49 Cl3 111.8(5) . . ? Cl2 C49 H49 106.4 . . ? Cl1 C49 H49 106.4 . . ? Cl3 C49 H49 106.4 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.585 _refine_diff_density_min -1.991 _refine_diff_density_rms 0.119 # Attachment '7_HgCl2.cif' data_e1446a _database_code_depnum_ccdc_archive 'CCDC 744816' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H54 Br4 Hg N4, C H Cl3' _chemical_formula_sum 'C49 H55 Br4 Cl3 Hg N4' _chemical_formula_weight 1326.55 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' Br Br -0.2901 2.4595 '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' 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' Hg Hg -2.3894 9.2266 '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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.4429(6) _cell_length_b 14.9630(9) _cell_length_c 15.3162(11) _cell_angle_alpha 92.715(2) _cell_angle_beta 90.510(2) _cell_angle_gamma 110.905(2) _cell_volume 2446.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1607 _cell_measurement_theta_min 2.66 _cell_measurement_theta_max 23.41 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.801 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1296 _exptl_absorpt_coefficient_mu 6.615 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5575 _exptl_absorpt_correction_T_max 0.6197 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 45948 _diffrn_reflns_av_R_equivalents 0.0604 _diffrn_reflns_av_sigmaI/netI 0.0716 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 27.50 _reflns_number_total 11001 _reflns_number_gt 7573 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0696P)^2^+8.0620P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11001 _refine_ls_number_parameters 556 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0935 _refine_ls_R_factor_gt 0.0564 _refine_ls_wR_factor_ref 0.1576 _refine_ls_wR_factor_gt 0.1317 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.030 _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 Hg1 Hg 0.53822(3) 0.29239(2) 0.59277(2) 0.04185(12) Uani 1 1 d . . . Br1 Br 0.44966(8) 0.21847(6) 0.44038(5) 0.0421(2) Uani 1 1 d . . . Br2 Br 0.44914(10) 0.30068(8) 0.74065(6) 0.0599(3) Uani 1 1 d . . . C1 C 0.7736(7) 0.3989(5) 0.1836(5) 0.0289(15) Uani 1 1 d . . . C2 C 0.7333(6) 0.4521(5) 0.2472(5) 0.0289(15) Uani 1 1 d . . . C3 C 0.8196(7) 0.5183(5) 0.3054(5) 0.0333(16) Uani 1 1 d . . . C4 C 0.9461(7) 0.5280(5) 0.3052(5) 0.0344(17) Uani 1 1 d . . . C5 C 0.9878(7) 0.4783(5) 0.2386(5) 0.0331(16) Uani 1 1 d . . . C6 C 0.9026(7) 0.4181(5) 0.1764(5) 0.0338(17) Uani 1 1 d . . . C7 C 0.5942(7) 0.4387(6) 0.2522(6) 0.044(2) Uani 1 1 d . . . H7A H 0.5469 0.3742 0.2707 0.065 Uiso 1 1 calc R . . H7B H 0.5629 0.4468 0.1945 0.065 Uiso 1 1 calc R . . H7C H 0.5841 0.4864 0.2945 0.065 Uiso 1 1 calc R . . C8 C 0.7791(8) 0.5859(6) 0.3634(5) 0.0408(19) Uani 1 1 d . . . H8A H 0.8524 0.6449 0.3774 0.049 Uiso 1 1 calc R . . H8B H 0.7165 0.6041 0.3310 0.049 Uiso 1 1 calc R . . N1 N 0.7244(6) 0.5438(4) 0.4459(4) 0.0352(14) Uani 1 1 d . . . C9 C 0.7046(8) 0.4545(6) 0.4707(5) 0.0398(19) Uani 1 1 d . . . H9 H 0.7243 0.4071 0.4370 0.048 Uiso 1 1 calc R . . N2 N 0.6540(7) 0.4419(5) 0.5482(4) 0.0426(16) Uani 1 1 d . . . C10 C 0.6383(7) 0.5262(6) 0.5734(6) 0.0424(19) Uani 1 1 d . . . H10 H 0.6034 0.5382 0.6268 0.051 Uiso 1 1 calc R . . C11 C 0.6807(7) 0.5896(6) 0.5099(5) 0.041(2) Uani 1 1 d . . . H11 H 0.6800 0.6529 0.5100 0.049 Uiso 1 1 calc R . . C12 C 1.0333(8) 0.5924(6) 0.3765(6) 0.048(2) Uani 1 1 d . . . H12A H 1.0703 0.6576 0.3566 0.072 Uiso 1 1 calc R . . H12B H 1.1000 0.5679 0.3897 0.072 Uiso 1 1 calc R . . H12C H 0.9859 0.5932 0.4294 0.072 Uiso 1 1 calc R . . C13 C 0.9468(7) 0.3775(6) 0.0963(5) 0.0398(19) Uani 1 1 d . . . H13A H 0.9519 0.3153 0.1087 0.060 Uiso 1 1 calc R . . H13B H 1.0297 0.4217 0.0811 0.060 Uiso 1 1 calc R . . H13C H 0.8876 0.3694 0.0474 0.060 Uiso 1 1 calc R . . C14 C 1.1276(7) 0.4983(6) 0.2310(6) 0.0406(19) Uani 1 1 d . . . H14A H 1.1698 0.5335 0.2856 0.049 Uiso 1 1 calc R . . H14B H 1.1585 0.5418 0.1828 0.049 Uiso 1 1 calc R . . C15 C 1.1703(7) 0.4126(6) 0.2147(5) 0.0370(18) Uani 1 1 d . . . C16 C 1.2485(7) 0.4124(5) 0.1446(6) 0.0386(18) Uani 1 1 d . . . C17 C 1.2852(7) 0.3327(6) 0.1332(5) 0.0348(17) Uani 1 1 d . . . Br3 Br 1.37742(7) 0.32492(7) 0.03023(5) 0.0441(2) Uani 1 1 d . . . C18 C 1.2551(7) 0.2588(5) 0.1896(5) 0.0325(16) Uani 1 1 d . . . C19 C 1.1768(6) 0.2607(5) 0.2600(5) 0.0293(15) Uani 1 1 d . . . C20 C 1.1357(7) 0.3382(5) 0.2726(5) 0.0315(16) Uani 1 1 d . . . C21 C 1.2955(9) 0.4938(7) 0.0848(7) 0.059(3) Uani 1 1 d . . . H21A H 1.3832 0.5052 0.0718 0.088 Uiso 1 1 calc R . . H21B H 1.2890 0.5518 0.1134 0.088 Uiso 1 1 calc R . . H21C H 1.2451 0.4775 0.0304 0.088 Uiso 1 1 calc R . . C22 C 1.3095(8) 0.1802(6) 0.1793(5) 0.0395(18) Uani 1 1 d . . . H22A H 1.3498 0.1751 0.2346 0.059 Uiso 1 1 calc R . . H22B H 1.3716 0.1956 0.1333 0.059 Uiso 1 1 calc R . . H22C H 1.2424 0.1191 0.1633 0.059 Uiso 1 1 calc R . . C23 C 1.0599(7) 0.3427(6) 0.3508(5) 0.0364(17) Uani 1 1 d . . . H23A H 1.0789 0.4098 0.3705 0.055 Uiso 1 1 calc R . . H23B H 1.0807 0.3084 0.3979 0.055 Uiso 1 1 calc R . . H23C H 0.9707 0.3129 0.3351 0.055 Uiso 1 1 calc R . . C24 C 1.1406(7) 0.1785(5) 0.3211(5) 0.0332(16) Uani 1 1 d . . . H24A H 1.1695 0.1285 0.2951 0.040 Uiso 1 1 calc R . . H24B H 1.1890 0.2027 0.3766 0.040 Uiso 1 1 calc R . . C25 C 1.0044(7) 0.1298(5) 0.3441(5) 0.0283(15) Uani 1 1 d . . . C26 C 0.9691(7) 0.1146(5) 0.4321(5) 0.0308(16) Uani 1 1 d . . . C27 C 0.8438(7) 0.0615(5) 0.4494(4) 0.0302(16) Uani 1 1 d . . . C28 C 0.7524(7) 0.0324(5) 0.3845(5) 0.0302(15) Uani 1 1 d . . . C29 C 0.7861(7) 0.0497(5) 0.2972(5) 0.0282(15) Uani 1 1 d . . . C30 C 0.9131(7) 0.0935(5) 0.2762(4) 0.0280(15) Uani 1 1 d . . . C31 C 1.0638(8) 0.1539(6) 0.5069(5) 0.0395(18) Uani 1 1 d . . . H31A H 1.0330 0.1910 0.5491 0.059 Uiso 1 1 calc R . . H31B H 1.1436 0.1953 0.4843 0.059 Uiso 1 1 calc R . . H31C H 1.0760 0.1007 0.5358 0.059 Uiso 1 1 calc R . . C32 C 0.8108(7) 0.0391(5) 0.5428(5) 0.0328(16) Uani 1 1 d . . . H32A H 0.7442 -0.0250 0.5437 0.039 Uiso 1 1 calc R . . H32B H 0.8852 0.0363 0.5744 0.039 Uiso 1 1 calc R . . N3 N 0.7676(6) 0.1101(4) 0.5895(4) 0.0326(14) Uani 1 1 d . . . C33 C 0.7134(7) 0.1652(6) 0.5535(5) 0.0348(17) Uani 1 1 d . . . H33 H 0.7027 0.1686 0.4924 0.042 Uiso 1 1 calc R . . N4 N 0.6765(6) 0.2146(5) 0.6140(4) 0.0370(15) Uani 1 1 d . . . C34 C 0.7065(8) 0.1878(7) 0.6920(5) 0.047(2) Uani 1 1 d . . . H34 H 0.6900 0.2106 0.7477 0.057 Uiso 1 1 calc R . . C35 C 0.7641(9) 0.1231(7) 0.6775(5) 0.047(2) Uani 1 1 d . . . H35 H 0.7955 0.0932 0.7205 0.056 Uiso 1 1 calc R . . C36 C 0.6165(7) -0.0188(6) 0.4045(5) 0.0407(19) Uani 1 1 d . . . H36A H 0.6082 -0.0273 0.4674 0.061 Uiso 1 1 calc R . . H36B H 0.5855 -0.0815 0.3727 0.061 Uiso 1 1 calc R . . H36C H 0.5674 0.0194 0.3862 0.061 Uiso 1 1 calc R . . C37 C 0.9520(7) 0.0980(6) 0.1824(5) 0.0366(18) Uani 1 1 d . . . H37A H 0.8946 0.0424 0.1481 0.055 Uiso 1 1 calc R . . H37B H 1.0373 0.0975 0.1793 0.055 Uiso 1 1 calc R . . H37C H 0.9494 0.1570 0.1586 0.055 Uiso 1 1 calc R . . C38 C 0.6855(7) 0.0124(5) 0.2247(5) 0.0354(17) Uani 1 1 d . . . H38A H 0.6031 -0.0061 0.2525 0.043 Uiso 1 1 calc R . . H38B H 0.6923 -0.0470 0.1977 0.043 Uiso 1 1 calc R . . C39 C 0.6842(7) 0.0772(5) 0.1509(4) 0.0284(15) Uani 1 1 d . . . C40 C 0.6772(7) 0.0397(5) 0.0638(5) 0.0319(16) Uani 1 1 d . . . C41 C 0.6715(7) 0.0996(6) -0.0018(5) 0.0345(17) Uani 1 1 d . . . Br4 Br 0.65780(9) 0.05032(6) -0.12003(5) 0.0442(2) Uani 1 1 d . . . C42 C 0.6740(7) 0.1929(5) 0.0137(5) 0.0334(17) Uani 1 1 d . . . C43 C 0.6816(6) 0.2282(5) 0.1009(5) 0.0293(15) Uani 1 1 d . . . C44 C 0.6812(6) 0.1686(5) 0.1692(5) 0.0279(15) Uani 1 1 d . . . C45 C 0.6714(9) -0.0606(6) 0.0408(5) 0.045(2) Uani 1 1 d . . . H45A H 0.6080 -0.0896 -0.0058 0.068 Uiso 1 1 calc R . . H45B H 0.6491 -0.0988 0.0925 0.068 Uiso 1 1 calc R . . H45C H 0.7532 -0.0589 0.0207 0.068 Uiso 1 1 calc R . . C46 C 0.6695(10) 0.2517(6) -0.0618(5) 0.050(2) Uani 1 1 d . . . H46A H 0.6192 0.2098 -0.1100 0.076 Uiso 1 1 calc R . . H46B H 0.7546 0.2852 -0.0813 0.076 Uiso 1 1 calc R . . H46C H 0.6317 0.2988 -0.0435 0.076 Uiso 1 1 calc R . . C47 C 0.6733(7) 0.2022(6) 0.2630(5) 0.0354(17) Uani 1 1 d . . . H47A H 0.7577 0.2385 0.2868 0.053 Uiso 1 1 calc R . . H47B H 0.6340 0.1465 0.2980 0.053 Uiso 1 1 calc R . . H47C H 0.6230 0.2432 0.2651 0.053 Uiso 1 1 calc R . . C48 C 0.6755(7) 0.3272(5) 0.1221(5) 0.0341(17) Uani 1 1 d . . . H48A H 0.6778 0.3579 0.0660 0.041 Uiso 1 1 calc R . . H48B H 0.5926 0.3175 0.1470 0.041 Uiso 1 1 calc R . . C49 C 0.8938(11) 0.7846(8) 0.1314(7) 0.068(3) Uani 1 1 d . . . H49 H 0.8028 0.7614 0.1147 0.082 Uiso 1 1 calc R . . Cl1 Cl 0.9346(4) 0.6848(3) 0.1480(2) 0.108 Uani 1 1 d . . . Cl2 Cl 0.9170(3) 0.8575(3) 0.2264(2) 0.0940(10) Uani 1 1 d . . . Cl3 Cl 0.9772(4) 0.8474(3) 0.0456(2) 0.1025(11) 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 Hg1 0.0449(2) 0.0457(2) 0.04115(19) -0.00126(14) -0.00217(14) 0.02432(16) Br1 0.0458(5) 0.0424(5) 0.0408(4) -0.0012(3) -0.0073(4) 0.0199(4) Br2 0.0710(6) 0.0800(7) 0.0473(5) 0.0064(5) 0.0117(5) 0.0490(6) C1 0.031(4) 0.024(4) 0.034(4) 0.003(3) -0.006(3) 0.013(3) C2 0.022(3) 0.028(4) 0.039(4) -0.005(3) -0.005(3) 0.012(3) C3 0.039(4) 0.022(4) 0.040(4) 0.003(3) -0.001(3) 0.012(3) C4 0.040(4) 0.030(4) 0.033(4) 0.000(3) -0.006(3) 0.012(3) C5 0.030(4) 0.024(4) 0.046(4) 0.001(3) -0.005(3) 0.011(3) C6 0.034(4) 0.026(4) 0.044(4) 0.001(3) 0.002(3) 0.014(3) C7 0.039(4) 0.047(5) 0.050(5) -0.015(4) -0.006(4) 0.023(4) C8 0.045(5) 0.035(4) 0.044(5) -0.004(4) -0.005(4) 0.018(4) N1 0.038(4) 0.028(3) 0.040(4) -0.005(3) -0.005(3) 0.015(3) C9 0.048(5) 0.034(4) 0.044(5) -0.008(4) 0.001(4) 0.023(4) N2 0.050(4) 0.042(4) 0.038(4) -0.007(3) -0.002(3) 0.020(3) C10 0.036(4) 0.041(5) 0.046(5) -0.011(4) 0.000(4) 0.009(4) C11 0.031(4) 0.037(5) 0.053(5) -0.021(4) -0.001(4) 0.014(4) C12 0.036(4) 0.041(5) 0.062(6) -0.011(4) -0.014(4) 0.011(4) C13 0.028(4) 0.042(5) 0.052(5) 0.005(4) 0.001(3) 0.015(4) C14 0.029(4) 0.031(4) 0.059(5) 0.006(4) -0.001(4) 0.008(3) C15 0.030(4) 0.037(4) 0.045(5) -0.003(4) -0.001(3) 0.015(3) C16 0.031(4) 0.031(4) 0.055(5) 0.007(4) -0.001(4) 0.013(3) C17 0.025(4) 0.039(4) 0.038(4) -0.001(3) 0.000(3) 0.009(3) Br3 0.0354(4) 0.0590(6) 0.0402(4) 0.0083(4) 0.0062(3) 0.0186(4) C18 0.026(4) 0.032(4) 0.039(4) -0.004(3) -0.008(3) 0.010(3) C19 0.025(3) 0.034(4) 0.030(4) 0.001(3) -0.007(3) 0.013(3) C20 0.026(4) 0.037(4) 0.031(4) 0.000(3) -0.002(3) 0.012(3) C21 0.063(6) 0.045(6) 0.075(7) 0.027(5) 0.025(5) 0.023(5) C22 0.044(5) 0.030(4) 0.044(5) -0.003(3) 0.004(4) 0.013(4) C23 0.040(4) 0.034(4) 0.041(4) 0.000(3) 0.001(3) 0.020(4) C24 0.035(4) 0.035(4) 0.033(4) 0.004(3) -0.002(3) 0.018(3) C25 0.033(4) 0.023(4) 0.031(4) -0.004(3) -0.001(3) 0.014(3) C26 0.042(4) 0.029(4) 0.029(4) -0.007(3) -0.004(3) 0.024(3) C27 0.044(4) 0.032(4) 0.023(3) 0.006(3) 0.005(3) 0.023(4) C28 0.032(4) 0.025(4) 0.036(4) 0.007(3) -0.002(3) 0.013(3) C29 0.030(4) 0.020(3) 0.033(4) -0.001(3) -0.007(3) 0.008(3) C30 0.032(4) 0.029(4) 0.025(3) 0.002(3) -0.002(3) 0.012(3) C31 0.043(5) 0.049(5) 0.029(4) -0.007(3) -0.010(3) 0.020(4) C32 0.038(4) 0.037(4) 0.031(4) 0.007(3) 0.004(3) 0.021(4) N3 0.032(3) 0.039(4) 0.032(3) 0.009(3) -0.002(3) 0.018(3) C33 0.042(4) 0.040(4) 0.027(4) 0.004(3) -0.001(3) 0.020(4) N4 0.036(4) 0.044(4) 0.034(3) -0.002(3) -0.004(3) 0.019(3) C34 0.063(6) 0.071(6) 0.021(4) 0.000(4) 0.002(4) 0.041(5) C35 0.063(6) 0.069(6) 0.026(4) 0.016(4) 0.005(4) 0.043(5) C36 0.036(4) 0.042(5) 0.039(4) 0.008(4) 0.000(3) 0.008(4) C37 0.040(4) 0.045(5) 0.025(4) 0.001(3) 0.004(3) 0.015(4) C38 0.034(4) 0.027(4) 0.040(4) -0.003(3) -0.005(3) 0.004(3) C39 0.032(4) 0.028(4) 0.025(3) 0.000(3) -0.001(3) 0.010(3) C40 0.030(4) 0.031(4) 0.030(4) -0.006(3) -0.005(3) 0.007(3) C41 0.031(4) 0.044(5) 0.027(4) -0.005(3) -0.007(3) 0.012(4) Br4 0.0616(5) 0.0480(5) 0.0269(4) -0.0052(3) -0.0044(4) 0.0255(4) C42 0.046(4) 0.035(4) 0.024(4) -0.004(3) -0.006(3) 0.020(4) C43 0.025(3) 0.025(4) 0.036(4) 0.002(3) -0.003(3) 0.006(3) C44 0.023(3) 0.024(4) 0.033(4) 0.000(3) -0.004(3) 0.005(3) C45 0.070(6) 0.041(5) 0.029(4) -0.001(3) -0.006(4) 0.026(5) C46 0.090(7) 0.047(5) 0.025(4) 0.003(4) -0.004(4) 0.037(5) C47 0.037(4) 0.036(4) 0.035(4) -0.005(3) 0.000(3) 0.015(4) C48 0.039(4) 0.028(4) 0.040(4) 0.000(3) -0.009(3) 0.018(3) C49 0.070(7) 0.061(7) 0.075(7) 0.019(6) -0.010(6) 0.023(6) Cl1 0.150 0.139 0.070 0.017 0.018 0.092 Cl2 0.091(2) 0.115(3) 0.080(2) 0.0083(19) -0.0041(18) 0.042(2) Cl3 0.102(3) 0.118(3) 0.083(2) 0.035(2) 0.0176(19) 0.029(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 N2 2.296(7) . ? Hg1 N4 2.303(6) . ? Hg1 Br2 2.5079(10) . ? Hg1 Br1 2.5712(9) . ? C1 C6 1.407(10) . ? C1 C2 1.411(9) . ? C1 C48 1.524(10) . ? C2 C3 1.398(10) . ? C2 C7 1.534(10) . ? C3 C4 1.403(10) . ? C3 C8 1.511(10) . ? C4 C5 1.418(10) . ? C4 C12 1.521(11) . ? C5 C6 1.394(11) . ? C5 C14 1.526(10) . ? C6 C13 1.512(10) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 N1 1.481(10) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? N1 C9 1.348(10) . ? N1 C11 1.368(9) . ? C9 N2 1.316(10) . ? C9 H9 0.9500 . ? N2 C10 1.374(10) . ? C10 C11 1.361(12) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.538(11) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C20 1.402(11) . ? C15 C16 1.404(11) . ? C16 C17 1.403(10) . ? C16 C21 1.502(11) . ? C17 C18 1.382(11) . ? C17 Br3 1.928(7) . ? C18 C19 1.414(10) . ? C18 C22 1.519(10) . ? C19 C20 1.405(10) . ? C19 C24 1.521(10) . ? C20 C23 1.499(10) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.519(10) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C30 1.410(10) . ? C25 C26 1.416(10) . ? C26 C27 1.404(11) . ? C26 C31 1.514(10) . ? C27 C28 1.373(10) . ? C27 C32 1.506(9) . ? C28 C29 1.404(10) . ? C28 C36 1.510(10) . ? C29 C30 1.412(10) . ? C29 C38 1.527(10) . ? C30 C37 1.506(9) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 N3 1.481(9) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? N3 C33 1.331(9) . ? N3 C35 1.357(10) . ? C33 N4 1.322(9) . ? C33 H33 0.9500 . ? N4 C34 1.356(10) . ? C34 C35 1.363(11) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C39 1.528(10) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C44 1.395(10) . ? C39 C40 1.413(10) . ? C40 C41 1.393(11) . ? C40 C45 1.504(10) . ? C41 C42 1.394(10) . ? C41 Br4 1.907(7) . ? C42 C43 1.404(10) . ? C42 C46 1.498(10) . ? C43 C44 1.406(10) . ? C43 C48 1.528(10) . ? C44 C47 1.514(10) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 Cl2 1.737(12) . ? C49 Cl3 1.738(11) . ? C49 Cl1 1.745(11) . ? C49 H49 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 Hg1 N4 106.6(2) . . ? N2 Hg1 Br2 111.75(16) . . ? N4 Hg1 Br2 104.22(16) . . ? N2 Hg1 Br1 96.40(17) . . ? N4 Hg1 Br1 99.22(16) . . ? Br2 Hg1 Br1 135.72(4) . . ? C6 C1 C2 118.7(6) . . ? C6 C1 C48 122.8(6) . . ? C2 C1 C48 118.3(6) . . ? C3 C2 C1 120.5(6) . . ? C3 C2 C7 119.4(6) . . ? C1 C2 C7 120.2(6) . . ? C2 C3 C4 120.3(7) . . ? C2 C3 C8 120.0(7) . . ? C4 C3 C8 119.5(7) . . ? C3 C4 C5 119.0(7) . . ? C3 C4 C12 118.3(7) . . ? C5 C4 C12 122.7(7) . . ? C6 C5 C4 120.1(7) . . ? C6 C5 C14 120.4(7) . . ? C4 C5 C14 119.3(7) . . ? C5 C6 C1 120.6(7) . . ? C5 C6 C13 121.0(7) . . ? C1 C6 C13 118.2(7) . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 C3 113.0(6) . . ? N1 C8 H8A 109.0 . . ? C3 C8 H8A 109.0 . . ? N1 C8 H8B 109.0 . . ? C3 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? C9 N1 C11 107.7(7) . . ? C9 N1 C8 127.3(6) . . ? C11 N1 C8 125.0(7) . . ? N2 C9 N1 110.7(7) . . ? N2 C9 H9 124.7 . . ? N1 C9 H9 124.7 . . ? C9 N2 C10 106.4(7) . . ? C9 N2 Hg1 121.9(5) . . ? C10 N2 Hg1 126.1(5) . . ? C11 C10 N2 109.2(7) . . ? C11 C10 H10 125.4 . . ? N2 C10 H10 125.4 . . ? C10 C11 N1 106.1(7) . . ? C10 C11 H11 127.0 . . ? N1 C11 H11 127.0 . . ? C4 C12 H12A 109.5 . . ? C4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C6 C13 H13A 109.5 . . ? C6 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C6 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C5 C14 C15 118.2(6) . . ? C5 C14 H14A 107.8 . . ? C15 C14 H14A 107.8 . . ? C5 C14 H14B 107.8 . . ? C15 C14 H14B 107.8 . . ? H14A C14 H14B 107.1 . . ? C20 C15 C16 121.1(7) . . ? C20 C15 C14 119.5(7) . . ? C16 C15 C14 119.3(7) . . ? C17 C16 C15 116.9(7) . . ? C17 C16 C21 120.1(7) . . ? C15 C16 C21 123.0(7) . . ? C18 C17 C16 123.8(7) . . ? C18 C17 Br3 118.8(6) . . ? C16 C17 Br3 117.3(6) . . ? C17 C18 C19 118.2(6) . . ? C17 C18 C22 121.2(7) . . ? C19 C18 C22 120.5(7) . . ? C20 C19 C18 119.6(7) . . ? C20 C19 C24 121.7(6) . . ? C18 C19 C24 118.6(6) . . ? C15 C20 C19 120.2(6) . . ? C15 C20 C23 120.5(6) . . ? C19 C20 C23 119.2(7) . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C18 C22 H22A 109.5 . . ? C18 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C18 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C19 119.8(6) . . ? C25 C24 H24A 107.4 . . ? C19 C24 H24A 107.4 . . ? C25 C24 H24B 107.4 . . ? C19 C24 H24B 107.4 . . ? H24A C24 H24B 106.9 . . ? C30 C25 C26 119.6(7) . . ? C30 C25 C24 119.3(6) . . ? C26 C25 C24 121.0(6) . . ? C27 C26 C25 118.8(7) . . ? C27 C26 C31 120.0(6) . . ? C25 C26 C31 121.3(7) . . ? C28 C27 C26 122.0(6) . . ? C28 C27 C32 120.3(7) . . ? C26 C27 C32 117.7(7) . . ? C27 C28 C29 119.3(7) . . ? C27 C28 C36 121.7(7) . . ? C29 C28 C36 119.1(7) . . ? C28 C29 C30 120.3(6) . . ? C28 C29 C38 119.3(6) . . ? C30 C29 C38 120.2(6) . . ? C25 C30 C29 119.5(6) . . ? C25 C30 C37 119.9(6) . . ? C29 C30 C37 120.5(6) . . ? C26 C31 H31A 109.5 . . ? C26 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C26 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N3 C32 C27 113.4(6) . . ? N3 C32 H32A 108.9 . . ? C27 C32 H32A 108.9 . . ? N3 C32 H32B 108.9 . . ? C27 C32 H32B 108.9 . . ? H32A C32 H32B 107.7 . . ? C33 N3 C35 107.4(6) . . ? C33 N3 C32 126.5(6) . . ? C35 N3 C32 125.7(6) . . ? N4 C33 N3 111.2(7) . . ? N4 C33 H33 124.4 . . ? N3 C33 H33 124.4 . . ? C33 N4 C34 105.9(6) . . ? C33 N4 Hg1 126.0(5) . . ? C34 N4 Hg1 125.7(5) . . ? N4 C34 C35 109.2(7) . . ? N4 C34 H34 125.4 . . ? C35 C34 H34 125.4 . . ? N3 C35 C34 106.3(7) . . ? N3 C35 H35 126.9 . . ? C34 C35 H35 126.9 . . ? C28 C36 H36A 109.5 . . ? C28 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C28 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C30 C37 H37A 109.5 . . ? C30 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C30 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C29 C38 C39 119.2(6) . . ? C29 C38 H38A 107.5 . . ? C39 C38 H38A 107.5 . . ? C29 C38 H38B 107.5 . . ? C39 C38 H38B 107.5 . . ? H38A C38 H38B 107.0 . . ? C44 C39 C40 121.0(6) . . ? C44 C39 C38 120.7(6) . . ? C40 C39 C38 118.2(6) . . ? C41 C40 C39 116.6(7) . . ? C41 C40 C45 120.4(6) . . ? C39 C40 C45 123.0(7) . . ? C40 C41 C42 124.2(7) . . ? C40 C41 Br4 117.8(6) . . ? C42 C41 Br4 118.0(5) . . ? C41 C42 C43 117.8(6) . . ? C41 C42 C46 119.8(6) . . ? C43 C42 C46 122.4(7) . . ? C42 C43 C44 119.9(6) . . ? C42 C43 C48 120.1(6) . . ? C44 C43 C48 119.6(6) . . ? C39 C44 C43 120.3(6) . . ? C39 C44 C47 119.7(6) . . ? C43 C44 C47 120.0(6) . . ? C40 C45 H45A 109.5 . . ? C40 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C40 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C42 C46 H46A 109.5 . . ? C42 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C42 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C44 C47 H47A 109.5 . . ? C44 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C44 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C1 C48 C43 120.0(6) . . ? C1 C48 H48A 107.3 . . ? C43 C48 H48A 107.3 . . ? C1 C48 H48B 107.3 . . ? C43 C48 H48B 107.3 . . ? H48A C48 H48B 106.9 . . ? Cl2 C49 Cl3 111.4(6) . . ? Cl2 C49 Cl1 111.1(6) . . ? Cl3 C49 Cl1 110.1(7) . . ? Cl2 C49 H49 108.0 . . ? Cl3 C49 H49 108.0 . . ? Cl1 C49 H49 108.0 . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.527 _refine_diff_density_min -0.945 _refine_diff_density_rms 0.150 # Attachment '7_ZnBr2.cif' data_e1435a _database_code_depnum_ccdc_archive 'CCDC 744817' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H58 Br4 N4 Zn, C H Cl3' _chemical_formula_sum 'C49 H55 Br4 Cl3 N4 Zn' _chemical_formula_weight 1191.33 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' Br Br -0.2901 2.4595 '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' 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.5652(2) _cell_length_b 14.7038(4) _cell_length_c 15.2283(4) _cell_angle_alpha 92.5000(10) _cell_angle_beta 92.9650(10) _cell_angle_gamma 110.0270(10) _cell_volume 2424.56(10) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9974 _cell_measurement_theta_min 2.68 _cell_measurement_theta_max 27.50 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.632 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1196 _exptl_absorpt_coefficient_mu 4.007 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5165 _exptl_absorpt_correction_T_max 0.6901 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 48230 _diffrn_reflns_av_R_equivalents 0.0450 _diffrn_reflns_av_sigmaI/netI 0.0497 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 27.71 _reflns_number_total 10879 _reflns_number_gt 8726 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0546P)^2^+13.5313P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10879 _refine_ls_number_parameters 556 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0861 _refine_ls_R_factor_gt 0.0646 _refine_ls_wR_factor_ref 0.1594 _refine_ls_wR_factor_gt 0.1422 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.025 _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 0.55928(6) 0.29309(5) 0.57916(4) 0.02853(16) Uani 1 1 d . . . Br1 Br 0.44925(6) 0.21679(4) 0.44159(4) 0.03345(15) Uani 1 1 d . . . Br2 Br 0.46047(7) 0.30085(6) 0.70959(5) 0.04555(19) Uani 1 1 d . . . C1 C 0.7663(5) 0.3990(4) 0.1857(4) 0.0253(11) Uani 1 1 d . . . C2 C 0.7271(5) 0.4533(4) 0.2487(4) 0.0250(11) Uani 1 1 d . . . C3 C 0.8160(5) 0.5191(4) 0.3093(4) 0.0250(11) Uani 1 1 d . . . C4 C 0.9394(5) 0.5280(4) 0.3108(4) 0.0257(11) Uani 1 1 d . . . C5 C 0.9800(5) 0.4789(4) 0.2440(4) 0.0256(11) Uani 1 1 d . . . C6 C 0.8937(5) 0.4180(4) 0.1794(4) 0.0253(11) Uani 1 1 d . . . C7 C 0.5927(5) 0.4408(5) 0.2516(4) 0.0344(14) Uani 1 1 d . . . H7A H 0.5472 0.3756 0.2694 0.052 Uiso 1 1 calc R . . H7B H 0.5599 0.4493 0.1931 0.052 Uiso 1 1 calc R . . H7C H 0.5836 0.4893 0.2943 0.052 Uiso 1 1 calc R . . C8 C 0.7756(5) 0.5851(4) 0.3702(4) 0.0294(12) Uani 1 1 d . . . H8A H 0.8479 0.6436 0.3888 0.035 Uiso 1 1 calc R . . H8B H 0.7143 0.6064 0.3373 0.035 Uiso 1 1 calc R . . N1 N 0.7214(4) 0.5385(3) 0.4489(3) 0.0251(10) Uani 1 1 d . . . C9 C 0.7024(6) 0.4473(4) 0.4694(4) 0.0318(13) Uani 1 1 d . . . H9 H 0.7243 0.4017 0.4341 0.038 Uiso 1 1 calc R . . N2 N 0.6496(5) 0.4282(4) 0.5446(3) 0.0323(11) Uani 1 1 d . . . C10 C 0.6343(5) 0.5133(4) 0.5741(4) 0.0334(13) Uani 1 1 d . . . H10 H 0.5987 0.5224 0.6272 0.040 Uiso 1 1 calc R . . C11 C 0.6776(5) 0.5811(4) 0.5163(4) 0.0321(13) Uani 1 1 d . . . H11 H 0.6780 0.6459 0.5207 0.039 Uiso 1 1 calc R . . C12 C 1.0290(6) 0.5932(5) 0.3826(4) 0.0389(15) Uani 1 1 d . . . H12A H 1.0609 0.6595 0.3637 0.058 Uiso 1 1 calc R . . H12B H 1.0976 0.5695 0.3939 0.058 Uiso 1 1 calc R . . H12C H 0.9863 0.5926 0.4367 0.058 Uiso 1 1 calc R . . C13 C 0.9351(6) 0.3761(5) 0.0996(4) 0.0338(13) Uani 1 1 d . . . H13A H 0.9424 0.3135 0.1126 0.051 Uiso 1 1 calc R . . H13B H 1.0154 0.4208 0.0849 0.051 Uiso 1 1 calc R . . H13C H 0.8744 0.3668 0.0497 0.051 Uiso 1 1 calc R . . C14 C 1.1166(5) 0.4980(4) 0.2370(4) 0.0310(13) Uani 1 1 d . . . H14A H 1.1607 0.5355 0.2917 0.037 Uiso 1 1 calc R . . H14B H 1.1435 0.5405 0.1879 0.037 Uiso 1 1 calc R . . C15 C 1.1608(5) 0.4121(4) 0.2228(4) 0.0262(11) Uani 1 1 d . . . C16 C 1.2355(5) 0.4105(4) 0.1534(4) 0.0299(12) Uani 1 1 d . . . C17 C 1.2729(5) 0.3301(4) 0.1429(4) 0.0268(11) Uani 1 1 d . . . Br3 Br 1.36291(6) 0.32231(5) 0.04158(4) 0.03627(16) Uani 1 1 d . . . C18 C 1.2455(5) 0.2545(4) 0.1990(4) 0.0250(11) Uani 1 1 d . . . C19 C 1.1683(5) 0.2565(4) 0.2668(3) 0.0226(10) Uani 1 1 d . . . C20 C 1.1283(5) 0.3359(4) 0.2795(4) 0.0246(11) Uani 1 1 d . . . C21 C 1.2791(7) 0.4944(5) 0.0952(5) 0.0494(19) Uani 1 1 d . . . H21A H 1.3544 0.4940 0.0688 0.074 Uiso 1 1 calc R . . H21B H 1.2963 0.5555 0.1305 0.074 Uiso 1 1 calc R . . H21C H 1.2148 0.4882 0.0484 0.074 Uiso 1 1 calc R . . C22 C 1.2996(6) 0.1751(4) 0.1887(4) 0.0308(12) Uani 1 1 d . . . H22A H 1.3667 0.1945 0.1490 0.046 Uiso 1 1 calc R . . H22B H 1.2354 0.1153 0.1639 0.046 Uiso 1 1 calc R . . H22C H 1.3319 0.1638 0.2464 0.046 Uiso 1 1 calc R . . C23 C 1.0547(5) 0.3417(4) 0.3576(4) 0.0267(11) Uani 1 1 d . . . H23A H 0.9664 0.3118 0.3402 0.040 Uiso 1 1 calc R . . H23B H 1.0732 0.4098 0.3775 0.040 Uiso 1 1 calc R . . H23C H 1.0768 0.3071 0.4056 0.040 Uiso 1 1 calc R . . C24 C 1.1349(5) 0.1738(4) 0.3276(4) 0.0263(11) Uani 1 1 d . . . H24A H 1.1844 0.1981 0.3842 0.032 Uiso 1 1 calc R . . H24B H 1.1625 0.1224 0.3017 0.032 Uiso 1 1 calc R . . C25 C 1.0011(5) 0.1260(4) 0.3487(3) 0.0206(10) Uani 1 1 d . . . C26 C 0.9687(5) 0.1131(4) 0.4360(4) 0.0249(11) Uani 1 1 d . . . C27 C 0.8456(5) 0.0623(4) 0.4518(3) 0.0224(10) Uani 1 1 d . . . C28 C 0.7530(5) 0.0299(4) 0.3828(4) 0.0237(11) Uani 1 1 d . . . C29 C 0.7853(5) 0.0454(4) 0.2956(3) 0.0220(10) Uani 1 1 d . . . C30 C 0.9098(5) 0.0882(4) 0.2786(3) 0.0247(11) Uani 1 1 d . . . C31 C 1.0615(6) 0.1527(4) 0.5140(4) 0.0303(12) Uani 1 1 d . . . H31A H 1.0840 0.0998 0.5382 0.046 Uiso 1 1 calc R . . H31B H 1.0254 0.1818 0.5593 0.046 Uiso 1 1 calc R . . H31C H 1.1354 0.2021 0.4950 0.046 Uiso 1 1 calc R . . C32 C 0.8129(5) 0.0407(4) 0.5454(4) 0.0277(12) Uani 1 1 d . . . H32A H 0.7477 -0.0239 0.5452 0.033 Uiso 1 1 calc R . . H32B H 0.8864 0.0385 0.5803 0.033 Uiso 1 1 calc R . . N3 N 0.7692(4) 0.1145(3) 0.5877(3) 0.0249(9) Uani 1 1 d . . . C33 C 0.7112(5) 0.1676(4) 0.5471(4) 0.0268(11) Uani 1 1 d . . . H33 H 0.6988 0.1682 0.4850 0.032 Uiso 1 1 calc R . . N4 N 0.6735(4) 0.2191(4) 0.6055(3) 0.0281(10) Uani 1 1 d . . . C34 C 0.7095(6) 0.1975(5) 0.6869(4) 0.0384(15) Uani 1 1 d . . . H34 H 0.6956 0.2236 0.7419 0.046 Uiso 1 1 calc R . . C35 C 0.7685(6) 0.1326(5) 0.6760(4) 0.0391(15) Uani 1 1 d . . . H35 H 0.8027 0.1051 0.7213 0.047 Uiso 1 1 calc R . . C36 C 0.6191(5) -0.0211(4) 0.4007(4) 0.0318(13) Uani 1 1 d . . . H36A H 0.6122 -0.0267 0.4642 0.048 Uiso 1 1 calc R . . H36B H 0.5891 -0.0859 0.3705 0.048 Uiso 1 1 calc R . . H36C H 0.5694 0.0166 0.3789 0.048 Uiso 1 1 calc R . . C37 C 0.9474(5) 0.0917(5) 0.1849(4) 0.0315(13) Uani 1 1 d . . . H37A H 0.8866 0.0387 0.1482 0.047 Uiso 1 1 calc R . . H37B H 1.0286 0.0849 0.1835 0.047 Uiso 1 1 calc R . . H37C H 0.9511 0.1540 0.1621 0.047 Uiso 1 1 calc R . . C38 C 0.6854(5) 0.0082(4) 0.2207(4) 0.0287(12) Uani 1 1 d . . . H38A H 0.6926 -0.0518 0.1934 0.034 Uiso 1 1 calc R . . H38B H 0.6047 -0.0105 0.2470 0.034 Uiso 1 1 calc R . . C39 C 0.6821(5) 0.0738(4) 0.1476(3) 0.0232(11) Uani 1 1 d . . . C40 C 0.6745(5) 0.0378(4) 0.0594(3) 0.0248(11) Uani 1 1 d . . . C41 C 0.6653(5) 0.0989(4) -0.0056(3) 0.0256(11) Uani 1 1 d . . . Br4 Br 0.65021(6) 0.04989(5) -0.12623(4) 0.03665(16) Uani 1 1 d . . . C42 C 0.6655(5) 0.1930(4) 0.0097(4) 0.0271(11) Uani 1 1 d . . . C43 C 0.6744(5) 0.2280(4) 0.0989(3) 0.0244(11) Uani 1 1 d . . . C44 C 0.6783(5) 0.1669(4) 0.1665(3) 0.0225(10) Uani 1 1 d . . . C45 C 0.6741(7) -0.0627(4) 0.0347(4) 0.0382(15) Uani 1 1 d . . . H45A H 0.7538 -0.0584 0.0128 0.057 Uiso 1 1 calc R . . H45B H 0.6082 -0.0940 -0.0113 0.057 Uiso 1 1 calc R . . H45C H 0.6599 -0.1011 0.0867 0.057 Uiso 1 1 calc R . . C46 C 0.6516(7) 0.2526(5) -0.0647(4) 0.0417(16) Uani 1 1 d . . . H46A H 0.7330 0.2875 -0.0852 0.063 Uiso 1 1 calc R . . H46B H 0.6137 0.2993 -0.0444 0.063 Uiso 1 1 calc R . . H46C H 0.5991 0.2099 -0.1132 0.063 Uiso 1 1 calc R . . C47 C 0.6705(6) 0.1995(4) 0.2610(4) 0.0310(12) Uani 1 1 d . . . H47A H 0.7539 0.2300 0.2892 0.046 Uiso 1 1 calc R . . H47B H 0.6253 0.1432 0.2930 0.046 Uiso 1 1 calc R . . H47C H 0.6272 0.2463 0.2620 0.046 Uiso 1 1 calc R . . C48 C 0.6699(5) 0.3289(4) 0.1197(4) 0.0277(12) Uani 1 1 d . . . H48A H 0.5878 0.3206 0.1413 0.033 Uiso 1 1 calc R . . H48B H 0.6743 0.3608 0.0635 0.033 Uiso 1 1 calc R . . C49 C 0.9061(9) 0.7756(7) 0.1212(6) 0.074(3) Uani 1 1 d . . . H49 H 0.8202 0.7488 0.0929 0.089 Uiso 1 1 calc R . . Cl1 Cl 0.9582(4) 0.6787(3) 0.1369(2) 0.108 Uani 1 1 d . . . Cl2 Cl 0.9017(4) 0.8367(3) 0.2204(2) 0.1148(12) Uani 1 1 d . . . Cl3 Cl 0.9968(4) 0.8535(3) 0.0511(2) 0.1170(12) 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 0.0296(4) 0.0306(4) 0.0288(3) -0.0002(3) 0.0004(3) 0.0153(3) Br1 0.0340(3) 0.0325(3) 0.0333(3) -0.0008(2) -0.0066(2) 0.0124(2) Br2 0.0547(4) 0.0571(4) 0.0397(4) 0.0063(3) 0.0150(3) 0.0364(4) C1 0.031(3) 0.020(3) 0.025(3) -0.001(2) -0.003(2) 0.010(2) C2 0.022(3) 0.021(3) 0.034(3) 0.001(2) -0.002(2) 0.010(2) C3 0.028(3) 0.021(3) 0.027(3) 0.000(2) 0.002(2) 0.010(2) C4 0.026(3) 0.020(3) 0.031(3) -0.004(2) -0.005(2) 0.009(2) C5 0.022(3) 0.022(3) 0.033(3) 0.001(2) -0.002(2) 0.010(2) C6 0.030(3) 0.020(3) 0.026(3) 0.000(2) 0.000(2) 0.010(2) C7 0.026(3) 0.035(3) 0.044(4) -0.010(3) -0.003(3) 0.017(3) C8 0.032(3) 0.019(3) 0.038(3) -0.004(2) 0.002(2) 0.012(2) N1 0.024(2) 0.019(2) 0.032(2) -0.0056(18) -0.0002(18) 0.0084(18) C9 0.035(3) 0.025(3) 0.039(3) -0.003(2) 0.003(3) 0.016(2) N2 0.036(3) 0.033(3) 0.030(3) -0.007(2) 0.000(2) 0.016(2) C10 0.028(3) 0.034(3) 0.035(3) -0.011(3) 0.000(2) 0.010(2) C11 0.030(3) 0.028(3) 0.039(3) -0.015(3) -0.002(2) 0.014(2) C12 0.032(3) 0.035(3) 0.045(4) -0.014(3) -0.009(3) 0.010(3) C13 0.032(3) 0.035(3) 0.031(3) -0.003(3) 0.004(2) 0.008(3) C14 0.027(3) 0.021(3) 0.043(3) 0.000(2) 0.002(2) 0.007(2) C15 0.023(3) 0.023(3) 0.032(3) -0.002(2) -0.003(2) 0.008(2) C16 0.022(3) 0.032(3) 0.035(3) 0.008(2) 0.003(2) 0.008(2) C17 0.020(3) 0.029(3) 0.029(3) -0.003(2) -0.002(2) 0.006(2) Br3 0.0300(3) 0.0498(4) 0.0315(3) 0.0023(3) 0.0046(2) 0.0167(3) C18 0.022(3) 0.027(3) 0.028(3) -0.004(2) -0.003(2) 0.013(2) C19 0.021(3) 0.023(3) 0.023(3) 0.000(2) -0.001(2) 0.008(2) C20 0.015(2) 0.026(3) 0.031(3) 0.001(2) -0.002(2) 0.007(2) C21 0.050(4) 0.041(4) 0.066(5) 0.026(4) 0.027(4) 0.021(3) C22 0.036(3) 0.031(3) 0.033(3) 0.004(2) 0.009(2) 0.020(3) C23 0.024(3) 0.025(3) 0.033(3) 0.000(2) 0.003(2) 0.012(2) C24 0.027(3) 0.031(3) 0.025(3) 0.001(2) -0.002(2) 0.016(2) C25 0.021(3) 0.017(2) 0.026(3) -0.002(2) -0.001(2) 0.0115(19) C26 0.031(3) 0.022(3) 0.026(3) 0.001(2) -0.001(2) 0.015(2) C27 0.029(3) 0.019(2) 0.023(3) 0.000(2) 0.000(2) 0.013(2) C28 0.028(3) 0.017(2) 0.027(3) 0.004(2) 0.002(2) 0.009(2) C29 0.028(3) 0.018(2) 0.022(3) 0.001(2) 0.002(2) 0.011(2) C30 0.031(3) 0.025(3) 0.020(3) -0.001(2) -0.001(2) 0.012(2) C31 0.034(3) 0.032(3) 0.024(3) -0.003(2) -0.006(2) 0.013(2) C32 0.032(3) 0.029(3) 0.027(3) 0.002(2) 0.001(2) 0.017(2) N3 0.027(2) 0.034(3) 0.019(2) 0.0028(18) 0.0007(17) 0.017(2) C33 0.031(3) 0.029(3) 0.024(3) 0.002(2) 0.000(2) 0.016(2) N4 0.031(3) 0.033(3) 0.024(2) 0.002(2) 0.0010(19) 0.015(2) C34 0.044(4) 0.055(4) 0.024(3) 0.000(3) -0.002(3) 0.029(3) C35 0.049(4) 0.061(4) 0.019(3) 0.002(3) -0.001(3) 0.036(3) C36 0.032(3) 0.030(3) 0.031(3) 0.007(2) 0.002(2) 0.006(2) C37 0.028(3) 0.037(3) 0.025(3) -0.004(2) 0.002(2) 0.006(2) C38 0.030(3) 0.024(3) 0.027(3) 0.001(2) -0.003(2) 0.004(2) C39 0.022(3) 0.021(3) 0.024(3) -0.002(2) -0.006(2) 0.005(2) C40 0.026(3) 0.024(3) 0.023(3) -0.002(2) -0.004(2) 0.009(2) C41 0.031(3) 0.026(3) 0.017(2) -0.002(2) -0.003(2) 0.008(2) Br4 0.0501(4) 0.0396(3) 0.0214(3) -0.0058(2) -0.0023(2) 0.0186(3) C42 0.032(3) 0.025(3) 0.023(3) 0.000(2) -0.001(2) 0.009(2) C43 0.022(3) 0.025(3) 0.024(3) -0.002(2) -0.002(2) 0.007(2) C44 0.022(3) 0.024(3) 0.021(3) -0.004(2) -0.0041(19) 0.008(2) C45 0.058(4) 0.030(3) 0.028(3) -0.007(2) -0.006(3) 0.020(3) C46 0.068(5) 0.030(3) 0.028(3) 0.000(3) 0.000(3) 0.019(3) C47 0.035(3) 0.037(3) 0.023(3) -0.001(2) 0.000(2) 0.016(3) C48 0.026(3) 0.029(3) 0.030(3) -0.003(2) -0.005(2) 0.014(2) C49 0.066(6) 0.077(6) 0.070(6) 0.018(5) -0.018(5) 0.014(5) Cl1 0.150 0.139 0.070 0.017 0.018 0.092 Cl2 0.132(3) 0.165(3) 0.081(2) 0.025(2) 0.0236(19) 0.090(3) Cl3 0.121(3) 0.117(3) 0.111(3) 0.038(2) 0.054(2) 0.028(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N2 2.010(5) . ? Zn1 N4 2.014(5) . ? Zn1 Br2 2.3596(9) . ? Zn1 Br1 2.4100(9) . ? C1 C2 1.409(7) . ? C1 C6 1.412(8) . ? C1 C48 1.524(7) . ? C2 C3 1.409(7) . ? C2 C7 1.505(8) . ? C3 C4 1.386(8) . ? C3 C8 1.516(7) . ? C4 C5 1.412(8) . ? C4 C12 1.517(8) . ? C5 C6 1.405(7) . ? C5 C14 1.517(8) . ? C6 C13 1.510(8) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 N1 1.468(7) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? N1 C9 1.336(7) . ? N1 C11 1.385(7) . ? C9 N2 1.321(8) . ? C9 H9 0.9500 . ? N2 C10 1.382(7) . ? C10 C11 1.342(9) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.528(8) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C20 1.403(8) . ? C15 C16 1.403(8) . ? C16 C17 1.397(8) . ? C16 C21 1.509(9) . ? C17 C18 1.391(8) . ? C17 Br3 1.926(6) . ? C18 C19 1.406(7) . ? C18 C22 1.509(7) . ? C19 C20 1.405(7) . ? C19 C24 1.516(8) . ? C20 C23 1.514(7) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.522(7) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.404(7) . ? C25 C30 1.412(7) . ? C26 C27 1.402(8) . ? C26 C31 1.510(7) . ? C27 C28 1.402(7) . ? C27 C32 1.513(7) . ? C28 C29 1.404(7) . ? C28 C36 1.517(8) . ? C29 C30 1.403(8) . ? C29 C38 1.520(7) . ? C30 C37 1.511(7) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 N3 1.483(7) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? N3 C33 1.341(7) . ? N3 C35 1.360(7) . ? C33 N4 1.329(7) . ? C33 H33 0.9500 . ? N4 C34 1.372(7) . ? C34 C35 1.359(9) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C39 1.513(8) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C44 1.402(7) . ? C39 C40 1.409(7) . ? C40 C41 1.388(8) . ? C40 C45 1.508(8) . ? C41 C42 1.393(8) . ? C41 Br4 1.921(5) . ? C42 C43 1.418(7) . ? C42 C46 1.497(8) . ? C43 C44 1.406(8) . ? C43 C48 1.521(7) . ? C44 C47 1.513(7) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 Cl3 1.718(10) . ? C49 Cl2 1.735(11) . ? C49 Cl1 1.748(11) . ? C49 H49 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 Zn1 N4 112.5(2) . . ? N2 Zn1 Br2 109.51(14) . . ? N4 Zn1 Br2 106.28(14) . . ? N2 Zn1 Br1 101.35(14) . . ? N4 Zn1 Br1 104.06(14) . . ? Br2 Zn1 Br1 123.15(4) . . ? C2 C1 C6 119.5(5) . . ? C2 C1 C48 118.6(5) . . ? C6 C1 C48 121.6(5) . . ? C1 C2 C3 118.9(5) . . ? C1 C2 C7 120.6(5) . . ? C3 C2 C7 120.5(5) . . ? C4 C3 C2 121.4(5) . . ? C4 C3 C8 119.8(5) . . ? C2 C3 C8 118.6(5) . . ? C3 C4 C5 119.5(5) . . ? C3 C4 C12 119.2(5) . . ? C5 C4 C12 121.3(5) . . ? C6 C5 C4 119.5(5) . . ? C6 C5 C14 119.8(5) . . ? C4 C5 C14 120.5(5) . . ? C5 C6 C1 120.2(5) . . ? C5 C6 C13 121.0(5) . . ? C1 C6 C13 118.7(5) . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 C3 113.1(4) . . ? N1 C8 H8A 108.9 . . ? C3 C8 H8A 108.9 . . ? N1 C8 H8B 108.9 . . ? C3 C8 H8B 108.9 . . ? H8A C8 H8B 107.8 . . ? C9 N1 C11 106.4(5) . . ? C9 N1 C8 127.5(5) . . ? C11 N1 C8 126.1(5) . . ? N2 C9 N1 111.9(5) . . ? N2 C9 H9 124.0 . . ? N1 C9 H9 124.0 . . ? C9 N2 C10 105.4(5) . . ? C9 N2 Zn1 123.5(4) . . ? C10 N2 Zn1 127.6(4) . . ? C11 C10 N2 109.5(5) . . ? C11 C10 H10 125.3 . . ? N2 C10 H10 125.3 . . ? C10 C11 N1 106.8(5) . . ? C10 C11 H11 126.6 . . ? N1 C11 H11 126.6 . . ? C4 C12 H12A 109.5 . . ? C4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C6 C13 H13A 109.5 . . ? C6 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C6 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C5 C14 C15 119.1(5) . . ? C5 C14 H14A 107.5 . . ? C15 C14 H14A 107.5 . . ? C5 C14 H14B 107.5 . . ? C15 C14 H14B 107.5 . . ? H14A C14 H14B 107.0 . . ? C20 C15 C16 120.3(5) . . ? C20 C15 C14 120.2(5) . . ? C16 C15 C14 119.5(5) . . ? C17 C16 C15 117.3(5) . . ? C17 C16 C21 121.1(5) . . ? C15 C16 C21 121.5(5) . . ? C18 C17 C16 124.1(5) . . ? C18 C17 Br3 118.5(4) . . ? C16 C17 Br3 117.3(4) . . ? C17 C18 C19 117.5(5) . . ? C17 C18 C22 121.1(5) . . ? C19 C18 C22 121.4(5) . . ? C20 C19 C18 120.0(5) . . ? C20 C19 C24 121.4(5) . . ? C18 C19 C24 118.5(5) . . ? C15 C20 C19 120.6(5) . . ? C15 C20 C23 119.7(5) . . ? C19 C20 C23 119.6(5) . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C18 C22 H22A 109.5 . . ? C18 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C18 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C19 C24 C25 119.6(4) . . ? C19 C24 H24A 107.4 . . ? C25 C24 H24A 107.4 . . ? C19 C24 H24B 107.4 . . ? C25 C24 H24B 107.4 . . ? H24A C24 H24B 107.0 . . ? C26 C25 C30 119.7(5) . . ? C26 C25 C24 121.2(5) . . ? C30 C25 C24 118.9(5) . . ? C27 C26 C25 119.0(5) . . ? C27 C26 C31 118.6(5) . . ? C25 C26 C31 122.4(5) . . ? C26 C27 C28 121.6(5) . . ? C26 C27 C32 118.9(5) . . ? C28 C27 C32 119.6(5) . . ? C27 C28 C29 119.2(5) . . ? C27 C28 C36 121.2(5) . . ? C29 C28 C36 119.6(5) . . ? C30 C29 C28 119.7(5) . . ? C30 C29 C38 121.0(5) . . ? C28 C29 C38 119.2(5) . . ? C29 C30 C25 120.4(5) . . ? C29 C30 C37 120.0(5) . . ? C25 C30 C37 119.5(5) . . ? C26 C31 H31A 109.5 . . ? C26 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C26 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N3 C32 C27 112.1(4) . . ? N3 C32 H32A 109.2 . . ? C27 C32 H32A 109.2 . . ? N3 C32 H32B 109.2 . . ? C27 C32 H32B 109.2 . . ? H32A C32 H32B 107.9 . . ? C33 N3 C35 107.5(5) . . ? C33 N3 C32 126.6(5) . . ? C35 N3 C32 125.5(5) . . ? N4 C33 N3 110.7(5) . . ? N4 C33 H33 124.6 . . ? N3 C33 H33 124.6 . . ? C33 N4 C34 106.1(5) . . ? C33 N4 Zn1 126.0(4) . . ? C34 N4 Zn1 127.1(4) . . ? C35 C34 N4 108.8(5) . . ? C35 C34 H34 125.6 . . ? N4 C34 H34 125.6 . . ? C34 C35 N3 106.9(5) . . ? C34 C35 H35 126.6 . . ? N3 C35 H35 126.6 . . ? C28 C36 H36A 109.5 . . ? C28 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C28 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C30 C37 H37A 109.5 . . ? C30 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C30 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C39 C38 C29 119.0(5) . . ? C39 C38 H38A 107.6 . . ? C29 C38 H38A 107.6 . . ? C39 C38 H38B 107.6 . . ? C29 C38 H38B 107.6 . . ? H38A C38 H38B 107.0 . . ? C44 C39 C40 120.1(5) . . ? C44 C39 C38 120.8(5) . . ? C40 C39 C38 119.0(5) . . ? C41 C40 C39 117.0(5) . . ? C41 C40 C45 120.4(5) . . ? C39 C40 C45 122.6(5) . . ? C40 C41 C42 125.2(5) . . ? C40 C41 Br4 117.7(4) . . ? C42 C41 Br4 117.1(4) . . ? C41 C42 C43 116.8(5) . . ? C41 C42 C46 121.4(5) . . ? C43 C42 C46 121.8(5) . . ? C44 C43 C42 119.7(5) . . ? C44 C43 C48 121.0(5) . . ? C42 C43 C48 119.2(5) . . ? C39 C44 C43 121.1(5) . . ? C39 C44 C47 119.3(5) . . ? C43 C44 C47 119.5(5) . . ? C40 C45 H45A 109.5 . . ? C40 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C40 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C42 C46 H46A 109.5 . . ? C42 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C42 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C44 C47 H47A 109.5 . . ? C44 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C44 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C43 C48 C1 119.7(5) . . ? C43 C48 H48A 107.4 . . ? C1 C48 H48A 107.4 . . ? C43 C48 H48B 107.4 . . ? C1 C48 H48B 107.4 . . ? H48A C48 H48B 106.9 . . ? Cl3 C49 Cl2 110.8(6) . . ? Cl3 C49 Cl1 110.2(6) . . ? Cl2 C49 Cl1 111.6(5) . . ? Cl3 C49 H49 108.0 . . ? Cl2 C49 H49 108.0 . . ? Cl1 C49 H49 108.0 . . ? _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 27.71 _diffrn_measured_fraction_theta_full 0.959 _refine_diff_density_max 1.900 _refine_diff_density_min -1.870 _refine_diff_density_rms 0.139 # Attachment '_8-CoBr2_n.cif' data_e1464a _database_code_depnum_ccdc_archive 'CCDC 744818' #TrackingRef '_8-CoBr2_n.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H54 Br4 Co N4' _chemical_formula_sum 'C48 H54 Br4 Co N4' _chemical_formula_weight 1065.52 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pca2(1) _symmetry_space_group_name_Hall 'P 2c -2ac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 18.3656(4) _cell_length_b 16.0416(4) _cell_length_c 17.5199(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5161.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6340 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 27.43 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.371 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2148 _exptl_absorpt_coefficient_mu 3.462 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6814 _exptl_absorpt_correction_T_max 0.7458 _exptl_absorpt_process_details sadabs _exptl_special_details ; Owing to large disorder of the solvent present in the cavities of this structure, the SQUEEZE command has been applied Because of the floppiness of the phenyl ring we used the same thermal parameters for some atoms ; _diffrn_ambient_temperature 173(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 23482 _diffrn_reflns_av_R_equivalents 0.0540 _diffrn_reflns_av_sigmaI/netI 0.0440 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 27.54 _reflns_number_total 9338 _reflns_number_gt 7626 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^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 constr _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 0.03(2) _refine_ls_number_reflns 9338 _refine_ls_number_parameters 517 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1267 _refine_ls_R_factor_gt 0.0951 _refine_ls_wR_factor_ref 0.2672 _refine_ls_wR_factor_gt 0.2445 _refine_ls_goodness_of_fit_ref 1.256 _refine_ls_restrained_S_all 1.256 _refine_ls_shift/su_max 0.021 _refine_ls_shift/su_mean 0.001 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 -0.0868(4) 0.1607(5) -0.0891(4) 0.028(2) Uani 1 1 d G . . N2 N -0.1568(3) 0.1577(5) -0.1234(5) 0.033(2) Uani 1 1 d G . . C19 C -0.1503(4) 0.1147(6) -0.1939(5) 0.048(4) Uani 1 1 d G . . H19 H -0.1887 0.1036 -0.2288 0.058 Uiso 1 1 calc R . . C20 C -0.0763(5) 0.0912(6) -0.2032(5) 0.048(4) Uani 1 1 d G . . H20 H -0.0565 0.0617 -0.2454 0.058 Uiso 1 1 calc R . . C21 C -0.0370(3) 0.1197(6) -0.1385(5) 0.040(3) Uani 1 1 d G . . H21 H 0.0136 0.1125 -0.1297 0.048 Uiso 1 1 calc R . . Co1 Co -0.24360(9) 0.22445(10) -0.08856(11) 0.0316(4) Uani 1 1 d . . . Br1 Br -0.20987(7) 0.36076(8) -0.05016(11) 0.0444(4) Uani 1 1 d . . . Br2 Br -0.30141(8) 0.15154(8) 0.01278(10) 0.0449(4) Uani 1 1 d . . . C1 C 0.1886(5) 0.4345(6) 0.2269(6) 0.021(2) Uani 1 1 d . . . C2 C 0.2585(5) 0.4636(6) 0.2224(6) 0.021(2) Uani 1 1 d . . . C3 C 0.2927(6) 0.4578(6) 0.1527(6) 0.020(2) Uani 1 1 d . . . Br3 Br 0.39074(6) 0.50074(9) 0.14484(8) 0.0412(4) Uani 1 1 d . . . C4 C 0.2619(6) 0.4214(6) 0.0878(6) 0.018(2) Uani 1 1 d . . . C5 C 0.1899(5) 0.3949(5) 0.0945(5) 0.0140(18) Uani 1 1 d . . . C6 C 0.1536(5) 0.4026(5) 0.1616(5) 0.034(3) Uani 1 1 d . . . C7 C 0.3016(7) 0.5015(8) 0.2907(6) 0.034(3) Uani 1 1 d . . . H7A H 0.3245 0.5539 0.2748 0.051 Uiso 1 1 calc R . . H7B H 0.3393 0.4621 0.3072 0.051 Uiso 1 1 calc R . . H7C H 0.2681 0.5123 0.3332 0.051 Uiso 1 1 calc R . . C8 C 0.3054(6) 0.4175(6) 0.0148(6) 0.034(3) Uani 1 1 d . . . H8A H 0.3389 0.4650 0.0127 0.051 Uiso 1 1 calc R . . H8B H 0.2723 0.4197 -0.0290 0.051 Uiso 1 1 calc R . . H8C H 0.3332 0.3654 0.0133 0.051 Uiso 1 1 calc R . . C9 C 0.0699(5) 0.3825(6) 0.1650(6) 0.0189(19) Uani 1 1 d . . . H9A H 0.0481 0.3920 0.1147 0.028 Uiso 1 1 calc R . . H9B H 0.0464 0.4189 0.2027 0.028 Uiso 1 1 calc R . . H9C H 0.0629 0.3242 0.1798 0.028 Uiso 1 1 calc R . . C10 C 0.1516(5) 0.3629(6) 0.0225(5) 0.0142(18) Uani 1 1 d . . . H10A H 0.1890 0.3560 -0.0177 0.017 Uiso 1 1 calc R . . H10B H 0.1177 0.4069 0.0050 0.017 Uiso 1 1 calc R . . C11 C 0.1082(5) 0.2800(6) 0.0281(6) 0.0160(19) Uani 1 1 d . . . C12 C 0.0356(6) 0.2740(6) 0.0060(6) 0.020(2) Uani 1 1 d . . . C13 C 0.0006(5) 0.1961(6) 0.0088(6) 0.0193(19) Uani 1 1 d . . . C14 C 0.0369(5) 0.1271(5) 0.0394(6) 0.0152(18) Uani 1 1 d . . . C15 C 0.1100(5) 0.1306(5) 0.0630(5) 0.0152(18) Uani 1 1 d . . . C16 C 0.1466(4) 0.2082(6) 0.0562(5) 0.0152(18) Uani 1 1 d . . . C17 C -0.0026(7) 0.3477(6) -0.0318(8) 0.035(3) Uani 1 1 d . . . H17A H 0.0337 0.3892 -0.0471 0.052 Uiso 1 1 calc R . . H17B H -0.0368 0.3729 0.0044 0.052 Uiso 1 1 calc R . . H17C H -0.0292 0.3283 -0.0769 0.052 Uiso 1 1 calc R . . C18 C -0.0789(5) 0.1913(6) -0.0088(6) 0.023(2) Uani 1 1 d . . . H18A H -0.1015 0.2469 -0.0033 0.027 Uiso 1 1 calc R . . H18B H -0.1032 0.1524 0.0269 0.027 Uiso 1 1 calc R . . C22 C -0.0038(5) 0.0421(6) 0.0389(7) 0.023(2) Uani 1 1 d . . . H22A H -0.0329 0.0368 0.0855 0.034 Uiso 1 1 calc R . . H22B H 0.0317 -0.0034 0.0366 0.034 Uiso 1 1 calc R . . H22C H -0.0358 0.0393 -0.0058 0.034 Uiso 1 1 calc R . . C23 C 0.2282(5) 0.2117(6) 0.0713(6) 0.0158(19) Uani 1 1 d . . . H23A H 0.2369 0.2175 0.1262 0.024 Uiso 1 1 calc R . . H23B H 0.2493 0.2596 0.0444 0.024 Uiso 1 1 calc R . . H23C H 0.2510 0.1603 0.0529 0.024 Uiso 1 1 calc R . . C24 C 0.1482(5) 0.0547(5) 0.0959(5) 0.0117(17) Uani 1 1 d . . . H24A H 0.1113 0.0104 0.1029 0.014 Uiso 1 1 calc R . . H24B H 0.1834 0.0344 0.0573 0.014 Uiso 1 1 calc R . . C25 C 0.1879(5) 0.0646(6) 0.1691(5) 0.0119(17) Uani 1 1 d . . . C26 C 0.2621(5) 0.0366(5) 0.1766(5) 0.0111(17) Uani 1 1 d . . . C27 C 0.2929(5) 0.0406(6) 0.2486(6) 0.0138(18) Uani 1 1 d . . . Br4 Br 0.39036(6) -0.00115(8) 0.26121(8) 0.0348(3) Uani 1 1 d . . . C28 C 0.2596(5) 0.0724(6) 0.3154(6) 0.0168(19) Uani 1 1 d . . . C29 C 0.1870(5) 0.1027(5) 0.3067(6) 0.0123(17) Uani 1 1 d . . . C30 C 0.1517(6) 0.0942(5) 0.2336(6) 0.0123(17) Uani 1 1 d . . . C31 C 0.3041(7) 0.0075(8) 0.1116(8) 0.033(3) Uani 1 1 d . . . H31A H 0.3495 0.0393 0.1081 0.050 Uiso 1 1 calc R . . H31B H 0.2757 0.0155 0.0647 0.050 Uiso 1 1 calc R . . H31C H 0.3153 -0.0518 0.1179 0.050 Uiso 1 1 calc R . . C32 C 0.2967(7) 0.0706(8) 0.3926(7) 0.032(3) Uani 1 1 d . . . H32A H 0.3106 0.1274 0.4072 0.048 Uiso 1 1 calc R . . H32B H 0.3404 0.0357 0.3897 0.048 Uiso 1 1 calc R . . H32C H 0.2633 0.0476 0.4307 0.048 Uiso 1 1 calc R . . C33 C 0.0723(5) 0.1145(6) 0.2288(6) 0.0158(19) Uani 1 1 d . . . H33A H 0.0500 0.1081 0.2793 0.024 Uiso 1 1 calc R . . H33B H 0.0487 0.0766 0.1926 0.024 Uiso 1 1 calc R . . H33C H 0.0663 0.1721 0.2114 0.024 Uiso 1 1 calc R . . C34 C 0.1471(6) 0.1358(5) 0.3746(6) 0.0158(19) Uani 1 1 d . . . H34A H 0.1830 0.1438 0.4161 0.024 Uiso 1 1 calc R . . H34B H 0.1126 0.0923 0.3917 0.024 Uiso 1 1 calc R . . C35 C 0.1042(6) 0.2176(6) 0.3660(6) 0.018(2) Uani 1 1 d . . . C36 C 0.0290(6) 0.2221(6) 0.3819(7) 0.023(2) Uani 1 1 d . . . C37 C -0.0071(5) 0.2991(6) 0.3768(6) 0.019(2) Uani 1 1 d . . . C38 C 0.0312(5) 0.3707(6) 0.3539(6) 0.0161(19) Uani 1 1 d . . . C39 C 0.1046(5) 0.3642(6) 0.3320(6) 0.0161(19) Uani 1 1 d . . . C40 C 0.1425(5) 0.2884(5) 0.3434(5) 0.0108(17) Uani 1 1 d . . . C41 C -0.0159(8) 0.1455(7) 0.4028(9) 0.042(4) Uani 1 1 d . . . H41A H -0.0417 0.1557 0.4508 0.063 Uiso 1 1 calc R . . H41B H 0.0165 0.0973 0.4088 0.063 Uiso 1 1 calc R . . H41C H -0.0512 0.1342 0.3622 0.063 Uiso 1 1 calc R . . C42 C -0.0893(6) 0.3004(7) 0.3842(8) 0.032(3) Uani 1 1 d . . . H42A H -0.1038 0.2641 0.4273 0.038 Uiso 1 1 calc R . . H42B H -0.1053 0.3579 0.3963 0.038 Uiso 1 1 calc R . . N3 N -0.1262(5) 0.2726(7) 0.3157(6) 0.030(2) Uani 1 1 d . . . N4 N -0.1935(5) 0.2399(7) 0.3172(6) 0.032(2) Uani 1 1 d . . . C43 C -0.2138(10) 0.2391(18) 0.2410(9) 0.032(3) Uani 1 1 d . . . H43 H -0.2615 0.2292 0.2221 0.038 Uiso 1 1 calc R . . C44 C -0.1552(7) 0.2546(10) 0.1992(9) 0.044(3) Uani 1 1 d . . . H44 H -0.1524 0.2484 0.1453 0.053 Uiso 1 1 calc R . . C45 C -0.1032(8) 0.2792(8) 0.2418(7) 0.036(3) Uani 1 1 d . . . H45 H -0.0569 0.2985 0.2253 0.044 Uiso 1 1 calc R . . C46 C 0.2218(5) 0.2857(6) 0.3284(6) 0.0169(19) Uani 1 1 d . . . H46A H 0.2455 0.2501 0.3665 0.025 Uiso 1 1 calc R . . H46B H 0.2419 0.3422 0.3316 0.025 Uiso 1 1 calc R . . H46C H 0.2305 0.2630 0.2773 0.025 Uiso 1 1 calc R . . C47 C -0.0053(7) 0.4544(7) 0.3501(7) 0.030(3) Uani 1 1 d . . . H47A H 0.0237 0.4953 0.3784 0.046 Uiso 1 1 calc R . . H47B H -0.0540 0.4506 0.3727 0.046 Uiso 1 1 calc R . . H47C H -0.0094 0.4719 0.2967 0.046 Uiso 1 1 calc R . . C48 C 0.1455(6) 0.4411(6) 0.3034(6) 0.020(2) Uani 1 1 d . . . H48A H 0.1802 0.4580 0.3437 0.024 Uiso 1 1 calc R . . H48B H 0.1097 0.4868 0.2980 0.024 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.022(4) 0.030(5) 0.031(5) -0.015(4) 0.001(4) -0.009(4) N2 0.020(4) 0.031(5) 0.050(7) 0.003(4) 0.005(5) 0.000(4) C19 0.027(6) 0.030(6) 0.087(12) -0.035(7) 0.003(7) -0.009(5) C20 0.027(6) 0.030(6) 0.087(12) -0.035(7) 0.003(7) -0.009(5) C21 0.018(5) 0.067(9) 0.034(7) 0.035(6) 0.016(5) 0.026(6) Co1 0.0232(7) 0.0354(8) 0.0362(9) 0.0014(7) -0.0067(7) 0.0047(6) Br1 0.0368(7) 0.0298(6) 0.0665(10) -0.0010(6) -0.0071(7) 0.0023(5) Br2 0.0420(7) 0.0389(7) 0.0538(9) 0.0178(6) -0.0029(7) 0.0038(6) C1 0.010(5) 0.028(5) 0.024(6) -0.015(4) 0.001(4) 0.004(4) C2 0.010(5) 0.028(5) 0.024(6) -0.015(4) 0.001(4) 0.004(4) C3 0.025(5) 0.023(5) 0.014(5) 0.003(4) 0.011(4) -0.003(4) Br3 0.0181(6) 0.0718(10) 0.0336(7) -0.0128(6) 0.0084(5) -0.0234(5) C4 0.035(6) 0.011(4) 0.008(4) -0.001(3) 0.002(4) -0.002(4) C5 0.022(5) 0.012(4) 0.008(4) 0.003(3) 0.000(4) 0.000(4) C6 0.032(6) 0.062(8) 0.007(5) -0.005(5) 0.008(5) -0.030(5) C7 0.032(6) 0.062(8) 0.007(5) -0.005(5) 0.008(5) -0.030(5) C8 0.032(6) 0.062(8) 0.007(5) -0.005(5) 0.008(5) -0.030(5) C9 0.019(5) 0.016(4) 0.021(5) 0.001(4) 0.002(4) 0.004(4) C10 0.015(4) 0.023(4) 0.005(4) -0.002(3) 0.004(3) -0.004(3) C11 0.015(4) 0.016(4) 0.016(5) -0.002(4) 0.006(4) -0.005(3) C12 0.020(5) 0.023(5) 0.017(5) 0.004(4) -0.006(4) 0.001(4) C13 0.013(4) 0.019(4) 0.026(5) 0.001(4) -0.004(4) -0.003(4) C14 0.015(4) 0.011(4) 0.019(5) -0.009(3) 0.002(4) -0.001(3) C15 0.015(4) 0.011(4) 0.019(5) -0.009(3) 0.002(4) -0.001(3) C16 0.015(4) 0.011(4) 0.019(5) -0.009(3) 0.002(4) -0.001(3) C17 0.029(6) 0.021(5) 0.054(8) 0.002(5) -0.022(6) -0.002(4) C18 0.017(5) 0.022(5) 0.029(6) 0.012(4) -0.011(4) -0.010(4) C22 0.015(4) 0.010(4) 0.044(7) -0.001(4) -0.009(4) 0.001(3) C23 0.004(4) 0.022(5) 0.021(5) -0.003(4) -0.003(3) -0.001(3) C24 0.007(4) 0.013(4) 0.015(5) 0.000(3) -0.008(3) 0.003(3) C25 0.010(4) 0.017(4) 0.009(4) -0.001(3) -0.002(3) 0.008(3) C26 0.009(4) 0.009(4) 0.015(5) 0.005(3) 0.001(3) 0.005(3) C27 0.007(4) 0.019(4) 0.015(5) -0.006(4) 0.004(3) 0.004(3) Br4 0.0164(6) 0.0506(7) 0.0375(8) -0.0040(5) -0.0070(5) 0.0153(5) C28 0.005(4) 0.019(4) 0.026(6) -0.002(4) 0.002(4) 0.003(3) C29 0.013(4) 0.008(4) 0.016(5) 0.001(3) -0.004(3) 0.006(3) C30 0.013(4) 0.008(4) 0.016(5) 0.001(3) -0.004(3) 0.006(3) C31 0.030(6) 0.044(7) 0.025(7) -0.004(5) 0.007(5) 0.004(5) C32 0.036(6) 0.043(7) 0.018(6) -0.002(5) -0.006(5) 0.018(5) C33 0.008(4) 0.018(4) 0.022(5) -0.008(4) 0.005(3) 0.004(3) C34 0.008(4) 0.018(4) 0.022(5) -0.008(4) 0.005(3) 0.004(3) C35 0.033(6) 0.011(4) 0.009(5) -0.001(3) 0.013(4) -0.007(4) C36 0.028(5) 0.011(4) 0.030(6) 0.001(4) 0.011(4) -0.001(4) C37 0.007(4) 0.019(4) 0.031(6) -0.005(4) 0.005(4) 0.001(3) C38 0.016(5) 0.021(4) 0.012(4) 0.005(4) 0.008(4) 0.002(4) C39 0.016(5) 0.021(4) 0.012(4) 0.005(4) 0.008(4) 0.002(4) C40 0.015(4) 0.014(4) 0.004(4) -0.001(3) 0.005(3) -0.005(3) C41 0.046(8) 0.021(5) 0.058(9) 0.019(5) 0.033(7) 0.001(5) C42 0.011(4) 0.020(5) 0.065(9) 0.011(5) 0.019(5) 0.003(4) N3 0.014(4) 0.044(6) 0.031(6) 0.001(4) 0.004(4) -0.008(4) N4 0.010(4) 0.044(6) 0.043(6) 0.000(5) -0.004(4) 0.001(4) C43 0.011(4) 0.020(5) 0.065(9) 0.011(5) 0.019(5) 0.003(4) C44 0.036(7) 0.056(8) 0.039(7) 0.001(6) 0.007(6) -0.022(7) C45 0.054(8) 0.039(7) 0.016(6) -0.003(5) 0.010(5) -0.010(6) C46 0.013(4) 0.013(4) 0.024(5) 0.000(4) 0.003(4) 0.001(3) C47 0.033(6) 0.024(5) 0.034(6) 0.003(5) 0.023(5) 0.014(5) C48 0.027(5) 0.016(4) 0.017(5) -0.001(4) 0.002(4) -0.006(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 N1 C21 1.4200 . ? N1 N2 1.4200 . ? N1 C18 1.497(13) . ? N2 C19 1.4200 . ? N2 Co1 2.015(6) . ? C19 C20 1.4200 . ? C19 H19 0.9500 . ? C20 C21 1.4200 . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? Co1 N4 2.031(11) 4_454 ? Co1 Br1 2.370(2) . ? Co1 Br2 2.376(2) . ? C1 C2 1.369(13) . ? C1 C6 1.407(13) . ? C1 C48 1.561(14) . ? C2 C3 1.376(14) . ? C2 C7 1.559(15) . ? C3 C4 1.398(15) . ? C3 Br3 1.932(10) . ? C4 C5 1.394(14) . ? C4 C8 1.510(13) . ? C5 C6 1.357(12) . ? C5 C10 1.532(13) . ? C6 C9 1.572(13) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? 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 1.555(12) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.391(14) . ? C11 C16 1.437(14) . ? C12 C13 1.406(13) . ? C12 C17 1.525(14) . ? C13 C14 1.399(13) . ? C13 C18 1.494(13) . ? C14 C15 1.405(13) . ? C14 C22 1.555(12) . ? C15 C16 1.421(13) . ? C15 C24 1.519(12) . ? C16 C23 1.524(11) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.484(12) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C30 1.394(14) . ? C25 C26 1.441(11) . ? C26 C27 1.383(13) . ? C26 C31 1.453(15) . ? C27 C28 1.415(13) . ? C27 Br4 1.924(9) . ? C28 C29 1.428(12) . ? C28 C32 1.514(15) . ? C29 C30 1.443(14) . ? C29 C34 1.494(13) . ? C30 C33 1.496(14) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? 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 1.538(13) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C40 1.393(12) . ? C35 C36 1.410(15) . ? C36 C37 1.405(14) . ? C36 C41 1.524(14) . ? C37 C38 1.405(13) . ? C37 C42 1.516(13) . ? C38 C39 1.406(12) . ? C38 C47 1.502(13) . ? C39 C40 1.414(13) . ? C39 C48 1.528(13) . ? C40 C46 1.481(13) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 N3 1.448(18) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? N3 N4 1.342(13) . ? N3 C45 1.366(15) . ? N4 C43 1.386(19) . ? N4 Co1 2.031(11) 4_455 ? C43 C44 1.33(2) . ? C43 H43 0.9500 . ? C44 C45 1.28(2) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? 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 C21 N1 N2 108.0 . . ? C21 N1 C18 131.4(7) . . ? N2 N1 C18 119.8(7) . . ? N1 N2 C19 108.0 . . ? N1 N2 Co1 124.7(5) . . ? C19 N2 Co1 126.0(5) . . ? C20 C19 N2 108.0 . . ? C20 C19 H19 126.0 . . ? N2 C19 H19 126.0 . . ? C19 C20 C21 108.0 . . ? C19 C20 H20 126.0 . . ? C21 C20 H20 126.0 . . ? N1 C21 C20 108.0 . . ? N1 C21 H21 126.0 . . ? C20 C21 H21 126.0 . . ? N2 Co1 N4 105.6(4) . 4_454 ? N2 Co1 Br1 111.7(2) . . ? N4 Co1 Br1 105.5(3) 4_454 . ? N2 Co1 Br2 108.6(3) . . ? N4 Co1 Br2 114.4(3) 4_454 . ? Br1 Co1 Br2 111.03(10) . . ? C2 C1 C6 120.4(9) . . ? C2 C1 C48 120.2(9) . . ? C6 C1 C48 119.4(8) . . ? C1 C2 C3 117.1(9) . . ? C1 C2 C7 124.4(9) . . ? C3 C2 C7 118.5(9) . . ? C2 C3 C4 124.4(9) . . ? C2 C3 Br3 117.7(8) . . ? C4 C3 Br3 118.0(7) . . ? C5 C4 C3 116.3(9) . . ? C5 C4 C8 124.2(9) . . ? C3 C4 C8 119.4(9) . . ? C6 C5 C4 120.7(8) . . ? C6 C5 C10 121.3(8) . . ? C4 C5 C10 117.8(8) . . ? C5 C6 C1 120.9(8) . . ? C5 C6 C9 119.6(8) . . ? C1 C6 C9 119.4(8) . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 C11 118.0(8) . . ? C5 C10 H10A 107.8 . . ? C11 C10 H10A 107.8 . . ? C5 C10 H10B 107.8 . . ? C11 C10 H10B 107.8 . . ? H10A C10 H10B 107.1 . . ? C12 C11 C16 120.7(8) . . ? C12 C11 C10 122.2(9) . . ? C16 C11 C10 117.0(8) . . ? C11 C12 C13 119.3(9) . . ? C11 C12 C17 120.5(9) . . ? C13 C12 C17 119.6(9) . . ? C14 C13 C12 119.9(9) . . ? C14 C13 C18 120.2(8) . . ? C12 C13 C18 119.0(9) . . ? C13 C14 C15 122.4(8) . . ? C13 C14 C22 117.6(8) . . ? C15 C14 C22 119.7(8) . . ? C14 C15 C16 117.5(8) . . ? C14 C15 C24 121.4(8) . . ? C16 C15 C24 121.0(8) . . ? C15 C16 C11 119.9(8) . . ? C15 C16 C23 118.9(8) . . ? C11 C16 C23 120.9(8) . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 N1 107.8(9) . . ? C13 C18 H18A 110.1 . . ? N1 C18 H18A 110.1 . . ? C13 C18 H18B 110.1 . . ? N1 C18 H18B 110.1 . . ? H18A C18 H18B 108.5 . . ? C14 C22 H22A 109.5 . . ? C14 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C14 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C16 C23 H23A 109.5 . . ? C16 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C16 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C15 118.0(7) . . ? C25 C24 H24A 107.8 . . ? C15 C24 H24A 107.8 . . ? C25 C24 H24B 107.8 . . ? C15 C24 H24B 107.8 . . ? H24A C24 H24B 107.1 . . ? C30 C25 C26 118.9(8) . . ? C30 C25 C24 120.2(8) . . ? C26 C25 C24 120.7(8) . . ? C27 C26 C25 117.1(8) . . ? C27 C26 C31 120.9(9) . . ? C25 C26 C31 122.0(9) . . ? C26 C27 C28 126.5(8) . . ? C26 C27 Br4 117.9(6) . . ? C28 C27 Br4 115.6(7) . . ? C27 C28 C29 116.0(9) . . ? C27 C28 C32 122.5(8) . . ? C29 C28 C32 121.5(9) . . ? C28 C29 C30 118.8(9) . . ? C28 C29 C34 119.6(9) . . ? C30 C29 C34 121.3(8) . . ? C25 C30 C29 122.5(9) . . ? C25 C30 C33 119.6(9) . . ? C29 C30 C33 117.8(9) . . ? C26 C31 H31A 109.5 . . ? C26 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C26 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C28 C32 H32A 109.5 . . ? C28 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C28 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C29 C34 C35 118.5(8) . . ? C29 C34 H34A 107.7 . . ? C35 C34 H34A 107.7 . . ? C29 C34 H34B 107.7 . . ? C35 C34 H34B 107.7 . . ? H34A C34 H34B 107.1 . . ? C40 C35 C36 120.6(9) . . ? C40 C35 C34 117.7(9) . . ? C36 C35 C34 121.7(8) . . ? C37 C36 C35 119.6(9) . . ? C37 C36 C41 118.0(10) . . ? C35 C36 C41 122.4(9) . . ? C36 C37 C38 120.1(9) . . ? C36 C37 C42 118.5(9) . . ? C38 C37 C42 120.8(9) . . ? C37 C38 C39 119.8(9) . . ? C37 C38 C47 121.3(9) . . ? C39 C38 C47 118.9(9) . . ? C38 C39 C40 119.8(8) . . ? C38 C39 C48 120.0(8) . . ? C40 C39 C48 119.9(8) . . ? C35 C40 C39 119.5(8) . . ? C35 C40 C46 121.5(8) . . ? C39 C40 C46 118.9(8) . . ? C36 C41 H41A 109.5 . . ? C36 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C36 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N3 C42 C37 113.0(10) . . ? N3 C42 H42A 109.0 . . ? C37 C42 H42A 109.0 . . ? N3 C42 H42B 109.0 . . ? C37 C42 H42B 109.0 . . ? H42A C42 H42B 107.8 . . ? N4 N3 C45 109.5(11) . . ? N4 N3 C42 122.4(10) . . ? C45 N3 C42 128.0(10) . . ? N3 N4 C43 103.5(11) . . ? N3 N4 Co1 125.9(9) . 4_455 ? C43 N4 Co1 128.9(9) . 4_455 ? C44 C43 N4 108.2(14) . . ? C44 C43 H43 125.9 . . ? N4 C43 H43 125.9 . . ? C45 C44 C43 110.0(15) . . ? C45 C44 H44 125.0 . . ? C43 C44 H44 125.0 . . ? C44 C45 N3 107.4(12) . . ? C44 C45 H45 126.3 . . ? N3 C45 H45 126.3 . . ? C40 C46 H46A 109.5 . . ? C40 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C40 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C38 C47 H47A 109.5 . . ? C38 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C38 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C39 C48 C1 118.4(8) . . ? C39 C48 H48A 107.7 . . ? C1 C48 H48A 107.7 . . ? C39 C48 H48B 107.7 . . ? C1 C48 H48B 107.7 . . ? H48A C48 H48B 107.1 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.106 _refine_diff_density_min -1.343 _refine_diff_density_rms 0.305 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.518 0.298 0.160 303.3 87.9 2 0.982 0.298 0.660 303.6 87.5 3 0.018 0.702 0.160 303.6 86.8 4 0.482 0.702 0.660 303.6 88.0 _platon_squeeze_details ; ; # Attachment '_8-CoCl2_n.cif' data_e1470a _database_code_depnum_ccdc_archive 'CCDC 744819' #TrackingRef '_8-CoCl2_n.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H54 Br2 Cl2 Co N4' _chemical_formula_sum 'C48 H54 Br2 Cl2 Co N4' _chemical_formula_weight 976.60 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.0585(9) _cell_length_b 26.0298(18) _cell_length_c 16.2349(11) _cell_angle_alpha 90.00 _cell_angle_beta 101.517(2) _cell_angle_gamma 90.00 _cell_volume 5407.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6235 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 21.52 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.200 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2004 _exptl_absorpt_coefficient_mu 1.926 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3080 _exptl_absorpt_correction_T_max 0.9099 _exptl_absorpt_process_details sadabs _exptl_special_details ; Owing to large disorder of the solvent present in the cavities of this structure, the SQUEEZE command has been applied. WE observed some large Ueqmax so we fixed rhis atoms with identical thermal parameters ; _diffrn_ambient_temperature 173(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 42104 _diffrn_reflns_av_R_equivalents 0.0637 _diffrn_reflns_av_sigmaI/netI 0.1128 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 27.57 _reflns_number_total 12429 _reflns_number_gt 5871 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1031P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12429 _refine_ls_number_parameters 526 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1490 _refine_ls_R_factor_gt 0.0768 _refine_ls_wR_factor_ref 0.2146 _refine_ls_wR_factor_gt 0.1960 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 Co1 Co 0.77073(6) 0.23259(3) 0.82863(5) 0.0376(2) Uani 1 1 d . . 1 Cl1 Cl 0.74134(13) 0.25793(6) 0.95300(9) 0.0545(4) Uani 1 1 d . . 1 Cl2 Cl 0.92935(13) 0.20732(7) 0.81468(11) 0.0623(5) Uani 1 1 d . . 1 C1 C 0.5976(4) 0.11731(19) 0.1642(3) 0.0321(12) Uani 1 1 d . . 1 C2 C 0.5219(4) 0.0904(2) 0.1085(3) 0.0341(12) Uani 1 1 d . . 1 C3 C 0.4356(4) 0.0739(2) 0.1390(3) 0.0374(13) Uani 1 1 d . . 1 Br1 Br 0.32920(5) 0.03602(3) 0.06270(4) 0.0586(2) Uani 1 1 d . . 1 C4 C 0.4189(4) 0.0816(2) 0.2185(4) 0.0364(13) Uani 1 1 d . . 1 C5 C 0.4929(4) 0.1116(2) 0.2723(3) 0.0305(12) Uani 1 1 d . . 1 C6 C 0.5810(4) 0.13023(18) 0.2454(3) 0.0327(12) Uani 1 1 d . . 1 C7 C 0.5331(5) 0.0788(3) 0.0196(4) 0.0553(17) Uani 1 1 d . . 1 H7A H 0.6063 0.0710 0.0189 0.083 Uiso 1 1 calc R . 1 H7B H 0.5108 0.1088 -0.0161 0.083 Uiso 1 1 calc R . 1 H7C H 0.4894 0.0492 -0.0017 0.083 Uiso 1 1 calc R . 1 C8 C 0.3212(4) 0.0600(3) 0.2439(4) 0.0514(16) Uani 1 1 d . . 1 H8A H 0.3199 0.0704 0.3018 0.077 Uiso 1 1 calc R . 1 H8B H 0.3219 0.0224 0.2404 0.077 Uiso 1 1 calc R . 1 H8C H 0.2589 0.0734 0.2060 0.077 Uiso 1 1 calc R . 1 C9 C 0.6554(5) 0.1657(2) 0.3010(4) 0.0449(14) Uani 1 1 d . . 1 H9A H 0.6162 0.1881 0.3321 0.067 Uiso 1 1 calc R . 1 H9B H 0.6927 0.1867 0.2664 0.067 Uiso 1 1 calc R . 1 H9C H 0.7058 0.1454 0.3409 0.067 Uiso 1 1 calc R . 1 C10 C 0.4755(4) 0.1275(2) 0.3595(3) 0.0392(14) Uani 1 1 d . . 1 H10A H 0.4689 0.1654 0.3599 0.047 Uiso 1 1 calc R . 1 H10B H 0.4075 0.1131 0.3663 0.047 Uiso 1 1 calc R . 1 C11 C 0.5561(4) 0.1123(2) 0.4359(3) 0.0305(12) Uani 1 1 d . . 1 C12 C 0.5832(4) 0.1484(2) 0.5018(3) 0.0329(12) Uani 1 1 d . . 1 C13 C 0.6590(4) 0.1351(2) 0.5724(3) 0.0346(13) Uani 1 1 d . . 1 C14 C 0.7079(4) 0.0881(2) 0.5788(3) 0.0364(13) Uani 1 1 d . . 1 C15 C 0.6798(4) 0.05116(19) 0.5161(3) 0.0332(12) Uani 1 1 d . . 1 C16 C 0.6008(4) 0.06322(19) 0.4451(3) 0.0289(11) Uani 1 1 d . . 1 C17 C 0.5293(5) 0.2000(2) 0.4981(4) 0.0540(17) Uani 1 1 d . . 1 H17A H 0.5724 0.2260 0.4777 0.081 Uiso 1 1 calc R . 1 H17B H 0.5196 0.2094 0.5545 0.081 Uiso 1 1 calc R . 1 H17C H 0.4612 0.1979 0.4599 0.081 Uiso 1 1 calc R . 1 C18 C 0.6856(5) 0.1739(2) 0.6463(3) 0.0430(14) Uani 1 1 d . . 1 H18A H 0.7622 0.1772 0.6647 0.052 Uiso 1 1 calc R . 1 H18B H 0.6563 0.2082 0.6284 0.052 Uiso 1 1 calc R . 1 N1 N 0.6381(4) 0.15362(18) 0.7167(3) 0.0424(12) Uani 1 1 d . . 1 N2 N 0.6663(4) 0.17545(17) 0.7927(3) 0.0412(11) Uani 1 1 d . . 1 C19 C 0.5666(6) 0.1180(3) 0.7185(4) 0.083(3) Uani 1 1 d . . 1 H19 H 0.5337 0.0981 0.6716 0.100 Uiso 1 1 calc R . 1 C20 C 0.5476(7) 0.1140(3) 0.7961(4) 0.093(3) Uani 1 1 d . . 1 H20 H 0.5007 0.0911 0.8153 0.111 Uiso 1 1 calc R . 1 C21 C 0.6124(6) 0.1515(3) 0.8432(4) 0.0622(19) Uani 1 1 d . . 1 H21 H 0.6169 0.1585 0.9012 0.075 Uiso 1 1 calc R . 1 C22 C 0.7922(5) 0.0762(2) 0.6559(4) 0.0582(18) Uani 1 1 d . . 1 H22A H 0.7670 0.0494 0.6895 0.087 Uiso 1 1 calc R . 1 H22B H 0.8084 0.1073 0.6899 0.087 Uiso 1 1 calc R . 1 H22C H 0.8553 0.0641 0.6380 0.087 Uiso 1 1 calc R . 1 C23 C 0.5568(4) 0.0204(2) 0.3848(4) 0.0395(13) Uani 1 1 d . . 1 H23A H 0.4843 0.0284 0.3585 0.059 Uiso 1 1 calc R . 1 H23B H 0.5589 -0.0120 0.4158 0.059 Uiso 1 1 calc R . 1 H23C H 0.5986 0.0172 0.3413 0.059 Uiso 1 1 calc R . 1 C24 C 0.7299(5) -0.0015(2) 0.5242(4) 0.0409(14) Uani 1 1 d . . 1 H24A H 0.6775 -0.0259 0.5379 0.049 Uiso 1 1 calc R . 1 H24B H 0.7882 -0.0005 0.5736 0.049 Uiso 1 1 calc R . 1 C25 C 0.7728(4) -0.02490(19) 0.4514(3) 0.0346(13) Uani 1 1 d . . 1 C26 C 0.7435(4) -0.07428(19) 0.4250(4) 0.0399(14) Uani 1 1 d . . 1 C27 C 0.7852(5) -0.0948(2) 0.3604(4) 0.0507(17) Uani 1 1 d . . 1 Br2 Br 0.74803(8) -0.16202(3) 0.32286(6) 0.0973(4) Uani 1 1 d . . 1 C28 C 0.8538(5) -0.06782(19) 0.3164(4) 0.0482(16) Uani 1 1 d . . 1 C29 C 0.8805(4) -0.01703(18) 0.3463(4) 0.0379(13) Uani 1 1 d . . 1 C30 C 0.8431(4) 0.00306(18) 0.4133(3) 0.0325(12) Uani 1 1 d . . 1 C31 C 0.6732(5) -0.1074(2) 0.4660(4) 0.0522(17) Uani 1 1 d . . 1 H31A H 0.6654 -0.1412 0.4388 0.078 Uiso 1 1 calc R . 1 H31B H 0.6045 -0.0911 0.4599 0.078 Uiso 1 1 calc R . 1 H31C H 0.7041 -0.1115 0.5258 0.078 Uiso 1 1 calc R . 1 C32 C 0.8953(7) -0.0928(2) 0.2464(5) 0.085(3) Uani 1 1 d . . 1 H32A H 0.8384 -0.0969 0.1974 0.128 Uiso 1 1 calc R . 1 H32B H 0.9242 -0.1266 0.2648 0.128 Uiso 1 1 calc R . 1 H32C H 0.9502 -0.0712 0.2314 0.128 Uiso 1 1 calc R . 1 C33 C 0.8854(5) 0.0541(2) 0.4494(4) 0.0453(15) Uani 1 1 d . . 1 H33A H 0.9588 0.0573 0.4447 0.068 Uiso 1 1 calc R . 1 H33B H 0.8801 0.0560 0.5087 0.068 Uiso 1 1 calc R . 1 H33C H 0.8448 0.0820 0.4181 0.068 Uiso 1 1 calc R . 1 C34 C 0.9576(5) 0.0140(2) 0.3065(4) 0.0467(16) Uani 1 1 d . . 1 H34A H 1.0227 0.0178 0.3493 0.056 Uiso 1 1 calc R . 1 H34B H 0.9751 -0.0069 0.2602 0.056 Uiso 1 1 calc R . 1 C35 C 0.9257(4) 0.06709(18) 0.2714(3) 0.0342(13) Uani 1 1 d . . 1 C36 C 0.9998(4) 0.10683(19) 0.2902(3) 0.0326(12) Uani 1 1 d . . 1 C37 C 0.9739(4) 0.15548(18) 0.2556(3) 0.0307(12) Uani 1 1 d . . 1 C38 C 0.8760(4) 0.16524(18) 0.2054(3) 0.0324(12) Uani 1 1 d . . 1 C39 C 0.8018(4) 0.12626(18) 0.1889(3) 0.0299(12) Uani 1 1 d . . 1 C40 C 0.8300(4) 0.07612(18) 0.2187(3) 0.0334(13) Uani 1 1 d . . 1 C41 C 1.1055(4) 0.0972(2) 0.3441(4) 0.0462(15) Uani 1 1 d . . 1 H41A H 1.0984 0.0916 0.4023 0.069 Uiso 1 1 calc R . 1 H41B H 1.1506 0.1271 0.3415 0.069 Uiso 1 1 calc R . 1 H41C H 1.1368 0.0668 0.3235 0.069 Uiso 1 1 calc R . 1 C42 C 1.0566(4) 0.1973(2) 0.2707(3) 0.0370(13) Uani 1 1 d . . 1 H42A H 1.0224 0.2312 0.2597 0.044 Uiso 1 1 calc R . 1 H42B H 1.0929 0.1964 0.3304 0.044 Uiso 1 1 calc R . 1 N3 N 1.1336(3) 0.19123(15) 0.2171(3) 0.0339(10) Uani 1 1 d . . 1 N4 N 1.2297(4) 0.21220(16) 0.2410(3) 0.0385(11) Uani 1 1 d . . 1 C43 C 1.2799(5) 0.1998(2) 0.1800(4) 0.0433(15) Uani 1 1 d . . 1 H43 H 1.3501 0.2090 0.1792 0.052 Uiso 1 1 calc R . 1 C44 C 1.2174(5) 0.1723(2) 0.1195(4) 0.0530(17) Uani 1 1 d . . 1 H44 H 1.2347 0.1596 0.0691 0.064 Uiso 1 1 calc R . 1 C45 C 1.1248(5) 0.1663(2) 0.1446(4) 0.0496(16) Uani 1 1 d . . 1 H45 H 1.0655 0.1478 0.1160 0.060 Uiso 1 1 calc R . 1 C46 C 0.8509(5) 0.2177(2) 0.1651(5) 0.0585(18) Uani 1 1 d . . 1 H46A H 0.9106 0.2408 0.1827 0.088 Uiso 1 1 calc R . 1 H46B H 0.7893 0.2320 0.1828 0.088 Uiso 1 1 calc R . 1 H46C H 0.8366 0.2142 0.1037 0.088 Uiso 1 1 calc R . 1 C47 C 0.7570(5) 0.03121(19) 0.1872(4) 0.0442(15) Uani 1 1 d . . 1 H47A H 0.7066 0.0268 0.2241 0.066 Uiso 1 1 calc R . 1 H47B H 0.7981 -0.0003 0.1875 0.066 Uiso 1 1 calc R . 1 H47C H 0.7194 0.0383 0.1298 0.066 Uiso 1 1 calc R . 1 C48 C 0.6963(4) 0.1380(2) 0.1361(3) 0.0369(13) Uani 1 1 d . . 1 H48A H 0.6955 0.1247 0.0788 0.044 Uiso 1 1 calc R . 1 H48B H 0.6896 0.1758 0.1315 0.044 Uiso 1 1 calc R . 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0378(5) 0.0379(4) 0.0380(4) -0.0078(3) 0.0096(3) 0.0053(3) Cl1 0.0605(10) 0.0628(10) 0.0401(8) -0.0134(7) 0.0100(8) 0.0049(8) Cl2 0.0414(9) 0.0754(11) 0.0704(11) -0.0105(9) 0.0119(8) 0.0148(8) C1 0.037(3) 0.034(3) 0.029(3) 0.009(2) 0.014(3) 0.013(2) C2 0.031(3) 0.040(3) 0.030(3) 0.002(2) 0.004(2) 0.003(2) C3 0.032(3) 0.040(3) 0.041(3) -0.001(3) 0.009(3) 0.002(2) Br1 0.0418(4) 0.0756(5) 0.0576(4) -0.0226(3) 0.0081(3) -0.0106(3) C4 0.022(3) 0.043(3) 0.046(3) 0.008(3) 0.012(3) 0.007(2) C5 0.023(3) 0.039(3) 0.029(3) 0.001(2) 0.004(2) 0.010(2) C6 0.032(3) 0.026(3) 0.038(3) 0.007(2) 0.002(3) 0.003(2) C7 0.045(4) 0.072(4) 0.049(4) -0.004(3) 0.009(3) -0.003(3) C8 0.029(3) 0.076(4) 0.053(4) -0.004(3) 0.016(3) -0.007(3) C9 0.045(4) 0.043(3) 0.044(3) -0.007(3) 0.003(3) 0.005(3) C10 0.024(3) 0.055(3) 0.041(3) -0.005(3) 0.014(3) 0.005(3) C11 0.027(3) 0.041(3) 0.024(3) 0.003(2) 0.009(2) 0.010(2) C12 0.032(3) 0.037(3) 0.033(3) -0.003(2) 0.014(3) -0.001(2) C13 0.035(3) 0.041(3) 0.030(3) -0.002(2) 0.013(3) 0.005(2) C14 0.042(3) 0.045(3) 0.022(3) 0.008(2) 0.005(2) -0.005(3) C15 0.034(3) 0.034(3) 0.033(3) 0.014(2) 0.012(3) -0.002(2) C16 0.026(3) 0.036(3) 0.026(3) -0.002(2) 0.010(2) 0.003(2) C17 0.076(5) 0.041(3) 0.049(4) -0.012(3) 0.021(3) 0.016(3) C18 0.052(4) 0.045(3) 0.032(3) 0.002(3) 0.009(3) -0.006(3) N1 0.053(3) 0.047(3) 0.029(3) -0.007(2) 0.013(2) -0.011(2) N2 0.047(3) 0.045(3) 0.032(3) 0.001(2) 0.007(2) -0.004(2) C19 0.100(6) 0.110(6) 0.043(4) -0.026(4) 0.025(4) -0.066(5) C20 0.127(8) 0.115(7) 0.050(4) -0.013(5) 0.052(5) -0.058(6) C21 0.079(5) 0.063(4) 0.051(4) -0.010(3) 0.029(4) -0.034(4) C22 0.061(5) 0.054(4) 0.049(4) 0.005(3) -0.013(3) 0.007(3) C23 0.037(3) 0.032(3) 0.049(3) -0.006(3) 0.008(3) -0.004(2) C24 0.047(4) 0.034(3) 0.043(3) 0.005(3) 0.011(3) 0.001(3) C25 0.034(3) 0.030(3) 0.041(3) 0.021(2) 0.010(3) 0.008(2) C26 0.046(4) 0.030(3) 0.048(3) 0.015(3) 0.020(3) 0.011(3) C27 0.069(5) 0.022(3) 0.070(4) 0.007(3) 0.035(4) -0.001(3) Br2 0.1366(9) 0.0315(4) 0.1465(9) -0.0184(4) 0.0827(7) -0.0233(4) C28 0.053(4) 0.022(3) 0.078(4) 0.009(3) 0.033(3) 0.005(3) C29 0.033(3) 0.020(2) 0.063(4) 0.007(3) 0.018(3) 0.004(2) C30 0.026(3) 0.022(2) 0.050(3) 0.011(2) 0.009(3) 0.008(2) C31 0.049(4) 0.033(3) 0.077(5) 0.008(3) 0.019(3) -0.006(3) C32 0.122(7) 0.030(3) 0.133(7) -0.001(4) 0.095(6) 0.002(4) C33 0.040(4) 0.035(3) 0.062(4) 0.007(3) 0.013(3) -0.002(3) C34 0.039(3) 0.030(3) 0.080(4) 0.013(3) 0.034(3) 0.010(3) C35 0.038(3) 0.027(3) 0.044(3) 0.004(2) 0.024(3) 0.001(2) C36 0.028(3) 0.033(3) 0.041(3) 0.007(2) 0.017(3) 0.004(2) C37 0.027(3) 0.027(3) 0.043(3) 0.003(2) 0.021(3) 0.001(2) C38 0.039(3) 0.025(3) 0.037(3) 0.006(2) 0.017(3) 0.000(2) C39 0.033(3) 0.029(3) 0.031(3) 0.003(2) 0.015(2) 0.003(2) C40 0.037(3) 0.023(3) 0.045(3) -0.002(2) 0.018(3) -0.007(2) C41 0.028(3) 0.060(4) 0.051(4) 0.019(3) 0.010(3) -0.008(3) C42 0.032(3) 0.037(3) 0.046(3) -0.003(3) 0.017(3) 0.002(2) N3 0.040(3) 0.026(2) 0.040(3) 0.000(2) 0.018(2) -0.005(2) N4 0.038(3) 0.035(2) 0.046(3) 0.004(2) 0.017(2) -0.005(2) C43 0.045(4) 0.038(3) 0.058(4) 0.003(3) 0.036(3) 0.003(3) C44 0.065(5) 0.051(4) 0.056(4) -0.007(3) 0.042(4) -0.002(3) C45 0.071(5) 0.037(3) 0.043(4) -0.007(3) 0.016(3) -0.014(3) C46 0.053(4) 0.034(3) 0.089(5) 0.026(3) 0.013(4) -0.003(3) C47 0.053(4) 0.027(3) 0.058(4) -0.005(3) 0.022(3) -0.006(3) C48 0.030(3) 0.049(3) 0.033(3) 0.018(3) 0.009(2) 0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N4 2.018(5) 4_566 ? Co1 N2 2.023(5) . ? Co1 Cl2 2.2275(17) . ? Co1 Cl1 2.2291(16) . ? C1 C2 1.390(7) . ? C1 C6 1.419(7) . ? C1 C48 1.547(7) . ? C2 C3 1.387(7) . ? C2 C7 1.509(8) . ? C3 C4 1.365(7) . ? C3 Br1 1.937(6) . ? C4 C5 1.404(7) . ? C4 C8 1.525(7) . ? C5 C6 1.396(7) . ? C5 C10 1.534(7) . ? C6 C9 1.504(7) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? 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 1.511(7) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C16 1.399(7) . ? C11 C12 1.415(7) . ? C12 C13 1.401(7) . ? C12 C17 1.512(7) . ? C13 C14 1.374(7) . ? C13 C18 1.554(7) . ? C14 C15 1.394(7) . ? C14 C22 1.525(8) . ? C15 C16 1.421(7) . ? C15 C24 1.514(7) . ? C16 C23 1.518(7) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 N1 1.501(7) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? N1 C19 1.321(8) . ? N1 N2 1.342(6) . ? N2 C21 1.337(7) . ? C19 C20 1.335(9) . ? C19 H19 0.9500 . ? C20 C21 1.411(10) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.531(7) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.384(7) . ? C25 C30 1.407(7) . ? C26 C27 1.383(8) . ? C26 C31 1.508(7) . ? C27 C28 1.435(7) . ? C27 Br2 1.885(5) . ? C28 C29 1.427(7) . ? C28 C32 1.500(8) . ? C29 C30 1.381(7) . ? C29 C34 1.531(7) . ? C30 C33 1.511(7) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? 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 1.522(7) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C40 1.387(7) . ? C35 C36 1.407(7) . ? C36 C37 1.399(7) . ? C36 C41 1.501(7) . ? C37 C38 1.395(7) . ? C37 C42 1.519(7) . ? C38 C39 1.392(7) . ? C38 C46 1.522(7) . ? C39 C40 1.415(7) . ? C39 C48 1.501(7) . ? C40 C47 1.531(7) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 N3 1.463(6) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? N3 C45 1.329(7) . ? N3 N4 1.352(6) . ? N4 C43 1.332(6) . ? N4 Co1 2.018(5) 4_665 ? C43 C44 1.351(9) . ? C43 H43 0.9500 . ? C44 C45 1.361(8) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Co1 N2 104.57(18) 4_566 . ? N4 Co1 Cl2 105.08(14) 4_566 . ? N2 Co1 Cl2 109.92(14) . . ? N4 Co1 Cl1 111.00(13) 4_566 . ? N2 Co1 Cl1 104.49(14) . . ? Cl2 Co1 Cl1 120.75(7) . . ? C2 C1 C6 120.3(5) . . ? C2 C1 C48 120.6(4) . . ? C6 C1 C48 118.9(5) . . ? C3 C2 C1 116.5(5) . . ? C3 C2 C7 121.4(5) . . ? C1 C2 C7 122.1(5) . . ? C4 C3 C2 126.0(5) . . ? C4 C3 Br1 116.7(4) . . ? C2 C3 Br1 117.3(4) . . ? C3 C4 C5 116.7(5) . . ? C3 C4 C8 120.2(5) . . ? C5 C4 C8 123.0(5) . . ? C6 C5 C4 120.4(5) . . ? C6 C5 C10 118.6(5) . . ? C4 C5 C10 120.9(4) . . ? C5 C6 C1 119.8(5) . . ? C5 C6 C9 120.0(5) . . ? C1 C6 C9 120.2(5) . . ? C11 C10 C5 118.6(4) . . ? C11 C10 H10A 107.7 . . ? C5 C10 H10A 107.7 . . ? C11 C10 H10B 107.7 . . ? C5 C10 H10B 107.7 . . ? H10A C10 H10B 107.1 . . ? C16 C11 C12 119.3(5) . . ? C16 C11 C10 122.3(5) . . ? C12 C11 C10 118.4(5) . . ? C13 C12 C11 119.0(5) . . ? C13 C12 C17 119.9(5) . . ? C11 C12 C17 121.1(5) . . ? C14 C13 C12 121.6(5) . . ? C14 C13 C18 119.5(5) . . ? C12 C13 C18 118.9(5) . . ? C13 C14 C15 120.5(5) . . ? C13 C14 C22 119.4(5) . . ? C15 C14 C22 120.1(5) . . ? C14 C15 C16 118.9(5) . . ? C14 C15 C24 121.0(5) . . ? C16 C15 C24 120.1(5) . . ? C11 C16 C15 120.5(5) . . ? C11 C16 C23 120.3(5) . . ? C15 C16 C23 118.8(5) . . ? N1 C18 C13 107.2(4) . . ? N1 C18 H18A 110.3 . . ? C13 C18 H18A 110.3 . . ? N1 C18 H18B 110.3 . . ? C13 C18 H18B 110.3 . . ? H18A C18 H18B 108.5 . . ? C19 N1 N2 110.0(5) . . ? C19 N1 C18 131.7(5) . . ? N2 N1 C18 118.2(4) . . ? C21 N2 N1 106.5(5) . . ? C21 N2 Co1 125.0(4) . . ? N1 N2 Co1 128.4(3) . . ? N1 C19 C20 109.9(6) . . ? N1 C19 H19 125.0 . . ? C20 C19 H19 125.0 . . ? C19 C20 C21 104.7(6) . . ? C19 C20 H20 127.7 . . ? C21 C20 H20 127.7 . . ? N2 C21 C20 108.8(6) . . ? N2 C21 H21 125.6 . . ? C20 C21 H21 125.6 . . ? C15 C24 C25 120.8(4) . . ? C15 C24 H24A 107.1 . . ? C25 C24 H24A 107.1 . . ? C15 C24 H24B 107.1 . . ? C25 C24 H24B 107.1 . . ? H24A C24 H24B 106.8 . . ? C26 C25 C30 120.5(5) . . ? C26 C25 C24 119.1(4) . . ? C30 C25 C24 120.3(5) . . ? C27 C26 C25 117.9(5) . . ? C27 C26 C31 118.7(5) . . ? C25 C26 C31 123.3(5) . . ? C26 C27 C28 124.6(5) . . ? C26 C27 Br2 119.3(4) . . ? C28 C27 Br2 116.1(4) . . ? C29 C28 C27 114.7(5) . . ? C29 C28 C32 123.9(5) . . ? C27 C28 C32 121.3(5) . . ? C30 C29 C28 121.2(5) . . ? C30 C29 C34 120.0(5) . . ? C28 C29 C34 118.7(5) . . ? C29 C30 C25 121.0(5) . . ? C29 C30 C33 118.6(5) . . ? C25 C30 C33 120.3(5) . . ? C35 C34 C29 118.9(4) . . ? C35 C34 H34A 107.6 . . ? C29 C34 H34A 107.6 . . ? C35 C34 H34B 107.6 . . ? C29 C34 H34B 107.6 . . ? H34A C34 H34B 107.0 . . ? C40 C35 C36 120.3(5) . . ? C40 C35 C34 122.0(5) . . ? C36 C35 C34 117.5(5) . . ? C37 C36 C35 118.6(5) . . ? C37 C36 C41 120.3(5) . . ? C35 C36 C41 121.1(5) . . ? C38 C37 C36 121.3(5) . . ? C38 C37 C42 120.2(4) . . ? C36 C37 C42 118.4(5) . . ? C39 C38 C37 120.1(4) . . ? C39 C38 C46 119.3(5) . . ? C37 C38 C46 120.6(5) . . ? C38 C39 C40 118.9(5) . . ? C38 C39 C48 119.1(4) . . ? C40 C39 C48 121.9(5) . . ? C35 C40 C39 120.5(5) . . ? C35 C40 C47 120.1(5) . . ? C39 C40 C47 119.2(5) . . ? N3 C42 C37 112.2(4) . . ? N3 C42 H42A 109.2 . . ? C37 C42 H42A 109.2 . . ? N3 C42 H42B 109.2 . . ? C37 C42 H42B 109.2 . . ? H42A C42 H42B 107.9 . . ? C45 N3 N4 111.2(5) . . ? C45 N3 C42 129.1(5) . . ? N4 N3 C42 119.6(4) . . ? C43 N4 N3 104.8(4) . . ? C43 N4 Co1 126.6(4) . 4_665 ? N3 N4 Co1 126.2(3) . 4_665 ? N4 C43 C44 110.7(5) . . ? N4 C43 H43 124.7 . . ? C44 C43 H43 124.7 . . ? C43 C44 C45 106.7(5) . . ? C43 C44 H44 126.6 . . ? C45 C44 H44 126.6 . . ? N3 C45 C44 106.5(6) . . ? N3 C45 H45 126.7 . . ? C44 C45 H45 126.7 . . ? C38 C46 H46A 109.5 . . ? C38 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C38 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C39 C48 C1 118.9(4) . . ? C39 C48 H48A 107.6 . . ? C1 C48 H48A 107.6 . . ? C39 C48 H48B 107.6 . . ? C1 C48 H48B 107.6 . . ? H48A C48 H48B 107.0 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.57 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.248 _refine_diff_density_min -1.099 _refine_diff_density_rms 0.107 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 0.000 708.9 225.4 2 0.500 0.500 0.500 708.2 226.0 _platon_squeeze_details ; ; # Attachment '_8-ZnBr2_n.cif' data_e1451a _database_code_depnum_ccdc_archive 'CCDC 744820' #TrackingRef '_8-ZnBr2_n.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H54 Br4 N4 Zn' _chemical_formula_sum 'C48 H54 Br4 N4 Zn' _chemical_formula_weight 1071.96 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab' 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' '-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 21.8030(10) _cell_length_b 19.3128(9) _cell_length_c 33.4302(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 14076.7(11) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4573 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 18.86 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.012 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4320 _exptl_absorpt_coefficient_mu 2.644 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7250 _exptl_absorpt_correction_T_max 0.7779 _exptl_absorpt_process_details sadabs _exptl_special_details ; Owing to large disorder of the solvent present in the cavities of this structure, the SQUEEZE command has been applied Because of the floppiness of the phenyl ring C25 C26 C27 C28 C29 C30 we used a rigid-group refinement. Because of the poor diffraction powder the Ratio Observed / Unique Reflections is Low .... 32 Perc. Because of the flopiness of two atoms C6 C7 , their thermal parameters were fixed ; _diffrn_ambient_temperature 173(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 130795 _diffrn_reflns_av_R_equivalents 0.0845 _diffrn_reflns_av_sigmaI/netI 0.2039 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 1.22 _diffrn_reflns_theta_max 27.59 _reflns_number_total 16242 _reflns_number_gt 5178 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+0.1200P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16242 _refine_ls_number_parameters 502 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2001 _refine_ls_R_factor_gt 0.0867 _refine_ls_wR_factor_ref 0.1911 _refine_ls_wR_factor_gt 0.1729 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.006 _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 C25 C 1.0951(2) 0.5892(3) 0.39573(12) 0.043(2) Uani 1 1 d G . . C26 C 1.1164(2) 0.5435(2) 0.36672(19) 0.042(2) Uani 1 1 d G . . C27 C 1.1260(2) 0.5666(3) 0.32783(16) 0.036(2) Uani 1 1 d G . . C28 C 1.1143(2) 0.6352(3) 0.31795(12) 0.046(2) Uani 1 1 d G . . C29 C 1.0931(2) 0.6809(2) 0.34695(17) 0.046(2) Uani 1 1 d G . . C30 C 1.0834(2) 0.6578(3) 0.38585(14) 0.039(2) Uani 1 1 d G . . Zn1 Zn 0.71634(4) 0.38034(4) 0.24969(3) 0.0412(2) Uani 1 1 d . . . Br1 Br 0.63270(5) 0.31797(5) 0.22376(3) 0.0700(3) Uani 1 1 d . . . Br2 Br 0.80208(4) 0.32173(5) 0.27588(3) 0.0576(3) Uani 1 1 d . . . C1 C 0.8351(3) 0.6734(4) 0.3494(2) 0.0330(19) Uani 1 1 d . . . C2 C 0.8119(3) 0.6282(4) 0.3220(2) 0.035(2) Uani 1 1 d . . . C3 C 0.8033(3) 0.5631(5) 0.3335(2) 0.045(3) Uani 1 1 d . . . C4 C 0.8143(4) 0.5352(4) 0.3710(3) 0.049(2) Uani 1 1 d . . . C5 C 0.8380(3) 0.5837(4) 0.40090(19) 0.0243(17) Uani 1 1 d . . . C6 C 0.8468(3) 0.6527(4) 0.3894(2) 0.0325(19) Uani 1 1 d . . . C7 C 0.7970(4) 0.6506(4) 0.2789(2) 0.049 Uani 1 1 d . . . H7A H 0.8351 0.6620 0.2648 0.073 Uiso 1 1 calc R . . H7B H 0.7703 0.6914 0.2795 0.073 Uiso 1 1 calc R . . H7C H 0.7761 0.6127 0.2650 0.073 Uiso 1 1 calc R . . C8 C 0.7787(4) 0.5071(4) 0.3034(2) 0.049 Uani 1 1 d . . . H8A H 0.7919 0.5191 0.2759 0.059 Uiso 1 1 calc R . . H8B H 0.7963 0.4614 0.3102 0.059 Uiso 1 1 calc R . . N1 N 0.7117(3) 0.5029(3) 0.30463(18) 0.0318(16) Uani 1 1 d . . . N2 N 0.6805(3) 0.4468(3) 0.29000(19) 0.0458(19) Uani 1 1 d . . . C9 C 0.6199(4) 0.4594(5) 0.2979(2) 0.048(2) Uani 1 1 d . . . H9 H 0.5872 0.4297 0.2903 0.057 Uiso 1 1 calc R . . C10 C 0.6127(4) 0.5182(5) 0.3176(3) 0.056(3) Uani 1 1 d . . . H10 H 0.5748 0.5370 0.3265 0.067 Uiso 1 1 calc R . . C11 C 0.6692(4) 0.5473(5) 0.3229(2) 0.062(3) Uani 1 1 d . . . H11 H 0.6780 0.5896 0.3363 0.075 Uiso 1 1 calc R . . C12 C 0.8027(4) 0.4610(4) 0.3845(2) 0.045(2) Uani 1 1 d . . . H12A H 0.8415 0.4353 0.3846 0.068 Uiso 1 1 calc R . . H12B H 0.7738 0.4387 0.3661 0.068 Uiso 1 1 calc R . . H12C H 0.7853 0.4612 0.4115 0.068 Uiso 1 1 calc R . . C13 C 0.8627(4) 0.7076(4) 0.42032(19) 0.040(2) Uani 1 1 d . . . H13A H 0.8519 0.6908 0.4471 0.060 Uiso 1 1 calc R . . H13B H 0.8397 0.7501 0.4146 0.060 Uiso 1 1 calc R . . H13C H 0.9068 0.7174 0.4192 0.060 Uiso 1 1 calc R . . C14 C 0.8508(3) 0.5604(4) 0.4434(2) 0.047(2) Uani 1 1 d . . . H14A H 0.8181 0.5799 0.4606 0.057 Uiso 1 1 calc R . . H14B H 0.8462 0.5095 0.4441 0.057 Uiso 1 1 calc R . . C15 C 0.9105(4) 0.5775(4) 0.4625(2) 0.0306(19) Uani 1 1 d . . . C16 C 0.9117(4) 0.6097(4) 0.4991(2) 0.043(2) Uani 1 1 d . . . C17 C 0.9719(4) 0.6253(4) 0.51666(19) 0.041(2) Uani 1 1 d . . . Br3 Br 0.97297(5) 0.66922(5) 0.56890(2) 0.0666(3) Uani 1 1 d . . . C18 C 1.0275(4) 0.6091(4) 0.4984(2) 0.043(2) Uani 1 1 d . . . C19 C 1.0239(4) 0.5802(4) 0.4606(2) 0.035(2) Uani 1 1 d . . . C20 C 0.9669(4) 0.5620(4) 0.4444(2) 0.042(2) Uani 1 1 d . . . C21 C 0.8476(4) 0.6333(6) 0.5200(2) 0.092(4) Uani 1 1 d . . . H21A H 0.8508 0.6816 0.5287 0.138 Uiso 1 1 calc R . . H21B H 0.8393 0.6037 0.5432 0.138 Uiso 1 1 calc R . . H21C H 0.8141 0.6288 0.5007 0.138 Uiso 1 1 calc R . . C22 C 1.0851(4) 0.6295(5) 0.5223(2) 0.069(3) Uani 1 1 d . . . H22A H 1.0916 0.6795 0.5202 0.104 Uiso 1 1 calc R . . H22B H 1.1208 0.6050 0.5115 0.104 Uiso 1 1 calc R . . H22C H 1.0795 0.6168 0.5505 0.104 Uiso 1 1 calc R . . C23 C 0.9657(4) 0.5217(3) 0.40533(19) 0.0364(19) Uani 1 1 d . . . H23A H 0.9992 0.4879 0.4051 0.055 Uiso 1 1 calc R . . H23B H 0.9706 0.5537 0.3828 0.055 Uiso 1 1 calc R . . H23C H 0.9264 0.4974 0.4028 0.055 Uiso 1 1 calc R . . C24 C 1.0839(3) 0.5636(4) 0.4404(2) 0.037(2) Uani 1 1 d . . . H24A H 1.0888 0.5127 0.4407 0.045 Uiso 1 1 calc R . . H24B H 1.1172 0.5831 0.4571 0.045 Uiso 1 1 calc R . . C31 C 1.1332(4) 0.4686(4) 0.3764(2) 0.060(3) Uani 1 1 d . . . H31A H 1.1754 0.4667 0.3864 0.090 Uiso 1 1 calc R . . H31B H 1.1297 0.4404 0.3522 0.090 Uiso 1 1 calc R . . H31C H 1.1052 0.4507 0.3969 0.090 Uiso 1 1 calc R . . C32 C 1.1526(3) 0.5214(5) 0.2972(2) 0.048(2) Uani 1 1 d . . . H32A H 1.1479 0.5436 0.2707 0.058 Uiso 1 1 calc R . . H32B H 1.1297 0.4771 0.2967 0.058 Uiso 1 1 calc R . . C33 C 0.8090(4) 0.4547(5) 0.1977(2) 0.057(3) Uani 1 1 d . . . H33 H 0.8397 0.4211 0.2031 0.068 Uiso 1 1 calc R . . N3 N 0.7209(3) 0.5062(4) 0.19537(18) 0.0435(19) Uani 1 1 d . . . N4 N 0.7481(3) 0.4495(3) 0.21016(17) 0.0372(17) Uani 1 1 d . . . C34 C 0.8194(5) 0.5175(6) 0.1756(3) 0.077(3) Uani 1 1 d . . . H34 H 0.8569 0.5329 0.1641 0.093 Uiso 1 1 calc R . . C35 C 0.7583(4) 0.5539(6) 0.1747(3) 0.073(3) Uani 1 1 d . . . H35 H 0.7478 0.5973 0.1632 0.088 Uiso 1 1 calc R . . C36 C 1.0686(3) 0.7117(4) 0.4189(2) 0.054(3) Uani 1 1 d . . . H36A H 1.0241 0.7188 0.4203 0.081 Uiso 1 1 calc R . . H36B H 1.0888 0.7557 0.4126 0.081 Uiso 1 1 calc R . . H36C H 1.0835 0.6947 0.4447 0.081 Uiso 1 1 calc R . . C37 C 1.1261(4) 0.6606(4) 0.2762(2) 0.064(3) Uani 1 1 d . . . H37A H 1.0980 0.6376 0.2576 0.096 Uiso 1 1 calc R . . H37B H 1.1686 0.6501 0.2686 0.096 Uiso 1 1 calc R . . H37C H 1.1196 0.7108 0.2750 0.096 Uiso 1 1 calc R . . C38 C 1.0788(3) 0.7555(4) 0.3381(2) 0.049(2) Uani 1 1 d . . . H38A H 1.0838 0.7619 0.3089 0.059 Uiso 1 1 calc R . . H38B H 1.1112 0.7835 0.3511 0.059 Uiso 1 1 calc R . . C39 C 1.0192(4) 0.8531(4) 0.3693(2) 0.036(2) Uani 1 1 d . . . C40 C 0.9612(4) 0.8791(3) 0.38146(19) 0.0324(18) Uani 1 1 d . . . Br4 Br 0.95977(5) 0.96292(5) 0.41089(3) 0.0648(3) Uani 1 1 d . . . C41 C 0.9059(3) 0.8491(4) 0.3732(2) 0.0313(19) Uani 1 1 d . . . C42 C 0.9063(3) 0.7865(4) 0.3502(2) 0.0314(19) Uani 1 1 d . . . C43 C 0.9632(4) 0.7572(4) 0.3401(2) 0.045(2) Uani 1 1 d . . . C44 C 1.0171(3) 0.7883(4) 0.3496(2) 0.033(2) Uani 1 1 d . . . C45 C 1.0737(4) 0.8933(4) 0.3803(3) 0.064(3) Uani 1 1 d . . . H45A H 1.0892 0.8772 0.4062 0.096 Uiso 1 1 calc R . . H45B H 1.0628 0.9424 0.3822 0.096 Uiso 1 1 calc R . . H45C H 1.1054 0.8871 0.3598 0.096 Uiso 1 1 calc R . . C46 C 0.8456(3) 0.8830(4) 0.3887(2) 0.041(2) Uani 1 1 d . . . H46A H 0.8103 0.8596 0.3766 0.062 Uiso 1 1 calc R . . H46B H 0.8451 0.9321 0.3813 0.062 Uiso 1 1 calc R . . H46C H 0.8436 0.8786 0.4179 0.062 Uiso 1 1 calc R . . C47 C 0.9639(4) 0.6926(4) 0.3092(2) 0.047(2) Uani 1 1 d . . . H47A H 0.9613 0.6491 0.3242 0.070 Uiso 1 1 calc R . . H47B H 1.0020 0.6934 0.2936 0.070 Uiso 1 1 calc R . . H47C H 0.9288 0.6962 0.2910 0.070 Uiso 1 1 calc R . . C48 C 0.8458(3) 0.7519(4) 0.33853(19) 0.0299(19) Uani 1 1 d . . . H48A H 0.8411 0.7566 0.3092 0.036 Uiso 1 1 calc R . . H48B H 0.8123 0.7789 0.3510 0.036 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 C25 0.025(5) 0.051(6) 0.053(6) 0.025(5) -0.012(4) 0.017(4) C26 0.024(5) 0.034(5) 0.069(7) -0.016(5) -0.011(4) 0.007(4) C27 0.038(5) 0.031(5) 0.039(5) -0.012(4) -0.009(4) 0.006(4) C28 0.013(4) 0.061(7) 0.064(6) 0.026(5) 0.019(4) 0.013(4) C29 0.025(5) 0.028(5) 0.084(7) 0.005(5) -0.009(5) 0.010(4) C30 0.022(4) 0.080(7) 0.015(4) 0.008(5) 0.000(3) -0.009(4) Zn1 0.0330(5) 0.0368(5) 0.0539(6) -0.0036(6) -0.0046(5) -0.0032(5) Br1 0.0601(7) 0.0623(7) 0.0877(8) -0.0156(6) -0.0141(6) -0.0240(6) Br2 0.0366(5) 0.0386(5) 0.0975(8) 0.0068(5) -0.0070(5) 0.0043(4) C1 0.015(4) 0.045(5) 0.039(5) 0.000(4) 0.005(4) 0.013(4) C2 0.022(5) 0.028(5) 0.055(6) 0.006(4) -0.004(4) 0.004(4) C3 0.022(5) 0.093(8) 0.020(5) 0.004(5) -0.007(4) -0.012(5) C4 0.049(6) 0.039(5) 0.059(6) -0.010(5) 0.009(5) 0.009(5) C5 0.020(4) 0.036(5) 0.018(4) -0.002(4) 0.004(3) 0.004(4) C6 0.018(4) 0.047(5) 0.032(5) 0.004(4) 0.003(4) 0.005(4) C7 0.048 0.038 0.061 0.000 0.009 0.008 C8 0.048 0.038 0.061 0.000 0.009 0.008 N1 0.015(4) 0.032(4) 0.048(4) -0.010(3) -0.001(3) -0.010(3) N2 0.027(4) 0.048(5) 0.062(5) -0.003(4) -0.004(4) 0.005(4) C9 0.016(5) 0.070(7) 0.057(6) 0.002(5) -0.003(4) -0.009(5) C10 0.029(5) 0.042(6) 0.097(8) -0.001(5) 0.016(5) 0.007(5) C11 0.032(5) 0.073(7) 0.081(7) -0.060(6) -0.018(5) 0.015(5) C12 0.040(5) 0.048(6) 0.047(5) -0.007(5) -0.007(4) -0.018(5) C13 0.059(6) 0.038(5) 0.024(5) 0.022(4) -0.010(4) -0.004(4) C14 0.013(4) 0.057(6) 0.071(6) 0.026(5) 0.001(4) -0.017(4) C15 0.033(5) 0.038(5) 0.021(4) 0.015(4) -0.006(4) -0.002(4) C16 0.029(5) 0.059(6) 0.041(5) 0.029(5) -0.004(4) -0.007(4) C17 0.051(6) 0.054(5) 0.018(4) 0.012(4) -0.006(4) -0.004(5) Br3 0.0744(7) 0.0815(7) 0.0438(5) 0.0019(5) -0.0030(5) -0.0121(7) C18 0.029(5) 0.043(5) 0.058(6) 0.021(4) -0.012(5) 0.005(5) C19 0.049(6) 0.041(5) 0.015(4) -0.014(4) 0.000(4) 0.007(4) C20 0.016(4) 0.041(5) 0.067(6) 0.021(4) 0.001(5) 0.002(4) C21 0.073(8) 0.149(11) 0.054(6) -0.027(7) 0.033(6) -0.056(8) C22 0.058(7) 0.126(10) 0.025(5) 0.011(6) -0.024(5) -0.011(7) C23 0.040(5) 0.028(4) 0.041(5) -0.003(4) -0.004(4) 0.009(4) C24 0.021(5) 0.042(5) 0.049(5) 0.016(4) -0.004(4) 0.003(4) C31 0.043(6) 0.054(6) 0.082(7) 0.004(6) -0.010(5) -0.004(5) C32 0.022(5) 0.070(7) 0.052(6) 0.005(5) 0.006(4) -0.001(4) C33 0.035(6) 0.102(9) 0.034(5) 0.014(6) -0.004(4) 0.008(6) N3 0.035(4) 0.064(5) 0.031(4) -0.013(4) -0.007(3) 0.005(4) N4 0.040(4) 0.039(4) 0.033(4) 0.010(3) -0.007(3) 0.012(4) C34 0.055(7) 0.108(10) 0.068(7) 0.012(7) -0.018(6) 0.012(7) C35 0.026(6) 0.108(10) 0.086(8) 0.036(7) 0.020(5) -0.011(6) C36 0.022(5) 0.058(6) 0.083(7) 0.007(5) -0.001(5) 0.007(4) C37 0.086(8) 0.053(6) 0.053(6) -0.005(5) 0.002(5) 0.021(5) C38 0.018(5) 0.063(6) 0.067(6) -0.006(5) -0.003(4) -0.008(4) C39 0.041(6) 0.041(5) 0.026(5) 0.011(4) -0.007(4) -0.010(4) C40 0.044(5) 0.027(4) 0.027(4) -0.005(3) -0.012(4) 0.007(4) Br4 0.0624(7) 0.0522(6) 0.0797(7) -0.0217(5) -0.0112(6) 0.0012(6) C41 0.020(4) 0.036(5) 0.038(5) -0.003(4) -0.001(4) 0.012(4) C42 0.030(5) 0.033(5) 0.031(5) 0.003(4) -0.008(4) 0.009(4) C43 0.026(4) 0.031(4) 0.078(6) 0.013(4) 0.003(5) 0.008(5) C44 0.016(5) 0.049(5) 0.035(5) -0.003(4) -0.008(4) 0.001(4) C45 0.068(7) 0.050(6) 0.074(7) 0.026(5) 0.005(6) 0.010(5) C46 0.041(5) 0.050(5) 0.032(5) 0.005(4) 0.005(4) 0.013(4) C47 0.050(6) 0.044(5) 0.047(5) 0.015(4) 0.009(5) 0.006(5) C48 0.039(5) 0.031(5) 0.019(4) 0.008(4) 0.002(4) 0.005(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C25 C26 1.3900 . ? C25 C30 1.3900 . ? C25 C24 1.591(7) . ? C26 C27 1.3900 . ? C26 C31 1.527(9) . ? C27 C28 1.3900 . ? C27 C32 1.464(8) . ? C28 C29 1.3900 . ? C28 C37 1.503(8) . ? C29 C30 1.3900 . ? C29 C38 1.504(9) . ? C30 C36 1.552(8) . ? Zn1 N4 2.002(6) . ? Zn1 N2 2.018(6) . ? Zn1 Br1 2.3511(13) . ? Zn1 Br2 2.3542(13) . ? C1 C2 1.361(10) . ? C1 C6 1.420(9) . ? C1 C48 1.577(10) . ? C2 C3 1.326(11) . ? C2 C7 1.540(10) . ? C3 C4 1.387(10) . ? C3 C8 1.572(11) . ? C4 C5 1.465(10) . ? C4 C12 1.524(11) . ? C5 C6 1.399(9) . ? C5 C14 1.517(9) . ? C6 C13 1.522(9) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 N1 1.463(9) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? N1 N2 1.369(8) . ? N1 C11 1.403(9) . ? N2 C9 1.370(9) . ? C9 C10 1.321(11) . ? C9 H9 0.9500 . ? C10 C11 1.366(11) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.487(9) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.374(10) . ? C15 C20 1.403(10) . ? C16 C17 1.469(10) . ? C16 C21 1.627(11) . ? C17 C18 1.393(11) . ? C17 Br3 1.941(7) . ? C18 C19 1.382(10) . ? C18 C22 1.538(10) . ? C19 C20 1.401(10) . ? C19 C24 1.507(10) . ? C20 C23 1.520(9) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 N3 1.536(9) 6_656 ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 N4 1.397(9) . ? C33 C34 1.438(12) . ? C33 H33 0.9500 . ? N3 N4 1.340(8) . ? N3 C35 1.411(10) . ? N3 C32 1.537(9) 6_556 ? C34 C35 1.506(12) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C44 1.536(10) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C44 1.415(10) . ? C39 C40 1.418(10) . ? C39 C45 1.466(10) . ? C40 C41 1.366(10) . ? C40 Br4 1.895(7) . ? C41 C42 1.434(9) . ? C41 C46 1.557(9) . ? C42 C43 1.404(10) . ? C42 C48 1.528(9) . ? C43 C44 1.358(10) . ? C43 C47 1.621(10) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? 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 C26 C25 C30 120.0 . . ? C26 C25 C24 120.6(5) . . ? C30 C25 C24 119.4(5) . . ? C27 C26 C25 120.0 . . ? C27 C26 C31 117.8(5) . . ? C25 C26 C31 122.1(5) . . ? C26 C27 C28 120.0 . . ? C26 C27 C32 121.5(5) . . ? C28 C27 C32 118.4(5) . . ? C27 C28 C29 120.0 . . ? C27 C28 C37 120.1(5) . . ? C29 C28 C37 119.9(5) . . ? C30 C29 C28 120.0 . . ? C30 C29 C38 117.3(5) . . ? C28 C29 C38 122.7(5) . . ? C29 C30 C25 120.0 . . ? C29 C30 C36 118.9(5) . . ? C25 C30 C36 120.6(5) . . ? N4 Zn1 N2 98.6(2) . . ? N4 Zn1 Br1 111.49(18) . . ? N2 Zn1 Br1 105.8(2) . . ? N4 Zn1 Br2 106.95(19) . . ? N2 Zn1 Br2 111.39(18) . . ? Br1 Zn1 Br2 120.45(5) . . ? C2 C1 C6 121.3(7) . . ? C2 C1 C48 121.2(7) . . ? C6 C1 C48 117.4(7) . . ? C3 C2 C1 117.8(8) . . ? C3 C2 C7 120.5(8) . . ? C1 C2 C7 121.7(7) . . ? C2 C3 C4 127.2(8) . . ? C2 C3 C8 121.0(7) . . ? C4 C3 C8 111.8(8) . . ? C3 C4 C5 115.5(8) . . ? C3 C4 C12 127.2(8) . . ? C5 C4 C12 117.3(7) . . ? C6 C5 C4 118.0(7) . . ? C6 C5 C14 121.0(7) . . ? C4 C5 C14 121.0(7) . . ? C5 C6 C1 120.2(7) . . ? C5 C6 C13 120.5(6) . . ? C1 C6 C13 119.0(7) . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 C3 111.2(6) . . ? N1 C8 H8A 109.4 . . ? C3 C8 H8A 109.4 . . ? N1 C8 H8B 109.4 . . ? C3 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? N2 N1 C11 108.1(6) . . ? N2 N1 C8 122.0(6) . . ? C11 N1 C8 129.6(7) . . ? N1 N2 C9 105.6(6) . . ? N1 N2 Zn1 123.4(5) . . ? C9 N2 Zn1 128.0(6) . . ? C10 C9 N2 111.4(8) . . ? C10 C9 H9 124.3 . . ? N2 C9 H9 124.3 . . ? C9 C10 C11 108.1(8) . . ? C9 C10 H10 126.0 . . ? C11 C10 H10 126.0 . . ? C10 C11 N1 106.7(7) . . ? C10 C11 H11 126.6 . . ? N1 C11 H11 126.6 . . ? C4 C12 H12A 109.5 . . ? C4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C6 C13 H13A 109.5 . . ? C6 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C6 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C5 119.8(6) . . ? C15 C14 H14A 107.4 . . ? C5 C14 H14A 107.4 . . ? C15 C14 H14B 107.4 . . ? C5 C14 H14B 107.4 . . ? H14A C14 H14B 106.9 . . ? C16 C15 C20 117.7(7) . . ? C16 C15 C14 119.9(7) . . ? C20 C15 C14 122.4(7) . . ? C15 C16 C17 117.7(7) . . ? C15 C16 C21 119.5(7) . . ? C17 C16 C21 122.6(8) . . ? C18 C17 C16 123.9(7) . . ? C18 C17 Br3 118.8(6) . . ? C16 C17 Br3 117.3(7) . . ? C19 C18 C17 116.2(7) . . ? C19 C18 C22 128.6(8) . . ? C17 C18 C22 115.2(8) . . ? C18 C19 C20 120.4(8) . . ? C18 C19 C24 116.5(7) . . ? C20 C19 C24 122.8(7) . . ? C19 C20 C15 123.8(7) . . ? C19 C20 C23 118.6(7) . . ? C15 C20 C23 117.6(7) . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C18 C22 H22A 109.5 . . ? C18 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C18 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C19 C24 C25 119.2(6) . . ? C19 C24 H24A 107.5 . . ? C25 C24 H24A 107.5 . . ? C19 C24 H24B 107.5 . . ? C25 C24 H24B 107.5 . . ? H24A C24 H24B 107.0 . . ? C26 C31 H31A 109.5 . . ? C26 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C26 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C27 C32 N3 112.7(6) . 6_656 ? C27 C32 H32A 109.1 . . ? N3 C32 H32A 109.1 6_656 . ? C27 C32 H32B 109.1 . . ? N3 C32 H32B 109.1 6_656 . ? H32A C32 H32B 107.8 . . ? N4 C33 C34 111.3(8) . . ? N4 C33 H33 124.3 . . ? C34 C33 H33 124.3 . . ? N4 N3 C35 117.2(7) . . ? N4 N3 C32 121.7(7) . 6_556 ? C35 N3 C32 121.0(7) . 6_556 ? N3 N4 C33 104.6(7) . . ? N3 N4 Zn1 129.5(5) . . ? C33 N4 Zn1 125.0(6) . . ? C33 C34 C35 105.3(9) . . ? C33 C34 H34 127.3 . . ? C35 C34 H34 127.3 . . ? N3 C35 C34 101.4(9) . . ? N3 C35 H35 129.3 . . ? C34 C35 H35 129.3 . . ? C30 C36 H36A 109.5 . . ? C30 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C30 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C28 C37 H37A 109.5 . . ? C28 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C28 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C29 C38 C44 121.8(6) . . ? C29 C38 H38A 106.9 . . ? C44 C38 H38A 106.9 . . ? C29 C38 H38B 106.9 . . ? C44 C38 H38B 106.9 . . ? H38A C38 H38B 106.7 . . ? C44 C39 C40 114.7(7) . . ? C44 C39 C45 127.6(8) . . ? C40 C39 C45 117.6(8) . . ? C41 C40 C39 125.4(7) . . ? C41 C40 Br4 116.9(6) . . ? C39 C40 Br4 117.7(6) . . ? C40 C41 C42 117.5(7) . . ? C40 C41 C46 120.0(7) . . ? C42 C41 C46 122.5(7) . . ? C43 C42 C41 118.2(7) . . ? C43 C42 C48 121.7(7) . . ? C41 C42 C48 120.0(7) . . ? C44 C43 C42 122.1(7) . . ? C44 C43 C47 118.8(7) . . ? C42 C43 C47 118.1(7) . . ? C43 C44 C39 121.8(7) . . ? C43 C44 C38 121.2(8) . . ? C39 C44 C38 117.0(7) . . ? C39 C45 H45A 109.5 . . ? C39 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C39 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C41 C46 H46A 109.5 . . ? C41 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C41 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C43 C47 H47A 109.5 . . ? C43 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C43 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C42 C48 C1 119.3(6) . . ? C42 C48 H48A 107.5 . . ? C1 C48 H48A 107.5 . . ? C42 C48 H48B 107.5 . . ? C1 C48 H48B 107.5 . . ? H48A C48 H48B 107.0 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.59 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.662 _refine_diff_density_min -0.533 _refine_diff_density_rms 0.123 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.301 0.052 0.017 6536.0 2904.3 _platon_squeeze_details ; ; # Attachment '_8-ZnCl2_n.cif' data_e1447c _database_code_depnum_ccdc_archive 'CCDC 744821' #TrackingRef '_8-ZnCl2_n.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H54 Br2 Cl2 N4 Zn' _chemical_formula_sum 'C48 H54 Br2 Cl2 N4 Zn' _chemical_formula_weight 983.04 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' 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' Br Br -0.2901 2.4595 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab' 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' '-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 21.629(2) _cell_length_b 18.9786(18) _cell_length_c 34.265(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 14065(2) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9912 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 27.35 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 0.928 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4032 _exptl_absorpt_coefficient_mu 1.586 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7743 _exptl_absorpt_correction_T_max 0.8393 _exptl_absorpt_process_details sadabs _exptl_special_details ; Owing to large disorder of the solvent present in the cavities of this structure, the SQUEEZE command has been applied. Because of the floppiness of the phenyl ring we used the same thermal paramaters. Because of the poor diffraction powder the Ratio Observed / Unique Reflections is Low .... 38 Perc. ; _diffrn_ambient_temperature 173(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 70819 _diffrn_reflns_av_R_equivalents 0.1083 _diffrn_reflns_av_sigmaI/netI 0.1097 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 27.57 _reflns_number_total 15804 _reflns_number_gt 6084 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1253P)^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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00046(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 15804 _refine_ls_number_parameters 425 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2206 _refine_ls_R_factor_gt 0.1077 _refine_ls_wR_factor_ref 0.2901 _refine_ls_wR_factor_gt 0.2648 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.001 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 C25 C 1.0979(3) 0.5859(3) 0.39651(11) 0.0446(10) Uani 1 1 d G . . C26 C 1.1190(3) 0.5394(2) 0.36812(15) 0.0446(10) Uani 1 1 d G . . C27 C 1.1292(3) 0.5631(3) 0.33027(13) 0.0446(10) Uani 1 1 d G . . C28 C 1.1182(3) 0.6332(3) 0.32080(11) 0.0446(10) Uani 1 1 d G . . C29 C 1.0970(3) 0.6796(2) 0.34919(15) 0.0446(10) Uani 1 1 d G . . C30 C 1.0869(3) 0.6560(3) 0.38704(13) 0.0446(10) Uani 1 1 d G . . Zn1 Zn 0.72179(5) 0.37583(5) 0.24889(3) 0.0400(3) Uani 1 1 d . . . Cl1 Cl 0.64289(12) 0.31259(13) 0.22540(8) 0.0590(7) Uani 1 1 d . . . Cl2 Cl 0.80444(12) 0.32424(12) 0.27443(8) 0.0533(6) Uani 1 1 d . . . C1 C 0.8375(4) 0.6799(4) 0.3484(2) 0.0341(8) Uani 1 1 d . . . C2 C 0.8109(4) 0.6292(4) 0.3213(2) 0.0341(8) Uani 1 1 d . . . C3 C 0.8047(4) 0.5614(4) 0.3295(2) 0.0341(8) Uani 1 1 d . . . C4 C 0.8176(4) 0.5360(4) 0.3687(2) 0.0341(8) Uani 1 1 d . . . C5 C 0.8403(4) 0.5833(4) 0.3969(2) 0.0341(8) Uani 1 1 d . . . C6 C 0.8482(4) 0.6542(4) 0.3874(2) 0.0341(8) Uani 1 1 d . . . C7 C 0.7978(5) 0.6530(5) 0.2780(3) 0.057(3) Uani 1 1 d . . . H7A H 0.8371 0.6575 0.2639 0.086 Uiso 1 1 calc R . . H7B H 0.7765 0.6986 0.2781 0.086 Uiso 1 1 calc R . . H7C H 0.7718 0.6178 0.2651 0.086 Uiso 1 1 calc R . . C8 C 0.7772(4) 0.5100(4) 0.3023(2) 0.035(2) Uani 1 1 d . . . H8A H 0.7896 0.5235 0.2755 0.042 Uiso 1 1 calc R . . H8B H 0.7962 0.4635 0.3077 0.042 Uiso 1 1 calc R . . N1 N 0.7126(3) 0.5012(4) 0.30260(18) 0.0320(8) Uani 1 1 d . . . N2 N 0.6819(3) 0.4465(4) 0.28757(18) 0.0320(8) Uani 1 1 d . . . C9 C 0.6217(4) 0.4579(4) 0.2919(2) 0.0320(8) Uani 1 1 d . . . H9 H 0.5893 0.4280 0.2833 0.038 Uiso 1 1 calc R . . C10 C 0.6151(4) 0.5178(4) 0.3102(2) 0.0320(8) Uani 1 1 d . . . H10 H 0.5762 0.5367 0.3179 0.038 Uiso 1 1 calc R . . C11 C 0.6703(4) 0.5501(4) 0.3170(2) 0.0320(8) Uani 1 1 d . . . H11 H 0.6781 0.5947 0.3286 0.038 Uiso 1 1 calc R . . C12 C 0.8033(5) 0.4608(5) 0.3819(4) 0.071(4) Uani 1 1 d . . . H12A H 0.8420 0.4363 0.3880 0.107 Uiso 1 1 calc R . . H12B H 0.7817 0.4357 0.3610 0.107 Uiso 1 1 calc R . . H12C H 0.7771 0.4622 0.4052 0.107 Uiso 1 1 calc R . . C13 C 0.8655(4) 0.7069(5) 0.4193(2) 0.039(2) Uani 1 1 d . . . H13A H 0.8756 0.6814 0.4434 0.058 Uiso 1 1 calc R . . H13B H 0.8306 0.7386 0.4241 0.058 Uiso 1 1 calc R . . H13C H 0.9015 0.7344 0.4109 0.058 Uiso 1 1 calc R . . C14 C 0.8494(4) 0.5608(5) 0.4389(3) 0.043(2) Uani 1 1 d . . . H14A H 0.8424 0.5093 0.4402 0.052 Uiso 1 1 calc R . . H14B H 0.8165 0.5833 0.4546 0.052 Uiso 1 1 calc R . . C15 C 0.9130(4) 0.5764(5) 0.4598(2) 0.0360(15) Uani 1 1 d . . . C16 C 0.9121(4) 0.6063(5) 0.4959(2) 0.0360(15) Uani 1 1 d . . . C17 C 0.9708(4) 0.6167(5) 0.5113(2) 0.042(2) Uani 1 1 d . . . Br1 Br 0.97086(5) 0.66564(6) 0.56309(3) 0.0578(3) Uani 1 1 d . . . C18 C 1.0285(4) 0.6057(4) 0.4956(3) 0.038(2) Uani 1 1 d . . . C19 C 1.0254(4) 0.5766(4) 0.4584(2) 0.0329(19) Uani 1 1 d . . . C20 C 0.9659(4) 0.5541(5) 0.4391(3) 0.044(2) Uani 1 1 d . . . C21 C 0.8507(4) 0.6263(6) 0.5158(3) 0.055(3) Uani 1 1 d . . . H21A H 0.8257 0.6547 0.4979 0.083 Uiso 1 1 calc R . . H21B H 0.8594 0.6536 0.5395 0.083 Uiso 1 1 calc R . . H21C H 0.8281 0.5834 0.5228 0.083 Uiso 1 1 calc R . . C22 C 1.0853(5) 0.6203(7) 0.5173(3) 0.063(3) Uani 1 1 d . . . H22A H 1.1001 0.6677 0.5109 0.095 Uiso 1 1 calc R . . H22B H 1.1169 0.5855 0.5103 0.095 Uiso 1 1 calc R . . H22C H 1.0768 0.6174 0.5454 0.095 Uiso 1 1 calc R . . C23 C 0.9658(5) 0.5205(6) 0.4023(2) 0.058(3) Uani 1 1 d . . . H23A H 1.0017 0.4891 0.4004 0.086 Uiso 1 1 calc R . . H23B H 0.9680 0.5561 0.3816 0.086 Uiso 1 1 calc R . . H23C H 0.9278 0.4929 0.3993 0.086 Uiso 1 1 calc R . . C24 C 1.0847(4) 0.5544(6) 0.4391(3) 0.048(2) Uani 1 1 d . . . H24A H 1.0848 0.5023 0.4372 0.058 Uiso 1 1 calc R . . H24B H 1.1194 0.5680 0.4564 0.058 Uiso 1 1 calc R . . C31 C 1.1378(5) 0.4612(5) 0.3757(2) 0.045(2) Uani 1 1 d . . . H31A H 1.1533 0.4402 0.3515 0.067 Uiso 1 1 calc R . . H31B H 1.1016 0.4347 0.3848 0.067 Uiso 1 1 calc R . . H31C H 1.1702 0.4595 0.3957 0.067 Uiso 1 1 calc R . . C32 C 1.1554(4) 0.5124(7) 0.2998(3) 0.045(2) Uani 1 1 d . . . H32A H 1.1472 0.5307 0.2732 0.067 Uiso 1 1 calc R . . H32B H 1.1354 0.4658 0.3023 0.067 Uiso 1 1 calc R . . C33 C 0.8168(4) 0.4571(6) 0.1994(2) 0.045(2) Uani 1 1 d . . . H33 H 0.8493 0.4263 0.2068 0.067 Uiso 1 1 calc R . . N3 N 0.7265(4) 0.5052(5) 0.1937(2) 0.054(2) Uani 1 1 d . . . N4 N 0.7545(4) 0.4472(4) 0.20906(18) 0.044(2) Uani 1 1 d . . . C34 C 0.8245(5) 0.5185(7) 0.1774(2) 0.061(3) Uani 1 1 d . . . H34 H 0.8622 0.5363 0.1672 0.073 Uiso 1 1 calc R . . C35 C 0.7667(5) 0.5483(6) 0.1735(3) 0.054(3) Uani 1 1 d . . . H35 H 0.7566 0.5900 0.1596 0.064 Uiso 1 1 calc R . . C36 C 1.0718(4) 0.7048(5) 0.4153(2) 0.043(2) Uani 1 1 d . . . H36A H 1.0271 0.7133 0.4149 0.065 Uiso 1 1 calc R . . H36B H 1.0937 0.7491 0.4101 0.065 Uiso 1 1 calc R . . H36C H 1.0838 0.6868 0.4410 0.065 Uiso 1 1 calc R . . C37 C 1.1418(6) 0.6644(7) 0.2786(3) 0.043(2) Uani 1 1 d . . . H37A H 1.1062 0.6706 0.2612 0.065 Uiso 1 1 calc R . . H37B H 1.1710 0.6312 0.2667 0.065 Uiso 1 1 calc R . . H37C H 1.1622 0.7099 0.2826 0.065 Uiso 1 1 calc R . . C38 C 1.0838(5) 0.7601(6) 0.3392(3) 0.052(3) Uani 1 1 d . . . H38A H 1.1176 0.7881 0.3510 0.062 Uiso 1 1 calc R . . H38B H 1.0875 0.7654 0.3106 0.062 Uiso 1 1 calc R . . C39 C 1.0241(4) 0.8537(5) 0.3716(2) 0.037(2) Uani 1 1 d . . . C40 C 0.9645(4) 0.8837(6) 0.3806(2) 0.044(2) Uani 1 1 d . . . Br2 Br 0.96253(5) 0.96968(5) 0.40900(3) 0.0603(3) Uani 1 1 d . . . C41 C 0.9093(4) 0.8499(4) 0.3681(2) 0.036(2) Uani 1 1 d . . . C42 C 0.9113(4) 0.7874(4) 0.34980(19) 0.0250(17) Uani 1 1 d . . . C43 C 0.9667(4) 0.7588(4) 0.3392(2) 0.0283(17) Uani 1 1 d . . . C44 C 1.0229(4) 0.7948(5) 0.3514(2) 0.039(2) Uani 1 1 d . . . C45 C 1.0782(4) 0.8913(4) 0.3836(3) 0.038(2) Uani 1 1 d . . . H45A H 1.0877 0.8795 0.4108 0.057 Uiso 1 1 calc R . . H45B H 1.0708 0.9420 0.3814 0.057 Uiso 1 1 calc R . . H45C H 1.1131 0.8779 0.3670 0.057 Uiso 1 1 calc R . . C46 C 0.8451(4) 0.8846(6) 0.3863(3) 0.038(2) Uani 1 1 d . . . H46A H 0.8115 0.8799 0.3673 0.057 Uiso 1 1 calc R . . H46B H 0.8519 0.9346 0.3921 0.057 Uiso 1 1 calc R . . H46C H 0.8339 0.8599 0.4104 0.057 Uiso 1 1 calc R . . C47 C 0.9695(4) 0.6965(5) 0.3118(2) 0.036(2) Uani 1 1 d . . . H47A H 0.9848 0.6551 0.3259 0.054 Uiso 1 1 calc R . . H47B H 0.9975 0.7073 0.2901 0.054 Uiso 1 1 calc R . . H47C H 0.9281 0.6867 0.3015 0.054 Uiso 1 1 calc R . . C48 C 0.8468(4) 0.7521(4) 0.3378(2) 0.034(2) Uani 1 1 d . . . H48A H 0.8132 0.7803 0.3497 0.041 Uiso 1 1 calc R . . H48B H 0.8423 0.7559 0.3091 0.041 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 C25 0.041(2) 0.067(3) 0.0264(18) 0.0063(17) 0.0076(16) 0.0036(19) C26 0.041(2) 0.067(3) 0.0264(18) 0.0063(17) 0.0076(16) 0.0036(19) C27 0.041(2) 0.067(3) 0.0264(18) 0.0063(17) 0.0076(16) 0.0036(19) C28 0.041(2) 0.067(3) 0.0264(18) 0.0063(17) 0.0076(16) 0.0036(19) C29 0.041(2) 0.067(3) 0.0264(18) 0.0063(17) 0.0076(16) 0.0036(19) C30 0.041(2) 0.067(3) 0.0264(18) 0.0063(17) 0.0076(16) 0.0036(19) Zn1 0.0433(6) 0.0349(5) 0.0417(6) -0.0018(5) -0.0113(5) -0.0037(5) Cl1 0.0611(17) 0.0429(14) 0.0728(17) -0.0139(12) -0.0297(14) -0.0180(12) Cl2 0.0503(15) 0.0316(12) 0.0781(17) 0.0002(11) -0.0108(13) -0.0004(10) C1 0.036(2) 0.0285(18) 0.0383(19) -0.0027(14) -0.0121(16) -0.0050(15) C2 0.036(2) 0.0285(18) 0.0383(19) -0.0027(14) -0.0121(16) -0.0050(15) C3 0.036(2) 0.0285(18) 0.0383(19) -0.0027(14) -0.0121(16) -0.0050(15) C4 0.036(2) 0.0285(18) 0.0383(19) -0.0027(14) -0.0121(16) -0.0050(15) C5 0.036(2) 0.0285(18) 0.0383(19) -0.0027(14) -0.0121(16) -0.0050(15) C6 0.036(2) 0.0285(18) 0.0383(19) -0.0027(14) -0.0121(16) -0.0050(15) C7 0.080(8) 0.033(5) 0.058(6) -0.019(5) -0.034(6) 0.007(5) C8 0.036(5) 0.022(4) 0.047(5) -0.002(4) -0.025(4) -0.002(3) N1 0.039(2) 0.0313(18) 0.0253(16) -0.0100(13) 0.0003(15) 0.0037(14) N2 0.039(2) 0.0313(18) 0.0253(16) -0.0100(13) 0.0003(15) 0.0037(14) C9 0.039(2) 0.0313(18) 0.0253(16) -0.0100(13) 0.0003(15) 0.0037(14) C10 0.039(2) 0.0313(18) 0.0253(16) -0.0100(13) 0.0003(15) 0.0037(14) C11 0.039(2) 0.0313(18) 0.0253(16) -0.0100(13) 0.0003(15) 0.0037(14) C12 0.061(7) 0.044(6) 0.109(9) 0.025(6) -0.067(7) -0.023(5) C13 0.055(6) 0.045(5) 0.016(4) 0.006(4) -0.006(4) -0.003(4) C14 0.034(5) 0.046(6) 0.049(5) 0.026(4) -0.018(4) -0.015(4) C15 0.023(3) 0.068(4) 0.017(2) 0.025(3) 0.003(2) -0.007(3) C16 0.023(3) 0.068(4) 0.017(2) 0.025(3) 0.003(2) -0.007(3) C17 0.051(6) 0.039(5) 0.036(4) 0.013(4) -0.031(5) -0.009(4) Br1 0.0684(7) 0.0705(8) 0.0346(5) -0.0004(4) 0.0074(5) -0.0068(6) C18 0.031(5) 0.027(4) 0.056(5) 0.010(4) -0.011(4) 0.000(4) C19 0.035(5) 0.030(4) 0.034(4) 0.003(3) 0.007(4) -0.006(4) C20 0.026(5) 0.057(6) 0.048(5) 0.006(4) -0.031(4) -0.001(4) C21 0.049(6) 0.072(7) 0.045(5) 0.025(5) 0.013(5) 0.025(5) C22 0.047(6) 0.109(10) 0.034(5) -0.036(6) -0.023(5) 0.012(6) C23 0.070(7) 0.064(7) 0.039(5) 0.018(5) 0.044(5) 0.035(6) C24 0.031(5) 0.068(7) 0.046(5) 0.006(5) -0.011(4) 0.007(5) C31 0.065(6) 0.054(6) 0.015(4) 0.006(4) -0.001(4) 0.008(5) C32 0.065(6) 0.054(6) 0.015(4) 0.006(4) -0.001(4) 0.008(5) C33 0.065(6) 0.054(6) 0.015(4) 0.006(4) -0.001(4) 0.008(5) N3 0.038(5) 0.060(6) 0.064(5) 0.002(4) 0.001(4) 0.022(4) N4 0.055(5) 0.056(5) 0.022(3) 0.001(3) -0.015(3) 0.020(4) C34 0.056(7) 0.106(10) 0.020(4) -0.006(5) 0.012(4) 0.032(6) C35 0.049(6) 0.072(8) 0.041(5) 0.013(5) 0.013(5) 0.028(5) C36 0.034(5) 0.056(6) 0.040(5) 0.009(4) 0.003(4) -0.011(4) C37 0.034(5) 0.056(6) 0.040(5) 0.009(4) 0.003(4) -0.011(4) C38 0.059(7) 0.065(7) 0.032(4) -0.007(4) 0.003(5) 0.042(5) C39 0.035(5) 0.035(5) 0.041(5) 0.005(4) 0.009(4) -0.012(4) C40 0.016(5) 0.080(7) 0.036(4) 0.024(4) -0.005(4) -0.007(4) Br2 0.0734(8) 0.0389(5) 0.0685(7) -0.0183(5) -0.0108(6) 0.0008(5) C41 0.046(6) 0.026(4) 0.035(4) -0.011(3) -0.018(4) -0.004(4) C42 0.050(5) 0.008(3) 0.017(3) -0.008(3) 0.001(4) 0.008(3) C43 0.029(5) 0.035(4) 0.021(3) 0.002(3) 0.007(4) -0.007(4) C44 0.036(5) 0.048(6) 0.033(4) 0.008(4) 0.026(4) -0.001(4) C45 0.028(5) 0.031(5) 0.055(5) 0.012(4) -0.005(4) -0.009(4) C46 0.028(5) 0.031(5) 0.055(5) 0.012(4) -0.005(4) -0.009(4) C47 0.043(5) 0.046(5) 0.019(4) -0.004(3) 0.019(4) 0.007(4) C48 0.048(5) 0.027(4) 0.029(4) 0.004(3) -0.021(4) 0.020(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 C25 C26 1.3900 . ? C25 C30 1.3900 . ? C25 C24 1.604(10) . ? C26 C27 1.3900 . ? C26 C31 1.562(10) . ? C27 C28 1.3900 . ? C27 C32 1.530(9) . ? C28 C29 1.3900 . ? C28 C37 1.645(9) . ? C29 C30 1.3900 . ? C29 C38 1.590(10) . ? C30 C36 1.380(10) . ? Zn1 N4 2.048(8) . ? Zn1 N2 2.073(6) . ? Zn1 Cl2 2.218(3) . ? Zn1 Cl1 2.236(2) . ? C1 C48 1.432(11) . ? C1 C6 1.441(11) . ? C1 C2 1.457(11) . ? C2 C3 1.322(11) . ? C2 C7 1.577(12) . ? C3 C4 1.456(11) . ? C3 C8 1.475(11) . ? C4 C5 1.406(11) . ? C4 C12 1.529(12) . ? C5 C6 1.395(11) . ? C5 C14 1.515(11) . ? C6 C13 1.528(11) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 N1 1.408(11) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? N1 N2 1.336(9) . ? N1 C11 1.392(10) . ? N2 C9 1.328(10) . ? C9 C10 1.306(11) . ? C9 H9 0.9500 . ? C10 C11 1.363(12) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.579(11) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.359(12) . ? C15 C20 1.410(13) . ? C16 C17 1.389(11) . ? C16 C21 1.540(12) . ? C17 C18 1.375(12) . ? C17 Br1 2.004(9) . ? C18 C19 1.391(12) . ? C18 C22 1.463(12) . ? C19 C24 1.503(12) . ? C19 C20 1.508(11) . ? C20 C23 1.414(13) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 N3 1.560(12) 6_656 ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.397(15) . ? C33 N4 1.400(11) . ? C33 H33 0.9500 . ? N3 N4 1.361(10) . ? N3 C35 1.379(13) . ? N3 C32 1.560(12) 6_556 ? C34 C35 1.378(13) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C44 1.529(12) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C44 1.316(12) . ? C39 C45 1.430(11) . ? C39 C40 1.443(12) . ? C40 C41 1.421(12) . ? C40 Br2 1.901(11) . ? C41 C42 1.342(10) . ? C41 C46 1.661(13) . ? C42 C43 1.363(11) . ? C42 C48 1.602(12) . ? C43 C44 1.456(12) . ? C43 C47 1.512(11) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? 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 C26 C25 C30 120.0 . . ? C26 C25 C24 117.3(5) . . ? C30 C25 C24 122.6(5) . . ? C27 C26 C25 120.0 . . ? C27 C26 C31 115.0(4) . . ? C25 C26 C31 124.9(4) . . ? C26 C27 C28 120.0 . . ? C26 C27 C32 119.6(6) . . ? C28 C27 C32 120.4(6) . . ? C29 C28 C27 120.0 . . ? C29 C28 C37 119.3(6) . . ? C27 C28 C37 119.8(5) . . ? C28 C29 C30 120.0 . . ? C28 C29 C38 121.2(4) . . ? C30 C29 C38 118.8(4) . . ? C36 C30 C29 118.4(5) . . ? C36 C30 C25 121.3(5) . . ? C29 C30 C25 120.0 . . ? N4 Zn1 N2 98.2(3) . . ? N4 Zn1 Cl2 106.1(2) . . ? N2 Zn1 Cl2 111.6(2) . . ? N4 Zn1 Cl1 112.2(2) . . ? N2 Zn1 Cl1 105.0(2) . . ? Cl2 Zn1 Cl1 121.34(10) . . ? C48 C1 C6 122.5(7) . . ? C48 C1 C2 121.8(7) . . ? C6 C1 C2 115.5(7) . . ? C3 C2 C1 123.3(8) . . ? C3 C2 C7 117.4(7) . . ? C1 C2 C7 118.7(7) . . ? C2 C3 C4 119.9(7) . . ? C2 C3 C8 123.5(8) . . ? C4 C3 C8 116.2(7) . . ? C5 C4 C3 119.3(8) . . ? C5 C4 C12 117.6(8) . . ? C3 C4 C12 123.0(7) . . ? C6 C5 C4 119.9(7) . . ? C6 C5 C14 118.5(7) . . ? C4 C5 C14 121.1(8) . . ? C5 C6 C1 121.5(7) . . ? C5 C6 C13 119.7(7) . . ? C1 C6 C13 118.7(7) . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 C3 118.3(7) . . ? N1 C8 H8A 107.7 . . ? C3 C8 H8A 107.7 . . ? N1 C8 H8B 107.7 . . ? C3 C8 H8B 107.7 . . ? H8A C8 H8B 107.1 . . ? N2 N1 C11 109.2(7) . . ? N2 N1 C8 125.6(6) . . ? C11 N1 C8 125.2(7) . . ? C9 N2 N1 108.4(6) . . ? C9 N2 Zn1 125.8(5) . . ? N1 N2 Zn1 122.9(5) . . ? C10 C9 N2 107.7(8) . . ? C10 C9 H9 126.1 . . ? N2 C9 H9 126.1 . . ? C9 C10 C11 112.1(8) . . ? C9 C10 H10 124.0 . . ? C11 C10 H10 124.0 . . ? C10 C11 N1 102.5(7) . . ? C10 C11 H11 128.8 . . ? N1 C11 H11 128.8 . . ? C4 C12 H12A 109.5 . . ? C4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C6 C13 H13A 109.5 . . ? C6 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C6 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C5 C14 C15 119.5(7) . . ? C5 C14 H14A 107.4 . . ? C15 C14 H14A 107.4 . . ? C5 C14 H14B 107.4 . . ? C15 C14 H14B 107.4 . . ? H14A C14 H14B 107.0 . . ? C16 C15 C20 126.5(8) . . ? C16 C15 C14 118.5(8) . . ? C20 C15 C14 114.9(7) . . ? C15 C16 C17 113.0(8) . . ? C15 C16 C21 121.3(8) . . ? C17 C16 C21 125.8(8) . . ? C18 C17 C16 131.3(8) . . ? C18 C17 Br1 114.6(6) . . ? C16 C17 Br1 113.8(7) . . ? C17 C18 C19 112.0(8) . . ? C17 C18 C22 122.3(8) . . ? C19 C18 C22 125.7(8) . . ? C18 C19 C24 118.2(8) . . ? C18 C19 C20 123.7(8) . . ? C24 C19 C20 117.2(8) . . ? C15 C20 C23 125.8(8) . . ? C15 C20 C19 112.7(8) . . ? C23 C20 C19 121.2(8) . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C18 C22 H22A 109.5 . . ? C18 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C18 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C19 C24 C25 116.5(7) . . ? C19 C24 H24A 108.2 . . ? C25 C24 H24A 108.2 . . ? C19 C24 H24B 108.2 . . ? C25 C24 H24B 108.2 . . ? H24A C24 H24B 107.3 . . ? C26 C31 H31A 109.5 . . ? C26 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C26 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C27 C32 N3 108.9(7) . 6_656 ? C27 C32 H32A 109.9 . . ? N3 C32 H32A 109.9 6_656 . ? C27 C32 H32B 109.9 . . ? N3 C32 H32B 109.9 6_656 . ? H32A C32 H32B 108.3 . . ? C34 C33 N4 110.8(8) . . ? C34 C33 H33 124.6 . . ? N4 C33 H33 124.6 . . ? N4 N3 C35 113.2(8) . . ? N4 N3 C32 116.9(8) . 6_556 ? C35 N3 C32 129.8(8) . 6_556 ? N3 N4 C33 103.1(8) . . ? N3 N4 Zn1 129.7(6) . . ? C33 N4 Zn1 125.4(6) . . ? C35 C34 C33 106.6(10) . . ? C35 C34 H34 126.7 . . ? C33 C34 H34 126.7 . . ? C34 C35 N3 106.2(9) . . ? C34 C35 H35 126.9 . . ? N3 C35 H35 126.9 . . ? C30 C36 H36A 109.5 . . ? C30 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C30 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C28 C37 H37A 109.5 . . ? C28 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C28 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C44 C38 C29 120.7(8) . . ? C44 C38 H38A 107.2 . . ? C29 C38 H38A 107.2 . . ? C44 C38 H38B 107.2 . . ? C29 C38 H38B 107.2 . . ? H38A C38 H38B 106.8 . . ? C44 C39 C45 126.3(9) . . ? C44 C39 C40 115.4(8) . . ? C45 C39 C40 118.2(8) . . ? C41 C40 C39 120.6(9) . . ? C41 C40 Br2 121.5(7) . . ? C39 C40 Br2 117.9(6) . . ? C42 C41 C40 120.8(9) . . ? C42 C41 C46 123.6(8) . . ? C40 C41 C46 114.2(7) . . ? C41 C42 C43 120.3(8) . . ? C41 C42 C48 117.4(7) . . ? C43 C42 C48 122.0(6) . . ? C42 C43 C44 118.1(7) . . ? C42 C43 C47 120.8(7) . . ? C44 C43 C47 120.7(7) . . ? C39 C44 C43 124.5(8) . . ? C39 C44 C38 119.4(9) . . ? C43 C44 C38 116.1(8) . . ? C39 C45 H45A 109.5 . . ? C39 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C39 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C41 C46 H46A 109.5 . . ? C41 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C41 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C43 C47 H47A 109.5 . . ? C43 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C43 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C1 C48 C42 117.2(6) . . ? C1 C48 H48A 108.0 . . ? C42 C48 H48A 108.0 . . ? C1 C48 H48B 108.0 . . ? C42 C48 H48B 108.0 . . ? H48A C48 H48B 107.2 . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 27.57 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 1.240 _refine_diff_density_min -1.327 _refine_diff_density_rms 0.157 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.289 0.031 0.005 7082.8 2746.9 _platon_squeeze_details ; ;