# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Mir Wais Hosseini' 'Jerome Ehrhart' 'Nathalie Kyritsakas-Gruber' 'Jean-Marc Planeix' _publ_contact_author_name 'Mir Wais Hosseini' _publ_contact_author_email HOSSEINI@CHIMIE.U-STRASBG.FR _publ_section_title ; Synthesis and structural studies of metallamacrotricycles based on a metacyclophane in 1,3-alternate conformation bearing four imidazolyl units ; # Attachment '4-CoBr2.cif' data_e1445a _database_code_depnum_ccdc_archive 'CCDC 702193' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C56 H64 Br4 CO2 N8), 3.60(C2 H4 Cl2), C H3 OH' _chemical_formula_sum 'C120.20 H146.40 Br8 Cl7.20 Co4 N16 O' _chemical_formula_weight 2951.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 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 23.0347(10) _cell_length_b 20.1741(9) _cell_length_c 15.5101(6) _cell_angle_alpha 90.00 _cell_angle_beta 101.952(2) _cell_angle_gamma 90.00 _cell_volume 7051.4(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6270 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 22.01 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.390 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2986 _exptl_absorpt_coefficient_mu 2.910 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5937 _exptl_absorpt_correction_T_max 0.7596 _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 70499 _diffrn_reflns_av_R_equivalents 0.1026 _diffrn_reflns_av_sigmaI/netI 0.1159 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 0.90 _diffrn_reflns_theta_max 27.55 _reflns_number_total 16208 _reflns_number_gt 8650 _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^)+(0.1857P)^2^+73.1702P] 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 16208 _refine_ls_number_parameters 722 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.1805 _refine_ls_R_factor_gt 0.1096 _refine_ls_wR_factor_ref 0.3037 _refine_ls_wR_factor_gt 0.2860 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.018 _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 Co1 Co 0.98710(6) 0.26044(7) 1.06002(9) 0.0279(3) Uani 1 1 d . . . Br1 Br 1.06600(6) 0.33421(6) 1.12096(8) 0.0411(3) Uani 1 1 d . . . Br2 Br 0.89328(6) 0.30273(8) 0.98541(8) 0.0485(4) Uani 1 1 d . . . Co2 Co 0.55890(9) -0.15166(8) 0.61955(11) 0.0486(5) Uani 1 1 d . . . Br3 Br 0.64510(7) -0.12099(8) 0.56500(10) 0.0578(4) Uani 1 1 d . . . Br4 Br 0.48141(10) -0.21199(8) 0.52759(13) 0.0947(8) Uani 1 1 d . . . C1 C 0.8702(5) -0.0368(5) 0.8219(6) 0.028(2) Uani 1 1 d . . . C2 C 0.9267(5) -0.0084(5) 0.8311(6) 0.028(2) Uani 1 1 d . . . C3 C 0.9307(5) 0.0554(5) 0.7969(6) 0.025(2) Uani 1 1 d . . . C4 C 0.8795(5) 0.0920(5) 0.7610(6) 0.030(2) Uani 1 1 d . . . C5 C 0.8239(4) 0.0642(5) 0.7570(6) 0.024(2) Uani 1 1 d . . . C6 C 0.8183(5) 0.0001(5) 0.7836(6) 0.030(2) Uani 1 1 d . . . C7 C 0.9813(5) -0.0448(5) 0.8748(8) 0.032(2) Uani 1 1 d . . . H7A H 0.9716 -0.0753 0.9189 0.048 Uiso 1 1 calc R . . H7B H 1.0113 -0.0130 0.9037 0.048 Uiso 1 1 calc R . . H7C H 0.9969 -0.0699 0.8306 0.048 Uiso 1 1 calc R . . C8 C 0.9915(5) 0.0831(5) 0.7929(7) 0.032(2) Uani 1 1 d . . . H8A H 1.0206 0.0463 0.8005 0.039 Uiso 1 1 calc R . . H8B H 0.9898 0.1026 0.7338 0.039 Uiso 1 1 calc R . . N1 N 1.0127(4) 0.1346(4) 0.8610(5) 0.0261(18) Uani 1 1 d . . . C9 C 0.9844(5) 0.1570(5) 0.9222(7) 0.029(2) Uani 1 1 d . . . H9 H 0.9465 0.1419 0.9285 0.034 Uiso 1 1 calc R . . N2 N 1.0156(4) 0.2029(4) 0.9733(5) 0.0272(18) Uani 1 1 d . . . C10 C 1.0669(5) 0.2087(5) 0.9415(7) 0.033(2) Uani 1 1 d . . . H10 H 1.0990 0.2375 0.9647 0.039 Uiso 1 1 calc R . . C11 C 1.0648(5) 0.1672(5) 0.8723(7) 0.030(2) Uani 1 1 d . . . H11 H 1.0943 0.1621 0.8382 0.036 Uiso 1 1 calc R . . C12 C 0.8853(5) 0.1624(6) 0.7270(8) 0.036(3) Uani 1 1 d . . . H12A H 0.8682 0.1642 0.6637 0.054 Uiso 1 1 calc R . . H12B H 0.9273 0.1748 0.7373 0.054 Uiso 1 1 calc R . . H12C H 0.8642 0.1934 0.7583 0.054 Uiso 1 1 calc R . . C13 C 0.7595(5) -0.0342(5) 0.7638(8) 0.036(3) Uani 1 1 d . . . H13A H 0.7411 -0.0314 0.8152 0.054 Uiso 1 1 calc R . . H13B H 0.7651 -0.0808 0.7499 0.054 Uiso 1 1 calc R . . H13C H 0.7338 -0.0128 0.7132 0.054 Uiso 1 1 calc R . . C14 C 0.7702(5) 0.1055(5) 0.7141(7) 0.034(2) Uani 1 1 d . . . H14A H 0.7553 0.0875 0.6542 0.041 Uiso 1 1 calc R . . H14B H 0.7845 0.1511 0.7068 0.041 Uiso 1 1 calc R . . C15 C 0.7172(5) 0.1110(5) 0.7594(7) 0.032(2) Uani 1 1 d . . . C16 C 0.6587(5) 0.1059(5) 0.7088(8) 0.036(3) Uani 1 1 d . . . C17 C 0.6108(5) 0.1113(5) 0.7490(8) 0.039(3) Uani 1 1 d . . . C18 C 0.6186(5) 0.1180(6) 0.8408(8) 0.040(3) Uani 1 1 d . . . C19 C 0.6757(5) 0.1267(5) 0.8912(7) 0.035(3) Uani 1 1 d . . . C20 C 0.7256(5) 0.1260(5) 0.8507(7) 0.033(2) Uani 1 1 d . . . C21 C 0.6507(6) 0.0976(7) 0.6105(8) 0.048(3) Uani 1 1 d . . . H21A H 0.6084 0.1000 0.5832 0.072 Uiso 1 1 calc R . . H21B H 0.6665 0.0545 0.5975 0.072 Uiso 1 1 calc R . . H21C H 0.6720 0.1330 0.5868 0.072 Uiso 1 1 calc R . . C22 C 0.5487(5) 0.1117(6) 0.6921(10) 0.048(3) Uani 1 1 d . . . H22A H 0.5212 0.1322 0.7256 0.057 Uiso 1 1 calc R . . H22B H 0.5486 0.1393 0.6393 0.057 Uiso 1 1 calc R . . N3 N 0.5270(4) 0.0449(5) 0.6636(6) 0.038(2) Uani 1 1 d . . . C23 C 0.5577(6) -0.0128(6) 0.6782(8) 0.046(3) Uani 1 1 d . . . H23 H 0.5973 -0.0168 0.7110 0.055 Uiso 1 1 calc R . . N4 N 0.5247(5) -0.0633(5) 0.6399(6) 0.044(3) Uani 1 1 d . . . C24 C 0.4710(6) -0.0362(8) 0.6005(9) 0.055(4) Uani 1 1 d . . . H24 H 0.4383 -0.0602 0.5678 0.066 Uiso 1 1 calc R . . C25 C 0.4719(6) 0.0305(8) 0.6156(9) 0.056(4) Uani 1 1 d . . . H25 H 0.4403 0.0609 0.5964 0.067 Uiso 1 1 calc R . . C26 C 0.5655(6) 0.1163(7) 0.8827(9) 0.050(3) Uani 1 1 d . . . H26A H 0.5753 0.0918 0.9384 0.075 Uiso 1 1 calc R . . H26B H 0.5325 0.0942 0.8430 0.075 Uiso 1 1 calc R . . H26C H 0.5539 0.1616 0.8942 0.075 Uiso 1 1 calc R . . C27 C 0.7858(5) 0.1437(6) 0.9018(8) 0.039(3) Uani 1 1 d . . . H27A H 0.7820 0.1712 0.9524 0.059 Uiso 1 1 calc R . . H27B H 0.8073 0.1684 0.8638 0.059 Uiso 1 1 calc R . . H27C H 0.8077 0.1032 0.9226 0.059 Uiso 1 1 calc R . . C28 C 0.6843(6) 0.1449(6) 0.9890(7) 0.040(3) Uani 1 1 d . . . H28A H 0.6452 0.1409 1.0055 0.048 Uiso 1 1 calc R . . H28B H 0.6957 0.1922 0.9949 0.048 Uiso 1 1 calc R . . C29 C 0.7292(5) 0.1061(6) 1.0572(7) 0.035(3) Uani 1 1 d . . . C30 C 0.7671(5) 0.1415(6) 1.1243(8) 0.037(3) Uani 1 1 d . . . C31 C 0.8089(5) 0.1056(6) 1.1865(7) 0.033(2) Uani 1 1 d . . . C32 C 0.8139(5) 0.0374(6) 1.1826(7) 0.034(2) Uani 1 1 d . . . C33 C 0.7734(5) 0.0014(5) 1.1180(7) 0.034(2) Uani 1 1 d . . . C34 C 0.7312(5) 0.0372(6) 1.0570(7) 0.037(3) Uani 1 1 d . . . C35 C 0.7623(6) 0.2162(6) 1.1289(9) 0.046(3) Uani 1 1 d . . . H35A H 0.7878 0.2323 1.1834 0.069 Uiso 1 1 calc R . . H35B H 0.7210 0.2285 1.1282 0.069 Uiso 1 1 calc R . . H35C H 0.7748 0.2361 1.0781 0.069 Uiso 1 1 calc R . . C36 C 0.8485(5) 0.1427(6) 1.2610(7) 0.036(3) Uani 1 1 d . . . H36A H 0.8272 0.1821 1.2766 0.044 Uiso 1 1 calc R . . H36B H 0.8580 0.1137 1.3136 0.044 Uiso 1 1 calc R . . N5 N 0.9042(4) 0.1638(4) 1.2358(5) 0.0281(19) Uani 1 1 d . . . C37 C 0.9103(5) 0.1852(5) 1.1569(6) 0.028(2) Uani 1 1 d . . . H37 H 0.8792 0.1844 1.1061 0.033 Uiso 1 1 calc R . . N6 N 0.9645(4) 0.2078(4) 1.1567(5) 0.0283(19) Uani 1 1 d . . . C38 C 0.9948(5) 0.2006(5) 1.2449(7) 0.032(2) Uani 1 1 d . . . H38 H 1.0350 0.2126 1.2670 0.038 Uiso 1 1 calc R . . C39 C 0.9589(5) 0.1744(5) 1.2927(7) 0.030(2) Uani 1 1 d . . . H39 H 0.9685 0.1648 1.3539 0.036 Uiso 1 1 calc R . . C40 C 0.8616(5) 0.0019(6) 1.2477(7) 0.040(3) Uani 1 1 d . . . H40A H 0.8488 -0.0032 1.3037 0.060 Uiso 1 1 calc R . . H40B H 0.8983 0.0278 1.2571 0.060 Uiso 1 1 calc R . . H40C H 0.8685 -0.0419 1.2244 0.060 Uiso 1 1 calc R . . C41 C 0.6843(5) -0.0023(6) 0.9936(8) 0.043(3) Uani 1 1 d . . . H41A H 0.6502 0.0263 0.9707 0.064 Uiso 1 1 calc R . . H41B H 0.6713 -0.0399 1.0249 0.064 Uiso 1 1 calc R . . H41C H 0.7011 -0.0186 0.9446 0.064 Uiso 1 1 calc R . . C42 C 0.7739(6) -0.0738(5) 1.1164(7) 0.039(3) Uani 1 1 d . . . H42A H 0.7375 -0.0891 1.1349 0.046 Uiso 1 1 calc R . . H42B H 0.8080 -0.0885 1.1623 0.046 Uiso 1 1 calc R . . C43 C 0.7775(5) -0.1106(5) 1.0321(7) 0.031(2) Uani 1 1 d . . . C44 C 0.7388(5) -0.1658(5) 1.0073(8) 0.037(3) Uani 1 1 d . . . C45 C 0.7444(5) -0.2035(5) 0.9309(7) 0.036(3) Uani 1 1 d . . . C46 C 0.7824(5) -0.1842(5) 0.8798(7) 0.034(3) Uani 1 1 d . . . C47 C 0.8204(5) -0.1287(5) 0.9036(7) 0.031(2) Uani 1 1 d . . . C48 C 0.8177(5) -0.0946(5) 0.9816(6) 0.028(2) Uani 1 1 d . . . C49 C 0.6929(7) -0.1859(7) 1.0607(10) 0.061(4) Uani 1 1 d . . . H49A H 0.7131 -0.2055 1.1167 0.092 Uiso 1 1 calc R . . H49B H 0.6656 -0.2185 1.0273 0.092 Uiso 1 1 calc R . . H49C H 0.6705 -0.1468 1.0722 0.092 Uiso 1 1 calc R . . C50 C 0.7037(6) -0.2632(6) 0.9076(8) 0.042(3) Uani 1 1 d . . . H50A H 0.7256 -0.2988 0.8838 0.050 Uiso 1 1 calc R . . H50B H 0.6927 -0.2803 0.9619 0.050 Uiso 1 1 calc R . . N7 N 0.6501(5) -0.2477(5) 0.8435(7) 0.053(3) Uani 1 1 d D . . C51 C 0.6419(6) -0.2050(6) 0.7759(7) 0.043(3) Uani 1 1 d D . . H51 H 0.6725 -0.1773 0.7632 0.052 Uiso 1 1 calc R . . N8 N 0.5883(5) -0.2051(5) 0.7296(8) 0.065(4) Uani 1 1 d D . . C52 C 0.5540(7) -0.2431(6) 0.7781(9) 0.051 Uani 1 1 d D . . H52 H 0.5121 -0.2488 0.7640 0.061 Uiso 1 1 calc R . . C53 C 0.5932(6) -0.2706(6) 0.8506(9) 0.051 Uani 1 1 d D . . H53 H 0.5837 -0.2986 0.8950 0.061 Uiso 1 1 calc R . . C54 C 0.7900(6) -0.2240(6) 0.7973(8) 0.047(3) Uani 1 1 d . . . H54A H 0.8299 -0.2432 0.8076 0.070 Uiso 1 1 calc R . . H54B H 0.7844 -0.1943 0.7462 0.070 Uiso 1 1 calc R . . H54C H 0.7604 -0.2596 0.7861 0.070 Uiso 1 1 calc R . . C55 C 0.8632(5) -0.0411(6) 1.0131(7) 0.035(3) Uani 1 1 d . . . H55A H 0.8483 0.0015 0.9873 0.052 Uiso 1 1 calc R . . H55B H 0.9003 -0.0521 0.9949 0.052 Uiso 1 1 calc R . . H55C H 0.8704 -0.0381 1.0775 0.052 Uiso 1 1 calc R . . C56 C 0.8640(5) -0.1106(5) 0.8458(8) 0.030(2) Uani 1 1 d . . . H56A H 0.8526 -0.1358 0.7900 0.036 Uiso 1 1 calc R . . H56B H 0.9037 -0.1267 0.8757 0.036 Uiso 1 1 calc R . . C57 C 0.0245(7) 0.9950(13) 0.4859(13) 0.22(2) Uani 1 1 d D . . H57A H 0.0316 0.9466 0.4853 0.267 Uiso 1 1 calc R . . H57B H 0.0577 1.0147 0.5291 0.267 Uiso 1 1 calc R . . Cl1 Cl 0.0273(2) 1.0265(2) 0.3807(2) 0.0639(10) Uani 1 1 d D . . C58 C 0.1732(12) 0.4056(7) 0.9799(13) 0.064 Uani 0.650(6) 1 d PD A 1 H58A H 0.1308 0.4132 0.9804 0.077 Uiso 0.650(6) 1 calc PR A 1 H58B H 0.1949 0.4002 1.0416 0.077 Uiso 0.650(6) 1 calc PR A 1 C59 C 0.1946(12) 0.4574(7) 0.9441(15) 0.071(7) Uani 0.650(6) 1 d PD A 1 H59A H 0.1747 0.4610 0.8813 0.086 Uiso 0.650(6) 1 calc PR A 1 H59B H 0.2375 0.4511 0.9471 0.086 Uiso 0.650(6) 1 calc PR A 1 Cl2 Cl 0.1805(2) 0.3323(3) 0.9193(4) 0.0539(15) Uani 0.650(6) 1 d PD A 1 Cl3 Cl 0.1832(4) 0.5320(3) 1.0002(6) 0.095(3) Uani 0.650(6) 1 d PD A 1 C60 C 0.347(4) 0.426(3) 0.231(8) 0.133 Uani 0.150(6) 1 d PD A 2 H60A H 0.3699 0.3915 0.2065 0.159 Uiso 0.150(6) 1 calc PR A 2 H60B H 0.3164 0.4035 0.2565 0.159 Uiso 0.150(6) 1 calc PR A 2 C61 C 0.321(3) 0.467(5) 0.166(5) 0.133 Uani 0.150(6) 1 d PD A 2 H61A H 0.3454 0.4696 0.1206 0.159 Uiso 0.150(6) 1 calc PR A 2 H61B H 0.3185 0.5120 0.1904 0.159 Uiso 0.150(6) 1 calc PR A 2 Cl4 Cl 0.2507(18) 0.4389(18) 0.119(4) 0.133 Uani 0.150(6) 1 d PD A 2 Cl5 Cl 0.3947(19) 0.4703(18) 0.313(3) 0.133 Uani 0.150(6) 1 d PD A 2 Cl7 Cl 0.7230(6) 0.3303(5) 0.9099(11) 0.133 Uani 0.50 1 d PD . . Cl8 Cl 0.5995(6) 0.2856(5) 0.6829(10) 0.133 Uani 0.50 1 d PD . . C63 C 0.6628(13) 0.286(2) 0.7670(19) 0.133 Uani 0.50 1 d PD . . H63A H 0.6771 0.2396 0.7780 0.159 Uiso 0.50 1 calc PR . . H63B H 0.6944 0.3114 0.7473 0.159 Uiso 0.50 1 calc PR . . C62 C 0.6538(12) 0.312(2) 0.8419(17) 0.133 Uani 0.50 1 d PD . . H62A H 0.6321 0.2794 0.8718 0.159 Uiso 0.50 1 calc PR . . H62B H 0.6296 0.3523 0.8296 0.159 Uiso 0.50 1 calc PR . . O1 O 0.5604(9) 0.9109(11) 0.9020(12) 0.095(3) Uani 0.50 1 d PD . . C64 C 0.5455(14) 0.884(2) 0.986(2) 0.095(3) Uani 0.50 1 d PD . . 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 0.0355(8) 0.0280(7) 0.0191(7) -0.0016(6) 0.0028(5) -0.0010(6) Br1 0.0468(7) 0.0392(7) 0.0383(6) -0.0102(5) 0.0110(5) -0.0122(5) Br2 0.0463(7) 0.0690(9) 0.0292(6) 0.0155(6) 0.0050(5) 0.0148(6) Co2 0.0650(12) 0.0316(9) 0.0368(9) 0.0002(7) -0.0179(8) -0.0035(8) Br3 0.0615(9) 0.0566(9) 0.0510(8) -0.0098(7) 0.0019(7) 0.0215(7) Br4 0.1196(16) 0.0465(9) 0.0821(12) 0.0107(8) -0.0618(11) -0.0269(9) C1 0.039(6) 0.021(5) 0.020(5) -0.004(4) -0.003(4) 0.006(4) C2 0.034(6) 0.024(5) 0.022(5) -0.007(4) -0.004(4) 0.000(4) C3 0.039(6) 0.019(5) 0.016(4) -0.004(4) 0.002(4) -0.006(4) C4 0.050(7) 0.021(5) 0.018(5) -0.003(4) 0.001(4) 0.001(5) C5 0.024(5) 0.020(5) 0.024(5) -0.002(4) -0.006(4) -0.002(4) C6 0.034(6) 0.030(5) 0.020(5) -0.003(4) -0.008(4) -0.003(4) C7 0.032(6) 0.018(5) 0.044(6) 0.003(5) 0.002(5) -0.002(4) C8 0.032(6) 0.030(6) 0.037(6) -0.007(5) 0.012(5) 0.000(5) N1 0.030(5) 0.022(4) 0.023(4) 0.000(3) -0.001(3) 0.001(4) C9 0.027(5) 0.033(6) 0.025(5) 0.001(4) 0.002(4) -0.003(4) N2 0.031(5) 0.026(4) 0.025(4) -0.004(4) 0.006(3) -0.004(4) C10 0.035(6) 0.029(6) 0.030(6) 0.002(5) -0.002(4) -0.004(5) C11 0.031(6) 0.029(5) 0.029(5) -0.001(5) 0.007(4) -0.003(4) C12 0.040(6) 0.035(6) 0.032(6) 0.009(5) 0.003(5) -0.008(5) C13 0.038(6) 0.020(5) 0.044(6) 0.004(5) -0.006(5) -0.006(4) C14 0.045(7) 0.025(5) 0.032(6) 0.006(5) 0.005(5) 0.000(5) C15 0.038(6) 0.020(5) 0.028(5) -0.004(4) -0.018(4) -0.004(4) C16 0.037(6) 0.017(5) 0.044(7) -0.001(5) -0.016(5) 0.005(4) C17 0.037(6) 0.025(5) 0.047(7) -0.005(5) -0.013(5) 0.008(5) C18 0.034(6) 0.031(6) 0.049(7) -0.016(5) -0.004(5) 0.005(5) C19 0.038(6) 0.028(6) 0.031(6) -0.002(5) -0.008(5) 0.006(5) C20 0.031(6) 0.024(5) 0.036(6) -0.008(5) -0.009(4) 0.005(4) C21 0.054(8) 0.048(7) 0.033(6) 0.000(6) -0.015(5) 0.013(6) C22 0.038(7) 0.032(6) 0.064(9) -0.010(6) -0.011(6) 0.012(5) N3 0.030(5) 0.042(6) 0.034(5) -0.008(4) -0.010(4) 0.000(4) C23 0.045(7) 0.042(7) 0.042(7) 0.003(6) -0.009(5) 0.007(6) N4 0.041(6) 0.050(6) 0.033(5) -0.007(5) -0.010(4) -0.004(5) C24 0.041(7) 0.064(9) 0.053(8) -0.007(7) -0.007(6) -0.012(7) C25 0.032(7) 0.072(10) 0.056(8) -0.015(8) -0.006(6) 0.005(6) C26 0.041(7) 0.057(8) 0.049(8) -0.010(7) 0.002(6) 0.008(6) C27 0.041(7) 0.031(6) 0.039(6) -0.003(5) -0.007(5) 0.001(5) C28 0.053(7) 0.035(6) 0.027(6) -0.011(5) -0.002(5) 0.010(5) C29 0.038(6) 0.033(6) 0.033(6) -0.011(5) 0.003(5) -0.005(5) C30 0.039(6) 0.033(6) 0.036(6) -0.014(5) 0.004(5) -0.014(5) C31 0.040(6) 0.042(6) 0.017(5) -0.001(5) 0.008(4) -0.012(5) C32 0.043(7) 0.031(6) 0.028(5) -0.005(5) 0.003(5) -0.008(5) C33 0.037(6) 0.029(6) 0.035(6) -0.001(5) 0.006(5) -0.013(5) C34 0.039(6) 0.040(6) 0.027(5) -0.003(5) -0.004(5) -0.009(5) C35 0.048(7) 0.034(6) 0.048(7) -0.016(6) -0.004(6) -0.010(6) C36 0.042(7) 0.037(6) 0.028(6) -0.012(5) 0.004(5) -0.003(5) N5 0.033(5) 0.031(5) 0.020(4) -0.004(4) 0.004(3) -0.012(4) C37 0.032(6) 0.031(5) 0.015(4) -0.005(4) -0.006(4) -0.001(4) N6 0.038(5) 0.025(4) 0.019(4) -0.008(3) -0.001(3) 0.001(4) C38 0.038(6) 0.030(6) 0.025(5) -0.001(5) -0.002(4) 0.001(5) C39 0.035(6) 0.037(6) 0.016(5) -0.007(4) 0.000(4) -0.001(5) C40 0.042(7) 0.042(7) 0.028(6) -0.001(5) -0.011(5) 0.001(5) C41 0.036(6) 0.038(7) 0.045(7) -0.008(6) -0.014(5) -0.008(5) C42 0.048(7) 0.029(6) 0.033(6) 0.002(5) -0.005(5) -0.013(5) C43 0.038(6) 0.019(5) 0.031(6) 0.010(4) -0.008(5) 0.002(4) C44 0.036(6) 0.027(6) 0.043(7) 0.012(5) -0.004(5) -0.013(5) C45 0.050(7) 0.015(5) 0.033(6) 0.003(4) -0.011(5) -0.014(5) C46 0.043(6) 0.023(5) 0.029(6) 0.006(4) -0.012(5) -0.008(5) C47 0.030(5) 0.019(5) 0.034(6) 0.005(4) -0.015(4) 0.001(4) C48 0.032(5) 0.018(5) 0.025(5) 0.006(4) -0.013(4) -0.006(4) C49 0.071(10) 0.051(8) 0.061(9) -0.012(7) 0.012(8) -0.033(8) C50 0.059(8) 0.028(6) 0.032(6) 0.008(5) -0.006(5) -0.021(5) N7 0.055(7) 0.054(7) 0.040(6) 0.020(5) -0.015(5) -0.034(5) C51 0.054(8) 0.043(7) 0.026(6) 0.009(5) -0.007(5) -0.004(6) N8 0.067(8) 0.046(7) 0.063(8) 0.020(6) -0.030(6) -0.028(6) C52 0.062 0.035 0.051 0.000 0.000 0.000 C53 0.062 0.035 0.051 0.000 0.000 0.000 C54 0.054(8) 0.030(6) 0.047(7) -0.008(6) -0.012(6) -0.004(5) C55 0.037(6) 0.037(6) 0.026(5) -0.003(5) -0.004(4) -0.008(5) C56 0.033(6) 0.013(4) 0.044(6) 0.004(4) 0.005(5) -0.007(4) C57 0.44(7) 0.14(2) 0.14(2) -0.09(2) 0.19(3) -0.17(4) Cl1 0.089(3) 0.063(2) 0.0393(18) 0.0006(17) 0.0130(18) -0.006(2) C58 0.090 0.064 0.039 0.001 0.013 0.000 C59 0.072(17) 0.086(18) 0.063(15) 0.025(14) 0.030(13) 0.001(14) Cl2 0.046(3) 0.051(3) 0.072(4) 0.023(3) 0.028(3) 0.003(2) Cl3 0.120(7) 0.054(4) 0.118(7) -0.012(4) 0.042(5) -0.024(4) C60 0.108 0.065 0.210 0.000 0.000 0.033 C61 0.108 0.065 0.210 0.000 0.000 0.033 Cl4 0.108 0.065 0.210 0.000 0.000 0.033 Cl5 0.108 0.065 0.210 0.000 0.000 0.033 Cl7 0.108 0.065 0.210 0.000 0.000 0.033 Cl8 0.108 0.065 0.210 0.000 0.000 0.033 C63 0.108 0.065 0.210 0.000 0.000 0.033 C62 0.108 0.065 0.210 0.000 0.000 0.033 O1 0.120(7) 0.054(4) 0.118(7) -0.012(4) 0.042(5) -0.024(4) C64 0.120(7) 0.054(4) 0.118(7) -0.012(4) 0.042(5) -0.024(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N2 1.988(8) . ? Co1 N6 1.994(9) . ? Co1 Br1 2.3873(18) . ? Co1 Br2 2.3879(19) . ? Co2 N4 2.000(11) . ? Co2 N8 2.015(11) . ? Co2 Br4 2.376(2) . ? Co2 Br3 2.395(3) . ? C1 C2 1.401(15) . ? C1 C6 1.428(14) . ? C1 C56 1.549(13) . ? C2 C3 1.402(14) . ? C2 C7 1.492(14) . ? C3 C4 1.404(15) . ? C3 C8 1.523(15) . ? C4 C5 1.389(15) . ? C4 C12 1.531(15) . ? C5 C6 1.371(14) . ? C5 C14 1.525(14) . ? C6 C13 1.495(15) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 N1 1.490(13) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? N1 C9 1.337(13) . ? N1 C11 1.347(13) . ? C9 N2 1.328(13) . ? C9 H9 0.9500 . ? N2 C10 1.377(14) . ? C10 C11 1.354(15) . ? 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 1.535(16) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.416(14) . ? C15 C20 1.421(15) . ? C16 C17 1.380(18) . ? C16 C21 1.507(17) . ? C17 C18 1.404(17) . ? C17 C22 1.517(15) . ? C18 C19 1.395(15) . ? C18 C26 1.501(18) . ? C19 C20 1.418(17) . ? C19 C28 1.533(15) . ? C20 C27 1.492(15) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 N3 1.471(15) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? N3 C23 1.358(15) . ? N3 C25 1.364(15) . ? C23 N4 1.335(16) . ? C23 H23 0.9500 . ? N4 C24 1.374(17) . ? C24 C25 1.36(2) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.533(16) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C34 1.390(16) . ? C29 C30 1.407(14) . ? C30 C31 1.413(16) . ? C30 C35 1.514(16) . ? C31 C32 1.383(16) . ? C31 C36 1.514(14) . ? C32 C33 1.419(15) . ? C32 C40 1.510(15) . ? C33 C34 1.407(16) . ? C33 C42 1.517(15) . ? C34 C41 1.527(14) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 N5 1.479(14) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? N5 C37 1.331(13) . ? N5 C39 1.397(13) . ? C37 N6 1.329(13) . ? C37 H37 0.9500 . ? N6 C38 1.409(13) . ? C38 C39 1.329(16) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C43 1.521(16) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C48 1.370(16) . ? C43 C44 1.429(14) . ? C44 C45 1.436(17) . ? C44 C49 1.527(18) . ? C45 C46 1.353(17) . ? C45 C50 1.523(14) . ? C46 C47 1.423(14) . ? C46 C54 1.550(17) . ? C47 C48 1.405(15) . ? C47 C56 1.521(16) . ? C48 C55 1.512(14) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 N7 1.450(15) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? N7 C51 1.340(15) . ? N7 C53 1.416(17) . ? C51 N8 1.293(16) . ? C51 H51 0.9500 . ? N8 C52 1.424(19) . ? C52 C53 1.403(19) . ? C52 H52 0.9500 . ? C53 H53 0.9500 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C57 1.31(2) 3_576 ? C57 Cl1 1.764(16) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 C59 1.325(16) . ? C58 Cl2 1.779(14) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 Cl3 1.784(14) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 C61 1.34(2) . ? C60 Cl5 1.74(2) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 Cl4 1.73(2) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? Cl7 C62 1.760(18) . ? Cl8 C63 1.743(17) . ? C63 C62 1.327(19) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? O1 C64 1.52(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Co1 N6 111.9(3) . . ? N2 Co1 Br1 107.5(2) . . ? N6 Co1 Br1 109.3(2) . . ? N2 Co1 Br2 105.8(3) . . ? N6 Co1 Br2 101.8(3) . . ? Br1 Co1 Br2 120.49(8) . . ? N4 Co2 N8 114.7(5) . . ? N4 Co2 Br4 106.2(3) . . ? N8 Co2 Br4 108.3(3) . . ? N4 Co2 Br3 102.0(3) . . ? N8 Co2 Br3 106.2(4) . . ? Br4 Co2 Br3 119.67(11) . . ? C2 C1 C6 120.6(9) . . ? C2 C1 C56 119.9(9) . . ? C6 C1 C56 119.3(9) . . ? C1 C2 C3 117.9(9) . . ? C1 C2 C7 121.5(9) . . ? C3 C2 C7 120.6(9) . . ? C2 C3 C4 121.2(10) . . ? C2 C3 C8 119.1(9) . . ? C4 C3 C8 119.6(9) . . ? C5 C4 C3 119.7(9) . . ? C5 C4 C12 120.3(10) . . ? C3 C4 C12 120.0(10) . . ? C6 C5 C4 120.7(9) . . ? C6 C5 C14 122.0(9) . . ? C4 C5 C14 117.1(9) . . ? C5 C6 C1 119.6(10) . . ? C5 C6 C13 120.7(9) . . ? C1 C6 C13 119.3(9) . . ? 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(8) . . ? 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 107.1(9) . . ? C9 N1 C8 127.1(9) . . ? C11 N1 C8 125.8(9) . . ? N2 C9 N1 112.1(9) . . ? N2 C9 H9 123.9 . . ? N1 C9 H9 123.9 . . ? C9 N2 C10 104.1(9) . . ? C9 N2 Co1 126.7(7) . . ? C10 N2 Co1 128.4(7) . . ? C11 C10 N2 109.8(9) . . ? C11 C10 H10 125.1 . . ? N2 C10 H10 125.1 . . ? N1 C11 C10 106.9(9) . . ? N1 C11 H11 126.6 . . ? C10 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 119.3(9) . . ? 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 . . ? C16 C15 C20 119.0(11) . . ? C16 C15 C14 119.9(10) . . ? C20 C15 C14 120.9(9) . . ? C17 C16 C15 120.1(11) . . ? C17 C16 C21 121.6(10) . . ? C15 C16 C21 118.2(12) . . ? C16 C17 C18 121.2(10) . . ? C16 C17 C22 118.8(11) . . ? C18 C17 C22 119.9(12) . . ? C19 C18 C17 119.3(12) . . ? C19 C18 C26 121.3(11) . . ? C17 C18 C26 119.4(11) . . ? C18 C19 C20 120.4(11) . . ? C18 C19 C28 119.8(11) . . ? C20 C19 C28 119.4(10) . . ? C19 C20 C15 119.2(10) . . ? C19 C20 C27 120.8(10) . . ? C15 C20 C27 120.0(11) . . ? 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 . . ? N3 C22 C17 113.0(9) . . ? N3 C22 H22A 109.0 . . ? C17 C22 H22A 109.0 . . ? N3 C22 H22B 109.0 . . ? C17 C22 H22B 109.0 . . ? H22A C22 H22B 107.8 . . ? C23 N3 C25 107.6(11) . . ? C23 N3 C22 127.0(10) . . ? C25 N3 C22 125.4(11) . . ? N4 C23 N3 110.6(11) . . ? N4 C23 H23 124.7 . . ? N3 C23 H23 124.7 . . ? C23 N4 C24 105.7(11) . . ? C23 N4 Co2 122.9(9) . . ? C24 N4 Co2 129.3(9) . . ? C25 C24 N4 109.7(11) . . ? C25 C24 H24 125.1 . . ? N4 C24 H24 125.1 . . ? N3 C25 C24 106.4(12) . . ? N3 C25 H25 126.8 . . ? C24 C25 H25 126.8 . . ? C18 C26 H26A 109.5 . . ? C18 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C18 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C20 C27 H27A 109.5 . . ? C20 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C20 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C19 C28 C29 119.4(9) . . ? C19 C28 H28A 107.5 . . ? C29 C28 H28A 107.5 . . ? C19 C28 H28B 107.5 . . ? C29 C28 H28B 107.5 . . ? H28A C28 H28B 107.0 . . ? C34 C29 C30 119.5(11) . . ? C34 C29 C28 121.8(10) . . ? C30 C29 C28 118.6(10) . . ? C29 C30 C31 118.4(10) . . ? C29 C30 C35 120.0(11) . . ? C31 C30 C35 121.6(10) . . ? C32 C31 C30 122.0(10) . . ? C32 C31 C36 118.9(10) . . ? C30 C31 C36 119.1(10) . . ? C31 C32 C33 119.5(11) . . ? C31 C32 C40 119.9(10) . . ? C33 C32 C40 120.6(10) . . ? C34 C33 C32 118.2(10) . . ? C34 C33 C42 120.6(10) . . ? C32 C33 C42 121.1(10) . . ? C29 C34 C33 122.0(10) . . ? C29 C34 C41 120.2(10) . . ? C33 C34 C41 117.6(10) . . ? C30 C35 H35A 109.5 . . ? C30 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C30 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N5 C36 C31 111.0(9) . . ? N5 C36 H36A 109.4 . . ? C31 C36 H36A 109.4 . . ? N5 C36 H36B 109.4 . . ? C31 C36 H36B 109.4 . . ? H36A C36 H36B 108.0 . . ? C37 N5 C39 106.1(8) . . ? C37 N5 C36 126.8(9) . . ? C39 N5 C36 126.5(9) . . ? N6 C37 N5 113.1(9) . . ? N6 C37 H37 123.5 . . ? N5 C37 H37 123.5 . . ? C37 N6 C38 103.9(9) . . ? C37 N6 Co1 125.2(7) . . ? C38 N6 Co1 129.1(7) . . ? C39 C38 N6 109.9(10) . . ? C39 C38 H38 125.0 . . ? N6 C38 H38 125.0 . . ? C38 C39 N5 107.1(9) . . ? C38 C39 H39 126.5 . . ? N5 C39 H39 126.5 . . ? C32 C40 H40A 109.5 . . ? C32 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C32 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C34 C41 H41A 109.5 . . ? C34 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C34 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C33 C42 C43 120.3(9) . . ? C33 C42 H42A 107.3 . . ? C43 C42 H42A 107.3 . . ? C33 C42 H42B 107.3 . . ? C43 C42 H42B 107.3 . . ? H42A C42 H42B 106.9 . . ? C48 C43 C44 119.2(10) . . ? C48 C43 C42 122.7(9) . . ? C44 C43 C42 118.0(10) . . ? C43 C44 C45 118.5(10) . . ? C43 C44 C49 121.7(11) . . ? C45 C44 C49 119.8(10) . . ? C46 C45 C44 120.7(9) . . ? C46 C45 C50 121.9(11) . . ? C44 C45 C50 117.3(11) . . ? C45 C46 C47 120.8(11) . . ? C45 C46 C54 122.1(10) . . ? C47 C46 C54 116.9(11) . . ? C48 C47 C46 118.3(11) . . ? C48 C47 C56 122.9(9) . . ? C46 C47 C56 118.8(10) . . ? C43 C48 C47 122.2(9) . . ? C43 C48 C55 119.3(10) . . ? C47 C48 C55 118.4(10) . . ? C44 C49 H49A 109.5 . . ? C44 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C44 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? N7 C50 C45 112.7(9) . . ? N7 C50 H50A 109.1 . . ? C45 C50 H50A 109.1 . . ? N7 C50 H50B 109.1 . . ? C45 C50 H50B 109.1 . . ? H50A C50 H50B 107.8 . . ? C51 N7 C53 106.8(11) . . ? C51 N7 C50 129.6(10) . . ? C53 N7 C50 123.1(10) . . ? N8 C51 N7 113.4(12) . . ? N8 C51 H51 123.3 . . ? N7 C51 H51 123.3 . . ? C51 N8 C52 106.2(11) . . ? C51 N8 Co2 125.8(10) . . ? C52 N8 Co2 127.6(9) . . ? C53 C52 N8 107.4(13) . . ? C53 C52 H52 126.3 . . ? N8 C52 H52 126.3 . . ? C52 C53 N7 105.1(12) . . ? C52 C53 H53 127.4 . . ? N7 C53 H53 127.4 . . ? C46 C54 H54A 109.5 . . ? C46 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C46 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C48 C55 H55A 109.5 . . ? C48 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C48 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C47 C56 C1 118.5(9) . . ? C47 C56 H56A 107.7 . . ? C1 C56 H56A 107.7 . . ? C47 C56 H56B 107.7 . . ? C1 C56 H56B 107.7 . . ? H56A C56 H56B 107.1 . . ? C57 C57 Cl1 117(2) 3_576 . ? C57 C57 H57A 108.1 3_576 . ? Cl1 C57 H57A 108.1 . . ? C57 C57 H57B 108.1 3_576 . ? Cl1 C57 H57B 108.1 . . ? H57A C57 H57B 107.3 . . ? C59 C58 Cl2 110.5(13) . . ? C59 C58 H58A 109.5 . . ? Cl2 C58 H58A 109.5 . . ? C59 C58 H58B 109.5 . . ? Cl2 C58 H58B 109.5 . . ? H58A C58 H58B 108.1 . . ? C58 C59 Cl3 110.9(12) . . ? C58 C59 H59A 109.5 . . ? Cl3 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? Cl3 C59 H59B 109.5 . . ? H59A C59 H59B 108.1 . . ? C61 C60 Cl5 110(2) . . ? C61 C60 H60A 109.6 . . ? Cl5 C60 H60A 109.7 . . ? C61 C60 H60B 109.7 . . ? Cl5 C60 H60B 109.7 . . ? H60A C60 H60B 108.2 . . ? C60 C61 Cl4 110(2) . . ? C60 C61 H61A 109.6 . . ? Cl4 C61 H61A 109.6 . . ? C60 C61 H61B 109.6 . . ? Cl4 C61 H61B 109.6 . . ? H61A C61 H61B 108.1 . . ? C62 C63 Cl8 113.4(18) . . ? C62 C63 H63A 108.9 . . ? Cl8 C63 H63A 108.9 . . ? C62 C63 H63B 108.9 . . ? Cl8 C63 H63B 108.9 . . ? H63A C63 H63B 107.7 . . ? C63 C62 Cl7 108.8(17) . . ? C63 C62 H62A 109.9 . . ? C63 C62 H62B 109.9 . . ? H62A C62 H62B 108.3 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.814 _refine_diff_density_min -1.836 _refine_diff_density_rms 0.238 # Attachment '4-CoCl2.cif' data_4-CoCl2 _database_code_depnum_ccdc_archive 'CCDC 702194' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C56 H64 Cl4 Co2 N8), 5(C H Cl3), 5(H2 O)' _chemical_formula_sum 'C117 H143 Cl23 Co4 N16 O5' _chemical_formula_weight 2904.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 17.2495(7) _cell_length_b 16.7771(7) _cell_length_c 26.0051(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.02(3) _cell_angle_gamma 90.00 _cell_volume 7525.8(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5398 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 21.83 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.282 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2992 _exptl_absorpt_coefficient_mu 0.891 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9161 _exptl_absorpt_correction_T_max 0.9485 _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 70441 _diffrn_reflns_av_R_equivalents 0.0931 _diffrn_reflns_av_sigmaI/netI 0.2113 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 26.57 _reflns_number_total 15298 _reflns_number_gt 5570 _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^+0.8215P] 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 15298 _refine_ls_number_parameters 734 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.2699 _refine_ls_R_factor_gt 0.1487 _refine_ls_wR_factor_ref 0.4410 _refine_ls_wR_factor_gt 0.3953 _refine_ls_goodness_of_fit_ref 1.184 _refine_ls_restrained_S_all 1.184 _refine_ls_shift/su_max 0.026 _refine_ls_shift/su_mean 0.012 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 0.82154(9) 0.08551(10) 0.77002(7) 0.0576(5) Uani 1 1 d . . . Cl1 Cl 0.89528(14) 0.00238(17) 0.71789(17) 0.0820(13) Uani 1 1 d . . . Cl2 Cl 0.81574(14) 0.10127(16) 0.85987(8) 0.0442(6) Uani 1 1 d . . . Co2 Co 0.67235(9) 0.15424(9) 0.24635(6) 0.0518(5) Uani 1 1 d . . . Cl3 Cl 0.60477(14) 0.06203(16) 0.29565(14) 0.0642(10) Uani 1 1 d . . . Cl4 Cl 0.67964(14) 0.18552(18) 0.15948(9) 0.0545(8) Uani 1 1 d . . . C1 C 0.8169(6) 0.3115(5) 0.5396(4) 0.039(2) Uani 1 1 d . . . C2 C 0.8482(6) 0.3304(5) 0.5889(4) 0.038(2) Uani 1 1 d . . . C3 C 0.9146(6) 0.2925(6) 0.6057(4) 0.041(2) Uani 1 1 d . . . C4 C 0.9494(7) 0.2300(6) 0.5758(4) 0.048(3) Uani 1 1 d . . . C5 C 0.9180(6) 0.2096(5) 0.5290(4) 0.037(2) Uani 1 1 d . . . C6 C 0.8551(6) 0.2551(6) 0.5092(4) 0.042(2) Uani 1 1 d . . . C7 C 0.8075(7) 0.3928(7) 0.6224(4) 0.060(3) Uani 1 1 d . . . H7A H 0.8101 0.3764 0.6585 0.091 Uiso 1 1 calc R . . H7B H 0.7532 0.3974 0.6119 0.091 Uiso 1 1 calc R . . H7C H 0.8333 0.4444 0.6182 0.091 Uiso 1 1 calc R . . C8 C 0.9504(7) 0.3172(6) 0.6562(4) 0.051(3) Uani 1 1 d . . . H8A H 1.0070 0.3074 0.6542 0.061 Uiso 1 1 calc R . . H8B H 0.9429 0.3754 0.6604 0.061 Uiso 1 1 calc R . . N1 N 0.9221(5) 0.2794(5) 0.7003(3) 0.044(2) Uani 1 1 d . . . C9 C 0.8851(7) 0.2070(7) 0.7017(4) 0.052(3) Uani 1 1 d . . . H9 H 0.8744 0.1755 0.6722 0.063 Uiso 1 1 calc R . . N2 N 0.8661(6) 0.1865(5) 0.7498(3) 0.051(2) Uani 1 1 d . . . C10 C 0.8965(7) 0.2485(7) 0.7798(4) 0.053(3) Uani 1 1 d . . . H10 H 0.8952 0.2504 0.8163 0.063 Uiso 1 1 calc R . . C11 C 0.9277(7) 0.3048(6) 0.7495(4) 0.047(3) Uani 1 1 d . . . H11 H 0.9498 0.3538 0.7606 0.057 Uiso 1 1 calc R . . C12 C 1.0168(7) 0.1875(8) 0.5984(5) 0.060(3) Uani 1 1 d . . . H12A H 1.0000 0.1356 0.6116 0.089 Uiso 1 1 calc R . . H12B H 1.0384 0.2192 0.6267 0.089 Uiso 1 1 calc R . . H12C H 1.0565 0.1797 0.5720 0.089 Uiso 1 1 calc R . . C13 C 0.8293(7) 0.2414(7) 0.4536(4) 0.052(3) Uani 1 1 d . . . H13A H 0.7890 0.2003 0.4527 0.078 Uiso 1 1 calc R . . H13B H 0.8738 0.2240 0.4330 0.078 Uiso 1 1 calc R . . H13C H 0.8087 0.2912 0.4394 0.078 Uiso 1 1 calc R . . C14 C 0.9579(6) 0.1458(6) 0.4971(4) 0.047(2) Uani 1 1 d . . . H14A H 0.9922 0.1733 0.4723 0.056 Uiso 1 1 calc R . . H14B H 0.9918 0.1152 0.5206 0.056 Uiso 1 1 calc R . . C15 C 0.9100(6) 0.0862(5) 0.4671(4) 0.040(2) Uani 1 1 d . . . C16 C 0.9249(6) 0.0707(6) 0.4162(4) 0.039(2) Uani 1 1 d . . . C17 C 0.8853(6) 0.0099(6) 0.3879(4) 0.045(2) Uani 1 1 d . . . C18 C 0.8266(6) -0.0298(6) 0.4140(4) 0.048(3) Uani 1 1 d . . . C19 C 0.8102(6) -0.0156(5) 0.4654(4) 0.042(2) Uani 1 1 d . . . C20 C 0.8550(6) 0.0384(5) 0.4939(4) 0.039(2) Uani 1 1 d . . . C21 C 0.9874(7) 0.1202(8) 0.3865(4) 0.060(3) Uani 1 1 d . . . H21A H 0.9874 0.1752 0.3991 0.089 Uiso 1 1 calc R . . H21B H 0.9753 0.1198 0.3496 0.089 Uiso 1 1 calc R . . H21C H 1.0386 0.0964 0.3920 0.089 Uiso 1 1 calc R . . C22 C 0.9088(7) -0.0076(6) 0.3356(4) 0.051(3) Uani 1 1 d . . . H22A H 0.8969 -0.0641 0.3280 0.062 Uiso 1 1 calc R . . H22B H 0.9656 -0.0006 0.3327 0.062 Uiso 1 1 calc R . . N3 N 0.8704(5) 0.0431(5) 0.2969(3) 0.048(2) Uani 1 1 d . . . C23 C 0.7949(7) 0.0688(7) 0.2980(4) 0.053(3) Uani 1 1 d . . . H23 H 0.7606 0.0585 0.3258 0.064 Uiso 1 1 calc R . . N4 N 0.7750(5) 0.1089(6) 0.2570(3) 0.049(2) Uani 1 1 d . . . C24 C 0.8400(8) 0.1070(8) 0.2260(5) 0.071(4) Uani 1 1 d . . . H24 H 0.8435 0.1290 0.1924 0.085 Uiso 1 1 calc R . . C25 C 0.8968(6) 0.0696(7) 0.2506(5) 0.052(3) Uani 1 1 d . . . H25 H 0.9480 0.0623 0.2379 0.062 Uiso 1 1 calc R . . C26 C 0.7821(8) -0.0937(7) 0.3841(4) 0.058(3) Uani 1 1 d . . . H26A H 0.7263 -0.0870 0.3900 0.088 Uiso 1 1 calc R . . H26B H 0.7982 -0.1467 0.3960 0.088 Uiso 1 1 calc R . . H26C H 0.7932 -0.0884 0.3473 0.088 Uiso 1 1 calc R . . C27 C 0.8486(7) 0.0452(7) 0.5514(4) 0.053(3) Uani 1 1 d . . . H27A H 0.8981 0.0639 0.5655 0.079 Uiso 1 1 calc R . . H27B H 0.8361 -0.0071 0.5660 0.079 Uiso 1 1 calc R . . H27C H 0.8076 0.0832 0.5601 0.079 Uiso 1 1 calc R . . C28 C 0.7481(6) -0.0656(6) 0.4943(4) 0.046(2) Uani 1 1 d . . . H28A H 0.7208 -0.0984 0.4683 0.056 Uiso 1 1 calc R . . H28B H 0.7760 -0.1028 0.5173 0.056 Uiso 1 1 calc R . . C29 C 0.6869(6) -0.0245(6) 0.5262(4) 0.038(2) Uani 1 1 d . . . C30 C 0.6728(6) -0.0513(5) 0.5762(4) 0.041(2) Uani 1 1 d . . . C31 C 0.6123(6) -0.0138(6) 0.6055(4) 0.043(2) Uani 1 1 d . . . C32 C 0.5717(6) 0.0513(6) 0.5860(4) 0.044(2) Uani 1 1 d . . . C33 C 0.5857(5) 0.0782(5) 0.5364(4) 0.037(2) Uani 1 1 d . . . C34 C 0.6411(6) 0.0394(5) 0.5051(4) 0.039(2) Uani 1 1 d . . . C35 C 0.7162(7) -0.1219(7) 0.5983(4) 0.055(3) Uani 1 1 d . . . H35A H 0.7038 -0.1274 0.6349 0.083 Uiso 1 1 calc R . . H35B H 0.7721 -0.1136 0.5942 0.083 Uiso 1 1 calc R . . H35C H 0.7008 -0.1705 0.5800 0.083 Uiso 1 1 calc R . . C36 C 0.5922(7) -0.0466(6) 0.6569(4) 0.045(2) Uani 1 1 d . . . H36A H 0.5351 -0.0449 0.6611 0.054 Uiso 1 1 calc R . . H36B H 0.6081 -0.1033 0.6582 0.054 Uiso 1 1 calc R . . N5 N 0.6278(5) -0.0048(5) 0.7003(3) 0.042(2) Uani 1 1 d . . . C37 C 0.7014(6) 0.0095(6) 0.7063(4) 0.048(3) Uani 1 1 d . . . H37 H 0.7387 -0.0038 0.6808 0.057 Uiso 1 1 calc R . . N6 N 0.7208(5) 0.0437(6) 0.7502(3) 0.053(2) Uani 1 1 d . . . C38 C 0.6489(7) 0.0466(7) 0.7785(5) 0.059(3) Uani 1 1 d . . . H38 H 0.6414 0.0649 0.8127 0.071 Uiso 1 1 calc R . . C39 C 0.5940(7) 0.0177(7) 0.7460(5) 0.056(3) Uani 1 1 d . . . H39 H 0.5403 0.0136 0.7536 0.068 Uiso 1 1 calc R . . C40 C 0.5097(7) 0.0940(8) 0.6191(5) 0.063(3) Uani 1 1 d . . . H40A H 0.5292 0.1465 0.6295 0.094 Uiso 1 1 calc R . . H40B H 0.4987 0.0621 0.6498 0.094 Uiso 1 1 calc R . . H40C H 0.4621 0.1006 0.5990 0.094 Uiso 1 1 calc R . . C41 C 0.6508(7) 0.0618(6) 0.4498(4) 0.053(3) Uani 1 1 d . . . H41A H 0.6013 0.0551 0.4318 0.080 Uiso 1 1 calc R . . H41B H 0.6900 0.0275 0.4339 0.080 Uiso 1 1 calc R . . H41C H 0.6673 0.1176 0.4474 0.080 Uiso 1 1 calc R . . C42 C 0.5354(6) 0.1459(6) 0.5145(4) 0.046(2) Uani 1 1 d . . . H42A H 0.5014 0.1654 0.5425 0.055 Uiso 1 1 calc R . . H42B H 0.5015 0.1230 0.4876 0.055 Uiso 1 1 calc R . . C43 C 0.5781(6) 0.2194(5) 0.4909(4) 0.038(2) Uani 1 1 d . . . C44 C 0.5469(6) 0.2537(6) 0.4464(4) 0.048(3) Uani 1 1 d . . . C45 C 0.5818(6) 0.3232(6) 0.4253(4) 0.046(2) Uani 1 1 d . . . C46 C 0.6513(6) 0.3527(5) 0.4475(4) 0.039(2) Uani 1 1 d . . . C47 C 0.6827(6) 0.3196(6) 0.4913(4) 0.045(2) Uani 1 1 d . . . C48 C 0.6421(6) 0.2551(5) 0.5162(4) 0.039(2) Uani 1 1 d . . . C49 C 0.4788(9) 0.2209(8) 0.4216(6) 0.077(4) Uani 1 1 d . . . H49A H 0.4659 0.2530 0.3913 0.115 Uiso 1 1 calc R . . H49B H 0.4351 0.2215 0.4457 0.115 Uiso 1 1 calc R . . H49C H 0.4894 0.1659 0.4109 0.115 Uiso 1 1 calc R . . C50 C 0.5439(7) 0.3649(6) 0.3799(4) 0.053(3) Uani 1 1 d . . . H50A H 0.4869 0.3592 0.3823 0.063 Uiso 1 1 calc R . . H50B H 0.5564 0.4225 0.3810 0.063 Uiso 1 1 calc R . . N7 N 0.5711(5) 0.3309(5) 0.3307(3) 0.048(2) Uani 1 1 d . . . C51 C 0.6086(7) 0.2615(6) 0.3226(4) 0.050(3) Uani 1 1 d . . . H51 H 0.6244 0.2264 0.3493 0.060 Uiso 1 1 calc R . . N8 N 0.6207(7) 0.2483(5) 0.2744(4) 0.059(3) Uani 1 1 d . . . C52 C 0.5865(7) 0.3114(7) 0.2484(5) 0.057(3) Uani 1 1 d . . . H52 H 0.5854 0.3178 0.2122 0.068 Uiso 1 1 calc R . . C53 C 0.5542(7) 0.3635(6) 0.2838(4) 0.054(3) Uani 1 1 d . . . H53 H 0.5265 0.4113 0.2769 0.065 Uiso 1 1 calc R . . C54 C 0.6923(7) 0.4238(7) 0.4210(5) 0.060(3) Uani 1 1 d . . . H54A H 0.6986 0.4674 0.4457 0.090 Uiso 1 1 calc R . . H54B H 0.6609 0.4421 0.3919 0.090 Uiso 1 1 calc R . . H54C H 0.7434 0.4068 0.4086 0.090 Uiso 1 1 calc R . . C55 C 0.6674(7) 0.2278(7) 0.5684(4) 0.052(3) Uani 1 1 d . . . H55A H 0.7097 0.1892 0.5649 0.077 Uiso 1 1 calc R . . H55B H 0.6236 0.2027 0.5862 0.077 Uiso 1 1 calc R . . H55C H 0.6854 0.2737 0.5884 0.077 Uiso 1 1 calc R . . C56 C 0.7487(6) 0.3608(6) 0.5182(5) 0.049(3) Uani 1 1 d . . . H56A H 0.7263 0.3913 0.5473 0.059 Uiso 1 1 calc R . . H56B H 0.7705 0.4002 0.4939 0.059 Uiso 1 1 calc R . . C57 C 0.7082(18) 0.171(2) 0.9664(12) 0.087 Uani 0.50 1 d P . . H57 H 0.7272 0.1716 0.9301 0.104 Uiso 0.50 1 calc PR . . Cl5 Cl 0.6803(5) 0.0703(5) 0.9844(3) 0.087 Uani 0.50 1 d P . . Cl6 Cl 0.6349(6) 0.2345(5) 0.9732(8) 0.175(7) Uani 0.50 1 d P . . Cl7 Cl 0.7888(5) 0.2075(5) 1.0122(3) 0.087 Uani 0.50 1 d P . . C58 C 0.5107(15) 0.9611(13) 0.0810(8) 0.128 Uani 0.50 1 d PD . . H58 H 0.4662 0.9921 0.0667 0.154 Uiso 0.50 1 calc PR . . Cl8 Cl 0.5784(8) 1.0240(8) 0.1086(5) 0.136(4) Uani 0.50 1 d PD . . Cl9 Cl 0.5576(6) 0.9085(4) 0.0328(4) 0.104(3) Uani 0.50 1 d PD . . Cl10 Cl 0.4796(9) 0.8951(10) 0.1277(5) 0.173(6) Uani 0.50 1 d PD . . C59 C 0.6591(8) 0.8637(8) 0.2247(5) 0.085(4) Uiso 1 1 d D . . H59 H 0.6163 0.9020 0.2170 0.101 Uiso 1 1 calc R . . Cl11 Cl 0.7449(3) 0.9164(3) 0.21958(19) 0.1036(14) Uiso 1 1 d D . . Cl12 Cl 0.6433(4) 0.8284(4) 0.2857(2) 0.1287(18) Uiso 1 1 d D . . Cl13 Cl 0.6529(3) 0.7881(3) 0.1790(2) 0.1163(16) Uiso 1 1 d D . . C61 C 0.1267(8) 0.2062(9) 0.2534(5) 0.032(4) Uiso 0.50 1 d PD . . H61 H 0.1277 0.1468 0.2498 0.039 Uiso 0.50 1 calc PR . . Cl14 Cl 0.1781(5) 0.2541(5) 0.2041(3) 0.094(2) Uiso 0.50 1 d PD . . Cl15 Cl 0.0342(4) 0.2432(4) 0.2534(3) 0.0789(19) Uiso 0.50 1 d PD . . Cl16 Cl 0.1706(4) 0.2390(4) 0.3119(3) 0.0768(18) Uiso 0.50 1 d PD . . O1 O 0.9340(8) 0.9541(8) 0.9109(5) 0.113(4) Uiso 1 1 d . . . O2 O 0.0514(12) 0.8247(12) 0.9037(8) 0.178(7) Uiso 1 1 d . . . O3 O 0.5559(13) 0.5609(13) 0.4813(9) 0.091(6) Uiso 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 Co1 0.0445(9) 0.0646(10) 0.0636(10) -0.0172(8) -0.0046(7) -0.0130(7) Cl1 0.0215(11) 0.0545(16) 0.170(4) -0.071(2) 0.0219(16) -0.0082(11) Cl2 0.0449(13) 0.0661(15) 0.0217(10) -0.0141(10) 0.0037(9) -0.0312(11) Co2 0.0413(8) 0.0534(9) 0.0607(10) 0.0224(7) -0.0024(7) 0.0014(6) Cl3 0.0269(12) 0.0469(14) 0.119(3) 0.0482(16) 0.0263(14) 0.0063(10) Cl4 0.0362(12) 0.0895(19) 0.0379(13) 0.0471(13) 0.0065(10) 0.0222(12) C1 0.042(5) 0.032(5) 0.043(5) -0.004(4) -0.011(4) -0.003(4) C2 0.044(5) 0.034(5) 0.036(5) -0.001(4) 0.004(4) 0.002(4) C3 0.039(5) 0.049(5) 0.034(5) -0.001(4) -0.002(4) 0.002(4) C4 0.059(7) 0.036(5) 0.048(6) -0.004(4) -0.017(5) -0.001(5) C5 0.037(5) 0.042(5) 0.034(5) 0.001(4) 0.002(4) -0.002(4) C6 0.056(6) 0.043(5) 0.029(5) 0.000(4) -0.012(4) -0.003(5) C7 0.069(8) 0.053(6) 0.059(7) -0.023(5) -0.023(6) 0.006(6) C8 0.070(7) 0.036(5) 0.046(6) -0.007(5) -0.015(5) 0.005(5) N1 0.046(5) 0.040(4) 0.044(5) -0.005(4) -0.013(4) 0.000(4) C9 0.070(8) 0.055(6) 0.031(6) -0.007(5) -0.017(5) 0.001(5) N2 0.063(6) 0.046(5) 0.045(5) -0.007(4) -0.009(4) 0.005(4) C10 0.060(7) 0.068(7) 0.030(5) -0.009(5) -0.005(5) 0.001(6) C11 0.063(7) 0.042(5) 0.037(6) -0.013(5) -0.006(5) 0.012(5) C12 0.046(6) 0.073(8) 0.059(7) -0.025(6) -0.017(5) 0.014(6) C13 0.053(6) 0.064(7) 0.038(6) -0.009(5) -0.015(5) 0.013(5) C14 0.040(6) 0.046(6) 0.054(6) -0.011(5) -0.009(5) -0.003(4) C15 0.039(5) 0.039(5) 0.041(6) -0.005(4) 0.000(4) 0.002(4) C16 0.036(5) 0.044(5) 0.036(5) -0.008(4) -0.008(4) 0.003(4) C17 0.051(6) 0.045(5) 0.039(6) -0.003(4) -0.010(5) 0.013(5) C18 0.046(6) 0.036(5) 0.061(7) -0.009(5) -0.016(5) 0.010(4) C19 0.053(6) 0.033(5) 0.040(6) -0.007(4) -0.010(5) 0.007(4) C20 0.044(5) 0.037(5) 0.035(5) -0.006(4) -0.011(4) 0.006(4) C21 0.044(6) 0.080(8) 0.055(7) -0.011(6) 0.009(5) -0.001(6) C22 0.055(7) 0.051(6) 0.048(6) -0.020(5) -0.007(5) 0.012(5) N3 0.042(5) 0.056(5) 0.046(5) -0.009(4) -0.001(4) 0.013(4) C23 0.051(6) 0.061(7) 0.048(7) 0.002(5) 0.012(5) 0.009(5) N4 0.048(5) 0.065(5) 0.033(4) 0.007(4) 0.004(4) 0.009(4) C24 0.080(9) 0.072(8) 0.060(8) 0.018(7) 0.009(7) 0.004(7) C25 0.037(5) 0.062(7) 0.057(7) 0.017(6) 0.019(5) 0.010(5) C26 0.075(8) 0.058(7) 0.042(6) -0.027(5) -0.005(6) 0.006(6) C27 0.043(6) 0.057(7) 0.059(7) 0.003(5) -0.004(5) -0.006(5) C28 0.048(6) 0.039(5) 0.052(6) -0.005(5) -0.003(5) -0.005(5) C29 0.042(5) 0.041(5) 0.032(5) -0.011(4) -0.010(4) -0.002(4) C30 0.050(6) 0.026(4) 0.048(6) 0.003(4) -0.007(5) -0.006(4) C31 0.043(6) 0.042(5) 0.042(6) 0.007(4) -0.007(5) -0.016(4) C32 0.038(5) 0.046(6) 0.048(6) 0.001(5) -0.007(5) -0.002(4) C33 0.033(5) 0.043(5) 0.036(5) 0.007(4) -0.003(4) -0.005(4) C34 0.039(5) 0.038(5) 0.040(5) -0.001(4) -0.014(4) -0.003(4) C35 0.058(7) 0.056(6) 0.052(6) 0.004(5) -0.018(5) 0.000(5) C36 0.055(6) 0.047(6) 0.034(5) 0.007(4) -0.001(5) -0.001(5) N5 0.048(5) 0.051(5) 0.026(4) 0.005(3) -0.001(4) -0.015(4) C37 0.045(6) 0.062(6) 0.037(6) -0.006(5) -0.009(5) -0.008(5) N6 0.049(5) 0.070(6) 0.040(5) 0.003(4) 0.006(4) -0.008(4) C38 0.060(7) 0.058(7) 0.060(7) -0.001(6) 0.002(6) -0.010(6) C39 0.046(6) 0.053(6) 0.070(8) -0.004(6) 0.007(6) -0.012(5) C40 0.042(6) 0.085(9) 0.060(7) 0.006(6) 0.001(6) -0.001(6) C41 0.061(7) 0.045(6) 0.054(7) 0.004(5) -0.002(6) 0.004(5) C42 0.031(5) 0.059(6) 0.048(6) 0.001(5) -0.004(4) -0.004(4) C43 0.045(5) 0.027(4) 0.041(5) 0.000(4) -0.007(4) 0.007(4) C44 0.052(6) 0.051(6) 0.040(6) -0.003(5) -0.015(5) 0.005(5) C45 0.048(6) 0.042(5) 0.049(6) 0.003(5) -0.006(5) 0.009(4) C46 0.039(5) 0.034(5) 0.043(5) -0.002(4) -0.007(4) 0.005(4) C47 0.044(6) 0.033(5) 0.058(6) -0.005(4) -0.002(5) 0.007(4) C48 0.034(5) 0.035(5) 0.049(6) -0.004(4) 0.006(4) 0.007(4) C49 0.079(9) 0.065(8) 0.086(10) 0.024(7) -0.044(8) -0.013(7) C50 0.054(6) 0.041(5) 0.063(7) 0.003(5) -0.018(6) -0.004(5) N7 0.043(5) 0.052(5) 0.049(5) 0.003(4) -0.022(4) 0.001(4) C51 0.076(8) 0.045(6) 0.029(6) 0.012(4) -0.018(5) 0.011(5) N8 0.083(7) 0.043(5) 0.052(6) 0.016(4) -0.021(5) -0.009(5) C52 0.068(8) 0.052(6) 0.050(7) 0.017(5) -0.014(6) 0.006(6) C53 0.058(7) 0.043(6) 0.061(7) 0.024(5) -0.021(6) -0.007(5) C54 0.055(7) 0.052(6) 0.073(8) 0.014(6) -0.009(6) 0.003(5) C55 0.048(6) 0.057(6) 0.050(6) 0.004(5) 0.002(5) 0.002(5) C56 0.045(6) 0.032(5) 0.071(7) -0.002(5) -0.013(5) 0.004(4) C57 0.076 0.114 0.070 0.000 0.015 0.031 Cl5 0.076 0.114 0.070 0.000 0.015 0.031 Cl6 0.072(5) 0.050(4) 0.40(2) 0.007(8) 0.054(9) 0.011(4) Cl7 0.076 0.114 0.070 0.000 0.015 0.031 C58 0.131 0.129 0.124 0.000 0.008 0.024 Cl8 0.142(10) 0.143(9) 0.124(8) -0.050(7) -0.004(7) 0.048(8) Cl9 0.122(7) 0.056(4) 0.133(7) -0.009(4) 0.083(6) 0.017(4) Cl10 0.164(12) 0.226(15) 0.129(9) 0.070(10) 0.079(9) 0.057(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N2 1.933(9) . ? Co1 N6 1.943(9) . ? Co1 Cl1 2.324(3) . ? Co1 Cl2 2.354(3) . ? Co2 N4 1.946(9) . ? Co2 N8 1.954(11) . ? Co2 Cl4 2.323(3) . ? Co2 Cl3 2.323(3) . ? C1 C6 1.399(14) . ? C1 C2 1.426(13) . ? C1 C56 1.542(13) . ? C2 C3 1.381(14) . ? C2 C7 1.532(15) . ? C3 C4 1.436(15) . ? C3 C8 1.511(14) . ? C4 C5 1.375(14) . ? C4 C12 1.486(15) . ? C5 C6 1.423(14) . ? C5 C14 1.518(14) . ? C6 C13 1.530(13) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 N1 1.399(15) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? N1 C11 1.350(13) . ? N1 C9 1.373(14) . ? C9 N2 1.339(14) . ? C9 H9 0.9500 . ? N2 C10 1.403(14) . ? C10 C11 1.344(16) . ? 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 1.513(13) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.374(14) . ? C15 C20 1.425(14) . ? C16 C17 1.432(14) . ? C16 C21 1.564(15) . ? C17 C18 1.389(16) . ? C17 C22 1.448(15) . ? C18 C19 1.387(15) . ? C18 C26 1.530(15) . ? C19 C20 1.403(13) . ? C19 C28 1.555(15) . ? C20 C27 1.503(15) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 N3 1.476(14) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? N3 C25 1.362(14) . ? N3 C23 1.371(14) . ? C23 N4 1.308(14) . ? C23 H23 0.9500 . ? N4 C24 1.382(16) . ? C24 C25 1.329(17) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.509(14) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.398(14) . ? C29 C34 1.440(13) . ? C30 C31 1.436(15) . ? C30 C35 1.516(14) . ? C31 C32 1.393(14) . ? C31 C36 1.489(14) . ? C32 C33 1.387(14) . ? C32 C40 1.549(16) . ? C33 C34 1.416(14) . ? C33 C42 1.537(14) . ? C34 C41 1.496(15) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 N5 1.463(13) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? N5 C37 1.302(13) . ? N5 C39 1.377(15) . ? C37 N6 1.321(14) . ? C37 H37 0.9500 . ? N6 C38 1.444(16) . ? C38 C39 1.358(17) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C43 1.561(14) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.402(13) . ? C43 C48 1.417(14) . ? C44 C45 1.421(15) . ? C44 C49 1.449(16) . ? C45 C46 1.420(14) . ? C45 C50 1.522(14) . ? C46 C47 1.378(14) . ? C46 C54 1.548(15) . ? C47 C48 1.443(15) . ? C47 C56 1.503(14) . ? C48 C55 1.498(15) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 N7 1.476(15) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? N7 C51 1.350(14) . ? N7 C53 1.369(13) . ? C51 N8 1.290(15) . ? C51 H51 0.9500 . ? N8 C52 1.386(13) . ? C52 C53 1.386(17) . ? C52 H52 0.9500 . ? C53 H53 0.9500 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 Cl6 1.66(3) . ? C57 Cl5 1.82(4) . ? C57 Cl7 1.93(3) . ? C57 H57 1.0000 . ? C58 Cl10 1.729(19) . ? C58 Cl8 1.731(19) . ? C58 Cl9 1.732(18) . ? C58 H58 1.0000 . ? C59 Cl12 1.715(13) . ? C59 Cl11 1.729(13) . ? C59 Cl13 1.741(13) . ? C59 H59 1.0000 . ? C61 Cl15 1.712(14) . ? C61 Cl14 1.755(14) . ? C61 Cl16 1.785(14) . ? C61 H61 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 Co1 N6 126.8(4) . . ? N2 Co1 Cl1 98.6(3) . . ? N6 Co1 Cl1 96.8(3) . . ? N2 Co1 Cl2 100.9(3) . . ? N6 Co1 Cl2 105.4(3) . . ? Cl1 Co1 Cl2 132.05(15) . . ? N4 Co2 N8 132.7(4) . . ? N4 Co2 Cl4 100.2(3) . . ? N8 Co2 Cl4 101.9(3) . . ? N4 Co2 Cl3 96.8(3) . . ? N8 Co2 Cl3 95.9(3) . . ? Cl4 Co2 Cl3 135.60(15) . . ? C6 C1 C2 118.7(9) . . ? C6 C1 C56 121.2(8) . . ? C2 C1 C56 119.6(9) . . ? C3 C2 C1 119.7(9) . . ? C3 C2 C7 121.0(9) . . ? C1 C2 C7 119.3(9) . . ? C2 C3 C4 120.7(9) . . ? C2 C3 C8 119.2(9) . . ? C4 C3 C8 120.1(9) . . ? C5 C4 C3 119.7(9) . . ? C5 C4 C12 122.7(10) . . ? C3 C4 C12 117.5(9) . . ? C4 C5 C6 119.2(9) . . ? C4 C5 C14 118.7(9) . . ? C6 C5 C14 121.7(8) . . ? C1 C6 C5 121.1(8) . . ? C1 C6 C13 119.9(9) . . ? C5 C6 C13 118.9(9) . . ? 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 116.5(9) . . ? N1 C8 H8A 108.2 . . ? C3 C8 H8A 108.1 . . ? N1 C8 H8B 108.2 . . ? C3 C8 H8B 108.2 . . ? H8A C8 H8B 107.3 . . ? C11 N1 C9 106.8(9) . . ? C11 N1 C8 127.4(9) . . ? C9 N1 C8 125.7(8) . . ? N2 C9 N1 111.4(9) . . ? N2 C9 H9 124.3 . . ? N1 C9 H9 124.3 . . ? C9 N2 C10 103.7(9) . . ? C9 N2 Co1 125.3(7) . . ? C10 N2 Co1 130.3(7) . . ? C11 C10 N2 110.2(9) . . ? C11 C10 H10 124.9 . . ? N2 C10 H10 124.9 . . ? C10 C11 N1 107.8(9) . . ? C10 C11 H11 126.1 . . ? N1 C11 H11 126.1 . . ? 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 109.4 . . ? H13A C13 H13B 109.5 . . ? C6 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C5 120.0(9) . . ? C15 C14 H14A 107.3 . . ? C5 C14 H14A 107.3 . . ? C15 C14 H14B 107.3 . . ? C5 C14 H14B 107.3 . . ? H14A C14 H14B 106.9 . . ? C16 C15 C20 119.3(9) . . ? C16 C15 C14 121.4(9) . . ? C20 C15 C14 118.9(9) . . ? C15 C16 C17 122.8(10) . . ? C15 C16 C21 120.3(9) . . ? C17 C16 C21 116.9(9) . . ? C18 C17 C16 116.0(9) . . ? C18 C17 C22 124.4(10) . . ? C16 C17 C22 119.6(10) . . ? C19 C18 C17 122.5(9) . . ? C19 C18 C26 120.4(10) . . ? C17 C18 C26 117.0(10) . . ? C18 C19 C20 120.6(10) . . ? C18 C19 C28 120.9(9) . . ? C20 C19 C28 118.1(9) . . ? C19 C20 C15 118.2(9) . . ? C19 C20 C27 122.3(9) . . ? C15 C20 C27 119.5(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 . . ? C17 C22 N3 113.5(8) . . ? C17 C22 H22A 108.9 . . ? N3 C22 H22A 108.9 . . ? C17 C22 H22B 108.9 . . ? N3 C22 H22B 108.9 . . ? H22A C22 H22B 107.7 . . ? C25 N3 C23 103.6(9) . . ? C25 N3 C22 129.8(9) . . ? C23 N3 C22 126.3(10) . . ? N4 C23 N3 113.1(10) . . ? N4 C23 H23 123.4 . . ? N3 C23 H23 123.4 . . ? C23 N4 C24 104.5(10) . . ? C23 N4 Co2 123.8(8) . . ? C24 N4 Co2 131.6(8) . . ? C25 C24 N4 109.2(11) . . ? C25 C24 H24 125.4 . . ? N4 C24 H24 125.4 . . ? C24 C25 N3 109.4(10) . . ? C24 C25 H25 125.3 . . ? N3 C25 H25 125.3 . . ? C18 C26 H26A 109.5 . . ? C18 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C18 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C20 C27 H27A 109.5 . . ? C20 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C20 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C19 120.1(8) . . ? C29 C28 H28A 107.3 . . ? C19 C28 H28A 107.3 . . ? C29 C28 H28B 107.3 . . ? C19 C28 H28B 107.3 . . ? H28A C28 H28B 106.9 . . ? C30 C29 C34 119.9(9) . . ? C30 C29 C28 119.1(9) . . ? C34 C29 C28 120.9(9) . . ? C29 C30 C31 118.6(9) . . ? C29 C30 C35 121.2(10) . . ? C31 C30 C35 120.0(9) . . ? C32 C31 C30 121.0(9) . . ? C32 C31 C36 120.0(10) . . ? C30 C31 C36 119.0(9) . . ? C33 C32 C31 120.4(10) . . ? C33 C32 C40 119.1(9) . . ? C31 C32 C40 120.5(10) . . ? C32 C33 C34 120.2(9) . . ? C32 C33 C42 119.1(9) . . ? C34 C33 C42 120.5(8) . . ? C33 C34 C29 119.6(9) . . ? C33 C34 C41 120.8(9) . . ? C29 C34 C41 119.6(9) . . ? C30 C35 H35A 109.5 . . ? C30 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C30 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N5 C36 C31 114.6(8) . . ? N5 C36 H36A 108.6 . . ? C31 C36 H36A 108.6 . . ? N5 C36 H36B 108.6 . . ? C31 C36 H36B 108.6 . . ? H36A C36 H36B 107.6 . . ? C37 N5 C39 105.0(9) . . ? C37 N5 C36 126.2(9) . . ? C39 N5 C36 128.2(9) . . ? N5 C37 N6 115.6(10) . . ? N5 C37 H37 122.2 . . ? N6 C37 H37 122.2 . . ? C37 N6 C38 103.7(9) . . ? C37 N6 Co1 127.8(8) . . ? C38 N6 Co1 128.4(7) . . ? C39 C38 N6 105.6(10) . . ? C39 C38 H38 127.2 . . ? N6 C38 H38 127.2 . . ? C38 C39 N5 109.9(10) . . ? C38 C39 H39 125.0 . . ? N5 C39 H39 125.0 . . ? C32 C40 H40A 109.5 . . ? C32 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C32 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C34 C41 H41A 109.5 . . ? C34 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C34 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C33 C42 C43 117.6(8) . . ? C33 C42 H42A 107.9 . . ? C43 C42 H42A 107.9 . . ? C33 C42 H42B 107.9 . . ? C43 C42 H42B 107.9 . . ? H42A C42 H42B 107.2 . . ? C44 C43 C48 120.6(9) . . ? C44 C43 C42 117.9(9) . . ? C48 C43 C42 121.2(8) . . ? C43 C44 C45 119.5(9) . . ? C43 C44 C49 121.6(10) . . ? C45 C44 C49 118.9(9) . . ? C44 C45 C46 119.2(9) . . ? C44 C45 C50 119.6(9) . . ? C46 C45 C50 121.2(9) . . ? C47 C46 C45 121.8(9) . . ? C47 C46 C54 119.9(9) . . ? C45 C46 C54 118.3(9) . . ? C46 C47 C48 118.8(9) . . ? C46 C47 C56 119.8(9) . . ? C48 C47 C56 120.2(9) . . ? C43 C48 C47 119.1(9) . . ? C43 C48 C55 121.2(9) . . ? C47 C48 C55 119.7(9) . . ? C44 C49 H49A 109.5 . . ? C44 C49 H49B 109.4 . . ? H49A C49 H49B 109.5 . . ? C44 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? N7 C50 C45 111.0(9) . . ? N7 C50 H50A 109.4 . . ? C45 C50 H50A 109.5 . . ? N7 C50 H50B 109.4 . . ? C45 C50 H50B 109.4 . . ? H50A C50 H50B 108.0 . . ? C51 N7 C53 107.9(9) . . ? C51 N7 C50 128.4(8) . . ? C53 N7 C50 123.4(9) . . ? N8 C51 N7 112.1(8) . . ? N8 C51 H51 123.9 . . ? N7 C51 H51 123.9 . . ? C51 N8 C52 105.9(10) . . ? C51 N8 Co2 125.1(7) . . ? C52 N8 Co2 128.9(8) . . ? C53 C52 N8 109.3(10) . . ? C53 C52 H52 125.4 . . ? N8 C52 H52 125.4 . . ? N7 C53 C52 104.7(9) . . ? N7 C53 H53 127.6 . . ? C52 C53 H53 127.7 . . ? C46 C54 H54A 109.5 . . ? C46 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C46 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C48 C55 H55A 109.5 . . ? C48 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C48 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C47 C56 C1 119.9(8) . . ? C47 C56 H56A 107.3 . . ? C1 C56 H56A 107.3 . . ? C47 C56 H56B 107.4 . . ? C1 C56 H56B 107.4 . . ? H56A C56 H56B 106.9 . . ? Cl6 C57 Cl5 111.6(18) . . ? Cl6 C57 Cl7 106.1(18) . . ? Cl5 C57 Cl7 109.1(16) . . ? Cl6 C57 H57 109.9 . . ? Cl5 C57 H57 110.0 . . ? Cl7 C57 H57 110.0 . . ? Cl10 C58 Cl8 107.9(16) . . ? Cl10 C58 Cl9 109.1(13) . . ? Cl8 C58 Cl9 107.2(13) . . ? Cl10 C58 H58 110.8 . . ? Cl8 C58 H58 110.8 . . ? Cl9 C58 H58 110.8 . . ? Cl12 C59 Cl11 112.5(8) . . ? Cl12 C59 Cl13 111.7(8) . . ? Cl11 C59 Cl13 111.9(8) . . ? Cl12 C59 H59 106.7 . . ? Cl11 C59 H59 106.7 . . ? Cl13 C59 H59 106.8 . . ? Cl15 C61 Cl14 107.7(9) . . ? Cl15 C61 Cl16 106.5(8) . . ? Cl14 C61 Cl16 105.5(8) . . ? Cl15 C61 H61 112.2 . . ? Cl14 C61 H61 112.3 . . ? Cl16 C61 H61 112.2 . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 26.57 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.611 _refine_diff_density_min -1.435 _refine_diff_density_rms 0.202 # Attachment '4-CuBr2.cif' data_4-CuBr2 _database_code_depnum_ccdc_archive 'CCDC 702195' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '4(C56 H64 Br4 Cu2 N8), 11(C2 H4 Cl2)' _chemical_formula_sum 'C246 H300 Br16 Cl22 Cu8 N32' _chemical_formula_weight 6271.96 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' 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 23.0787(6) _cell_length_b 20.2256(5) _cell_length_c 15.4533(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.1210(10) _cell_angle_gamma 90.00 _cell_volume 7052.5(3) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7719 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 26.64 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.477 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3166 _exptl_absorpt_coefficient_mu 3.119 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6692 _exptl_absorpt_correction_T_max 0.7456 _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 52348 _diffrn_reflns_av_R_equivalents 0.0510 _diffrn_reflns_av_sigmaI/netI 0.0738 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 27.62 _reflns_number_total 15745 _reflns_number_gt 8982 _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^)+(0.1689P)^2^+20.1581P] 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 15745 _refine_ls_number_parameters 735 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.1468 _refine_ls_R_factor_gt 0.0856 _refine_ls_wR_factor_ref 0.3014 _refine_ls_wR_factor_gt 0.2549 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.003 _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 0.51323(4) 0.25892(5) 0.43851(6) 0.0313(3) Uani 1 1 d . . . Br1 Br 0.60676(4) 0.29986(5) 0.51393(6) 0.0467(3) Uani 1 1 d . . . Br2 Br 0.43469(4) 0.33281(4) 0.37816(6) 0.0406(2) Uani 1 1 d . . . Cu2 Cu 0.93989(6) -0.15163(6) 0.88243(7) 0.0473(3) Uani 1 1 d . . . Br3 Br 0.85352(5) -0.12182(5) 0.93609(7) 0.0517(3) Uani 1 1 d . . . Br4 Br 1.01668(6) -0.21212(6) 0.97408(8) 0.0775(4) Uani 1 1 d . . . C1 C 0.7704(3) 0.1037(4) 0.4420(5) 0.0273(16) Uani 1 1 d . . . C2 C 0.7324(4) 0.1391(4) 0.3739(5) 0.0304(17) Uani 1 1 d . . . C3 C 0.6908(3) 0.1039(4) 0.3120(5) 0.0282(16) Uani 1 1 d . . . C4 C 0.6860(3) 0.0356(4) 0.3161(5) 0.0259(16) Uani 1 1 d . . . C5 C 0.7258(3) 0.0002(4) 0.3815(5) 0.0268(16) Uani 1 1 d . . . C6 C 0.7687(3) 0.0348(4) 0.4418(5) 0.0278(16) Uani 1 1 d . . . C7 C 0.7372(4) 0.2134(4) 0.3700(6) 0.042(2) Uani 1 1 d . . . H7A H 0.7151 0.2334 0.4108 0.063 Uiso 1 1 calc R . . H7B H 0.7208 0.2286 0.3096 0.063 Uiso 1 1 calc R . . H7C H 0.7790 0.2263 0.3870 0.063 Uiso 1 1 calc R . . C8 C 0.6503(4) 0.1410(4) 0.2372(5) 0.0318(18) Uani 1 1 d . . . H8A H 0.6715 0.1802 0.2211 0.038 Uiso 1 1 calc R . . H8B H 0.6406 0.1120 0.1845 0.038 Uiso 1 1 calc R . . N1 N 0.5948(3) 0.1626(3) 0.2618(4) 0.0227(13) Uani 1 1 d . . . C9 C 0.5897(3) 0.1839(3) 0.3417(5) 0.0241(15) Uani 1 1 d . . . H9 H 0.6208 0.1828 0.3929 0.029 Uiso 1 1 calc R . . N2 N 0.5357(3) 0.2066(3) 0.3403(4) 0.0231(13) Uani 1 1 d . . . C10 C 0.5054(3) 0.1988(4) 0.2544(5) 0.0270(16) Uani 1 1 d . . . H10 H 0.4650 0.2103 0.2329 0.032 Uiso 1 1 calc R . . C11 C 0.5411(3) 0.1725(4) 0.2051(5) 0.0281(16) Uani 1 1 d . . . H11 H 0.5313 0.1627 0.1436 0.034 Uiso 1 1 calc R . . C12 C 0.6382(4) 0.0000(4) 0.2496(5) 0.0343(18) Uani 1 1 d . . . H12A H 0.6039 0.0292 0.2318 0.051 Uiso 1 1 calc R . . H12B H 0.6261 -0.0401 0.2768 0.051 Uiso 1 1 calc R . . H12C H 0.6538 -0.0121 0.1975 0.051 Uiso 1 1 calc R . . C13 C 0.8159(3) -0.0030(4) 0.5058(5) 0.0327(18) Uani 1 1 d . . . H13A H 0.8523 0.0233 0.5195 0.049 Uiso 1 1 calc R . . H13B H 0.8238 -0.0450 0.4790 0.049 Uiso 1 1 calc R . . H13C H 0.8020 -0.0117 0.5605 0.049 Uiso 1 1 calc R . . C14 C 0.7257(4) -0.0756(4) 0.3832(5) 0.0292(17) Uani 1 1 d . . . H14A H 0.7621 -0.0907 0.3648 0.035 Uiso 1 1 calc R . . H14B H 0.6917 -0.0906 0.3371 0.035 Uiso 1 1 calc R . . C15 C 0.7224(3) -0.1121(3) 0.4691(5) 0.0262(16) Uani 1 1 d . . . C16 C 0.7600(4) -0.1657(4) 0.4933(5) 0.0298(17) Uani 1 1 d . . . C17 C 0.7549(4) -0.2033(3) 0.5690(5) 0.0291(17) Uani 1 1 d . . . C18 C 0.7162(3) -0.1845(4) 0.6212(5) 0.0270(16) Uani 1 1 d . . . C19 C 0.6791(3) -0.1286(3) 0.5974(5) 0.0244(15) Uani 1 1 d . . . C20 C 0.6815(3) -0.0945(3) 0.5185(5) 0.0224(15) Uani 1 1 d . . . C21 C 0.8052(5) -0.1870(5) 0.4398(6) 0.051(3) Uani 1 1 d . . . H21A H 0.7868 -0.2187 0.3941 0.076 Uiso 1 1 calc R . . H21B H 0.8390 -0.2080 0.4791 0.076 Uiso 1 1 calc R . . H21C H 0.8188 -0.1483 0.4116 0.076 Uiso 1 1 calc R . . C22 C 0.7945(4) -0.2638(4) 0.5940(5) 0.037(2) Uani 1 1 d . . . H22A H 0.7724 -0.2980 0.6198 0.045 Uiso 1 1 calc R . . H22B H 0.8048 -0.2825 0.5399 0.045 Uiso 1 1 calc R . . N3 N 0.8490(4) -0.2472(4) 0.6578(6) 0.0635(13) Uani 1 1 d . . . C23 C 0.8572(5) -0.2045(5) 0.7244(7) 0.0635(13) Uani 1 1 d . . . H23 H 0.8269 -0.1759 0.7356 0.076 Uiso 1 1 calc R . . N4 N 0.9100(4) -0.2056(4) 0.7724(6) 0.0635(13) Uani 1 1 d . . . C24 C 0.9424(5) -0.2447(5) 0.7281(7) 0.0635(13) Uani 1 1 d . . . H24 H 0.9838 -0.2528 0.7453 0.076 Uiso 1 1 calc R . . C25 C 0.9057(5) -0.2701(5) 0.6555(7) 0.0635(13) Uani 1 1 d . . . H25 H 0.9164 -0.2979 0.6119 0.076 Uiso 1 1 calc R . . C26 C 0.7101(4) -0.2235(4) 0.7029(6) 0.0351(19) Uani 1 1 d . . . H26A H 0.7389 -0.2598 0.7122 0.053 Uiso 1 1 calc R . . H26B H 0.6699 -0.2417 0.6943 0.053 Uiso 1 1 calc R . . H26C H 0.7175 -0.1943 0.7546 0.053 Uiso 1 1 calc R . . C27 C 0.6363(4) -0.0407(4) 0.4876(5) 0.0279(16) Uani 1 1 d . . . H27A H 0.6520 0.0018 0.5127 0.042 Uiso 1 1 calc R . . H27B H 0.5996 -0.0510 0.5071 0.042 Uiso 1 1 calc R . . H27C H 0.6282 -0.0381 0.4228 0.042 Uiso 1 1 calc R . . C28 C 0.6359(3) -0.1092(3) 0.6552(5) 0.0253(15) Uani 1 1 d . . . H28A H 0.6471 -0.1343 0.7113 0.030 Uiso 1 1 calc R . . H28B H 0.5961 -0.1250 0.6253 0.030 Uiso 1 1 calc R . . C29 C 0.6298(3) -0.0365(3) 0.6793(4) 0.0203(14) Uani 1 1 d . . . C30 C 0.5737(3) -0.0075(3) 0.6693(4) 0.0207(14) Uani 1 1 d . . . C31 C 0.5688(3) 0.0560(3) 0.7035(4) 0.0210(14) Uani 1 1 d . . . C32 C 0.6198(3) 0.0932(3) 0.7383(4) 0.0238(15) Uani 1 1 d . . . C33 C 0.6760(3) 0.0657(3) 0.7439(4) 0.0228(15) Uani 1 1 d . . . C34 C 0.6808(3) 0.0001(3) 0.7185(4) 0.0209(14) Uani 1 1 d . . . C35 C 0.5179(3) -0.0441(4) 0.6271(5) 0.0298(17) Uani 1 1 d . . . H35A H 0.4990 -0.0618 0.6734 0.045 Uiso 1 1 calc R . . H35B H 0.5278 -0.0805 0.5910 0.045 Uiso 1 1 calc R . . H35C H 0.4905 -0.0136 0.5895 0.045 Uiso 1 1 calc R . . C36 C 0.5090(3) 0.0839(4) 0.7069(5) 0.0256(15) Uani 1 1 d . . . H36A H 0.4800 0.0472 0.7005 0.031 Uiso 1 1 calc R . . H36B H 0.5111 0.1042 0.7657 0.031 Uiso 1 1 calc R . . N5 N 0.4873(2) 0.1339(3) 0.6380(4) 0.0206(12) Uani 1 1 d . . . C37 C 0.5156(3) 0.1560(4) 0.5767(5) 0.0251(15) Uani 1 1 d . . . H37 H 0.5535 0.1411 0.5703 0.030 Uiso 1 1 calc R . . N6 N 0.4839(3) 0.2016(3) 0.5260(4) 0.0257(13) Uani 1 1 d . . . C38 C 0.4325(3) 0.2081(4) 0.5572(5) 0.0266(16) Uani 1 1 d . . . H38 H 0.4007 0.2371 0.5335 0.032 Uiso 1 1 calc R . . C39 C 0.4341(3) 0.1668(4) 0.6269(5) 0.0241(15) Uani 1 1 d . . . H39 H 0.4046 0.1617 0.6609 0.029 Uiso 1 1 calc R . . C40 C 0.6134(4) 0.1632(4) 0.7723(6) 0.0342(18) Uani 1 1 d . . . H40A H 0.6366 0.1672 0.8329 0.051 Uiso 1 1 calc R . . H40B H 0.5716 0.1721 0.7716 0.051 Uiso 1 1 calc R . . H40C H 0.6279 0.1951 0.7341 0.051 Uiso 1 1 calc R . . C41 C 0.7411(3) -0.0334(4) 0.7367(5) 0.0312(17) Uani 1 1 d . . . H41A H 0.7592 -0.0284 0.6851 0.047 Uiso 1 1 calc R . . H41B H 0.7363 -0.0805 0.7484 0.047 Uiso 1 1 calc R . . H41C H 0.7666 -0.0129 0.7884 0.047 Uiso 1 1 calc R . . C42 C 0.7302(4) 0.1055(4) 0.7856(5) 0.0317(17) Uani 1 1 d . . . H42A H 0.7452 0.0872 0.8455 0.038 Uiso 1 1 calc R . . H42B H 0.7166 0.1511 0.7936 0.038 Uiso 1 1 calc R . . C43 C 0.7827(3) 0.1108(3) 0.7411(5) 0.0254(15) Uani 1 1 d . . . C44 C 0.8406(4) 0.1057(4) 0.7932(5) 0.0335(18) Uani 1 1 d . . . C45 C 0.8885(3) 0.1101(4) 0.7512(5) 0.0307(17) Uani 1 1 d . . . C46 C 0.8812(3) 0.1169(4) 0.6587(6) 0.0323(18) Uani 1 1 d . . . C47 C 0.8236(3) 0.1259(4) 0.6084(5) 0.0282(16) Uani 1 1 d . . . C48 C 0.7751(3) 0.1249(3) 0.6487(5) 0.0261(16) Uani 1 1 d . . . C49 C 0.8491(4) 0.0976(5) 0.8911(5) 0.041(2) Uani 1 1 d . . . H49A H 0.8296 0.1341 0.9154 0.062 Uiso 1 1 calc R . . H49B H 0.8915 0.0978 0.9178 0.062 Uiso 1 1 calc R . . H49C H 0.8316 0.0556 0.9042 0.062 Uiso 1 1 calc R . . C50 C 0.9507(4) 0.1109(4) 0.8073(6) 0.041(2) Uani 1 1 d . . . H50A H 0.9779 0.1309 0.7728 0.050 Uiso 1 1 calc R . . H50B H 0.9514 0.1390 0.8600 0.050 Uiso 1 1 calc R . . N7 N 0.9726(3) 0.0434(3) 0.8368(5) 0.0326(15) Uani 1 1 d . . . C51 C 0.9419(4) -0.0131(4) 0.8253(6) 0.038(2) Uani 1 1 d . . . H51 H 0.9018 -0.0163 0.7943 0.046 Uiso 1 1 calc R . . N8 N 0.9736(3) -0.0637(3) 0.8618(5) 0.0374(16) Uani 1 1 d . . . C52 C 1.0276(4) -0.0364(5) 0.9000(6) 0.045(2) Uani 1 1 d . . . H52 H 1.0605 -0.0606 0.9319 0.054 Uiso 1 1 calc R . . C53 C 1.0274(4) 0.0287(5) 0.8859(6) 0.042(2) Uani 1 1 d . . . H53 H 1.0590 0.0587 0.9060 0.050 Uiso 1 1 calc R . . C54 C 0.9341(4) 0.1158(5) 0.6159(6) 0.041(2) Uani 1 1 d . . . H54A H 0.9232 0.0944 0.5578 0.061 Uiso 1 1 calc R . . H54B H 0.9664 0.0911 0.6534 0.061 Uiso 1 1 calc R . . H54C H 0.9471 0.1612 0.6086 0.061 Uiso 1 1 calc R . . C55 C 0.7138(3) 0.1434(4) 0.5964(5) 0.0319(17) Uani 1 1 d . . . H55A H 0.7177 0.1729 0.5477 0.048 Uiso 1 1 calc R . . H55B H 0.6917 0.1658 0.6355 0.048 Uiso 1 1 calc R . . H55C H 0.6926 0.1033 0.5724 0.048 Uiso 1 1 calc R . . C56 C 0.8148(4) 0.1432(4) 0.5103(5) 0.0342(18) Uani 1 1 d . . . H56A H 0.8538 0.1397 0.4938 0.041 Uiso 1 1 calc R . . H56B H 0.8028 0.1903 0.5037 0.041 Uiso 1 1 calc R . . C57 C 0.8466(9) 0.2129(11) 0.2307(11) 0.070 Uani 0.50 1 d PD . . H57A H 0.8142 0.1879 0.2487 0.084 Uiso 0.50 1 calc PR . . H57B H 0.8322 0.2590 0.2214 0.084 Uiso 0.50 1 calc PR . . C58 C 0.8471(8) 0.1906(12) 0.1489(11) 0.070 Uani 0.50 1 d PD . . H58A H 0.8704 0.1491 0.1534 0.084 Uiso 0.50 1 calc PR . . H58B H 0.8667 0.2236 0.1175 0.084 Uiso 0.50 1 calc PR . . Cl1 Cl 0.9005(3) 0.2166(3) 0.3240(5) 0.0798(19) Uani 0.50 1 d PD . . Cl2 Cl 0.7751(3) 0.1756(3) 0.0872(4) 0.0755(18) Uani 0.50 1 d PD . . C59 C 0.3100(7) 0.4567(9) 0.5598(11) 0.104(5) Uani 1 1 d . . . H59A H 0.3375 0.4585 0.6182 0.125 Uiso 1 1 calc R . . H59B H 0.2691 0.4508 0.5688 0.125 Uiso 1 1 calc R . . C60 C 0.3250(7) 0.4075(8) 0.5094(11) 0.103(6) Uani 1 1 d . . . H60A H 0.3655 0.4140 0.4987 0.124 Uiso 1 1 calc R . . H60B H 0.2966 0.4043 0.4519 0.124 Uiso 1 1 calc R . . Cl3 Cl 0.3160(3) 0.5340(2) 0.4933(3) 0.1189(17) Uani 1 1 d . . . Cl4 Cl 0.32124(14) 0.33277(14) 0.5797(2) 0.0665(8) Uani 1 1 d . . . C61 C 0.5245(5) 0.0144(7) 0.9949(15) 0.135(8) Uani 1 1 d D . . H61A H 0.5589 0.0022 1.0421 0.162 Uiso 1 1 calc R . . H61B H 0.5206 0.0631 0.9909 0.162 Uiso 1 1 calc R . . Cl5 Cl 0.52816(14) -0.02599(14) 0.88103(16) 0.0588(7) Uani 1 1 d . . . C62 C 0.8550(12) 1.0115(11) 0.2668(18) 0.090(8) Uiso 0.50 1 d PD . . H62A H 0.8426 1.0378 0.3138 0.108 Uiso 0.50 1 calc PR . . H62B H 0.8824 1.0391 0.2407 0.108 Uiso 0.50 1 calc PR . . C63 C 0.8068(12) 0.9971(17) 0.2034(14) 0.100(10) Uiso 0.50 1 d PD . . H63A H 0.7820 1.0374 0.1917 0.120 Uiso 0.50 1 calc PR . . H63B H 0.7833 0.9632 0.2271 0.120 Uiso 0.50 1 calc PR . . Cl6 Cl 0.8918(5) 0.9427(8) 0.3131(8) 0.159(5) Uani 0.50 1 d PD . . Cl7 Cl 0.8199(4) 0.9691(6) 0.1049(7) 0.133(4) Uani 0.50 1 d PD . . Cl8 Cl 1.0667(6) 0.9454(6) 0.6149(8) 0.070 Uani 0.25 1 d PD . . C64 C 0.9944(10) 0.933(2) 0.623(2) 0.070 Uani 0.25 1 d PD . . H64A H 0.9977 0.9151 0.6836 0.084 Uiso 0.25 1 calc PR . . H64B H 0.9788 0.9788 0.6260 0.084 Uiso 0.25 1 calc PR . . C65 C 0.9509(11) 0.902(2) 0.576(2) 0.070 Uani 0.25 1 d PD . . H65A H 0.9180 0.9339 0.5638 0.084 Uiso 0.25 1 calc PR . . H65B H 0.9395 0.8687 0.6173 0.084 Uiso 0.25 1 calc PR . . Cl9 Cl 0.9471(6) 0.8589(6) 0.4770(8) 0.070 Uani 0.25 1 d PD . . 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 0.0366(6) 0.0314(5) 0.0260(5) 0.0021(4) 0.0070(4) 0.0017(4) Br1 0.0451(6) 0.0648(6) 0.0309(5) -0.0152(4) 0.0092(4) -0.0146(4) Br2 0.0452(5) 0.0386(5) 0.0409(5) 0.0118(4) 0.0157(4) 0.0126(4) Cu2 0.0593(8) 0.0362(6) 0.0390(6) -0.0004(5) -0.0065(5) 0.0021(5) Br3 0.0548(6) 0.0506(6) 0.0495(6) 0.0067(4) 0.0102(5) -0.0138(5) Br4 0.0954(10) 0.0483(7) 0.0665(8) -0.0066(5) -0.0340(7) 0.0194(6) C1 0.031(4) 0.029(4) 0.022(4) 0.003(3) 0.005(3) 0.006(3) C2 0.032(4) 0.030(4) 0.032(4) 0.009(3) 0.013(3) 0.007(3) C3 0.032(4) 0.037(4) 0.018(4) 0.008(3) 0.008(3) 0.008(3) C4 0.024(4) 0.034(4) 0.019(3) 0.002(3) 0.004(3) 0.008(3) C5 0.029(4) 0.029(4) 0.022(4) 0.002(3) 0.004(3) 0.007(3) C6 0.030(4) 0.026(4) 0.028(4) 0.006(3) 0.008(3) 0.007(3) C7 0.049(6) 0.028(4) 0.047(5) 0.011(4) 0.007(4) 0.008(4) C8 0.036(4) 0.041(4) 0.020(4) 0.008(3) 0.009(3) 0.012(4) N1 0.031(3) 0.026(3) 0.011(3) 0.010(2) 0.005(2) 0.010(3) C9 0.029(4) 0.023(4) 0.019(4) 0.006(3) 0.003(3) 0.002(3) N2 0.029(3) 0.020(3) 0.021(3) 0.003(2) 0.006(3) -0.001(2) C10 0.029(4) 0.029(4) 0.022(4) 0.004(3) 0.003(3) 0.001(3) C11 0.031(4) 0.037(4) 0.014(3) 0.004(3) 0.001(3) 0.002(3) C12 0.033(4) 0.039(5) 0.024(4) 0.000(3) -0.007(3) 0.008(4) C13 0.028(4) 0.028(4) 0.039(5) 0.009(3) -0.002(3) 0.005(3) C14 0.034(4) 0.026(4) 0.027(4) -0.003(3) 0.006(3) 0.010(3) C15 0.032(4) 0.020(3) 0.024(4) -0.004(3) -0.003(3) 0.003(3) C16 0.035(4) 0.024(4) 0.028(4) -0.006(3) 0.001(3) 0.011(3) C17 0.036(4) 0.016(3) 0.029(4) -0.006(3) -0.008(3) 0.008(3) C18 0.031(4) 0.022(4) 0.024(4) -0.002(3) -0.006(3) 0.000(3) C19 0.031(4) 0.016(3) 0.024(4) -0.009(3) 0.001(3) -0.002(3) C20 0.023(4) 0.018(3) 0.025(4) -0.004(3) 0.000(3) 0.000(3) C21 0.068(7) 0.041(5) 0.047(6) 0.008(4) 0.021(5) 0.032(5) C22 0.057(6) 0.021(4) 0.027(4) -0.005(3) -0.006(4) 0.019(4) N3 0.064(3) 0.058(3) 0.054(3) -0.025(2) -0.020(2) 0.033(2) C23 0.064(3) 0.058(3) 0.054(3) -0.025(2) -0.020(2) 0.033(2) N4 0.064(3) 0.058(3) 0.054(3) -0.025(2) -0.020(2) 0.033(2) C24 0.064(3) 0.058(3) 0.054(3) -0.025(2) -0.020(2) 0.033(2) C25 0.064(3) 0.058(3) 0.054(3) -0.025(2) -0.020(2) 0.033(2) C26 0.039(5) 0.022(4) 0.045(5) 0.008(3) 0.008(4) 0.008(3) C27 0.035(4) 0.023(4) 0.024(4) -0.002(3) 0.001(3) 0.003(3) C28 0.031(4) 0.016(3) 0.028(4) -0.002(3) 0.003(3) -0.001(3) C29 0.025(4) 0.018(3) 0.016(3) 0.000(2) -0.001(3) 0.003(3) C30 0.023(4) 0.021(3) 0.019(3) 0.003(3) 0.005(3) 0.002(3) C31 0.024(4) 0.021(3) 0.019(3) 0.002(3) 0.007(3) -0.001(3) C32 0.033(4) 0.020(3) 0.019(3) 0.000(3) 0.007(3) 0.003(3) C33 0.032(4) 0.017(3) 0.018(3) 0.000(2) 0.002(3) 0.000(3) C34 0.025(4) 0.023(3) 0.013(3) 0.002(2) 0.001(3) 0.000(3) C35 0.026(4) 0.026(4) 0.035(4) 0.000(3) 0.002(3) 0.003(3) C36 0.027(4) 0.026(4) 0.026(4) 0.006(3) 0.010(3) 0.003(3) N5 0.019(3) 0.021(3) 0.021(3) -0.001(2) 0.004(2) 0.001(2) C37 0.023(4) 0.027(4) 0.026(4) 0.001(3) 0.006(3) 0.007(3) N6 0.031(3) 0.028(3) 0.018(3) 0.004(2) 0.005(3) 0.008(3) C38 0.027(4) 0.025(4) 0.027(4) 0.000(3) 0.002(3) 0.002(3) C39 0.022(4) 0.027(4) 0.024(4) 0.000(3) 0.007(3) 0.001(3) C40 0.041(5) 0.025(4) 0.035(4) -0.007(3) 0.004(4) 0.005(3) C41 0.029(4) 0.032(4) 0.030(4) -0.002(3) 0.000(3) 0.007(3) C42 0.034(4) 0.033(4) 0.025(4) -0.007(3) -0.001(3) -0.003(3) C43 0.026(4) 0.017(3) 0.028(4) -0.007(3) -0.004(3) -0.003(3) C44 0.036(5) 0.025(4) 0.033(4) 0.001(3) -0.008(4) -0.007(3) C45 0.022(4) 0.024(4) 0.039(4) 0.001(3) -0.010(3) -0.005(3) C46 0.026(4) 0.025(4) 0.042(5) 0.004(3) 0.000(3) -0.004(3) C47 0.028(4) 0.020(4) 0.034(4) 0.005(3) 0.000(3) 0.001(3) C48 0.030(4) 0.016(3) 0.028(4) 0.004(3) -0.005(3) 0.000(3) C49 0.033(5) 0.054(6) 0.030(4) -0.001(4) -0.007(4) -0.002(4) C50 0.039(5) 0.032(5) 0.046(5) 0.009(4) -0.007(4) -0.009(4) N7 0.024(3) 0.033(4) 0.039(4) 0.002(3) 0.003(3) -0.005(3) C51 0.033(5) 0.037(5) 0.040(5) -0.001(4) -0.003(4) -0.004(4) N8 0.033(4) 0.038(4) 0.038(4) 0.008(3) 0.000(3) 0.006(3) C52 0.036(5) 0.055(6) 0.040(5) 0.009(4) 0.000(4) 0.008(4) C53 0.024(4) 0.048(5) 0.046(5) 0.008(4) -0.008(4) -0.003(4) C54 0.032(5) 0.048(5) 0.043(5) 0.007(4) 0.007(4) -0.005(4) C55 0.029(4) 0.031(4) 0.032(4) 0.001(3) -0.002(3) 0.005(3) C56 0.036(5) 0.033(4) 0.032(4) 0.005(3) 0.006(4) -0.007(4) C57 0.072 0.055 0.077 0.003 0.000 0.000 C58 0.072 0.055 0.077 0.003 0.000 0.000 Cl1 0.061(4) 0.058(4) 0.105(5) 0.009(3) -0.019(3) -0.009(3) Cl2 0.070(4) 0.059(3) 0.086(4) 0.000(3) -0.009(3) -0.025(3) C59 0.080(11) 0.154(16) 0.088(11) -0.009(11) 0.043(9) -0.003(10) C60 0.079(10) 0.123(13) 0.109(12) -0.065(11) 0.023(9) 0.001(9) Cl3 0.177(5) 0.066(2) 0.126(4) 0.022(2) 0.060(3) 0.030(3) Cl4 0.0707(19) 0.0563(16) 0.079(2) -0.0035(14) 0.0294(16) 0.0056(14) C61 0.079(11) 0.051(9) 0.25(2) 0.013(11) -0.014(14) -0.019(7) Cl5 0.082(2) 0.0605(16) 0.0354(12) 0.0022(11) 0.0153(12) 0.0101(14) Cl6 0.109(8) 0.251(15) 0.123(8) 0.055(9) 0.037(6) 0.035(9) Cl7 0.074(5) 0.203(11) 0.123(7) -0.039(7) 0.024(5) 0.007(6) Cl8 0.072 0.055 0.077 0.003 0.000 0.000 C64 0.072 0.055 0.077 0.003 0.000 0.000 C65 0.072 0.055 0.077 0.003 0.000 0.000 Cl9 0.072 0.055 0.077 0.003 0.000 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N6 2.003(6) . ? Cu1 N2 2.005(6) . ? Cu1 Br1 2.3763(13) . ? Cu1 Br2 2.3831(13) . ? Cu2 N8 1.993(7) . ? Cu2 N4 2.015(8) . ? Cu2 Br4 2.3641(16) . ? Cu2 Br3 2.3915(17) . ? C1 C6 1.394(10) . ? C1 C2 1.416(10) . ? C1 C56 1.533(11) . ? C2 C3 1.399(11) . ? C2 C7 1.508(11) . ? C3 C4 1.387(11) . ? C3 C8 1.524(10) . ? C4 C5 1.409(10) . ? C4 C12 1.523(11) . ? C5 C6 1.397(11) . ? C5 C14 1.533(10) . ? C6 C13 1.514(10) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 N1 1.477(10) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? N1 C9 1.335(9) . ? N1 C11 1.373(9) . ? C9 N2 1.326(9) . ? C9 H9 0.9500 . ? N2 C10 1.374(9) . ? C10 C11 1.344(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 1.535(10) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C20 1.380(10) . ? C15 C16 1.390(10) . ? C16 C17 1.421(11) . ? C16 C21 1.522(12) . ? C17 C18 1.377(11) . ? C17 C22 1.528(10) . ? C18 C19 1.419(10) . ? C18 C26 1.520(11) . ? C19 C20 1.412(10) . ? C19 C28 1.524(10) . ? C20 C27 1.512(10) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 N3 1.467(12) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? N3 C23 1.327(12) . ? N3 C25 1.394(13) . ? C23 N4 1.287(13) . ? C23 H23 0.9500 . ? N4 C24 1.368(13) . ? C24 C25 1.357(14) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.531(9) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.400(10) . ? C29 C34 1.414(10) . ? C30 C31 1.402(9) . ? C30 C35 1.509(10) . ? C31 C32 1.406(10) . ? C31 C36 1.501(10) . ? C32 C33 1.398(10) . ? C32 C40 1.526(10) . ? C33 C34 1.396(9) . ? C33 C42 1.512(10) . ? C34 C41 1.520(10) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 N5 1.477(9) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? N5 C37 1.334(9) . ? N5 C39 1.377(9) . ? C37 N6 1.326(9) . ? C37 H37 0.9500 . ? N6 C38 1.378(10) . ? C38 C39 1.357(10) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C43 1.517(11) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.412(11) . ? C43 C48 1.430(10) . ? C44 C45 1.398(12) . ? C44 C49 1.493(12) . ? C45 C46 1.410(12) . ? C45 C50 1.513(11) . ? C46 C47 1.402(11) . ? C46 C54 1.508(12) . ? C47 C48 1.391(11) . ? C47 C56 1.528(11) . ? C48 C55 1.521(10) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 N7 1.493(11) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? N7 C51 1.337(10) . ? N7 C53 1.364(10) . ? C51 N8 1.314(11) . ? C51 H51 0.9500 . ? N8 C52 1.378(12) . ? C52 C53 1.334(13) . ? C52 H52 0.9500 . ? C53 H53 0.9500 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C58 1.346(16) . ? C57 Cl1 1.696(13) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 Cl2 1.760(15) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 C60 1.354(19) . ? C59 Cl3 1.892(18) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 Cl4 1.874(19) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C61 1.311(17) 3_657 ? C61 Cl5 1.96(2) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C63 1.352(18) . ? C62 Cl6 1.708(17) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 Cl7 1.710(17) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? Cl8 C64 1.717(18) . ? C64 C65 1.282(16) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 Cl9 1.749(18) . ? C65 H65A 0.9900 . ? C65 H65B 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 N6 Cu1 N2 112.5(2) . . ? N6 Cu1 Br1 105.74(18) . . ? N2 Cu1 Br1 101.70(18) . . ? N6 Cu1 Br2 106.86(18) . . ? N2 Cu1 Br2 109.32(17) . . ? Br1 Cu1 Br2 120.75(5) . . ? N8 Cu2 N4 115.1(4) . . ? N8 Cu2 Br4 106.8(2) . . ? N4 Cu2 Br4 107.8(2) . . ? N8 Cu2 Br3 102.2(2) . . ? N4 Cu2 Br3 105.4(3) . . ? Br4 Cu2 Br3 119.82(7) . . ? C6 C1 C2 119.5(7) . . ? C6 C1 C56 122.5(7) . . ? C2 C1 C56 117.9(7) . . ? C3 C2 C1 118.6(7) . . ? C3 C2 C7 121.8(7) . . ? C1 C2 C7 119.6(8) . . ? C4 C3 C2 121.7(7) . . ? C4 C3 C8 118.9(7) . . ? C2 C3 C8 119.4(7) . . ? C3 C4 C5 119.5(7) . . ? C3 C4 C12 119.6(7) . . ? C5 C4 C12 120.9(7) . . ? C6 C5 C4 119.2(7) . . ? C6 C5 C14 119.5(6) . . ? C4 C5 C14 121.1(7) . . ? C1 C6 C5 121.1(7) . . ? C1 C6 C13 119.2(7) . . ? C5 C6 C13 119.7(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 112.2(6) . . ? N1 C8 H8A 109.2 . . ? C3 C8 H8A 109.2 . . ? N1 C8 H8B 109.2 . . ? C3 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? C9 N1 C11 107.6(6) . . ? C9 N1 C8 125.6(6) . . ? C11 N1 C8 126.4(6) . . ? N2 C9 N1 111.2(6) . . ? N2 C9 H9 124.4 . . ? N1 C9 H9 124.4 . . ? C9 N2 C10 105.2(6) . . ? C9 N2 Cu1 124.2(5) . . ? C10 N2 Cu1 129.3(5) . . ? C11 C10 N2 110.2(7) . . ? C11 C10 H10 124.9 . . ? N2 C10 H10 124.9 . . ? C10 C11 N1 105.9(6) . . ? 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 119.8(6) . . ? C5 C14 H14A 107.4 . . ? C15 C14 H14A 107.4 . . ? C5 C14 H14B 107.4 . . ? C15 C14 H14B 107.4 . . ? H14A C14 H14B 106.9 . . ? C20 C15 C16 120.9(7) . . ? C20 C15 C14 121.2(6) . . ? C16 C15 C14 117.8(7) . . ? C15 C16 C17 118.9(7) . . ? C15 C16 C21 122.4(7) . . ? C17 C16 C21 118.7(7) . . ? C18 C17 C16 120.7(7) . . ? C18 C17 C22 120.0(7) . . ? C16 C17 C22 119.2(7) . . ? C17 C18 C19 119.9(7) . . ? C17 C18 C26 121.8(7) . . ? C19 C18 C26 118.3(7) . . ? C20 C19 C18 118.9(7) . . ? C20 C19 C28 122.0(6) . . ? C18 C19 C28 119.0(7) . . ? C15 C20 C19 120.4(6) . . ? C15 C20 C27 121.2(6) . . ? C19 C20 C27 118.3(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 . . ? N3 C22 C17 111.6(7) . . ? N3 C22 H22A 109.3 . . ? C17 C22 H22A 109.3 . . ? N3 C22 H22B 109.3 . . ? C17 C22 H22B 109.3 . . ? H22A C22 H22B 108.0 . . ? C23 N3 C25 104.8(9) . . ? C23 N3 C22 129.3(8) . . ? C25 N3 C22 125.7(8) . . ? N4 C23 N3 113.5(9) . . ? N4 C23 H23 123.2 . . ? N3 C23 H23 123.2 . . ? C23 N4 C24 105.8(8) . . ? C23 N4 Cu2 126.3(7) . . ? C24 N4 Cu2 127.5(7) . . ? C25 C24 N4 108.7(10) . . ? C25 C24 H24 125.6 . . ? N4 C24 H24 125.6 . . ? C24 C25 N3 106.2(9) . . ? C24 C25 H25 126.9 . . ? N3 C25 H25 126.9 . . ? C18 C26 H26A 109.5 . . ? C18 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C18 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C20 C27 H27A 109.5 . . ? C20 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C20 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C19 C28 C29 119.6(6) . . ? C19 C28 H28A 107.4 . . ? C29 C28 H28A 107.4 . . ? C19 C28 H28B 107.4 . . ? C29 C28 H28B 107.4 . . ? H28A C28 H28B 107.0 . . ? C30 C29 C34 119.7(6) . . ? C30 C29 C28 120.3(6) . . ? C34 C29 C28 119.8(6) . . ? C29 C30 C31 119.1(6) . . ? C29 C30 C35 121.9(6) . . ? C31 C30 C35 118.9(6) . . ? C30 C31 C32 120.6(6) . . ? C30 C31 C36 120.3(6) . . ? C32 C31 C36 119.1(6) . . ? C33 C32 C31 120.1(6) . . ? C33 C32 C40 120.2(7) . . ? C31 C32 C40 119.7(7) . . ? C34 C33 C32 119.2(7) . . ? C34 C33 C42 121.3(7) . . ? C32 C33 C42 119.2(6) . . ? C33 C34 C29 120.7(6) . . ? C33 C34 C41 119.6(6) . . ? C29 C34 C41 119.6(6) . . ? C30 C35 H35A 109.5 . . ? C30 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C30 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N5 C36 C31 114.0(6) . . ? N5 C36 H36A 108.7 . . ? C31 C36 H36A 108.7 . . ? N5 C36 H36B 108.7 . . ? C31 C36 H36B 108.7 . . ? H36A C36 H36B 107.6 . . ? C37 N5 C39 107.7(6) . . ? C37 N5 C36 126.8(6) . . ? C39 N5 C36 125.5(6) . . ? N6 C37 N5 111.3(6) . . ? N6 C37 H37 124.3 . . ? N5 C37 H37 124.3 . . ? C37 N6 C38 105.5(6) . . ? C37 N6 Cu1 125.4(5) . . ? C38 N6 Cu1 128.2(5) . . ? C39 C38 N6 109.7(6) . . ? C39 C38 H38 125.2 . . ? N6 C38 H38 125.2 . . ? C38 C39 N5 105.8(6) . . ? C38 C39 H39 127.1 . . ? N5 C39 H39 127.1 . . ? C32 C40 H40A 109.5 . . ? C32 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C32 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C34 C41 H41A 109.5 . . ? C34 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C34 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C33 C42 C43 120.8(6) . . ? C33 C42 H42A 107.1 . . ? C43 C42 H42A 107.1 . . ? C33 C42 H42B 107.1 . . ? C43 C42 H42B 107.1 . . ? H42A C42 H42B 106.8 . . ? C44 C43 C48 119.1(7) . . ? C44 C43 C42 119.1(7) . . ? C48 C43 C42 121.7(7) . . ? C45 C44 C43 118.5(7) . . ? C45 C44 C49 122.0(7) . . ? C43 C44 C49 119.5(8) . . ? C44 C45 C46 122.5(7) . . ? C44 C45 C50 118.9(7) . . ? C46 C45 C50 118.6(7) . . ? C47 C46 C45 118.3(7) . . ? C47 C46 C54 121.3(8) . . ? C45 C46 C54 120.5(7) . . ? C48 C47 C46 120.5(7) . . ? C48 C47 C56 119.6(7) . . ? C46 C47 C56 119.6(7) . . ? C47 C48 C43 120.6(7) . . ? C47 C48 C55 120.3(7) . . ? C43 C48 C55 118.9(7) . . ? C44 C49 H49A 109.5 . . ? C44 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C44 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? N7 C50 C45 112.5(7) . . ? N7 C50 H50A 109.1 . . ? C45 C50 H50A 109.1 . . ? N7 C50 H50B 109.1 . . ? C45 C50 H50B 109.1 . . ? H50A C50 H50B 107.8 . . ? C51 N7 C53 106.9(7) . . ? C51 N7 C50 127.3(7) . . ? C53 N7 C50 125.7(7) . . ? N8 C51 N7 112.1(8) . . ? N8 C51 H51 123.9 . . ? N7 C51 H51 123.9 . . ? C51 N8 C52 104.1(7) . . ? C51 N8 Cu2 124.3(6) . . ? C52 N8 Cu2 129.6(6) . . ? C53 C52 N8 110.7(8) . . ? C53 C52 H52 124.6 . . ? N8 C52 H52 124.6 . . ? C52 C53 N7 106.1(8) . . ? C52 C53 H53 127.0 . . ? N7 C53 H53 127.0 . . ? C46 C54 H54A 109.5 . . ? C46 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C46 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C48 C55 H55A 109.5 . . ? C48 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C48 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C47 C56 C1 119.6(6) . . ? C47 C56 H56A 107.4 . . ? C1 C56 H56A 107.4 . . ? C47 C56 H56B 107.4 . . ? C1 C56 H56B 107.4 . . ? H56A C56 H56B 106.9 . . ? C58 C57 Cl1 131.7(16) . . ? C58 C57 H57A 104.3 . . ? Cl1 C57 H57A 104.3 . . ? C58 C57 H57B 104.3 . . ? Cl1 C57 H57B 104.3 . . ? H57A C57 H57B 105.6 . . ? C57 C58 Cl2 112.0(14) . . ? C57 C58 H58A 109.2 . . ? Cl2 C58 H58A 109.2 . . ? C57 C58 H58B 109.2 . . ? Cl2 C58 H58B 109.2 . . ? H58A C58 H58B 107.9 . . ? C60 C59 Cl3 103.7(12) . . ? C60 C59 H59A 111.0 . . ? Cl3 C59 H59A 111.0 . . ? C60 C59 H59B 111.0 . . ? Cl3 C59 H59B 111.0 . . ? H59A C59 H59B 109.0 . . ? C59 C60 Cl4 102.2(12) . . ? C59 C60 H60A 111.3 . . ? Cl4 C60 H60A 111.3 . . ? C59 C60 H60B 111.3 . . ? Cl4 C60 H60B 111.3 . . ? H60A C60 H60B 109.2 . . ? C61 C61 Cl5 97(2) 3_657 . ? C61 C61 H61A 112.3 3_657 . ? Cl5 C61 H61A 112.3 . . ? C61 C61 H61B 112.3 3_657 . ? Cl5 C61 H61B 112.3 . . ? H61A C61 H61B 109.9 . . ? C63 C62 Cl6 113(2) . . ? C63 C62 H62A 109.0 . . ? Cl6 C62 H62A 109.0 . . ? C63 C62 H62B 109.0 . . ? Cl6 C62 H62B 109.0 . . ? H62A C62 H62B 107.8 . . ? C62 C63 Cl7 116(2) . . ? C62 C63 H63A 108.2 . . ? Cl7 C63 H63A 108.2 . . ? C62 C63 H63B 108.2 . . ? Cl7 C63 H63B 108.2 . . ? H63A C63 H63B 107.4 . . ? Cl8 C64 H64A 103.9 . . ? Cl8 C64 H64B 103.9 . . ? C64 C65 Cl9 129.4(18) . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 27.62 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 1.786 _refine_diff_density_min -1.510 _refine_diff_density_rms 0.215 # Attachment '4-CuCl2.cif' data_4-CuCl2 _database_code_depnum_ccdc_archive 'CCDC 702196' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '4(C56 H64 Cl4 Cu2 N8), 9(C H Cl3), 10(H2 O)' _chemical_formula_sum 'C233 H285 Cl43 Cu8 N32 O10' _chemical_formula_weight 5726.60 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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 16.9105(11) _cell_length_b 17.1432(13) _cell_length_c 25.9620(19) _cell_angle_alpha 90.00 _cell_angle_beta 91.011(4) _cell_angle_gamma 90.00 _cell_volume 7525.2(9) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1982 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 26.83 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.264 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2950 _exptl_absorpt_coefficient_mu 0.989 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8578 _exptl_absorpt_correction_T_max 0.9076 _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 48792 _diffrn_reflns_av_R_equivalents 0.0875 _diffrn_reflns_av_sigmaI/netI 0.1702 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 27.56 _reflns_number_total 15935 _reflns_number_gt 4085 _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^+0.8947P] 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 15935 _refine_ls_number_parameters 772 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.3804 _refine_ls_R_factor_gt 0.1534 _refine_ls_wR_factor_ref 0.4897 _refine_ls_wR_factor_gt 0.3893 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.100 _refine_ls_shift/su_max 0.005 _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 0.82427(12) 0.09461(14) 0.76462(8) 0.0576(7) Uani 1 1 d . . . Cl1 Cl 0.8945(3) 0.0196(3) 0.7111(2) 0.0784(17) Uani 1 1 d . . . Cl2 Cl 0.8092(3) 0.1204(4) 0.84858(17) 0.0843(18) Uani 1 1 d . . . Cu2 Cu 0.67422(12) 0.16277(13) 0.25121(8) 0.0520(7) Uani 1 1 d . . . Cl3 Cl 0.6053(2) 0.0782(3) 0.29959(19) 0.0649(14) Uani 1 1 d . . . Cl4 Cl 0.6957(3) 0.2133(3) 0.17287(17) 0.0698(15) Uani 1 1 d . . . C1 C 0.8237(10) 0.3080(10) 0.5408(7) 0.049(5) Uani 1 1 d . . . C2 C 0.8586(9) 0.3251(10) 0.5878(6) 0.043(4) Uani 1 1 d . . . C3 C 0.9264(10) 0.2913(10) 0.6048(6) 0.051(5) Uani 1 1 d . . . C4 C 0.9602(9) 0.2326(9) 0.5740(6) 0.041(4) Uani 1 1 d . . . C5 C 0.9250(9) 0.2109(9) 0.5267(5) 0.039(4) Uani 1 1 d . . . C6 C 0.8600(8) 0.2493(9) 0.5085(6) 0.036(4) Uani 1 1 d . . . C7 C 0.8203(10) 0.3896(12) 0.6209(7) 0.076(6) Uani 1 1 d . . . H7A H 0.8034 0.3672 0.6536 0.114 Uiso 1 1 calc R . . H7B H 0.7743 0.4112 0.6023 0.114 Uiso 1 1 calc R . . H7C H 0.8589 0.4312 0.6276 0.114 Uiso 1 1 calc R . . C8 C 0.9670(9) 0.3175(11) 0.6533(6) 0.054(5) Uani 1 1 d . . . H8A H 1.0242 0.3059 0.6512 0.065 Uiso 1 1 calc R . . H8B H 0.9609 0.3746 0.6569 0.065 Uiso 1 1 calc R . . N1 N 0.9354(7) 0.2793(9) 0.6985(5) 0.042(3) Uani 1 1 d . . . C9 C 0.9002(10) 0.2112(13) 0.6990(6) 0.056(5) Uani 1 1 d . . . H9 H 0.8903 0.1804 0.6691 0.068 Uiso 1 1 calc R . . N2 N 0.8795(8) 0.1901(8) 0.7471(5) 0.056(4) Uani 1 1 d . . . C10 C 0.9058(9) 0.2513(11) 0.7785(6) 0.049(5) Uani 1 1 d . . . H10 H 0.9009 0.2541 0.8148 0.058 Uiso 1 1 calc R . . C11 C 0.9393(10) 0.3058(11) 0.7483(7) 0.052(5) Uani 1 1 d . . . H11 H 0.9615 0.3539 0.7596 0.062 Uiso 1 1 calc R . . C12 C 1.0359(9) 0.1898(11) 0.5939(7) 0.063(5) Uani 1 1 d . . . H12A H 1.0216 0.1381 0.6069 0.095 Uiso 1 1 calc R . . H12B H 1.0609 0.2203 0.6216 0.095 Uiso 1 1 calc R . . H12C H 1.0730 0.1839 0.5655 0.095 Uiso 1 1 calc R . . C13 C 0.8306(10) 0.2358(10) 0.4535(5) 0.054(5) Uani 1 1 d . . . H13A H 0.7819 0.2050 0.4538 0.081 Uiso 1 1 calc R . . H13B H 0.8711 0.2077 0.4343 0.081 Uiso 1 1 calc R . . H13C H 0.8201 0.2862 0.4368 0.081 Uiso 1 1 calc R . . C14 C 0.9642(10) 0.1445(10) 0.4959(6) 0.052(5) Uani 1 1 d . . . H14A H 0.9995 0.1691 0.4705 0.062 Uiso 1 1 calc R . . H14B H 0.9984 0.1148 0.5202 0.062 Uiso 1 1 calc R . . C15 C 0.9120(8) 0.0853(8) 0.4666(6) 0.033(4) Uani 1 1 d . . . C16 C 0.9263(9) 0.0690(10) 0.4152(5) 0.041(4) Uani 1 1 d . . . C17 C 0.8845(8) 0.0084(10) 0.3896(5) 0.040(4) Uani 1 1 d . . . C18 C 0.8262(8) -0.0298(9) 0.4140(6) 0.039(4) Uani 1 1 d . . . C19 C 0.8128(8) -0.0124(9) 0.4658(6) 0.033(4) Uani 1 1 d . . . C20 C 0.8573(8) 0.0411(9) 0.4936(5) 0.030(4) Uani 1 1 d . . . C21 C 0.9884(9) 0.1168(11) 0.3857(6) 0.058(5) Uani 1 1 d . . . H21A H 0.9982 0.1662 0.4036 0.088 Uiso 1 1 calc R . . H21B H 0.9686 0.1273 0.3507 0.088 Uiso 1 1 calc R . . H21C H 1.0378 0.0871 0.3840 0.088 Uiso 1 1 calc R . . C22 C 0.9083(10) -0.0098(10) 0.3351(6) 0.048(5) Uani 1 1 d . . . H22A H 0.9662 -0.0033 0.3323 0.058 Uiso 1 1 calc R . . H22B H 0.8954 -0.0649 0.3273 0.058 Uiso 1 1 calc R . . N3 N 0.8683(7) 0.0408(8) 0.2972(5) 0.043(3) Uani 1 1 d . . . C23 C 0.7921(9) 0.0660(9) 0.2976(6) 0.042(4) Uani 1 1 d . . . H23 H 0.7568 0.0565 0.3250 0.050 Uiso 1 1 calc R . . N4 N 0.7734(7) 0.1045(8) 0.2565(5) 0.044(4) Uani 1 1 d . . . C24 C 0.8388(10) 0.1050(10) 0.2263(7) 0.052(5) Uani 1 1 d . . . H24 H 0.8418 0.1286 0.1933 0.062 Uiso 1 1 calc R . . C25 C 0.8995(12) 0.0659(11) 0.2512(6) 0.060(5) Uani 1 1 d . . . H25 H 0.9516 0.0579 0.2393 0.072 Uiso 1 1 calc R . . C26 C 0.7753(10) -0.0901(10) 0.3845(6) 0.057(5) Uani 1 1 d . . . H26A H 0.7197 -0.0742 0.3852 0.085 Uiso 1 1 calc R . . H26B H 0.7813 -0.1413 0.4009 0.085 Uiso 1 1 calc R . . H26C H 0.7925 -0.0931 0.3487 0.085 Uiso 1 1 calc R . . C27 C 0.8514(10) 0.0472(10) 0.5525(6) 0.053(5) Uani 1 1 d . . . H27A H 0.9047 0.0509 0.5678 0.079 Uiso 1 1 calc R . . H27B H 0.8249 0.0007 0.5658 0.079 Uiso 1 1 calc R . . H27C H 0.8210 0.0937 0.5614 0.079 Uiso 1 1 calc R . . C28 C 0.7490(8) -0.0619(9) 0.4944(6) 0.044(4) Uani 1 1 d . . . H28A H 0.7197 -0.0924 0.4679 0.053 Uiso 1 1 calc R . . H28B H 0.7776 -0.0998 0.5166 0.053 Uiso 1 1 calc R . . C29 C 0.6871(9) -0.0209(10) 0.5281(5) 0.038(4) Uani 1 1 d . . . C30 C 0.6733(9) -0.0479(10) 0.5779(6) 0.044(4) Uani 1 1 d . . . C31 C 0.6129(9) -0.0155(10) 0.6069(6) 0.042(4) Uani 1 1 d . . . C32 C 0.5715(9) 0.0520(11) 0.5881(6) 0.047(5) Uani 1 1 d . . . C33 C 0.5860(9) 0.0789(10) 0.5386(6) 0.043(4) Uani 1 1 d . . . C34 C 0.6398(9) 0.0411(9) 0.5081(6) 0.038(4) Uani 1 1 d . . . C35 C 0.7195(10) -0.1201(11) 0.5991(6) 0.060(5) Uani 1 1 d . . . H35A H 0.7019 -0.1320 0.6340 0.090 Uiso 1 1 calc R . . H35B H 0.7763 -0.1085 0.6000 0.090 Uiso 1 1 calc R . . H35C H 0.7094 -0.1651 0.5767 0.090 Uiso 1 1 calc R . . C36 C 0.5906(9) -0.0490(11) 0.6592(6) 0.052(5) Uani 1 1 d . . . H36A H 0.5326 -0.0454 0.6631 0.062 Uiso 1 1 calc R . . H36B H 0.6055 -0.1048 0.6606 0.062 Uiso 1 1 calc R . . N5 N 0.6296(7) -0.0079(7) 0.7015(4) 0.038(3) Uani 1 1 d . . . C37 C 0.7044(9) 0.0099(10) 0.7045(6) 0.047(5) Uani 1 1 d . . . H37 H 0.7414 0.0011 0.6780 0.056 Uiso 1 1 calc R . . N6 N 0.7214(7) 0.0416(8) 0.7492(5) 0.051(4) Uani 1 1 d . . . C38 C 0.6547(9) 0.0422(12) 0.7775(7) 0.060(5) Uani 1 1 d . . . H38 H 0.6499 0.0602 0.8119 0.072 Uiso 1 1 calc R . . C39 C 0.5955(11) 0.0117(10) 0.7467(6) 0.054(5) Uani 1 1 d . . . H39 H 0.5415 0.0056 0.7553 0.064 Uiso 1 1 calc R . . C40 C 0.5078(10) 0.0887(11) 0.6222(6) 0.058(5) Uani 1 1 d . . . H40A H 0.5093 0.1456 0.6187 0.087 Uiso 1 1 calc R . . H40B H 0.5179 0.0743 0.6582 0.087 Uiso 1 1 calc R . . H40C H 0.4555 0.0695 0.6113 0.087 Uiso 1 1 calc R . . C41 C 0.6485(10) 0.0634(11) 0.4512(6) 0.058(5) Uani 1 1 d . . . H41A H 0.5961 0.0730 0.4358 0.087 Uiso 1 1 calc R . . H41B H 0.6743 0.0207 0.4328 0.087 Uiso 1 1 calc R . . H41C H 0.6807 0.1107 0.4487 0.087 Uiso 1 1 calc R . . C42 C 0.5365(9) 0.1453(11) 0.5165(6) 0.056(5) Uani 1 1 d . . . H42A H 0.5028 0.1233 0.4885 0.067 Uiso 1 1 calc R . . H42B H 0.5005 0.1628 0.5439 0.067 Uiso 1 1 calc R . . C43 C 0.5763(9) 0.2166(9) 0.4954(6) 0.037(4) Uani 1 1 d . . . C44 C 0.5407(9) 0.2544(10) 0.4507(6) 0.046(4) Uani 1 1 d . . . C45 C 0.5770(11) 0.3204(9) 0.4308(6) 0.045(4) Uani 1 1 d . . . C46 C 0.6502(10) 0.3464(11) 0.4497(7) 0.054(5) Uani 1 1 d . . . C47 C 0.6799(9) 0.3132(9) 0.4949(6) 0.040(4) Uani 1 1 d . . . C48 C 0.6428(9) 0.2502(10) 0.5180(6) 0.040(4) Uani 1 1 d . . . C49 C 0.4641(9) 0.2240(11) 0.4268(7) 0.065(6) Uani 1 1 d . . . H49A H 0.4253 0.2156 0.4538 0.097 Uiso 1 1 calc R . . H49B H 0.4742 0.1745 0.4091 0.097 Uiso 1 1 calc R . . H49C H 0.4433 0.2622 0.4019 0.097 Uiso 1 1 calc R . . C50 C 0.5371(10) 0.3603(11) 0.3831(7) 0.058(5) Uani 1 1 d . . . H50A H 0.4792 0.3526 0.3844 0.070 Uiso 1 1 calc R . . H50B H 0.5476 0.4171 0.3845 0.070 Uiso 1 1 calc R . . N7 N 0.5660(8) 0.3293(10) 0.3345(5) 0.058(4) Uani 1 1 d . . . C51 C 0.6047(11) 0.2628(10) 0.3264(7) 0.054(5) Uani 1 1 d . . . H51 H 0.6203 0.2273 0.3528 0.065 Uiso 1 1 calc R . . N8 N 0.6184(7) 0.2529(8) 0.2781(5) 0.044(3) Uani 1 1 d . . . C52 C 0.5897(10) 0.3204(13) 0.2539(8) 0.069(6) Uani 1 1 d . . . H52 H 0.5928 0.3301 0.2180 0.083 Uiso 1 1 calc R . . C53 C 0.5560(11) 0.3715(15) 0.2887(8) 0.083(7) Uani 1 1 d . . . H53 H 0.5328 0.4212 0.2830 0.099 Uiso 1 1 calc R . . C54 C 0.6901(10) 0.4162(11) 0.4236(7) 0.062(5) Uani 1 1 d . . . H54A H 0.6965 0.4587 0.4485 0.093 Uiso 1 1 calc R . . H54B H 0.6572 0.4339 0.3944 0.093 Uiso 1 1 calc R . . H54C H 0.7421 0.4003 0.4112 0.093 Uiso 1 1 calc R . . C55 C 0.6742(10) 0.2204(10) 0.5696(5) 0.052(5) Uani 1 1 d . . . H55A H 0.7124 0.1784 0.5638 0.078 Uiso 1 1 calc R . . H55B H 0.6303 0.2004 0.5898 0.078 Uiso 1 1 calc R . . H55C H 0.7003 0.2631 0.5884 0.078 Uiso 1 1 calc R . . C56 C 0.7514(9) 0.3524(9) 0.5209(6) 0.044(4) Uani 1 1 d . . . H56A H 0.7710 0.3915 0.4961 0.052 Uiso 1 1 calc R . . H56B H 0.7308 0.3820 0.5505 0.052 Uiso 1 1 calc R . . C57 C 0.701(2) 0.168(3) 0.9601(15) 0.087 Uani 0.50 1 d P . . H57 H 0.7336 0.1726 0.9286 0.104 Uiso 0.50 1 calc PR . . Cl5 Cl 0.6906(6) 0.0694(7) 0.9721(4) 0.087 Uani 0.50 1 d P . . Cl6 Cl 0.6347(6) 0.2210(6) 0.9524(6) 0.103(4) Uani 0.50 1 d P . . Cl7 Cl 0.7646(6) 0.2072(7) 1.0164(4) 0.087 Uani 0.50 1 d P . . C58 C 0.533(3) 0.982(3) 0.0817(12) 0.10(2) Uani 0.50 1 d P . . H58 H 0.4870 1.0126 0.0680 0.124 Uiso 0.50 1 calc PR . . Cl8 Cl 0.6048(6) 1.0467(7) 0.1018(4) 0.081(3) Uani 0.50 1 d P . . Cl9 Cl 0.5611(5) 0.9173(5) 0.0344(3) 0.045(2) Uani 0.50 1 d P . . Cl10 Cl 0.5005(6) 0.9276(8) 0.1362(3) 0.094(4) Uani 0.50 1 d P . . C59 C 0.6811(12) 0.8260(12) 0.2371(8) 0.080(7) Uani 1 1 d . . . H59 H 0.7200 0.7961 0.2587 0.096 Uiso 1 1 calc R . . Cl11 Cl 0.7262(4) 0.9194(4) 0.2205(3) 0.122(3) Uani 1 1 d . . . Cl12 Cl 0.6005(5) 0.8419(6) 0.2725(4) 0.169(4) Uani 1 1 d . . . Cl13 Cl 0.6652(4) 0.7749(4) 0.1801(2) 0.100(2) Uani 1 1 d . . . C61 C 0.143(5) 0.204(3) 0.253(3) 0.087 Uani 0.25 1 d PD . . H61 H 0.1032 0.1672 0.2381 0.104 Uiso 0.25 1 calc PR . . Cl15 Cl 0.2199(12) 0.1646(12) 0.2519(7) 0.087 Uani 0.25 1 d PD . . Cl14 Cl 0.1562(12) 0.2798(12) 0.2073(6) 0.087 Uani 0.25 1 d PD . . Cl17 Cl 0.1092(11) 0.2397(13) 0.2991(6) 0.087 Uani 0.25 1 d PD . . O1 O 0.9251(7) 0.9492(8) 0.9015(7) 0.176(10) Uani 1 1 d . . . O2 O 0.0407(11) 0.8282(11) 0.8935(8) 0.176(10) Uani 1 1 d . . . O3 O 0.5539(12) 0.5692(12) 0.4721(14) 0.176(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 Cu1 0.0365(12) 0.0828(19) 0.0532(13) -0.0178(13) -0.0100(10) -0.0018(12) Cl1 0.038(3) 0.097(4) 0.100(4) -0.035(3) 0.006(3) -0.006(3) Cl2 0.080(4) 0.129(5) 0.043(3) -0.015(3) -0.006(2) -0.016(4) Cu2 0.0366(12) 0.0609(16) 0.0582(13) 0.0231(12) -0.0106(10) -0.0041(11) Cl3 0.035(2) 0.064(3) 0.095(4) 0.034(3) 0.002(2) -0.001(2) Cl4 0.068(3) 0.088(4) 0.053(3) 0.027(3) -0.017(2) -0.002(3) C1 0.044(11) 0.035(11) 0.067(12) 0.003(9) -0.005(9) -0.007(9) C2 0.036(9) 0.059(12) 0.035(9) -0.014(9) -0.012(7) 0.007(9) C3 0.043(11) 0.053(12) 0.056(11) -0.018(10) -0.019(9) 0.001(9) C4 0.031(9) 0.042(11) 0.048(10) -0.008(9) -0.029(8) -0.001(8) C5 0.050(10) 0.036(10) 0.032(8) -0.005(8) -0.008(8) -0.006(9) C6 0.021(8) 0.046(11) 0.043(9) 0.006(8) -0.008(7) 0.009(7) C7 0.055(13) 0.092(17) 0.080(14) -0.048(13) -0.027(10) 0.004(12) C8 0.034(9) 0.081(15) 0.046(10) -0.021(10) -0.030(8) -0.004(10) N1 0.031(8) 0.055(10) 0.041(8) -0.004(8) -0.016(6) -0.003(7) C9 0.053(12) 0.081(16) 0.034(9) -0.008(10) -0.023(8) 0.003(11) N2 0.069(10) 0.055(10) 0.045(8) -0.008(8) 0.009(7) 0.015(8) C10 0.040(10) 0.066(13) 0.040(9) -0.029(10) -0.010(8) -0.011(9) C11 0.046(11) 0.056(13) 0.052(11) -0.028(10) -0.022(9) 0.004(10) C12 0.038(11) 0.073(14) 0.077(13) -0.019(11) -0.024(9) 0.004(10) C13 0.070(13) 0.069(13) 0.023(8) -0.005(9) -0.035(8) -0.005(10) C14 0.053(11) 0.055(13) 0.048(10) -0.007(9) -0.014(8) -0.004(10) C15 0.032(8) 0.026(9) 0.042(9) -0.004(8) -0.010(7) -0.006(7) C16 0.039(10) 0.051(12) 0.032(8) -0.012(8) -0.014(7) 0.017(9) C17 0.024(8) 0.067(13) 0.028(8) -0.008(8) -0.006(7) 0.003(8) C18 0.031(9) 0.043(11) 0.042(9) -0.003(8) -0.022(8) 0.008(8) C19 0.024(8) 0.026(9) 0.051(10) 0.005(8) -0.017(7) 0.010(7) C20 0.027(8) 0.024(9) 0.039(8) -0.010(7) -0.012(7) 0.000(7) C21 0.043(10) 0.080(14) 0.053(11) 0.005(10) 0.006(9) 0.000(10) C22 0.058(11) 0.043(11) 0.043(9) -0.022(9) -0.002(8) 0.018(9) N3 0.028(7) 0.065(10) 0.036(7) -0.005(7) 0.003(6) 0.001(7) C23 0.034(9) 0.052(12) 0.039(9) 0.008(8) 0.003(7) -0.004(8) N4 0.030(7) 0.061(10) 0.040(8) 0.015(7) -0.011(6) 0.001(7) C24 0.042(10) 0.058(13) 0.057(11) 0.014(10) 0.010(9) -0.006(9) C25 0.066(13) 0.061(13) 0.052(11) 0.013(10) 0.018(10) -0.015(11) C26 0.060(12) 0.049(12) 0.060(11) -0.013(10) -0.009(9) 0.010(10) C27 0.070(13) 0.042(11) 0.046(10) 0.003(9) -0.011(9) -0.016(10) C28 0.033(9) 0.023(9) 0.077(12) -0.003(9) -0.006(9) -0.005(8) C29 0.037(9) 0.045(11) 0.033(8) 0.006(8) -0.006(7) -0.005(8) C30 0.034(9) 0.050(12) 0.046(10) -0.010(9) -0.022(8) -0.004(9) C31 0.049(10) 0.045(11) 0.032(8) -0.003(8) -0.006(8) -0.008(9) C32 0.028(9) 0.071(13) 0.041(9) 0.008(9) -0.011(7) 0.011(9) C33 0.042(10) 0.046(11) 0.041(9) 0.009(9) -0.004(8) 0.014(9) C34 0.036(9) 0.028(10) 0.049(10) -0.010(8) -0.002(8) -0.012(8) C35 0.048(11) 0.083(15) 0.049(10) 0.032(10) -0.007(9) 0.019(10) C36 0.043(10) 0.071(13) 0.040(9) 0.006(9) -0.013(8) -0.022(9) N5 0.036(8) 0.049(9) 0.028(6) -0.007(6) 0.001(6) -0.003(7) C37 0.037(10) 0.066(13) 0.038(9) -0.018(9) -0.015(8) -0.011(9) N6 0.030(8) 0.056(10) 0.065(10) -0.010(8) -0.012(7) 0.005(7) C38 0.027(9) 0.093(16) 0.059(11) 0.018(11) -0.001(9) -0.005(10) C39 0.061(12) 0.061(13) 0.039(9) -0.011(9) -0.001(9) -0.008(10) C40 0.050(11) 0.067(14) 0.057(11) -0.001(10) 0.001(9) 0.003(10) C41 0.066(13) 0.058(13) 0.049(11) 0.010(10) -0.029(9) 0.016(10) C42 0.040(10) 0.075(15) 0.053(11) -0.004(10) -0.003(8) 0.011(10) C43 0.042(10) 0.029(10) 0.038(9) -0.008(8) -0.004(8) -0.004(8) C44 0.041(10) 0.048(12) 0.048(10) -0.009(9) -0.028(8) 0.020(9) C45 0.064(12) 0.020(10) 0.052(10) 0.005(8) -0.020(9) 0.006(9) C46 0.039(10) 0.060(13) 0.063(12) 0.003(11) -0.031(9) 0.017(10) C47 0.034(9) 0.030(10) 0.056(11) -0.007(8) -0.014(8) 0.002(8) C48 0.029(9) 0.040(11) 0.050(10) -0.007(9) -0.020(8) 0.007(8) C49 0.046(11) 0.056(13) 0.091(15) 0.003(11) -0.040(10) -0.003(10) C50 0.040(10) 0.063(13) 0.071(13) 0.028(11) -0.009(9) 0.010(9) N7 0.055(10) 0.073(12) 0.044(9) 0.001(9) -0.028(7) -0.004(9) C51 0.077(14) 0.023(11) 0.061(12) 0.005(9) -0.001(10) 0.007(10) N8 0.045(8) 0.046(9) 0.040(8) 0.005(7) -0.004(7) 0.003(7) C52 0.042(11) 0.089(17) 0.076(14) 0.057(14) -0.026(10) -0.011(11) C53 0.058(14) 0.12(2) 0.065(14) 0.038(15) -0.016(11) 0.020(14) C54 0.047(11) 0.060(13) 0.078(13) 0.026(11) -0.026(10) -0.010(10) C55 0.075(13) 0.046(11) 0.034(9) 0.003(9) -0.032(9) -0.007(10) C56 0.044(10) 0.049(11) 0.038(9) -0.013(8) -0.017(8) -0.006(9) C57 0.076 0.114 0.070 0.000 0.015 0.031 Cl5 0.076 0.114 0.070 0.000 0.015 0.031 Cl6 0.054(7) 0.059(7) 0.195(14) 0.034(8) -0.006(7) 0.025(6) Cl7 0.076 0.114 0.070 0.000 0.015 0.031 C58 0.12(4) 0.16(5) 0.035(19) 0.05(3) 0.04(2) 0.13(4) Cl8 0.064(7) 0.083(8) 0.096(8) -0.043(7) 0.022(6) -0.007(6) Cl9 0.050(5) 0.038(5) 0.050(4) -0.010(4) 0.018(4) 0.017(4) Cl10 0.059(6) 0.176(13) 0.046(5) 0.019(7) 0.020(5) 0.004(7) C59 0.079(15) 0.079(16) 0.081(14) -0.018(13) 0.007(11) 0.040(13) Cl11 0.124(6) 0.112(6) 0.129(6) -0.024(5) -0.030(5) 0.003(5) Cl12 0.143(7) 0.191(9) 0.176(8) 0.020(7) 0.073(6) 0.049(6) Cl13 0.113(5) 0.098(5) 0.088(4) -0.027(4) -0.028(3) 0.013(4) C61 0.076 0.114 0.070 0.000 0.015 0.031 Cl15 0.076 0.114 0.070 0.000 0.015 0.031 Cl14 0.076 0.114 0.070 0.000 0.015 0.031 Cl17 0.076 0.114 0.070 0.000 0.015 0.031 O1 0.148(16) 0.154(18) 0.23(2) 0.114(17) 0.134(16) 0.048(14) O2 0.148(16) 0.154(18) 0.23(2) 0.114(17) 0.134(16) 0.048(14) O3 0.148(16) 0.154(18) 0.23(2) 0.114(17) 0.134(16) 0.048(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 1.943(15) . ? Cu1 N6 1.997(13) . ? Cu1 Cl2 2.243(5) . ? Cu1 Cl1 2.248(5) . ? Cu2 N8 1.947(13) . ? Cu2 N4 1.955(13) . ? Cu2 Cl4 2.246(5) . ? Cu2 Cl3 2.256(5) . ? C1 C2 1.38(2) . ? C1 C6 1.45(2) . ? C1 C56 1.52(2) . ? C2 C3 1.35(2) . ? C2 C7 1.55(2) . ? C3 C4 1.41(2) . ? C3 C8 1.49(2) . ? C4 C5 1.406(19) . ? C4 C12 1.56(2) . ? C5 C6 1.36(2) . ? C5 C14 1.55(2) . ? C6 C13 1.521(19) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 N1 1.45(2) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? N1 C9 1.31(2) . ? N1 C11 1.372(19) . ? C9 N2 1.352(19) . ? C9 H9 0.9500 . ? N2 C10 1.397(19) . ? C10 C11 1.35(2) . ? 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 1.54(2) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.389(18) . ? C15 C20 1.395(18) . ? C16 C17 1.42(2) . ? C16 C21 1.55(2) . ? C17 C18 1.35(2) . ? C17 C22 1.509(18) . ? C18 C19 1.402(19) . ? C18 C26 1.54(2) . ? C19 C20 1.381(19) . ? C19 C28 1.568(19) . ? C20 C27 1.538(19) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 N3 1.468(19) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? N3 C23 1.359(17) . ? N3 C25 1.383(18) . ? C23 N4 1.289(18) . ? C23 H23 0.9500 . ? N4 C24 1.367(18) . ? C24 C25 1.38(2) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.546(19) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.40(2) . ? C29 C34 1.42(2) . ? C30 C31 1.39(2) . ? C30 C35 1.56(2) . ? C31 C32 1.43(2) . ? C31 C36 1.53(2) . ? C32 C33 1.39(2) . ? C32 C40 1.54(2) . ? C33 C34 1.377(19) . ? C33 C42 1.52(2) . ? C34 C41 1.54(2) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 N5 1.453(19) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? N5 C37 1.303(17) . ? N5 C39 1.360(18) . ? C37 N6 1.311(18) . ? C37 H37 0.9500 . ? N6 C38 1.355(18) . ? C38 C39 1.37(2) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C43 1.50(2) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C48 1.38(2) . ? C43 C44 1.45(2) . ? C44 C45 1.39(2) . ? C44 C49 1.52(2) . ? C45 C46 1.40(2) . ? C45 C50 1.56(2) . ? C46 C47 1.39(2) . ? C46 C54 1.54(2) . ? C47 C48 1.39(2) . ? C47 C56 1.53(2) . ? C48 C55 1.52(2) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 N7 1.46(2) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? N7 C51 1.33(2) . ? N7 C53 1.40(2) . ? C51 N8 1.290(19) . ? C51 H51 0.9500 . ? N8 C52 1.40(2) . ? C52 C53 1.39(3) . ? C52 H52 0.9500 . ? C53 H53 0.9500 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 Cl6 1.45(4) . ? C57 Cl5 1.73(5) . ? C57 Cl7 1.92(4) . ? C57 H57 1.0000 . ? C58 Cl8 1.72(6) . ? C58 Cl9 1.73(4) . ? C58 Cl10 1.79(4) . ? C58 H58 1.0000 . ? C59 Cl12 1.679(19) . ? C59 Cl13 1.74(2) . ? C59 Cl11 1.83(2) . ? C59 H59 1.0000 . ? C61 Cl15 1.46(7) . ? C61 Cl17 1.47(7) . ? C61 Cl14 1.77(2) . ? C61 H61 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 N6 139.3(6) . . ? N2 Cu1 Cl2 97.2(4) . . ? N6 Cu1 Cl2 99.8(4) . . ? N2 Cu1 Cl1 94.3(4) . . ? N6 Cu1 Cl1 94.8(4) . . ? Cl2 Cu1 Cl1 141.6(2) . . ? N8 Cu2 N4 143.2(6) . . ? N8 Cu2 Cl4 96.1(4) . . ? N4 Cu2 Cl4 96.2(4) . . ? N8 Cu2 Cl3 93.0(4) . . ? N4 Cu2 Cl3 94.8(4) . . ? Cl4 Cu2 Cl3 147.7(2) . . ? C2 C1 C6 118.7(15) . . ? C2 C1 C56 121.6(15) . . ? C6 C1 C56 119.6(15) . . ? C3 C2 C1 123.2(15) . . ? C3 C2 C7 118.9(14) . . ? C1 C2 C7 117.8(15) . . ? C2 C3 C4 117.9(14) . . ? C2 C3 C8 121.6(16) . . ? C4 C3 C8 120.4(15) . . ? C5 C4 C3 120.9(14) . . ? C5 C4 C12 119.9(14) . . ? C3 C4 C12 119.2(14) . . ? C6 C5 C4 120.3(15) . . ? C6 C5 C14 121.9(13) . . ? C4 C5 C14 117.9(14) . . ? C5 C6 C1 118.8(14) . . ? C5 C6 C13 120.1(14) . . ? C1 C6 C13 120.9(14) . . ? 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 112.0(14) . . ? N1 C8 H8A 109.2 . . ? C3 C8 H8A 109.2 . . ? N1 C8 H8B 109.2 . . ? C3 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? C9 N1 C11 107.4(15) . . ? C9 N1 C8 125.7(14) . . ? C11 N1 C8 126.9(15) . . ? N1 C9 N2 111.9(16) . . ? N1 C9 H9 124.1 . . ? N2 C9 H9 124.1 . . ? C9 N2 C10 104.7(15) . . ? C9 N2 Cu1 125.1(13) . . ? C10 N2 Cu1 130.2(12) . . ? C11 C10 N2 108.3(14) . . ? C11 C10 H10 125.8 . . ? N2 C10 H10 125.8 . . ? C10 C11 N1 107.8(15) . . ? C10 C11 H11 126.1 . . ? N1 C11 H11 126.1 . . ? 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 119.6(13) . . ? C15 C14 H14A 107.4 . . ? C5 C14 H14A 107.4 . . ? C15 C14 H14B 107.4 . . ? C5 C14 H14B 107.4 . . ? H14A C14 H14B 107.0 . . ? C16 C15 C20 120.1(13) . . ? C16 C15 C14 120.0(13) . . ? C20 C15 C14 119.4(13) . . ? C15 C16 C17 120.3(14) . . ? C15 C16 C21 120.1(14) . . ? C17 C16 C21 119.6(13) . . ? C18 C17 C16 119.9(13) . . ? C18 C17 C22 123.3(15) . . ? C16 C17 C22 116.8(13) . . ? C17 C18 C19 118.7(14) . . ? C17 C18 C26 119.9(14) . . ? C19 C18 C26 121.4(14) . . ? C20 C19 C18 123.1(14) . . ? C20 C19 C28 119.1(13) . . ? C18 C19 C28 117.6(13) . . ? C19 C20 C15 117.4(13) . . ? C19 C20 C27 121.3(13) . . ? C15 C20 C27 121.2(13) . . ? 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 . . ? N3 C22 C17 112.3(12) . . ? N3 C22 H22A 109.1 . . ? C17 C22 H22A 109.1 . . ? N3 C22 H22B 109.1 . . ? C17 C22 H22B 109.1 . . ? H22A C22 H22B 107.9 . . ? C23 N3 C25 106.5(14) . . ? C23 N3 C22 127.4(12) . . ? C25 N3 C22 125.8(14) . . ? N4 C23 N3 112.0(13) . . ? N4 C23 H23 124.0 . . ? N3 C23 H23 124.0 . . ? C23 N4 C24 106.9(14) . . ? C23 N4 Cu2 121.1(11) . . ? C24 N4 Cu2 131.1(12) . . ? N4 C24 C25 109.3(15) . . ? N4 C24 H24 125.4 . . ? C25 C24 H24 125.4 . . ? C24 C25 N3 105.3(15) . . ? C24 C25 H25 127.3 . . ? N3 C25 H25 127.3 . . ? C18 C26 H26A 109.5 . . ? C18 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C18 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C20 C27 H27A 109.5 . . ? C20 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C20 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C19 120.1(12) . . ? C29 C28 H28A 107.3 . . ? C19 C28 H28A 107.3 . . ? C29 C28 H28B 107.3 . . ? C19 C28 H28B 107.3 . . ? H28A C28 H28B 106.9 . . ? C30 C29 C34 118.9(14) . . ? C30 C29 C28 120.0(14) . . ? C34 C29 C28 121.0(13) . . ? C31 C30 C29 120.2(15) . . ? C31 C30 C35 119.5(15) . . ? C29 C30 C35 120.0(14) . . ? C30 C31 C32 119.7(14) . . ? C30 C31 C36 121.7(15) . . ? C32 C31 C36 118.6(14) . . ? C33 C32 C31 119.2(14) . . ? C33 C32 C40 122.2(14) . . ? C31 C32 C40 118.5(14) . . ? C34 C33 C32 120.2(14) . . ? C34 C33 C42 120.1(14) . . ? C32 C33 C42 119.4(13) . . ? C33 C34 C29 121.0(14) . . ? C33 C34 C41 120.7(15) . . ? C29 C34 C41 118.3(13) . . ? C30 C35 H35A 109.5 . . ? C30 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C30 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N5 C36 C31 112.0(13) . . ? N5 C36 H36A 109.2 . . ? C31 C36 H36A 109.2 . . ? N5 C36 H36B 109.2 . . ? C31 C36 H36B 109.2 . . ? H36A C36 H36B 107.9 . . ? C37 N5 C39 108.5(13) . . ? C37 N5 C36 125.9(13) . . ? C39 N5 C36 125.4(14) . . ? N5 C37 N6 110.3(14) . . ? N5 C37 H37 124.9 . . ? N6 C37 H37 124.9 . . ? C37 N6 C38 108.2(15) . . ? C37 N6 Cu1 122.8(12) . . ? C38 N6 Cu1 128.2(13) . . ? N6 C38 C39 106.8(17) . . ? N6 C38 H38 126.6 . . ? C39 C38 H38 126.6 . . ? N5 C39 C38 106.3(15) . . ? N5 C39 H39 126.9 . . ? C38 C39 H39 126.9 . . ? C32 C40 H40A 109.5 . . ? C32 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C32 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C34 C41 H41A 109.5 . . ? C34 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C34 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C43 C42 C33 120.0(13) . . ? C43 C42 H42A 107.3 . . ? C33 C42 H42A 107.3 . . ? C43 C42 H42B 107.3 . . ? C33 C42 H42B 107.3 . . ? H42A C42 H42B 106.9 . . ? C48 C43 C44 118.5(15) . . ? C48 C43 C42 123.3(14) . . ? C44 C43 C42 118.1(14) . . ? C45 C44 C43 118.7(15) . . ? C45 C44 C49 120.4(15) . . ? C43 C44 C49 120.9(16) . . ? C44 C45 C46 121.6(15) . . ? C44 C45 C50 117.7(15) . . ? C46 C45 C50 120.5(16) . . ? C47 C46 C45 118.1(17) . . ? C47 C46 C54 122.4(15) . . ? C45 C46 C54 119.2(15) . . ? C46 C47 C48 121.6(15) . . ? C46 C47 C56 117.6(15) . . ? C48 C47 C56 120.6(14) . . ? C43 C48 C47 120.5(14) . . ? C43 C48 C55 120.2(15) . . ? C47 C48 C55 119.2(14) . . ? C44 C49 H49A 109.5 . . ? C44 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C44 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? N7 C50 C45 112.3(14) . . ? N7 C50 H50A 109.1 . . ? C45 C50 H50A 109.1 . . ? N7 C50 H50B 109.1 . . ? C45 C50 H50B 109.1 . . ? H50A C50 H50B 107.9 . . ? C51 N7 C53 111.1(17) . . ? C51 N7 C50 128.3(15) . . ? C53 N7 C50 120.6(18) . . ? N8 C51 N7 111.3(16) . . ? N8 C51 H51 124.4 . . ? N7 C51 H51 124.4 . . ? C51 N8 C52 105.1(16) . . ? C51 N8 Cu2 123.4(12) . . ? C52 N8 Cu2 131.5(13) . . ? C53 C52 N8 111.9(17) . . ? C53 C52 H52 124.0 . . ? N8 C52 H52 124.0 . . ? C52 C53 N7 100.5(19) . . ? C52 C53 H53 129.7 . . ? N7 C53 H53 129.7 . . ? C46 C54 H54A 109.5 . . ? C46 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C46 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C48 C55 H55A 109.5 . . ? C48 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C48 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C1 C56 C47 123.7(14) . . ? C1 C56 H56A 106.4 . . ? C47 C56 H56A 106.4 . . ? C1 C56 H56B 106.4 . . ? C47 C56 H56B 106.4 . . ? H56A C56 H56B 106.5 . . ? Cl6 C57 Cl5 124(3) . . ? Cl6 C57 Cl7 108(3) . . ? Cl5 C57 Cl7 105(2) . . ? Cl6 C57 H57 106.3 . . ? Cl5 C57 H57 106.3 . . ? Cl7 C57 H57 106.3 . . ? Cl8 C58 Cl9 115(2) . . ? Cl8 C58 Cl10 109(2) . . ? Cl9 C58 Cl10 109(3) . . ? Cl8 C58 H58 107.9 . . ? Cl9 C58 H58 107.9 . . ? Cl10 C58 H58 107.9 . . ? Cl12 C59 Cl13 115.7(13) . . ? Cl12 C59 Cl11 109.5(11) . . ? Cl13 C59 Cl11 107.5(11) . . ? Cl12 C59 H59 108.0 . . ? Cl13 C59 H59 108.0 . . ? Cl11 C59 H59 108.0 . . ? Cl15 C61 Cl17 124(6) . . ? Cl15 C61 Cl14 102(3) . . ? Cl17 C61 Cl14 107(4) . . ? Cl15 C61 H61 107.3 . . ? Cl17 C61 H61 107.3 . . ? Cl14 C61 H61 107.3 . . ? _diffrn_measured_fraction_theta_max 0.916 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.916 _refine_diff_density_max 1.935 _refine_diff_density_min -0.762 _refine_diff_density_rms 0.219 # Attachment '4-HgBr2.cif' data_4-HgBr2 _database_code_depnum_ccdc_archive 'CCDC 702197' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H64 Br4 Hg2 N8, 5(C2 H2 Cl4)' _chemical_formula_sum 'C66 H74 Br4 Cl20 Hg2 N8' _chemical_formula_weight 2409.15 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' 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' Hg Hg -2.3894 9.2266 '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 Pbcn _symmetry_space_group_name_Hall '-P 2n 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 17.8054(16) _cell_length_b 18.6149(16) _cell_length_c 27.751(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9197.9(14) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5431 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 22.24 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.740 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4664 _exptl_absorpt_coefficient_mu 5.694 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4272 _exptl_absorpt_correction_T_max 0.5028 _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 83112 _diffrn_reflns_av_R_equivalents 0.0823 _diffrn_reflns_av_sigmaI/netI 0.1088 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 27.53 _reflns_number_total 10575 _reflns_number_gt 5106 _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^)+(0.1854P)^2^+243.5121P] 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 10575 _refine_ls_number_parameters 455 _refine_ls_number_restraints 44 _refine_ls_R_factor_all 0.2310 _refine_ls_R_factor_gt 0.1340 _refine_ls_wR_factor_ref 0.3722 _refine_ls_wR_factor_gt 0.3065 _refine_ls_goodness_of_fit_ref 1.154 _refine_ls_restrained_S_all 1.579 _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 Hg1 Hg -0.12437(7) 0.14549(7) 0.48986(5) 0.0510(5) Uani 1 1 d . . . Br1 Br -0.1659(3) 0.1404(2) 0.57778(17) 0.0831(13) Uani 1 1 d . . . Br2 Br -0.19383(18) 0.07421(15) 0.41842(10) 0.0473(8) Uani 1 1 d . . . C1 C 0.0586(14) 0.0843(13) 0.2802(9) 0.032(5) Uani 1 1 d . . . C2 C 0.0746(14) 0.0627(12) 0.3273(10) 0.036(6) Uani 1 1 d . . . C3 C 0.1271(14) 0.0980(14) 0.3535(9) 0.035(6) Uani 1 1 d . . . C4 C 0.1653(15) 0.1610(12) 0.3347(9) 0.032(6) Uani 1 1 d . . . C5 C 0.1533(13) 0.1798(13) 0.2875(10) 0.031(5) Uani 1 1 d . . . C6 C 0.1004(13) 0.1416(12) 0.2586(9) 0.029(5) Uani 1 1 d . . . C7 C 0.0317(18) 0.0002(16) 0.3484(13) 0.056(8) Uani 1 1 d . . . H7A H -0.0201 0.0150 0.3550 0.084 Uiso 1 1 calc R . . H7B H 0.0558 -0.0151 0.3784 0.084 Uiso 1 1 calc R . . H7C H 0.0316 -0.0397 0.3254 0.084 Uiso 1 1 calc R . . C8 C 0.154(2) 0.0723(15) 0.4030(13) 0.059(9) Uani 1 1 d . . . H8A H 0.1639 0.0200 0.4015 0.070 Uiso 1 1 calc R . . H8B H 0.2028 0.0962 0.4104 0.070 Uiso 1 1 calc R . . N1 N 0.1017(14) 0.0868(13) 0.4420(8) 0.044(6) Uani 1 1 d . . . C9 C 0.0324(18) 0.1199(16) 0.4394(11) 0.048(7) Uani 1 1 d . . . H9 H 0.0114 0.1389 0.4106 0.058 Uiso 1 1 calc R . . N2 N -0.0002(14) 0.1218(14) 0.4808(8) 0.047(6) Uani 1 1 d . . . C10 C 0.048(2) 0.0844(18) 0.5109(13) 0.065(10) Uani 1 1 d . . . H10 H 0.0364 0.0722 0.5433 0.078 Uiso 1 1 calc R . . C11 C 0.1077(19) 0.0687(18) 0.4900(12) 0.053(8) Uani 1 1 d . . . H11 H 0.1505 0.0477 0.5048 0.064 Uiso 1 1 calc R . . C12 C 0.2197(15) 0.2040(17) 0.3654(10) 0.045(7) Uani 1 1 d . . . H12A H 0.2714 0.1920 0.3563 0.067 Uiso 1 1 calc R . . H12B H 0.2119 0.1925 0.3995 0.067 Uiso 1 1 calc R . . H12C H 0.2111 0.2555 0.3602 0.067 Uiso 1 1 calc R . . C13 C 0.0918(15) 0.1566(14) 0.2052(10) 0.039(6) Uani 1 1 d . . . H13A H 0.0946 0.1113 0.1873 0.059 Uiso 1 1 calc R . . H13B H 0.1321 0.1887 0.1946 0.059 Uiso 1 1 calc R . . H13C H 0.0430 0.1794 0.1993 0.059 Uiso 1 1 calc R . . C14 C 0.2005(14) 0.2391(13) 0.2620(11) 0.041(7) Uani 1 1 d . . . H14A H 0.2327 0.2619 0.2867 0.049 Uiso 1 1 calc R . . H14B H 0.2345 0.2148 0.2389 0.049 Uiso 1 1 calc R . . C15 C 0.1609(16) 0.2980(14) 0.2353(11) 0.042(7) Uani 1 1 d . . . C16 C 0.1905(15) 0.3162(15) 0.1898(10) 0.042(7) Uani 1 1 d . . . C17 C 0.1537(18) 0.3719(15) 0.1641(10) 0.045(7) Uani 1 1 d . . . C18 C 0.0896(16) 0.4073(13) 0.1799(9) 0.038(6) Uani 1 1 d . . . C19 C 0.0632(15) 0.3879(13) 0.2282(10) 0.038(6) Uani 1 1 d . . . C20 C 0.1016(15) 0.3358(13) 0.2551(10) 0.035(6) Uani 1 1 d . . . C21 C 0.2573(16) 0.2787(18) 0.1693(12) 0.056(8) Uani 1 1 d . . . H21A H 0.2723 0.3023 0.1392 0.084 Uiso 1 1 calc R . . H21B H 0.2446 0.2284 0.1627 0.084 Uiso 1 1 calc R . . H21C H 0.2989 0.2808 0.1924 0.084 Uiso 1 1 calc R . . C22 C 0.192(2) 0.399(2) 0.1180(11) 0.061(9) Uani 1 1 d . . . H22A H 0.1805 0.4501 0.1132 0.073 Uiso 1 1 calc R . . H22B H 0.2472 0.3936 0.1213 0.073 Uiso 1 1 calc R . . N3 N -0.1657(16) 0.3563(12) 0.4251(9) 0.052(7) Uani 1 1 d . . . C23 C -0.1484(17) 0.2856(16) 0.4258(11) 0.047(7) Uani 1 1 d . . . H23 H -0.1441 0.2563 0.3979 0.057 Uiso 1 1 calc R . . N4 N -0.1383(13) 0.2629(13) 0.4697(9) 0.044(6) Uani 1 1 d . . . C24 C -0.152(2) 0.320(2) 0.4995(14) 0.067(10) Uani 1 1 d . . . H24 H -0.1487 0.3188 0.5337 0.080 Uiso 1 1 calc R . . C25 C -0.170(2) 0.377(2) 0.4744(13) 0.075(12) Uani 1 1 d . . . H25 H -0.1835 0.4229 0.4865 0.090 Uiso 1 1 calc R . . C26 C 0.0535(17) 0.4617(15) 0.1494(12) 0.051(8) Uani 1 1 d . . . H26A H 0.0807 0.5072 0.1523 0.077 Uiso 1 1 calc R . . H26B H 0.0014 0.4684 0.1598 0.077 Uiso 1 1 calc R . . H26C H 0.0543 0.4457 0.1158 0.077 Uiso 1 1 calc R . . C27 C 0.0823(16) 0.3254(15) 0.3069(11) 0.044(7) Uani 1 1 d . . . H27A H 0.0793 0.3723 0.3229 0.066 Uiso 1 1 calc R . . H27B H 0.1212 0.2962 0.3224 0.066 Uiso 1 1 calc R . . H27C H 0.0337 0.3009 0.3094 0.066 Uiso 1 1 calc R . . C28 C 0.0000 0.4329(16) 0.2500 0.037(9) Uani 1 2 d S . . H28A H 0.0213 0.4643 0.2754 0.045 Uiso 0.50 1 calc PR . . H28B H -0.0213 0.4643 0.2246 0.045 Uiso 0.50 1 calc PR . . C29 C 0.0000 0.0432(16) 0.2500 0.037(9) Uani 1 2 d S . . H29A H -0.0280 0.0115 0.2723 0.045 Uiso 0.50 1 calc PR . . H29B H 0.0280 0.0115 0.2277 0.045 Uiso 0.50 1 calc PR . . C30 C 0.139(3) 0.401(3) 0.4859(19) 0.101(18) Uani 1 1 d . . . H30 H 0.1884 0.4050 0.5023 0.121 Uiso 1 1 calc R . . Cl1 Cl 0.1393(8) 0.4694(6) 0.4398(5) 0.098(4) Uani 1 1 d . . . Cl2 Cl 0.0733(9) 0.4217(8) 0.5297(5) 0.119(5) Uani 1 1 d . . . C31 C 0.138(2) 0.334(3) 0.465(2) 0.091(14) Uani 1 1 d . . . H31 H 0.1802 0.3301 0.4413 0.109 Uiso 1 1 calc R . . Cl3 Cl 0.0473(7) 0.3203(7) 0.4339(5) 0.100(4) Uani 1 1 d . . . Cl4 Cl 0.1504(8) 0.2668(6) 0.5103(6) 0.104(4) Uani 1 1 d . . . C32 C 0.0087(11) 0.3082(10) 0.6295(10) 0.108 Uani 0.50 1 d PD . . H32 H 0.0335 0.2995 0.5977 0.130 Uiso 0.50 1 calc PR . . Cl5 Cl -0.0648(7) 0.3647(6) 0.6184(5) 0.041(3) Uani 0.50 1 d PD . . Cl6 Cl 0.0787(9) 0.3337(7) 0.6685(9) 0.041(3) Uani 0.50 1 d PD . . C33 C -0.0262(13) 0.2390(11) 0.6437(10) 0.108 Uani 0.50 1 d PD . . H33 H -0.0652 0.2285 0.6187 0.130 Uiso 0.50 1 calc PR . . Cl7 Cl -0.0734(14) 0.2446(14) 0.6978(8) 0.134(11) Uani 0.50 1 d PD . . Cl8 Cl 0.0449(8) 0.1785(6) 0.6339(8) 0.073(6) Uani 0.50 1 d PD . . C34 C 0.7490(10) 0.0537(10) 0.7419(6) 0.167(5) Uani 1 1 d D . . C35 C 0.7533(10) -0.0319(10) 0.7379(6) 0.167(5) Uani 1 1 d D . . Cl9 Cl 0.8277(12) 0.0611(15) 0.7785(10) 0.167(5) Uani 0.50 1 d PD . . Cl10 Cl 0.7805(15) 0.0766(13) 0.6856(8) 0.167(5) Uani 0.50 1 d PD . . Cl11 Cl 0.6767(11) -0.0414(14) 0.6997(10) 0.167(5) Uani 0.50 1 d PD . . Cl12 Cl 0.7178(15) -0.0521(13) 0.7936(8) 0.167(5) Uani 0.50 1 d PD . . Cl1A Cl 0.8383(11) 0.0712(14) 0.7611(11) 0.167(5) Uani 0.50 1 d PD . . Cl1B Cl 0.7512(15) 0.0694(14) 0.6806(7) 0.167(5) Uani 0.50 1 d PD . . Cl1C Cl 0.6617(10) -0.0488(13) 0.7226(11) 0.167(5) Uani 0.50 1 d PD . . Cl1D Cl 0.7517(15) -0.0464(14) 0.7998(7) 0.167(5) Uani 0.50 1 d PD . . 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 0.0576(8) 0.0521(8) 0.0434(7) -0.0004(5) 0.0068(6) -0.0030(6) Br1 0.086(3) 0.079(3) 0.085(3) 0.002(2) -0.004(2) 0.008(2) Br2 0.0629(19) 0.0427(16) 0.0362(14) -0.0033(12) -0.0036(13) -0.0119(13) C1 0.029(13) 0.038(14) 0.030(13) 0.004(11) 0.005(10) 0.007(10) C2 0.035(14) 0.013(11) 0.059(17) 0.007(11) 0.002(12) 0.013(10) C3 0.031(13) 0.045(15) 0.030(13) 0.002(11) 0.000(11) 0.009(12) C4 0.042(15) 0.027(13) 0.027(12) 0.004(10) -0.006(11) 0.001(10) C5 0.017(11) 0.028(13) 0.047(16) -0.007(11) 0.004(11) 0.003(9) C6 0.027(12) 0.019(11) 0.042(14) -0.003(10) -0.003(10) 0.013(9) C7 0.053(18) 0.044(17) 0.07(2) 0.017(16) 0.006(17) -0.003(14) C8 0.07(2) 0.026(15) 0.08(2) 0.014(15) -0.003(19) 0.012(14) N1 0.051(15) 0.047(14) 0.035(13) 0.005(10) 0.004(11) 0.012(11) C9 0.057(19) 0.053(18) 0.035(15) -0.003(13) 0.012(14) 0.010(14) N2 0.042(14) 0.061(15) 0.037(13) -0.002(11) 0.002(11) 0.002(12) C10 0.09(3) 0.044(18) 0.06(2) 0.014(16) -0.01(2) -0.017(18) C11 0.05(2) 0.06(2) 0.051(18) 0.019(16) -0.010(16) 0.010(15) C12 0.033(15) 0.063(18) 0.038(15) -0.010(13) -0.006(12) -0.008(13) C13 0.028(13) 0.037(15) 0.052(17) -0.006(12) 0.004(12) -0.010(11) C14 0.027(13) 0.031(13) 0.065(19) -0.009(13) 0.003(13) -0.012(11) C15 0.041(16) 0.028(13) 0.057(18) 0.003(12) -0.011(14) -0.004(11) C16 0.041(16) 0.028(13) 0.057(18) 0.003(12) -0.011(14) -0.004(11) C17 0.061(19) 0.041(16) 0.032(14) -0.006(12) -0.002(14) -0.034(14) C18 0.051(16) 0.026(13) 0.036(14) 0.001(11) -0.006(13) -0.020(12) C19 0.045(16) 0.022(12) 0.048(16) -0.001(11) -0.006(13) -0.006(11) C20 0.037(14) 0.031(13) 0.037(14) -0.001(11) 0.007(11) -0.006(10) C21 0.030(15) 0.07(2) 0.07(2) 0.003(17) 0.015(15) -0.013(14) C22 0.07(2) 0.07(2) 0.048(19) -0.003(16) 0.023(17) 0.002(18) N3 0.071(18) 0.033(13) 0.051(15) -0.011(11) 0.014(13) 0.012(12) C23 0.050(18) 0.044(17) 0.048(18) -0.002(14) 0.001(14) 0.010(13) N4 0.045(14) 0.043(13) 0.042(13) -0.019(11) 0.002(11) 0.005(10) C24 0.07(2) 0.07(3) 0.06(2) 0.000(19) -0.015(18) 0.00(2) C25 0.10(3) 0.08(3) 0.05(2) -0.04(2) 0.03(2) -0.02(2) C26 0.053(18) 0.038(16) 0.06(2) 0.019(14) -0.009(15) -0.015(13) C27 0.043(16) 0.036(15) 0.054(18) 0.004(13) 0.000(14) 0.004(12) C28 0.05(2) 0.006(14) 0.05(2) 0.000 -0.003(19) 0.000 C29 0.026(18) 0.007(14) 0.08(3) 0.000 -0.005(18) 0.000 C30 0.07(3) 0.11(4) 0.12(4) -0.05(3) 0.02(3) -0.04(3) Cl1 0.131(10) 0.060(6) 0.105(9) 0.013(6) 0.007(7) 0.004(6) Cl2 0.128(11) 0.105(10) 0.123(11) -0.042(8) 0.052(9) 0.005(8) C31 0.06(3) 0.09(3) 0.12(4) -0.01(3) 0.01(3) -0.01(2) Cl3 0.107(9) 0.090(8) 0.104(9) -0.008(7) -0.009(7) -0.031(7) Cl4 0.098(8) 0.065(6) 0.149(12) 0.024(7) 0.008(8) 0.016(6) C32 0.111 0.146 0.068 0.015 0.002 0.000 Cl5 0.032(6) 0.042(7) 0.049(8) -0.002(6) -0.012(6) 0.002(5) Cl6 0.032(6) 0.042(7) 0.049(8) -0.002(6) -0.012(6) 0.002(5) C33 0.111 0.146 0.068 0.015 0.002 0.000 Cl7 0.16(3) 0.17(3) 0.071(15) 0.029(17) 0.010(16) -0.05(2) Cl8 0.052(10) 0.029(8) 0.139(18) 0.001(9) -0.024(10) -0.020(7) C34 0.103(8) 0.179(9) 0.219(12) -0.076(9) 0.045(8) 0.058(7) C35 0.103(8) 0.179(9) 0.219(12) -0.076(9) 0.045(8) 0.058(7) Cl9 0.103(8) 0.179(9) 0.219(12) -0.076(9) 0.045(8) 0.058(7) Cl10 0.103(8) 0.179(9) 0.219(12) -0.076(9) 0.045(8) 0.058(7) Cl11 0.103(8) 0.179(9) 0.219(12) -0.076(9) 0.045(8) 0.058(7) Cl12 0.103(8) 0.179(9) 0.219(12) -0.076(9) 0.045(8) 0.058(7) Cl1A 0.103(8) 0.179(9) 0.219(12) -0.076(9) 0.045(8) 0.058(7) Cl1B 0.103(8) 0.179(9) 0.219(12) -0.076(9) 0.045(8) 0.058(7) Cl1C 0.103(8) 0.179(9) 0.219(12) -0.076(9) 0.045(8) 0.058(7) Cl1D 0.103(8) 0.179(9) 0.219(12) -0.076(9) 0.045(8) 0.058(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 N2 2.27(3) . ? Hg1 N4 2.27(3) . ? Hg1 Br1 2.551(5) . ? Hg1 Br2 2.687(3) . ? C1 C2 1.40(4) . ? C1 C6 1.43(3) . ? C1 C29 1.54(3) . ? C2 C3 1.35(4) . ? C2 C7 1.51(4) . ? C3 C4 1.45(4) . ? C3 C8 1.53(4) . ? C4 C5 1.37(4) . ? C4 C12 1.52(4) . ? C5 C6 1.43(3) . ? C5 C14 1.56(4) . ? C6 C13 1.52(4) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 N1 1.46(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? N1 C11 1.38(4) . ? N1 C9 1.38(4) . ? C9 N2 1.29(4) . ? C9 H9 0.9500 . ? N2 C10 1.38(4) . ? C10 C11 1.25(5) . ? 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 1.50(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C20 1.38(4) . ? C15 C16 1.41(4) . ? C16 C17 1.42(4) . ? C16 C21 1.49(4) . ? C17 C18 1.39(4) . ? C17 C22 1.53(4) . ? C18 C19 1.47(4) . ? C18 C26 1.47(4) . ? C19 C20 1.40(4) . ? C19 C28 1.53(3) . ? C20 C27 1.49(4) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 N3 1.51(4) 3 ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? N3 C23 1.35(4) . ? N3 C25 1.42(4) . ? N3 C22 1.51(4) 3 ? C23 N4 1.30(4) . ? C23 H23 0.9500 . ? N4 C24 1.37(5) . ? C24 C25 1.31(6) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C19 1.53(3) 3 ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C1 1.54(3) 3 ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.38(6) . ? C30 Cl2 1.73(5) . ? C30 Cl1 1.81(6) . ? C30 H30 1.0000 . ? C31 Cl4 1.78(6) . ? C31 Cl3 1.85(5) . ? C31 H31 1.0000 . ? C32 C33 1.48(2) . ? C32 Cl5 1.707(13) . ? C32 Cl6 1.718(13) . ? C32 H32 1.0000 . ? C33 Cl8 1.715(13) . ? C33 Cl7 1.724(13) . ? C33 H33 1.0000 . ? C34 Cl1A 1.709(13) . ? C34 Cl10 1.715(13) . ? C34 Cl1B 1.726(13) . ? C34 Cl9 1.736(13) . ? C35 Cl12 1.712(13) . ? C35 Cl1C 1.713(13) . ? C35 Cl11 1.735(13) . ? C35 Cl1D 1.740(13) . ? 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 105.5(9) . . ? N2 Hg1 Br1 112.4(6) . . ? N4 Hg1 Br1 103.9(6) . . ? N2 Hg1 Br2 105.7(6) . . ? N4 Hg1 Br2 104.1(6) . . ? Br1 Hg1 Br2 123.62(13) . . ? C2 C1 C6 120(2) . . ? C2 C1 C29 120(2) . . ? C6 C1 C29 120(2) . . ? C3 C2 C1 120(2) . . ? C3 C2 C7 121(3) . . ? C1 C2 C7 119(3) . . ? C2 C3 C4 121(2) . . ? C2 C3 C8 123(3) . . ? C4 C3 C8 115(2) . . ? C5 C4 C3 118(2) . . ? C5 C4 C12 120(2) . . ? C3 C4 C12 122(2) . . ? C4 C5 C6 121(2) . . ? C4 C5 C14 122(2) . . ? C6 C5 C14 117(2) . . ? C5 C6 C1 119(2) . . ? C5 C6 C13 122(2) . . ? C1 C6 C13 120(2) . . ? 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(2) . . ? N1 C8 H8A 108.8 . . ? C3 C8 H8A 108.8 . . ? N1 C8 H8B 108.8 . . ? C3 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? C11 N1 C9 103(2) . . ? C11 N1 C8 129(3) . . ? C9 N1 C8 128(2) . . ? N2 C9 N1 112(3) . . ? N2 C9 H9 124.2 . . ? N1 C9 H9 124.2 . . ? C9 N2 C10 104(3) . . ? C9 N2 Hg1 123(2) . . ? C10 N2 Hg1 129(2) . . ? C11 C10 N2 111(3) . . ? C11 C10 H10 124.3 . . ? N2 C10 H10 124.3 . . ? C10 C11 N1 109(3) . . ? C10 C11 H11 125.6 . . ? N1 C11 H11 125.6 . . ? 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(2) . . ? C15 C14 H14A 107.5 . . ? C5 C14 H14A 107.5 . . ? C15 C14 H14B 107.5 . . ? C5 C14 H14B 107.5 . . ? H14A C14 H14B 107.0 . . ? C20 C15 C16 121(2) . . ? C20 C15 C14 122(3) . . ? C16 C15 C14 116(3) . . ? C15 C16 C17 117(2) . . ? C15 C16 C21 122(3) . . ? C17 C16 C21 121(3) . . ? C18 C17 C16 124(2) . . ? C18 C17 C22 118(3) . . ? C16 C17 C22 117(3) . . ? C17 C18 C19 116(2) . . ? C17 C18 C26 120(3) . . ? C19 C18 C26 124(3) . . ? C20 C19 C18 120(2) . . ? C20 C19 C28 122(2) . . ? C18 C19 C28 118(2) . . ? C15 C20 C19 121(3) . . ? C15 C20 C27 120(2) . . ? C19 C20 C27 119(2) . . ? 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 . . ? N3 C22 C17 111(3) 3 . ? N3 C22 H22A 109.5 3 . ? C17 C22 H22A 109.5 . . ? N3 C22 H22B 109.5 3 . ? C17 C22 H22B 109.5 . . ? H22A C22 H22B 108.1 . . ? C23 N3 C25 105(3) . . ? C23 N3 C22 126(3) . 3 ? C25 N3 C22 127(3) . 3 ? N4 C23 N3 111(3) . . ? N4 C23 H23 124.4 . . ? N3 C23 H23 124.4 . . ? C23 N4 C24 107(3) . . ? C23 N4 Hg1 123.9(19) . . ? C24 N4 Hg1 128(2) . . ? C25 C24 N4 110(3) . . ? C25 C24 H24 124.8 . . ? N4 C24 H24 124.8 . . ? C24 C25 N3 106(3) . . ? C24 C25 H25 126.8 . . ? N3 C25 H25 126.8 . . ? C18 C26 H26A 109.5 . . ? C18 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C18 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C20 C27 H27A 109.5 . . ? C20 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C20 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C19 C28 C19 113(3) 3 . ? C19 C28 H28A 108.9 3 . ? C19 C28 H28A 108.9 . . ? C19 C28 H28B 108.9 3 . ? C19 C28 H28B 108.9 . . ? H28A C28 H28B 107.7 . . ? C1 C29 C1 120(3) . 3 ? C1 C29 H29A 107.2 . . ? C1 C29 H29A 107.2 3 . ? C1 C29 H29B 107.2 . . ? C1 C29 H29B 107.2 3 . ? H29A C29 H29B 106.8 . . ? C31 C30 Cl2 120(4) . . ? C31 C30 Cl1 110(4) . . ? Cl2 C30 Cl1 110(3) . . ? C31 C30 H30 105.1 . . ? Cl2 C30 H30 105.1 . . ? Cl1 C30 H30 105.1 . . ? C30 C31 Cl4 110(4) . . ? C30 C31 Cl3 109(4) . . ? Cl4 C31 Cl3 110(2) . . ? C30 C31 H31 109.4 . . ? Cl4 C31 H31 109.4 . . ? Cl3 C31 H31 109.4 . . ? C33 C32 Cl5 105.2(13) . . ? C33 C32 Cl6 112.1(15) . . ? Cl5 C32 Cl6 119.9(13) . . ? C33 C32 H32 106.2 . . ? Cl5 C32 H32 106.2 . . ? Cl6 C32 H32 106.2 . . ? C32 C33 Cl8 102.7(12) . . ? C32 C33 Cl7 112.5(15) . . ? Cl8 C33 Cl7 122.5(16) . . ? C32 C33 H33 106.0 . . ? Cl8 C33 H33 106.0 . . ? Cl7 C33 H33 106.0 . . ? C35 C34 Cl1A 99.6(12) . . ? C35 C34 Cl10 99.6(12) . . ? Cl1A C34 Cl10 86.1(16) . . ? C35 C34 Cl1B 95.6(11) . . ? Cl1A C34 Cl1B 104.7(13) . . ? C35 C34 Cl9 94.7(11) . . ? Cl10 C34 Cl9 104.4(13) . . ? Cl1B C34 Cl9 123.0(16) . . ? C34 C35 Cl12 97.9(11) . . ? C34 C35 Cl1C 98.9(11) . . ? Cl12 C35 Cl1C 80.3(15) . . ? C34 C35 Cl11 96.1(11) . . ? Cl12 C35 Cl11 103.8(12) . . ? C34 C35 Cl1D 94.8(11) . . ? Cl1C C35 Cl1D 101.5(12) . . ? Cl11 C35 Cl1D 125.1(15) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.148 _refine_diff_density_min -1.107 _refine_diff_density_rms 0.361 # Attachment '4-HgCl2.cif' data_4-HgCl2 _database_code_depnum_ccdc_archive 'CCDC 702198' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C56 H64 Cl4 Hg2 N8),C2 H4 Cl2, C H3 OH, 6(H2 O)' _chemical_formula_sum 'C115 H148 Cl10 Hg4 N16 O7' _chemical_formula_weight 3023.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 '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 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 23.0451(6) _cell_length_b 20.3100(5) _cell_length_c 14.8872(4) _cell_angle_alpha 90.00 _cell_angle_beta 101.1480(10) _cell_angle_gamma 90.00 _cell_volume 6836.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9901 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 25.21 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.469 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2992 _exptl_absorpt_coefficient_mu 4.726 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3729 _exptl_absorpt_correction_T_max 0.6757 _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 118316 _diffrn_reflns_av_R_equivalents 0.0825 _diffrn_reflns_av_sigmaI/netI 0.0655 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 27.59 _reflns_number_total 15815 _reflns_number_gt 11792 _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^)+(0.1023P)^2^+252.6564P] 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 15815 _refine_ls_number_parameters 688 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.1461 _refine_ls_R_factor_gt 0.1158 _refine_ls_wR_factor_ref 0.3051 _refine_ls_wR_factor_gt 0.2859 _refine_ls_goodness_of_fit_ref 1.138 _refine_ls_restrained_S_all 1.139 _refine_ls_shift/su_max 0.003 _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 0.99063(3) 0.26105(3) 1.07190(4) 0.03522(18) Uani 1 1 d . . . Cl1 Cl 1.06976(19) 0.3380(2) 1.1129(3) 0.0461(10) Uani 1 1 d . . . Cl2 Cl 0.88902(18) 0.2720(2) 0.9878(3) 0.0419(9) Uani 1 1 d . . . Hg2 Hg 0.55799(4) -0.15963(4) 0.60275(5) 0.0539(2) Uani 1 1 d . . . Cl3 Cl 0.6486(2) -0.1172(3) 0.5576(3) 0.0608(13) Uani 1 1 d . . . Cl4 Cl 0.4765(4) -0.2176(3) 0.5121(5) 0.0608(13) Uani 1 1 d . . . C1 C 0.8704(6) -0.0351(7) 0.8125(8) 0.024(3) Uani 1 1 d . . . C2 C 0.9266(6) -0.0048(7) 0.8194(9) 0.023(3) Uani 1 1 d . . . C3 C 0.9294(7) 0.0586(7) 0.7833(9) 0.027(3) Uani 1 1 d . . . C4 C 0.8784(7) 0.0959(7) 0.7513(9) 0.029(3) Uani 1 1 d . . . C5 C 0.8228(7) 0.0654(7) 0.7484(9) 0.027(3) Uani 1 1 d . . . C6 C 0.8200(6) -0.0007(7) 0.7739(8) 0.022(3) Uani 1 1 d . . . C7 C 0.9837(6) -0.0378(7) 0.8627(11) 0.033(3) Uani 1 1 d . . . H7A H 0.9776 -0.0637 0.9156 0.050 Uiso 1 1 calc R . . H7B H 1.0141 -0.0043 0.8826 0.050 Uiso 1 1 calc R . . H7C H 0.9966 -0.0670 0.8179 0.050 Uiso 1 1 calc R . . C8 C 0.9873(7) 0.0874(8) 0.7732(10) 0.033(3) Uani 1 1 d . . . H8A H 1.0153 0.0509 0.7699 0.040 Uiso 1 1 calc R . . H8B H 0.9817 0.1116 0.7145 0.040 Uiso 1 1 calc R . . N1 N 1.0143(5) 0.1325(6) 0.8476(8) 0.028(2) Uani 1 1 d . . . C9 C 0.9900(6) 0.1508(8) 0.9199(10) 0.032(3) Uani 1 1 d . . . H9 H 0.9528 0.1362 0.9308 0.038 Uiso 1 1 calc R . . N2 N 1.0258(6) 0.1917(6) 0.9728(8) 0.034(3) Uani 1 1 d . . . C10 C 1.0725(7) 0.2020(8) 0.9334(10) 0.032(3) Uani 1 1 d . . . H10 H 1.1049 0.2302 0.9562 0.038 Uiso 1 1 calc R . . C11 C 1.0662(7) 0.1658(7) 0.8564(10) 0.030(3) Uani 1 1 d . . . H11 H 1.0932 0.1639 0.8156 0.036 Uiso 1 1 calc R . . C12 C 0.8827(7) 0.1660(8) 0.7240(10) 0.037(3) Uani 1 1 d . . . H12A H 0.8682 0.1704 0.6579 0.055 Uiso 1 1 calc R . . H12B H 0.9241 0.1803 0.7392 0.055 Uiso 1 1 calc R . . H12C H 0.8587 0.1935 0.7568 0.055 Uiso 1 1 calc R . . C13 C 0.7599(6) -0.0346(7) 0.7543(10) 0.031(3) Uani 1 1 d . . . H13A H 0.7398 -0.0277 0.8058 0.046 Uiso 1 1 calc R . . H13B H 0.7654 -0.0819 0.7458 0.046 Uiso 1 1 calc R . . H13C H 0.7358 -0.0161 0.6985 0.046 Uiso 1 1 calc R . . C14 C 0.7664(7) 0.1049(8) 0.7100(10) 0.038(4) Uani 1 1 d . . . H14A H 0.7789 0.1508 0.7014 0.045 Uiso 1 1 calc R . . H14B H 0.7504 0.0872 0.6482 0.045 Uiso 1 1 calc R . . C15 C 0.7168(6) 0.1085(7) 0.7587(11) 0.032(3) Uani 1 1 d . . . C16 C 0.6585(7) 0.1052(8) 0.7076(11) 0.037(4) Uani 1 1 d . . . C17 C 0.6102(6) 0.1089(7) 0.7524(11) 0.031(3) Uani 1 1 d . . . C18 C 0.6190(7) 0.1143(8) 0.8504(11) 0.035(3) Uani 1 1 d . . . C19 C 0.6780(7) 0.1219(8) 0.8990(10) 0.034(3) Uani 1 1 d . . . C20 C 0.7256(7) 0.1208(7) 0.8551(10) 0.034(4) Uani 1 1 d . . . C21 C 0.6488(8) 0.0971(11) 0.6044(11) 0.049(5) Uani 1 1 d . . . H21A H 0.6068 0.1033 0.5779 0.074 Uiso 1 1 calc R . . H21B H 0.6611 0.0529 0.5896 0.074 Uiso 1 1 calc R . . H21C H 0.6722 0.1300 0.5789 0.074 Uiso 1 1 calc R . . C22 C 0.5483(8) 0.1115(9) 0.6978(13) 0.049(5) Uani 1 1 d . . . H22A H 0.5218 0.1311 0.7357 0.059 Uiso 1 1 calc R . . H22B H 0.5473 0.1402 0.6437 0.059 Uiso 1 1 calc R . . N3 N 0.5260(6) 0.0446(8) 0.6666(9) 0.041(3) Uani 1 1 d . . . C23 C 0.5549(9) -0.0129(9) 0.6782(13) 0.055(5) Uani 1 1 d . . . H23 H 0.5945 -0.0181 0.7102 0.066 Uiso 1 1 calc R . . N4 N 0.5213(7) -0.0609(8) 0.6394(10) 0.046(4) Uani 1 1 d . . . C24 C 0.4677(8) -0.0345(11) 0.6002(13) 0.055(5) Uani 1 1 d . . . H24 H 0.4348 -0.0582 0.5673 0.066 Uiso 1 1 calc R . . C25 C 0.4696(7) 0.0322(11) 0.6164(12) 0.049(5) Uani 1 1 d . . . H25 H 0.4389 0.0633 0.5974 0.059 Uiso 1 1 calc R . . C26 C 0.5667(8) 0.1113(10) 0.8977(13) 0.047(4) Uani 1 1 d . . . H26A H 0.5797 0.0957 0.9607 0.071 Uiso 1 1 calc R . . H26B H 0.5369 0.0811 0.8646 0.071 Uiso 1 1 calc R . . H26C H 0.5494 0.1554 0.8987 0.071 Uiso 1 1 calc R . . C27 C 0.7857(7) 0.1373(8) 0.9071(10) 0.034(3) Uani 1 1 d . . . H27A H 0.7826 0.1708 0.9533 0.052 Uiso 1 1 calc R . . H27B H 0.8099 0.1543 0.8648 0.052 Uiso 1 1 calc R . . H27C H 0.8043 0.0976 0.9373 0.052 Uiso 1 1 calc R . . C28 C 0.6867(7) 0.1383(9) 0.9999(11) 0.039(4) Uani 1 1 d . . . H28A H 0.6476 0.1355 1.0177 0.047 Uiso 1 1 calc R . . H28B H 0.6995 0.1849 1.0073 0.047 Uiso 1 1 calc R . . C29 C 0.7303(7) 0.0974(7) 1.0691(10) 0.031(3) Uani 1 1 d . . . C30 C 0.7675(6) 0.1314(8) 1.1426(10) 0.031(3) Uani 1 1 d . . . C31 C 0.8097(6) 0.0967(8) 1.2047(10) 0.030(3) Uani 1 1 d . . . C32 C 0.8155(7) 0.0272(7) 1.1974(9) 0.028(3) Uani 1 1 d . . . C33 C 0.7751(7) -0.0053(8) 1.1266(10) 0.033(3) Uani 1 1 d . . . C34 C 0.7338(7) 0.0290(8) 1.0668(10) 0.031(3) Uani 1 1 d . . . C35 C 0.7616(8) 0.2051(8) 1.1506(12) 0.042(4) Uani 1 1 d . . . H35A H 0.7839 0.2198 1.2100 0.062 Uiso 1 1 calc R . . H35B H 0.7198 0.2166 1.1454 0.062 Uiso 1 1 calc R . . H35C H 0.7773 0.2267 1.1014 0.062 Uiso 1 1 calc R . . C36 C 0.8488(7) 0.1318(9) 1.2846(10) 0.037(4) Uani 1 1 d . . . H36A H 0.8280 0.1713 1.3010 0.044 Uiso 1 1 calc R . . H36B H 0.8563 0.1022 1.3384 0.044 Uiso 1 1 calc R . . N5 N 0.9053(5) 0.1515(6) 1.2612(7) 0.027(3) Uani 1 1 d . . . C37 C 0.9135(7) 0.1761(7) 1.1803(10) 0.032(3) Uani 1 1 d . . . H37 H 0.8839 0.1779 1.1262 0.038 Uiso 1 1 calc R . . N6 N 0.9671(5) 0.1969(6) 1.1867(9) 0.030(3) Uani 1 1 d . . . C38 C 0.9964(8) 0.1844(8) 1.2724(10) 0.037(4) Uani 1 1 d . . . H38 H 1.0370 0.1932 1.2951 0.045 Uiso 1 1 calc R . . C39 C 0.9585(7) 0.1572(9) 1.3213(11) 0.039(4) Uani 1 1 d . . . H39 H 0.9669 0.1447 1.3839 0.047 Uiso 1 1 calc R . . C40 C 0.8624(7) -0.0077(9) 1.2629(11) 0.039(4) Uani 1 1 d . . . H40A H 0.8447 -0.0294 1.3099 0.059 Uiso 1 1 calc R . . H40B H 0.8922 0.0241 1.2919 0.059 Uiso 1 1 calc R . . H40C H 0.8811 -0.0407 1.2299 0.059 Uiso 1 1 calc R . . C41 C 0.6867(8) -0.0079(8) 1.0003(11) 0.039(4) Uani 1 1 d . . . H41A H 0.6540 0.0220 0.9764 0.059 Uiso 1 1 calc R . . H41B H 0.6719 -0.0447 1.0321 0.059 Uiso 1 1 calc R . . H41C H 0.7038 -0.0249 0.9496 0.059 Uiso 1 1 calc R . . C42 C 0.7775(7) -0.0802(8) 1.1227(10) 0.034(3) Uani 1 1 d . . . H42A H 0.7417 -0.0969 1.1428 0.041 Uiso 1 1 calc R . . H42B H 0.8118 -0.0943 1.1695 0.041 Uiso 1 1 calc R . . C43 C 0.7818(6) -0.1168(7) 1.0330(8) 0.025(3) Uani 1 1 d . . . C44 C 0.7460(7) -0.1717(7) 1.0081(9) 0.028(3) Uani 1 1 d . . . C45 C 0.7522(7) -0.2082(7) 0.9299(10) 0.030(3) Uani 1 1 d . . . C46 C 0.7919(7) -0.1868(7) 0.8748(9) 0.031(3) Uani 1 1 d . . . C47 C 0.8248(6) -0.1300(7) 0.8982(9) 0.025(3) Uani 1 1 d . . . C48 C 0.8218(7) -0.0960(7) 0.9803(10) 0.032(3) Uani 1 1 d . . . C49 C 0.6998(10) -0.1945(9) 1.0618(12) 0.052(5) Uani 1 1 d . . . H49A H 0.7196 -0.2137 1.1201 0.077 Uiso 1 1 calc R . . H49B H 0.6742 -0.2277 1.0263 0.077 Uiso 1 1 calc R . . H49C H 0.6758 -0.1568 1.0737 0.077 Uiso 1 1 calc R . . C50 C 0.7162(9) -0.2698(8) 0.9071(11) 0.044(4) Uani 1 1 d . . . H50A H 0.7396 -0.3027 0.8802 0.053 Uiso 1 1 calc R . . H50B H 0.7069 -0.2888 0.9639 0.053 Uiso 1 1 calc R . . N7 N 0.6609(8) -0.2562(8) 0.8421(11) 0.065(6) Uani 1 1 d D . . C51 C 0.6500(7) -0.2164(8) 0.7732(10) 0.039(4) Uani 1 1 d D . . H51 H 0.6796 -0.1886 0.7574 0.046 Uiso 1 1 calc R . . N8 N 0.5974(8) -0.2168(9) 0.7279(12) 0.073(6) Uani 1 1 d D . . C52 C 0.5644(10) -0.2579(9) 0.7806(13) 0.051 Uani 1 1 d D . . H52 H 0.5232 -0.2673 0.7667 0.061 Uiso 1 1 calc R . . C53 C 0.6046(9) -0.2801(9) 0.8539(14) 0.051 Uani 1 1 d D . . H53 H 0.5967 -0.3063 0.9031 0.061 Uiso 1 1 calc R . . C54 C 0.7986(9) -0.2263(8) 0.7897(11) 0.042(4) Uani 1 1 d . . . H54A H 0.8404 -0.2368 0.7925 0.063 Uiso 1 1 calc R . . H54B H 0.7838 -0.2001 0.7347 0.063 Uiso 1 1 calc R . . H54C H 0.7757 -0.2672 0.7874 0.063 Uiso 1 1 calc R . . C55 C 0.8660(7) -0.0423(7) 1.0122(10) 0.033(3) Uani 1 1 d . . . H55A H 0.8501 0.0000 0.9869 0.050 Uiso 1 1 calc R . . H55B H 0.9029 -0.0518 0.9912 0.050 Uiso 1 1 calc R . . H55C H 0.8738 -0.0401 1.0792 0.050 Uiso 1 1 calc R . . C56 C 0.8675(6) -0.1072(7) 0.8399(9) 0.025(3) Uani 1 1 d . . . H56A H 0.8591 -0.1332 0.7826 0.030 Uiso 1 1 calc R . . H56B H 0.9076 -0.1198 0.8722 0.030 Uiso 1 1 calc R . . Cl5 Cl 0.4063(7) 0.7947(8) 0.7836(12) 0.105(5) Uani 0.50 1 d PD . . Cl6 Cl 0.2648(5) 0.8209(10) 0.5729(10) 0.112(7) Uani 0.50 1 d PD . . C57 C 0.3499(17) 0.7860(16) 0.687(2) 0.067(13) Uani 0.50 1 d PD . . H57A H 0.3664 0.7661 0.6370 0.080 Uiso 0.50 1 calc PR . . H57B H 0.3194 0.7557 0.7020 0.080 Uiso 0.50 1 calc PR . . C58 C 0.324(2) 0.8437(16) 0.659(4) 0.139 Uani 0.50 1 d PD . . H58A H 0.3521 0.8726 0.6342 0.167 Uiso 0.50 1 calc PR . . H58B H 0.3105 0.8667 0.7093 0.167 Uiso 0.50 1 calc PR . . O2 O 0.5639(7) 0.8951(6) 0.8996(7) 0.0516(19) Uani 1 1 d . . . O1 O 0.0762(7) 0.5560(6) 0.9745(7) 0.0516(19) Uani 1 1 d . . . O3 O 0.8295(7) 0.8565(6) 0.5731(7) 0.0516(19) Uani 1 1 d . . . O4 O 0.7403(9) 0.5411(11) 0.8893(14) 0.034(4) Uani 0.50 1 d P . . C59 C 0.7294(14) 0.4659(16) 0.895(2) 0.034(4) 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 Hg1 0.0362(3) 0.0360(3) 0.0337(3) -0.0059(2) 0.0073(2) -0.0043(3) Cl1 0.042(2) 0.048(2) 0.050(2) -0.0176(19) 0.0130(18) -0.0124(19) Cl2 0.036(2) 0.054(2) 0.0324(19) 0.0055(17) -0.0001(15) 0.0008(18) Hg2 0.0661(5) 0.0443(4) 0.0422(4) 0.0022(3) -0.0123(3) -0.0027(4) Cl3 0.057(3) 0.072(3) 0.051(3) -0.009(2) 0.005(2) 0.022(3) Cl4 0.057(3) 0.072(3) 0.051(3) -0.009(2) 0.005(2) 0.022(3) C1 0.024(7) 0.029(7) 0.017(6) 0.001(5) -0.003(5) 0.000(6) C2 0.015(6) 0.032(7) 0.023(6) -0.003(5) 0.004(5) 0.006(5) C3 0.034(8) 0.027(7) 0.021(6) -0.004(5) 0.010(6) -0.007(6) C4 0.030(8) 0.032(7) 0.020(6) -0.005(5) -0.007(5) -0.002(6) C5 0.034(8) 0.029(7) 0.016(6) 0.004(5) 0.001(5) 0.003(6) C6 0.019(6) 0.033(7) 0.014(5) 0.002(5) -0.001(5) 0.008(5) C7 0.021(7) 0.027(7) 0.048(9) -0.003(6) -0.002(6) -0.002(6) C8 0.034(8) 0.041(8) 0.028(7) -0.007(6) 0.014(6) 0.007(7) N1 0.028(6) 0.030(6) 0.025(6) 0.002(5) 0.001(5) -0.001(5) C9 0.022(7) 0.036(8) 0.037(8) -0.001(6) 0.004(6) -0.003(6) N2 0.039(7) 0.034(7) 0.026(6) -0.009(5) 0.002(5) -0.003(6) C10 0.026(7) 0.038(8) 0.031(7) 0.003(6) 0.005(6) 0.001(6) C11 0.028(7) 0.025(7) 0.038(8) 0.005(6) 0.011(6) -0.004(6) C12 0.041(9) 0.041(9) 0.027(7) 0.012(6) 0.004(6) -0.001(7) C13 0.026(7) 0.034(8) 0.029(7) 0.001(6) -0.003(6) 0.001(6) C14 0.040(9) 0.041(9) 0.028(7) -0.001(6) -0.006(6) 0.014(7) C15 0.018(7) 0.030(7) 0.042(8) 0.003(6) -0.008(6) 0.001(6) C16 0.025(8) 0.037(8) 0.039(8) -0.009(7) -0.015(6) 0.014(6) C17 0.021(7) 0.030(7) 0.039(8) -0.002(6) -0.007(6) 0.005(6) C18 0.029(8) 0.032(8) 0.040(8) -0.006(6) -0.007(6) 0.004(6) C19 0.035(8) 0.034(8) 0.028(7) -0.006(6) -0.004(6) 0.003(7) C20 0.044(9) 0.025(7) 0.024(7) -0.010(5) -0.018(6) 0.001(6) C21 0.037(9) 0.074(13) 0.029(8) -0.004(8) -0.014(7) 0.012(9) C22 0.039(10) 0.042(9) 0.052(10) -0.004(8) -0.028(8) 0.014(8) N3 0.027(7) 0.059(9) 0.031(7) -0.010(6) -0.011(5) 0.000(6) C23 0.045(11) 0.043(10) 0.057(11) -0.005(8) -0.036(9) 0.006(8) N4 0.036(8) 0.062(10) 0.037(7) -0.004(7) 0.000(6) -0.005(7) C24 0.034(10) 0.081(15) 0.043(10) 0.002(10) -0.011(8) -0.022(10) C25 0.022(8) 0.078(14) 0.042(9) -0.001(9) -0.007(7) -0.003(8) C26 0.030(9) 0.060(11) 0.049(10) -0.010(9) 0.002(7) 0.006(8) C27 0.029(8) 0.040(8) 0.032(8) -0.009(6) 0.000(6) 0.005(7) C28 0.028(8) 0.042(9) 0.044(9) -0.005(7) 0.000(7) 0.009(7) C29 0.034(8) 0.034(8) 0.026(7) -0.005(6) 0.006(6) -0.004(6) C30 0.023(7) 0.039(8) 0.028(7) -0.002(6) 0.000(5) -0.001(6) C31 0.025(7) 0.042(8) 0.024(7) -0.011(6) 0.004(5) -0.006(6) C32 0.029(7) 0.038(8) 0.017(6) -0.001(5) 0.003(5) 0.002(6) C33 0.032(8) 0.041(8) 0.026(7) 0.000(6) 0.004(6) -0.002(7) C34 0.025(7) 0.039(8) 0.028(7) -0.006(6) 0.001(6) 0.000(6) C35 0.043(10) 0.040(9) 0.039(9) -0.009(7) -0.001(7) 0.006(8) C36 0.034(8) 0.053(10) 0.023(7) -0.017(7) 0.003(6) -0.008(7) N5 0.036(7) 0.028(6) 0.015(5) -0.006(4) -0.003(4) -0.010(5) C37 0.029(8) 0.034(8) 0.030(7) -0.001(6) -0.004(6) 0.002(6) N6 0.028(6) 0.021(6) 0.039(7) -0.007(5) 0.004(5) -0.003(5) C38 0.038(9) 0.047(9) 0.026(7) -0.008(6) 0.004(6) -0.004(7) C39 0.021(7) 0.054(10) 0.035(8) -0.015(7) -0.011(6) 0.006(7) C40 0.036(9) 0.049(10) 0.028(8) -0.002(7) -0.003(6) 0.011(7) C41 0.047(10) 0.034(8) 0.031(8) -0.003(6) -0.005(7) -0.001(7) C42 0.035(8) 0.045(9) 0.021(7) 0.001(6) 0.002(6) -0.007(7) C43 0.028(7) 0.030(7) 0.013(6) 0.008(5) -0.003(5) -0.005(6) C44 0.036(8) 0.028(7) 0.022(6) 0.001(5) 0.007(6) -0.005(6) C45 0.028(7) 0.027(7) 0.029(7) 0.011(6) -0.011(6) -0.003(6) C46 0.031(8) 0.029(7) 0.025(7) -0.001(5) -0.012(6) 0.009(6) C47 0.015(6) 0.031(7) 0.022(6) 0.001(5) -0.012(5) -0.005(5) C48 0.030(8) 0.026(7) 0.032(7) 0.002(6) -0.008(6) -0.007(6) C49 0.074(14) 0.046(10) 0.040(9) -0.001(8) 0.024(9) -0.016(10) C50 0.065(12) 0.032(8) 0.028(8) 0.002(6) -0.006(7) -0.005(8) N7 0.061(11) 0.070(11) 0.051(9) 0.027(8) -0.023(8) -0.050(9) C51 0.035(9) 0.043(9) 0.034(8) 0.008(7) -0.003(6) -0.004(7) N8 0.059(11) 0.072(12) 0.070(12) 0.029(10) -0.038(9) -0.037(10) C52 0.062 0.035 0.051 0.000 0.000 0.000 C53 0.062 0.035 0.051 0.000 0.000 0.000 C54 0.056(11) 0.034(8) 0.033(8) -0.006(6) -0.001(7) -0.006(8) C55 0.042(9) 0.033(8) 0.024(7) -0.004(6) 0.004(6) -0.008(7) C56 0.021(7) 0.024(6) 0.029(7) -0.002(5) 0.002(5) 0.007(5) Cl5 0.084(10) 0.095(10) 0.112(12) 0.003(9) -0.039(9) -0.003(8) Cl6 0.038(6) 0.216(19) 0.087(9) -0.077(11) 0.024(6) -0.063(9) C57 0.09(4) 0.030(18) 0.08(3) -0.018(19) 0.02(3) -0.01(2) C58 0.080 0.024 0.298 0.008 0.000 0.000 O2 0.085(6) 0.051(4) 0.015(3) 0.000(3) -0.001(3) 0.001(4) O1 0.085(6) 0.051(4) 0.015(3) 0.000(3) -0.001(3) 0.001(4) O3 0.085(6) 0.051(4) 0.015(3) 0.000(3) -0.001(3) 0.001(4) O4 0.034(9) 0.042(10) 0.033(9) -0.006(7) 0.025(7) 0.015(8) C59 0.034(9) 0.042(10) 0.033(9) -0.006(7) 0.025(7) 0.015(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 N6 2.295(13) . ? Hg1 N2 2.297(12) . ? Hg1 Cl1 2.390(4) . ? Hg1 Cl2 2.443(4) . ? Hg2 N8 2.234(16) . ? Hg2 N4 2.283(16) . ? Hg2 Cl4 2.400(6) . ? Hg2 Cl3 2.469(6) . ? C1 C6 1.382(18) . ? C1 C2 1.420(19) . ? C1 C56 1.525(19) . ? C2 C3 1.402(19) . ? C2 C7 1.507(19) . ? C3 C4 1.40(2) . ? C3 C8 1.49(2) . ? C4 C5 1.41(2) . ? C4 C12 1.49(2) . ? C5 C6 1.401(19) . ? C5 C14 1.54(2) . ? C6 C13 1.52(2) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 N1 1.479(19) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? N1 C9 1.358(19) . ? N1 C11 1.359(18) . ? C9 N2 1.319(19) . ? C9 H9 0.9500 . ? N2 C10 1.34(2) . ? C10 C11 1.35(2) . ? 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 1.47(2) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.413(19) . ? C15 C20 1.43(2) . ? C16 C17 1.40(2) . ? C16 C21 1.52(2) . ? C17 C18 1.44(2) . ? C17 C22 1.50(2) . ? C18 C19 1.42(2) . ? C18 C26 1.51(2) . ? C19 C20 1.38(2) . ? C19 C28 1.51(2) . ? C20 C27 1.49(2) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 N3 1.49(2) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? N3 C23 1.34(2) . ? N3 C25 1.39(2) . ? C23 N4 1.31(2) . ? C23 H23 0.9500 . ? N4 C24 1.37(2) . ? C24 C25 1.38(3) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.54(2) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C34 1.39(2) . ? C29 C30 1.43(2) . ? C30 C31 1.40(2) . ? C30 C35 1.51(2) . ? C31 C32 1.42(2) . ? C31 C36 1.523(19) . ? C32 C33 1.43(2) . ? C32 C40 1.49(2) . ? C33 C34 1.36(2) . ? C33 C42 1.52(2) . ? C34 C41 1.52(2) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 N5 1.47(2) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? N5 C37 1.351(19) . ? N5 C39 1.374(17) . ? C37 N6 1.292(19) . ? C37 H37 0.9500 . ? N6 C38 1.35(2) . ? C38 C39 1.36(2) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C43 1.55(2) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C48 1.39(2) . ? C43 C44 1.394(19) . ? C44 C45 1.41(2) . ? C44 C49 1.52(2) . ? C45 C46 1.41(2) . ? C45 C50 1.50(2) . ? C46 C47 1.39(2) . ? C46 C54 1.53(2) . ? C47 C48 1.42(2) . ? C47 C56 1.506(19) . ? C48 C55 1.51(2) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 N7 1.47(2) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? N7 C51 1.29(2) . ? N7 C53 1.43(3) . ? C51 N8 1.27(2) . ? C51 H51 0.9500 . ? N8 C52 1.46(3) . ? C52 C53 1.37(3) . ? C52 H52 0.9500 . ? C53 H53 0.9500 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? Cl5 C57 1.749(19) . ? Cl6 C58 1.75(2) . ? C57 C58 1.341(19) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? O4 C59 1.55(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 Hg1 N2 107.0(4) . . ? N6 Hg1 Cl1 117.3(3) . . ? N2 Hg1 Cl1 102.6(3) . . ? N6 Hg1 Cl2 95.3(3) . . ? N2 Hg1 Cl2 98.5(3) . . ? Cl1 Hg1 Cl2 132.84(16) . . ? N8 Hg2 N4 111.5(7) . . ? N8 Hg2 Cl4 111.2(4) . . ? N4 Hg2 Cl4 106.2(4) . . ? N8 Hg2 Cl3 100.4(5) . . ? N4 Hg2 Cl3 97.5(4) . . ? Cl4 Hg2 Cl3 129.0(3) . . ? C6 C1 C2 119.5(13) . . ? C6 C1 C56 121.3(12) . . ? C2 C1 C56 118.9(12) . . ? C3 C2 C1 118.7(12) . . ? C3 C2 C7 118.1(13) . . ? C1 C2 C7 123.2(13) . . ? C2 C3 C4 121.8(13) . . ? C2 C3 C8 120.5(13) . . ? C4 C3 C8 117.6(13) . . ? C3 C4 C5 118.0(13) . . ? C3 C4 C12 120.8(14) . . ? C5 C4 C12 121.2(13) . . ? C6 C5 C4 120.1(13) . . ? C6 C5 C14 121.3(13) . . ? C4 C5 C14 118.5(13) . . ? C1 C6 C5 121.2(13) . . ? C1 C6 C13 120.8(13) . . ? C5 C6 C13 118.0(12) . . ? 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 115.0(11) . . ? N1 C8 H8A 108.5 . . ? C3 C8 H8A 108.5 . . ? N1 C8 H8B 108.5 . . ? C3 C8 H8B 108.5 . . ? H8A C8 H8B 107.5 . . ? C9 N1 C11 106.1(12) . . ? C9 N1 C8 125.8(12) . . ? C11 N1 C8 128.0(12) . . ? N2 C9 N1 109.9(13) . . ? N2 C9 H9 125.1 . . ? N1 C9 H9 125.1 . . ? C9 N2 C10 107.4(13) . . ? C9 N2 Hg1 120.8(11) . . ? C10 N2 Hg1 126.8(10) . . ? N2 C10 C11 109.0(14) . . ? N2 C10 H10 125.5 . . ? C11 C10 H10 125.5 . . ? C10 C11 N1 107.5(13) . . ? C10 C11 H11 126.2 . . ? N1 C11 H11 126.2 . . ? 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 121.6(13) . . ? C15 C14 H14A 106.9 . . ? C5 C14 H14A 106.9 . . ? C15 C14 H14B 106.9 . . ? C5 C14 H14B 106.9 . . ? H14A C14 H14B 106.7 . . ? C16 C15 C20 118.9(15) . . ? C16 C15 C14 118.8(14) . . ? C20 C15 C14 122.1(13) . . ? C17 C16 C15 119.9(14) . . ? C17 C16 C21 120.8(13) . . ? C15 C16 C21 119.3(15) . . ? C16 C17 C18 121.2(13) . . ? C16 C17 C22 120.1(15) . . ? C18 C17 C22 118.6(15) . . ? C19 C18 C17 117.3(15) . . ? C19 C18 C26 122.6(15) . . ? C17 C18 C26 120.1(14) . . ? C20 C19 C18 121.8(14) . . ? C20 C19 C28 120.5(14) . . ? C18 C19 C28 117.4(14) . . ? C19 C20 C15 120.4(13) . . ? C19 C20 C27 119.7(13) . . ? C15 C20 C27 119.8(15) . . ? 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 . . ? N3 C22 C17 111.7(13) . . ? N3 C22 H22A 109.3 . . ? C17 C22 H22A 109.3 . . ? N3 C22 H22B 109.3 . . ? C17 C22 H22B 109.3 . . ? H22A C22 H22B 107.9 . . ? C23 N3 C25 107.6(15) . . ? C23 N3 C22 128.3(13) . . ? C25 N3 C22 124.1(15) . . ? N4 C23 N3 110.8(15) . . ? N4 C23 H23 124.6 . . ? N3 C23 H23 124.6 . . ? C23 N4 C24 107.8(17) . . ? C23 N4 Hg2 123.0(13) . . ? C24 N4 Hg2 125.9(13) . . ? N4 C24 C25 108.3(16) . . ? N4 C24 H24 125.8 . . ? C25 C24 H24 125.8 . . ? C24 C25 N3 105.5(17) . . ? C24 C25 H25 127.2 . . ? N3 C25 H25 127.2 . . ? C18 C26 H26A 109.5 . . ? C18 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C18 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C20 C27 H27A 109.5 . . ? C20 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C20 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C19 C28 C29 119.4(13) . . ? C19 C28 H28A 107.5 . . ? C29 C28 H28A 107.5 . . ? C19 C28 H28B 107.5 . . ? C29 C28 H28B 107.5 . . ? H28A C28 H28B 107.0 . . ? C34 C29 C30 118.2(14) . . ? C34 C29 C28 123.8(14) . . ? C30 C29 C28 117.9(13) . . ? C31 C30 C29 120.0(14) . . ? C31 C30 C35 120.7(13) . . ? C29 C30 C35 119.3(14) . . ? C30 C31 C32 120.9(13) . . ? C30 C31 C36 120.7(14) . . ? C32 C31 C36 118.3(14) . . ? C31 C32 C33 117.2(13) . . ? C31 C32 C40 119.3(13) . . ? C33 C32 C40 123.5(14) . . ? C34 C33 C32 121.3(15) . . ? C34 C33 C42 120.8(14) . . ? C32 C33 C42 117.8(13) . . ? C33 C34 C29 122.0(14) . . ? C33 C34 C41 119.6(14) . . ? C29 C34 C41 118.2(14) . . ? C30 C35 H35A 109.5 . . ? C30 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C30 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N5 C36 C31 111.2(11) . . ? N5 C36 H36A 109.4 . . ? C31 C36 H36A 109.4 . . ? N5 C36 H36B 109.4 . . ? C31 C36 H36B 109.4 . . ? H36A C36 H36B 108.0 . . ? C37 N5 C39 106.8(13) . . ? C37 N5 C36 126.5(12) . . ? C39 N5 C36 126.1(13) . . ? N6 C37 N5 110.6(13) . . ? N6 C37 H37 124.7 . . ? N5 C37 H37 124.7 . . ? C37 N6 C38 107.7(13) . . ? C37 N6 Hg1 119.4(10) . . ? C38 N6 Hg1 131.7(11) . . ? N6 C38 C39 109.2(14) . . ? N6 C38 H38 125.4 . . ? C39 C38 H38 125.4 . . ? C38 C39 N5 105.7(14) . . ? C38 C39 H39 127.1 . . ? N5 C39 H39 127.1 . . ? C32 C40 H40A 109.5 . . ? C32 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C32 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C34 C41 H41A 109.5 . . ? C34 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C34 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C33 C42 C43 121.4(12) . . ? C33 C42 H42A 107.0 . . ? C43 C42 H42A 107.0 . . ? C33 C42 H42B 107.0 . . ? C43 C42 H42B 107.0 . . ? H42A C42 H42B 106.7 . . ? C48 C43 C44 121.2(13) . . ? C48 C43 C42 120.1(12) . . ? C44 C43 C42 118.7(12) . . ? C43 C44 C45 119.4(13) . . ? C43 C44 C49 122.8(13) . . ? C45 C44 C49 117.8(13) . . ? C44 C45 C46 119.9(13) . . ? C44 C45 C50 119.0(14) . . ? C46 C45 C50 121.1(14) . . ? C47 C46 C45 119.6(13) . . ? C47 C46 C54 120.4(14) . . ? C45 C46 C54 120.0(14) . . ? C46 C47 C48 120.5(13) . . ? C46 C47 C56 119.8(13) . . ? C48 C47 C56 119.6(12) . . ? C43 C48 C47 119.2(13) . . ? C43 C48 C55 121.7(13) . . ? C47 C48 C55 118.9(14) . . ? C44 C49 H49A 109.5 . . ? C44 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C44 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? N7 C50 C45 111.2(13) . . ? N7 C50 H50A 109.4 . . ? C45 C50 H50A 109.4 . . ? N7 C50 H50B 109.4 . . ? C45 C50 H50B 109.4 . . ? H50A C50 H50B 108.0 . . ? C51 N7 C53 105.6(16) . . ? C51 N7 C50 130.7(15) . . ? C53 N7 C50 123.2(15) . . ? N8 C51 N7 116.0(17) . . ? N8 C51 H51 122.0 . . ? N7 C51 H51 122.0 . . ? C51 N8 C52 105.2(16) . . ? C51 N8 Hg2 129.3(14) . . ? C52 N8 Hg2 125.2(13) . . ? C53 C52 N8 106.0(18) . . ? C53 C52 H52 127.0 . . ? N8 C52 H52 127.0 . . ? C52 C53 N7 106.3(18) . . ? C52 C53 H53 126.8 . . ? N7 C53 H53 126.8 . . ? C46 C54 H54A 109.5 . . ? C46 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C46 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C48 C55 H55A 109.5 . . ? C48 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C48 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C47 C56 C1 121.1(11) . . ? C47 C56 H56A 107.0 . . ? C1 C56 H56A 107.0 . . ? C47 C56 H56B 107.0 . . ? C1 C56 H56B 107.0 . . ? H56A C56 H56B 106.8 . . ? C58 C57 Cl5 113(2) . . ? C58 C57 H57A 109.1 . . ? Cl5 C57 H57A 109.1 . . ? C58 C57 H57B 109.1 . . ? Cl5 C57 H57B 109.1 . . ? H57A C57 H57B 107.8 . . ? C57 C58 Cl6 104(2) . . ? C57 C58 H58A 111.0 . . ? Cl6 C58 H58A 111.0 . . ? C57 C58 H58B 111.0 . . ? Cl6 C58 H58B 111.0 . . ? H58A C58 H58B 109.0 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.59 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.669 _refine_diff_density_min -1.462 _refine_diff_density_rms 0.317 # Attachment '4-ZnBr2.cif' data_4-ZnBr2 _database_code_depnum_ccdc_archive 'CCDC 702199' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C56 H64 Br4 N8 Zn2), 5(C H Cl3)' _chemical_formula_sum 'C117 H133 Br8 Cl15 N16 Zn4' _chemical_formula_weight 3195.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 23.051(3) _cell_length_b 20.621(3) _cell_length_c 15.319(2) _cell_angle_alpha 90.00 _cell_angle_beta 103.778(3) _cell_angle_gamma 90.00 _cell_volume 7072.4(16) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3906 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 18.78 _exptl_crystal_description needdle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.501 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3204 _exptl_absorpt_coefficient_mu 3.262 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7362 _exptl_absorpt_correction_T_max 0.9376 _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 64341 _diffrn_reflns_av_R_equivalents 0.0637 _diffrn_reflns_av_sigmaI/netI 0.1086 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 27.27 _reflns_number_total 15818 _reflns_number_gt 6059 _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^)+(0.1900P)^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 15818 _refine_ls_number_parameters 764 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.2470 _refine_ls_R_factor_gt 0.1019 _refine_ls_wR_factor_ref 0.3630 _refine_ls_wR_factor_gt 0.2789 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.024 _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 0.98783(6) 0.25786(7) 1.05676(10) 0.0343(4) Uani 1 1 d . . . Br1 Br 1.06568(6) 0.33260(6) 1.11877(10) 0.0429(4) Uani 1 1 d . . . Br2 Br 0.89052(6) 0.29039(8) 0.97373(10) 0.0501(4) Uani 1 1 d . . . Zn2 Zn 0.56153(8) -0.16167(8) 0.59132(11) 0.0514(5) Uani 1 1 d . . . Br3 Br 0.64845(7) -0.12574(8) 0.54153(11) 0.0586(5) Uani 1 1 d . . . Br4 Br 0.48991(8) -0.22672(8) 0.49446(12) 0.0649(5) Uani 1 1 d . . . C1 C 0.8238(5) 0.0671(5) 0.7435(8) 0.030(3) Uani 1 1 d . . . C2 C 0.8797(5) 0.0957(6) 0.7524(8) 0.033(3) Uani 1 1 d . . . C3 C 0.9310(5) 0.0603(6) 0.7900(8) 0.031(3) Uani 1 1 d . . . C4 C 0.9268(5) -0.0023(6) 0.8222(7) 0.027(3) Uani 1 1 d . . . C5 C 0.8715(5) -0.0336(6) 0.8103(8) 0.034(3) Uani 1 1 d . . . C6 C 0.8202(5) 0.0013(6) 0.7698(8) 0.029(3) Uani 1 1 d . . . C7 C 0.8848(6) 0.1635(6) 0.7200(10) 0.047(4) Uani 1 1 d . . . H7A H 0.9270 0.1756 0.7310 0.070 Uiso 1 1 calc R . . H7B H 0.8643 0.1934 0.7524 0.070 Uiso 1 1 calc R . . H7C H 0.8664 0.1660 0.6555 0.070 Uiso 1 1 calc R . . C8 C 0.9921(5) 0.0877(6) 0.7851(8) 0.033(3) Uani 1 1 d . . . H8A H 1.0213 0.0518 0.7913 0.040 Uiso 1 1 calc R . . H8B H 0.9888 0.1082 0.7257 0.040 Uiso 1 1 calc R . . N1 N 1.0141(4) 0.1367(5) 0.8576(7) 0.033(2) Uani 1 1 d . . . C9 C 0.9866(5) 0.1579(6) 0.9191(8) 0.030(3) Uani 1 1 d . . . H9 H 0.9483 0.1438 0.9241 0.036 Uiso 1 1 calc R . . N2 N 1.0191(5) 0.2005(5) 0.9717(7) 0.037(3) Uani 1 1 d . . . C10 C 1.0708(5) 0.2082(6) 0.9430(8) 0.035(3) Uani 1 1 d . . . H10 H 1.1029 0.2364 0.9689 0.042 Uiso 1 1 calc R . . C11 C 1.0683(5) 0.1684(6) 0.8713(8) 0.032(3) Uani 1 1 d . . . H11 H 1.0977 0.1634 0.8376 0.038 Uiso 1 1 calc R . . C12 C 0.9828(5) -0.0380(6) 0.8642(9) 0.040(3) Uani 1 1 d . . . H12A H 0.9756 -0.0666 0.9116 0.060 Uiso 1 1 calc R . . H12B H 1.0143 -0.0069 0.8904 0.060 Uiso 1 1 calc R . . H12C H 0.9954 -0.0639 0.8184 0.060 Uiso 1 1 calc R . . C13 C 0.7596(5) -0.0327(6) 0.7447(9) 0.038(3) Uani 1 1 d . . . H13A H 0.7648 -0.0770 0.7247 0.057 Uiso 1 1 calc R . . H13B H 0.7328 -0.0087 0.6960 0.057 Uiso 1 1 calc R . . H13C H 0.7423 -0.0341 0.7972 0.057 Uiso 1 1 calc R . . C14 C 0.8674(5) -0.1031(5) 0.8342(8) 0.030(3) Uani 1 1 d . . . H14A H 0.9077 -0.1173 0.8670 0.036 Uiso 1 1 calc R . . H14B H 0.8571 -0.1281 0.7774 0.036 Uiso 1 1 calc R . . C15 C 0.8243(5) -0.1228(6) 0.8893(8) 0.033(3) Uani 1 1 d . . . C16 C 0.8220(5) -0.0910(5) 0.9697(8) 0.028(3) Uani 1 1 d . . . C17 C 0.7824(5) -0.1102(6) 1.0212(8) 0.032(3) Uani 1 1 d . . . C18 C 0.7451(5) -0.1645(6) 0.9929(9) 0.037(3) Uani 1 1 d . . . C19 C 0.7495(5) -0.2002(6) 0.9165(8) 0.032(3) Uani 1 1 d . . . C20 C 0.7877(6) -0.1806(6) 0.8653(9) 0.040(3) Uani 1 1 d . . . C21 C 0.8681(5) -0.0399(6) 1.0043(8) 0.035(3) Uani 1 1 d . . . H21A H 0.9035 -0.0479 0.9810 0.052 Uiso 1 1 calc R . . H21B H 0.8792 -0.0411 1.0701 0.052 Uiso 1 1 calc R . . H21C H 0.8516 0.0029 0.9842 0.052 Uiso 1 1 calc R . . C22 C 0.7003(6) -0.1859(6) 1.0461(10) 0.048(4) Uani 1 1 d . . . H22A H 0.664 -0.196 1.007 0.071 Uiso 1 1 calc R . . H22B H 0.695 -0.153 1.084 0.071 Uiso 1 1 calc R . . H22C H 0.715 -0.223 1.080 0.071 Uiso 1 1 calc R . . C23 C 0.7121(6) -0.2601(6) 0.8913(10) 0.046(3) Uani 1 1 d . . . H23A H 0.7353 -0.2927 0.8665 0.055 Uiso 1 1 calc R . . H23B H 0.7029 -0.2787 0.9461 0.055 Uiso 1 1 calc R . . N3 N 0.6555(5) -0.2469(6) 0.8245(7) 0.048(3) Uani 1 1 d . . . C24 C 0.6009(9) -0.2745(10) 0.8231(15) 0.113(10) Uani 1 1 d . . . H24 H 0.5924 -0.3026 0.8676 0.136 Uiso 1 1 calc R . . C25 C 0.5612(9) -0.2547(12) 0.7476(15) 0.116(9) Uani 1 1 d . . . H25 H 0.5208 -0.2679 0.7269 0.139 Uiso 1 1 calc R . . N4 N 0.5927(6) -0.2104(6) 0.7064(8) 0.055(3) Uani 1 1 d . . . C26 C 0.6471(6) -0.2072(6) 0.7558(9) 0.044(3) Uani 1 1 d . . . H26 H 0.6771 -0.1794 0.7435 0.052 Uiso 1 1 calc R . . C27 C 0.7949(6) -0.2177(6) 0.7820(9) 0.042(3) Uani 1 1 d . . . H27A H 0.8369 -0.2297 0.7891 0.063 Uiso 1 1 calc R . . H27B H 0.7821 -0.1901 0.7288 0.063 Uiso 1 1 calc R . . H27C H 0.7703 -0.2570 0.7747 0.063 Uiso 1 1 calc R . . C28 C 0.7809(5) -0.0766(6) 1.1057(9) 0.035(3) Uani 1 1 d . . . H28A H 0.8171 -0.0898 1.1513 0.042 Uiso 1 1 calc R . . H28B H 0.7461 -0.0936 1.1259 0.042 Uiso 1 1 calc R . . C29 C 0.7775(6) -0.0010(6) 1.1080(9) 0.038(3) Uani 1 1 d . . . C30 C 0.8187(5) 0.0353(6) 1.1743(8) 0.033(3) Uani 1 1 d . . . C31 C 0.8114(5) 0.1028(6) 1.1776(8) 0.031(3) Uani 1 1 d . . . C32 C 0.7678(5) 0.1358(6) 1.1116(9) 0.038(3) Uani 1 1 d . . . C33 C 0.7292(5) 0.1005(6) 1.0467(8) 0.033(3) Uani 1 1 d . . . C34 C 0.7330(5) 0.0312(6) 1.0464(8) 0.035(3) Uani 1 1 d . . . C35 C 0.8680(5) 0.0026(6) 1.2442(9) 0.041(3) Uani 1 1 d . . . H35A H 0.9034 0.0304 1.2577 0.062 Uiso 1 1 calc R . . H35B H 0.8780 -0.0391 1.2208 0.062 Uiso 1 1 calc R . . H35C H 0.8542 -0.0047 1.2992 0.062 Uiso 1 1 calc R . . C36 C 0.8520(5) 0.1390(6) 1.2542(8) 0.036(3) Uani 1 1 d . . . H36A H 0.8305 0.1773 1.2697 0.043 Uiso 1 1 calc R . . H36B H 0.8619 0.1104 1.3076 0.043 Uiso 1 1 calc R . . N5 N 0.9086(4) 0.1608(5) 1.2314(7) 0.036(2) Uani 1 1 d . . . C37 C 0.9623(5) 0.1719(6) 1.2914(9) 0.034(3) Uani 1 1 d . . . H37 H 0.9722 0.1627 1.3539 0.041 Uiso 1 1 calc R . . C38 C 0.9980(5) 0.1983(6) 1.2434(9) 0.036(3) Uani 1 1 d . . . H38 H 1.0385 0.2103 1.2672 0.043 Uiso 1 1 calc R . . N6 N 0.9683(4) 0.2054(5) 1.1559(7) 0.033(2) Uani 1 1 d . . . C39 C 0.9127(5) 0.1808(6) 1.1507(8) 0.032(3) Uani 1 1 d . . . H39 H 0.8817 0.1784 1.0974 0.039 Uiso 1 1 calc R . . C40 C 0.7625(6) 0.2089(6) 1.1152(9) 0.041(3) Uani 1 1 d . . . H40A H 0.7572 0.2268 1.0545 0.062 Uiso 1 1 calc R . . H40B H 0.7989 0.2268 1.1543 0.062 Uiso 1 1 calc R . . H40C H 0.7280 0.2204 1.1390 0.062 Uiso 1 1 calc R . . C41 C 0.6862(5) -0.0071(6) 0.9798(9) 0.043(3) Uani 1 1 d . . . H41A H 0.6475 0.0147 0.9709 0.065 Uiso 1 1 calc R . . H41B H 0.6833 -0.0509 1.0033 0.065 Uiso 1 1 calc R . . H41C H 0.6977 -0.0098 0.9223 0.065 Uiso 1 1 calc R . . C42 C 0.6828(5) 0.1337(6) 0.9771(9) 0.039(3) Uani 1 1 d . . . H42A H 0.6913 0.1808 0.9833 0.047 Uiso 1 1 calc R . . H42B H 0.6442 0.1268 0.9933 0.047 Uiso 1 1 calc R . . C43 C 0.6726(6) 0.1171(6) 0.8751(9) 0.039(3) Uani 1 1 d . . . C44 C 0.6171(5) 0.1062(6) 0.8227(9) 0.034(3) Uani 1 1 d . . . C45 C 0.6086(6) 0.1003(6) 0.7315(10) 0.041(3) Uani 1 1 d . . . C46 C 0.6566(6) 0.0981(6) 0.6921(8) 0.043(4) Uani 1 1 d . . . C47 C 0.7150(5) 0.1069(6) 0.7459(9) 0.039(3) Uani 1 1 d . . . C48 C 0.7233(5) 0.1196(6) 0.8378(9) 0.034(3) Uani 1 1 d . . . C49 C 0.5626(5) 0.1016(7) 0.8637(10) 0.048(4) Uani 1 1 d . . . H49A H 0.5460 0.1450 0.8673 0.072 Uiso 1 1 calc R . . H49B H 0.5747 0.0829 0.9241 0.072 Uiso 1 1 calc R . . H49C H 0.5322 0.0739 0.8258 0.072 Uiso 1 1 calc R . . C50 C 0.5451(6) 0.0954(7) 0.6713(11) 0.052(4) Uani 1 1 d . . . H50A H 0.5171 0.1182 0.7006 0.062 Uiso 1 1 calc R . . H50B H 0.5439 0.1174 0.6134 0.062 Uiso 1 1 calc R . . N7 N 0.5251(4) 0.0270(5) 0.6534(7) 0.042(3) Uani 1 1 d . . . C51 C 0.4675(7) 0.0048(10) 0.6346(13) 0.083(6) Uani 1 1 d . . . H51 H 0.4327 0.0294 0.6344 0.100 Uiso 1 1 calc R . . C52 C 0.4701(8) -0.0592(9) 0.6166(13) 0.076(5) Uani 1 1 d . . . H52 H 0.4365 -0.0872 0.6027 0.091 Uiso 1 1 calc R . . N8 N 0.5265(5) -0.0777(5) 0.6208(9) 0.052(3) Uani 1 1 d . . . C53 C 0.5590(6) -0.0256(6) 0.6447(11) 0.049(4) Uani 1 1 d . . . H53 H 0.6013 -0.0246 0.6547 0.059 Uiso 1 1 calc R . . C54 C 0.6470(6) 0.0916(8) 0.5882(9) 0.054(4) Uani 1 1 d . . . H54A H 0.6052 0.0806 0.5615 0.080 Uiso 1 1 calc R . . H54B H 0.6729 0.0573 0.5746 0.080 Uiso 1 1 calc R . . H54C H 0.6568 0.1328 0.5632 0.080 Uiso 1 1 calc R . . C55 C 0.7840(5) 0.1384(6) 0.8919(9) 0.039(3) Uani 1 1 d . . . H55A H 0.7802 0.1595 0.9477 0.059 Uiso 1 1 calc R . . H55B H 0.8025 0.1685 0.8571 0.059 Uiso 1 1 calc R . . H55C H 0.8089 0.0995 0.9064 0.059 Uiso 1 1 calc R . . C56 C 0.7682(5) 0.1075(6) 0.7016(8) 0.038(3) Uani 1 1 d . . . H56A H 0.7533 0.0928 0.6387 0.045 Uiso 1 1 calc R . . H56B H 0.7811 0.1531 0.6993 0.045 Uiso 1 1 calc R . . C57 C 0.4798(13) 0.3921(13) 0.579(2) 0.054(8) Uani 0.50 1 d P . . H57 H 0.4937 0.3461 0.5872 0.064 Uiso 0.50 1 calc PR . . Cl1 Cl 0.5443(5) 0.4420(5) 0.6024(7) 0.094(3) Uani 0.50 1 d P . . Cl2 Cl 0.4379(4) 0.4047(5) 0.6488(6) 0.078(3) Uani 0.50 1 d P . . Cl3 Cl 0.4452(3) 0.4025(5) 0.4667(6) 0.081(3) Uani 0.50 1 d P . . C58 C 0.3451(6) 0.7788(11) 0.7034(10) 0.111(9) Uani 1 1 d D . . H58 H 0.3439 0.7323 0.7209 0.133 Uiso 1 1 calc R . . Cl4 Cl 0.3714(3) 0.8173(7) 0.7971(5) 0.252(7) Uani 1 1 d D . . Cl5 Cl 0.3917(2) 0.7809(3) 0.6301(4) 0.0849(15) Uani 1 1 d D . . Cl6 Cl 0.27201(19) 0.7979(2) 0.6489(4) 0.0848(15) Uani 1 1 d D . . C59 C 0.7050(9) 0.5537(10) 0.846(2) 0.150 Uani 0.50 1 d PD . . H59 H 0.6927 0.5727 0.8987 0.180 Uiso 0.50 1 calc PR . . Cl7 Cl 0.7744(3) 0.5849(4) 0.8456(6) 0.060(2) Uani 0.50 1 d PD . . Cl8 Cl 0.6521(4) 0.5777(6) 0.7498(7) 0.100(4) Uani 0.50 1 d PD . . Cl9 Cl 0.7050(6) 0.4705(5) 0.8578(13) 0.153(7) Uani 0.50 1 d PD . . C60 C 0.9143(9) 0.5357(9) 0.0291(16) 0.113(3) Uani 0.50 1 d PD . . H60 H 0.9172 0.5566 -0.0286 0.135 Uiso 0.50 1 calc PR . . Cl10 Cl 0.9837(6) 0.5272(5) 0.1044(6) 0.113(3) Uani 0.50 1 d PD . . Cl11 Cl 0.8834(6) 0.5857(5) 0.0941(6) 0.113(3) Uani 0.50 1 d PD . . Cl12 Cl 0.8769(6) 0.4606(5) 0.0123(6) 0.113(3) Uani 0.50 1 d PD . . 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 0.0407(8) 0.0343(9) 0.0297(8) -0.0011(6) 0.0122(6) -0.0002(6) Br1 0.0517(8) 0.0366(8) 0.0440(8) -0.0062(6) 0.0185(6) -0.0089(6) Br2 0.0470(8) 0.0691(11) 0.0351(8) 0.0147(7) 0.0112(6) 0.0099(7) Zn2 0.0731(12) 0.0386(10) 0.0385(10) -0.0042(8) 0.0056(8) -0.0014(8) Br3 0.0790(11) 0.0474(10) 0.0551(10) -0.0039(7) 0.0270(8) 0.0074(8) Br4 0.0781(11) 0.0550(11) 0.0555(11) -0.0073(8) 0.0042(8) -0.0075(8) C1 0.040(7) 0.022(7) 0.025(7) 0.000(5) 0.000(5) 0.005(5) C2 0.041(7) 0.022(7) 0.040(8) 0.003(5) 0.017(6) -0.005(5) C3 0.035(6) 0.031(7) 0.028(7) -0.009(5) 0.008(5) -0.007(5) C4 0.028(6) 0.035(7) 0.022(6) -0.004(5) 0.012(5) -0.006(5) C5 0.044(7) 0.036(8) 0.022(7) -0.002(5) 0.010(5) 0.002(6) C6 0.037(6) 0.023(7) 0.030(7) -0.007(5) 0.016(5) -0.005(5) C7 0.048(8) 0.036(8) 0.060(10) 0.004(7) 0.020(7) -0.008(6) C8 0.048(7) 0.029(7) 0.028(7) -0.007(5) 0.019(6) -0.009(5) N1 0.034(5) 0.033(6) 0.035(6) -0.001(5) 0.013(5) 0.005(4) C9 0.040(7) 0.025(7) 0.031(7) -0.009(5) 0.018(5) -0.007(5) N2 0.047(6) 0.029(6) 0.041(7) -0.001(5) 0.018(5) -0.005(5) C10 0.044(7) 0.029(7) 0.032(7) 0.004(6) 0.008(6) 0.002(6) C11 0.032(6) 0.027(7) 0.039(8) 0.002(6) 0.013(5) 0.002(5) C12 0.037(7) 0.040(8) 0.044(8) 0.007(6) 0.011(6) 0.000(6) C13 0.029(6) 0.042(8) 0.039(8) 0.007(6) -0.002(5) -0.004(5) C14 0.040(7) 0.021(7) 0.030(7) -0.004(5) 0.009(5) 0.005(5) C15 0.037(7) 0.026(7) 0.035(7) -0.002(6) 0.005(5) 0.012(5) C16 0.028(6) 0.025(7) 0.030(7) -0.002(5) 0.007(5) -0.007(5) C17 0.040(7) 0.020(7) 0.032(7) -0.001(5) -0.001(5) 0.000(5) C18 0.039(7) 0.034(8) 0.037(8) 0.001(6) 0.010(6) -0.006(6) C19 0.047(7) 0.034(7) 0.019(6) 0.011(5) 0.013(5) -0.005(6) C20 0.051(8) 0.026(7) 0.038(8) -0.005(6) 0.002(6) 0.009(6) C21 0.044(7) 0.038(8) 0.021(7) 0.007(5) 0.008(5) 0.004(6) C22 0.066(9) 0.033(8) 0.052(9) -0.003(7) 0.030(8) -0.014(7) C23 0.055(8) 0.034(8) 0.047(9) 0.004(6) 0.012(7) -0.005(6) N3 0.063(7) 0.042(7) 0.034(7) 0.002(5) 0.000(6) -0.023(6) C24 0.093(14) 0.111(17) 0.106(17) 0.074(14) -0.037(13) -0.062(13) C25 0.085(14) 0.14(2) 0.095(17) 0.065(16) -0.024(13) -0.033(14) N4 0.064(8) 0.054(8) 0.045(8) 0.010(6) 0.013(6) -0.019(6) C26 0.060(9) 0.032(8) 0.039(8) 0.010(6) 0.014(7) -0.007(6) C27 0.061(8) 0.026(7) 0.040(8) -0.007(6) 0.016(7) -0.005(6) C28 0.042(7) 0.031(8) 0.035(7) -0.002(6) 0.015(6) -0.009(5) C29 0.047(7) 0.038(8) 0.033(7) -0.006(6) 0.017(6) -0.003(6) C30 0.041(7) 0.034(8) 0.022(7) -0.003(5) 0.003(5) -0.003(5) C31 0.042(7) 0.028(7) 0.027(7) -0.006(5) 0.015(5) -0.005(5) C32 0.039(7) 0.036(8) 0.045(8) -0.007(6) 0.022(6) -0.008(6) C33 0.041(7) 0.033(8) 0.027(7) 0.002(5) 0.013(5) -0.004(5) C34 0.033(6) 0.040(8) 0.033(7) -0.006(6) 0.012(5) -0.001(5) C35 0.043(7) 0.037(8) 0.047(9) -0.008(6) 0.018(6) 0.001(6) C36 0.044(7) 0.040(8) 0.027(7) -0.006(6) 0.016(6) -0.017(6) N5 0.043(6) 0.034(6) 0.033(6) -0.011(5) 0.016(5) -0.010(5) C37 0.033(6) 0.034(7) 0.035(7) 0.007(6) 0.005(6) 0.000(5) C38 0.031(6) 0.044(8) 0.034(8) -0.010(6) 0.009(6) -0.001(6) N6 0.039(6) 0.027(6) 0.036(6) -0.004(5) 0.014(5) 0.009(4) C39 0.037(7) 0.034(8) 0.027(7) 0.006(5) 0.010(5) 0.007(5) C40 0.047(7) 0.042(9) 0.037(8) -0.015(6) 0.016(6) -0.001(6) C41 0.038(7) 0.038(8) 0.047(9) -0.005(6) -0.004(6) -0.009(6) C42 0.041(7) 0.032(8) 0.045(8) -0.007(6) 0.012(6) -0.001(6) C43 0.044(7) 0.032(8) 0.040(8) -0.007(6) 0.007(6) 0.013(6) C44 0.041(7) 0.018(7) 0.043(8) -0.007(5) 0.011(6) -0.001(5) C45 0.043(7) 0.022(7) 0.054(10) -0.009(6) 0.004(7) 0.001(6) C46 0.067(9) 0.028(7) 0.024(7) -0.007(6) -0.009(7) 0.005(6) C47 0.041(7) 0.023(7) 0.050(9) 0.006(6) 0.004(6) 0.010(5) C48 0.033(6) 0.029(7) 0.038(8) 0.000(6) 0.003(6) 0.006(5) C49 0.041(7) 0.040(9) 0.059(10) -0.008(7) 0.005(7) -0.001(6) C50 0.052(8) 0.034(8) 0.063(10) 0.002(7) 0.004(7) 0.009(7) N7 0.037(6) 0.049(8) 0.041(7) -0.011(5) 0.009(5) -0.006(5) C51 0.043(9) 0.096(16) 0.099(16) -0.035(12) -0.004(9) 0.004(9) C52 0.067(12) 0.069(13) 0.081(14) -0.012(10) -0.006(10) -0.008(9) N8 0.050(7) 0.036(7) 0.069(9) -0.009(6) 0.013(6) -0.005(6) C53 0.045(8) 0.029(8) 0.076(11) -0.015(7) 0.021(7) -0.006(6) C54 0.061(9) 0.062(10) 0.029(8) 0.000(7) -0.006(7) 0.013(7) C55 0.041(7) 0.041(8) 0.035(8) -0.005(6) 0.010(6) -0.014(6) C56 0.045(7) 0.045(8) 0.022(7) 0.006(6) 0.007(6) 0.006(6) C57 0.08(2) 0.027(16) 0.049(19) 0.016(13) -0.002(15) 0.018(14) Cl1 0.114(8) 0.088(7) 0.079(7) -0.028(6) 0.022(6) -0.022(6) Cl2 0.101(7) 0.083(7) 0.058(6) 0.012(5) 0.036(5) 0.009(5) Cl3 0.049(4) 0.153(9) 0.052(5) 0.034(5) 0.033(4) 0.041(5) C58 0.051(11) 0.17(2) 0.12(2) -0.060(17) 0.035(12) -0.005(12) Cl4 0.096(5) 0.57(2) 0.092(6) -0.062(9) 0.030(4) -0.103(9) Cl5 0.068(3) 0.093(4) 0.101(4) -0.010(3) 0.033(3) -0.014(2) Cl6 0.056(2) 0.093(4) 0.107(4) -0.004(3) 0.022(3) 0.003(2) C59 0.147 0.028 0.250 0.000 0.000 0.000 Cl7 0.069(5) 0.037(4) 0.089(6) 0.008(4) 0.045(4) 0.023(3) Cl8 0.076(6) 0.160(11) 0.067(7) 0.036(7) 0.022(5) -0.009(6) Cl9 0.144(10) 0.027(5) 0.260(19) -0.005(8) -0.006(11) -0.011(6) C60 0.219(7) 0.074(4) 0.039(3) 0.003(3) 0.018(4) -0.069(4) Cl10 0.219(7) 0.074(4) 0.039(3) 0.003(3) 0.018(4) -0.069(4) Cl11 0.219(7) 0.074(4) 0.039(3) 0.003(3) 0.018(4) -0.069(4) Cl12 0.219(7) 0.074(4) 0.039(3) 0.003(3) 0.018(4) -0.069(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 Zn1 N6 2.002(11) . ? Zn1 N2 2.016(11) . ? Zn1 Br1 2.3846(19) . ? Zn1 Br2 2.3959(19) . ? Zn2 N8 2.006(12) . ? Zn2 N4 2.007(12) . ? Zn2 Br4 2.358(2) . ? Zn2 Br3 2.424(3) . ? C1 C2 1.395(16) . ? C1 C6 1.423(16) . ? C1 C56 1.536(15) . ? C2 C3 1.392(16) . ? C2 C7 1.497(17) . ? C3 C4 1.394(17) . ? C3 C8 1.535(16) . ? C4 C5 1.402(16) . ? C4 C12 1.494(16) . ? C5 C6 1.396(16) . ? C5 C14 1.488(17) . ? C6 C13 1.529(15) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 N1 1.497(15) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? N1 C9 1.329(15) . ? N1 C11 1.381(15) . ? C9 N2 1.302(15) . ? C9 H9 0.9500 . ? N2 C10 1.373(16) . ? C10 C11 1.362(17) . ? 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 1.504(17) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.407(17) . ? C15 C20 1.457(17) . ? C16 C17 1.398(17) . ? C16 C21 1.502(15) . ? C17 C18 1.415(16) . ? C17 C28 1.475(17) . ? C18 C19 1.408(17) . ? C18 C22 1.526(17) . ? C19 C20 1.372(18) . ? C19 C23 1.504(17) . ? C20 C27 1.530(18) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9300 . ? C22 H22B 0.9300 . ? C22 H22C 0.9300 . ? C23 N3 1.479(16) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? N3 C26 1.312(16) . ? N3 C24 1.38(2) . ? C24 C25 1.36(2) . ? C24 H24 0.9500 . ? C25 N4 1.41(2) . ? C25 H25 0.9500 . ? N4 C26 1.303(17) . ? C26 H26 0.9500 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.561(17) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C34 1.388(17) . ? C29 C30 1.426(17) . ? C30 C31 1.406(17) . ? C30 C35 1.520(17) . ? C31 C32 1.418(17) . ? C31 C36 1.511(16) . ? C32 C33 1.374(17) . ? C32 C40 1.513(17) . ? C33 C34 1.431(17) . ? C33 C42 1.487(17) . ? C34 C41 1.517(16) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 N5 1.498(15) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? N5 C39 1.329(15) . ? N5 C37 1.374(15) . ? C37 C38 1.343(17) . ? C37 H37 0.9500 . ? C38 N6 1.360(15) . ? C38 H38 0.9500 . ? N6 C39 1.361(15) . ? C39 H39 0.9500 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C43 1.561(18) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.359(16) . ? C43 C48 1.419(18) . ? C44 C45 1.370(19) . ? C44 C49 1.535(18) . ? C45 C46 1.38(2) . ? C45 C50 1.536(17) . ? C46 C47 1.412(17) . ? C46 C54 1.560(18) . ? C47 C48 1.399(19) . ? C47 C56 1.536(18) . ? C48 C55 1.497(16) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 N7 1.490(17) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? N7 C53 1.361(17) . ? N7 C51 1.369(19) . ? C51 C52 1.35(2) . ? C51 H51 0.9500 . ? C52 N8 1.34(2) . ? C52 H52 0.9500 . ? N8 C53 1.311(16) . ? C53 H53 0.9500 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 Cl2 1.62(3) . ? C57 Cl3 1.73(3) . ? C57 Cl1 1.77(3) . ? C57 H57 1.0000 . ? C58 Cl4 1.626(14) . ? C58 Cl5 1.729(14) . ? C58 Cl6 1.738(14) . ? C58 H58 1.0000 . ? C59 Cl7 1.725(19) . ? C59 Cl9 1.726(18) . ? C59 Cl8 1.743(19) . ? C59 H59 1.0000 . ? C60 Cl11 1.702(19) . ? C60 Cl10 1.744(18) . ? C60 Cl12 1.762(18) . ? C60 H60 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 N6 Zn1 N2 110.7(4) . . ? N6 Zn1 Br1 109.4(3) . . ? N2 Zn1 Br1 106.6(3) . . ? N6 Zn1 Br2 101.7(3) . . ? N2 Zn1 Br2 104.8(3) . . ? Br1 Zn1 Br2 123.44(8) . . ? N8 Zn2 N4 108.2(5) . . ? N8 Zn2 Br4 111.9(3) . . ? N4 Zn2 Br4 108.6(3) . . ? N8 Zn2 Br3 102.4(4) . . ? N4 Zn2 Br3 106.2(4) . . ? Br4 Zn2 Br3 118.90(9) . . ? C2 C1 C6 119.4(10) . . ? C2 C1 C56 118.1(10) . . ? C6 C1 C56 122.5(10) . . ? C3 C2 C1 119.5(10) . . ? C3 C2 C7 120.1(11) . . ? C1 C2 C7 120.4(11) . . ? C2 C3 C4 120.5(10) . . ? C2 C3 C8 119.1(11) . . ? C4 C3 C8 120.0(10) . . ? C3 C4 C5 121.3(10) . . ? C3 C4 C12 118.9(10) . . ? C5 C4 C12 119.7(11) . . ? C6 C5 C4 117.8(11) . . ? C6 C5 C14 120.7(11) . . ? C4 C5 C14 121.4(11) . . ? C5 C6 C1 121.2(10) . . ? C5 C6 C13 120.1(10) . . ? C1 C6 C13 118.4(10) . . ? 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 111.4(9) . . ? 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 C11 107.7(10) . . ? C9 N1 C8 127.8(10) . . ? C11 N1 C8 124.5(10) . . ? N2 C9 N1 111.0(10) . . ? N2 C9 H9 124.5 . . ? N1 C9 H9 124.5 . . ? C9 N2 C10 107.2(11) . . ? C9 N2 Zn1 123.6(8) . . ? C10 N2 Zn1 127.6(8) . . ? C11 C10 N2 108.3(11) . . ? C11 C10 H10 125.8 . . ? N2 C10 H10 125.8 . . ? C10 C11 N1 105.7(11) . . ? C10 C11 H11 127.1 . . ? N1 C11 H11 127.1 . . ? 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(10) . . ? 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 . . ? C16 C15 C20 117.5(12) . . ? C16 C15 C14 122.3(11) . . ? C20 C15 C14 119.9(11) . . ? C17 C16 C15 121.9(10) . . ? C17 C16 C21 120.1(11) . . ? C15 C16 C21 117.7(10) . . ? C16 C17 C18 118.8(11) . . ? C16 C17 C28 121.2(10) . . ? C18 C17 C28 120.0(12) . . ? C19 C18 C17 120.6(12) . . ? C19 C18 C22 119.0(11) . . ? C17 C18 C22 120.4(12) . . ? C20 C19 C18 120.4(11) . . ? C20 C19 C23 120.2(12) . . ? C18 C19 C23 119.5(11) . . ? C19 C20 C15 120.5(12) . . ? C19 C20 C27 122.8(12) . . ? C15 C20 C27 116.6(12) . . ? 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 . . ? N3 C23 C19 112.5(11) . . ? N3 C23 H23A 109.1 . . ? C19 C23 H23A 109.1 . . ? N3 C23 H23B 109.1 . . ? C19 C23 H23B 109.1 . . ? H23A C23 H23B 107.8 . . ? C26 N3 C24 106.7(12) . . ? C26 N3 C23 127.4(12) . . ? C24 N3 C23 125.9(12) . . ? C25 C24 N3 108.5(16) . . ? C25 C24 H24 125.8 . . ? N3 C24 H24 125.8 . . ? C24 C25 N4 105.2(16) . . ? C24 C25 H25 127.4 . . ? N4 C25 H25 127.4 . . ? C26 N4 C25 107.5(13) . . ? C26 N4 Zn2 125.3(10) . . ? C25 N4 Zn2 127.1(11) . . ? N4 C26 N3 111.8(12) . . ? N4 C26 H26 124.1 . . ? N3 C26 H26 124.1 . . ? C20 C27 H27A 109.5 . . ? C20 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C20 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C17 C28 C29 120.0(11) . . ? C17 C28 H28A 107.3 . . ? C29 C28 H28A 107.3 . . ? C17 C28 H28B 107.3 . . ? C29 C28 H28B 107.3 . . ? H28A C28 H28B 106.9 . . ? C34 C29 C30 119.4(12) . . ? C34 C29 C28 119.7(11) . . ? C30 C29 C28 120.8(11) . . ? C31 C30 C29 118.7(11) . . ? C31 C30 C35 119.4(10) . . ? C29 C30 C35 121.8(11) . . ? C30 C31 C32 121.4(11) . . ? C30 C31 C36 117.3(11) . . ? C32 C31 C36 121.3(11) . . ? C33 C32 C31 119.2(12) . . ? C33 C32 C40 120.7(12) . . ? C31 C32 C40 120.1(11) . . ? C32 C33 C34 120.2(11) . . ? C32 C33 C42 120.4(12) . . ? C34 C33 C42 119.4(11) . . ? C29 C34 C33 120.8(11) . . ? C29 C34 C41 120.0(12) . . ? C33 C34 C41 119.2(11) . . ? C30 C35 H35A 109.5 . . ? C30 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C30 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N5 C36 C31 112.3(10) . . ? N5 C36 H36A 109.1 . . ? C31 C36 H36A 109.1 . . ? N5 C36 H36B 109.1 . . ? C31 C36 H36B 109.1 . . ? H36A C36 H36B 107.9 . . ? C39 N5 C37 108.5(10) . . ? C39 N5 C36 124.7(10) . . ? C37 N5 C36 126.2(10) . . ? C38 C37 N5 105.9(11) . . ? C38 C37 H37 127.0 . . ? N5 C37 H37 127.0 . . ? C37 C38 N6 110.6(11) . . ? C37 C38 H38 124.7 . . ? N6 C38 H38 124.7 . . ? C38 N6 C39 105.4(10) . . ? C38 N6 Zn1 130.8(8) . . ? C39 N6 Zn1 122.3(8) . . ? N5 C39 N6 109.6(10) . . ? N5 C39 H39 125.2 . . ? N6 C39 H39 125.2 . . ? C32 C40 H40A 109.5 . . ? C32 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C32 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C34 C41 H41A 109.5 . . ? C34 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C34 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C33 C42 C43 121.8(11) . . ? C33 C42 H42A 106.9 . . ? C43 C42 H42A 106.9 . . ? C33 C42 H42B 106.9 . . ? C43 C42 H42B 106.9 . . ? H42A C42 H42B 106.7 . . ? C44 C43 C48 121.2(12) . . ? C44 C43 C42 121.5(12) . . ? C48 C43 C42 117.0(11) . . ? C43 C44 C45 120.2(12) . . ? C43 C44 C49 121.1(12) . . ? C45 C44 C49 118.7(11) . . ? C44 C45 C46 120.9(11) . . ? C44 C45 C50 120.2(13) . . ? C46 C45 C50 118.9(13) . . ? C45 C46 C47 119.5(12) . . ? C45 C46 C54 120.9(12) . . ? C47 C46 C54 119.4(14) . . ? C48 C47 C46 119.6(13) . . ? C48 C47 C56 120.7(11) . . ? C46 C47 C56 119.5(12) . . ? C47 C48 C43 118.1(11) . . ? C47 C48 C55 119.5(12) . . ? C43 C48 C55 122.4(12) . . ? C44 C49 H49A 109.5 . . ? C44 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C44 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? N7 C50 C45 112.4(10) . . ? N7 C50 H50A 109.1 . . ? C45 C50 H50A 109.1 . . ? N7 C50 H50B 109.1 . . ? C45 C50 H50B 109.1 . . ? H50A C50 H50B 107.9 . . ? C53 N7 C51 105.3(12) . . ? C53 N7 C50 127.8(11) . . ? C51 N7 C50 126.6(13) . . ? C52 C51 N7 106.3(15) . . ? C52 C51 H51 126.8 . . ? N7 C51 H51 126.8 . . ? N8 C52 C51 111.0(15) . . ? N8 C52 H52 124.5 . . ? C51 C52 H52 124.5 . . ? C53 N8 C52 105.2(13) . . ? C53 N8 Zn2 122.4(10) . . ? C52 N8 Zn2 132.2(11) . . ? N8 C53 N7 112.2(12) . . ? N8 C53 H53 123.9 . . ? N7 C53 H53 123.9 . . ? C46 C54 H54A 109.5 . . ? C46 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C46 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C48 C55 H55A 109.5 . . ? C48 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C48 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C1 C56 C47 119.0(10) . . ? C1 C56 H56A 107.6 . . ? C47 C56 H56A 107.6 . . ? C1 C56 H56B 107.6 . . ? C47 C56 H56B 107.6 . . ? H56A C56 H56B 107.0 . . ? Cl2 C57 Cl3 115.5(16) . . ? Cl2 C57 Cl1 112.2(18) . . ? Cl3 C57 Cl1 107.0(17) . . ? Cl2 C57 H57 107.3 . . ? Cl3 C57 H57 107.3 . . ? Cl1 C57 H57 107.3 . . ? Cl4 C58 Cl5 113.8(10) . . ? Cl4 C58 Cl6 115.3(10) . . ? Cl5 C58 Cl6 111.4(10) . . ? Cl4 C58 H58 105.1 . . ? Cl5 C58 H58 105.1 . . ? Cl6 C58 H58 105.1 . . ? Cl7 C59 Cl9 113.2(14) . . ? Cl7 C59 Cl8 110.8(14) . . ? Cl9 C59 Cl8 110.8(15) . . ? Cl7 C59 H59 107.3 . . ? Cl9 C59 H59 107.3 . . ? Cl8 C59 H59 107.3 . . ? Cl11 C60 Cl10 96.9(13) . . ? Cl11 C60 Cl12 111.1(14) . . ? Cl10 C60 Cl12 110.3(13) . . ? Cl11 C60 H60 112.5 . . ? Cl10 C60 H60 112.5 . . ? Cl12 C60 H60 112.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.27 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.638 _refine_diff_density_min -1.543 _refine_diff_density_rms 0.219 # Attachment '4-ZnCl2.cif' data_4-ZnCl2 _database_code_depnum_ccdc_archive 'CCDC 702200' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H64 Cl4 N8 Zn2' _chemical_formula_sum 'C56 H64 Cl4 N8 Zn2' _chemical_formula_weight 1121.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _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 22.797(2) _cell_length_b 20.070(2) _cell_length_c 15.0139(14) _cell_angle_alpha 90.00 _cell_angle_beta 101.144(4) _cell_angle_gamma 90.00 _cell_volume 6739.7(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6692 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 23.68 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.105 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2336 _exptl_absorpt_coefficient_mu 0.906 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7985 _exptl_absorpt_correction_T_max 0.9229 _exptl_absorpt_process_details sadabs _exptl_special_details ; Owing to large disorder of the solvent present in the cavities of this structure, the SQUEEZ command has been applied. ; _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 98420 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0709 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 27.56 _reflns_number_total 15289 _reflns_number_gt 9176 _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^)+(0.1198P)^2^+26.1214P] 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 15279 _refine_ls_number_parameters 631 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1445 _refine_ls_R_factor_gt 0.0990 _refine_ls_wR_factor_ref 0.2846 _refine_ls_wR_factor_gt 0.2666 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.103 _refine_ls_shift/su_max 0.005 _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 0.98512(3) 0.25801(4) 1.06352(5) 0.0363(2) Uani 1 1 d . . . Cl1 Cl 1.05827(7) 0.32968(9) 1.11659(12) 0.0473(4) Uani 1 1 d . . . Cl2 Cl 0.89394(8) 0.28993(14) 0.98898(13) 0.0684(6) Uani 1 1 d . . . Zn2 Zn 0.56273(4) -0.15327(4) 0.60929(6) 0.0525(3) Uani 1 1 d . . . Cl3 Cl 0.64366(9) -0.11831(10) 0.55733(14) 0.0585(5) Uani 1 1 d . . . Cl4 Cl 0.49142(14) -0.21016(11) 0.5181(2) 0.1072(12) Uani 1 1 d . . . C1 C 0.8696(3) -0.0384(3) 0.8173(4) 0.0290(12) Uani 1 1 d . . . C2 C 0.9255(2) -0.0083(3) 0.8254(4) 0.0289(12) Uani 1 1 d . . . C3 C 0.9296(3) 0.0566(3) 0.7906(4) 0.0286(12) Uani 1 1 d . . . C4 C 0.8781(3) 0.0938(3) 0.7560(4) 0.0295(12) Uani 1 1 d . . . C5 C 0.8217(3) 0.0640(3) 0.7528(4) 0.0281(12) Uani 1 1 d . . . C6 C 0.8174(2) -0.0022(3) 0.7770(4) 0.0300(12) Uani 1 1 d . . . C7 C 0.9827(3) -0.0433(3) 0.8715(5) 0.0402(15) Uani 1 1 d . . . H7A H 0.9739 -0.0725 0.9197 0.060 Uiso 1 1 calc R . . H7B H 1.0125 -0.0101 0.8979 0.060 Uiso 1 1 calc R . . H7C H 0.9983 -0.0700 0.8267 0.060 Uiso 1 1 calc R . . C8 C 0.9900(3) 0.0851(3) 0.7846(4) 0.0333(13) Uani 1 1 d . . . H8A H 1.0192 0.0482 0.7885 0.040 Uiso 1 1 calc R . . H8B H 0.9873 0.1068 0.7247 0.040 Uiso 1 1 calc R . . N1 N 1.0122(2) 0.1340(2) 0.8561(3) 0.0285(10) Uani 1 1 d . . . C9 C 0.9838(2) 0.1550(3) 0.9205(4) 0.0322(13) Uani 1 1 d . . . H9 H 0.9454 0.1399 0.9273 0.039 Uiso 1 1 calc R . . N2 N 1.0161(2) 0.1998(3) 0.9739(3) 0.0357(11) Uani 1 1 d . . . C10 C 1.0677(2) 0.2068(3) 0.9398(4) 0.0324(13) Uani 1 1 d . . . H10 H 1.1002 0.2351 0.9644 0.039 Uiso 1 1 calc R . . C11 C 1.0650(2) 0.1672(3) 0.8657(4) 0.0284(12) Uani 1 1 d . . . H11 H 1.0941 0.1635 0.8283 0.034 Uiso 1 1 calc R . . C12 C 0.8827(3) 0.1637(3) 0.7237(5) 0.0392(15) Uani 1 1 d . . . H12A H 0.8587 0.1685 0.6625 0.059 Uiso 1 1 calc R . . H12B H 0.9246 0.1740 0.7226 0.059 Uiso 1 1 calc R . . H12C H 0.8679 0.1945 0.7650 0.059 Uiso 1 1 calc R . . C13 C 0.7563(3) -0.0374(3) 0.7586(5) 0.0381(14) Uani 1 1 d . . . H13A H 0.7386 -0.0353 0.8131 0.057 Uiso 1 1 calc R . . H13B H 0.7616 -0.0841 0.7428 0.057 Uiso 1 1 calc R . . H13C H 0.7297 -0.0153 0.7082 0.057 Uiso 1 1 calc R . . C14 C 0.7659(3) 0.1038(3) 0.7124(4) 0.0359(14) Uani 1 1 d . . . H14A H 0.7791 0.1496 0.7021 0.043 Uiso 1 1 calc R . . H14B H 0.7499 0.0845 0.6519 0.043 Uiso 1 1 calc R . . C15 C 0.7141(2) 0.1098(3) 0.7612(4) 0.0315(13) Uani 1 1 d . . . C16 C 0.6555(3) 0.1056(3) 0.7095(4) 0.0363(14) Uani 1 1 d . . . C17 C 0.6064(3) 0.1100(3) 0.7547(5) 0.0387(15) Uani 1 1 d . . . C18 C 0.6144(3) 0.1155(3) 0.8494(5) 0.0433(16) Uani 1 1 d . . . C19 C 0.6734(3) 0.1249(3) 0.8983(5) 0.0377(14) Uani 1 1 d . . . C20 C 0.7214(3) 0.1234(3) 0.8553(5) 0.0405(16) Uani 1 1 d . . . C21 C 0.6442(3) 0.0969(4) 0.6097(4) 0.0506(18) Uani 1 1 d . . . H21A H 0.6010 0.0960 0.5861 0.076 Uiso 1 1 calc R . . H21B H 0.6621 0.0549 0.5948 0.076 Uiso 1 1 calc R . . H21C H 0.6621 0.1341 0.5821 0.076 Uiso 1 1 calc R . . C22 C 0.5431(3) 0.1082(3) 0.6977(5) 0.0430(16) Uani 1 1 d . . . H22A H 0.5148 0.1266 0.7339 0.052 Uiso 1 1 calc R . . H22B H 0.5414 0.1369 0.6437 0.052 Uiso 1 1 calc R . . N3 N 0.5241(2) 0.0400(3) 0.6680(4) 0.0358(12) Uani 1 1 d . . . C23 C 0.5553(3) -0.0162(3) 0.6797(5) 0.0401(15) Uani 1 1 d . . . H23 H 0.5950 -0.0190 0.7136 0.048 Uiso 1 1 calc R . . N4 N 0.5256(2) -0.0673(3) 0.6397(4) 0.0450(14) Uani 1 1 d . . . C24 C 0.4715(3) -0.0415(4) 0.6016(5) 0.0495(18) Uani 1 1 d . . . H24 H 0.4392 -0.0668 0.5690 0.059 Uiso 1 1 calc R . . C25 C 0.4695(3) 0.0235(4) 0.6156(5) 0.0464(17) Uani 1 1 d . . . H25 H 0.4371 0.0527 0.5940 0.056 Uiso 1 1 calc R . . C26 C 0.5617(3) 0.1157(4) 0.8966(5) 0.0538(19) Uani 1 1 d . . . H26A H 0.5721 0.0913 0.9540 0.081 Uiso 1 1 calc R . . H26B H 0.5275 0.0942 0.8577 0.081 Uiso 1 1 calc R . . H26C H 0.5513 0.1617 0.9087 0.081 Uiso 1 1 calc R . . C27 C 0.7848(3) 0.1417(3) 0.9060(5) 0.0412(15) Uani 1 1 d . . . H27A H 0.7826 0.1801 0.9455 0.062 Uiso 1 1 calc R . . H27B H 0.8099 0.1529 0.8619 0.062 Uiso 1 1 calc R . . H27C H 0.8023 0.1037 0.9428 0.062 Uiso 1 1 calc R . . C28 C 0.6827(3) 0.1426(3) 0.9984(5) 0.0469(17) Uani 1 1 d . . . H28A H 0.6434 0.1394 1.0169 0.056 Uiso 1 1 calc R . . H28B H 0.6951 0.1899 1.0047 0.056 Uiso 1 1 calc R . . C29 C 0.7277(3) 0.1021(3) 1.0667(5) 0.0358(14) Uani 1 1 d . . . C30 C 0.7652(3) 0.1370(3) 1.1395(5) 0.0408(15) Uani 1 1 d . . . C31 C 0.8073(3) 0.1010(3) 1.2009(5) 0.0409(15) Uani 1 1 d . . . C32 C 0.8124(3) 0.0321(3) 1.1929(4) 0.0338(13) Uani 1 1 d . . . C33 C 0.7721(2) -0.0036(3) 1.1264(4) 0.0316(13) Uani 1 1 d . . . C34 C 0.7292(3) 0.0324(3) 1.0648(4) 0.0373(14) Uani 1 1 d . . . C35 C 0.7597(3) 0.2118(4) 1.1458(6) 0.060(2) Uani 1 1 d . . . H35A H 0.7914 0.2288 1.1939 0.090 Uiso 1 1 calc R . . H35B H 0.7206 0.2231 1.1599 0.090 Uiso 1 1 calc R . . H35C H 0.7634 0.2320 1.0877 0.090 Uiso 1 1 calc R . . C36 C 0.8490(3) 0.1364(4) 1.2788(5) 0.0483(18) Uani 1 1 d . . . H36A H 0.8283 0.1754 1.2986 0.058 Uiso 1 1 calc R . . H36B H 0.8595 0.1056 1.3310 0.058 Uiso 1 1 calc R . . N5 N 0.9048(2) 0.1587(3) 1.2488(4) 0.0372(12) Uani 1 1 d . . . C37 C 0.9097(3) 0.1807(3) 1.1662(5) 0.0365(14) Uani 1 1 d . . . H37 H 0.8780 0.1802 1.1148 0.044 Uiso 1 1 calc R . . N6 N 0.9640(2) 0.2030(3) 1.1653(4) 0.0346(11) Uani 1 1 d . . . C38 C 0.9953(3) 0.1951(3) 1.2524(5) 0.0389(15) Uani 1 1 d . . . H38 H 1.0361 0.2067 1.2730 0.047 Uiso 1 1 calc R . . C39 C 0.9592(3) 0.1684(3) 1.3044(5) 0.0398(15) Uani 1 1 d . . . H39 H 0.9695 0.1583 1.3673 0.048 Uiso 1 1 calc R . . C40 C 0.8619(3) -0.0054(4) 1.2593(5) 0.0462(16) Uani 1 1 d . . . H40A H 0.8472 -0.0169 1.3146 0.069 Uiso 1 1 calc R . . H40B H 0.8973 0.0232 1.2750 0.069 Uiso 1 1 calc R . . H40C H 0.8726 -0.0463 1.2304 0.069 Uiso 1 1 calc R . . C41 C 0.6823(3) -0.0062(3) 0.9985(5) 0.0441(16) Uani 1 1 d . . . H41A H 0.6479 0.0226 0.9766 0.066 Uiso 1 1 calc R . . H41B H 0.6694 -0.0451 1.0292 0.066 Uiso 1 1 calc R . . H41C H 0.6996 -0.0211 0.9469 0.066 Uiso 1 1 calc R . . C42 C 0.7726(3) -0.0783(3) 1.1224(4) 0.0363(14) Uani 1 1 d . . . H42A H 0.7362 -0.0939 1.1428 0.044 Uiso 1 1 calc R . . H42B H 0.8071 -0.0935 1.1685 0.044 Uiso 1 1 calc R . . C43 C 0.7755(3) -0.1155(3) 1.0349(4) 0.0313(12) Uani 1 1 d . . . C44 C 0.7379(3) -0.1698(3) 1.0092(4) 0.0328(13) Uani 1 1 d . . . C45 C 0.7436(3) -0.2069(3) 0.9317(4) 0.0376(14) Uani 1 1 d . . . C46 C 0.7854(3) -0.1890(3) 0.8779(4) 0.0340(14) Uani 1 1 d . . . C47 C 0.8206(2) -0.1311(3) 0.9025(4) 0.0299(12) Uani 1 1 d . . . C48 C 0.8181(2) -0.0977(3) 0.9820(4) 0.0294(12) Uani 1 1 d . . . C49 C 0.6919(3) -0.1919(4) 1.0630(5) 0.0531(19) Uani 1 1 d . . . H49A H 0.6548 -0.1668 1.0429 0.080 Uiso 1 1 calc R . . H49B H 0.7069 -0.1835 1.1277 0.080 Uiso 1 1 calc R . . H49C H 0.6840 -0.2396 1.0533 0.080 Uiso 1 1 calc R . . C50 C 0.7046(3) -0.2680(3) 0.9046(5) 0.0431(16) Uani 1 1 d . . . H50A H 0.7286 -0.3028 0.8817 0.052 Uiso 1 1 calc R . . H50B H 0.6914 -0.2859 0.9589 0.052 Uiso 1 1 calc R . . N7 N 0.6530(2) -0.2533(3) 0.8361(4) 0.0404(13) Uani 1 1 d . . . C51 C 0.6438(3) -0.2066(3) 0.7743(4) 0.0375(14) Uani 1 1 d . . . H51 H 0.6723 -0.1727 0.7703 0.045 Uiso 1 1 calc R . . N8 N 0.5931(3) -0.2102(3) 0.7193(5) 0.0580(18) Uani 1 1 d . . . C52 C 0.5603(4) -0.2554(3) 0.7623(5) 0.051 Uani 1 1 d . . . H52 H 0.5190 -0.2655 0.7436 0.061 Uiso 1 1 calc R . . C53 C 0.5988(3) -0.2832(4) 0.8373(5) 0.051 Uani 1 1 d . . . H53 H 0.5896 -0.3151 0.8793 0.061 Uiso 1 1 calc R . . C54 C 0.7934(3) -0.2300(3) 0.7948(5) 0.0474(17) Uani 1 1 d . . . H54A H 0.8350 -0.2448 0.8022 0.071 Uiso 1 1 calc R . . H54B H 0.7832 -0.2025 0.7400 0.071 Uiso 1 1 calc R . . H54C H 0.7670 -0.2690 0.7890 0.071 Uiso 1 1 calc R . . C55 C 0.8621(3) -0.0428(3) 1.0137(4) 0.0344(13) Uani 1 1 d . . . H55A H 0.8505 -0.0027 0.9775 0.052 Uiso 1 1 calc R . . H55B H 0.9021 -0.0568 1.0066 0.052 Uiso 1 1 calc R . . H55C H 0.8624 -0.0332 1.0778 0.052 Uiso 1 1 calc R . . C56 C 0.8649(3) -0.1117(3) 0.8413(4) 0.0335(13) Uani 1 1 d . . . H56A H 0.9052 -0.1270 0.8715 0.040 Uiso 1 1 calc R . . H56B H 0.8540 -0.1370 0.7839 0.040 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0282(3) 0.0447(4) 0.0366(4) -0.0084(3) 0.0079(3) 0.0002(3) Cl1 0.0424(9) 0.0496(10) 0.0537(10) -0.0107(8) 0.0190(8) -0.0142(7) Cl2 0.0386(9) 0.125(2) 0.0423(10) 0.0132(11) 0.0089(8) 0.0248(11) Zn2 0.0597(5) 0.0337(4) 0.0513(5) -0.0022(4) -0.0208(4) -0.0007(4) Cl3 0.0588(11) 0.0524(11) 0.0608(12) -0.0134(9) 0.0029(9) 0.0196(9) Cl4 0.130(2) 0.0507(13) 0.1015(19) 0.0075(12) -0.0763(18) -0.0277(14) C1 0.032(3) 0.026(3) 0.030(3) -0.005(2) 0.006(2) -0.003(2) C2 0.028(3) 0.028(3) 0.030(3) -0.011(2) 0.002(2) 0.005(2) C3 0.031(3) 0.032(3) 0.025(3) -0.011(2) 0.009(2) 0.000(2) C4 0.034(3) 0.024(3) 0.030(3) -0.002(2) 0.007(2) 0.002(2) C5 0.033(3) 0.023(3) 0.028(3) -0.004(2) 0.006(2) 0.003(2) C6 0.029(3) 0.026(3) 0.034(3) -0.003(2) 0.003(2) 0.001(2) C7 0.021(3) 0.041(4) 0.054(4) -0.002(3) -0.004(3) 0.008(3) C8 0.026(3) 0.039(3) 0.038(3) -0.011(3) 0.014(2) -0.004(2) N1 0.024(2) 0.030(2) 0.030(3) 0.001(2) 0.0023(19) -0.0020(19) C9 0.021(3) 0.040(3) 0.036(3) -0.002(3) 0.008(2) 0.000(2) N2 0.026(2) 0.047(3) 0.035(3) -0.005(2) 0.007(2) -0.002(2) C10 0.023(3) 0.035(3) 0.038(3) 0.000(3) 0.003(2) -0.001(2) C11 0.023(3) 0.031(3) 0.032(3) -0.001(2) 0.009(2) 0.003(2) C12 0.039(3) 0.029(3) 0.046(4) 0.008(3) 0.001(3) -0.003(3) C13 0.029(3) 0.030(3) 0.050(4) 0.000(3) -0.004(3) -0.001(2) C14 0.035(3) 0.034(3) 0.035(3) 0.000(3) -0.001(3) 0.010(3) C15 0.023(3) 0.023(3) 0.043(3) -0.003(2) -0.005(2) 0.005(2) C16 0.028(3) 0.035(3) 0.041(4) -0.005(3) -0.007(3) 0.011(2) C17 0.027(3) 0.031(3) 0.051(4) -0.010(3) -0.010(3) 0.011(2) C18 0.027(3) 0.038(4) 0.062(4) -0.008(3) 0.001(3) 0.015(3) C19 0.029(3) 0.032(3) 0.046(4) -0.009(3) -0.009(3) 0.003(2) C20 0.031(3) 0.024(3) 0.058(4) -0.005(3) -0.013(3) 0.007(2) C21 0.039(4) 0.075(5) 0.031(3) 0.007(3) -0.010(3) 0.010(3) C22 0.026(3) 0.039(4) 0.058(4) -0.013(3) -0.008(3) 0.015(3) N3 0.025(2) 0.044(3) 0.036(3) -0.005(2) -0.001(2) 0.010(2) C23 0.023(3) 0.050(4) 0.044(4) 0.000(3) -0.002(3) 0.007(3) N4 0.025(3) 0.053(3) 0.051(3) 0.004(3) -0.007(2) -0.004(2) C24 0.027(3) 0.063(5) 0.050(4) 0.002(3) -0.014(3) -0.010(3) C25 0.023(3) 0.063(5) 0.049(4) -0.007(3) -0.003(3) 0.002(3) C26 0.032(3) 0.065(5) 0.063(5) -0.010(4) 0.006(3) 0.016(3) C27 0.030(3) 0.041(4) 0.048(4) -0.006(3) -0.005(3) -0.006(3) C28 0.040(4) 0.038(4) 0.060(5) -0.017(3) 0.001(3) 0.006(3) C29 0.026(3) 0.034(3) 0.048(4) -0.012(3) 0.009(3) -0.002(2) C30 0.029(3) 0.038(3) 0.056(4) -0.015(3) 0.012(3) -0.011(3) C31 0.029(3) 0.042(4) 0.052(4) -0.016(3) 0.009(3) -0.013(3) C32 0.026(3) 0.038(3) 0.039(3) -0.012(3) 0.009(2) -0.007(2) C33 0.021(3) 0.033(3) 0.041(3) -0.008(3) 0.008(2) -0.005(2) C34 0.034(3) 0.038(3) 0.040(4) -0.007(3) 0.008(3) -0.009(3) C35 0.041(4) 0.050(4) 0.083(6) -0.028(4) 0.001(4) -0.005(3) C36 0.025(3) 0.054(4) 0.069(5) -0.027(4) 0.018(3) -0.013(3) N5 0.024(2) 0.040(3) 0.048(3) -0.019(2) 0.006(2) -0.010(2) C37 0.023(3) 0.039(3) 0.046(4) -0.014(3) 0.003(3) 0.000(2) N6 0.025(2) 0.034(3) 0.046(3) -0.012(2) 0.011(2) -0.001(2) C38 0.025(3) 0.048(4) 0.045(4) -0.016(3) 0.010(3) -0.003(3) C39 0.025(3) 0.049(4) 0.044(4) -0.017(3) 0.005(3) -0.005(3) C40 0.039(4) 0.053(4) 0.044(4) -0.009(3) 0.003(3) -0.012(3) C41 0.031(3) 0.046(4) 0.049(4) -0.011(3) -0.008(3) 0.000(3) C42 0.036(3) 0.032(3) 0.039(3) -0.005(3) 0.001(3) -0.012(3) C43 0.027(3) 0.027(3) 0.036(3) 0.001(2) -0.005(2) -0.005(2) C44 0.031(3) 0.023(3) 0.039(3) 0.002(2) -0.005(3) -0.003(2) C45 0.032(3) 0.028(3) 0.045(4) 0.001(3) -0.013(3) -0.002(2) C46 0.035(3) 0.021(3) 0.040(3) -0.001(2) -0.010(3) -0.003(2) C47 0.027(3) 0.019(3) 0.039(3) 0.000(2) -0.007(2) -0.002(2) C48 0.021(3) 0.028(3) 0.037(3) 0.003(2) 0.000(2) -0.001(2) C49 0.059(5) 0.045(4) 0.059(5) -0.005(3) 0.021(4) -0.029(4) C50 0.050(4) 0.032(3) 0.043(4) 0.004(3) -0.004(3) -0.005(3) N7 0.039(3) 0.045(3) 0.034(3) 0.006(2) -0.002(2) -0.016(2) C51 0.036(3) 0.033(3) 0.040(4) 0.000(3) -0.002(3) -0.003(3) N8 0.053(4) 0.037(3) 0.068(4) 0.012(3) -0.028(3) -0.025(3) C52 0.062 0.035 0.051 0.000 0.000 0.000 C53 0.062 0.035 0.051 0.000 0.000 0.000 C54 0.049(4) 0.027(3) 0.061(5) -0.012(3) -0.003(3) 0.001(3) C55 0.030(3) 0.031(3) 0.039(3) -0.004(3) -0.002(3) -0.007(2) C56 0.034(3) 0.026(3) 0.039(3) -0.004(2) 0.001(3) -0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N2 2.010(5) . ? Zn1 N6 2.018(5) . ? Zn1 Cl1 2.2296(18) . ? Zn1 Cl2 2.2547(19) . ? Zn2 N4 2.013(6) . ? Zn2 N8 2.017(6) . ? Zn2 Cl4 2.227(2) . ? Zn2 Cl3 2.250(2) . ? C1 C2 1.395(8) . ? C1 C6 1.426(8) . ? C1 C56 1.523(8) . ? C2 C3 1.413(8) . ? C2 C7 1.524(8) . ? C3 C4 1.403(8) . ? C3 C8 1.510(8) . ? C4 C5 1.411(8) . ? C4 C12 1.495(8) . ? C5 C6 1.385(8) . ? C5 C14 1.525(8) . ? C6 C13 1.539(8) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 N1 1.469(7) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? N1 C9 1.331(7) . ? N1 C11 1.360(7) . ? C9 N2 1.328(8) . ? C9 H9 0.9500 . ? N2 C10 1.378(7) . ? C10 C11 1.359(8) . ? 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 1.509(9) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.413(8) . ? C15 C20 1.417(9) . ? C16 C17 1.418(9) . ? C16 C21 1.482(9) . ? C17 C18 1.402(10) . ? C17 C22 1.531(8) . ? C18 C19 1.416(8) . ? C18 C26 1.509(10) . ? C19 C20 1.374(10) . ? C19 C28 1.519(9) . ? C20 C27 1.543(8) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 N3 1.478(8) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? N3 C23 1.327(8) . ? N3 C25 1.378(8) . ? C23 N4 1.309(9) . ? C23 H23 0.9500 . ? N4 C24 1.359(8) . ? C24 C25 1.323(10) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.536(9) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C34 1.401(9) . ? C29 C30 1.433(9) . ? C30 C31 1.397(10) . ? C30 C35 1.511(10) . ? C31 C32 1.395(9) . ? C31 C36 1.532(9) . ? C32 C33 1.413(8) . ? C32 C40 1.548(9) . ? C33 C34 1.409(9) . ? C33 C42 1.502(8) . ? C34 C41 1.524(8) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 N5 1.498(8) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? N5 C37 1.340(9) . ? N5 C39 1.369(8) . ? C37 N6 1.317(7) . ? C37 H37 0.9500 . ? N6 C38 1.374(8) . ? C38 C39 1.349(9) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C43 1.524(9) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.395(8) . ? C43 C48 1.415(8) . ? C44 C45 1.407(9) . ? C44 C49 1.509(9) . ? C45 C46 1.411(9) . ? C45 C50 1.522(8) . ? C46 C47 1.419(8) . ? C46 C54 1.535(9) . ? C47 C48 1.380(8) . ? C47 C56 1.540(9) . ? C48 C55 1.503(8) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 N7 1.436(8) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? N7 C51 1.307(8) . ? N7 C53 1.376(9) . ? C51 N8 1.285(8) . ? C51 H51 0.9500 . ? N8 C52 1.411(10) . ? C52 C53 1.403(10) . ? C52 H52 0.9500 . ? C53 H53 0.9500 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9900 . ? C56 H56B 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 N2 Zn1 N6 110.8(2) . . ? N2 Zn1 Cl1 106.21(15) . . ? N6 Zn1 Cl1 110.76(15) . . ? N2 Zn1 Cl2 104.00(16) . . ? N6 Zn1 Cl2 101.48(15) . . ? Cl1 Zn1 Cl2 123.24(9) . . ? N4 Zn2 N8 113.1(3) . . ? N4 Zn2 Cl4 106.86(17) . . ? N8 Zn2 Cl4 107.91(16) . . ? N4 Zn2 Cl3 102.73(17) . . ? N8 Zn2 Cl3 106.6(2) . . ? Cl4 Zn2 Cl3 119.79(12) . . ? C2 C1 C6 119.3(5) . . ? C2 C1 C56 120.2(5) . . ? C6 C1 C56 120.2(5) . . ? C1 C2 C3 119.5(5) . . ? C1 C2 C7 121.7(5) . . ? C3 C2 C7 118.8(5) . . ? C4 C3 C2 121.1(5) . . ? C4 C3 C8 118.9(5) . . ? C2 C3 C8 119.8(5) . . ? C3 C4 C5 118.6(5) . . ? C3 C4 C12 120.8(5) . . ? C5 C4 C12 120.5(5) . . ? C6 C5 C4 120.5(5) . . ? C6 C5 C14 120.7(5) . . ? C4 C5 C14 118.4(5) . . ? C5 C6 C1 120.3(5) . . ? C5 C6 C13 120.0(5) . . ? C1 C6 C13 119.6(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 113.5(5) . . ? 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 108.2(5) . . ? C9 N1 C8 126.5(5) . . ? C11 N1 C8 125.3(5) . . ? N2 C9 N1 111.2(5) . . ? N2 C9 H9 124.4 . . ? N1 C9 H9 124.4 . . ? C9 N2 C10 105.0(5) . . ? C9 N2 Zn1 124.9(4) . . ? C10 N2 Zn1 128.6(4) . . ? C11 C10 N2 109.7(5) . . ? C11 C10 H10 125.1 . . ? N2 C10 H10 125.1 . . ? C10 C11 N1 105.8(5) . . ? C10 C11 H11 127.1 . . ? N1 C11 H11 127.1 . . ? 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 121.3(5) . . ? C15 C14 H14A 107.0 . . ? C5 C14 H14A 107.0 . . ? C15 C14 H14B 107.0 . . ? C5 C14 H14B 107.0 . . ? H14A C14 H14B 106.8 . . ? C16 C15 C20 118.3(6) . . ? C16 C15 C14 118.4(6) . . ? C20 C15 C14 123.2(5) . . ? C15 C16 C17 118.9(6) . . ? C15 C16 C21 121.5(6) . . ? C17 C16 C21 119.6(5) . . ? C18 C17 C16 122.0(5) . . ? C18 C17 C22 119.4(6) . . ? C16 C17 C22 118.5(6) . . ? C17 C18 C19 117.4(6) . . ? C17 C18 C26 121.2(6) . . ? C19 C18 C26 121.3(7) . . ? C20 C19 C18 121.1(6) . . ? C20 C19 C28 120.0(5) . . ? C18 C19 C28 118.8(6) . . ? C19 C20 C15 121.5(5) . . ? C19 C20 C27 121.2(6) . . ? C15 C20 C27 117.1(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 . . ? N3 C22 C17 112.4(5) . . ? N3 C22 H22A 109.1 . . ? C17 C22 H22A 109.1 . . ? N3 C22 H22B 109.1 . . ? C17 C22 H22B 109.1 . . ? H22A C22 H22B 107.9 . . ? C23 N3 C25 105.9(6) . . ? C23 N3 C22 128.9(5) . . ? C25 N3 C22 125.1(5) . . ? N4 C23 N3 112.9(5) . . ? N4 C23 H23 123.6 . . ? N3 C23 H23 123.6 . . ? C23 N4 C24 103.9(6) . . ? C23 N4 Zn2 125.0(4) . . ? C24 N4 Zn2 128.3(5) . . ? C25 C24 N4 111.5(6) . . ? C25 C24 H24 124.3 . . ? N4 C24 H24 124.3 . . ? C24 C25 N3 105.8(6) . . ? C24 C25 H25 127.1 . . ? N3 C25 H25 127.1 . . ? C18 C26 H26A 109.5 . . ? C18 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C18 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C20 C27 H27A 109.5 . . ? C20 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C20 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C19 C28 C29 118.9(5) . . ? C19 C28 H28A 107.6 . . ? C29 C28 H28A 107.6 . . ? C19 C28 H28B 107.6 . . ? C29 C28 H28B 107.6 . . ? H28A C28 H28B 107.0 . . ? C34 C29 C30 119.4(6) . . ? C34 C29 C28 122.1(5) . . ? C30 C29 C28 118.3(6) . . ? C31 C30 C29 118.9(6) . . ? C31 C30 C35 121.8(6) . . ? C29 C30 C35 119.3(6) . . ? C32 C31 C30 121.0(6) . . ? C32 C31 C36 118.4(6) . . ? C30 C31 C36 120.7(6) . . ? C31 C32 C33 120.5(6) . . ? C31 C32 C40 119.3(5) . . ? C33 C32 C40 120.1(5) . . ? C34 C33 C32 118.6(6) . . ? C34 C33 C42 119.6(5) . . ? C32 C33 C42 121.7(5) . . ? C29 C34 C33 121.0(5) . . ? C29 C34 C41 120.3(6) . . ? C33 C34 C41 118.7(6) . . ? C30 C35 H35A 109.5 . . ? C30 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C30 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N5 C36 C31 110.3(6) . . ? N5 C36 H36A 109.6 . . ? C31 C36 H36A 109.6 . . ? N5 C36 H36B 109.6 . . ? C31 C36 H36B 109.6 . . ? H36A C36 H36B 108.1 . . ? C37 N5 C39 106.8(5) . . ? C37 N5 C36 127.2(6) . . ? C39 N5 C36 125.5(6) . . ? N6 C37 N5 111.6(6) . . ? N6 C37 H37 124.2 . . ? N5 C37 H37 124.2 . . ? C37 N6 C38 105.5(5) . . ? C37 N6 Zn1 123.8(5) . . ? C38 N6 Zn1 128.9(4) . . ? C39 C38 N6 109.4(5) . . ? C39 C38 H38 125.3 . . ? N6 C38 H38 125.3 . . ? C38 C39 N5 106.6(6) . . ? C38 C39 H39 126.7 . . ? N5 C39 H39 126.7 . . ? C32 C40 H40A 109.5 . . ? C32 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C32 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C34 C41 H41A 109.5 . . ? C34 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C34 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C33 C42 C43 121.7(5) . . ? C33 C42 H42A 106.9 . . ? C43 C42 H42A 106.9 . . ? C33 C42 H42B 106.9 . . ? C43 C42 H42B 106.9 . . ? H42A C42 H42B 106.7 . . ? C44 C43 C48 119.6(6) . . ? C44 C43 C42 119.7(5) . . ? C48 C43 C42 120.6(5) . . ? C43 C44 C45 119.5(6) . . ? C43 C44 C49 122.3(6) . . ? C45 C44 C49 118.1(5) . . ? C44 C45 C46 121.2(5) . . ? C44 C45 C50 120.3(6) . . ? C46 C45 C50 118.5(6) . . ? C45 C46 C47 118.1(6) . . ? C45 C46 C54 121.9(5) . . ? C47 C46 C54 120.1(6) . . ? C48 C47 C46 120.5(6) . . ? C48 C47 C56 122.3(5) . . ? C46 C47 C56 117.0(5) . . ? C47 C48 C43 120.7(5) . . ? C47 C48 C55 119.6(5) . . ? C43 C48 C55 119.7(5) . . ? C44 C49 H49A 109.5 . . ? C44 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C44 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? N7 C50 C45 112.5(5) . . ? N7 C50 H50A 109.1 . . ? C45 C50 H50A 109.1 . . ? N7 C50 H50B 109.1 . . ? C45 C50 H50B 109.1 . . ? H50A C50 H50B 107.8 . . ? C51 N7 C53 107.5(6) . . ? C51 N7 C50 130.7(5) . . ? C53 N7 C50 121.0(6) . . ? N8 C51 N7 114.7(6) . . ? N8 C51 H51 122.7 . . ? N7 C51 H51 122.7 . . ? C51 N8 C52 103.4(6) . . ? C51 N8 Zn2 128.2(5) . . ? C52 N8 Zn2 127.6(5) . . ? C53 C52 N8 108.5(7) . . ? C53 C52 H52 125.7 . . ? N8 C52 H52 125.7 . . ? N7 C53 C52 103.9(7) . . ? N7 C53 H53 128.0 . . ? C52 C53 H53 128.0 . . ? C46 C54 H54A 109.5 . . ? C46 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C46 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C48 C55 H55A 109.5 . . ? C48 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C48 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C1 C56 C47 118.0(5) . . ? C1 C56 H56A 107.8 . . ? C47 C56 H56A 107.8 . . ? C1 C56 H56B 107.8 . . ? C47 C56 H56B 107.8 . . ? H56A C56 H56B 107.2 . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.433 _refine_diff_density_min -1.763 _refine_diff_density_rms 0.123 # Attachment '4.cif' data_4 _database_code_depnum_ccdc_archive 'CCDC 702201' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H64 N8, 1.5(C2 H4 Cl2), 3(H2 O)' _chemical_formula_sum 'C59 H76 Cl3 N8 O3' _chemical_formula_weight 1051.63 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' 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 11.8093(4) _cell_length_b 14.6475(6) _cell_length_c 16.0027(7) _cell_angle_alpha 102.773(2) _cell_angle_beta 94.242(3) _cell_angle_gamma 94.968(3) _cell_volume 2677.07(18) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1776 _cell_measurement_theta_min 2.11 _cell_measurement_theta_max 27.000 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.305 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1122 _exptl_absorpt_coefficient_mu 0.225 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9649 _exptl_absorpt_correction_T_max 0.9778 _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 24992 _diffrn_reflns_av_R_equivalents 0.0637 _diffrn_reflns_av_sigmaI/netI 0.1127 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 27.00 _reflns_number_total 11183 _reflns_number_gt 4697 _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^)+(0.1741P)^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 0.0060(19) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 11183 _refine_ls_number_parameters 671 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1938 _refine_ls_R_factor_gt 0.0966 _refine_ls_wR_factor_ref 0.3407 _refine_ls_wR_factor_gt 0.2606 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.012 _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 C1 C 0.6983(4) 0.4474(4) 0.0451(3) 0.0347(12) Uani 1 1 d . . . C2 C 0.6509(4) 0.4612(4) -0.0337(3) 0.0354(12) Uani 1 1 d . . . C3 C 0.5520(4) 0.4049(4) -0.0758(3) 0.0369(12) Uani 1 1 d . . . C4 C 0.4989(4) 0.3352(4) -0.0397(3) 0.0367(12) Uani 1 1 d . . . C5 C 0.5439(4) 0.3216(3) 0.0393(3) 0.0337(12) Uani 1 1 d . . . C6 C 0.6430(4) 0.3790(4) 0.0828(3) 0.0337(11) Uani 1 1 d . . . C7 C 0.7042(5) 0.5389(4) -0.0719(3) 0.0408(13) Uani 1 1 d . . . H7A H 0.7693 0.5171 -0.1023 0.061 Uiso 1 1 calc R . . H7B H 0.7303 0.5945 -0.0257 0.061 Uiso 1 1 calc R . . H7C H 0.6473 0.5554 -0.1123 0.061 Uiso 1 1 calc R . . C8 C 0.5042(4) 0.4196(4) -0.1607(3) 0.0442(14) Uani 1 1 d . . . H8A H 0.4303 0.3802 -0.1788 0.053 Uiso 1 1 calc R . . H8B H 0.4898 0.4863 -0.1541 0.053 Uiso 1 1 calc R . . N1 N 0.5825(4) 0.3953(3) -0.2275(3) 0.0454(12) Uani 1 1 d . . . C9 C 0.6765(5) 0.3495(5) -0.2268(4) 0.0566(17) Uani 1 1 d . . . H9 H 0.7059 0.3231 -0.1816 0.068 Uiso 1 1 calc R . . C10 C 0.7213(6) 0.3482(5) -0.3022(5) 0.0651(19) Uani 1 1 d . . . H10 H 0.7866 0.3182 -0.3198 0.078 Uiso 1 1 calc R . . N2 N 0.6590(6) 0.3957(6) -0.3485(4) 0.091(2) Uani 1 1 d . . . C11 C 0.5776(7) 0.4231(7) -0.3009(5) 0.084(3) Uani 1 1 d . . . H11 H 0.5205 0.4593 -0.3172 0.101 Uiso 1 1 calc R . . C12 C 0.3925(4) 0.2771(4) -0.0895(4) 0.0431(13) Uani 1 1 d . . . H12A H 0.3603 0.2349 -0.0555 0.065 Uiso 1 1 calc R . . H12B H 0.4124 0.2397 -0.1441 0.065 Uiso 1 1 calc R . . H12C H 0.3360 0.3191 -0.1010 0.065 Uiso 1 1 calc R . . C13 C 0.6833(4) 0.3724(4) 0.1721(3) 0.0398(13) Uani 1 1 d . . . H13A H 0.6174 0.3581 0.2025 0.060 Uiso 1 1 calc R . . H13B H 0.7251 0.4325 0.2031 0.060 Uiso 1 1 calc R . . H13C H 0.7338 0.3223 0.1690 0.060 Uiso 1 1 calc R . . C14 C 0.4842(4) 0.2498(4) 0.0834(3) 0.0356(12) Uani 1 1 d . . . H14A H 0.4543 0.2854 0.1357 0.043 Uiso 1 1 calc R . . H14B H 0.4177 0.2161 0.0441 0.043 Uiso 1 1 calc R . . C15 C 0.5547(4) 0.1761(3) 0.1097(3) 0.0309(11) Uani 1 1 d . . . C16 C 0.5611(4) 0.1636(4) 0.1945(3) 0.0345(12) Uani 1 1 d . . . C17 C 0.6267(4) 0.0958(4) 0.2166(3) 0.0340(12) Uani 1 1 d . . . C18 C 0.6877(4) 0.0411(3) 0.1561(3) 0.0313(11) Uani 1 1 d . . . C19 C 0.6825(4) 0.0530(3) 0.0712(3) 0.0313(11) Uani 1 1 d . . . C20 C 0.6113(4) 0.1180(3) 0.0471(3) 0.0327(12) Uani 1 1 d . . . C21 C 0.4962(5) 0.2198(4) 0.2629(3) 0.0429(14) Uani 1 1 d . . . H21A H 0.4685 0.1796 0.3002 0.064 Uiso 1 1 calc R . . H21B H 0.4312 0.2429 0.2353 0.064 Uiso 1 1 calc R . . H21C H 0.5470 0.2735 0.2976 0.064 Uiso 1 1 calc R . . C22 C 0.6359(4) 0.0851(4) 0.3090(3) 0.0393(13) Uani 1 1 d . . . H22A H 0.7086 0.0595 0.3211 0.047 Uiso 1 1 calc R . . H22B H 0.6379 0.1480 0.3481 0.047 Uiso 1 1 calc R . . N3 N 0.5412(3) 0.0232(3) 0.3270(3) 0.0359(10) Uani 1 1 d . . . C23 C 0.4805(5) 0.0415(4) 0.3958(4) 0.0495(16) Uani 1 1 d . . . H23 H 0.4919 0.0985 0.4389 0.059 Uiso 1 1 calc R . . N4 N 0.4030(4) -0.0296(4) 0.3960(3) 0.0497(13) Uani 1 1 d . . . C24 C 0.4179(5) -0.0978(4) 0.3250(4) 0.0483(15) Uani 1 1 d . . . H24 H 0.3757 -0.1583 0.3084 0.058 Uiso 1 1 calc R . . C25 C 0.5011(5) -0.0663(4) 0.2823(4) 0.0458(14) Uani 1 1 d . . . H25 H 0.5272 -0.0998 0.2307 0.055 Uiso 1 1 calc R . . C26 C 0.7557(4) -0.0345(4) 0.1807(3) 0.0392(13) Uani 1 1 d . . . H26A H 0.8370 -0.0111 0.1910 0.059 Uiso 1 1 calc R . . H26B H 0.7445 -0.0911 0.1338 0.059 Uiso 1 1 calc R . . H26C H 0.7294 -0.0498 0.2331 0.059 Uiso 1 1 calc R . . C27 C 0.5925(4) 0.1209(4) -0.0455(3) 0.0401(13) Uani 1 1 d . . . H27A H 0.5182 0.1432 -0.0564 0.060 Uiso 1 1 calc R . . H27B H 0.5940 0.0575 -0.0815 0.060 Uiso 1 1 calc R . . H27C H 0.6530 0.1637 -0.0593 0.060 Uiso 1 1 calc R . . C28 C 0.7489(4) -0.0032(3) 0.0034(3) 0.0335(11) Uani 1 1 d . . . H28A H 0.6931 -0.0456 -0.0404 0.040 Uiso 1 1 calc R . . H28B H 0.7948 -0.0435 0.0314 0.040 Uiso 1 1 calc R . . C29 C 0.8287(4) 0.0513(3) -0.0433(3) 0.0285(11) Uani 1 1 d . . . C30 C 0.8197(4) 0.0325(3) -0.1331(3) 0.0315(11) Uani 1 1 d . . . C31 C 0.8931(4) 0.0852(3) -0.1741(3) 0.0320(11) Uani 1 1 d . . . C32 C 0.9775(4) 0.1564(4) -0.1263(3) 0.0340(12) Uani 1 1 d . . . C33 C 0.9858(4) 0.1745(3) -0.0363(3) 0.0319(11) Uani 1 1 d . . . C34 C 0.9142(4) 0.1189(3) 0.0053(3) 0.0330(11) Uani 1 1 d . . . C35 C 0.7346(4) -0.0458(4) -0.1870(3) 0.0426(13) Uani 1 1 d . . . H35A H 0.6620 -0.0207 -0.1980 0.064 Uiso 1 1 calc R . . H35B H 0.7221 -0.0959 -0.1560 0.064 Uiso 1 1 calc R . . H35C H 0.7646 -0.0713 -0.2419 0.064 Uiso 1 1 calc R . . C36 C 0.8795(4) 0.0718(4) -0.2714(3) 0.0379(12) Uani 1 1 d . . . H36A H 0.8002 0.0449 -0.2932 0.046 Uiso 1 1 calc R . . H36B H 0.8919 0.1340 -0.2857 0.046 Uiso 1 1 calc R . . N5 N 0.9598(3) 0.0090(3) -0.3159(3) 0.0344(10) Uani 1 1 d . . . C37 C 1.0272(5) 0.0300(4) -0.3749(3) 0.0439(14) Uani 1 1 d . . . H37 H 1.0310 0.0877 -0.3929 0.053 Uiso 1 1 calc R . . N6 N 1.0881(4) -0.0413(3) -0.4049(3) 0.0473(12) Uani 1 1 d . . . C38 C 1.0543(5) -0.1093(4) -0.3634(4) 0.0452(14) Uani 1 1 d . . . H38 H 1.0818 -0.1694 -0.3722 0.054 Uiso 1 1 calc R . . C39 C 0.9760(5) -0.0802(4) -0.3077(3) 0.0399(13) Uani 1 1 d . . . H39 H 0.9402 -0.1143 -0.2711 0.048 Uiso 1 1 calc R . . C40 C 1.0546(4) 0.2099(4) -0.1748(3) 0.0401(13) Uani 1 1 d . . . H40A H 1.0108 0.2526 -0.2000 0.060 Uiso 1 1 calc R . . H40B H 1.0848 0.1652 -0.2206 0.060 Uiso 1 1 calc R . . H40C H 1.1180 0.2463 -0.1350 0.060 Uiso 1 1 calc R . . C41 C 0.9345(4) 0.1297(4) 0.1005(3) 0.0404(13) Uani 1 1 d . . . H41A H 0.8829 0.1725 0.1296 0.061 Uiso 1 1 calc R . . H41B H 1.0139 0.1554 0.1200 0.061 Uiso 1 1 calc R . . H41C H 0.9201 0.0680 0.1144 0.061 Uiso 1 1 calc R . . C42 C 1.0737(4) 0.2523(4) 0.0194(3) 0.0341(11) Uani 1 1 d . . . H42A H 1.1301 0.2213 0.0493 0.041 Uiso 1 1 calc R . . H42B H 1.1151 0.2836 -0.0199 0.041 Uiso 1 1 calc R . . C43 C 1.0301(4) 0.3290(4) 0.0872(3) 0.0340(12) Uani 1 1 d . . . C44 C 1.0779(4) 0.3524(4) 0.1729(3) 0.0369(12) Uani 1 1 d . . . C45 C 1.0400(4) 0.4270(4) 0.2320(3) 0.0382(13) Uani 1 1 d . . . C46 C 0.9524(4) 0.4773(4) 0.2062(3) 0.0367(12) Uani 1 1 d . . . C47 C 0.9049(4) 0.4532(3) 0.1209(3) 0.0319(11) Uani 1 1 d . . . C48 C 0.9458(4) 0.3814(4) 0.0605(3) 0.0341(12) Uani 1 1 d . . . C49 C 1.1711(4) 0.3021(4) 0.2055(3) 0.0449(14) Uani 1 1 d . . . H49A H 1.1886 0.2511 0.1589 0.067 Uiso 1 1 calc R . . H49B H 1.1459 0.2758 0.2531 0.067 Uiso 1 1 calc R . . H49C H 1.2396 0.3465 0.2259 0.067 Uiso 1 1 calc R . . C50 C 1.0912(5) 0.4528(4) 0.3250(3) 0.0435(14) Uani 1 1 d . . . H50A H 1.1701 0.4351 0.3278 0.052 Uiso 1 1 calc R . . H50B H 1.0950 0.5219 0.3468 0.052 Uiso 1 1 calc R . . N7 N 1.0249(4) 0.4060(3) 0.3809(3) 0.0410(11) Uani 1 1 d . . . C51 C 1.0603(5) 0.3971(4) 0.4585(3) 0.0492(15) Uani 1 1 d . . . H51 H 1.1368 0.4151 0.4834 0.059 Uiso 1 1 calc R . . N8 N 0.9801(4) 0.3610(3) 0.4986(3) 0.0495(13) Uani 1 1 d . . . C52 C 0.8834(5) 0.3493(4) 0.4427(4) 0.0521(16) Uani 1 1 d . . . H52 H 0.8094 0.3265 0.4534 0.063 Uiso 1 1 calc R . . C53 C 0.9099(5) 0.3753(4) 0.3696(4) 0.0497(15) Uani 1 1 d . . . H53 H 0.8590 0.3728 0.3201 0.060 Uiso 1 1 calc R . . C54 C 0.9144(5) 0.5581(4) 0.2708(4) 0.0457(14) Uani 1 1 d . . . H54A H 0.9536 0.6176 0.2643 0.069 Uiso 1 1 calc R . . H54B H 0.9333 0.5501 0.3292 0.069 Uiso 1 1 calc R . . H54C H 0.8317 0.5590 0.2605 0.069 Uiso 1 1 calc R . . C55 C 0.9039(5) 0.3659(4) -0.0327(3) 0.0403(13) Uani 1 1 d . . . H55A H 0.9641 0.3427 -0.0682 0.060 Uiso 1 1 calc R . . H55B H 0.8837 0.4254 -0.0450 0.060 Uiso 1 1 calc R . . H55C H 0.8364 0.3194 -0.0460 0.060 Uiso 1 1 calc R . . C56 C 0.8084(4) 0.5062(4) 0.0907(3) 0.0376(12) Uani 1 1 d . . . H56A H 0.7879 0.5514 0.1417 0.045 Uiso 1 1 calc R . . H56B H 0.8393 0.5434 0.0513 0.045 Uiso 1 1 calc R . . C57 C 0.2271(8) 0.1780(10) 0.5042(7) 0.157(6) Uani 1 1 d . . . H57A H 0.1590 0.2084 0.5238 0.188 Uiso 1 1 calc R . . H57B H 0.2016 0.1111 0.4769 0.188 Uiso 1 1 calc R . . C58 C 0.3119(11) 0.1822(13) 0.5838(8) 0.209(9) Uani 1 1 d . . . H58A H 0.3114 0.1179 0.5940 0.250 Uiso 1 1 calc R . . H58B H 0.3895 0.2009 0.5698 0.250 Uiso 1 1 calc R . . Cl1 Cl 0.28159(18) 0.23139(17) 0.42757(15) 0.0913(7) Uani 1 1 d . . . Cl2 Cl 0.2903(3) 0.2476(3) 0.6662(2) 0.1728(16) Uani 1 1 d . . . C59 C 0.5437(10) 0.5335(8) 0.5093(7) 0.165(6) Uani 1 1 d D . . H59A H 0.5818 0.5395 0.5678 0.198 Uiso 1 1 calc R . . H59B H 0.5206 0.5952 0.5032 0.198 Uiso 1 1 calc R . . Cl3 Cl 0.63869(18) 0.48070(19) 0.41989(16) 0.0978(8) Uani 1 1 d D . . O1 O 0.9463(4) 0.2374(3) 0.6118(2) 0.0565(11) Uani 1 1 d . . . O2 O 0.7610(3) 0.1119(3) 0.5208(2) 0.0535(11) Uani 1 1 d . . . O3 O 0.6203(5) 0.2493(4) 0.4910(3) 0.0856(16) 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 C1 0.031(2) 0.031(3) 0.040(3) 0.007(2) 0.002(2) 0.001(2) C2 0.036(3) 0.032(3) 0.036(3) 0.006(2) 0.003(2) -0.001(2) C3 0.038(3) 0.038(3) 0.034(3) 0.005(2) 0.002(2) 0.006(2) C4 0.033(3) 0.034(3) 0.041(3) 0.007(2) -0.001(2) 0.004(2) C5 0.034(3) 0.029(3) 0.036(3) 0.002(2) 0.005(2) 0.003(2) C6 0.030(2) 0.036(3) 0.033(3) 0.003(2) 0.005(2) 0.004(2) C7 0.043(3) 0.034(3) 0.048(3) 0.014(2) 0.006(3) 0.003(2) C8 0.034(3) 0.054(4) 0.043(3) 0.011(3) 0.000(2) 0.001(3) N1 0.040(3) 0.055(3) 0.041(3) 0.012(2) 0.004(2) 0.002(2) C9 0.056(4) 0.059(4) 0.052(4) 0.003(3) 0.009(3) 0.011(3) C10 0.070(5) 0.063(5) 0.058(4) 0.005(4) 0.014(4) 0.002(4) N2 0.100(5) 0.130(6) 0.054(4) 0.033(4) 0.021(4) 0.031(5) C11 0.083(5) 0.136(8) 0.051(4) 0.048(5) 0.019(4) 0.033(5) C12 0.041(3) 0.041(3) 0.043(3) 0.005(2) -0.002(2) -0.001(2) C13 0.042(3) 0.037(3) 0.038(3) 0.008(2) 0.003(2) -0.005(2) C14 0.030(2) 0.037(3) 0.039(3) 0.007(2) 0.004(2) 0.003(2) C15 0.029(2) 0.030(3) 0.031(3) 0.004(2) -0.001(2) -0.003(2) C16 0.031(3) 0.035(3) 0.036(3) 0.006(2) 0.007(2) -0.003(2) C17 0.034(3) 0.036(3) 0.028(3) 0.003(2) 0.008(2) -0.006(2) C18 0.028(2) 0.031(3) 0.035(3) 0.008(2) 0.005(2) -0.002(2) C19 0.031(2) 0.031(3) 0.030(3) 0.006(2) 0.003(2) -0.004(2) C20 0.029(2) 0.031(3) 0.033(3) 0.002(2) 0.004(2) -0.004(2) C21 0.045(3) 0.046(3) 0.038(3) 0.004(2) 0.014(3) 0.006(3) C22 0.035(3) 0.045(3) 0.035(3) 0.008(2) 0.008(2) -0.008(2) N3 0.034(2) 0.037(2) 0.037(2) 0.0090(19) 0.0093(19) 0.0013(19) C23 0.046(3) 0.062(4) 0.036(3) 0.002(3) 0.016(3) -0.004(3) N4 0.043(3) 0.060(3) 0.046(3) 0.014(2) 0.009(2) -0.006(2) C24 0.046(3) 0.038(3) 0.063(4) 0.017(3) 0.008(3) -0.002(3) C25 0.044(3) 0.044(3) 0.045(3) 0.003(3) 0.006(3) -0.003(3) C26 0.031(3) 0.044(3) 0.041(3) 0.009(2) 0.004(2) 0.001(2) C27 0.040(3) 0.038(3) 0.040(3) 0.006(2) 0.004(2) 0.004(2) C28 0.037(3) 0.030(3) 0.033(3) 0.004(2) 0.011(2) 0.004(2) C29 0.029(2) 0.028(3) 0.029(3) 0.005(2) 0.007(2) 0.002(2) C30 0.030(2) 0.030(3) 0.032(3) 0.001(2) 0.005(2) 0.003(2) C31 0.033(2) 0.033(3) 0.032(3) 0.007(2) 0.008(2) 0.006(2) C32 0.033(3) 0.038(3) 0.032(3) 0.008(2) 0.005(2) 0.004(2) C33 0.030(2) 0.030(3) 0.035(3) 0.005(2) 0.004(2) 0.005(2) C34 0.032(3) 0.033(3) 0.034(3) 0.006(2) 0.005(2) 0.004(2) C35 0.042(3) 0.046(3) 0.036(3) 0.004(2) 0.003(2) -0.004(3) C36 0.036(3) 0.042(3) 0.036(3) 0.007(2) 0.009(2) 0.006(2) N5 0.034(2) 0.040(3) 0.027(2) 0.0024(18) 0.0082(18) 0.0035(19) C37 0.050(3) 0.044(3) 0.040(3) 0.009(3) 0.015(3) 0.009(3) N6 0.049(3) 0.048(3) 0.042(3) 0.002(2) 0.009(2) 0.008(2) C38 0.044(3) 0.040(3) 0.048(3) 0.001(3) 0.006(3) 0.008(3) C39 0.044(3) 0.032(3) 0.043(3) 0.007(2) 0.005(2) 0.001(2) C40 0.041(3) 0.043(3) 0.035(3) 0.009(2) 0.005(2) -0.003(2) C41 0.038(3) 0.051(3) 0.032(3) 0.012(2) 0.002(2) -0.007(2) C42 0.028(2) 0.035(3) 0.038(3) 0.007(2) 0.002(2) 0.003(2) C43 0.030(2) 0.034(3) 0.037(3) 0.007(2) 0.002(2) -0.003(2) C44 0.032(3) 0.040(3) 0.036(3) 0.011(2) -0.002(2) -0.009(2) C45 0.036(3) 0.040(3) 0.034(3) 0.007(2) -0.002(2) -0.010(2) C46 0.036(3) 0.036(3) 0.033(3) 0.001(2) 0.001(2) -0.006(2) C47 0.033(2) 0.025(3) 0.034(3) 0.001(2) 0.001(2) -0.001(2) C48 0.032(3) 0.034(3) 0.034(3) 0.006(2) 0.000(2) -0.005(2) C49 0.040(3) 0.054(4) 0.039(3) 0.009(3) -0.008(2) 0.006(3) C50 0.042(3) 0.043(3) 0.040(3) 0.002(2) -0.003(2) -0.007(2) N7 0.042(2) 0.043(3) 0.033(2) 0.002(2) 0.001(2) -0.005(2) C51 0.058(4) 0.050(4) 0.034(3) 0.006(3) -0.009(3) -0.001(3) N8 0.064(3) 0.042(3) 0.041(3) 0.011(2) 0.000(2) -0.001(2) C52 0.057(4) 0.049(4) 0.054(4) 0.018(3) 0.009(3) 0.003(3) C53 0.043(3) 0.056(4) 0.049(4) 0.017(3) -0.001(3) -0.007(3) C54 0.046(3) 0.042(3) 0.043(3) 0.002(3) 0.000(3) -0.002(3) C55 0.043(3) 0.037(3) 0.038(3) 0.001(2) 0.000(2) 0.007(2) C56 0.036(3) 0.030(3) 0.044(3) 0.001(2) 0.009(2) 0.000(2) C57 0.088(7) 0.297(18) 0.119(9) 0.130(11) 0.009(6) 0.002(9) C58 0.152(12) 0.40(3) 0.123(11) 0.095(14) 0.061(9) 0.148(15) Cl1 0.0731(13) 0.1022(17) 0.1041(17) 0.0316(13) 0.0203(12) 0.0087(12) Cl2 0.138(3) 0.193(3) 0.133(3) -0.077(2) -0.033(2) 0.048(2) C59 0.218(15) 0.136(11) 0.128(9) 0.063(9) -0.075(10) -0.061(9) Cl3 0.0731(13) 0.128(2) 0.1007(17) 0.0380(15) 0.0115(12) 0.0220(13) O1 0.069(3) 0.050(3) 0.047(2) 0.011(2) -0.002(2) -0.004(2) O2 0.048(2) 0.061(3) 0.050(2) 0.008(2) 0.0141(19) -0.003(2) O3 0.087(4) 0.088(4) 0.078(4) 0.017(3) 0.000(3) 0.004(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 C1 C2 1.404(7) . ? C1 C6 1.416(6) . ? C1 C56 1.534(7) . ? C2 C3 1.403(7) . ? C2 C7 1.519(7) . ? C3 C4 1.405(7) . ? C3 C8 1.500(7) . ? C4 C5 1.396(7) . ? C4 C12 1.518(7) . ? C5 C6 1.418(7) . ? C5 C14 1.540(6) . ? C6 C13 1.499(7) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 N1 1.470(7) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? N1 C11 1.324(8) . ? N1 C9 1.347(8) . ? C9 C10 1.349(9) . ? C9 H9 0.9500 . ? C10 N2 1.347(9) . ? C10 H10 0.9500 . ? N2 C11 1.306(9) . ? 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(7) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.407(7) . ? C15 C20 1.413(7) . ? C16 C17 1.400(7) . ? C16 C21 1.516(7) . ? C17 C18 1.400(7) . ? C17 C22 1.517(7) . ? C18 C19 1.405(6) . ? C18 C26 1.525(7) . ? C19 C20 1.420(7) . ? C19 C28 1.521(7) . ? C20 C27 1.491(7) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 N3 1.465(5) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? N3 C23 1.347(6) . ? N3 C25 1.373(7) . ? C23 N4 1.327(7) . ? C23 H23 0.9500 . ? N4 C24 1.370(7) . ? C24 C25 1.343(7) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.525(6) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.395(6) . ? C29 C34 1.405(6) . ? C30 C31 1.404(6) . ? C30 C35 1.519(7) . ? C31 C32 1.422(7) . ? C31 C36 1.519(7) . ? C32 C33 1.401(7) . ? C32 C40 1.514(6) . ? C33 C34 1.422(6) . ? C33 C42 1.541(6) . ? C34 C41 1.497(7) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 N5 1.488(6) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? N5 C37 1.347(6) . ? N5 C39 1.369(7) . ? C37 N6 1.340(7) . ? C37 H37 0.9500 . ? N6 C38 1.363(7) . ? C38 C39 1.361(7) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C43 1.532(7) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.401(7) . ? C43 C48 1.407(7) . ? C44 C45 1.407(8) . ? C44 C49 1.500(7) . ? C45 C46 1.409(8) . ? C45 C50 1.517(7) . ? C46 C47 1.394(7) . ? C46 C54 1.513(7) . ? C47 C48 1.407(7) . ? C47 C56 1.540(7) . ? C48 C55 1.498(7) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 N7 1.471(6) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? N7 C51 1.319(6) . ? N7 C53 1.378(7) . ? C51 N8 1.320(7) . ? C51 H51 0.9500 . ? N8 C52 1.371(7) . ? C52 C53 1.356(8) . ? C52 H52 0.9500 . ? C53 H53 0.9500 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C58 1.548(15) . ? C57 Cl1 1.728(9) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 Cl2 1.501(13) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 C59 1.329(19) 2_666 ? C59 Cl3 1.950(12) . ? C59 H59A 0.9900 . ? C59 H59B 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 C2 C1 C6 119.4(4) . . ? C2 C1 C56 120.6(4) . . ? C6 C1 C56 120.0(5) . . ? C1 C2 C3 119.9(4) . . ? C1 C2 C7 120.1(4) . . ? C3 C2 C7 120.0(5) . . ? C4 C3 C2 120.8(5) . . ? C4 C3 C8 120.3(5) . . ? C2 C3 C8 118.9(5) . . ? C5 C4 C3 120.1(4) . . ? C5 C4 C12 122.4(5) . . ? C3 C4 C12 117.5(5) . . ? C4 C5 C6 119.5(4) . . ? C4 C5 C14 121.6(4) . . ? C6 C5 C14 118.8(5) . . ? C1 C6 C5 120.3(5) . . ? C1 C6 C13 120.0(4) . . ? C5 C6 C13 119.5(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 111.6(4) . . ? N1 C8 H8A 109.3 . . ? C3 C8 H8A 109.3 . . ? N1 C8 H8B 109.3 . . ? C3 C8 H8B 109.3 . . ? H8A C8 H8B 108.0 . . ? C11 N1 C9 105.3(5) . . ? C11 N1 C8 124.5(6) . . ? C9 N1 C8 130.0(5) . . ? N1 C9 C10 107.3(6) . . ? N1 C9 H9 126.4 . . ? C10 C9 H9 126.4 . . ? N2 C10 C9 109.5(7) . . ? N2 C10 H10 125.3 . . ? C9 C10 H10 125.3 . . ? C11 N2 C10 104.5(6) . . ? N2 C11 N1 113.4(7) . . ? N2 C11 H11 123.3 . . ? N1 C11 H11 123.3 . . ? 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 117.9(4) . . ? C15 C14 H14A 107.8 . . ? C5 C14 H14A 107.8 . . ? C15 C14 H14B 107.8 . . ? C5 C14 H14B 107.8 . . ? H14A C14 H14B 107.2 . . ? C16 C15 C20 119.7(5) . . ? C16 C15 C14 121.0(4) . . ? C20 C15 C14 119.3(4) . . ? C17 C16 C15 119.6(5) . . ? C17 C16 C21 118.5(4) . . ? C15 C16 C21 121.9(5) . . ? C16 C17 C18 121.2(4) . . ? C16 C17 C22 119.1(4) . . ? C18 C17 C22 119.7(5) . . ? C17 C18 C19 119.9(5) . . ? C17 C18 C26 120.4(4) . . ? C19 C18 C26 119.7(4) . . ? C18 C19 C20 119.3(4) . . ? C18 C19 C28 122.1(5) . . ? C20 C19 C28 118.6(4) . . ? C15 C20 C19 120.1(4) . . ? C15 C20 C27 120.5(5) . . ? C19 C20 C27 119.3(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 . . ? N3 C22 C17 112.9(4) . . ? N3 C22 H22A 109.0 . . ? C17 C22 H22A 109.0 . . ? N3 C22 H22B 109.0 . . ? C17 C22 H22B 109.0 . . ? H22A C22 H22B 107.8 . . ? C23 N3 C25 106.0(4) . . ? C23 N3 C22 125.8(4) . . ? C25 N3 C22 128.1(4) . . ? N4 C23 N3 111.8(5) . . ? N4 C23 H23 124.1 . . ? N3 C23 H23 124.1 . . ? C23 N4 C24 105.1(4) . . ? C25 C24 N4 109.8(5) . . ? C25 C24 H24 125.1 . . ? N4 C24 H24 125.1 . . ? C24 C25 N3 107.3(5) . . ? C24 C25 H25 126.4 . . ? N3 C25 H25 126.4 . . ? C18 C26 H26A 109.5 . . ? C18 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C18 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C20 C27 H27A 109.5 . . ? C20 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C20 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C19 C28 C29 117.8(4) . . ? C19 C28 H28A 107.9 . . ? C29 C28 H28A 107.9 . . ? C19 C28 H28B 107.9 . . ? C29 C28 H28B 107.9 . . ? H28A C28 H28B 107.2 . . ? C30 C29 C34 120.3(4) . . ? C30 C29 C28 120.7(4) . . ? C34 C29 C28 119.0(4) . . ? C29 C30 C31 119.3(4) . . ? C29 C30 C35 121.2(4) . . ? C31 C30 C35 119.5(4) . . ? C30 C31 C32 121.4(4) . . ? C30 C31 C36 120.6(4) . . ? C32 C31 C36 117.9(4) . . ? C33 C32 C31 118.7(4) . . ? C33 C32 C40 122.6(4) . . ? C31 C32 C40 118.7(4) . . ? C32 C33 C34 119.8(4) . . ? C32 C33 C42 121.3(4) . . ? C34 C33 C42 118.9(4) . . ? C29 C34 C33 120.2(4) . . ? C29 C34 C41 120.3(4) . . ? C33 C34 C41 119.4(4) . . ? C30 C35 H35A 109.5 . . ? C30 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C30 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N5 C36 C31 113.3(4) . . ? N5 C36 H36A 108.9 . . ? C31 C36 H36A 108.9 . . ? N5 C36 H36B 108.9 . . ? C31 C36 H36B 108.9 . . ? H36A C36 H36B 107.7 . . ? C37 N5 C39 107.8(4) . . ? C37 N5 C36 124.9(5) . . ? C39 N5 C36 127.2(4) . . ? N6 C37 N5 111.1(5) . . ? N6 C37 H37 124.4 . . ? N5 C37 H37 124.4 . . ? C37 N6 C38 104.5(4) . . ? N6 C38 C39 111.4(5) . . ? N6 C38 H38 124.3 . . ? C39 C38 H38 124.3 . . ? C38 C39 N5 105.1(5) . . ? C38 C39 H39 127.4 . . ? N5 C39 H39 127.4 . . ? C32 C40 H40A 109.5 . . ? C32 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C32 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C34 C41 H41A 109.5 . . ? C34 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C34 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C43 C42 C33 118.3(4) . . ? C43 C42 H42A 107.7 . . ? C33 C42 H42A 107.7 . . ? C43 C42 H42B 107.7 . . ? C33 C42 H42B 107.7 . . ? H42A C42 H42B 107.1 . . ? C44 C43 C48 119.6(5) . . ? C44 C43 C42 121.7(5) . . ? C48 C43 C42 118.5(5) . . ? C43 C44 C45 119.9(5) . . ? C43 C44 C49 122.8(5) . . ? C45 C44 C49 117.3(5) . . ? C44 C45 C46 120.6(5) . . ? C44 C45 C50 120.3(5) . . ? C46 C45 C50 119.1(5) . . ? C47 C46 C45 119.2(5) . . ? C47 C46 C54 121.3(5) . . ? C45 C46 C54 119.5(5) . . ? C46 C47 C48 120.6(5) . . ? C46 C47 C56 120.5(5) . . ? C48 C47 C56 118.9(4) . . ? C47 C48 C43 120.0(5) . . ? C47 C48 C55 119.3(5) . . ? C43 C48 C55 120.6(5) . . ? C44 C49 H49A 109.5 . . ? C44 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C44 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? N7 C50 C45 112.6(4) . . ? N7 C50 H50A 109.1 . . ? C45 C50 H50A 109.1 . . ? N7 C50 H50B 109.1 . . ? C45 C50 H50B 109.1 . . ? H50A C50 H50B 107.8 . . ? C51 N7 C53 105.5(5) . . ? C51 N7 C50 126.2(5) . . ? C53 N7 C50 127.7(5) . . ? N8 C51 N7 114.0(5) . . ? N8 C51 H51 123.0 . . ? N7 C51 H51 123.0 . . ? C51 N8 C52 104.2(5) . . ? C53 C52 N8 109.4(5) . . ? C53 C52 H52 125.3 . . ? N8 C52 H52 125.3 . . ? C52 C53 N7 106.9(5) . . ? C52 C53 H53 126.6 . . ? N7 C53 H53 126.6 . . ? C46 C54 H54A 109.5 . . ? C46 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C46 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C48 C55 H55A 109.5 . . ? C48 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C48 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C1 C56 C47 117.5(4) . . ? C1 C56 H56A 107.9 . . ? C47 C56 H56A 107.9 . . ? C1 C56 H56B 107.9 . . ? C47 C56 H56B 107.9 . . ? H56A C56 H56B 107.2 . . ? C58 C57 Cl1 114.6(8) . . ? C58 C57 H57A 108.6 . . ? Cl1 C57 H57A 108.6 . . ? C58 C57 H57B 108.6 . . ? Cl1 C57 H57B 108.6 . . ? H57A C57 H57B 107.6 . . ? Cl2 C58 C57 116.6(10) . . ? Cl2 C58 H58A 108.1 . . ? C57 C58 H58A 108.1 . . ? Cl2 C58 H58B 108.1 . . ? C57 C58 H58B 108.1 . . ? H58A C58 H58B 107.3 . . ? C59 C59 Cl3 98.7(12) 2_666 . ? C59 C59 H59A 112.0 2_666 . ? Cl3 C59 H59A 112.0 . . ? C59 C59 H59B 112.0 2_666 . ? Cl3 C59 H59B 112.0 . . ? H59A C59 H59B 109.7 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.878 _refine_diff_density_min -0.662 _refine_diff_density_rms 0.088