# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email 'gw@jlu.edu.cn ' _publ_contact_author_name 'Wei Gao' loop_ _publ_author_name 'Wei Gao' 'Bo Gao' 'Xuyang Luo' 'Long Huang' 'Xiaoming Liu' 'Qiaolin Wu' 'Ying Mu' data_Ligand_6 _database_code_depnum_ccdc_archive 'CCDC 835686' #TrackingRef '- combined cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H50 N2 O' _chemical_formula_weight 598.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.962(5) _cell_length_b 15.711(5) _cell_length_c 16.132(5) _cell_angle_alpha 90.00 _cell_angle_beta 106.670(5) _cell_angle_gamma 90.00 _cell_volume 3632.6(19) _cell_formula_units_Z 4 _cell_measurement_temperature 185(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.095 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1296 _exptl_absorpt_coefficient_mu 0.065 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9822 _exptl_absorpt_correction_T_max 0.9866 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 185(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 scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21057 _diffrn_reflns_av_R_equivalents 0.0452 _diffrn_reflns_av_sigmaI/netI 0.0510 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 25.11 _reflns_number_total 6401 _reflns_number_gt 3333 _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^)+(0.1416P)^2^+0.2420P] 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 6401 _refine_ls_number_parameters 389 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1388 _refine_ls_R_factor_gt 0.0740 _refine_ls_wR_factor_ref 0.2608 _refine_ls_wR_factor_gt 0.2158 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8707(2) 0.18623(19) 0.16594(19) 0.0512(7) Uani 1 1 d . . . C2 C 0.8265(2) 0.1987(2) 0.2363(2) 0.0598(9) Uani 1 1 d . . . C3 C 0.7613(3) 0.2638(3) 0.2333(2) 0.0796(11) Uani 1 1 d . . . H3 H 0.7455 0.3020 0.1857 0.096 Uiso 1 1 calc R . . C4 C 0.7201(3) 0.2724(3) 0.2991(3) 0.1009(14) Uani 1 1 d . . . H4 H 0.6754 0.3161 0.2961 0.121 Uiso 1 1 calc R . . C5 C 0.7431(3) 0.2188(4) 0.3684(3) 0.1088(16) Uani 1 1 d . . . H5 H 0.7146 0.2256 0.4136 0.131 Uiso 1 1 calc R . . C6 C 0.8079(3) 0.1545(3) 0.3733(2) 0.0927(13) Uani 1 1 d . . . H6 H 0.8233 0.1176 0.4220 0.111 Uiso 1 1 calc R . . C7 C 0.8510(2) 0.1432(2) 0.3081(2) 0.0662(9) Uani 1 1 d . . . C8 C 0.9222(3) 0.0769(2) 0.31213(19) 0.0660(9) Uani 1 1 d . . . C9 C 0.9353(3) 0.0076(3) 0.3702(2) 0.0908(13) Uani 1 1 d . . . H9 H 0.8949 0.0013 0.4057 0.109 Uiso 1 1 calc R . . C10 C 1.0048(4) -0.0503(3) 0.3764(3) 0.1018(14) Uani 1 1 d . . . H10 H 1.0120 -0.0965 0.4157 0.122 Uiso 1 1 calc R . . C11 C 1.0646(3) -0.0422(3) 0.3259(3) 0.0916(12) Uani 1 1 d . . . H11 H 1.1135 -0.0823 0.3312 0.110 Uiso 1 1 calc R . . C12 C 1.0536(3) 0.0237(2) 0.2680(2) 0.0668(9) Uani 1 1 d . . . H12 H 1.0951 0.0292 0.2334 0.080 Uiso 1 1 calc R . . C13 C 0.9820(2) 0.0822(2) 0.25968(18) 0.0552(8) Uani 1 1 d . . . C14 C 0.9683(2) 0.15156(18) 0.19444(17) 0.0498(7) Uani 1 1 d . . . C15 C 0.7373(2) 0.2116(2) 0.04800(19) 0.0561(8) Uani 1 1 d . . . C16 C 0.7130(2) 0.2884(2) 0.0030(2) 0.0661(9) Uani 1 1 d . . . C17 C 0.6195(3) 0.3047(3) -0.0356(3) 0.0846(12) Uani 1 1 d . . . H17 H 0.6017 0.3574 -0.0644 0.102 Uiso 1 1 calc R . . C18 C 0.5519(3) 0.2468(3) -0.0333(3) 0.0927(13) Uani 1 1 d . . . H18 H 0.4880 0.2594 -0.0596 0.111 Uiso 1 1 calc R . . C19 C 0.5776(3) 0.1703(3) 0.0075(3) 0.0822(11) Uani 1 1 d . . . H19 H 0.5305 0.1296 0.0072 0.099 Uiso 1 1 calc R . . C20 C 0.6701(2) 0.1501(2) 0.0492(2) 0.0619(9) Uani 1 1 d . . . C21 C 0.7873(3) 0.3522(2) -0.0032(3) 0.0778(11) Uani 1 1 d . . . H21 H 0.8496 0.3283 0.0287 0.093 Uiso 1 1 calc R . . C22 C 0.7763(4) 0.4380(3) 0.0376(4) 0.1302(18) Uani 1 1 d . . . H22A H 0.7169 0.4639 0.0056 0.195 Uiso 1 1 calc R . . H22B H 0.8278 0.4756 0.0352 0.195 Uiso 1 1 calc R . . H22C H 0.7773 0.4294 0.0980 0.195 Uiso 1 1 calc R . . C23 C 0.7854(4) 0.3648(3) -0.0976(3) 0.1185(17) Uani 1 1 d . . . H23A H 0.7233 0.3839 -0.1312 0.178 Uiso 1 1 calc R . . H23B H 0.8000 0.3107 -0.1212 0.178 Uiso 1 1 calc R . . H23C H 0.8319 0.4076 -0.1010 0.178 Uiso 1 1 calc R . . C24 C 0.6942(2) 0.0627(2) 0.0894(2) 0.0740(10) Uani 1 1 d . . . H24 H 0.7627 0.0621 0.1191 0.089 Uiso 1 1 calc R . . C25 C 0.6750(4) -0.0062(3) 0.0196(3) 0.1097(15) Uani 1 1 d . . . H25A H 0.6080 -0.0079 -0.0104 0.165 Uiso 1 1 calc R . . H25B H 0.6950 -0.0615 0.0465 0.165 Uiso 1 1 calc R . . H25C H 0.7096 0.0068 -0.0220 0.165 Uiso 1 1 calc R . . C26 C 0.6445(3) 0.0420(3) 0.1575(3) 0.1086(15) Uani 1 1 d . . . H26A H 0.6572 0.0870 0.2014 0.163 Uiso 1 1 calc R . . H26B H 0.6672 -0.0125 0.1849 0.163 Uiso 1 1 calc R . . H26C H 0.5771 0.0384 0.1297 0.163 Uiso 1 1 calc R . . C27 C 1.0322(2) 0.23934(19) 0.10520(19) 0.0518(8) Uani 1 1 d . . . C28 C 1.0207(2) 0.2194(2) 0.0179(2) 0.0579(8) Uani 1 1 d . . . C29 C 1.0273(2) 0.2853(2) -0.0376(2) 0.0709(10) Uani 1 1 d . . . H29 H 1.0181 0.2733 -0.0972 0.085 Uiso 1 1 calc R . . C30 C 1.0467(3) 0.3668(3) -0.0089(3) 0.0851(12) Uani 1 1 d . . . H30 H 1.0520 0.4106 -0.0478 0.102 Uiso 1 1 calc R . . C31 C 1.0584(3) 0.3849(2) 0.0767(3) 0.0839(11) Uani 1 1 d . . . H31 H 1.0706 0.4420 0.0960 0.101 Uiso 1 1 calc R . . C32 C 1.0530(2) 0.3225(2) 0.1363(2) 0.0692(9) Uani 1 1 d . . . C33 C 1.0021(3) 0.1296(2) -0.0156(2) 0.0660(9) Uani 1 1 d . . . H33 H 0.9991 0.0927 0.0340 0.079 Uiso 1 1 calc R . . C34 C 0.9086(3) 0.1219(3) -0.0852(3) 0.0977(14) Uani 1 1 d . . . H34A H 0.8585 0.1414 -0.0618 0.147 Uiso 1 1 calc R . . H34B H 0.8977 0.0624 -0.1034 0.147 Uiso 1 1 calc R . . H34C H 0.9095 0.1571 -0.1351 0.147 Uiso 1 1 calc R . . C35 C 1.0798(3) 0.0956(3) -0.0497(3) 0.1105(16) Uani 1 1 d . . . H35A H 1.0858 0.1316 -0.0975 0.166 Uiso 1 1 calc R . . H35B H 1.0652 0.0372 -0.0705 0.166 Uiso 1 1 calc R . . H35C H 1.1387 0.0961 -0.0032 0.166 Uiso 1 1 calc R . . C36 C 1.0710(3) 0.3433(3) 0.2326(3) 0.0924(13) Uani 1 1 d . . . H36 H 1.0671 0.2885 0.2630 0.111 Uiso 1 1 calc R . . C37 C 0.9999(4) 0.4007(4) 0.2486(3) 0.144(2) Uani 1 1 d . . . H37A H 1.0073 0.4037 0.3109 0.216 Uiso 1 1 calc R . . H37B H 0.9376 0.3790 0.2187 0.216 Uiso 1 1 calc R . . H37C H 1.0074 0.4577 0.2268 0.216 Uiso 1 1 calc R . . C38 C 1.1673(4) 0.3790(5) 0.2724(4) 0.183(3) Uani 1 1 d . . . H38A H 1.1783 0.4264 0.2371 0.274 Uiso 1 1 calc R . . H38B H 1.2139 0.3344 0.2751 0.274 Uiso 1 1 calc R . . H38C H 1.1725 0.3993 0.3310 0.274 Uiso 1 1 calc R . . C39 C 0.2840(6) 0.2319(5) 0.1124(5) 0.173(3) Uiso 1 1 d . . . H39A H 0.2444 0.2129 0.0551 0.208 Uiso 1 1 calc R . . H39B H 0.2518 0.2794 0.1322 0.208 Uiso 1 1 calc R . . C40 C 0.2980(6) 0.1620(5) 0.1737(5) 0.179(3) Uiso 1 1 d . . . H40A H 0.2667 0.1099 0.1450 0.215 Uiso 1 1 calc R . . H40B H 0.2724 0.1765 0.2221 0.215 Uiso 1 1 calc R . . C41 C 0.4001(6) 0.1488(5) 0.2058(5) 0.187(3) Uiso 1 1 d . . . H41A H 0.4205 0.1470 0.2699 0.225 Uiso 1 1 calc R . . H41B H 0.4176 0.0945 0.1836 0.225 Uiso 1 1 calc R . . C42 C 0.4424(6) 0.2178(5) 0.1757(5) 0.182(3) Uiso 1 1 d . . . H42A H 0.4941 0.1973 0.1540 0.219 Uiso 1 1 calc R . . H42B H 0.4682 0.2587 0.2233 0.219 Uiso 1 1 calc R . . N1 N 0.83396(17) 0.19358(15) 0.08485(16) 0.0532(6) Uani 1 1 d . . . N2 N 1.03609(17) 0.17230(16) 0.16544(15) 0.0543(7) Uani 1 1 d . . . O1 O 0.3704(4) 0.2594(3) 0.1055(4) 0.1920(19) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0457(18) 0.0582(18) 0.0509(18) -0.0028(14) 0.0160(14) -0.0046(14) C2 0.0456(19) 0.083(2) 0.0540(19) -0.0115(17) 0.0194(15) -0.0075(17) C3 0.065(2) 0.108(3) 0.070(2) -0.019(2) 0.0268(19) 0.001(2) C4 0.080(3) 0.141(4) 0.090(3) -0.032(3) 0.038(3) 0.014(3) C5 0.088(3) 0.173(5) 0.078(3) -0.030(3) 0.046(3) -0.007(3) C6 0.081(3) 0.144(4) 0.059(2) -0.004(2) 0.029(2) -0.017(3) C7 0.057(2) 0.096(3) 0.0492(18) -0.0098(18) 0.0196(16) -0.0168(19) C8 0.066(2) 0.083(2) 0.0439(17) -0.0012(17) 0.0089(16) -0.0194(19) C9 0.096(3) 0.110(3) 0.064(2) 0.014(2) 0.020(2) -0.026(3) C10 0.124(4) 0.094(3) 0.080(3) 0.029(2) 0.017(3) 0.000(3) C11 0.109(4) 0.080(3) 0.077(3) 0.010(2) 0.012(2) 0.008(2) C12 0.074(3) 0.065(2) 0.0561(19) 0.0031(17) 0.0095(17) 0.0029(18) C13 0.056(2) 0.063(2) 0.0427(16) -0.0037(14) 0.0080(15) -0.0121(16) C14 0.0488(19) 0.0580(18) 0.0414(15) -0.0085(14) 0.0109(14) -0.0029(14) C15 0.0444(19) 0.074(2) 0.0491(17) 0.0026(15) 0.0125(14) 0.0059(16) C16 0.054(2) 0.080(2) 0.064(2) 0.0095(18) 0.0156(17) 0.0123(18) C17 0.061(3) 0.104(3) 0.085(3) 0.025(2) 0.015(2) 0.018(2) C18 0.050(2) 0.116(3) 0.101(3) 0.018(3) 0.004(2) 0.016(2) C19 0.051(2) 0.100(3) 0.089(3) 0.003(2) 0.011(2) -0.007(2) C20 0.047(2) 0.077(2) 0.0597(19) 0.0021(16) 0.0118(16) 0.0013(17) C21 0.070(3) 0.077(2) 0.091(3) 0.019(2) 0.029(2) 0.0109(19) C22 0.140(5) 0.095(4) 0.173(5) -0.009(3) 0.072(4) -0.016(3) C23 0.107(4) 0.147(4) 0.114(4) 0.041(3) 0.052(3) 0.011(3) C24 0.051(2) 0.086(3) 0.079(2) 0.002(2) 0.0103(18) -0.0105(18) C25 0.104(4) 0.088(3) 0.128(4) -0.016(3) 0.019(3) 0.000(3) C26 0.094(3) 0.119(4) 0.119(4) 0.035(3) 0.041(3) -0.011(3) C27 0.0403(17) 0.0586(19) 0.0585(18) 0.0001(15) 0.0176(14) -0.0009(14) C28 0.0480(19) 0.069(2) 0.0573(19) 0.0025(16) 0.0158(15) -0.0060(15) C29 0.069(2) 0.078(3) 0.070(2) 0.009(2) 0.0275(18) -0.0063(19) C30 0.089(3) 0.073(3) 0.097(3) 0.022(2) 0.033(2) -0.006(2) C31 0.091(3) 0.055(2) 0.106(3) -0.002(2) 0.029(2) -0.007(2) C32 0.069(2) 0.061(2) 0.079(2) -0.0062(19) 0.0222(19) 0.0025(17) C33 0.073(2) 0.068(2) 0.0574(19) -0.0030(16) 0.0196(18) -0.0131(18) C34 0.082(3) 0.118(3) 0.090(3) -0.035(2) 0.020(2) -0.017(2) C35 0.087(3) 0.089(3) 0.159(4) -0.026(3) 0.041(3) 0.006(2) C36 0.118(4) 0.073(3) 0.087(3) -0.025(2) 0.030(3) -0.005(2) C37 0.132(5) 0.183(5) 0.122(4) -0.056(4) 0.042(4) 0.022(4) C38 0.099(4) 0.303(9) 0.122(5) -0.085(5) -0.008(4) 0.035(5) N1 0.0440(15) 0.0635(16) 0.0518(15) 0.0018(12) 0.0133(12) 0.0004(12) N2 0.0474(16) 0.0638(16) 0.0540(15) 0.0018(12) 0.0182(12) 0.0000(12) _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 N1 1.270(3) . ? C1 C2 1.481(4) . ? C1 C14 1.501(4) . ? C2 C3 1.404(5) . ? C2 C7 1.412(5) . ? C3 C4 1.379(5) . ? C3 H3 0.9500 . ? C4 C5 1.362(6) . ? C4 H4 0.9500 . ? C5 C6 1.387(6) . ? C5 H5 0.9500 . ? C6 C7 1.394(5) . ? C6 H6 0.9500 . ? C7 C8 1.478(5) . ? C8 C13 1.399(4) . ? C8 C9 1.412(5) . ? C9 C10 1.364(6) . ? C9 H9 0.9500 . ? C10 C11 1.377(6) . ? C10 H10 0.9500 . ? C11 C12 1.372(5) . ? C11 H11 0.9500 . ? C12 C13 1.389(4) . ? C12 H12 0.9500 . ? C13 C14 1.488(4) . ? C14 N2 1.276(4) . ? C15 C20 1.399(4) . ? C15 C16 1.401(4) . ? C15 N1 1.426(4) . ? C16 C17 1.382(5) . ? C16 C21 1.521(5) . ? C17 C18 1.369(6) . ? C17 H17 0.9500 . ? C18 C19 1.370(5) . ? C18 H18 0.9500 . ? C19 C20 1.390(5) . ? C19 H19 0.9500 . ? C20 C24 1.517(5) . ? C21 C22 1.528(6) . ? C21 C23 1.528(6) . ? C21 H21 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.527(5) . ? C24 C26 1.527(5) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C32 1.402(4) . ? C27 C28 1.404(4) . ? C27 N2 1.423(4) . ? C28 C29 1.391(4) . ? C28 C33 1.509(4) . ? C29 C30 1.364(5) . ? C29 H29 0.9500 . ? C30 C31 1.371(5) . ? C30 H30 0.9500 . ? C31 C32 1.392(5) . ? C31 H31 0.9500 . ? C32 C36 1.534(5) . ? C33 C35 1.519(5) . ? C33 C34 1.526(5) . ? C33 H33 1.0000 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C37 1.473(6) . ? C36 C38 1.507(7) . ? C36 H36 1.0000 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 O1 1.398(8) . ? C39 C40 1.452(8) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.480(9) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.410(9) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 O1 1.474(8) . ? C42 H42A 0.9900 . ? C42 H42B 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 N1 C1 C2 128.4(3) . . ? N1 C1 C14 116.3(2) . . ? C2 C1 C14 115.0(3) . . ? C3 C2 C7 119.4(3) . . ? C3 C2 C1 121.9(3) . . ? C7 C2 C1 118.7(3) . . ? C4 C3 C2 120.3(4) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C5 C4 C3 120.5(4) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C4 C5 C6 120.3(4) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C7 121.1(4) . . ? C5 C6 H6 119.4 . . ? C7 C6 H6 119.4 . . ? C6 C7 C2 118.3(4) . . ? C6 C7 C8 122.7(3) . . ? C2 C7 C8 119.0(3) . . ? C13 C8 C9 117.1(4) . . ? C13 C8 C7 120.6(3) . . ? C9 C8 C7 122.2(3) . . ? C10 C9 C8 121.4(4) . . ? C10 C9 H9 119.3 . . ? C8 C9 H9 119.3 . . ? C9 C10 C11 120.4(4) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C12 C11 C10 120.0(4) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C13 120.2(4) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C12 C13 C8 120.8(3) . . ? C12 C13 C14 119.9(3) . . ? C8 C13 C14 119.3(3) . . ? N2 C14 C13 118.9(3) . . ? N2 C14 C1 126.9(3) . . ? C13 C14 C1 114.0(3) . . ? C20 C15 C16 121.4(3) . . ? C20 C15 N1 120.3(3) . . ? C16 C15 N1 117.9(3) . . ? C17 C16 C15 118.1(3) . . ? C17 C16 C21 120.8(3) . . ? C15 C16 C21 121.1(3) . . ? C18 C17 C16 121.6(4) . . ? C18 C17 H17 119.2 . . ? C16 C17 H17 119.2 . . ? C19 C18 C17 119.2(4) . . ? C19 C18 H18 120.4 . . ? C17 C18 H18 120.4 . . ? C18 C19 C20 122.4(4) . . ? C18 C19 H19 118.8 . . ? C20 C19 H19 118.8 . . ? C19 C20 C15 117.0(3) . . ? C19 C20 C24 119.7(3) . . ? C15 C20 C24 123.2(3) . . ? C16 C21 C22 112.5(3) . . ? C16 C21 C23 110.2(3) . . ? C22 C21 C23 110.0(4) . . ? C16 C21 H21 108.0 . . ? C22 C21 H21 108.0 . . ? C23 C21 H21 108.0 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C20 C24 C25 110.8(3) . . ? C20 C24 C26 113.2(3) . . ? C25 C24 C26 110.6(4) . . ? C20 C24 H24 107.3 . . ? C25 C24 H24 107.3 . . ? C26 C24 H24 107.3 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C32 C27 C28 121.2(3) . . ? C32 C27 N2 118.9(3) . . ? C28 C27 N2 119.3(3) . . ? C29 C28 C27 118.0(3) . . ? C29 C28 C33 120.4(3) . . ? C27 C28 C33 121.7(3) . . ? C30 C29 C28 121.8(3) . . ? C30 C29 H29 119.1 . . ? C28 C29 H29 119.1 . . ? C29 C30 C31 119.4(3) . . ? C29 C30 H30 120.3 . . ? C31 C30 H30 120.3 . . ? C30 C31 C32 122.2(3) . . ? C30 C31 H31 118.9 . . ? C32 C31 H31 118.9 . . ? C31 C32 C27 117.4(3) . . ? C31 C32 C36 121.4(3) . . ? C27 C32 C36 121.2(3) . . ? C28 C33 C35 112.2(3) . . ? C28 C33 C34 111.9(3) . . ? C35 C33 C34 110.0(3) . . ? C28 C33 H33 107.5 . . ? C35 C33 H33 107.5 . . ? C34 C33 H33 107.5 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C37 C36 C38 110.4(4) . . ? C37 C36 C32 112.5(4) . . ? C38 C36 C32 112.3(4) . . ? C37 C36 H36 107.1 . . ? C38 C36 H36 107.1 . . ? C32 C36 H36 107.1 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O1 C39 C40 109.3(7) . . ? O1 C39 H39A 109.8 . . ? C40 C39 H39A 109.8 . . ? O1 C39 H39B 109.8 . . ? C40 C39 H39B 109.8 . . ? H39A C39 H39B 108.3 . . ? C39 C40 C41 106.1(7) . . ? C39 C40 H40A 110.5 . . ? C41 C40 H40A 110.5 . . ? C39 C40 H40B 110.5 . . ? C41 C40 H40B 110.5 . . ? H40A C40 H40B 108.7 . . ? C42 C41 C40 107.0(7) . . ? C42 C41 H41A 110.3 . . ? C40 C41 H41A 110.3 . . ? C42 C41 H41B 110.3 . . ? C40 C41 H41B 110.3 . . ? H41A C41 H41B 108.6 . . ? C41 C42 O1 107.7(7) . . ? C41 C42 H42A 110.2 . . ? O1 C42 H42A 110.2 . . ? C41 C42 H42B 110.2 . . ? O1 C42 H42B 110.2 . . ? H42A C42 H42B 108.5 . . ? C1 N1 C15 122.3(2) . . ? C14 N2 C27 123.9(3) . . ? C39 O1 C42 106.9(6) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.11 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.354 _refine_diff_density_min -0.371 _refine_diff_density_rms 0.040 #===END data_Complex_1 _database_code_depnum_ccdc_archive 'CCDC 835687' #TrackingRef '- combined cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H33 Cl2 Cr N O3' _chemical_formula_weight 578.47 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' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1315(7) _cell_length_b 10.2073(8) _cell_length_c 13.7621(10) _cell_angle_alpha 72.7880(10) _cell_angle_beta 80.1120(10) _cell_angle_gamma 87.2260(10) _cell_volume 1339.28(17) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.434 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 604 _exptl_absorpt_coefficient_mu 0.660 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7971 _exptl_absorpt_correction_T_max 0.8630 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7031 _diffrn_reflns_av_R_equivalents 0.0134 _diffrn_reflns_av_sigmaI/netI 0.0319 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 26.04 _reflns_number_total 5113 _reflns_number_gt 4074 _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^)+(0.0464P)^2^+1.4133P] 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 5113 _refine_ls_number_parameters 336 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0603 _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.1077 _refine_ls_wR_factor_gt 0.0977 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6508(3) 0.4390(3) 0.3052(2) 0.0192(5) Uani 1 1 d . . . C2 C 0.6810(3) 0.5115(3) 0.3761(2) 0.0212(6) Uani 1 1 d . . . C3 C 0.7899(3) 0.4762(3) 0.4307(2) 0.0262(6) Uani 1 1 d . . . H3 H 0.8476 0.4065 0.4196 0.031 Uiso 1 1 calc R . . C4 C 0.8125(3) 0.5428(3) 0.5001(2) 0.0295(6) Uani 1 1 d . . . H4 H 0.8853 0.5185 0.5347 0.035 Uiso 1 1 calc R . . C5 C 0.7265(3) 0.6464(3) 0.5186(2) 0.0299(7) Uani 1 1 d . . . H5 H 0.7415 0.6913 0.5654 0.036 Uiso 1 1 calc R . . C6 C 0.6194(3) 0.6819(3) 0.4673(2) 0.0259(6) Uani 1 1 d . . . H6 H 0.5621 0.7507 0.4806 0.031 Uiso 1 1 calc R . . C7 C 0.5938(3) 0.6170(3) 0.3952(2) 0.0216(6) Uani 1 1 d . . . C8 C 0.4769(3) 0.6566(3) 0.3426(2) 0.0215(6) Uani 1 1 d . . . C9 C 0.3903(3) 0.7640(3) 0.3565(2) 0.0276(6) Uani 1 1 d . . . H9 H 0.4077 0.8140 0.3995 0.033 Uiso 1 1 calc R . . C10 C 0.2806(3) 0.7961(3) 0.3078(2) 0.0329(7) Uani 1 1 d . . . H10 H 0.2240 0.8664 0.3192 0.039 Uiso 1 1 calc R . . C11 C 0.2529(3) 0.7252(3) 0.2417(2) 0.0319(7) Uani 1 1 d . . . H11 H 0.1786 0.7482 0.2087 0.038 Uiso 1 1 calc R . . C12 C 0.3360(3) 0.6207(3) 0.2254(2) 0.0267(6) Uani 1 1 d . . . H12 H 0.3180 0.5731 0.1810 0.032 Uiso 1 1 calc R . . C13 C 0.4478(3) 0.5855(3) 0.2755(2) 0.0213(6) Uani 1 1 d . . . C14 C 0.5346(3) 0.4758(3) 0.2586(2) 0.0200(5) Uani 1 1 d . . . C15 C 0.8568(3) 0.3043(3) 0.2838(2) 0.0228(6) Uani 1 1 d . . . C16 C 0.9577(3) 0.3942(3) 0.2193(2) 0.0296(7) Uani 1 1 d . . . C17 C 1.0902(3) 0.3520(4) 0.2206(3) 0.0399(8) Uani 1 1 d . . . H17 H 1.1581 0.4092 0.1770 0.048 Uiso 1 1 calc R . . C18 C 1.1235(3) 0.2278(4) 0.2847(3) 0.0441(9) Uani 1 1 d . . . H18 H 1.2127 0.2011 0.2832 0.053 Uiso 1 1 calc R . . C19 C 1.0236(3) 0.1435(4) 0.3510(3) 0.0384(8) Uani 1 1 d . . . H19 H 1.0466 0.0609 0.3955 0.046 Uiso 1 1 calc R . . C20 C 0.8881(3) 0.1796(3) 0.3529(2) 0.0282(7) Uani 1 1 d . . . C21 C 0.7843(3) 0.0927(3) 0.4331(2) 0.0366(8) Uani 1 1 d . . . H21A H 0.7810 0.1140 0.4969 0.055 Uiso 1 1 calc R . . H21B H 0.8065 -0.0023 0.4428 0.055 Uiso 1 1 calc R . . H21C H 0.6985 0.1105 0.4112 0.055 Uiso 1 1 calc R . . C22 C 0.9284(3) 0.5347(3) 0.1527(3) 0.0381(8) Uani 1 1 d . . . H22A H 0.8505 0.5307 0.1227 0.057 Uiso 1 1 calc R . . H22B H 1.0036 0.5665 0.0989 0.057 Uiso 1 1 calc R . . H22C H 0.9125 0.5968 0.1940 0.057 Uiso 1 1 calc R . . C23 C 0.4446(3) 0.0702(3) 0.1163(2) 0.0350(7) Uani 1 1 d . . . H23A H 0.4246 0.0202 0.1890 0.042 Uiso 1 1 calc R . . H23B H 0.5086 0.0179 0.0818 0.042 Uiso 1 1 calc R . . C24 C 0.3185(3) 0.0945(4) 0.0691(3) 0.0400(8) Uani 1 1 d . . . H24A H 0.2410 0.1020 0.1194 0.048 Uiso 1 1 calc R . . H24B H 0.3033 0.0214 0.0405 0.048 Uiso 1 1 calc R . . C25 C 0.3480(4) 0.2292(3) -0.0148(3) 0.0443(9) Uani 1 1 d . . . H25A H 0.4004 0.2149 -0.0767 0.053 Uiso 1 1 calc R . . H25B H 0.2659 0.2765 -0.0317 0.053 Uiso 1 1 calc R . . C26 C 0.4267(3) 0.3085(3) 0.0328(2) 0.0317(7) Uani 1 1 d . . . H26A H 0.4896 0.3707 -0.0198 0.038 Uiso 1 1 calc R . . H26B H 0.3674 0.3610 0.0702 0.038 Uiso 1 1 calc R . . C27 C 0.8757(3) 0.0926(3) 0.1202(2) 0.0329(7) Uani 1 1 d . . . H27A H 0.9357 0.1535 0.1342 0.040 Uiso 1 1 calc R . . H27B H 0.8660 0.1259 0.0481 0.040 Uiso 1 1 calc R . . C28 C 0.9294(4) -0.0523(3) 0.1455(3) 0.0485(9) Uani 1 1 d . . . H28A H 0.9138 -0.0965 0.0950 0.058 Uiso 1 1 calc R . . H28B H 1.0247 -0.0529 0.1471 0.058 Uiso 1 1 calc R . . C29 C 0.8531(3) -0.1231(4) 0.2498(3) 0.0441(9) Uani 1 1 d . . . H29A H 0.8947 -0.1079 0.3040 0.053 Uiso 1 1 calc R . . H29B H 0.8470 -0.2209 0.2600 0.053 Uiso 1 1 calc R . . C30 C 0.7177(3) -0.0570(3) 0.2475(3) 0.0326(7) Uani 1 1 d . . . H30A H 0.6622 -0.1010 0.2153 0.039 Uiso 1 1 calc R . . H30B H 0.6726 -0.0626 0.3167 0.039 Uiso 1 1 calc R . . Cl1 Cl 0.74589(7) 0.37717(7) 0.03483(5) 0.02914(17) Uani 1 1 d . . . Cl2 Cl 0.48010(7) 0.12665(7) 0.33678(5) 0.02514(16) Uani 1 1 d . . . Cr1 Cr 0.62146(4) 0.25695(4) 0.19105(3) 0.01857(12) Uani 1 1 d . . . N1 N 0.7192(2) 0.3370(2) 0.27428(17) 0.0199(5) Uani 1 1 d . . . O1 O 0.51027(18) 0.41078(18) 0.19561(14) 0.0223(4) Uani 1 1 d . . . O2 O 0.74471(18) 0.08599(19) 0.18663(15) 0.0241(4) Uani 1 1 d . . . O3 O 0.4974(2) 0.20394(19) 0.10259(15) 0.0264(4) 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 0.0183(13) 0.0161(13) 0.0216(13) -0.0048(10) -0.0008(11) 0.0001(10) C2 0.0203(14) 0.0206(13) 0.0220(14) -0.0075(11) 0.0012(11) -0.0032(10) C3 0.0205(14) 0.0315(16) 0.0291(15) -0.0133(13) -0.0033(12) 0.0017(12) C4 0.0227(15) 0.0390(17) 0.0304(16) -0.0143(13) -0.0069(12) -0.0009(12) C5 0.0330(17) 0.0337(16) 0.0263(15) -0.0146(13) -0.0014(13) -0.0080(13) C6 0.0278(15) 0.0243(15) 0.0259(15) -0.0106(12) 0.0014(12) -0.0020(12) C7 0.0215(14) 0.0193(13) 0.0214(13) -0.0052(11) 0.0031(11) -0.0031(10) C8 0.0206(14) 0.0183(13) 0.0231(14) -0.0050(11) 0.0017(11) -0.0016(10) C9 0.0293(16) 0.0223(14) 0.0318(16) -0.0121(12) 0.0000(13) 0.0026(12) C10 0.0296(16) 0.0269(16) 0.0390(17) -0.0092(13) -0.0007(14) 0.0099(13) C11 0.0273(16) 0.0302(16) 0.0371(17) -0.0063(13) -0.0110(13) 0.0097(13) C12 0.0254(15) 0.0247(15) 0.0305(15) -0.0084(12) -0.0069(12) 0.0042(11) C13 0.0196(13) 0.0168(13) 0.0244(14) -0.0036(11) 0.0000(11) 0.0012(10) C14 0.0193(13) 0.0179(13) 0.0207(13) -0.0034(11) -0.0010(11) -0.0018(10) C15 0.0180(13) 0.0291(15) 0.0267(14) -0.0156(12) -0.0072(11) 0.0063(11) C16 0.0211(15) 0.0366(17) 0.0384(17) -0.0217(14) -0.0059(13) 0.0006(12) C17 0.0212(16) 0.057(2) 0.051(2) -0.0311(18) -0.0044(15) -0.0022(15) C18 0.0186(16) 0.075(3) 0.055(2) -0.042(2) -0.0154(16) 0.0165(16) C19 0.0353(18) 0.052(2) 0.0380(18) -0.0226(16) -0.0209(15) 0.0221(16) C20 0.0294(16) 0.0355(17) 0.0275(15) -0.0182(13) -0.0133(13) 0.0117(13) C21 0.0426(19) 0.0374(18) 0.0299(16) -0.0075(14) -0.0139(15) 0.0120(15) C22 0.0325(17) 0.0337(18) 0.047(2) -0.0143(15) 0.0021(15) -0.0083(14) C23 0.049(2) 0.0247(16) 0.0364(18) -0.0101(13) -0.0181(15) -0.0034(14) C24 0.0347(18) 0.044(2) 0.046(2) -0.0176(16) -0.0113(15) -0.0070(15) C25 0.052(2) 0.0375(19) 0.051(2) -0.0121(16) -0.0324(18) 0.0072(16) C26 0.0355(17) 0.0258(15) 0.0354(17) -0.0052(13) -0.0175(14) 0.0040(13) C27 0.0265(16) 0.0316(17) 0.0360(17) -0.0093(14) 0.0058(13) 0.0032(13) C28 0.0376(19) 0.0342(19) 0.062(2) -0.0072(17) 0.0067(18) 0.0141(15) C29 0.041(2) 0.0318(18) 0.051(2) -0.0049(16) -0.0026(17) 0.0110(15) C30 0.0314(17) 0.0209(15) 0.0403(18) -0.0042(13) -0.0011(14) 0.0033(12) Cl1 0.0280(4) 0.0282(4) 0.0258(4) -0.0014(3) -0.0015(3) 0.0003(3) Cl2 0.0208(3) 0.0287(4) 0.0246(3) -0.0077(3) -0.0009(3) 0.0011(3) Cr1 0.0172(2) 0.0183(2) 0.0210(2) -0.00642(17) -0.00476(17) 0.00304(16) N1 0.0149(11) 0.0223(11) 0.0225(11) -0.0071(9) -0.0032(9) 0.0024(9) O1 0.0212(10) 0.0207(10) 0.0281(10) -0.0093(8) -0.0095(8) 0.0054(8) O2 0.0210(10) 0.0203(10) 0.0277(10) -0.0046(8) -0.0001(8) 0.0025(8) O3 0.0319(11) 0.0179(10) 0.0310(11) -0.0045(8) -0.0144(9) 0.0015(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 C1 N1 1.355(3) . ? C1 C14 1.418(4) . ? C1 C2 1.465(4) . ? C2 C3 1.413(4) . ? C2 C7 1.416(4) . ? C3 C4 1.379(4) . ? C3 H3 0.9300 . ? C4 C5 1.391(4) . ? C4 H4 0.9300 . ? C5 C6 1.370(4) . ? C5 H5 0.9300 . ? C6 C7 1.409(4) . ? C6 H6 0.9300 . ? C7 C8 1.472(4) . ? C8 C13 1.407(4) . ? C8 C9 1.407(4) . ? C9 C10 1.372(4) . ? C9 H9 0.9300 . ? C10 C11 1.389(4) . ? C10 H10 0.9300 . ? C11 C12 1.373(4) . ? C11 H11 0.9300 . ? C12 C13 1.403(4) . ? C12 H12 0.9300 . ? C13 C14 1.439(3) . ? C14 O1 1.298(3) . ? C15 C20 1.404(4) . ? C15 C16 1.404(4) . ? C15 N1 1.437(3) . ? C16 C17 1.391(4) . ? C16 C22 1.504(4) . ? C17 C18 1.377(5) . ? C17 H17 0.9300 . ? C18 C19 1.379(5) . ? C18 H18 0.9300 . ? C19 C20 1.403(4) . ? C19 H19 0.9300 . ? C20 C21 1.491(4) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 O3 1.438(3) . ? C23 C24 1.507(4) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.515(5) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.508(4) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 O3 1.459(3) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 O2 1.468(3) . ? C27 C28 1.513(4) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.496(5) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.500(4) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 O2 1.464(3) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? Cl1 Cr1 2.3183(8) . ? Cl2 Cr1 2.3370(8) . ? Cr1 O1 1.8977(17) . ? Cr1 N1 1.995(2) . ? Cr1 O3 2.0826(19) . ? Cr1 O2 2.1056(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C14 111.5(2) . . ? N1 C1 C2 129.5(2) . . ? C14 C1 C2 119.0(2) . . ? C3 C2 C7 118.2(2) . . ? C3 C2 C1 122.9(2) . . ? C7 C2 C1 118.9(2) . . ? C4 C3 C2 121.5(3) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C3 C4 C5 120.1(3) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C6 C5 C4 119.7(3) . . ? C6 C5 H5 120.2 . . ? C4 C5 H5 120.2 . . ? C5 C6 C7 121.9(3) . . ? C5 C6 H6 119.1 . . ? C7 C6 H6 119.1 . . ? C6 C7 C2 118.7(2) . . ? C6 C7 C8 120.4(2) . . ? C2 C7 C8 120.9(2) . . ? C13 C8 C9 117.3(2) . . ? C13 C8 C7 119.8(2) . . ? C9 C8 C7 122.8(2) . . ? C10 C9 C8 121.2(3) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C9 C10 C11 121.0(3) . . ? C9 C10 H10 119.5 . . ? C11 C10 H10 119.5 . . ? C12 C11 C10 119.5(3) . . ? C12 C11 H11 120.3 . . ? C10 C11 H11 120.3 . . ? C11 C12 C13 120.3(3) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C12 C13 C8 120.7(2) . . ? C12 C13 C14 120.3(2) . . ? C8 C13 C14 119.0(2) . . ? O1 C14 C1 117.9(2) . . ? O1 C14 C13 119.7(2) . . ? C1 C14 C13 122.3(2) . . ? C20 C15 C16 121.3(3) . . ? C20 C15 N1 119.4(3) . . ? C16 C15 N1 119.1(2) . . ? C17 C16 C15 118.0(3) . . ? C17 C16 C22 119.2(3) . . ? C15 C16 C22 122.8(3) . . ? C18 C17 C16 121.8(3) . . ? C18 C17 H17 119.1 . . ? C16 C17 H17 119.1 . . ? C17 C18 C19 119.5(3) . . ? C17 C18 H18 120.3 . . ? C19 C18 H18 120.3 . . ? C18 C19 C20 121.5(3) . . ? C18 C19 H19 119.3 . . ? C20 C19 H19 119.3 . . ? C19 C20 C15 117.8(3) . . ? C19 C20 C21 119.7(3) . . ? C15 C20 C21 122.3(2) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C16 C22 H22A 109.5 . . ? C16 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C16 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O3 C23 C24 105.9(2) . . ? O3 C23 H23A 110.5 . . ? C24 C23 H23A 110.5 . . ? O3 C23 H23B 110.5 . . ? C24 C23 H23B 110.5 . . ? H23A C23 H23B 108.7 . . ? C23 C24 C25 102.6(3) . . ? C23 C24 H24A 111.2 . . ? C25 C24 H24A 111.2 . . ? C23 C24 H24B 111.2 . . ? C25 C24 H24B 111.2 . . ? H24A C24 H24B 109.2 . . ? C26 C25 C24 103.3(3) . . ? C26 C25 H25A 111.1 . . ? C24 C25 H25A 111.1 . . ? C26 C25 H25B 111.1 . . ? C24 C25 H25B 111.1 . . ? H25A C25 H25B 109.1 . . ? O3 C26 C25 104.7(2) . . ? O3 C26 H26A 110.8 . . ? C25 C26 H26A 110.8 . . ? O3 C26 H26B 110.8 . . ? C25 C26 H26B 110.8 . . ? H26A C26 H26B 108.9 . . ? O2 C27 C28 106.0(2) . . ? O2 C27 H27A 110.5 . . ? C28 C27 H27A 110.5 . . ? O2 C27 H27B 110.5 . . ? C28 C27 H27B 110.5 . . ? H27A C27 H27B 108.7 . . ? C29 C28 C27 104.5(3) . . ? C29 C28 H28A 110.8 . . ? C27 C28 H28A 110.8 . . ? C29 C28 H28B 110.8 . . ? C27 C28 H28B 110.8 . . ? H28A C28 H28B 108.9 . . ? C28 C29 C30 103.2(3) . . ? C28 C29 H29A 111.1 . . ? C30 C29 H29A 111.1 . . ? C28 C29 H29B 111.1 . . ? C30 C29 H29B 111.1 . . ? H29A C29 H29B 109.1 . . ? O2 C30 C29 104.8(2) . . ? O2 C30 H30A 110.8 . . ? C29 C30 H30A 110.8 . . ? O2 C30 H30B 110.8 . . ? C29 C30 H30B 110.8 . . ? H30A C30 H30B 108.9 . . ? O1 Cr1 N1 80.77(8) . . ? O1 Cr1 O3 88.98(8) . . ? N1 Cr1 O3 169.73(8) . . ? O1 Cr1 O2 179.77(8) . . ? N1 Cr1 O2 99.10(8) . . ? O3 Cr1 O2 91.15(7) . . ? O1 Cr1 Cl1 91.90(6) . . ? N1 Cr1 Cl1 94.03(7) . . ? O3 Cr1 Cl1 85.68(6) . . ? O2 Cr1 Cl1 88.30(6) . . ? O1 Cr1 Cl2 88.47(6) . . ? N1 Cr1 Cl2 92.88(7) . . ? O3 Cr1 Cl2 87.39(6) . . ? O2 Cr1 Cl2 91.35(6) . . ? Cl1 Cr1 Cl2 173.06(3) . . ? C1 N1 C15 124.1(2) . . ? C1 N1 Cr1 113.21(17) . . ? C15 N1 Cr1 121.84(16) . . ? C14 O1 Cr1 115.29(16) . . ? C30 O2 C27 108.3(2) . . ? C30 O2 Cr1 127.23(16) . . ? C27 O2 Cr1 124.42(16) . . ? C23 O3 C26 110.1(2) . . ? C23 O3 Cr1 127.22(16) . . ? C26 O3 Cr1 121.15(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -4.2(5) . . . . ? C14 C1 C2 C3 176.0(3) . . . . ? N1 C1 C2 C7 179.2(3) . . . . ? C14 C1 C2 C7 -0.6(4) . . . . ? C7 C2 C3 C4 -0.7(4) . . . . ? C1 C2 C3 C4 -177.3(3) . . . . ? C2 C3 C4 C5 0.7(5) . . . . ? C3 C4 C5 C6 -0.1(5) . . . . ? C4 C5 C6 C7 -0.5(5) . . . . ? C5 C6 C7 C2 0.5(4) . . . . ? C5 C6 C7 C8 179.2(3) . . . . ? C3 C2 C7 C6 0.1(4) . . . . ? C1 C2 C7 C6 176.9(2) . . . . ? C3 C2 C7 C8 -178.7(3) . . . . ? C1 C2 C7 C8 -1.9(4) . . . . ? C6 C7 C8 C13 -176.2(3) . . . . ? C2 C7 C8 C13 2.6(4) . . . . ? C6 C7 C8 C9 3.5(4) . . . . ? C2 C7 C8 C9 -177.7(3) . . . . ? C13 C8 C9 C10 1.1(4) . . . . ? C7 C8 C9 C10 -178.6(3) . . . . ? C8 C9 C10 C11 -1.2(5) . . . . ? C9 C10 C11 C12 0.5(5) . . . . ? C10 C11 C12 C13 0.2(5) . . . . ? C11 C12 C13 C8 -0.2(4) . . . . ? C11 C12 C13 C14 179.8(3) . . . . ? C9 C8 C13 C12 -0.4(4) . . . . ? C7 C8 C13 C12 179.3(3) . . . . ? C9 C8 C13 C14 179.5(2) . . . . ? C7 C8 C13 C14 -0.7(4) . . . . ? N1 C1 C14 O1 -0.2(4) . . . . ? C2 C1 C14 O1 179.6(2) . . . . ? N1 C1 C14 C13 -177.3(2) . . . . ? C2 C1 C14 C13 2.5(4) . . . . ? C12 C13 C14 O1 1.1(4) . . . . ? C8 C13 C14 O1 -178.9(2) . . . . ? C12 C13 C14 C1 178.2(3) . . . . ? C8 C13 C14 C1 -1.8(4) . . . . ? C20 C15 C16 C17 4.3(4) . . . . ? N1 C15 C16 C17 -171.8(3) . . . . ? C20 C15 C16 C22 -173.4(3) . . . . ? N1 C15 C16 C22 10.5(4) . . . . ? C15 C16 C17 C18 -1.8(5) . . . . ? C22 C16 C17 C18 176.0(3) . . . . ? C16 C17 C18 C19 -1.2(5) . . . . ? C17 C18 C19 C20 1.7(5) . . . . ? C18 C19 C20 C15 0.8(4) . . . . ? C18 C19 C20 C21 -173.7(3) . . . . ? C16 C15 C20 C19 -3.8(4) . . . . ? N1 C15 C20 C19 172.3(2) . . . . ? C16 C15 C20 C21 170.4(3) . . . . ? N1 C15 C20 C21 -13.4(4) . . . . ? O3 C23 C24 C25 29.4(3) . . . . ? C23 C24 C25 C26 -36.4(3) . . . . ? C24 C25 C26 O3 30.3(3) . . . . ? O2 C27 C28 C29 -20.5(4) . . . . ? C27 C28 C29 C30 34.1(4) . . . . ? C28 C29 C30 O2 -35.3(3) . . . . ? C14 C1 N1 C15 161.7(2) . . . . ? C2 C1 N1 C15 -18.1(4) . . . . ? C14 C1 N1 Cr1 -8.0(3) . . . . ? C2 C1 N1 Cr1 172.3(2) . . . . ? C20 C15 N1 C1 112.1(3) . . . . ? C16 C15 N1 C1 -71.7(3) . . . . ? C20 C15 N1 Cr1 -79.1(3) . . . . ? C16 C15 N1 Cr1 97.1(3) . . . . ? O1 Cr1 N1 C1 9.94(18) . . . . ? O3 Cr1 N1 C1 13.2(6) . . . . ? O2 Cr1 N1 C1 -169.87(18) . . . . ? Cl1 Cr1 N1 C1 101.21(18) . . . . ? Cl2 Cr1 N1 C1 -78.04(18) . . . . ? O1 Cr1 N1 C15 -160.0(2) . . . . ? O3 Cr1 N1 C15 -156.7(4) . . . . ? O2 Cr1 N1 C15 20.2(2) . . . . ? Cl1 Cr1 N1 C15 -68.7(2) . . . . ? Cl2 Cr1 N1 C15 112.0(2) . . . . ? C1 C14 O1 Cr1 8.8(3) . . . . ? C13 C14 O1 Cr1 -173.95(19) . . . . ? N1 Cr1 O1 C14 -10.12(18) . . . . ? O3 Cr1 O1 C14 170.47(19) . . . . ? O2 Cr1 O1 C14 47(20) . . . . ? Cl1 Cr1 O1 C14 -103.89(18) . . . . ? Cl2 Cr1 O1 C14 83.05(18) . . . . ? C29 C30 O2 C27 23.1(3) . . . . ? C29 C30 O2 Cr1 -156.6(2) . . . . ? C28 C27 O2 C30 -1.6(3) . . . . ? C28 C27 O2 Cr1 178.0(2) . . . . ? O1 Cr1 O2 C30 46(20) . . . . ? N1 Cr1 O2 C30 102.8(2) . . . . ? O3 Cr1 O2 C30 -77.7(2) . . . . ? Cl1 Cr1 O2 C30 -163.4(2) . . . . ? Cl2 Cr1 O2 C30 9.7(2) . . . . ? O1 Cr1 O2 C27 -134(47) . . . . ? N1 Cr1 O2 C27 -76.7(2) . . . . ? O3 Cr1 O2 C27 102.7(2) . . . . ? Cl1 Cr1 O2 C27 17.1(2) . . . . ? Cl2 Cr1 O2 C27 -169.9(2) . . . . ? C24 C23 O3 C26 -10.9(3) . . . . ? C24 C23 O3 Cr1 155.1(2) . . . . ? C25 C26 O3 C23 -12.3(3) . . . . ? C25 C26 O3 Cr1 -179.3(2) . . . . ? O1 Cr1 O3 C23 -133.8(2) . . . . ? N1 Cr1 O3 C23 -137.0(5) . . . . ? O2 Cr1 O3 C23 46.0(2) . . . . ? Cl1 Cr1 O3 C23 134.2(2) . . . . ? Cl2 Cr1 O3 C23 -45.3(2) . . . . ? O1 Cr1 O3 C26 30.8(2) . . . . ? N1 Cr1 O3 C26 27.6(6) . . . . ? O2 Cr1 O3 C26 -149.4(2) . . . . ? Cl1 Cr1 O3 C26 -61.2(2) . . . . ? Cl2 Cr1 O3 C26 119.3(2) . . . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 26.04 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 0.489 _refine_diff_density_min -0.346 _refine_diff_density_rms 0.066 #===END data_Complex_3 _database_code_depnum_ccdc_archive 'CCDC 835688' #TrackingRef '- combined cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H49 Cl2 Cr N O4' _chemical_formula_weight 706.68 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' 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' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 20.3272(15) _cell_length_b 15.4329(11) _cell_length_c 11.7029(9) _cell_angle_alpha 90.00 _cell_angle_beta 104.2640(10) _cell_angle_gamma 90.00 _cell_volume 3558.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.319 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 0.512 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8870 _exptl_absorpt_correction_T_max 0.9272 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21976 _diffrn_reflns_av_R_equivalents 0.0298 _diffrn_reflns_av_sigmaI/netI 0.0331 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 26.04 _reflns_number_total 7005 _reflns_number_gt 4864 _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^)+(0.1487P)^2^+1.6351P] 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 7005 _refine_ls_number_parameters 394 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0961 _refine_ls_R_factor_gt 0.0702 _refine_ls_wR_factor_ref 0.2349 _refine_ls_wR_factor_gt 0.2097 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.010 _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 C1 C 0.30357(18) 0.49866(18) 0.4192(3) 0.0302(7) Uani 1 1 d . . . C2 C 0.3458(2) 0.4976(2) 0.5364(3) 0.0354(8) Uani 1 1 d . . . C3 C 0.4163(2) 0.5013(3) 0.5568(4) 0.0523(11) Uani 1 1 d . . . H3 H 0.4360 0.5040 0.4931 0.063 Uiso 1 1 calc R . . C4 C 0.4572(3) 0.5010(3) 0.6697(5) 0.0662(14) Uani 1 1 d . . . H45 H 0.5042 0.5028 0.6824 0.079 Uiso 1 1 calc R . . C5 C 0.4271(3) 0.4981(3) 0.7652(4) 0.0581(12) Uani 1 1 d . . . H5 H 0.4544 0.4980 0.8418 0.070 Uiso 1 1 calc R . . C6 C 0.3590(3) 0.4952(2) 0.7474(4) 0.0483(10) Uani 1 1 d . . . H6 H 0.3403 0.4937 0.8123 0.058 Uiso 1 1 calc R . . C7 C 0.3149(2) 0.4945(2) 0.6321(3) 0.0359(8) Uani 1 1 d . . . C8 C 0.2415(2) 0.4906(2) 0.6088(3) 0.0403(9) Uani 1 1 d . . . C9 C 0.2103(3) 0.4872(3) 0.7040(4) 0.0582(12) Uani 1 1 d . . . H9 H 0.2375 0.4887 0.7805 0.070 Uiso 1 1 calc R . . C10 C 0.1426(3) 0.4818(4) 0.6879(4) 0.0788(17) Uani 1 1 d . . . H10 H 0.1238 0.4789 0.7526 0.095 Uiso 1 1 calc R . . C11 C 0.1006(3) 0.4805(4) 0.5736(4) 0.0770(17) Uani 1 1 d . . . H11 H 0.0537 0.4769 0.5623 0.092 Uiso 1 1 calc R . . C12 C 0.1283(2) 0.4845(3) 0.4789(4) 0.0624(13) Uani 1 1 d . . . H12 H 0.0996 0.4831 0.4034 0.075 Uiso 1 1 calc R . . C13 C 0.1990(2) 0.4906(2) 0.4915(3) 0.0380(8) Uani 1 1 d . . . C14 C 0.23094(18) 0.4961(2) 0.3929(3) 0.0313(7) Uani 1 1 d . . . C15 C 0.13043(18) 0.4975(2) 0.2272(3) 0.0379(9) Uani 1 1 d . . . C16 C 0.09444(19) 0.5765(3) 0.2097(3) 0.0473(10) Uani 1 1 d . . . C17 C 0.0232(2) 0.5709(4) 0.1662(4) 0.0620(13) Uani 1 1 d . . . H17 H -0.0021 0.6217 0.1551 0.074 Uiso 1 1 calc R . . C18 C -0.0095(2) 0.4937(4) 0.1400(4) 0.0714(17) Uani 1 1 d . . . H18 H -0.0564 0.4922 0.1109 0.086 Uiso 1 1 calc R . . C19 C 0.0268(2) 0.4187(4) 0.1567(4) 0.0608(13) Uani 1 1 d . . . H19 H 0.0038 0.3665 0.1390 0.073 Uiso 1 1 calc R . . C20 C 0.09765(18) 0.4171(3) 0.1993(3) 0.0454(9) Uani 1 1 d . . . C21 C 0.1264(2) 0.6631(3) 0.2371(4) 0.0599(12) Uani 1 1 d . . . H21 H 0.1757 0.6557 0.2513 0.072 Uiso 1 1 calc R . . C22 C 0.1119(3) 0.7026(4) 0.3477(5) 0.0919(19) Uani 1 1 d . . . H22A H 0.0639 0.7116 0.3355 0.138 Uiso 1 1 calc R . . H22B H 0.1351 0.7571 0.3643 0.138 Uiso 1 1 calc R . . H22C H 0.1275 0.6640 0.4131 0.138 Uiso 1 1 calc R . . C23 C 0.1039(4) 0.7252(4) 0.1352(5) 0.098(2) Uani 1 1 d . . . H23A H 0.1172 0.7031 0.0676 0.147 Uiso 1 1 calc R . . H23B H 0.1249 0.7806 0.1564 0.147 Uiso 1 1 calc R . . H23C H 0.0555 0.7314 0.1170 0.147 Uiso 1 1 calc R . . C24 C 0.1338(2) 0.3313(3) 0.2150(4) 0.0555(11) Uani 1 1 d . . . H24 H 0.1827 0.3427 0.2337 0.067 Uiso 1 1 calc R . . C25 C 0.1187(3) 0.2809(4) 0.3170(5) 0.0897(18) Uani 1 1 d . . . H25A H 0.1309 0.3152 0.3875 0.135 Uiso 1 1 calc R . . H25B H 0.1444 0.2281 0.3282 0.135 Uiso 1 1 calc R . . H25C H 0.0711 0.2675 0.2997 0.135 Uiso 1 1 calc R . . C26 C 0.1155(3) 0.2785(4) 0.1019(5) 0.0890(18) Uani 1 1 d . . . H26A H 0.0676 0.2669 0.0814 0.133 Uiso 1 1 calc R . . H26B H 0.1400 0.2248 0.1135 0.133 Uiso 1 1 calc R . . H26C H 0.1273 0.3106 0.0396 0.133 Uiso 1 1 calc R . . C27 C 0.2749(3) 0.6932(3) 0.0780(4) 0.0751(15) Uani 1 1 d . . . H27A H 0.2297 0.6938 0.0260 0.090 Uiso 1 1 calc R . . H27B H 0.3062 0.6705 0.0349 0.090 Uiso 1 1 calc R . . C28 C 0.2952(4) 0.7815(3) 0.1215(6) 0.106(2) Uani 1 1 d . . . H28A H 0.2616 0.8234 0.0822 0.128 Uiso 1 1 calc R . . H28B H 0.3386 0.7966 0.1062 0.128 Uiso 1 1 calc R . . C29 C 0.3004(4) 0.7812(3) 0.2514(6) 0.098(2) Uani 1 1 d . . . H29A H 0.2583 0.8006 0.2682 0.117 Uiso 1 1 calc R . . H29B H 0.3372 0.8181 0.2930 0.117 Uiso 1 1 calc R . . C30 C 0.3145(3) 0.6860(3) 0.2856(5) 0.0761(15) Uani 1 1 d . . . H30A H 0.3626 0.6731 0.3011 0.091 Uiso 1 1 calc R . . H30B H 0.2984 0.6713 0.3546 0.091 Uiso 1 1 calc R . . C31 C 0.2787(3) 0.3318(3) 0.0481(4) 0.0748(15) Uani 1 1 d . . . H31A H 0.3126 0.3570 0.0125 0.090 Uiso 1 1 calc R . . H31B H 0.2345 0.3373 -0.0066 0.090 Uiso 1 1 calc R . . C32 C 0.2948(3) 0.2378(3) 0.0786(6) 0.095(2) Uani 1 1 d . . . H32A H 0.2565 0.2013 0.0423 0.114 Uiso 1 1 calc R . . H32B H 0.3339 0.2194 0.0513 0.114 Uiso 1 1 calc R . . C33 C 0.3094(4) 0.2319(3) 0.2103(6) 0.097(2) Uani 1 1 d . . . H33A H 0.3482 0.1947 0.2411 0.116 Uiso 1 1 calc R . . H33B H 0.2705 0.2091 0.2347 0.116 Uiso 1 1 calc R . . C34 C 0.3244(3) 0.3244(3) 0.2532(5) 0.0708(14) Uani 1 1 d . . . H34A H 0.3137 0.3333 0.3287 0.085 Uiso 1 1 calc R . . H34B H 0.3716 0.3392 0.2602 0.085 Uiso 1 1 calc R . . C41 C 0.4890(9) 0.7912(11) 1.0342(14) 0.250(7) Uiso 1 1 d . . . H41A H 0.4409 0.8047 1.0129 0.300 Uiso 1 1 calc R . . H41B H 0.5117 0.8327 1.0931 0.300 Uiso 1 1 calc R . . C42 C 0.5055(7) 0.7046(9) 0.8896(12) 0.209(5) Uiso 1 1 d . . . H42A H 0.4627 0.6978 0.8313 0.251 Uiso 1 1 calc R . . H42B H 0.5425 0.6891 0.8547 0.251 Uiso 1 1 calc R . . C43 C 0.5139(9) 0.7966(10) 0.9396(15) 0.257(7) Uiso 1 1 d . . . H43A H 0.5613 0.8137 0.9610 0.309 Uiso 1 1 calc R . . H43B H 0.4884 0.8380 0.8832 0.309 Uiso 1 1 calc R . . C44 C 0.4991(9) 0.7061(12) 1.0808(15) 0.255(7) Uiso 1 1 d . . . H44A H 0.5393 0.7035 1.1459 0.306 Uiso 1 1 calc R . . H44B H 0.4602 0.6871 1.1084 0.306 Uiso 1 1 calc R . . Cl1 Cl 0.19385(5) 0.51362(7) -0.00072(8) 0.0522(3) Uani 1 1 d . . . Cl2 Cl 0.36903(5) 0.51393(7) 0.09663(9) 0.0510(3) Uani 1 1 d . . . Cr1 Cr 0.27387(3) 0.50694(3) 0.17490(5) 0.0301(2) Uani 1 1 d . . . N1 N 0.20357(15) 0.49967(16) 0.2756(3) 0.0312(6) Uani 1 1 d . . . O1 O 0.33167(13) 0.50234(13) 0.3306(2) 0.0342(6) Uani 1 1 d . . . O2 O 0.27935(13) 0.37472(16) 0.1602(2) 0.0442(6) Uani 1 1 d . . . O3 O 0.27633(13) 0.63988(16) 0.1818(2) 0.0454(6) Uani 1 1 d . . . O4 O 0.5070(5) 0.6561(11) 0.9896(11) 0.309(7) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0292(17) 0.0349(17) 0.0238(17) 0.0004(13) 0.0015(14) 0.0009(12) C2 0.039(2) 0.0378(18) 0.0245(18) 0.0003(13) -0.0020(15) 0.0005(14) C3 0.037(2) 0.081(3) 0.032(2) 0.0020(18) -0.0045(17) -0.0011(18) C4 0.043(3) 0.095(4) 0.047(3) 0.003(2) -0.015(2) -0.002(2) C5 0.063(3) 0.065(3) 0.032(2) 0.0020(18) -0.017(2) -0.005(2) C6 0.067(3) 0.048(2) 0.023(2) 0.0028(15) -0.0040(19) 0.0005(18) C7 0.046(2) 0.0358(18) 0.0196(18) 0.0007(13) -0.0040(16) 0.0015(14) C8 0.053(2) 0.047(2) 0.0202(18) -0.0020(14) 0.0072(17) 0.0055(16) C9 0.064(3) 0.091(3) 0.020(2) 0.0005(19) 0.010(2) 0.009(2) C10 0.071(4) 0.147(5) 0.024(2) 0.011(3) 0.023(2) 0.021(3) C11 0.042(3) 0.158(5) 0.033(3) 0.008(3) 0.016(2) 0.016(3) C12 0.043(2) 0.119(4) 0.025(2) 0.001(2) 0.0093(18) 0.006(2) C13 0.037(2) 0.056(2) 0.0198(18) 0.0022(15) 0.0050(15) 0.0054(15) C14 0.0317(18) 0.0422(18) 0.0185(17) 0.0010(13) 0.0034(14) 0.0023(13) C15 0.0257(18) 0.074(3) 0.0137(16) 0.0015(15) 0.0048(14) 0.0008(15) C16 0.037(2) 0.082(3) 0.0232(19) -0.0044(18) 0.0081(16) 0.0159(19) C17 0.036(2) 0.119(4) 0.030(2) -0.002(2) 0.0063(18) 0.029(2) C18 0.027(2) 0.152(6) 0.034(3) -0.004(3) 0.0043(19) 0.000(3) C19 0.035(2) 0.114(4) 0.033(2) -0.003(2) 0.0079(18) -0.017(2) C20 0.0320(19) 0.082(3) 0.0224(18) 0.0027(18) 0.0075(15) -0.0127(18) C21 0.050(3) 0.070(3) 0.057(3) 0.000(2) 0.010(2) 0.027(2) C22 0.104(5) 0.099(4) 0.065(4) -0.023(3) 0.006(3) 0.036(3) C23 0.121(5) 0.087(4) 0.085(4) 0.013(3) 0.023(4) 0.027(4) C24 0.046(2) 0.069(3) 0.049(3) 0.003(2) 0.008(2) -0.021(2) C25 0.102(5) 0.094(4) 0.067(4) 0.027(3) 0.010(3) -0.029(3) C26 0.115(5) 0.072(3) 0.070(4) -0.011(3) 0.004(3) -0.013(3) C27 0.094(4) 0.066(3) 0.066(3) 0.034(3) 0.022(3) 0.002(3) C28 0.159(7) 0.057(3) 0.119(6) 0.026(3) 0.063(5) -0.005(4) C29 0.128(6) 0.046(3) 0.106(5) 0.006(3) 0.005(4) -0.019(3) C30 0.088(4) 0.051(3) 0.074(3) 0.000(2) -0.011(3) -0.021(2) C31 0.085(4) 0.075(3) 0.068(3) -0.039(3) 0.026(3) -0.008(3) C32 0.106(5) 0.067(3) 0.110(5) -0.041(3) 0.025(4) 0.006(3) C33 0.106(5) 0.048(3) 0.127(6) -0.014(3) 0.010(4) 0.014(3) C34 0.072(3) 0.052(3) 0.078(4) -0.004(2) -0.003(3) 0.016(2) Cl1 0.0335(5) 0.1016(8) 0.0194(5) -0.0007(4) 0.0025(4) 0.0013(5) Cl2 0.0331(5) 0.0821(7) 0.0416(6) 0.0003(5) 0.0164(4) -0.0033(4) Cr1 0.0250(3) 0.0454(4) 0.0194(3) -0.0007(2) 0.0044(2) 0.0001(2) N1 0.0272(15) 0.0447(16) 0.0205(14) 0.0006(11) 0.0033(12) 0.0000(11) O1 0.0279(13) 0.0460(13) 0.0272(13) 0.0007(10) 0.0041(10) 0.0003(9) O2 0.0445(15) 0.0495(14) 0.0392(15) -0.0101(12) 0.0117(12) -0.0003(11) O3 0.0539(17) 0.0451(14) 0.0372(15) 0.0054(11) 0.0108(12) -0.0001(12) _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 O1 1.302(4) . ? C1 C2 1.428(5) . ? C1 C14 1.433(5) . ? C2 C3 1.395(6) . ? C2 C7 1.413(5) . ? C3 C4 1.377(6) . ? C3 H3 0.9300 . ? C4 C5 1.401(8) . ? C4 H45 0.9300 . ? C5 C6 1.348(7) . ? C5 H5 0.9300 . ? C6 C7 1.425(5) . ? C6 H6 0.9300 . ? C7 C8 1.450(6) . ? C8 C9 1.411(6) . ? C8 C13 1.431(5) . ? C9 C10 1.344(7) . ? C9 H9 0.9300 . ? C10 C11 1.399(7) . ? C10 H10 0.9300 . ? C11 C12 1.364(6) . ? C11 H11 0.9300 . ? C12 C13 1.412(6) . ? C12 H12 0.9300 . ? C13 C14 1.460(5) . ? C14 N1 1.349(5) . ? C15 C20 1.408(5) . ? C15 C16 1.411(5) . ? C15 N1 1.455(4) . ? C16 C17 1.414(6) . ? C16 C21 1.487(6) . ? C17 C18 1.363(7) . ? C17 H17 0.9300 . ? C18 C19 1.360(7) . ? C18 H18 0.9300 . ? C19 C20 1.403(6) . ? C19 H19 0.9300 . ? C20 C24 1.503(6) . ? C21 C23 1.510(7) . ? C21 C22 1.524(6) . ? C21 H21 0.9800 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C25 1.517(6) . ? C24 C26 1.520(6) . ? C24 H24 0.9800 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 O3 1.461(5) . ? C27 C28 1.477(7) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.498(8) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.532(7) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 O3 1.456(5) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 O2 1.467(5) . ? C31 C32 1.510(7) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33 1.499(9) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.519(6) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 O2 1.461(5) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C41 C43 1.33(2) . ? C41 C44 1.418(18) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 O4 1.383(15) . ? C42 C43 1.530(16) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 O4 1.358(16) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? Cl1 Cr1 2.2876(11) . ? Cl2 Cr1 2.3379(10) . ? Cr1 O1 1.911(3) . ? Cr1 O2 2.053(3) . ? Cr1 O3 2.053(3) . ? Cr1 N1 2.067(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C2 119.2(3) . . ? O1 C1 C14 117.5(3) . . ? C2 C1 C14 123.3(3) . . ? C3 C2 C7 120.3(4) . . ? C3 C2 C1 120.8(4) . . ? C7 C2 C1 118.9(3) . . ? C4 C3 C2 121.1(5) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C3 C4 C5 119.1(5) . . ? C3 C4 H45 120.5 . . ? C5 C4 H45 120.5 . . ? C6 C5 C4 120.7(4) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C7 122.0(4) . . ? C5 C6 H6 119.0 . . ? C7 C6 H6 119.0 . . ? C2 C7 C6 116.8(4) . . ? C2 C7 C8 119.3(3) . . ? C6 C7 C8 123.8(4) . . ? C9 C8 C13 118.3(4) . . ? C9 C8 C7 119.7(4) . . ? C13 C8 C7 122.0(3) . . ? C10 C9 C8 122.3(4) . . ? C10 C9 H9 118.8 . . ? C8 C9 H9 118.8 . . ? C9 C10 C11 119.9(4) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C12 C11 C10 119.9(5) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C13 122.1(4) . . ? C11 C12 H12 118.9 . . ? C13 C12 H12 118.9 . . ? C12 C13 C8 117.3(3) . . ? C12 C13 C14 124.1(4) . . ? C8 C13 C14 118.6(4) . . ? N1 C14 C1 111.3(3) . . ? N1 C14 C13 130.9(3) . . ? C1 C14 C13 117.8(3) . . ? C20 C15 C16 122.0(4) . . ? C20 C15 N1 119.4(3) . . ? C16 C15 N1 118.6(3) . . ? C15 C16 C17 116.5(4) . . ? C15 C16 C21 124.2(3) . . ? C17 C16 C21 119.2(4) . . ? C18 C17 C16 122.4(4) . . ? C18 C17 H17 118.8 . . ? C16 C17 H17 118.8 . . ? C19 C18 C17 119.5(4) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C18 C19 C20 122.7(5) . . ? C18 C19 H19 118.7 . . ? C20 C19 H19 118.7 . . ? C19 C20 C15 116.9(4) . . ? C19 C20 C24 119.1(4) . . ? C15 C20 C24 124.0(3) . . ? C16 C21 C23 111.7(4) . . ? C16 C21 C22 112.1(4) . . ? C23 C21 C22 109.4(4) . . ? C16 C21 H21 107.8 . . ? C23 C21 H21 107.8 . . ? C22 C21 H21 107.8 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C20 C24 C25 111.1(4) . . ? C20 C24 C26 111.0(4) . . ? C25 C24 C26 110.9(4) . . ? C20 C24 H24 107.9 . . ? C25 C24 H24 107.9 . . ? C26 C24 H24 107.9 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O3 C27 C28 106.7(4) . . ? O3 C27 H27A 110.4 . . ? C28 C27 H27A 110.4 . . ? O3 C27 H27B 110.4 . . ? C28 C27 H27B 110.4 . . ? H27A C27 H27B 108.6 . . ? C27 C28 C29 106.9(4) . . ? C27 C28 H28A 110.3 . . ? C29 C28 H28A 110.3 . . ? C27 C28 H28B 110.3 . . ? C29 C28 H28B 110.3 . . ? H28A C28 H28B 108.6 . . ? C28 C29 C30 103.2(5) . . ? C28 C29 H29A 111.1 . . ? C30 C29 H29A 111.1 . . ? C28 C29 H29B 111.1 . . ? C30 C29 H29B 111.1 . . ? H29A C29 H29B 109.1 . . ? O3 C30 C29 103.0(4) . . ? O3 C30 H30A 111.2 . . ? C29 C30 H30A 111.2 . . ? O3 C30 H30B 111.2 . . ? C29 C30 H30B 111.2 . . ? H30A C30 H30B 109.1 . . ? O2 C31 C32 105.6(4) . . ? O2 C31 H31A 110.6 . . ? C32 C31 H31A 110.6 . . ? O2 C31 H31B 110.6 . . ? C32 C31 H31B 110.6 . . ? H31A C31 H31B 108.8 . . ? C33 C32 C31 106.1(4) . . ? C33 C32 H32A 110.5 . . ? C31 C32 H32A 110.5 . . ? C33 C32 H32B 110.5 . . ? C31 C32 H32B 110.5 . . ? H32A C32 H32B 108.7 . . ? C32 C33 C34 104.8(5) . . ? C32 C33 H33A 110.8 . . ? C34 C33 H33A 110.8 . . ? C32 C33 H33B 110.8 . . ? C34 C33 H33B 110.8 . . ? H33A C33 H33B 108.9 . . ? O2 C34 C33 102.5(4) . . ? O2 C34 H34A 111.3 . . ? C33 C34 H34A 111.3 . . ? O2 C34 H34B 111.3 . . ? C33 C34 H34B 111.3 . . ? H34A C34 H34B 109.2 . . ? C43 C41 C44 109.3(14) . . ? C43 C41 H41A 109.8 . . ? C44 C41 H41A 109.8 . . ? C43 C41 H41B 109.8 . . ? C44 C41 H41B 109.8 . . ? H41A C41 H41B 108.3 . . ? O4 C42 C43 101.6(14) . . ? O4 C42 H42A 111.4 . . ? C43 C42 H42A 111.4 . . ? O4 C42 H42B 111.4 . . ? C43 C42 H42B 111.4 . . ? H42A C42 H42B 109.3 . . ? C41 C43 C42 103.3(12) . . ? C41 C43 H43A 111.1 . . ? C42 C43 H43A 111.1 . . ? C41 C43 H43B 111.1 . . ? C42 C43 H43B 111.1 . . ? H43A C43 H43B 109.1 . . ? O4 C44 C41 104.9(16) . . ? O4 C44 H44A 110.8 . . ? C41 C44 H44A 110.8 . . ? O4 C44 H44B 110.8 . . ? C41 C44 H44B 110.8 . . ? H44A C44 H44B 108.8 . . ? O1 Cr1 O2 90.55(9) . . ? O1 Cr1 O3 89.80(10) . . ? O2 Cr1 O3 174.29(11) . . ? O1 Cr1 N1 78.66(11) . . ? O2 Cr1 N1 93.05(10) . . ? O3 Cr1 N1 92.61(10) . . ? O1 Cr1 Cl1 172.99(8) . . ? O2 Cr1 Cl1 90.62(8) . . ? O3 Cr1 Cl1 89.73(8) . . ? N1 Cr1 Cl1 94.38(9) . . ? O1 Cr1 Cl2 90.09(8) . . ? O2 Cr1 Cl2 86.89(7) . . ? O3 Cr1 Cl2 87.40(8) . . ? N1 Cr1 Cl2 168.75(9) . . ? Cl1 Cr1 Cl2 96.87(4) . . ? C14 N1 C15 121.4(3) . . ? C14 N1 Cr1 114.4(2) . . ? C15 N1 Cr1 124.2(2) . . ? C1 O1 Cr1 118.3(2) . . ? C34 O2 C31 107.0(3) . . ? C34 O2 Cr1 120.2(2) . . ? C31 O2 Cr1 122.4(3) . . ? C30 O3 C27 108.4(3) . . ? C30 O3 Cr1 121.6(2) . . ? C27 O3 Cr1 122.3(3) . . ? C44 O4 C42 112.1(18) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 0.7(4) . . . . ? C14 C1 C2 C3 -179.2(3) . . . . ? O1 C1 C2 C7 179.4(3) . . . . ? C14 C1 C2 C7 -0.5(4) . . . . ? C7 C2 C3 C4 0.8(6) . . . . ? C1 C2 C3 C4 179.4(3) . . . . ? C2 C3 C4 C5 -0.8(6) . . . . ? C3 C4 C5 C6 0.2(6) . . . . ? C4 C5 C6 C7 0.5(6) . . . . ? C3 C2 C7 C6 -0.1(5) . . . . ? C1 C2 C7 C6 -178.8(3) . . . . ? C3 C2 C7 C8 -180.0(3) . . . . ? C1 C2 C7 C8 1.3(4) . . . . ? C5 C6 C7 C2 -0.5(5) . . . . ? C5 C6 C7 C8 179.4(3) . . . . ? C2 C7 C8 C9 179.8(3) . . . . ? C6 C7 C8 C9 -0.1(5) . . . . ? C2 C7 C8 C13 -0.6(5) . . . . ? C6 C7 C8 C13 179.6(3) . . . . ? C13 C8 C9 C10 1.7(6) . . . . ? C7 C8 C9 C10 -178.6(4) . . . . ? C8 C9 C10 C11 -0.8(8) . . . . ? C9 C10 C11 C12 0.2(8) . . . . ? C10 C11 C12 C13 -0.5(8) . . . . ? C11 C12 C13 C8 1.4(7) . . . . ? C11 C12 C13 C14 -179.2(4) . . . . ? C9 C8 C13 C12 -1.9(5) . . . . ? C7 C8 C13 C12 178.4(3) . . . . ? C9 C8 C13 C14 178.7(3) . . . . ? C7 C8 C13 C14 -1.0(5) . . . . ? O1 C1 C14 N1 -1.2(4) . . . . ? C2 C1 C14 N1 178.7(3) . . . . ? O1 C1 C14 C13 179.1(3) . . . . ? C2 C1 C14 C13 -1.1(4) . . . . ? C12 C13 C14 N1 2.7(6) . . . . ? C8 C13 C14 N1 -177.9(3) . . . . ? C12 C13 C14 C1 -177.6(3) . . . . ? C8 C13 C14 C1 1.8(4) . . . . ? C20 C15 C16 C17 2.0(5) . . . . ? N1 C15 C16 C17 -177.9(3) . . . . ? C20 C15 C16 C21 -179.8(3) . . . . ? N1 C15 C16 C21 0.3(5) . . . . ? C15 C16 C17 C18 -1.2(6) . . . . ? C21 C16 C17 C18 -179.6(4) . . . . ? C16 C17 C18 C19 0.5(7) . . . . ? C17 C18 C19 C20 -0.5(7) . . . . ? C18 C19 C20 C15 1.2(6) . . . . ? C18 C19 C20 C24 180.0(4) . . . . ? C16 C15 C20 C19 -2.0(5) . . . . ? N1 C15 C20 C19 177.9(3) . . . . ? C16 C15 C20 C24 179.3(3) . . . . ? N1 C15 C20 C24 -0.8(5) . . . . ? C15 C16 C21 C23 130.7(4) . . . . ? C17 C16 C21 C23 -51.1(5) . . . . ? C15 C16 C21 C22 -106.1(4) . . . . ? C17 C16 C21 C22 72.1(5) . . . . ? C19 C20 C24 C25 -70.3(5) . . . . ? C15 C20 C24 C25 108.4(4) . . . . ? C19 C20 C24 C26 53.6(5) . . . . ? C15 C20 C24 C26 -127.7(4) . . . . ? O3 C27 C28 C29 -6.7(7) . . . . ? C27 C28 C29 C30 25.1(7) . . . . ? C28 C29 C30 O3 -34.0(6) . . . . ? O2 C31 C32 C33 -4.3(6) . . . . ? C31 C32 C33 C34 -18.3(7) . . . . ? C32 C33 C34 O2 34.0(6) . . . . ? C44 C41 C43 C42 30(2) . . . . ? O4 C42 C43 C41 -27(2) . . . . ? C43 C41 C44 O4 -22(2) . . . . ? C1 C14 N1 C15 179.6(3) . . . . ? C13 C14 N1 C15 -0.7(5) . . . . ? C1 C14 N1 Cr1 0.3(3) . . . . ? C13 C14 N1 Cr1 180.0(3) . . . . ? C20 C15 N1 C14 -89.7(4) . . . . ? C16 C15 N1 C14 90.2(4) . . . . ? C20 C15 N1 Cr1 89.5(3) . . . . ? C16 C15 N1 Cr1 -90.6(3) . . . . ? O1 Cr1 N1 C14 0.4(2) . . . . ? O2 Cr1 N1 C14 90.3(2) . . . . ? O3 Cr1 N1 C14 -88.9(2) . . . . ? Cl1 Cr1 N1 C14 -178.8(2) . . . . ? Cl2 Cr1 N1 C14 0.9(5) . . . . ? O1 Cr1 N1 C15 -178.9(3) . . . . ? O2 Cr1 N1 C15 -89.0(3) . . . . ? O3 Cr1 N1 C15 91.8(3) . . . . ? Cl1 Cr1 N1 C15 1.9(2) . . . . ? Cl2 Cr1 N1 C15 -178.4(3) . . . . ? C2 C1 O1 Cr1 -178.3(2) . . . . ? C14 C1 O1 Cr1 1.6(3) . . . . ? O2 Cr1 O1 C1 -94.1(2) . . . . ? O3 Cr1 O1 C1 91.6(2) . . . . ? N1 Cr1 O1 C1 -1.1(2) . . . . ? Cl1 Cr1 O1 C1 5.5(7) . . . . ? Cl2 Cr1 O1 C1 179.1(2) . . . . ? C33 C34 O2 C31 -37.6(5) . . . . ? C33 C34 O2 Cr1 176.8(3) . . . . ? C32 C31 O2 C34 26.5(5) . . . . ? C32 C31 O2 Cr1 171.2(3) . . . . ? O1 Cr1 O2 C34 -5.6(3) . . . . ? O3 Cr1 O2 C34 87.9(12) . . . . ? N1 Cr1 O2 C34 -84.3(3) . . . . ? Cl1 Cr1 O2 C34 -178.7(3) . . . . ? Cl2 Cr1 O2 C34 84.5(3) . . . . ? O1 Cr1 O2 C31 -145.8(3) . . . . ? O3 Cr1 O2 C31 -52.3(12) . . . . ? N1 Cr1 O2 C31 135.5(3) . . . . ? Cl1 Cr1 O2 C31 41.1(3) . . . . ? Cl2 Cr1 O2 C31 -55.7(3) . . . . ? C29 C30 O3 C27 31.1(6) . . . . ? C29 C30 O3 Cr1 -178.9(3) . . . . ? C28 C27 O3 C30 -15.8(6) . . . . ? C28 C27 O3 Cr1 -165.5(4) . . . . ? O1 Cr1 O3 C30 -0.3(3) . . . . ? O2 Cr1 O3 C30 -93.8(12) . . . . ? N1 Cr1 O3 C30 78.3(3) . . . . ? Cl1 Cr1 O3 C30 172.7(3) . . . . ? Cl2 Cr1 O3 C30 -90.4(3) . . . . ? O1 Cr1 O3 C27 145.6(3) . . . . ? O2 Cr1 O3 C27 52.1(12) . . . . ? N1 Cr1 O3 C27 -135.8(3) . . . . ? Cl1 Cr1 O3 C27 -41.4(3) . . . . ? Cl2 Cr1 O3 C27 55.5(3) . . . . ? C41 C44 O4 C42 2.6(19) . . . . ? C43 C42 O4 C44 14.2(16) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.04 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.906 _refine_diff_density_min -0.688 _refine_diff_density_rms 0.101 #===END data_Complex_4 _database_code_depnum_ccdc_archive 'CCDC 835689' #TrackingRef '- combined cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H65 Cl8 Cr2 N4 O' _chemical_formula_weight 1317.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.7054(8) _cell_length_b 14.9361(8) _cell_length_c 17.9334(10) _cell_angle_alpha 72.4660(10) _cell_angle_beta 66.4290(10) _cell_angle_gamma 65.2780(10) _cell_volume 3236.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 185(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.352 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1362 _exptl_absorpt_coefficient_mu 0.710 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8424 _exptl_absorpt_correction_T_max 0.8652 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 185(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 scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17743 _diffrn_reflns_av_R_equivalents 0.0244 _diffrn_reflns_av_sigmaI/netI 0.0620 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 26.04 _reflns_number_total 12486 _reflns_number_gt 8545 _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^)+(0.1960P)^2^+9.2365P] 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 12486 _refine_ls_number_parameters 720 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1355 _refine_ls_R_factor_gt 0.1018 _refine_ls_wR_factor_ref 0.3197 _refine_ls_wR_factor_gt 0.2863 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2958(5) 0.2666(4) 0.1305(4) 0.0282(14) Uani 1 1 d . . . C2 C 0.2700(5) 0.3301(5) 0.0564(4) 0.0301(14) Uani 1 1 d . . . C3 C 0.3375(6) 0.3778(5) -0.0087(4) 0.0365(16) Uani 1 1 d . . . H3 H 0.4048 0.3667 -0.0060 0.044 Uiso 1 1 calc R . . C4 C 0.3080(7) 0.4397(6) -0.0753(5) 0.0424(18) Uani 1 1 d . . . H4 H 0.3554 0.4696 -0.1183 0.051 Uiso 1 1 calc R . . C5 C 0.2106(7) 0.4589(6) -0.0807(5) 0.0455(19) Uani 1 1 d . . . H5 H 0.1893 0.5040 -0.1257 0.055 Uiso 1 1 calc R . . C6 C 0.1443(6) 0.4118(6) -0.0197(5) 0.0420(18) Uani 1 1 d . . . H6 H 0.0780 0.4236 -0.0246 0.050 Uiso 1 1 calc R . . C7 C 0.1710(6) 0.3466(5) 0.0496(4) 0.0350(16) Uani 1 1 d . . . C8 C 0.1029(5) 0.2926(5) 0.1088(4) 0.0339(15) Uani 1 1 d . . . C9 C 0.0122(6) 0.2971(6) 0.0953(5) 0.0465(19) Uani 1 1 d . . . H9 H -0.0057 0.3390 0.0479 0.056 Uiso 1 1 calc R . . C10 C -0.0495(7) 0.2431(7) 0.1481(6) 0.054(2) Uani 1 1 d . . . H10 H -0.1097 0.2478 0.1373 0.065 Uiso 1 1 calc R . . C11 C -0.0256(6) 0.1812(7) 0.2177(6) 0.050(2) Uani 1 1 d . . . H11 H -0.0697 0.1443 0.2550 0.060 Uiso 1 1 calc R . . C12 C 0.0621(6) 0.1736(6) 0.2322(5) 0.0420(17) Uani 1 1 d . . . H12 H 0.0794 0.1293 0.2790 0.050 Uiso 1 1 calc R . . C13 C 0.1275(5) 0.2301(5) 0.1795(4) 0.0333(15) Uani 1 1 d . . . C14 C 0.2221(5) 0.2219(5) 0.1934(4) 0.0286(14) Uani 1 1 d . . . C15 C 0.4585(5) 0.2978(5) 0.1064(4) 0.0330(15) Uani 1 1 d . . . C16 C 0.5512(6) 0.2517(5) 0.0476(4) 0.0391(17) Uani 1 1 d . . . C17 C 0.6298(6) 0.2963(7) 0.0137(5) 0.054(2) Uani 1 1 d . . . H17 H 0.6948 0.2654 -0.0251 0.065 Uiso 1 1 calc R . . C18 C 0.6146(8) 0.3819(7) 0.0352(6) 0.058(2) Uani 1 1 d . . . H18 H 0.6703 0.4085 0.0135 0.070 Uiso 1 1 calc R . . C19 C 0.5201(7) 0.4309(6) 0.0879(5) 0.052(2) Uani 1 1 d . . . H19 H 0.5097 0.4934 0.0990 0.062 Uiso 1 1 calc R . . C20 C 0.4388(6) 0.3911(5) 0.1256(5) 0.0389(17) Uani 1 1 d . . . C21 C 0.5645(7) 0.1629(6) 0.0183(5) 0.051(2) Uani 1 1 d . . . H21A H 0.5905 0.1024 0.0556 0.076 Uiso 1 1 calc R . . H21B H 0.6154 0.1598 -0.0373 0.076 Uiso 1 1 calc R . . H21C H 0.4965 0.1676 0.0174 0.076 Uiso 1 1 calc R . . C22 C 0.3344(7) 0.4508(5) 0.1766(5) 0.048(2) Uani 1 1 d . . . H22A H 0.3317 0.5197 0.1681 0.072 Uiso 1 1 calc R . . H22B H 0.3242 0.4217 0.2349 0.072 Uiso 1 1 calc R . . H22C H 0.2784 0.4503 0.1602 0.072 Uiso 1 1 calc R . . C23 C 0.1707(5) 0.1654(6) 0.3414(4) 0.0352(15) Uani 1 1 d . . . C24 C 0.1674(6) 0.0699(6) 0.3825(5) 0.0453(19) Uani 1 1 d . . . C25 C 0.0935(7) 0.0627(8) 0.4601(6) 0.059(3) Uani 1 1 d . . . H25 H 0.0919 -0.0013 0.4901 0.070 Uiso 1 1 calc R . . C26 C 0.0230(9) 0.1460(11) 0.4941(6) 0.076(4) Uani 1 1 d . . . H26 H -0.0269 0.1391 0.5472 0.092 Uiso 1 1 calc R . . C27 C 0.0234(7) 0.2402(10) 0.4520(6) 0.070(3) Uani 1 1 d . . . H27 H -0.0279 0.2975 0.4756 0.084 Uiso 1 1 calc R . . C28 C 0.0987(6) 0.2519(6) 0.3748(5) 0.0406(17) Uani 1 1 d . . . C29 C 0.2340(7) -0.0216(6) 0.3429(6) 0.054(2) Uani 1 1 d . . . H29A H 0.2395 -0.0051 0.2844 0.081 Uiso 1 1 calc R . . H29B H 0.2015 -0.0734 0.3702 0.081 Uiso 1 1 calc R . . H29C H 0.3046 -0.0461 0.3481 0.081 Uiso 1 1 calc R . . C30 C 0.0977(6) 0.3554(6) 0.3306(6) 0.051(2) Uani 1 1 d . . . H30A H 0.1506 0.3709 0.3397 0.076 Uiso 1 1 calc R . . H30B H 0.0277 0.4039 0.3519 0.076 Uiso 1 1 calc R . . H30C H 0.1142 0.3586 0.2714 0.076 Uiso 1 1 calc R . . C31 C 0.6929(5) -0.2588(4) 0.2716(4) 0.0275(13) Uani 1 1 d . . . C32 C 0.7256(6) -0.3684(5) 0.2974(4) 0.0310(14) Uani 1 1 d . . . C33 C 0.6616(6) -0.4164(5) 0.3641(5) 0.0401(17) Uani 1 1 d . . . H33 H 0.5950 -0.3772 0.3960 0.048 Uiso 1 1 calc R . . C34 C 0.6935(7) -0.5194(5) 0.3843(5) 0.0454(19) Uani 1 1 d . . . H34 H 0.6483 -0.5501 0.4291 0.054 Uiso 1 1 calc R . . C35 C 0.7896(7) -0.5772(5) 0.3403(6) 0.049(2) Uani 1 1 d . . . H35 H 0.8111 -0.6479 0.3542 0.058 Uiso 1 1 calc R . . C36 C 0.8556(6) -0.5325(5) 0.2753(5) 0.0404(17) Uani 1 1 d . . . H36 H 0.9217 -0.5733 0.2443 0.048 Uiso 1 1 calc R . . C37 C 0.8267(6) -0.4270(5) 0.2538(4) 0.0330(15) Uani 1 1 d . . . C38 C 0.9015(5) -0.3809(5) 0.1911(4) 0.0303(14) Uani 1 1 d . . . C39 C 1.0067(6) -0.4415(5) 0.1527(5) 0.0401(17) Uani 1 1 d . . . H39 H 1.0248 -0.5121 0.1652 0.048 Uiso 1 1 calc R . . C40 C 1.0823(6) -0.4020(5) 0.0986(5) 0.0403(17) Uani 1 1 d . . . H40 H 1.1513 -0.4440 0.0731 0.048 Uiso 1 1 calc R . . C41 C 1.0553(6) -0.2971(5) 0.0817(5) 0.0427(18) Uani 1 1 d . . . H41 H 1.1075 -0.2681 0.0463 0.051 Uiso 1 1 calc R . . C42 C 0.9553(6) -0.2375(5) 0.1156(5) 0.0382(16) Uani 1 1 d . . . H42 H 0.9384 -0.1671 0.1024 0.046 Uiso 1 1 calc R . . C43 C 0.8753(5) -0.2771(5) 0.1702(4) 0.0297(14) Uani 1 1 d . . . C44 C 0.7655(5) -0.2144(5) 0.2078(4) 0.0280(13) Uani 1 1 d . . . C45 C 0.5031(5) -0.2213(5) 0.3475(4) 0.0311(14) Uani 1 1 d . . . C46 C 0.4612(6) -0.2507(5) 0.3040(5) 0.0397(17) Uani 1 1 d . . . C47 C 0.3725(7) -0.2781(6) 0.3491(6) 0.050(2) Uani 1 1 d . . . H47 H 0.3421 -0.2976 0.3215 0.060 Uiso 1 1 calc R . . C48 C 0.3277(7) -0.2779(6) 0.4323(6) 0.052(2) Uani 1 1 d . . . H48 H 0.2668 -0.2968 0.4617 0.062 Uiso 1 1 calc R . . C49 C 0.3709(6) -0.2504(5) 0.4726(5) 0.0451(19) Uani 1 1 d . . . H49 H 0.3392 -0.2506 0.5303 0.054 Uiso 1 1 calc R . . C50 C 0.4594(6) -0.2223(5) 0.4320(4) 0.0347(15) Uani 1 1 d . . . C51 C 0.5098(7) -0.2548(6) 0.2141(5) 0.050(2) Uani 1 1 d . . . H51A H 0.5044 -0.1873 0.1834 0.075 Uiso 1 1 calc R . . H51B H 0.4729 -0.2828 0.1972 0.075 Uiso 1 1 calc R . . H51C H 0.5843 -0.2971 0.2025 0.075 Uiso 1 1 calc R . . C52 C 0.5122(7) -0.2061(6) 0.4815(5) 0.0458(18) Uani 1 1 d . . . H52A H 0.5775 -0.2626 0.4821 0.069 Uiso 1 1 calc R . . H52B H 0.4646 -0.2008 0.5381 0.069 Uiso 1 1 calc R . . H52C H 0.5286 -0.1444 0.4564 0.069 Uiso 1 1 calc R . . C53 C 0.7695(5) -0.0599(5) 0.1096(4) 0.0324(15) Uani 1 1 d . . . C54 C 0.7629(6) -0.0749(5) 0.0387(4) 0.0378(16) Uani 1 1 d . . . C55 C 0.8096(7) -0.0259(7) -0.0367(5) 0.052(2) Uani 1 1 d . . . H55 H 0.8070 -0.0357 -0.0856 0.062 Uiso 1 1 calc R . . C56 C 0.8606(7) 0.0375(7) -0.0423(6) 0.060(3) Uani 1 1 d . . . H56 H 0.8921 0.0705 -0.0946 0.072 Uiso 1 1 calc R . . C57 C 0.8649(6) 0.0517(6) 0.0260(6) 0.052(2) Uani 1 1 d . . . H57 H 0.8985 0.0963 0.0212 0.062 Uiso 1 1 calc R . . C58 C 0.8213(6) 0.0028(5) 0.1056(5) 0.0386(17) Uani 1 1 d . . . C59 C 0.7039(7) -0.1383(6) 0.0434(5) 0.048(2) Uani 1 1 d . . . H59A H 0.7055 -0.1369 -0.0121 0.072 Uiso 1 1 calc R . . H59B H 0.6306 -0.1124 0.0782 0.072 Uiso 1 1 calc R . . H59C H 0.7370 -0.2072 0.0672 0.072 Uiso 1 1 calc R . . C60 C 0.8396(7) 0.0126(6) 0.1785(6) 0.050(2) Uani 1 1 d . . . H60A H 0.7801 0.0065 0.2281 0.075 Uiso 1 1 calc R . . H60B H 0.8461 0.0780 0.1697 0.075 Uiso 1 1 calc R . . H60C H 0.9048 -0.0402 0.1856 0.075 Uiso 1 1 calc R . . C61 C 0.6381(6) 0.0112(5) 0.3965(5) 0.0386(16) Uani 1 1 d . . . H61A H 0.5766 0.0098 0.4467 0.046 Uiso 1 1 calc R . . H61B H 0.6218 0.0784 0.3627 0.046 Uiso 1 1 calc R . . C62 C 0.7361(6) -0.0152(6) 0.4187(5) 0.0423(17) Uani 1 1 d . . . H62A H 0.7197 0.0127 0.4680 0.051 Uiso 1 1 calc R . . H62B H 0.7902 0.0086 0.3724 0.051 Uiso 1 1 calc R . . C63 C 0.7715(7) -0.1290(6) 0.4363(5) 0.048(2) Uani 1 1 d . . . H63A H 0.8470 -0.1589 0.4324 0.058 Uiso 1 1 calc R . . H63B H 0.7289 -0.1529 0.4916 0.058 Uiso 1 1 calc R . . C64 C 0.7522(6) -0.1533(5) 0.3691(5) 0.0394(17) Uani 1 1 d . . . H64A H 0.8162 -0.1639 0.3201 0.047 Uiso 1 1 calc R . . H64B H 0.7329 -0.2144 0.3887 0.047 Uiso 1 1 calc R . . C65 C 0.5679(10) 0.3352(9) 0.2764(8) 0.080(3) Uiso 1 1 d . . . H65A H 0.5731 0.3408 0.2185 0.096 Uiso 1 1 calc R . . H65B H 0.5193 0.2980 0.3118 0.096 Uiso 1 1 calc R . . C66 C 0.913(2) 0.2283(17) 0.725(2) 0.151(14) Uiso 0.50 1 d PD . . H66A H 0.9197 0.2664 0.6687 0.181 Uiso 0.50 1 calc PR . . H66B H 0.9624 0.2368 0.7453 0.181 Uiso 0.50 1 calc PR . . Cl12 Cl 0.7841(9) 0.2749(8) 0.7895(7) 0.141(3) Uiso 0.50 1 d PD . . Cl11 Cl 0.9459(8) 0.1086(7) 0.7231(6) 0.130(3) Uiso 0.50 1 d PD . . Cl1 Cl 0.42427(12) 0.02130(11) 0.37020(9) 0.0289(4) Uani 1 1 d . . . Cl2 Cl 0.58264(12) 0.11914(10) 0.22063(9) 0.0270(4) Uani 1 1 d . . . Cl3 Cl 0.47225(13) 0.00182(11) 0.18975(10) 0.0302(4) Uani 1 1 d . . . Cl4 Cl 0.35373(13) 0.26200(12) 0.33728(10) 0.0337(4) Uani 1 1 d . . . Cl5 Cl 0.6930(3) 0.2669(3) 0.2879(2) 0.0910(9) Uiso 1 1 d . . . Cl6 Cl 0.5149(3) 0.4539(3) 0.3013(2) 0.1054(11) Uiso 1 1 d . . . Cr2 Cr 0.58768(8) -0.05099(7) 0.26909(6) 0.0246(3) Uani 1 1 d . . . Cr1 Cr 0.39598(8) 0.15245(7) 0.25255(6) 0.0245(3) Uani 1 1 d . . . N1 N 0.3819(4) 0.2486(4) 0.1507(3) 0.0258(11) Uani 1 1 d . . . N2 N 0.2500(4) 0.1762(4) 0.2621(3) 0.0276(11) Uani 1 1 d . . . N3 N 0.5956(4) -0.1927(4) 0.3025(3) 0.0297(12) Uani 1 1 d . . . N4 N 0.7235(4) -0.1141(4) 0.1888(3) 0.0271(11) Uani 1 1 d . . . O1 O 0.6650(3) -0.0667(3) 0.3491(3) 0.0290(10) Uani 1 1 d . . . Cl14 Cl 0.8844(6) 0.5877(6) 0.4351(5) 0.104(2) Uiso 0.50 1 d PD . . Cl13 Cl 0.8000(9) 0.4522(9) 0.5881(7) 0.151(4) Uiso 0.50 1 d PD . . C67 C 0.7855(17) 0.5476(17) 0.5193(13) 0.101(8) Uiso 0.50 1 d PD . . H67A H 0.7426 0.6048 0.5498 0.122 Uiso 1 1 calc R . . H67B H 0.7394 0.5427 0.4940 0.122 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 C1 0.028(3) 0.021(3) 0.035(3) -0.007(3) -0.013(3) -0.003(3) C2 0.036(4) 0.024(3) 0.032(3) -0.006(3) -0.020(3) -0.002(3) C3 0.040(4) 0.032(4) 0.037(4) 0.001(3) -0.020(3) -0.008(3) C4 0.054(5) 0.036(4) 0.038(4) 0.001(3) -0.022(4) -0.013(3) C5 0.059(5) 0.037(4) 0.044(4) -0.003(3) -0.035(4) -0.005(4) C6 0.037(4) 0.040(4) 0.046(4) -0.007(3) -0.027(4) 0.002(3) C7 0.038(4) 0.027(3) 0.040(4) -0.010(3) -0.021(3) 0.000(3) C8 0.031(4) 0.033(4) 0.038(4) -0.012(3) -0.016(3) -0.002(3) C9 0.035(4) 0.059(5) 0.048(5) -0.009(4) -0.023(4) -0.009(4) C10 0.042(5) 0.065(6) 0.071(6) -0.014(5) -0.032(4) -0.017(4) C11 0.037(4) 0.059(5) 0.063(5) -0.010(4) -0.022(4) -0.019(4) C12 0.035(4) 0.048(4) 0.047(4) -0.007(3) -0.018(3) -0.014(3) C13 0.032(4) 0.029(3) 0.041(4) -0.011(3) -0.019(3) -0.001(3) C14 0.024(3) 0.025(3) 0.035(3) -0.005(3) -0.015(3) -0.001(2) C15 0.029(3) 0.026(3) 0.039(4) 0.006(3) -0.018(3) -0.006(3) C16 0.031(4) 0.039(4) 0.035(4) 0.006(3) -0.012(3) -0.006(3) C17 0.031(4) 0.058(5) 0.048(5) 0.011(4) -0.004(4) -0.013(4) C18 0.051(5) 0.059(6) 0.063(6) 0.014(5) -0.022(5) -0.030(5) C19 0.064(6) 0.042(4) 0.057(5) 0.012(4) -0.031(5) -0.029(4) C20 0.042(4) 0.038(4) 0.039(4) 0.010(3) -0.024(3) -0.016(3) C21 0.046(5) 0.037(4) 0.043(5) 0.000(3) -0.002(4) -0.005(4) C22 0.061(5) 0.026(4) 0.056(5) -0.004(3) -0.023(4) -0.012(3) C23 0.027(3) 0.045(4) 0.037(4) -0.001(3) -0.016(3) -0.015(3) C24 0.034(4) 0.055(5) 0.053(5) 0.013(4) -0.025(4) -0.024(4) C25 0.048(5) 0.084(7) 0.052(5) 0.022(5) -0.028(4) -0.041(5) C26 0.058(6) 0.144(12) 0.040(5) 0.007(6) -0.006(5) -0.070(8) C27 0.032(4) 0.127(10) 0.062(6) -0.054(7) 0.004(4) -0.029(5) C28 0.028(4) 0.061(5) 0.039(4) -0.016(4) -0.010(3) -0.016(3) C29 0.047(5) 0.040(4) 0.077(6) 0.011(4) -0.027(5) -0.024(4) C30 0.029(4) 0.054(5) 0.068(6) -0.029(4) -0.014(4) -0.001(3) C31 0.027(3) 0.020(3) 0.036(4) -0.005(3) -0.014(3) -0.004(2) C32 0.038(4) 0.022(3) 0.033(4) -0.001(3) -0.016(3) -0.009(3) C33 0.043(4) 0.024(3) 0.052(5) 0.004(3) -0.019(4) -0.013(3) C34 0.052(5) 0.022(3) 0.060(5) 0.008(3) -0.025(4) -0.014(3) C35 0.064(5) 0.021(3) 0.071(6) 0.005(3) -0.042(5) -0.013(4) C36 0.042(4) 0.026(3) 0.054(5) -0.005(3) -0.025(4) -0.004(3) C37 0.041(4) 0.023(3) 0.043(4) -0.004(3) -0.029(3) -0.003(3) C38 0.032(3) 0.027(3) 0.034(4) -0.005(3) -0.021(3) -0.002(3) C39 0.041(4) 0.025(3) 0.050(4) -0.006(3) -0.023(4) 0.000(3) C40 0.035(4) 0.028(3) 0.046(4) -0.009(3) -0.015(3) 0.005(3) C41 0.035(4) 0.033(4) 0.055(5) -0.001(3) -0.018(4) -0.006(3) C42 0.034(4) 0.028(3) 0.044(4) 0.000(3) -0.015(3) -0.003(3) C43 0.028(3) 0.023(3) 0.035(4) -0.007(3) -0.013(3) -0.001(3) C44 0.029(3) 0.021(3) 0.035(3) -0.006(3) -0.016(3) -0.003(2) C45 0.030(3) 0.020(3) 0.043(4) 0.003(3) -0.014(3) -0.010(3) C46 0.043(4) 0.026(3) 0.049(4) 0.002(3) -0.018(4) -0.013(3) C47 0.051(5) 0.037(4) 0.071(6) -0.001(4) -0.026(4) -0.023(4) C48 0.038(4) 0.041(4) 0.067(6) 0.010(4) -0.014(4) -0.021(4) C49 0.046(4) 0.030(4) 0.043(4) 0.006(3) -0.008(4) -0.012(3) C50 0.038(4) 0.020(3) 0.038(4) 0.004(3) -0.013(3) -0.008(3) C51 0.064(6) 0.051(5) 0.048(5) -0.008(4) -0.017(4) -0.032(4) C52 0.055(5) 0.043(4) 0.040(4) -0.002(3) -0.017(4) -0.020(4) C53 0.026(3) 0.020(3) 0.037(4) -0.002(3) -0.005(3) -0.002(3) C54 0.035(4) 0.031(4) 0.030(4) -0.003(3) -0.006(3) -0.001(3) C55 0.041(5) 0.054(5) 0.035(4) -0.004(4) -0.004(3) -0.003(4) C56 0.040(5) 0.050(5) 0.046(5) 0.013(4) 0.001(4) -0.005(4) C57 0.031(4) 0.033(4) 0.066(6) 0.003(4) -0.003(4) -0.008(3) C58 0.029(4) 0.025(3) 0.045(4) 0.001(3) -0.001(3) -0.009(3) C59 0.055(5) 0.042(4) 0.041(4) -0.015(3) -0.015(4) -0.007(4) C60 0.040(4) 0.042(4) 0.069(6) -0.008(4) -0.013(4) -0.020(4) C61 0.042(4) 0.035(4) 0.042(4) -0.006(3) -0.021(3) -0.009(3) C62 0.041(4) 0.050(4) 0.042(4) -0.006(3) -0.015(3) -0.021(4) C63 0.047(5) 0.044(4) 0.055(5) -0.009(4) -0.030(4) -0.004(4) C64 0.036(4) 0.034(4) 0.049(4) -0.002(3) -0.026(3) -0.004(3) Cl1 0.0263(8) 0.0259(7) 0.0298(8) -0.0015(6) -0.0088(6) -0.0065(6) Cl2 0.0245(8) 0.0208(7) 0.0337(8) -0.0001(6) -0.0118(6) -0.0064(6) Cl3 0.0311(8) 0.0254(7) 0.0366(9) -0.0051(6) -0.0159(7) -0.0068(6) Cl4 0.0338(9) 0.0281(8) 0.0405(9) -0.0092(7) -0.0152(7) -0.0059(7) Cr2 0.0241(5) 0.0181(5) 0.0293(6) -0.0010(4) -0.0106(4) -0.0051(4) Cr1 0.0228(5) 0.0209(5) 0.0292(6) -0.0016(4) -0.0123(4) -0.0048(4) N1 0.024(3) 0.023(3) 0.029(3) -0.002(2) -0.011(2) -0.007(2) N2 0.024(3) 0.027(3) 0.032(3) -0.002(2) -0.011(2) -0.008(2) N3 0.034(3) 0.021(3) 0.034(3) 0.000(2) -0.014(2) -0.009(2) N4 0.028(3) 0.021(3) 0.028(3) -0.001(2) -0.009(2) -0.006(2) O1 0.027(2) 0.024(2) 0.035(2) -0.0016(18) -0.016(2) -0.0046(18) _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 N1 1.352(8) . ? C1 C14 1.438(10) . ? C1 C2 1.467(9) . ? C2 C7 1.421(9) . ? C2 C3 1.422(10) . ? C3 C4 1.373(10) . ? C3 H3 0.9500 . ? C4 C5 1.376(11) . ? C4 H4 0.9500 . ? C5 C6 1.378(12) . ? C5 H5 0.9500 . ? C6 C7 1.411(10) . ? C6 H6 0.9500 . ? C7 C8 1.445(11) . ? C8 C13 1.408(9) . ? C8 C9 1.421(10) . ? C9 C10 1.354(12) . ? C9 H9 0.9500 . ? C10 C11 1.385(12) . ? C10 H10 0.9500 . ? C11 C12 1.369(10) . ? C11 H11 0.9500 . ? C12 C13 1.414(11) . ? C12 H12 0.9500 . ? C13 C14 1.458(9) . ? C14 N2 1.347(8) . ? C15 C16 1.396(10) . ? C15 C20 1.419(10) . ? C15 N1 1.437(9) . ? C16 C17 1.409(11) . ? C16 C21 1.481(12) . ? C17 C18 1.351(13) . ? C17 H17 0.9500 . ? C18 C19 1.369(13) . ? C18 H18 0.9500 . ? C19 C20 1.395(11) . ? C19 H19 0.9500 . ? C20 C22 1.488(11) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C28 1.401(10) . ? C23 C24 1.406(11) . ? C23 N2 1.450(9) . ? C24 C25 1.388(12) . ? C24 C29 1.497(12) . ? C25 C26 1.366(16) . ? C25 H25 0.9500 . ? C26 C27 1.383(17) . ? C26 H26 0.9500 . ? C27 C28 1.402(12) . ? C27 H27 0.9500 . ? C28 C30 1.506(12) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 N3 1.357(8) . ? C31 C44 1.431(10) . ? C31 C32 1.479(8) . ? C32 C33 1.406(10) . ? C32 C37 1.408(10) . ? C33 C34 1.385(9) . ? C33 H33 0.9500 . ? C34 C35 1.365(12) . ? C34 H34 0.9500 . ? C35 C36 1.384(12) . ? C35 H35 0.9500 . ? C36 C37 1.420(9) . ? C36 H36 0.9500 . ? C37 C38 1.458(10) . ? C38 C43 1.400(9) . ? C38 C39 1.428(10) . ? C39 C40 1.366(11) . ? C39 H39 0.9500 . ? C40 C41 1.411(10) . ? C40 H40 0.9500 . ? C41 C42 1.357(10) . ? C41 H41 0.9500 . ? C42 C43 1.416(10) . ? C42 H42 0.9500 . ? C43 C44 1.477(9) . ? C44 N4 1.353(8) . ? C45 C50 1.387(10) . ? C45 C46 1.415(10) . ? C45 N3 1.444(9) . ? C46 C47 1.388(11) . ? C46 C51 1.488(11) . ? C47 C48 1.369(13) . ? C47 H47 0.9500 . ? C48 C49 1.364(12) . ? C48 H48 0.9500 . ? C49 C50 1.384(11) . ? C49 H49 0.9500 . ? C50 C52 1.513(10) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 C54 1.403(10) . ? C53 C58 1.405(10) . ? C53 N4 1.458(8) . ? C54 C55 1.384(11) . ? C54 C59 1.495(12) . ? C55 C56 1.394(14) . ? C55 H55 0.9500 . ? C56 C57 1.334(14) . ? C56 H56 0.9500 . ? C57 C58 1.420(11) . ? C57 H57 0.9500 . ? C58 C60 1.495(12) . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 O1 1.476(8) . ? C61 C62 1.510(10) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C63 1.526(11) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.512(10) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 O1 1.466(8) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 Cl6 1.730(12) . ? C65 Cl5 1.754(12) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 Cl11 1.653(18) . ? C66 Cl12 1.746(18) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? Cl1 Cr2 2.3985(18) . ? Cl1 Cr1 2.4479(18) . ? Cl2 Cr2 2.4044(17) . ? Cl2 Cr1 2.4253(18) . ? Cl3 Cr2 2.3798(18) . ? Cl3 Cr1 2.4482(18) . ? Cl4 Cr1 2.2945(18) . ? Cr2 N4 1.973(5) . ? Cr2 N3 1.984(5) . ? Cr2 O1 2.069(4) . ? Cr1 N2 1.967(5) . ? Cr1 N1 1.979(5) . ? Cl14 C67 1.783(16) . ? Cl13 C67 1.579(16) . ? C67 H67A 0.9900 . ? C67 H67B 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 N1 C1 C14 113.3(6) . . ? N1 C1 C2 126.8(6) . . ? C14 C1 C2 119.8(6) . . ? C7 C2 C3 117.7(6) . . ? C7 C2 C1 118.4(6) . . ? C3 C2 C1 123.9(6) . . ? C4 C3 C2 121.6(7) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C3 C4 C5 120.8(8) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C4 C5 C6 119.1(7) . . ? C4 C5 H5 120.5 . . ? C6 C5 H5 120.5 . . ? C5 C6 C7 122.5(7) . . ? C5 C6 H6 118.7 . . ? C7 C6 H6 118.7 . . ? C6 C7 C2 118.1(7) . . ? C6 C7 C8 120.8(7) . . ? C2 C7 C8 120.9(6) . . ? C13 C8 C9 118.1(7) . . ? C13 C8 C7 120.9(6) . . ? C9 C8 C7 120.9(7) . . ? C10 C9 C8 121.7(7) . . ? C10 C9 H9 119.2 . . ? C8 C9 H9 119.2 . . ? C9 C10 C11 120.6(7) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C12 C11 C10 119.5(8) . . ? C12 C11 H11 120.3 . . ? C10 C11 H11 120.3 . . ? C11 C12 C13 121.8(7) . . ? C11 C12 H12 119.1 . . ? C13 C12 H12 119.1 . . ? C8 C13 C12 118.4(6) . . ? C8 C13 C14 119.0(7) . . ? C12 C13 C14 122.5(6) . . ? N2 C14 C1 113.3(6) . . ? N2 C14 C13 126.6(6) . . ? C1 C14 C13 120.1(6) . . ? C16 C15 C20 121.8(7) . . ? C16 C15 N1 119.4(6) . . ? C20 C15 N1 118.8(6) . . ? C15 C16 C17 117.2(7) . . ? C15 C16 C21 121.6(7) . . ? C17 C16 C21 121.0(7) . . ? C18 C17 C16 121.4(8) . . ? C18 C17 H17 119.3 . . ? C16 C17 H17 119.3 . . ? C17 C18 C19 120.8(8) . . ? C17 C18 H18 119.6 . . ? C19 C18 H18 119.6 . . ? C18 C19 C20 121.5(8) . . ? C18 C19 H19 119.3 . . ? C20 C19 H19 119.3 . . ? C19 C20 C15 116.9(7) . . ? C19 C20 C22 119.6(7) . . ? C15 C20 C22 123.3(7) . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C28 C23 C24 121.9(7) . . ? C28 C23 N2 118.3(6) . . ? C24 C23 N2 119.9(7) . . ? C25 C24 C23 117.9(8) . . ? C25 C24 C29 119.6(8) . . ? C23 C24 C29 122.3(7) . . ? C26 C25 C24 121.2(9) . . ? C26 C25 H25 119.4 . . ? C24 C25 H25 119.4 . . ? C25 C26 C27 120.8(9) . . ? C25 C26 H26 119.6 . . ? C27 C26 H26 119.6 . . ? C26 C27 C28 120.6(10) . . ? C26 C27 H27 119.7 . . ? C28 C27 H27 119.7 . . ? C23 C28 C27 117.6(9) . . ? C23 C28 C30 123.0(7) . . ? C27 C28 C30 119.4(8) . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N3 C31 C44 114.4(5) . . ? N3 C31 C32 125.4(6) . . ? C44 C31 C32 120.2(6) . . ? C33 C32 C37 118.7(6) . . ? C33 C32 C31 123.2(6) . . ? C37 C32 C31 118.1(6) . . ? C34 C33 C32 121.4(7) . . ? C34 C33 H33 119.3 . . ? C32 C33 H33 119.3 . . ? C35 C34 C33 120.3(8) . . ? C35 C34 H34 119.8 . . ? C33 C34 H34 119.8 . . ? C34 C35 C36 119.8(7) . . ? C34 C35 H35 120.1 . . ? C36 C35 H35 120.1 . . ? C35 C36 C37 121.6(7) . . ? C35 C36 H36 119.2 . . ? C37 C36 H36 119.2 . . ? C32 C37 C36 118.0(7) . . ? C32 C37 C38 121.0(6) . . ? C36 C37 C38 120.8(6) . . ? C43 C38 C39 118.0(7) . . ? C43 C38 C37 121.7(6) . . ? C39 C38 C37 120.2(6) . . ? C40 C39 C38 122.6(6) . . ? C40 C39 H39 118.7 . . ? C38 C39 H39 118.7 . . ? C39 C40 C41 118.4(7) . . ? C39 C40 H40 120.8 . . ? C41 C40 H40 120.8 . . ? C42 C41 C40 120.4(8) . . ? C42 C41 H41 119.8 . . ? C40 C41 H41 119.8 . . ? C41 C42 C43 122.0(7) . . ? C41 C42 H42 119.0 . . ? C43 C42 H42 119.0 . . ? C38 C43 C42 118.6(6) . . ? C38 C43 C44 118.0(6) . . ? C42 C43 C44 123.4(6) . . ? N4 C44 C31 113.6(5) . . ? N4 C44 C43 126.2(6) . . ? C31 C44 C43 120.3(6) . . ? C50 C45 C46 121.6(6) . . ? C50 C45 N3 119.9(6) . . ? C46 C45 N3 118.5(6) . . ? C47 C46 C45 117.1(7) . . ? C47 C46 C51 120.4(7) . . ? C45 C46 C51 122.5(7) . . ? C48 C47 C46 121.8(8) . . ? C48 C47 H47 119.1 . . ? C46 C47 H47 119.1 . . ? C49 C48 C47 119.6(8) . . ? C49 C48 H48 120.2 . . ? C47 C48 H48 120.2 . . ? C48 C49 C50 122.0(8) . . ? C48 C49 H49 119.0 . . ? C50 C49 H49 119.0 . . ? C49 C50 C45 117.9(7) . . ? C49 C50 C52 119.4(7) . . ? C45 C50 C52 122.3(7) . . ? C46 C51 H51A 109.5 . . ? C46 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C46 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C50 C52 H52A 109.5 . . ? C50 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C50 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C54 C53 C58 121.9(7) . . ? C54 C53 N4 117.9(6) . . ? C58 C53 N4 120.1(6) . . ? C55 C54 C53 117.8(8) . . ? C55 C54 C59 120.3(7) . . ? C53 C54 C59 121.8(7) . . ? C54 C55 C56 121.4(8) . . ? C54 C55 H55 119.3 . . ? C56 C55 H55 119.3 . . ? C57 C56 C55 119.8(8) . . ? C57 C56 H56 120.1 . . ? C55 C56 H56 120.1 . . ? C56 C57 C58 122.6(9) . . ? C56 C57 H57 118.7 . . ? C58 C57 H57 118.7 . . ? C53 C58 C57 116.4(8) . . ? C53 C58 C60 123.5(7) . . ? C57 C58 C60 119.9(7) . . ? C54 C59 H59A 109.5 . . ? C54 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C54 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C58 C60 H60A 109.5 . . ? C58 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C58 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? O1 C61 C62 104.1(6) . . ? O1 C61 H61A 110.9 . . ? C62 C61 H61A 110.9 . . ? O1 C61 H61B 110.9 . . ? C62 C61 H61B 110.9 . . ? H61A C61 H61B 109.0 . . ? C61 C62 C63 101.5(6) . . ? C61 C62 H62A 111.5 . . ? C63 C62 H62A 111.5 . . ? C61 C62 H62B 111.5 . . ? C63 C62 H62B 111.5 . . ? H62A C62 H62B 109.3 . . ? C64 C63 C62 102.7(6) . . ? C64 C63 H63A 111.2 . . ? C62 C63 H63A 111.2 . . ? C64 C63 H63B 111.2 . . ? C62 C63 H63B 111.2 . . ? H63A C63 H63B 109.1 . . ? O1 C64 C63 105.7(6) . . ? O1 C64 H64A 110.6 . . ? C63 C64 H64A 110.6 . . ? O1 C64 H64B 110.6 . . ? C63 C64 H64B 110.6 . . ? H64A C64 H64B 108.7 . . ? Cl6 C65 Cl5 113.7(7) . . ? Cl6 C65 H65A 108.8 . . ? Cl5 C65 H65A 108.8 . . ? Cl6 C65 H65B 108.8 . . ? Cl5 C65 H65B 108.8 . . ? H65A C65 H65B 107.7 . . ? Cl11 C66 Cl12 110.7(14) . . ? Cl11 C66 H66A 109.5 . . ? Cl12 C66 H66A 109.5 . . ? Cl11 C66 H66B 109.5 . . ? Cl12 C66 H66B 109.5 . . ? H66A C66 H66B 108.1 . . ? Cr2 Cl1 Cr1 82.58(6) . . ? Cr2 Cl2 Cr1 82.94(6) . . ? Cr2 Cl3 Cr1 82.96(6) . . ? N4 Cr2 N3 79.6(2) . . ? N4 Cr2 O1 90.5(2) . . ? N3 Cr2 O1 92.1(2) . . ? N4 Cr2 Cl3 100.46(16) . . ? N3 Cr2 Cl3 97.32(16) . . ? O1 Cr2 Cl3 166.70(13) . . ? N4 Cr2 Cl1 178.13(16) . . ? N3 Cr2 Cl1 99.10(17) . . ? O1 Cr2 Cl1 88.28(13) . . ? Cl3 Cr2 Cl1 80.97(6) . . ? N4 Cr2 Cl2 97.82(16) . . ? N3 Cr2 Cl2 176.74(17) . . ? O1 Cr2 Cl2 89.88(13) . . ? Cl3 Cr2 Cl2 81.21(6) . . ? Cl1 Cr2 Cl2 83.57(6) . . ? N2 Cr1 N1 78.8(2) . . ? N2 Cr1 Cl4 96.22(16) . . ? N1 Cr1 Cl4 99.22(16) . . ? N2 Cr1 Cl2 171.66(17) . . ? N1 Cr1 Cl2 95.69(16) . . ? Cl4 Cr1 Cl2 90.84(6) . . ? N2 Cr1 Cl1 102.78(16) . . ? N1 Cr1 Cl1 174.54(16) . . ? Cl4 Cr1 Cl1 85.84(6) . . ? Cl2 Cr1 Cl1 82.10(6) . . ? N2 Cr1 Cl3 94.80(16) . . ? N1 Cr1 Cl3 96.07(16) . . ? Cl4 Cr1 Cl3 162.62(7) . . ? Cl2 Cr1 Cl3 79.42(6) . . ? Cl1 Cr1 Cl3 78.64(6) . . ? C1 N1 C15 124.8(5) . . ? C1 N1 Cr1 116.0(4) . . ? C15 N1 Cr1 119.0(4) . . ? C14 N2 C23 120.7(5) . . ? C14 N2 Cr1 116.3(4) . . ? C23 N2 Cr1 121.8(4) . . ? C31 N3 C45 123.1(5) . . ? C31 N3 Cr2 114.2(4) . . ? C45 N3 Cr2 122.3(4) . . ? C44 N4 C53 121.4(5) . . ? C44 N4 Cr2 115.0(4) . . ? C53 N4 Cr2 123.1(4) . . ? C64 O1 C61 108.7(5) . . ? C64 O1 Cr2 127.6(4) . . ? C61 O1 Cr2 123.7(4) . . ? Cl13 C67 Cl14 128.7(15) . . ? Cl13 C67 H67A 105.1 . . ? Cl14 C67 H67A 105.1 . . ? Cl13 C67 H67B 105.1 . . ? Cl14 C67 H67B 105.1 . . ? H67A C67 H67B 105.9 . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 26.04 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 4.177 _refine_diff_density_min -1.585 _refine_diff_density_rms 0.183 #===END data_Complex_5 _database_code_depnum_ccdc_archive 'CCDC 835690' #TrackingRef '- combined cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H80 Cl8 Cr2 N4 O' _chemical_formula_weight 1429.02 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' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.8940(11) _cell_length_b 13.7174(12) _cell_length_c 21.3485(18) _cell_angle_alpha 79.533(2) _cell_angle_beta 74.9210(10) _cell_angle_gamma 69.836(2) _cell_volume 3404.8(5) _cell_formula_units_Z 2 _cell_measurement_temperature 185(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.394 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1488 _exptl_absorpt_coefficient_mu 0.681 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8482 _exptl_absorpt_correction_T_max 0.8702 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 185(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 scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18766 _diffrn_reflns_av_R_equivalents 0.0231 _diffrn_reflns_av_sigmaI/netI 0.0572 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 26.06 _reflns_number_total 13130 _reflns_number_gt 9526 _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^)+(0.0998P)^2^+11.5740P] 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 13130 _refine_ls_number_parameters 780 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1061 _refine_ls_R_factor_gt 0.0787 _refine_ls_wR_factor_ref 0.2168 _refine_ls_wR_factor_gt 0.1953 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1397(4) 0.1556(4) 0.1660(2) 0.0251(10) Uani 1 1 d . . . C2 C 0.1251(4) 0.0923(4) 0.1229(3) 0.0277(11) Uani 1 1 d . . . C3 C 0.1751(5) 0.0948(5) 0.0555(3) 0.0364(13) Uani 1 1 d . . . H3 H 0.2169 0.1418 0.0368 0.044 Uiso 1 1 calc R . . C4 C 0.1646(5) 0.0307(5) 0.0165(3) 0.0413(14) Uani 1 1 d . . . H4 H 0.1993 0.0336 -0.0285 0.050 Uiso 1 1 calc R . . C5 C 0.1037(5) -0.0378(5) 0.0429(3) 0.0426(14) Uani 1 1 d . . . H5 H 0.0977 -0.0828 0.0160 0.051 Uiso 1 1 calc R . . C6 C 0.0515(5) -0.0412(4) 0.1081(3) 0.0379(13) Uani 1 1 d . . . H6 H 0.0087 -0.0879 0.1255 0.046 Uiso 1 1 calc R . . C7 C 0.0607(4) 0.0236(4) 0.1494(3) 0.0308(11) Uani 1 1 d . . . C8 C 0.0012(4) 0.0232(4) 0.2178(3) 0.0303(11) Uani 1 1 d . . . C9 C -0.0578(5) -0.0492(5) 0.2457(3) 0.0396(13) Uani 1 1 d . . . H9 H -0.0534 -0.1016 0.2206 0.048 Uiso 1 1 calc R . . C10 C -0.1207(5) -0.0458(5) 0.3077(3) 0.0446(15) Uani 1 1 d . . . H10 H -0.1559 -0.0979 0.3264 0.054 Uiso 1 1 calc R . . C11 C -0.1335(5) 0.0341(5) 0.3436(3) 0.0415(14) Uani 1 1 d . . . H11 H -0.1826 0.0403 0.3854 0.050 Uiso 1 1 calc R . . C12 C -0.0746(4) 0.1045(4) 0.3182(3) 0.0330(12) Uani 1 1 d . . . H12 H -0.0837 0.1588 0.3431 0.040 Uiso 1 1 calc R . . C13 C -0.0014(4) 0.0981(4) 0.2563(2) 0.0266(11) Uani 1 1 d . . . C14 C 0.0742(4) 0.1610(4) 0.2316(2) 0.0235(10) Uani 1 1 d . . . C15 C 0.3186(4) 0.1818(4) 0.1005(2) 0.0272(11) Uani 1 1 d . . . C16 C 0.4004(4) 0.0834(4) 0.1057(3) 0.0302(11) Uani 1 1 d . . . C17 C 0.5033(5) 0.0650(5) 0.0607(3) 0.0369(13) Uani 1 1 d . . . H17 H 0.5606 -0.0003 0.0640 0.044 Uiso 1 1 calc R . . C18 C 0.5228(5) 0.1415(5) 0.0108(3) 0.0431(15) Uani 1 1 d . . . H18 H 0.5938 0.1291 -0.0191 0.052 Uiso 1 1 calc R . . C19 C 0.4397(5) 0.2342(5) 0.0050(3) 0.0426(14) Uani 1 1 d . . . H19 H 0.4531 0.2847 -0.0303 0.051 Uiso 1 1 calc R . . C20 C 0.3360(5) 0.2576(4) 0.0490(2) 0.0320(12) Uani 1 1 d . . . C21 C 0.3783(5) -0.0024(4) 0.1573(3) 0.0354(12) Uani 1 1 d . . . H21A H 0.3249 -0.0293 0.1452 0.043 Uiso 1 1 calc R . . H21B H 0.3399 0.0288 0.1989 0.043 Uiso 1 1 calc R . . C22 C 0.4800(6) -0.0944(5) 0.1695(3) 0.0528(17) Uani 1 1 d . . . H22A H 0.5203 -0.1258 0.1287 0.079 Uiso 1 1 calc R . . H22B H 0.4547 -0.1465 0.2020 0.079 Uiso 1 1 calc R . . H22C H 0.5308 -0.0706 0.1856 0.079 Uiso 1 1 calc R . . C23 C 0.2483(5) 0.3612(5) 0.0365(3) 0.0392(13) Uani 1 1 d . . . H23A H 0.2090 0.3899 0.0788 0.047 Uiso 1 1 calc R . . H23B H 0.2876 0.4102 0.0096 0.047 Uiso 1 1 calc R . . C24 C 0.1609(7) 0.3574(6) 0.0028(4) 0.067(2) Uani 1 1 d . . . H24A H 0.1986 0.3188 -0.0356 0.100 Uiso 1 1 calc R . . H24B H 0.1171 0.4286 -0.0109 0.100 Uiso 1 1 calc R . . H24C H 0.1100 0.3223 0.0329 0.100 Uiso 1 1 calc R . . C25 C 0.0717(4) 0.2079(4) 0.3375(2) 0.0246(10) Uani 1 1 d . . . C26 C 0.1261(4) 0.1146(4) 0.3719(2) 0.0272(11) Uani 1 1 d . . . C27 C 0.0960(5) 0.1065(5) 0.4403(3) 0.0375(13) Uani 1 1 d . . . H27 H 0.1307 0.0437 0.4645 0.045 Uiso 1 1 calc R . . C28 C 0.0172(5) 0.1878(5) 0.4729(3) 0.0437(15) Uani 1 1 d . . . H28 H -0.0014 0.1812 0.5192 0.052 Uiso 1 1 calc R . . C29 C -0.0344(5) 0.2783(5) 0.4383(3) 0.0383(13) Uani 1 1 d . . . H29 H -0.0887 0.3337 0.4615 0.046 Uiso 1 1 calc R . . C30 C -0.0103(4) 0.2918(4) 0.3706(2) 0.0292(11) Uani 1 1 d . . . C31 C 0.2136(5) 0.0222(4) 0.3402(3) 0.0325(12) Uani 1 1 d . . . H31A H 0.2862 0.0106 0.3525 0.039 Uiso 1 1 calc R . . H31B H 0.2253 0.0387 0.2922 0.039 Uiso 1 1 calc R . . C32 C 0.1824(5) -0.0788(4) 0.3587(3) 0.0413(14) Uani 1 1 d . . . H32A H 0.1627 -0.0919 0.4063 0.062 Uiso 1 1 calc R . . H32B H 0.2470 -0.1371 0.3411 0.062 Uiso 1 1 calc R . . H32C H 0.1176 -0.0720 0.3405 0.062 Uiso 1 1 calc R . . C33 C -0.0763(4) 0.3911(4) 0.3364(3) 0.0345(12) Uani 1 1 d . . . H33A H -0.0222 0.4208 0.3037 0.041 Uiso 1 1 calc R . . H33B H -0.1180 0.4420 0.3688 0.041 Uiso 1 1 calc R . . C34 C -0.1605(4) 0.3786(5) 0.3022(3) 0.0391(13) Uani 1 1 d . . . H34A H -0.1198 0.3318 0.2680 0.059 Uiso 1 1 calc R . . H34B H -0.2011 0.4470 0.2827 0.059 Uiso 1 1 calc R . . H34C H -0.2146 0.3491 0.3340 0.059 Uiso 1 1 calc R . . C35 C 0.4943(4) 0.3574(4) 0.3647(2) 0.0202(9) Uani 1 1 d . . . C36 C 0.5575(4) 0.3322(4) 0.4163(2) 0.0206(9) Uani 1 1 d . . . C37 C 0.5913(4) 0.2313(4) 0.4499(2) 0.0281(11) Uani 1 1 d . . . H37 H 0.5708 0.1772 0.4392 0.034 Uiso 1 1 calc R . . C38 C 0.6523(5) 0.2093(4) 0.4972(3) 0.0320(12) Uani 1 1 d . . . H38 H 0.6751 0.1404 0.5181 0.038 Uiso 1 1 calc R . . C39 C 0.6809(5) 0.2880(4) 0.5143(3) 0.0354(13) Uani 1 1 d . . . H39 H 0.7206 0.2741 0.5483 0.042 Uiso 1 1 calc R . . C40 C 0.6516(5) 0.3857(4) 0.4820(3) 0.0324(12) Uani 1 1 d . . . H40 H 0.6727 0.4387 0.4938 0.039 Uiso 1 1 calc R . . C41 C 0.5914(4) 0.4110(4) 0.4319(2) 0.0241(10) Uani 1 1 d . . . C42 C 0.5697(4) 0.5130(4) 0.3946(2) 0.0251(10) Uani 1 1 d . . . C43 C 0.6049(5) 0.5902(4) 0.4104(3) 0.0371(13) Uani 1 1 d . . . H43 H 0.6387 0.5759 0.4470 0.045 Uiso 1 1 calc R . . C44 C 0.5917(6) 0.6855(5) 0.3744(3) 0.0444(15) Uani 1 1 d . . . H44 H 0.6147 0.7368 0.3867 0.053 Uiso 1 1 calc R . . C45 C 0.5454(5) 0.7064(4) 0.3210(3) 0.0412(14) Uani 1 1 d . . . H45 H 0.5381 0.7716 0.2953 0.049 Uiso 1 1 calc R . . C46 C 0.5093(5) 0.6334(4) 0.3044(3) 0.0350(12) Uani 1 1 d . . . H46 H 0.4772 0.6496 0.2670 0.042 Uiso 1 1 calc R . . C47 C 0.5181(4) 0.5356(4) 0.3407(2) 0.0237(10) Uani 1 1 d . . . C48 C 0.4794(4) 0.4557(4) 0.3250(2) 0.0209(10) Uani 1 1 d . . . C49 C 0.4095(4) 0.2166(4) 0.3980(2) 0.0219(10) Uani 1 1 d . . . C50 C 0.4635(4) 0.1100(4) 0.3894(2) 0.0253(10) Uani 1 1 d . . . C51 C 0.4274(5) 0.0376(4) 0.4370(3) 0.0326(12) Uani 1 1 d . . . H51 H 0.4610 -0.0348 0.4320 0.039 Uiso 1 1 calc R . . C52 C 0.3440(5) 0.0690(5) 0.4909(3) 0.0370(13) Uani 1 1 d . . . H52 H 0.3224 0.0180 0.5232 0.044 Uiso 1 1 calc R . . C53 C 0.2912(5) 0.1731(5) 0.4987(3) 0.0353(12) Uani 1 1 d . . . H53 H 0.2329 0.1932 0.5360 0.042 Uiso 1 1 calc R . . C54 C 0.3224(4) 0.2499(4) 0.4520(2) 0.0251(10) Uani 1 1 d . . . C55 C 0.5646(4) 0.0750(4) 0.3350(3) 0.0278(11) Uani 1 1 d . . . H55A H 0.6323 0.0761 0.3482 0.033 Uiso 1 1 calc R . . H55B H 0.5542 0.1262 0.2962 0.033 Uiso 1 1 calc R . . C56 C 0.5875(6) -0.0330(5) 0.3156(3) 0.0469(15) Uani 1 1 d . . . H56A H 0.6107 -0.0858 0.3512 0.070 Uiso 1 1 calc R . . H56B H 0.6480 -0.0451 0.2763 0.070 Uiso 1 1 calc R . . H56C H 0.5186 -0.0378 0.3068 0.070 Uiso 1 1 calc R . . C57 C 0.2628(4) 0.3647(4) 0.4597(2) 0.0300(11) Uani 1 1 d . . . H57A H 0.3188 0.3959 0.4644 0.036 Uiso 1 1 calc R . . H57B H 0.2368 0.3987 0.4191 0.036 Uiso 1 1 calc R . . C58 C 0.1628(5) 0.3908(5) 0.5162(3) 0.0482(16) Uani 1 1 d . . . H58A H 0.1073 0.3586 0.5133 0.072 Uiso 1 1 calc R . . H58B H 0.1279 0.4667 0.5148 0.072 Uiso 1 1 calc R . . H58C H 0.1882 0.3640 0.5573 0.072 Uiso 1 1 calc R . . C59 C 0.3711(4) 0.5643(4) 0.2436(2) 0.0225(10) Uani 1 1 d . . . C60 C 0.2727(4) 0.6332(4) 0.2780(2) 0.0271(11) Uani 1 1 d . . . C61 C 0.2206(5) 0.7272(4) 0.2451(3) 0.0347(12) Uani 1 1 d . . . H61 H 0.1529 0.7738 0.2671 0.042 Uiso 1 1 calc R . . C62 C 0.2657(5) 0.7540(4) 0.1808(3) 0.0381(13) Uani 1 1 d . . . H62 H 0.2296 0.8189 0.1590 0.046 Uiso 1 1 calc R . . C63 C 0.3634(5) 0.6863(4) 0.1482(3) 0.0357(13) Uani 1 1 d . . . H63 H 0.3942 0.7059 0.1041 0.043 Uiso 1 1 calc R . . C64 C 0.4181(4) 0.5898(4) 0.1785(2) 0.0275(11) Uani 1 1 d . . . C65 C 0.2283(5) 0.6096(4) 0.3496(3) 0.0322(12) Uani 1 1 d . . . H65A H 0.2639 0.6389 0.3742 0.039 Uiso 1 1 calc R . . H65B H 0.2531 0.5329 0.3602 0.039 Uiso 1 1 calc R . . C66 C 0.1015(6) 0.6502(6) 0.3735(3) 0.0589(19) Uani 1 1 d . . . H66A H 0.0766 0.7267 0.3690 0.088 Uiso 1 1 calc R . . H66B H 0.0814 0.6245 0.4195 0.088 Uiso 1 1 calc R . . H66C H 0.0644 0.6258 0.3477 0.088 Uiso 1 1 calc R . . C67 C 0.5277(4) 0.5230(4) 0.1414(3) 0.0321(12) Uani 1 1 d . . . H67A H 0.5243 0.5317 0.0948 0.039 Uiso 1 1 calc R . . H67B H 0.5369 0.4489 0.1578 0.039 Uiso 1 1 calc R . . C68 C 0.6302(5) 0.5490(5) 0.1468(3) 0.0433(14) Uani 1 1 d . . . H68A H 0.6178 0.6241 0.1356 0.065 Uiso 1 1 calc R . . H68B H 0.6973 0.5103 0.1167 0.065 Uiso 1 1 calc R . . H68C H 0.6418 0.5294 0.1915 0.065 Uiso 1 1 calc R . . C69 C 0.6659(4) 0.2781(4) 0.2285(3) 0.0295(11) Uani 1 1 d . . . H69A H 0.6845 0.2310 0.2678 0.035 Uiso 1 1 calc R . . H69B H 0.6567 0.3502 0.2356 0.035 Uiso 1 1 calc R . . C70 C 0.7577(5) 0.2439(5) 0.1685(3) 0.0436(15) Uani 1 1 d . . . H70A H 0.7608 0.3035 0.1349 0.052 Uiso 1 1 calc R . . H70B H 0.8329 0.2108 0.1798 0.052 Uiso 1 1 calc R . . C71 C 0.7199(5) 0.1661(5) 0.1459(3) 0.0464(15) Uani 1 1 d . . . H71A H 0.7546 0.1561 0.0994 0.056 Uiso 1 1 calc R . . H71B H 0.7393 0.0977 0.1724 0.056 Uiso 1 1 calc R . . C72 C 0.5930(5) 0.2166(5) 0.1561(3) 0.0398(14) Uani 1 1 d . . . H72A H 0.5726 0.2659 0.1179 0.048 Uiso 1 1 calc R . . H72B H 0.5542 0.1633 0.1634 0.048 Uiso 1 1 calc R . . C73 C 0.8432(9) 0.6737(8) 0.2048(5) 0.089(3) Uiso 1 1 d . . . H73A H 0.9089 0.6301 0.1754 0.106 Uiso 1 1 calc R . . H73B H 0.7851 0.6377 0.2186 0.106 Uiso 1 1 calc R . . C74 C 0.8121(7) 0.3656(7) 0.9323(4) 0.071(2) Uiso 1 1 d . . . H74A H 0.8151 0.3232 0.8986 0.085 Uiso 1 1 calc R . . H74B H 0.8127 0.4359 0.9109 0.085 Uiso 1 1 calc R . . Cl1 Cl 0.34220(10) 0.38759(10) 0.16204(6) 0.0267(3) Uani 1 1 d . . . Cl2 Cl 0.20099(10) 0.39330(10) 0.30503(6) 0.0264(3) Uani 1 1 d . . . Cl3 Cl 0.36004(10) 0.17987(9) 0.25787(6) 0.0245(3) Uani 1 1 d . . . Cl4 Cl 0.06004(11) 0.43254(10) 0.17984(6) 0.0344(3) Uani 1 1 d . . . Cl5 Cl 0.7890(3) 0.7933(3) 0.16342(16) 0.1151(10) Uiso 1 1 d . . . Cl6 Cl 0.8852(3) 0.6876(3) 0.27326(17) 0.1172(10) Uiso 1 1 d . . . Cl7 Cl 0.9286(3) 0.3083(3) 0.96649(19) 0.1319(12) Uiso 1 1 d . . . Cl8 Cl 0.6863(2) 0.37653(19) 0.99252(12) 0.0819(6) Uiso 1 1 d . . . Cr1 Cr 0.20116(6) 0.29825(6) 0.21732(4) 0.02113(19) Uani 1 1 d . . . Cr2 Cr 0.39762(6) 0.33669(6) 0.26496(3) 0.01957(19) Uani 1 1 d . . . N1 N 0.2163(3) 0.2072(3) 0.15138(18) 0.0214(8) Uani 1 1 d . . . N2 N 0.0993(3) 0.2189(3) 0.26726(18) 0.0217(8) Uani 1 1 d . . . N3 N 0.4436(3) 0.2951(3) 0.34993(18) 0.0200(8) Uani 1 1 d . . . N4 N 0.4246(3) 0.4647(3) 0.27707(18) 0.0203(8) Uani 1 1 d . . . O1 O 0.5626(3) 0.2724(3) 0.21464(16) 0.0261(7) 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 0.024(2) 0.024(2) 0.029(3) -0.002(2) -0.012(2) -0.006(2) C2 0.023(2) 0.028(3) 0.034(3) -0.008(2) -0.011(2) -0.004(2) C3 0.040(3) 0.041(3) 0.035(3) -0.009(2) -0.013(2) -0.015(3) C4 0.046(3) 0.048(4) 0.035(3) -0.016(3) -0.014(3) -0.010(3) C5 0.048(4) 0.038(3) 0.049(4) -0.018(3) -0.025(3) -0.005(3) C6 0.039(3) 0.031(3) 0.053(4) -0.009(3) -0.021(3) -0.013(2) C7 0.026(3) 0.029(3) 0.041(3) -0.008(2) -0.017(2) -0.003(2) C8 0.020(2) 0.030(3) 0.044(3) -0.003(2) -0.014(2) -0.007(2) C9 0.034(3) 0.034(3) 0.058(4) -0.007(3) -0.012(3) -0.017(3) C10 0.035(3) 0.042(4) 0.064(4) 0.001(3) -0.012(3) -0.023(3) C11 0.030(3) 0.046(4) 0.051(4) -0.001(3) -0.006(3) -0.019(3) C12 0.023(3) 0.037(3) 0.043(3) -0.004(2) -0.010(2) -0.013(2) C13 0.020(2) 0.027(3) 0.034(3) 0.000(2) -0.010(2) -0.008(2) C14 0.020(2) 0.022(2) 0.029(3) -0.001(2) -0.0105(19) -0.0044(19) C15 0.026(3) 0.035(3) 0.025(2) -0.009(2) -0.006(2) -0.012(2) C16 0.034(3) 0.030(3) 0.030(3) -0.012(2) -0.007(2) -0.011(2) C17 0.032(3) 0.040(3) 0.038(3) -0.013(3) -0.005(2) -0.007(2) C18 0.038(3) 0.054(4) 0.033(3) -0.013(3) 0.011(2) -0.017(3) C19 0.049(4) 0.050(4) 0.028(3) -0.002(3) 0.003(3) -0.024(3) C20 0.041(3) 0.041(3) 0.020(2) -0.005(2) -0.004(2) -0.020(3) C21 0.039(3) 0.028(3) 0.037(3) -0.006(2) -0.007(2) -0.008(2) C22 0.050(4) 0.051(4) 0.053(4) 0.004(3) -0.017(3) -0.011(3) C23 0.049(3) 0.041(3) 0.027(3) 0.002(2) -0.009(2) -0.015(3) C24 0.067(5) 0.057(5) 0.087(6) 0.007(4) -0.048(4) -0.015(4) C25 0.019(2) 0.032(3) 0.027(2) -0.005(2) -0.0022(19) -0.014(2) C26 0.024(2) 0.035(3) 0.027(3) -0.002(2) -0.004(2) -0.017(2) C27 0.040(3) 0.043(3) 0.032(3) 0.004(2) -0.012(2) -0.018(3) C28 0.050(4) 0.061(4) 0.024(3) -0.006(3) -0.001(3) -0.026(3) C29 0.034(3) 0.050(4) 0.033(3) -0.016(3) 0.003(2) -0.018(3) C30 0.026(3) 0.036(3) 0.030(3) -0.007(2) -0.004(2) -0.015(2) C31 0.035(3) 0.034(3) 0.030(3) 0.003(2) -0.009(2) -0.014(2) C32 0.045(3) 0.028(3) 0.050(4) 0.000(3) -0.013(3) -0.010(3) C33 0.028(3) 0.037(3) 0.036(3) -0.013(2) 0.000(2) -0.008(2) C34 0.024(3) 0.042(3) 0.048(3) -0.007(3) -0.007(2) -0.005(2) C35 0.021(2) 0.019(2) 0.021(2) -0.0035(18) -0.0043(18) -0.0065(19) C36 0.020(2) 0.023(2) 0.020(2) -0.0032(18) -0.0045(18) -0.0073(19) C37 0.031(3) 0.025(3) 0.033(3) -0.002(2) -0.014(2) -0.010(2) C38 0.042(3) 0.022(3) 0.036(3) 0.005(2) -0.020(2) -0.010(2) C39 0.047(3) 0.034(3) 0.034(3) 0.001(2) -0.025(3) -0.013(3) C40 0.037(3) 0.029(3) 0.040(3) -0.008(2) -0.015(2) -0.014(2) C41 0.019(2) 0.028(3) 0.026(2) -0.005(2) -0.0038(19) -0.007(2) C42 0.025(2) 0.021(2) 0.031(3) -0.005(2) -0.006(2) -0.008(2) C43 0.053(4) 0.032(3) 0.038(3) 0.002(2) -0.022(3) -0.021(3) C44 0.064(4) 0.033(3) 0.053(4) 0.008(3) -0.030(3) -0.030(3) C45 0.061(4) 0.028(3) 0.048(3) 0.012(3) -0.028(3) -0.027(3) C46 0.047(3) 0.031(3) 0.038(3) 0.006(2) -0.020(3) -0.022(3) C47 0.023(2) 0.023(2) 0.028(2) -0.002(2) -0.0061(19) -0.012(2) C48 0.018(2) 0.025(2) 0.022(2) -0.0034(19) -0.0007(18) -0.0106(19) C49 0.027(2) 0.024(2) 0.021(2) 0.0021(19) -0.0100(19) -0.014(2) C50 0.028(3) 0.025(3) 0.029(3) 0.002(2) -0.014(2) -0.012(2) C51 0.036(3) 0.026(3) 0.042(3) 0.007(2) -0.017(2) -0.015(2) C52 0.046(3) 0.037(3) 0.032(3) 0.012(2) -0.009(2) -0.025(3) C53 0.038(3) 0.046(3) 0.026(3) 0.001(2) -0.004(2) -0.022(3) C54 0.030(3) 0.026(3) 0.024(2) -0.002(2) -0.009(2) -0.013(2) C55 0.029(3) 0.022(3) 0.034(3) 0.002(2) -0.013(2) -0.008(2) C56 0.052(4) 0.032(3) 0.058(4) -0.017(3) -0.005(3) -0.013(3) C57 0.035(3) 0.034(3) 0.026(3) -0.005(2) -0.008(2) -0.014(2) C58 0.041(3) 0.048(4) 0.050(4) -0.015(3) 0.008(3) -0.016(3) C59 0.027(2) 0.018(2) 0.026(2) -0.0019(19) -0.0105(19) -0.0084(19) C60 0.033(3) 0.022(2) 0.032(3) 0.000(2) -0.013(2) -0.013(2) C61 0.032(3) 0.024(3) 0.045(3) -0.008(2) -0.009(2) -0.003(2) C62 0.042(3) 0.027(3) 0.043(3) 0.007(2) -0.016(3) -0.008(2) C63 0.044(3) 0.029(3) 0.033(3) 0.011(2) -0.011(2) -0.014(3) C64 0.033(3) 0.024(3) 0.028(3) 0.002(2) -0.009(2) -0.012(2) C65 0.037(3) 0.029(3) 0.030(3) -0.011(2) -0.003(2) -0.009(2) C66 0.042(4) 0.068(5) 0.049(4) -0.007(3) 0.000(3) -0.001(3) C67 0.034(3) 0.031(3) 0.028(3) 0.005(2) -0.003(2) -0.012(2) C68 0.033(3) 0.049(4) 0.046(3) 0.003(3) -0.003(3) -0.019(3) C69 0.022(2) 0.032(3) 0.032(3) 0.000(2) -0.007(2) -0.006(2) C70 0.023(3) 0.053(4) 0.047(4) -0.009(3) -0.003(2) -0.004(3) C71 0.039(3) 0.044(4) 0.043(3) -0.013(3) 0.004(3) -0.001(3) C72 0.042(3) 0.048(4) 0.031(3) -0.015(3) -0.001(2) -0.015(3) Cl1 0.0296(6) 0.0297(6) 0.0241(6) 0.0002(5) -0.0080(5) -0.0129(5) Cl2 0.0233(6) 0.0306(6) 0.0275(6) -0.0100(5) -0.0036(5) -0.0092(5) Cl3 0.0255(6) 0.0224(6) 0.0290(6) -0.0026(5) -0.0096(5) -0.0091(5) Cl4 0.0289(7) 0.0333(7) 0.0345(7) 0.0005(5) -0.0093(5) -0.0019(5) Cr1 0.0211(4) 0.0224(4) 0.0215(4) -0.0032(3) -0.0049(3) -0.0081(3) Cr2 0.0212(4) 0.0199(4) 0.0196(4) -0.0020(3) -0.0051(3) -0.0083(3) N1 0.021(2) 0.024(2) 0.0199(19) -0.0015(16) -0.0058(15) -0.0087(17) N2 0.021(2) 0.023(2) 0.021(2) -0.0032(16) -0.0040(15) -0.0070(16) N3 0.0205(19) 0.020(2) 0.0203(19) -0.0010(15) -0.0049(15) -0.0071(16) N4 0.0213(19) 0.0179(19) 0.022(2) -0.0006(15) -0.0051(15) -0.0064(16) O1 0.0250(18) 0.0293(19) 0.0239(17) -0.0049(14) -0.0029(14) -0.0092(15) _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 N1 1.347(6) . ? C1 C14 1.435(7) . ? C1 C2 1.461(7) . ? C2 C3 1.414(7) . ? C2 C7 1.413(7) . ? C3 C4 1.375(8) . ? C3 H3 0.9500 . ? C4 C5 1.379(9) . ? C4 H4 0.9500 . ? C5 C6 1.380(9) . ? C5 H5 0.9500 . ? C6 C7 1.413(7) . ? C6 H6 0.9500 . ? C7 C8 1.462(8) . ? C8 C9 1.411(7) . ? C8 C13 1.415(7) . ? C9 C10 1.359(9) . ? C9 H9 0.9500 . ? C10 C11 1.390(9) . ? C10 H10 0.9500 . ? C11 C12 1.380(8) . ? C11 H11 0.9500 . ? C12 C13 1.406(7) . ? C12 H12 0.9500 . ? C13 C14 1.456(7) . ? C14 N2 1.356(6) . ? C15 C20 1.399(7) . ? C15 C16 1.405(7) . ? C15 N1 1.455(6) . ? C16 C17 1.394(7) . ? C16 C21 1.508(8) . ? C17 C18 1.391(8) . ? C17 H17 0.9500 . ? C18 C19 1.361(9) . ? C18 H18 0.9500 . ? C19 C20 1.390(8) . ? C19 H19 0.9500 . ? C20 C23 1.510(8) . ? C21 C22 1.516(8) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.506(9) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.406(7) . ? C25 C30 1.417(7) . ? C25 N2 1.441(6) . ? C26 C27 1.403(7) . ? C26 C31 1.507(7) . ? C27 C28 1.376(9) . ? C27 H27 0.9500 . ? C28 C29 1.373(9) . ? C28 H28 0.9500 . ? C29 C30 1.388(7) . ? C29 H29 0.9500 . ? C30 C33 1.509(8) . ? C31 C32 1.529(7) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.525(8) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 N3 1.359(6) . ? C35 C48 1.437(6) . ? C35 C36 1.461(6) . ? C36 C37 1.415(7) . ? C36 C41 1.415(7) . ? C37 C38 1.366(7) . ? C37 H37 0.9500 . ? C38 C39 1.387(7) . ? C38 H38 0.9500 . ? C39 C40 1.366(8) . ? C39 H39 0.9500 . ? C40 C41 1.405(7) . ? C40 H40 0.9500 . ? C41 C42 1.454(7) . ? C42 C43 1.408(7) . ? C42 C47 1.410(7) . ? C43 C44 1.370(8) . ? C43 H43 0.9500 . ? C44 C45 1.362(8) . ? C44 H44 0.9500 . ? C45 C46 1.372(7) . ? C45 H45 0.9500 . ? C46 C47 1.406(7) . ? C46 H46 0.9500 . ? C47 C48 1.470(6) . ? C48 N4 1.354(6) . ? C49 C54 1.401(7) . ? C49 C50 1.410(7) . ? C49 N3 1.448(6) . ? C50 C51 1.393(7) . ? C50 C55 1.503(7) . ? C51 C52 1.372(8) . ? C51 H51 0.9500 . ? C52 C53 1.373(8) . ? C52 H52 0.9500 . ? C53 C54 1.402(7) . ? C53 H53 0.9500 . ? C54 C57 1.514(7) . ? C55 C56 1.521(7) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 C58 1.508(7) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 C64 1.397(7) . ? C59 C60 1.409(7) . ? C59 N4 1.451(6) . ? C60 C61 1.388(7) . ? C60 C65 1.503(7) . ? C61 C62 1.380(8) . ? C61 H61 0.9500 . ? C62 C63 1.380(8) . ? C62 H62 0.9500 . ? C63 C64 1.397(7) . ? C63 H63 0.9500 . ? C64 C67 1.501(7) . ? C65 C66 1.512(8) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 C68 1.520(8) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 O1 1.468(6) . ? C69 C70 1.520(7) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 C71 1.510(9) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 C72 1.514(8) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 O1 1.479(6) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 Cl5 1.722(10) . ? C73 Cl6 1.746(10) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 Cl7 1.719(9) . ? C74 Cl8 1.768(8) . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? Cl1 Cr2 2.3963(14) . ? Cl1 Cr1 2.4690(14) . ? Cl2 Cr2 2.3492(13) . ? Cl2 Cr1 2.4676(13) . ? Cl3 Cr1 2.3878(14) . ? Cl3 Cr2 2.4000(13) . ? Cl4 Cr1 2.2924(15) . ? Cr1 N2 1.970(4) . ? Cr1 N1 1.977(4) . ? Cr2 N4 1.976(4) . ? Cr2 N3 1.979(4) . ? Cr2 O1 2.078(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C14 114.3(4) . . ? N1 C1 C2 125.6(4) . . ? C14 C1 C2 119.9(4) . . ? C3 C2 C7 118.3(5) . . ? C3 C2 C1 122.7(5) . . ? C7 C2 C1 119.0(5) . . ? C4 C3 C2 121.6(5) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C3 C4 C5 120.0(6) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C6 C5 C4 120.4(5) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C5 C6 C7 121.0(5) . . ? C5 C6 H6 119.5 . . ? C7 C6 H6 119.5 . . ? C2 C7 C6 118.8(5) . . ? C2 C7 C8 120.3(5) . . ? C6 C7 C8 120.9(5) . . ? C9 C8 C13 119.0(5) . . ? C9 C8 C7 120.6(5) . . ? C13 C8 C7 120.3(5) . . ? C10 C9 C8 121.5(6) . . ? C10 C9 H9 119.2 . . ? C8 C9 H9 119.2 . . ? C9 C10 C11 119.9(5) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C12 C11 C10 119.7(6) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C11 C12 C13 121.7(5) . . ? C11 C12 H12 119.1 . . ? C13 C12 H12 119.1 . . ? C12 C13 C8 117.5(5) . . ? C12 C13 C14 123.4(5) . . ? C8 C13 C14 119.0(5) . . ? N2 C14 C1 114.0(4) . . ? N2 C14 C13 125.8(4) . . ? C1 C14 C13 119.9(4) . . ? C20 C15 C16 121.3(5) . . ? C20 C15 N1 119.4(5) . . ? C16 C15 N1 119.2(5) . . ? C17 C16 C15 118.3(5) . . ? C17 C16 C21 119.9(5) . . ? C15 C16 C21 121.8(5) . . ? C18 C17 C16 120.6(6) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C19 C18 C17 119.7(5) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C18 C19 C20 122.3(6) . . ? C18 C19 H19 118.8 . . ? C20 C19 H19 118.8 . . ? C19 C20 C15 117.6(5) . . ? C19 C20 C23 117.9(5) . . ? C15 C20 C23 124.4(5) . . ? C16 C21 C22 117.0(5) . . ? C16 C21 H21A 108.0 . . ? C22 C21 H21A 108.0 . . ? C16 C21 H21B 108.0 . . ? C22 C21 H21B 108.0 . . ? H21A C21 H21B 107.3 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C20 115.2(5) . . ? C24 C23 H23A 108.5 . . ? C20 C23 H23A 108.5 . . ? C24 C23 H23B 108.5 . . ? C20 C23 H23B 108.5 . . ? H23A C23 H23B 107.5 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C30 121.3(5) . . ? C26 C25 N2 119.7(4) . . ? C30 C25 N2 119.1(4) . . ? C27 C26 C25 117.9(5) . . ? C27 C26 C31 117.8(5) . . ? C25 C26 C31 124.2(4) . . ? C28 C27 C26 121.3(5) . . ? C28 C27 H27 119.4 . . ? C26 C27 H27 119.4 . . ? C27 C28 C29 119.7(5) . . ? C27 C28 H28 120.1 . . ? C29 C28 H28 120.1 . . ? C28 C29 C30 122.4(5) . . ? C28 C29 H29 118.8 . . ? C30 C29 H29 118.8 . . ? C29 C30 C25 117.4(5) . . ? C29 C30 C33 118.9(5) . . ? C25 C30 C33 123.6(5) . . ? C26 C31 C32 114.0(4) . . ? C26 C31 H31A 108.7 . . ? C32 C31 H31A 108.7 . . ? C26 C31 H31B 108.7 . . ? C32 C31 H31B 108.7 . . ? H31A C31 H31B 107.6 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C33 C34 115.1(5) . . ? C30 C33 H33A 108.5 . . ? C34 C33 H33A 108.5 . . ? C30 C33 H33B 108.5 . . ? C34 C33 H33B 108.5 . . ? H33A C33 H33B 107.5 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N3 C35 C48 113.9(4) . . ? N3 C35 C36 125.5(4) . . ? C48 C35 C36 120.6(4) . . ? C37 C36 C41 117.9(4) . . ? C37 C36 C35 123.4(4) . . ? C41 C36 C35 118.7(4) . . ? C38 C37 C36 122.3(5) . . ? C38 C37 H37 118.9 . . ? C36 C37 H37 118.9 . . ? C37 C38 C39 119.6(5) . . ? C37 C38 H38 120.2 . . ? C39 C38 H38 120.2 . . ? C40 C39 C38 119.6(5) . . ? C40 C39 H39 120.2 . . ? C38 C39 H39 120.2 . . ? C39 C40 C41 122.5(5) . . ? C39 C40 H40 118.7 . . ? C41 C40 H40 118.7 . . ? C40 C41 C36 118.0(5) . . ? C40 C41 C42 121.3(4) . . ? C36 C41 C42 120.5(4) . . ? C43 C42 C47 118.6(5) . . ? C43 C42 C41 119.8(5) . . ? C47 C42 C41 121.5(4) . . ? C44 C43 C42 121.8(5) . . ? C44 C43 H43 119.1 . . ? C42 C43 H43 119.1 . . ? C45 C44 C43 119.7(5) . . ? C45 C44 H44 120.2 . . ? C43 C44 H44 120.2 . . ? C44 C45 C46 120.2(5) . . ? C44 C45 H45 119.9 . . ? C46 C45 H45 119.9 . . ? C45 C46 C47 122.3(5) . . ? C45 C46 H46 118.9 . . ? C47 C46 H46 118.9 . . ? C46 C47 C42 117.3(4) . . ? C46 C47 C48 124.1(4) . . ? C42 C47 C48 118.6(4) . . ? N4 C48 C35 113.3(4) . . ? N4 C48 C47 127.0(4) . . ? C35 C48 C47 119.7(4) . . ? C54 C49 C50 121.9(4) . . ? C54 C49 N3 118.3(4) . . ? C50 C49 N3 119.8(4) . . ? C51 C50 C49 117.5(5) . . ? C51 C50 C55 120.8(5) . . ? C49 C50 C55 121.4(4) . . ? C52 C51 C50 121.1(5) . . ? C52 C51 H51 119.4 . . ? C50 C51 H51 119.4 . . ? C51 C52 C53 121.0(5) . . ? C51 C52 H52 119.5 . . ? C53 C52 H52 119.5 . . ? C52 C53 C54 120.7(5) . . ? C52 C53 H53 119.7 . . ? C54 C53 H53 119.7 . . ? C53 C54 C49 117.7(5) . . ? C53 C54 C57 120.8(5) . . ? C49 C54 C57 121.4(4) . . ? C50 C55 C56 115.4(4) . . ? C50 C55 H55A 108.4 . . ? C56 C55 H55A 108.4 . . ? C50 C55 H55B 108.4 . . ? C56 C55 H55B 108.4 . . ? H55A C55 H55B 107.5 . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C58 C57 C54 116.5(5) . . ? C58 C57 H57A 108.2 . . ? C54 C57 H57A 108.2 . . ? C58 C57 H57B 108.2 . . ? C54 C57 H57B 108.2 . . ? H57A C57 H57B 107.3 . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C64 C59 C60 121.6(4) . . ? C64 C59 N4 119.6(4) . . ? C60 C59 N4 118.8(4) . . ? C61 C60 C59 118.3(5) . . ? C61 C60 C65 120.3(5) . . ? C59 C60 C65 121.4(4) . . ? C62 C61 C60 121.0(5) . . ? C62 C61 H61 119.5 . . ? C60 C61 H61 119.5 . . ? C63 C62 C61 119.9(5) . . ? C63 C62 H62 120.0 . . ? C61 C62 H62 120.0 . . ? C62 C63 C64 121.5(5) . . ? C62 C63 H63 119.2 . . ? C64 C63 H63 119.2 . . ? C63 C64 C59 117.6(5) . . ? C63 C64 C67 118.6(5) . . ? C59 C64 C67 123.6(4) . . ? C60 C65 C66 116.3(5) . . ? C60 C65 H65A 108.2 . . ? C66 C65 H65A 108.2 . . ? C60 C65 H65B 108.2 . . ? C66 C65 H65B 108.2 . . ? H65A C65 H65B 107.4 . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C64 C67 C68 113.4(5) . . ? C64 C67 H67A 108.9 . . ? C68 C67 H67A 108.9 . . ? C64 C67 H67B 108.9 . . ? C68 C67 H67B 108.9 . . ? H67A C67 H67B 107.7 . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? O1 C69 C70 105.1(4) . . ? O1 C69 H69A 110.7 . . ? C70 C69 H69A 110.7 . . ? O1 C69 H69B 110.7 . . ? C70 C69 H69B 110.7 . . ? H69A C69 H69B 108.8 . . ? C71 C70 C69 102.3(5) . . ? C71 C70 H70A 111.3 . . ? C69 C70 H70A 111.3 . . ? C71 C70 H70B 111.3 . . ? C69 C70 H70B 111.3 . . ? H70A C70 H70B 109.2 . . ? C72 C71 C70 103.0(5) . . ? C72 C71 H71A 111.2 . . ? C70 C71 H71A 111.2 . . ? C72 C71 H71B 111.2 . . ? C70 C71 H71B 111.2 . . ? H71A C71 H71B 109.1 . . ? O1 C72 C71 104.3(5) . . ? O1 C72 H72A 110.9 . . ? C71 C72 H72A 110.9 . . ? O1 C72 H72B 110.9 . . ? C71 C72 H72B 110.9 . . ? H72A C72 H72B 108.9 . . ? Cl5 C73 Cl6 111.1(6) . . ? Cl5 C73 H73A 109.4 . . ? Cl6 C73 H73A 109.4 . . ? Cl5 C73 H73B 109.4 . . ? Cl6 C73 H73B 109.4 . . ? H73A C73 H73B 108.0 . . ? Cl7 C74 Cl8 110.6(5) . . ? Cl7 C74 H74A 109.5 . . ? Cl8 C74 H74A 109.5 . . ? Cl7 C74 H74B 109.5 . . ? Cl8 C74 H74B 109.5 . . ? H74A C74 H74B 108.1 . . ? Cr2 Cl1 Cr1 81.98(4) . . ? Cr2 Cl2 Cr1 82.96(4) . . ? Cr1 Cl3 Cr2 83.61(4) . . ? N2 Cr1 N1 80.15(16) . . ? N2 Cr1 Cl4 94.28(12) . . ? N1 Cr1 Cl4 93.61(12) . . ? N2 Cr1 Cl3 92.99(12) . . ? N1 Cr1 Cl3 93.28(12) . . ? Cl4 Cr1 Cl3 170.74(6) . . ? N2 Cr1 Cl2 99.09(12) . . ? N1 Cr1 Cl2 172.73(12) . . ? Cl4 Cr1 Cl2 93.65(5) . . ? Cl3 Cr1 Cl2 79.52(5) . . ? N2 Cr1 Cl1 174.16(12) . . ? N1 Cr1 Cl1 101.66(12) . . ? Cl4 Cr1 Cl1 91.16(5) . . ? Cl3 Cr1 Cl1 81.39(5) . . ? Cl2 Cr1 Cl1 78.41(4) . . ? N4 Cr2 N3 79.38(16) . . ? N4 Cr2 O1 93.39(14) . . ? N3 Cr2 O1 91.75(14) . . ? N4 Cr2 Cl2 96.47(12) . . ? N3 Cr2 Cl2 97.84(11) . . ? O1 Cr2 Cl2 167.35(10) . . ? N4 Cr2 Cl1 100.40(12) . . ? N3 Cr2 Cl1 179.78(12) . . ? O1 Cr2 Cl1 88.22(10) . . ? Cl2 Cr2 Cl1 82.22(5) . . ? N4 Cr2 Cl3 176.22(12) . . ? N3 Cr2 Cl3 97.57(12) . . ? O1 Cr2 Cl3 88.91(10) . . ? Cl2 Cr2 Cl3 81.68(5) . . ? Cl1 Cr2 Cl3 82.66(5) . . ? C1 N1 C15 123.9(4) . . ? C1 N1 Cr1 114.8(3) . . ? C15 N1 Cr1 119.8(3) . . ? C14 N2 C25 122.3(4) . . ? C14 N2 Cr1 114.9(3) . . ? C25 N2 Cr1 121.8(3) . . ? C35 N3 C49 121.2(4) . . ? C35 N3 Cr2 114.7(3) . . ? C49 N3 Cr2 123.3(3) . . ? C48 N4 C59 123.0(4) . . ? C48 N4 Cr2 115.9(3) . . ? C59 N4 Cr2 120.3(3) . . ? C69 O1 C72 109.1(4) . . ? C69 O1 Cr2 126.8(3) . . ? C72 O1 Cr2 124.1(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -13.1(8) . . . . ? C14 C1 C2 C3 171.1(5) . . . . ? N1 C1 C2 C7 165.3(5) . . . . ? C14 C1 C2 C7 -10.5(7) . . . . ? C7 C2 C3 C4 -1.6(8) . . . . ? C1 C2 C3 C4 176.8(5) . . . . ? C2 C3 C4 C5 0.3(9) . . . . ? C3 C4 C5 C6 1.1(9) . . . . ? C4 C5 C6 C7 -1.1(9) . . . . ? C3 C2 C7 C6 1.6(7) . . . . ? C1 C2 C7 C6 -176.9(5) . . . . ? C3 C2 C7 C8 -176.0(5) . . . . ? C1 C2 C7 C8 5.5(7) . . . . ? C5 C6 C7 C2 -0.3(8) . . . . ? C5 C6 C7 C8 177.3(5) . . . . ? C2 C7 C8 C9 -176.2(5) . . . . ? C6 C7 C8 C9 6.2(8) . . . . ? C2 C7 C8 C13 6.1(7) . . . . ? C6 C7 C8 C13 -171.5(5) . . . . ? C13 C8 C9 C10 2.8(8) . . . . ? C7 C8 C9 C10 -174.9(5) . . . . ? C8 C9 C10 C11 3.9(9) . . . . ? C9 C10 C11 C12 -5.4(9) . . . . ? C10 C11 C12 C13 0.2(9) . . . . ? C11 C12 C13 C8 6.4(8) . . . . ? C11 C12 C13 C14 -171.0(5) . . . . ? C9 C8 C13 C12 -7.8(7) . . . . ? C7 C8 C13 C12 170.0(5) . . . . ? C9 C8 C13 C14 169.7(5) . . . . ? C7 C8 C13 C14 -12.6(7) . . . . ? N1 C1 C14 N2 1.1(6) . . . . ? C2 C1 C14 N2 177.4(4) . . . . ? N1 C1 C14 C13 -172.3(4) . . . . ? C2 C1 C14 C13 4.0(7) . . . . ? C12 C13 C14 N2 12.3(8) . . . . ? C8 C13 C14 N2 -165.0(5) . . . . ? C12 C13 C14 C1 -175.2(5) . . . . ? C8 C13 C14 C1 7.5(7) . . . . ? C20 C15 C16 C17 4.3(7) . . . . ? N1 C15 C16 C17 -172.6(4) . . . . ? C20 C15 C16 C21 -174.2(5) . . . . ? N1 C15 C16 C21 8.9(7) . . . . ? C15 C16 C17 C18 -1.8(8) . . . . ? C21 C16 C17 C18 176.8(5) . . . . ? C16 C17 C18 C19 -1.5(9) . . . . ? C17 C18 C19 C20 2.5(9) . . . . ? C18 C19 C20 C15 0.0(9) . . . . ? C18 C19 C20 C23 -177.7(6) . . . . ? C16 C15 C20 C19 -3.4(7) . . . . ? N1 C15 C20 C19 173.5(5) . . . . ? C16 C15 C20 C23 174.1(5) . . . . ? N1 C15 C20 C23 -9.0(7) . . . . ? C17 C16 C21 C22 16.4(8) . . . . ? C15 C16 C21 C22 -165.1(5) . . . . ? C19 C20 C23 C24 97.7(7) . . . . ? C15 C20 C23 C24 -79.9(7) . . . . ? C30 C25 C26 C27 0.6(7) . . . . ? N2 C25 C26 C27 -179.3(4) . . . . ? C30 C25 C26 C31 179.8(4) . . . . ? N2 C25 C26 C31 -0.1(7) . . . . ? C25 C26 C27 C28 -1.1(8) . . . . ? C31 C26 C27 C28 179.6(5) . . . . ? C26 C27 C28 C29 0.9(9) . . . . ? C27 C28 C29 C30 -0.1(9) . . . . ? C28 C29 C30 C25 -0.4(8) . . . . ? C28 C29 C30 C33 176.1(5) . . . . ? C26 C25 C30 C29 0.1(7) . . . . ? N2 C25 C30 C29 -179.9(4) . . . . ? C26 C25 C30 C33 -176.3(5) . . . . ? N2 C25 C30 C33 3.7(7) . . . . ? C27 C26 C31 C32 57.7(6) . . . . ? C25 C26 C31 C32 -121.5(5) . . . . ? C29 C30 C33 C34 -108.5(6) . . . . ? C25 C30 C33 C34 67.9(6) . . . . ? N3 C35 C36 C37 11.9(7) . . . . ? C48 C35 C36 C37 -169.2(4) . . . . ? N3 C35 C36 C41 -171.0(4) . . . . ? C48 C35 C36 C41 7.9(6) . . . . ? C41 C36 C37 C38 1.5(7) . . . . ? C35 C36 C37 C38 178.7(5) . . . . ? C36 C37 C38 C39 1.3(8) . . . . ? C37 C38 C39 C40 -2.6(9) . . . . ? C38 C39 C40 C41 0.9(9) . . . . ? C39 C40 C41 C36 1.9(8) . . . . ? C39 C40 C41 C42 -174.7(5) . . . . ? C37 C36 C41 C40 -3.1(7) . . . . ? C35 C36 C41 C40 179.6(4) . . . . ? C37 C36 C41 C42 173.6(4) . . . . ? C35 C36 C41 C42 -3.7(7) . . . . ? C40 C41 C42 C43 -2.9(7) . . . . ? C36 C41 C42 C43 -179.4(5) . . . . ? C40 C41 C42 C47 174.4(5) . . . . ? C36 C41 C42 C47 -2.2(7) . . . . ? C47 C42 C43 C44 -0.9(9) . . . . ? C41 C42 C43 C44 176.5(6) . . . . ? C42 C43 C44 C45 -1.3(10) . . . . ? C43 C44 C45 C46 1.8(10) . . . . ? C44 C45 C46 C47 -0.1(10) . . . . ? C45 C46 C47 C42 -2.1(8) . . . . ? C45 C46 C47 C48 179.3(5) . . . . ? C43 C42 C47 C46 2.5(7) . . . . ? C41 C42 C47 C46 -174.8(5) . . . . ? C43 C42 C47 C48 -178.8(5) . . . . ? C41 C42 C47 C48 3.9(7) . . . . ? N3 C35 C48 N4 -4.6(6) . . . . ? C36 C35 C48 N4 176.4(4) . . . . ? N3 C35 C48 C47 172.8(4) . . . . ? C36 C35 C48 C47 -6.2(6) . . . . ? C46 C47 C48 N4 -4.1(8) . . . . ? C42 C47 C48 N4 177.3(4) . . . . ? C46 C47 C48 C35 178.9(5) . . . . ? C42 C47 C48 C35 0.3(7) . . . . ? C54 C49 C50 C51 -0.2(7) . . . . ? N3 C49 C50 C51 -179.8(4) . . . . ? C54 C49 C50 C55 -173.6(4) . . . . ? N3 C49 C50 C55 6.7(7) . . . . ? C49 C50 C51 C52 -1.4(7) . . . . ? C55 C50 C51 C52 172.1(5) . . . . ? C50 C51 C52 C53 1.9(8) . . . . ? C51 C52 C53 C54 -0.9(8) . . . . ? C52 C53 C54 C49 -0.7(8) . . . . ? C52 C53 C54 C57 178.8(5) . . . . ? C50 C49 C54 C53 1.2(7) . . . . ? N3 C49 C54 C53 -179.2(4) . . . . ? C50 C49 C54 C57 -178.2(4) . . . . ? N3 C49 C54 C57 1.4(7) . . . . ? C51 C50 C55 C56 28.4(7) . . . . ? C49 C50 C55 C56 -158.3(5) . . . . ? C53 C54 C57 C58 -5.4(7) . . . . ? C49 C54 C57 C58 174.0(5) . . . . ? C64 C59 C60 C61 1.8(7) . . . . ? N4 C59 C60 C61 -178.4(4) . . . . ? C64 C59 C60 C65 -174.6(5) . . . . ? N4 C59 C60 C65 5.2(7) . . . . ? C59 C60 C61 C62 -1.9(8) . . . . ? C65 C60 C61 C62 174.5(5) . . . . ? C60 C61 C62 C63 0.7(9) . . . . ? C61 C62 C63 C64 0.7(9) . . . . ? C62 C63 C64 C59 -0.8(8) . . . . ? C62 C63 C64 C67 -176.4(5) . . . . ? C60 C59 C64 C63 -0.4(7) . . . . ? N4 C59 C64 C63 179.8(4) . . . . ? C60 C59 C64 C67 174.8(5) . . . . ? N4 C59 C64 C67 -4.9(7) . . . . ? C61 C60 C65 C66 35.2(7) . . . . ? C59 C60 C65 C66 -148.5(5) . . . . ? C63 C64 C67 C68 85.7(6) . . . . ? C59 C64 C67 C68 -89.6(6) . . . . ? O1 C69 C70 C71 -32.0(6) . . . . ? C69 C70 C71 C72 40.3(6) . . . . ? C70 C71 C72 O1 -33.6(6) . . . . ? Cr2 Cl3 Cr1 N2 -138.80(12) . . . . ? Cr2 Cl3 Cr1 N1 140.91(12) . . . . ? Cr2 Cl3 Cr1 Cl4 2.9(4) . . . . ? Cr2 Cl3 Cr1 Cl2 -40.10(4) . . . . ? Cr2 Cl3 Cr1 Cl1 39.60(4) . . . . ? Cr2 Cl2 Cr1 N2 132.61(12) . . . . ? Cr2 Cl2 Cr1 N1 49.2(9) . . . . ? Cr2 Cl2 Cr1 Cl4 -132.46(5) . . . . ? Cr2 Cl2 Cr1 Cl3 41.22(4) . . . . ? Cr2 Cl2 Cr1 Cl1 -42.03(4) . . . . ? Cr2 Cl1 Cr1 N2 -24.0(12) . . . . ? Cr2 Cl1 Cr1 N1 -131.45(12) . . . . ? Cr2 Cl1 Cr1 Cl4 134.63(5) . . . . ? Cr2 Cl1 Cr1 Cl3 -39.85(4) . . . . ? Cr2 Cl1 Cr1 Cl2 41.13(4) . . . . ? Cr1 Cl2 Cr2 N4 142.67(12) . . . . ? Cr1 Cl2 Cr2 N3 -137.22(12) . . . . ? Cr1 Cl2 Cr2 O1 1.7(5) . . . . ? Cr1 Cl2 Cr2 Cl1 43.00(4) . . . . ? Cr1 Cl2 Cr2 Cl3 -40.66(4) . . . . ? Cr1 Cl1 Cr2 N4 -138.29(12) . . . . ? Cr1 Cl1 Cr2 N3 -148(81) . . . . ? Cr1 Cl1 Cr2 O1 128.59(10) . . . . ? Cr1 Cl1 Cr2 Cl2 -43.09(4) . . . . ? Cr1 Cl1 Cr2 Cl3 39.46(4) . . . . ? Cr1 Cl3 Cr2 N4 103.2(18) . . . . ? Cr1 Cl3 Cr2 N3 139.12(11) . . . . ? Cr1 Cl3 Cr2 O1 -129.25(10) . . . . ? Cr1 Cl3 Cr2 Cl2 42.26(4) . . . . ? Cr1 Cl3 Cr2 Cl1 -40.90(4) . . . . ? C14 C1 N1 C15 155.0(4) . . . . ? C2 C1 N1 C15 -21.0(7) . . . . ? C14 C1 N1 Cr1 -10.7(5) . . . . ? C2 C1 N1 Cr1 173.3(4) . . . . ? C20 C15 N1 C1 120.6(5) . . . . ? C16 C15 N1 C1 -62.4(6) . . . . ? C20 C15 N1 Cr1 -74.4(5) . . . . ? C16 C15 N1 Cr1 102.5(5) . . . . ? N2 Cr1 N1 C1 12.1(3) . . . . ? Cl4 Cr1 N1 C1 -81.7(3) . . . . ? Cl3 Cr1 N1 C1 104.5(3) . . . . ? Cl2 Cr1 N1 C1 96.6(10) . . . . ? Cl1 Cr1 N1 C1 -173.6(3) . . . . ? N2 Cr1 N1 C15 -154.2(4) . . . . ? Cl4 Cr1 N1 C15 112.1(3) . . . . ? Cl3 Cr1 N1 C15 -61.7(3) . . . . ? Cl2 Cr1 N1 C15 -69.6(11) . . . . ? Cl1 Cr1 N1 C15 20.1(4) . . . . ? C1 C14 N2 C25 -159.8(4) . . . . ? C13 C14 N2 C25 13.2(7) . . . . ? C1 C14 N2 Cr1 9.0(5) . . . . ? C13 C14 N2 Cr1 -178.1(4) . . . . ? C26 C25 N2 C14 66.7(6) . . . . ? C30 C25 N2 C14 -113.2(5) . . . . ? C26 C25 N2 Cr1 -101.3(4) . . . . ? C30 C25 N2 Cr1 78.8(5) . . . . ? N1 Cr1 N2 C14 -11.4(3) . . . . ? Cl4 Cr1 N2 C14 81.5(3) . . . . ? Cl3 Cr1 N2 C14 -104.3(3) . . . . ? Cl2 Cr1 N2 C14 175.9(3) . . . . ? Cl1 Cr1 N2 C14 -120.0(11) . . . . ? N1 Cr1 N2 C25 157.4(4) . . . . ? Cl4 Cr1 N2 C25 -109.7(3) . . . . ? Cl3 Cr1 N2 C25 64.6(3) . . . . ? Cl2 Cr1 N2 C25 -15.3(4) . . . . ? Cl1 Cr1 N2 C25 48.9(14) . . . . ? C48 C35 N3 C49 -154.7(4) . . . . ? C36 C35 N3 C49 24.2(7) . . . . ? C48 C35 N3 Cr2 15.2(5) . . . . ? C36 C35 N3 Cr2 -165.9(4) . . . . ? C54 C49 N3 C35 66.7(6) . . . . ? C50 C49 N3 C35 -113.6(5) . . . . ? C54 C49 N3 Cr2 -102.4(4) . . . . ? C50 C49 N3 Cr2 77.3(5) . . . . ? N4 Cr2 N3 C35 -15.2(3) . . . . ? O1 Cr2 N3 C35 77.9(3) . . . . ? Cl2 Cr2 N3 C35 -110.4(3) . . . . ? Cl1 Cr2 N3 C35 -6(41) . . . . ? Cl3 Cr2 N3 C35 167.0(3) . . . . ? N4 Cr2 N3 C49 154.5(4) . . . . ? O1 Cr2 N3 C49 -112.4(4) . . . . ? Cl2 Cr2 N3 C49 59.4(4) . . . . ? Cl1 Cr2 N3 C49 164(100) . . . . ? Cl3 Cr2 N3 C49 -23.2(4) . . . . ? C35 C48 N4 C59 161.5(4) . . . . ? C47 C48 N4 C59 -15.7(7) . . . . ? C35 C48 N4 Cr2 -8.2(5) . . . . ? C47 C48 N4 Cr2 174.6(4) . . . . ? C64 C59 N4 C48 109.8(5) . . . . ? C60 C59 N4 C48 -70.0(6) . . . . ? C64 C59 N4 Cr2 -80.9(5) . . . . ? C60 C59 N4 Cr2 99.3(4) . . . . ? N3 Cr2 N4 C48 12.8(3) . . . . ? O1 Cr2 N4 C48 -78.4(3) . . . . ? Cl2 Cr2 N4 C48 109.6(3) . . . . ? Cl1 Cr2 N4 C48 -167.2(3) . . . . ? Cl3 Cr2 N4 C48 49(2) . . . . ? N3 Cr2 N4 C59 -157.2(4) . . . . ? O1 Cr2 N4 C59 111.6(3) . . . . ? Cl2 Cr2 N4 C59 -60.4(3) . . . . ? Cl1 Cr2 N4 C59 22.8(3) . . . . ? Cl3 Cr2 N4 C59 -121.0(17) . . . . ? C70 C69 O1 C72 11.4(6) . . . . ? C70 C69 O1 Cr2 -166.0(3) . . . . ? C71 C72 O1 C69 13.8(6) . . . . ? C71 C72 O1 Cr2 -168.6(4) . . . . ? N4 Cr2 O1 C69 38.7(4) . . . . ? N3 Cr2 O1 C69 -40.8(4) . . . . ? Cl2 Cr2 O1 C69 179.8(4) . . . . ? Cl1 Cr2 O1 C69 139.0(4) . . . . ? Cl3 Cr2 O1 C69 -138.3(4) . . . . ? N4 Cr2 O1 C72 -138.4(4) . . . . ? N3 Cr2 O1 C72 142.1(4) . . . . ? Cl2 Cr2 O1 C72 2.7(8) . . . . ? Cl1 Cr2 O1 C72 -38.1(4) . . . . ? Cl3 Cr2 O1 C72 44.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 26.06 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 2.565 _refine_diff_density_min -1.956 _refine_diff_density_rms 0.112 #===END data_Complex_7 _database_code_depnum_ccdc_archive 'CCDC 835691' #TrackingRef '- combined cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C73 H78 Cl6 Cr2 N4 O' _chemical_formula_weight 1344.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 25.162(2) _cell_length_b 15.3030(14) _cell_length_c 18.2914(18) _cell_angle_alpha 90.00 _cell_angle_beta 110.053(2) _cell_angle_gamma 90.00 _cell_volume 6616.3(11) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.349 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2808 _exptl_absorpt_coefficient_mu 0.618 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8608 _exptl_absorpt_correction_T_max 0.8811 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38207 _diffrn_reflns_av_R_equivalents 0.1628 _diffrn_reflns_av_sigmaI/netI 0.1973 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 25.03 _reflns_number_total 11688 _reflns_number_gt 5384 _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^)+(0.0900P)^2^+8.8311P] 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 11688 _refine_ls_number_parameters 772 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2086 _refine_ls_R_factor_gt 0.0916 _refine_ls_wR_factor_ref 0.2298 _refine_ls_wR_factor_gt 0.1791 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C48 C 0.1127(3) 0.6860(5) -0.0080(4) 0.0248(19) Uani 1 1 d . . . C47 C 0.0647(3) 0.7458(6) -0.0428(4) 0.027(2) Uani 1 1 d . . . C46 C 0.0596(4) 0.8292(7) -0.0124(5) 0.054(3) Uani 1 1 d . . . H3 H 0.0894 0.8500 0.0300 0.065 Uiso 1 1 calc R . . C45 C 0.0132(5) 0.8795(7) -0.0426(6) 0.065(3) Uani 1 1 d . . . H4 H 0.0118 0.9344 -0.0216 0.078 Uiso 1 1 calc R . . C44 C -0.0324(4) 0.8498(7) -0.1050(6) 0.052(3) Uani 1 1 d . . . H5 H -0.0655 0.8826 -0.1232 0.063 Uiso 1 1 calc R . . C43 C -0.0285(4) 0.7718(6) -0.1395(5) 0.041(2) Uani 1 1 d . . . H6 H -0.0586 0.7526 -0.1822 0.049 Uiso 1 1 calc R . . C42 C 0.0206(3) 0.7203(6) -0.1111(4) 0.031(2) Uani 1 1 d . . . C41 C 0.0251(3) 0.6414(6) -0.1511(4) 0.029(2) Uani 1 1 d . . . C40 C -0.0132(4) 0.6242(7) -0.2268(5) 0.043(2) Uani 1 1 d . . . H9 H -0.0418 0.6643 -0.2501 0.051 Uiso 1 1 calc R . . C39 C -0.0096(4) 0.5504(7) -0.2666(5) 0.048(3) Uani 1 1 d . . . H10 H -0.0354 0.5408 -0.3163 0.057 Uiso 1 1 calc R . . C38 C 0.0320(4) 0.4904(6) -0.2336(5) 0.044(2) Uani 1 1 d . . . H11 H 0.0340 0.4394 -0.2603 0.053 Uiso 1 1 calc R . . C37 C 0.0710(4) 0.5055(6) -0.1609(5) 0.039(2) Uani 1 1 d . . . H12 H 0.0997 0.4649 -0.1398 0.046 Uiso 1 1 calc R . . C36 C 0.0689(3) 0.5801(5) -0.1176(4) 0.026(2) Uani 1 1 d . . . C35 C 0.1117(3) 0.6013(5) -0.0427(4) 0.0241(19) Uani 1 1 d . . . C15 C 0.1588(3) 0.7680(5) 0.1113(4) 0.028(2) Uani 1 1 d . . . C16 C 0.1920(3) 0.8419(6) 0.1119(5) 0.033(2) Uani 1 1 d . . . C17 C 0.1899(4) 0.9117(6) 0.1592(5) 0.041(2) Uani 1 1 d . . . H17 H 0.2117 0.9610 0.1597 0.049 Uiso 1 1 calc R . . C18 C 0.1566(4) 0.9105(6) 0.2054(5) 0.045(2) Uani 1 1 d . . . H18 H 0.1543 0.9591 0.2346 0.054 Uiso 1 1 calc R . . C19 C 0.1268(4) 0.8353(6) 0.2072(5) 0.039(2) Uani 1 1 d . . . H19 H 0.1053 0.8332 0.2396 0.047 Uiso 1 1 calc R . . C20 C 0.1280(3) 0.7627(6) 0.1620(4) 0.030(2) Uani 1 1 d . . . C21 C 0.0932(3) 0.6822(6) 0.1670(5) 0.036(2) Uani 1 1 d . . . H21 H 0.1030 0.6348 0.1378 0.043 Uiso 1 1 calc R . . C22 C 0.0289(4) 0.6993(6) 0.1301(6) 0.054(3) Uani 1 1 d . . . H22A H 0.0176 0.7413 0.1609 0.081 Uiso 1 1 calc R . . H22B H 0.0086 0.6457 0.1282 0.081 Uiso 1 1 calc R . . H22C H 0.0205 0.7215 0.0783 0.081 Uiso 1 1 calc R . . C23 C 0.1082(4) 0.6520(6) 0.2518(5) 0.054(3) Uani 1 1 d . . . H23A H 0.1485 0.6475 0.2756 0.081 Uiso 1 1 calc R . . H23B H 0.0913 0.5960 0.2530 0.081 Uiso 1 1 calc R . . H23C H 0.0940 0.6937 0.2799 0.081 Uiso 1 1 calc R . . C24 C 0.2267(4) 0.8534(6) 0.0585(5) 0.045(3) Uani 1 1 d . . . H24 H 0.2336 0.7947 0.0423 0.054 Uiso 1 1 calc R . . C25 C 0.1935(5) 0.9031(7) -0.0157(6) 0.065(3) Uani 1 1 d . . . H25A H 0.1867 0.9618 -0.0026 0.097 Uiso 1 1 calc R . . H25B H 0.1580 0.8744 -0.0409 0.097 Uiso 1 1 calc R . . H25C H 0.2149 0.9044 -0.0502 0.097 Uiso 1 1 calc R . . C26 C 0.2842(4) 0.8947(7) 0.0975(6) 0.064(3) Uani 1 1 d . . . H26A H 0.2795 0.9543 0.1105 0.096 Uiso 1 1 calc R . . H26B H 0.3053 0.8932 0.0626 0.096 Uiso 1 1 calc R . . H26C H 0.3043 0.8630 0.1440 0.096 Uiso 1 1 calc R . . C27 C 0.1511(3) 0.4526(6) -0.0077(4) 0.028(2) Uani 1 1 d . . . C28 C 0.1144(3) 0.4106(6) 0.0210(5) 0.032(2) Uani 1 1 d . . . C29 C 0.1141(4) 0.3206(6) 0.0189(5) 0.045(2) Uani 1 1 d . . . H29 H 0.0901 0.2905 0.0389 0.054 Uiso 1 1 calc R . . C30 C 0.1485(4) 0.2735(7) -0.0122(6) 0.056(3) Uani 1 1 d . . . H30 H 0.1478 0.2127 -0.0125 0.067 Uiso 1 1 calc R . . C31 C 0.1831(4) 0.3178(7) -0.0421(5) 0.045(2) Uani 1 1 d . . . H31 H 0.2055 0.2867 -0.0643 0.053 Uiso 1 1 calc R . . C32 C 0.1859(3) 0.4082(6) -0.0404(5) 0.034(2) Uani 1 1 d . . . C33 C 0.0743(3) 0.4549(6) 0.0531(5) 0.043(2) Uani 1 1 d . . . H33A H 0.0851 0.5150 0.0639 0.065 Uiso 1 1 calc R . . H33B H 0.0752 0.4263 0.1002 0.065 Uiso 1 1 calc R . . H33C H 0.0366 0.4520 0.0157 0.065 Uiso 1 1 calc R . . C34 C 0.2223(4) 0.4527(6) -0.0793(5) 0.043(2) Uani 1 1 d . . . H34A H 0.1987 0.4799 -0.1265 0.064 Uiso 1 1 calc R . . H34B H 0.2463 0.4104 -0.0911 0.064 Uiso 1 1 calc R . . H34C H 0.2452 0.4963 -0.0451 0.064 Uiso 1 1 calc R . . C14 C 0.3753(3) 0.4122(5) 0.3356(4) 0.0198(18) Uani 1 1 d . . . C13 C 0.3990(3) 0.3391(5) 0.3886(4) 0.0228(19) Uani 1 1 d . . . C12 C 0.3667(3) 0.2702(5) 0.4014(4) 0.028(2) Uani 1 1 d . . . H37 H 0.3278 0.2706 0.3754 0.033 Uiso 1 1 calc R . . C11 C 0.3900(3) 0.2021(5) 0.4505(4) 0.029(2) Uani 1 1 d . . . H38 H 0.3675 0.1563 0.4563 0.035 Uiso 1 1 calc R . . C10 C 0.4472(4) 0.2025(6) 0.4912(5) 0.035(2) Uani 1 1 d . . . H39 H 0.4636 0.1569 0.5250 0.042 Uiso 1 1 calc R . . C9 C 0.4794(3) 0.2687(6) 0.4821(4) 0.033(2) Uani 1 1 d . . . H40 H 0.5179 0.2678 0.5108 0.040 Uiso 1 1 calc R . . C8 C 0.4580(3) 0.3395(5) 0.4316(4) 0.0229(19) Uani 1 1 d . . . C7 C 0.4949(3) 0.4115(5) 0.4248(4) 0.0226(18) Uani 1 1 d . . . C6 C 0.5524(3) 0.4130(6) 0.4693(4) 0.029(2) Uani 1 1 d . . . H43 H 0.5674 0.3663 0.5025 0.035 Uiso 1 1 calc R . . C5 C 0.5871(3) 0.4788(6) 0.4664(4) 0.031(2) Uani 1 1 d . . . H44 H 0.6255 0.4764 0.4953 0.037 Uiso 1 1 calc R . . C4 C 0.5645(3) 0.5502(6) 0.4194(5) 0.033(2) Uani 1 1 d . . . H45 H 0.5876 0.5971 0.4176 0.040 Uiso 1 1 calc R . . C3 C 0.5084(3) 0.5514(6) 0.3759(5) 0.033(2) Uani 1 1 d . . . H46 H 0.4940 0.6000 0.3449 0.040 Uiso 1 1 calc R . . C2 C 0.4712(3) 0.4824(5) 0.3757(4) 0.0256(19) Uani 1 1 d . . . C1 C 0.4110(3) 0.4816(5) 0.3281(4) 0.0190(18) Uani 1 1 d . . . C49 C 0.2836(3) 0.3445(5) 0.2626(4) 0.0183(17) Uani 1 1 d . . . C50 C 0.2364(3) 0.3381(5) 0.2862(4) 0.0220(18) Uani 1 1 d . . . C51 C 0.2023(3) 0.2645(6) 0.2631(5) 0.037(2) Uani 1 1 d . . . H51 H 0.1712 0.2580 0.2790 0.044 Uiso 1 1 calc R . . C52 C 0.2136(4) 0.2012(6) 0.2173(5) 0.045(3) Uani 1 1 d . . . H52 H 0.1900 0.1528 0.2023 0.054 Uiso 1 1 calc R . . C53 C 0.2596(4) 0.2090(6) 0.1933(5) 0.038(2) Uani 1 1 d . . . H53 H 0.2666 0.1656 0.1622 0.046 Uiso 1 1 calc R . . C54 C 0.2956(3) 0.2801(6) 0.2145(4) 0.030(2) Uani 1 1 d . . . C55 C 0.2241(3) 0.4061(6) 0.3385(4) 0.028(2) Uani 1 1 d . . . H55 H 0.2344 0.4631 0.3229 0.033 Uiso 1 1 calc R . . C56 C 0.2614(3) 0.3913(6) 0.4251(4) 0.034(2) Uani 1 1 d . . . H56A H 0.2565 0.3326 0.4401 0.051 Uiso 1 1 calc R . . H56B H 0.2504 0.4316 0.4575 0.051 Uiso 1 1 calc R . . H56C H 0.3004 0.4007 0.4313 0.051 Uiso 1 1 calc R . . C57 C 0.1618(3) 0.4108(6) 0.3311(5) 0.038(2) Uani 1 1 d . . . H57A H 0.1393 0.4245 0.2784 0.057 Uiso 1 1 calc R . . H57B H 0.1569 0.4554 0.3652 0.057 Uiso 1 1 calc R . . H57C H 0.1501 0.3554 0.3452 0.057 Uiso 1 1 calc R . . C58 C 0.3457(4) 0.2834(6) 0.1861(5) 0.036(2) Uani 1 1 d . . . H58 H 0.3635 0.3410 0.1998 0.043 Uiso 1 1 calc R . . C59 C 0.3900(4) 0.2150(6) 0.2250(5) 0.047(3) Uani 1 1 d . . . H59A H 0.3995 0.2185 0.2804 0.071 Uiso 1 1 calc R . . H59B H 0.4233 0.2253 0.2119 0.071 Uiso 1 1 calc R . . H59C H 0.3754 0.1579 0.2073 0.071 Uiso 1 1 calc R . . C60 C 0.3278(4) 0.2737(6) 0.0986(5) 0.048(3) Uani 1 1 d . . . H60A H 0.3111 0.2171 0.0836 0.072 Uiso 1 1 calc R . . H60B H 0.3603 0.2797 0.0828 0.072 Uiso 1 1 calc R . . H60C H 0.3006 0.3181 0.0739 0.072 Uiso 1 1 calc R . . C61 C 0.4124(3) 0.6009(6) 0.2371(4) 0.027(2) Uani 1 1 d . . . C62 C 0.4345(3) 0.5666(6) 0.1819(5) 0.031(2) Uani 1 1 d . . . C63 C 0.4565(3) 0.6262(7) 0.1417(5) 0.043(3) Uani 1 1 d . . . H63 H 0.4710 0.6057 0.1045 0.051 Uiso 1 1 calc R . . C64 C 0.4571(4) 0.7149(7) 0.1560(5) 0.047(3) Uani 1 1 d . . . H64 H 0.4705 0.7536 0.1271 0.056 Uiso 1 1 calc R . . C65 C 0.4379(4) 0.7459(6) 0.2128(5) 0.041(2) Uani 1 1 d . . . H65 H 0.4403 0.8054 0.2237 0.050 Uiso 1 1 calc R . . C66 C 0.4152(3) 0.6904(6) 0.2544(5) 0.032(2) Uani 1 1 d . . . C67 C 0.4358(3) 0.4713(6) 0.1666(5) 0.038(2) Uani 1 1 d . . . H67A H 0.4539 0.4616 0.1288 0.058 Uiso 1 1 calc R . . H67B H 0.3978 0.4492 0.1469 0.058 Uiso 1 1 calc R . . H67C H 0.4564 0.4416 0.2140 0.058 Uiso 1 1 calc R . . C68 C 0.3996(4) 0.7269(6) 0.3197(5) 0.040(2) Uani 1 1 d . . . H68A H 0.4296 0.7638 0.3511 0.060 Uiso 1 1 calc R . . H68B H 0.3938 0.6799 0.3509 0.060 Uiso 1 1 calc R . . H68C H 0.3655 0.7604 0.2992 0.060 Uiso 1 1 calc R . . C69 C 0.2214(4) 0.6817(6) -0.0792(4) 0.039(2) Uani 1 1 d . . . H69A H 0.2044 0.7387 -0.0797 0.047 Uiso 1 1 calc R . . H69B H 0.1920 0.6406 -0.1066 0.047 Uiso 1 1 calc R . . C70 C 0.2660(4) 0.6862(6) -0.1166(5) 0.046(3) Uani 1 1 d . . . H70A H 0.2572 0.7308 -0.1567 0.055 Uiso 1 1 calc R . . H70B H 0.2704 0.6304 -0.1391 0.055 Uiso 1 1 calc R . . C71 C 0.3186(4) 0.7098(7) -0.0479(5) 0.053(3) Uani 1 1 d . . . H71A H 0.3527 0.6922 -0.0574 0.064 Uiso 1 1 calc R . . H71B H 0.3202 0.7721 -0.0377 0.064 Uiso 1 1 calc R . . C72 C 0.3117(4) 0.6601(7) 0.0175(5) 0.048(3) Uani 1 1 d . . . H72A H 0.3287 0.6026 0.0212 0.058 Uiso 1 1 calc R . . H72B H 0.3294 0.6907 0.0663 0.058 Uiso 1 1 calc R . . C73 C 0.4013(5) 1.0077(9) 0.3325(7) 0.090(4) Uiso 1 1 d . . . H73A H 0.4150 1.0669 0.3323 0.107 Uiso 1 1 calc R . . H73B H 0.4136 0.9731 0.2968 0.107 Uiso 1 1 calc R . . Cl1 Cl 0.28272(8) 0.68228(14) 0.18247(11) 0.0323(5) Uani 1 1 d . . . Cl2 Cl 0.19794(8) 0.53311(14) 0.18301(11) 0.0284(5) Uani 1 1 d . . . Cl3 Cl 0.28853(8) 0.49342(14) 0.11062(11) 0.0285(5) Uani 1 1 d . . . Cl4 Cl 0.30016(8) 0.59315(14) 0.35582(11) 0.0312(5) Uani 1 1 d . . . Cl5 Cl 0.42992(14) 0.9636(2) 0.42716(19) 0.0906(10) Uiso 1 1 d . . . Cl6 Cl 0.3290(2) 1.0081(3) 0.3024(3) 0.1369(16) Uiso 1 1 d . . . Cr1 Cr 0.30225(5) 0.53668(9) 0.24068(7) 0.0239(3) Uani 1 1 d . . . Cr2 Cr 0.21578(5) 0.60497(9) 0.08067(7) 0.0252(3) Uani 1 1 d . . . N4 N 0.1571(2) 0.6969(4) 0.0586(3) 0.0211(15) Uani 1 1 d . . . N3 N 0.1545(2) 0.5477(4) -0.0017(3) 0.0223(15) Uani 1 1 d . . . N2 N 0.3214(2) 0.4195(4) 0.2855(3) 0.0243(16) Uani 1 1 d . . . N1 N 0.3846(2) 0.5428(4) 0.2740(3) 0.0237(15) Uani 1 1 d . . . O1 O 0.2504(2) 0.6528(3) 0.0005(3) 0.0279(14) 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 C48 0.036(5) 0.021(5) 0.020(4) 0.005(4) 0.014(4) 0.002(4) C47 0.036(5) 0.030(6) 0.018(4) 0.011(4) 0.011(4) 0.015(4) C46 0.068(7) 0.053(7) 0.031(5) -0.001(5) 0.005(5) 0.028(6) C45 0.085(8) 0.057(8) 0.049(7) 0.013(6) 0.020(6) 0.049(7) C44 0.047(6) 0.056(8) 0.054(7) 0.025(6) 0.016(5) 0.031(6) C43 0.040(5) 0.041(7) 0.041(6) 0.008(5) 0.014(5) 0.014(5) C42 0.034(5) 0.038(6) 0.025(5) 0.012(4) 0.016(4) 0.004(4) C41 0.030(5) 0.033(6) 0.025(5) 0.006(4) 0.011(4) -0.009(4) C40 0.033(5) 0.055(7) 0.037(6) 0.007(5) 0.008(4) 0.000(5) C39 0.033(5) 0.071(8) 0.032(6) 0.007(6) 0.002(4) 0.000(5) C38 0.063(7) 0.039(6) 0.031(5) -0.005(5) 0.016(5) -0.010(5) C37 0.046(6) 0.040(6) 0.029(5) 0.006(5) 0.013(4) 0.001(5) C36 0.034(5) 0.026(5) 0.020(4) 0.001(4) 0.011(4) 0.000(4) C35 0.028(4) 0.025(5) 0.025(4) 0.005(4) 0.017(4) 0.000(4) C15 0.036(5) 0.026(5) 0.020(4) -0.001(4) 0.009(4) 0.007(4) C16 0.043(5) 0.022(5) 0.035(5) -0.007(4) 0.014(4) -0.003(4) C17 0.053(6) 0.026(6) 0.049(6) -0.004(5) 0.023(5) -0.007(5) C18 0.065(7) 0.035(7) 0.038(6) -0.014(5) 0.019(5) -0.005(5) C19 0.045(5) 0.038(6) 0.037(5) 0.000(5) 0.018(4) 0.004(5) C20 0.036(5) 0.029(6) 0.024(5) -0.009(4) 0.008(4) 0.002(4) C21 0.040(5) 0.036(6) 0.039(5) -0.003(4) 0.024(4) 0.002(5) C22 0.048(6) 0.048(7) 0.070(7) -0.004(6) 0.026(5) -0.005(5) C23 0.068(7) 0.042(7) 0.063(7) -0.002(5) 0.037(6) -0.003(5) C24 0.066(7) 0.025(6) 0.054(6) 0.001(5) 0.032(5) -0.003(5) C25 0.100(9) 0.052(8) 0.057(7) 0.014(6) 0.047(7) 0.002(7) C26 0.083(8) 0.043(7) 0.088(8) -0.009(6) 0.057(7) -0.018(6) C27 0.031(5) 0.025(5) 0.021(4) 0.001(4) 0.000(4) 0.005(4) C28 0.033(5) 0.031(6) 0.034(5) -0.005(4) 0.013(4) -0.002(4) C29 0.056(6) 0.033(6) 0.045(6) -0.004(5) 0.014(5) -0.013(5) C30 0.071(7) 0.034(7) 0.051(7) -0.003(5) 0.007(6) -0.007(6) C31 0.056(6) 0.042(7) 0.038(6) -0.008(5) 0.019(5) 0.012(5) C32 0.039(5) 0.023(6) 0.034(5) 0.001(4) 0.003(4) 0.004(4) C33 0.037(5) 0.046(7) 0.044(6) 0.004(5) 0.010(4) -0.008(5) C34 0.058(6) 0.044(7) 0.029(5) -0.007(5) 0.018(5) 0.013(5) C14 0.028(4) 0.021(5) 0.013(4) 0.007(3) 0.012(3) 0.004(4) C13 0.031(4) 0.029(5) 0.013(4) 0.000(4) 0.014(4) 0.006(4) C12 0.035(5) 0.037(6) 0.015(4) 0.006(4) 0.014(4) 0.000(4) C11 0.040(5) 0.027(6) 0.026(5) 0.003(4) 0.020(4) -0.002(4) C10 0.049(6) 0.028(6) 0.033(5) 0.011(4) 0.019(5) 0.005(5) C9 0.030(5) 0.040(6) 0.028(5) 0.009(4) 0.009(4) 0.007(4) C8 0.036(5) 0.022(5) 0.015(4) -0.002(4) 0.014(4) 0.012(4) C7 0.030(4) 0.026(5) 0.013(4) 0.000(4) 0.008(3) 0.009(4) C6 0.023(4) 0.041(6) 0.021(4) 0.008(4) 0.006(4) 0.013(4) C5 0.026(4) 0.041(6) 0.028(5) -0.003(4) 0.013(4) 0.007(4) C4 0.027(5) 0.035(6) 0.036(5) -0.002(4) 0.008(4) -0.010(4) C3 0.039(5) 0.033(6) 0.029(5) 0.004(4) 0.013(4) 0.001(4) C2 0.029(4) 0.025(5) 0.023(4) -0.003(4) 0.010(4) 0.004(4) C1 0.026(4) 0.017(5) 0.015(4) 0.000(3) 0.009(3) 0.000(4) C49 0.026(4) 0.013(5) 0.016(4) 0.009(3) 0.007(3) 0.005(4) C50 0.027(4) 0.014(5) 0.023(4) 0.002(4) 0.006(4) 0.002(4) C51 0.036(5) 0.041(6) 0.038(5) 0.000(5) 0.019(4) -0.007(5) C52 0.063(7) 0.030(6) 0.042(6) -0.014(5) 0.018(5) -0.017(5) C53 0.048(6) 0.032(6) 0.037(5) -0.011(4) 0.017(5) -0.002(5) C54 0.034(5) 0.029(6) 0.026(5) 0.003(4) 0.008(4) -0.005(4) C55 0.029(4) 0.037(6) 0.018(4) 0.005(4) 0.008(4) -0.002(4) C56 0.043(5) 0.034(6) 0.030(5) -0.001(4) 0.021(4) -0.005(4) C57 0.043(5) 0.034(6) 0.045(6) 0.001(4) 0.025(5) 0.003(4) C58 0.052(6) 0.029(6) 0.030(5) -0.002(4) 0.019(4) 0.006(5) C59 0.045(6) 0.057(7) 0.043(6) 0.000(5) 0.020(5) 0.017(5) C60 0.068(7) 0.041(7) 0.040(6) 0.003(5) 0.025(5) 0.013(5) C61 0.019(4) 0.034(6) 0.025(4) 0.014(4) 0.004(3) -0.001(4) C62 0.026(4) 0.035(6) 0.035(5) 0.004(4) 0.015(4) -0.004(4) C63 0.033(5) 0.072(8) 0.032(5) 0.015(5) 0.022(4) 0.002(5) C64 0.056(6) 0.042(7) 0.045(6) 0.019(5) 0.021(5) -0.015(5) C65 0.049(6) 0.029(6) 0.044(6) 0.009(5) 0.013(5) -0.015(5) C66 0.033(5) 0.023(5) 0.040(5) 0.005(4) 0.012(4) -0.004(4) C67 0.038(5) 0.045(7) 0.040(5) -0.001(5) 0.024(4) 0.001(5) C68 0.042(5) 0.040(6) 0.033(5) -0.005(4) 0.006(4) -0.006(5) C69 0.059(6) 0.037(6) 0.024(5) 0.004(4) 0.015(4) 0.005(5) C70 0.063(6) 0.046(7) 0.039(6) -0.001(5) 0.029(5) -0.006(5) C71 0.054(6) 0.061(8) 0.050(6) 0.015(6) 0.024(5) 0.001(6) C72 0.043(6) 0.062(8) 0.043(6) 0.012(5) 0.018(5) -0.009(5) Cl1 0.0360(11) 0.0291(13) 0.0288(12) 0.0047(10) 0.0072(9) -0.0001(10) Cl2 0.0293(11) 0.0332(13) 0.0246(11) 0.0066(10) 0.0117(9) 0.0038(10) Cl3 0.0338(11) 0.0308(13) 0.0228(11) 0.0054(9) 0.0122(9) 0.0058(10) Cl4 0.0404(12) 0.0293(13) 0.0275(11) -0.0009(10) 0.0161(9) -0.0009(10) Cr1 0.0257(7) 0.0240(8) 0.0234(7) 0.0048(6) 0.0104(6) 0.0011(6) Cr2 0.0300(7) 0.0261(8) 0.0207(7) 0.0033(6) 0.0103(6) 0.0022(6) N4 0.031(4) 0.017(4) 0.017(3) 0.000(3) 0.010(3) 0.001(3) N3 0.025(4) 0.019(4) 0.024(4) 0.005(3) 0.010(3) 0.008(3) N2 0.022(3) 0.029(4) 0.023(4) 0.001(3) 0.009(3) 0.000(3) N1 0.028(4) 0.023(4) 0.023(4) 0.006(3) 0.013(3) -0.002(3) O1 0.031(3) 0.030(4) 0.026(3) 0.012(3) 0.014(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 C48 N4 1.351(9) . ? C48 C35 1.440(10) . ? C48 C47 1.475(10) . ? C47 C42 1.411(11) . ? C47 C46 1.414(12) . ? C46 C45 1.348(12) . ? C46 H3 0.9300 . ? C45 C44 1.389(13) . ? C45 H4 0.9300 . ? C44 C43 1.369(12) . ? C44 H5 0.9300 . ? C43 C42 1.405(11) . ? C43 H6 0.9300 . ? C42 C41 1.437(11) . ? C41 C40 1.415(11) . ? C41 C36 1.417(11) . ? C40 C39 1.363(12) . ? C40 H9 0.9300 . ? C39 C38 1.368(12) . ? C39 H10 0.9300 . ? C38 C37 1.373(11) . ? C38 H11 0.9300 . ? C37 C36 1.401(11) . ? C37 H12 0.9300 . ? C36 C35 1.459(10) . ? C35 N3 1.357(9) . ? C15 C20 1.400(10) . ? C15 C16 1.404(11) . ? C15 N4 1.445(9) . ? C16 C17 1.386(11) . ? C16 C24 1.527(11) . ? C17 C18 1.379(11) . ? C17 H17 0.9300 . ? C18 C19 1.379(12) . ? C18 H18 0.9300 . ? C19 C20 1.392(11) . ? C19 H19 0.9300 . ? C20 C21 1.532(11) . ? C21 C23 1.537(11) . ? C21 C22 1.548(11) . ? C21 H21 0.9800 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C26 1.515(12) . ? C24 C25 1.531(12) . ? C24 H24 0.9800 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C28 1.370(11) . ? C27 C32 1.393(11) . ? C27 N3 1.460(10) . ? C28 C29 1.378(12) . ? C28 C33 1.492(11) . ? C29 C30 1.389(13) . ? C29 H29 0.9300 . ? C30 C31 1.360(12) . ? C30 H30 0.9300 . ? C31 C32 1.385(12) . ? C31 H31 0.9300 . ? C32 C34 1.502(11) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C14 N2 1.357(9) . ? C14 C1 1.426(10) . ? C14 C13 1.466(10) . ? C13 C12 1.398(10) . ? C13 C8 1.422(10) . ? C12 C11 1.370(10) . ? C12 H37 0.9300 . ? C11 C10 1.376(11) . ? C11 H38 0.9300 . ? C10 C9 1.343(11) . ? C10 H39 0.9300 . ? C9 C8 1.405(10) . ? C9 H40 0.9300 . ? C8 C7 1.474(11) . ? C7 C6 1.395(10) . ? C7 C2 1.405(10) . ? C6 C5 1.347(11) . ? C6 H43 0.9300 . ? C5 C4 1.385(11) . ? C5 H44 0.9300 . ? C4 C3 1.362(10) . ? C4 H45 0.9300 . ? C3 C2 1.411(11) . ? C3 H46 0.9300 . ? C2 C1 1.466(10) . ? C1 N1 1.360(9) . ? C49 C50 1.401(10) . ? C49 C54 1.419(10) . ? C49 N2 1.457(9) . ? C50 C51 1.391(11) . ? C50 C55 1.515(10) . ? C51 C52 1.372(11) . ? C51 H51 0.9300 . ? C52 C53 1.376(11) . ? C52 H52 0.9300 . ? C53 C54 1.383(11) . ? C53 H53 0.9300 . ? C54 C58 1.520(11) . ? C55 C57 1.528(10) . ? C55 C56 1.557(10) . ? C55 H55 0.9800 . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C57 H57A 0.9600 . ? C57 H57B 0.9600 . ? C57 H57C 0.9600 . ? C58 C60 1.515(10) . ? C58 C59 1.518(11) . ? C58 H58 0.9800 . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? C60 H60A 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 0.9600 . ? C61 C66 1.403(11) . ? C61 C62 1.409(11) . ? C61 N1 1.435(9) . ? C62 C63 1.400(11) . ? C62 C67 1.487(11) . ? C63 C64 1.381(12) . ? C63 H63 0.9300 . ? C64 C65 1.371(12) . ? C64 H64 0.9300 . ? C65 C66 1.388(11) . ? C65 H65 0.9300 . ? C66 C68 1.487(11) . ? C67 H67A 0.9600 . ? C67 H67B 0.9600 . ? C67 H67C 0.9600 . ? C68 H68A 0.9600 . ? C68 H68B 0.9600 . ? C68 H68C 0.9600 . ? C69 O1 1.457(9) . ? C69 C70 1.502(11) . ? C69 H69A 0.9700 . ? C69 H69B 0.9700 . ? C70 C71 1.523(12) . ? C70 H70A 0.9700 . ? C70 H70B 0.9700 . ? C71 C72 1.478(11) . ? C71 H71A 0.9700 . ? C71 H71B 0.9700 . ? C72 O1 1.468(9) . ? C72 H72A 0.9700 . ? C72 H72B 0.9700 . ? C73 Cl6 1.712(12) . ? C73 Cl5 1.765(12) . ? C73 H73A 0.9700 . ? C73 H73B 0.9700 . ? Cl1 Cr2 2.357(2) . ? Cl1 Cr1 2.446(2) . ? Cl2 Cr2 2.343(2) . ? Cl2 Cr1 2.471(2) . ? Cl3 Cr1 2.378(2) . ? Cl3 Cr2 2.424(2) . ? Cl4 Cr1 2.294(2) . ? Cr1 N1 1.951(6) . ? Cr1 N2 1.963(6) . ? Cr2 N3 1.956(6) . ? Cr2 N4 1.978(6) . ? Cr2 O1 2.080(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 C48 C35 113.1(7) . . ? N4 C48 C47 128.0(7) . . ? C35 C48 C47 118.7(7) . . ? C42 C47 C46 116.6(7) . . ? C42 C47 C48 119.3(8) . . ? C46 C47 C48 124.0(7) . . ? C45 C46 C47 122.4(9) . . ? C45 C46 H3 118.8 . . ? C47 C46 H3 118.8 . . ? C46 C45 C44 120.3(10) . . ? C46 C45 H4 119.8 . . ? C44 C45 H4 119.8 . . ? C43 C44 C45 119.6(9) . . ? C43 C44 H5 120.2 . . ? C45 C44 H5 120.2 . . ? C44 C43 C42 120.8(9) . . ? C44 C43 H6 119.6 . . ? C42 C43 H6 119.6 . . ? C43 C42 C47 119.8(8) . . ? C43 C42 C41 119.7(8) . . ? C47 C42 C41 120.5(7) . . ? C40 C41 C36 117.9(8) . . ? C40 C41 C42 120.6(8) . . ? C36 C41 C42 121.5(7) . . ? C39 C40 C41 121.9(9) . . ? C39 C40 H9 119.1 . . ? C41 C40 H9 119.1 . . ? C40 C39 C38 120.1(9) . . ? C40 C39 H10 119.9 . . ? C38 C39 H10 119.9 . . ? C39 C38 C37 119.9(9) . . ? C39 C38 H11 120.1 . . ? C37 C38 H11 120.1 . . ? C38 C37 C36 122.2(9) . . ? C38 C37 H12 118.9 . . ? C36 C37 H12 118.9 . . ? C37 C36 C41 117.9(7) . . ? C37 C36 C35 123.7(7) . . ? C41 C36 C35 118.2(7) . . ? N3 C35 C48 114.2(7) . . ? N3 C35 C36 125.0(7) . . ? C48 C35 C36 120.7(7) . . ? C20 C15 C16 120.3(7) . . ? C20 C15 N4 120.2(7) . . ? C16 C15 N4 119.5(7) . . ? C17 C16 C15 118.5(8) . . ? C17 C16 C24 117.5(8) . . ? C15 C16 C24 123.9(7) . . ? C18 C17 C16 122.1(9) . . ? C18 C17 H17 118.9 . . ? C16 C17 H17 118.9 . . ? C19 C18 C17 118.4(9) . . ? C19 C18 H18 120.8 . . ? C17 C18 H18 120.8 . . ? C18 C19 C20 121.9(8) . . ? C18 C19 H19 119.0 . . ? C20 C19 H19 119.0 . . ? C19 C20 C15 118.5(8) . . ? C19 C20 C21 118.6(7) . . ? C15 C20 C21 122.9(7) . . ? C20 C21 C23 110.8(7) . . ? C20 C21 C22 111.8(7) . . ? C23 C21 C22 110.4(7) . . ? C20 C21 H21 107.9 . . ? C23 C21 H21 107.9 . . ? C22 C21 H21 107.9 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C26 C24 C16 114.3(8) . . ? C26 C24 C25 110.7(8) . . ? C16 C24 C25 111.5(8) . . ? C26 C24 H24 106.6 . . ? C16 C24 H24 106.6 . . ? C25 C24 H24 106.6 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C32 122.8(8) . . ? C28 C27 N3 117.9(7) . . ? C32 C27 N3 119.3(7) . . ? C27 C28 C29 117.1(8) . . ? C27 C28 C33 125.1(8) . . ? C29 C28 C33 117.9(8) . . ? C28 C29 C30 122.2(9) . . ? C28 C29 H29 118.9 . . ? C30 C29 H29 118.9 . . ? C31 C30 C29 118.7(10) . . ? C31 C30 H30 120.6 . . ? C29 C30 H30 120.6 . . ? C30 C31 C32 121.5(9) . . ? C30 C31 H31 119.2 . . ? C32 C31 H31 119.2 . . ? C31 C32 C27 117.6(8) . . ? C31 C32 C34 118.4(8) . . ? C27 C32 C34 123.8(8) . . ? C28 C33 H33A 109.5 . . ? C28 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C28 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N2 C14 C1 113.1(6) . . ? N2 C14 C13 126.4(7) . . ? C1 C14 C13 120.4(7) . . ? C12 C13 C8 117.8(7) . . ? C12 C13 C14 124.0(7) . . ? C8 C13 C14 118.2(7) . . ? C11 C12 C13 122.8(8) . . ? C11 C12 H37 118.6 . . ? C13 C12 H37 118.6 . . ? C12 C11 C10 119.0(8) . . ? C12 C11 H38 120.5 . . ? C10 C11 H38 120.5 . . ? C9 C10 C11 120.0(8) . . ? C9 C10 H39 120.0 . . ? C11 C10 H39 120.0 . . ? C10 C9 C8 123.5(8) . . ? C10 C9 H40 118.3 . . ? C8 C9 H40 118.3 . . ? C9 C8 C13 116.9(7) . . ? C9 C8 C7 121.4(7) . . ? C13 C8 C7 121.7(7) . . ? C6 C7 C2 119.2(7) . . ? C6 C7 C8 121.4(7) . . ? C2 C7 C8 119.3(7) . . ? C5 C6 C7 123.1(8) . . ? C5 C6 H43 118.4 . . ? C7 C6 H43 118.4 . . ? C6 C5 C4 118.7(8) . . ? C6 C5 H44 120.6 . . ? C4 C5 H44 120.6 . . ? C3 C4 C5 119.7(8) . . ? C3 C4 H45 120.1 . . ? C5 C4 H45 120.1 . . ? C4 C3 C2 123.0(8) . . ? C4 C3 H46 118.5 . . ? C2 C3 H46 118.5 . . ? C7 C2 C3 116.2(7) . . ? C7 C2 C1 119.9(7) . . ? C3 C2 C1 123.9(7) . . ? N1 C1 C14 114.6(6) . . ? N1 C1 C2 125.0(7) . . ? C14 C1 C2 120.4(7) . . ? C50 C49 C54 121.7(7) . . ? C50 C49 N2 120.3(7) . . ? C54 C49 N2 118.0(6) . . ? C51 C50 C49 117.6(7) . . ? C51 C50 C55 120.7(7) . . ? C49 C50 C55 121.7(7) . . ? C52 C51 C50 121.5(8) . . ? C52 C51 H51 119.3 . . ? C50 C51 H51 119.3 . . ? C51 C52 C53 120.4(8) . . ? C51 C52 H52 119.8 . . ? C53 C52 H52 119.8 . . ? C52 C53 C54 121.3(8) . . ? C52 C53 H53 119.3 . . ? C54 C53 H53 119.3 . . ? C53 C54 C49 117.5(7) . . ? C53 C54 C58 118.1(8) . . ? C49 C54 C58 124.4(7) . . ? C50 C55 C57 113.7(7) . . ? C50 C55 C56 111.1(6) . . ? C57 C55 C56 109.8(6) . . ? C50 C55 H55 107.3 . . ? C57 C55 H55 107.3 . . ? C56 C55 H55 107.3 . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C55 C57 H57A 109.5 . . ? C55 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C55 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C60 C58 C59 109.4(7) . . ? C60 C58 C54 112.1(7) . . ? C59 C58 C54 112.3(7) . . ? C60 C58 H58 107.6 . . ? C59 C58 H58 107.6 . . ? C54 C58 H58 107.6 . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C58 C60 H60A 109.5 . . ? C58 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C58 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C66 C61 C62 121.6(7) . . ? C66 C61 N1 119.5(7) . . ? C62 C61 N1 118.8(8) . . ? C63 C62 C61 117.3(8) . . ? C63 C62 C67 120.1(8) . . ? C61 C62 C67 122.6(7) . . ? C64 C63 C62 121.4(8) . . ? C64 C63 H63 119.3 . . ? C62 C63 H63 119.3 . . ? C65 C64 C63 120.0(8) . . ? C65 C64 H64 120.0 . . ? C63 C64 H64 120.0 . . ? C64 C65 C66 121.5(9) . . ? C64 C65 H65 119.3 . . ? C66 C65 H65 119.3 . . ? C65 C66 C61 118.1(8) . . ? C65 C66 C68 118.9(8) . . ? C61 C66 C68 122.8(7) . . ? C62 C67 H67A 109.5 . . ? C62 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C62 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C66 C68 H68A 109.5 . . ? C66 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C66 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? O1 C69 C70 105.9(7) . . ? O1 C69 H69A 110.6 . . ? C70 C69 H69A 110.6 . . ? O1 C69 H69B 110.6 . . ? C70 C69 H69B 110.6 . . ? H69A C69 H69B 108.7 . . ? C69 C70 C71 102.0(7) . . ? C69 C70 H70A 111.4 . . ? C71 C70 H70A 111.4 . . ? C69 C70 H70B 111.4 . . ? C71 C70 H70B 111.4 . . ? H70A C70 H70B 109.2 . . ? C72 C71 C70 103.7(8) . . ? C72 C71 H71A 111.0 . . ? C70 C71 H71A 111.0 . . ? C72 C71 H71B 111.0 . . ? C70 C71 H71B 111.0 . . ? H71A C71 H71B 109.0 . . ? O1 C72 C71 105.8(7) . . ? O1 C72 H72A 110.6 . . ? C71 C72 H72A 110.6 . . ? O1 C72 H72B 110.6 . . ? C71 C72 H72B 110.6 . . ? H72A C72 H72B 108.7 . . ? Cl6 C73 Cl5 110.4(7) . . ? Cl6 C73 H73A 109.6 . . ? Cl5 C73 H73A 109.6 . . ? Cl6 C73 H73B 109.6 . . ? Cl5 C73 H73B 109.6 . . ? H73A C73 H73B 108.1 . . ? Cr2 Cl1 Cr1 82.48(8) . . ? Cr2 Cl2 Cr1 82.20(7) . . ? Cr1 Cl3 Cr2 82.49(7) . . ? N1 Cr1 N2 80.3(3) . . ? N1 Cr1 Cl4 92.93(19) . . ? N2 Cr1 Cl4 92.29(18) . . ? N1 Cr1 Cl3 95.77(19) . . ? N2 Cr1 Cl3 95.43(19) . . ? Cl4 Cr1 Cl3 169.23(9) . . ? N1 Cr1 Cl1 97.2(2) . . ? N2 Cr1 Cl1 176.98(18) . . ? Cl4 Cr1 Cl1 89.54(8) . . ? Cl3 Cr1 Cl1 83.08(8) . . ? N1 Cr1 Cl2 173.28(18) . . ? N2 Cr1 Cl2 103.33(18) . . ? Cl4 Cr1 Cl2 92.57(8) . . ? Cl3 Cr1 Cl2 78.35(7) . . ? Cl1 Cr1 Cl2 78.98(8) . . ? N3 Cr2 N4 79.9(3) . . ? N3 Cr2 O1 91.4(2) . . ? N4 Cr2 O1 94.0(2) . . ? N3 Cr2 Cl2 95.10(19) . . ? N4 Cr2 Cl2 99.40(18) . . ? O1 Cr2 Cl2 165.95(16) . . ? N3 Cr2 Cl1 174.32(19) . . ? N4 Cr2 Cl1 94.91(19) . . ? O1 Cr2 Cl1 91.23(16) . . ? Cl2 Cr2 Cl1 83.41(8) . . ? N3 Cr2 Cl3 101.17(19) . . ? N4 Cr2 Cl3 178.77(19) . . ? O1 Cr2 Cl3 86.58(15) . . ? Cl2 Cr2 Cl3 79.96(8) . . ? Cl1 Cr2 Cl3 83.99(8) . . ? C48 N4 C15 121.3(6) . . ? C48 N4 Cr2 115.2(5) . . ? C15 N4 Cr2 123.4(5) . . ? C35 N3 C27 123.2(6) . . ? C35 N3 Cr2 114.9(5) . . ? C27 N3 Cr2 120.9(4) . . ? C14 N2 C49 122.2(6) . . ? C14 N2 Cr1 113.7(5) . . ? C49 N2 Cr1 123.9(4) . . ? C1 N1 C61 125.0(6) . . ? C1 N1 Cr1 113.3(5) . . ? C61 N1 Cr1 121.3(5) . . ? C69 O1 C72 108.6(6) . . ? C69 O1 Cr2 128.7(5) . . ? C72 O1 Cr2 122.7(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 C48 C47 C42 -176.7(7) . . . . ? C35 C48 C47 C42 -3.1(11) . . . . ? N4 C48 C47 C46 3.8(13) . . . . ? C35 C48 C47 C46 177.4(8) . . . . ? C42 C47 C46 C45 5.3(14) . . . . ? C48 C47 C46 C45 -175.2(9) . . . . ? C47 C46 C45 C44 1.2(16) . . . . ? C46 C45 C44 C43 -4.9(16) . . . . ? C45 C44 C43 C42 1.9(14) . . . . ? C44 C43 C42 C47 4.8(13) . . . . ? C44 C43 C42 C41 -176.2(8) . . . . ? C46 C47 C42 C43 -8.2(12) . . . . ? C48 C47 C42 C43 172.3(7) . . . . ? C46 C47 C42 C41 172.9(8) . . . . ? C48 C47 C42 C41 -6.6(11) . . . . ? C43 C42 C41 C40 13.4(12) . . . . ? C47 C42 C41 C40 -167.7(7) . . . . ? C43 C42 C41 C36 -168.8(7) . . . . ? C47 C42 C41 C36 10.1(12) . . . . ? C36 C41 C40 C39 1.3(12) . . . . ? C42 C41 C40 C39 179.2(8) . . . . ? C41 C40 C39 C38 -0.1(14) . . . . ? C40 C39 C38 C37 -1.5(14) . . . . ? C39 C38 C37 C36 1.8(13) . . . . ? C38 C37 C36 C41 -0.5(12) . . . . ? C38 C37 C36 C35 -175.6(8) . . . . ? C40 C41 C36 C37 -1.0(11) . . . . ? C42 C41 C36 C37 -178.9(7) . . . . ? C40 C41 C36 C35 174.4(7) . . . . ? C42 C41 C36 C35 -3.5(11) . . . . ? N4 C48 C35 N3 1.3(9) . . . . ? C47 C48 C35 N3 -173.1(6) . . . . ? N4 C48 C35 C36 -175.8(6) . . . . ? C47 C48 C35 C36 9.7(10) . . . . ? C37 C36 C35 N3 -8.2(12) . . . . ? C41 C36 C35 N3 176.7(7) . . . . ? C37 C36 C35 C48 168.6(7) . . . . ? C41 C36 C35 C48 -6.5(11) . . . . ? C20 C15 C16 C17 -5.1(12) . . . . ? N4 C15 C16 C17 175.7(7) . . . . ? C20 C15 C16 C24 -179.8(8) . . . . ? N4 C15 C16 C24 1.0(12) . . . . ? C15 C16 C17 C18 0.3(13) . . . . ? C24 C16 C17 C18 175.2(8) . . . . ? C16 C17 C18 C19 3.4(14) . . . . ? C17 C18 C19 C20 -2.3(13) . . . . ? C18 C19 C20 C15 -2.5(13) . . . . ? C18 C19 C20 C21 -179.4(8) . . . . ? C16 C15 C20 C19 6.2(12) . . . . ? N4 C15 C20 C19 -174.6(7) . . . . ? C16 C15 C20 C21 -177.0(7) . . . . ? N4 C15 C20 C21 2.2(12) . . . . ? C19 C20 C21 C23 -54.1(10) . . . . ? C15 C20 C21 C23 129.1(8) . . . . ? C19 C20 C21 C22 69.4(10) . . . . ? C15 C20 C21 C22 -107.4(9) . . . . ? C17 C16 C24 C26 45.1(12) . . . . ? C15 C16 C24 C26 -140.2(9) . . . . ? C17 C16 C24 C25 -81.3(10) . . . . ? C15 C16 C24 C25 93.4(10) . . . . ? C32 C27 C28 C29 2.2(12) . . . . ? N3 C27 C28 C29 -176.5(7) . . . . ? C32 C27 C28 C33 -176.8(8) . . . . ? N3 C27 C28 C33 4.5(12) . . . . ? C27 C28 C29 C30 -1.3(13) . . . . ? C33 C28 C29 C30 177.9(8) . . . . ? C28 C29 C30 C31 -0.6(14) . . . . ? C29 C30 C31 C32 1.7(14) . . . . ? C30 C31 C32 C27 -0.8(13) . . . . ? C30 C31 C32 C34 -176.0(8) . . . . ? C28 C27 C32 C31 -1.2(12) . . . . ? N3 C27 C32 C31 177.4(7) . . . . ? C28 C27 C32 C34 173.7(8) . . . . ? N3 C27 C32 C34 -7.6(11) . . . . ? N2 C14 C13 C12 -7.8(12) . . . . ? C1 C14 C13 C12 177.7(7) . . . . ? N2 C14 C13 C8 174.2(7) . . . . ? C1 C14 C13 C8 -0.2(10) . . . . ? C8 C13 C12 C11 -2.9(11) . . . . ? C14 C13 C12 C11 179.2(7) . . . . ? C13 C12 C11 C10 2.2(12) . . . . ? C12 C11 C10 C9 -0.4(12) . . . . ? C11 C10 C9 C8 -0.7(13) . . . . ? C10 C9 C8 C13 0.1(12) . . . . ? C10 C9 C8 C7 178.8(7) . . . . ? C12 C13 C8 C9 1.7(10) . . . . ? C14 C13 C8 C9 179.8(7) . . . . ? C12 C13 C8 C7 -177.1(7) . . . . ? C14 C13 C8 C7 1.0(10) . . . . ? C9 C8 C7 C6 -1.1(11) . . . . ? C13 C8 C7 C6 177.6(7) . . . . ? C9 C8 C7 C2 -177.6(7) . . . . ? C13 C8 C7 C2 1.1(10) . . . . ? C2 C7 C6 C5 -1.6(11) . . . . ? C8 C7 C6 C5 -178.0(7) . . . . ? C7 C6 C5 C4 2.7(12) . . . . ? C6 C5 C4 C3 -1.7(12) . . . . ? C5 C4 C3 C2 -0.2(12) . . . . ? C6 C7 C2 C3 -0.4(10) . . . . ? C8 C7 C2 C3 176.1(6) . . . . ? C6 C7 C2 C1 179.5(7) . . . . ? C8 C7 C2 C1 -4.0(10) . . . . ? C4 C3 C2 C7 1.3(12) . . . . ? C4 C3 C2 C1 -178.6(7) . . . . ? N2 C14 C1 N1 1.4(9) . . . . ? C13 C14 C1 N1 176.5(6) . . . . ? N2 C14 C1 C2 -177.7(6) . . . . ? C13 C14 C1 C2 -2.6(10) . . . . ? C7 C2 C1 N1 -174.3(7) . . . . ? C3 C2 C1 N1 5.6(12) . . . . ? C7 C2 C1 C14 4.8(10) . . . . ? C3 C2 C1 C14 -175.3(7) . . . . ? C54 C49 C50 C51 2.1(11) . . . . ? N2 C49 C50 C51 -179.3(7) . . . . ? C54 C49 C50 C55 179.1(7) . . . . ? N2 C49 C50 C55 -2.4(10) . . . . ? C49 C50 C51 C52 -1.5(12) . . . . ? C55 C50 C51 C52 -178.5(8) . . . . ? C50 C51 C52 C53 0.4(14) . . . . ? C51 C52 C53 C54 0.1(14) . . . . ? C52 C53 C54 C49 0.5(12) . . . . ? C52 C53 C54 C58 179.5(8) . . . . ? C50 C49 C54 C53 -1.7(11) . . . . ? N2 C49 C54 C53 179.8(7) . . . . ? C50 C49 C54 C58 179.4(7) . . . . ? N2 C49 C54 C58 0.8(11) . . . . ? C51 C50 C55 C57 -27.2(10) . . . . ? C49 C50 C55 C57 156.0(7) . . . . ? C51 C50 C55 C56 97.4(8) . . . . ? C49 C50 C55 C56 -79.5(9) . . . . ? C53 C54 C58 C60 54.0(10) . . . . ? C49 C54 C58 C60 -127.1(8) . . . . ? C53 C54 C58 C59 -69.6(10) . . . . ? C49 C54 C58 C59 109.3(9) . . . . ? C66 C61 C62 C63 -3.6(11) . . . . ? N1 C61 C62 C63 174.0(7) . . . . ? C66 C61 C62 C67 175.6(7) . . . . ? N1 C61 C62 C67 -6.8(11) . . . . ? C61 C62 C63 C64 0.8(12) . . . . ? C67 C62 C63 C64 -178.5(8) . . . . ? C62 C63 C64 C65 2.6(14) . . . . ? C63 C64 C65 C66 -3.1(14) . . . . ? C64 C65 C66 C61 0.3(13) . . . . ? C64 C65 C66 C68 174.9(8) . . . . ? C62 C61 C66 C65 3.1(12) . . . . ? N1 C61 C66 C65 -174.5(7) . . . . ? C62 C61 C66 C68 -171.3(7) . . . . ? N1 C61 C66 C68 11.1(11) . . . . ? O1 C69 C70 C71 -31.1(9) . . . . ? C69 C70 C71 C72 37.4(10) . . . . ? C70 C71 C72 O1 -30.0(10) . . . . ? Cr2 Cl3 Cr1 N1 -134.3(2) . . . . ? Cr2 Cl3 Cr1 N2 144.97(18) . . . . ? Cr2 Cl3 Cr1 Cl4 9.4(5) . . . . ? Cr2 Cl3 Cr1 Cl1 -37.67(7) . . . . ? Cr2 Cl3 Cr1 Cl2 42.45(7) . . . . ? Cr2 Cl1 Cr1 N1 133.92(19) . . . . ? Cr2 Cl1 Cr1 N2 99(4) . . . . ? Cr2 Cl1 Cr1 Cl4 -133.18(8) . . . . ? Cr2 Cl1 Cr1 Cl3 38.95(7) . . . . ? Cr2 Cl1 Cr1 Cl2 -40.47(7) . . . . ? Cr2 Cl2 Cr1 N1 -15.1(18) . . . . ? Cr2 Cl2 Cr1 N2 -137.22(19) . . . . ? Cr2 Cl2 Cr1 Cl4 129.82(8) . . . . ? Cr2 Cl2 Cr1 Cl3 -44.33(7) . . . . ? Cr2 Cl2 Cr1 Cl1 40.78(7) . . . . ? Cr1 Cl2 Cr2 N3 143.45(19) . . . . ? Cr1 Cl2 Cr2 N4 -135.96(19) . . . . ? Cr1 Cl2 Cr2 O1 26.1(7) . . . . ? Cr1 Cl2 Cr2 Cl1 -42.05(8) . . . . ? Cr1 Cl2 Cr2 Cl3 42.98(7) . . . . ? Cr1 Cl1 Cr2 N3 118(2) . . . . ? Cr1 Cl1 Cr2 N4 141.48(18) . . . . ? Cr1 Cl1 Cr2 O1 -124.42(15) . . . . ? Cr1 Cl1 Cr2 Cl2 42.56(7) . . . . ? Cr1 Cl1 Cr2 Cl3 -37.99(7) . . . . ? Cr1 Cl3 Cr2 N3 -138.33(18) . . . . ? Cr1 Cl3 Cr2 N4 14(9) . . . . ? Cr1 Cl3 Cr2 O1 130.87(16) . . . . ? Cr1 Cl3 Cr2 Cl2 -45.07(7) . . . . ? Cr1 Cl3 Cr2 Cl1 39.27(7) . . . . ? C35 C48 N4 C15 -165.3(6) . . . . ? C47 C48 N4 C15 8.5(12) . . . . ? C35 C48 N4 Cr2 10.7(8) . . . . ? C47 C48 N4 Cr2 -175.5(6) . . . . ? C20 C15 N4 C48 78.6(9) . . . . ? C16 C15 N4 C48 -102.2(9) . . . . ? C20 C15 N4 Cr2 -97.1(8) . . . . ? C16 C15 N4 Cr2 82.1(8) . . . . ? N3 Cr2 N4 C48 -13.8(5) . . . . ? O1 Cr2 N4 C48 76.9(5) . . . . ? Cl2 Cr2 N4 C48 -107.4(5) . . . . ? Cl1 Cr2 N4 C48 168.5(5) . . . . ? Cl3 Cr2 N4 C48 -166(9) . . . . ? N3 Cr2 N4 C15 162.2(6) . . . . ? O1 Cr2 N4 C15 -107.1(6) . . . . ? Cl2 Cr2 N4 C15 68.6(6) . . . . ? Cl1 Cr2 N4 C15 -15.5(6) . . . . ? Cl3 Cr2 N4 C15 10(9) . . . . ? C48 C35 N3 C27 156.1(7) . . . . ? C36 C35 N3 C27 -26.9(11) . . . . ? C48 C35 N3 Cr2 -12.9(8) . . . . ? C36 C35 N3 Cr2 164.1(6) . . . . ? C28 C27 N3 C35 -68.3(9) . . . . ? C32 C27 N3 C35 113.0(8) . . . . ? C28 C27 N3 Cr2 100.1(7) . . . . ? C32 C27 N3 Cr2 -78.6(8) . . . . ? N4 Cr2 N3 C35 14.4(5) . . . . ? O1 Cr2 N3 C35 -79.3(5) . . . . ? Cl2 Cr2 N3 C35 113.1(5) . . . . ? Cl1 Cr2 N3 C35 39(2) . . . . ? Cl3 Cr2 N3 C35 -166.1(5) . . . . ? N4 Cr2 N3 C27 -154.8(6) . . . . ? O1 Cr2 N3 C27 111.4(5) . . . . ? Cl2 Cr2 N3 C27 -56.2(5) . . . . ? Cl1 Cr2 N3 C27 -130.6(18) . . . . ? Cl3 Cr2 N3 C27 24.6(5) . . . . ? C1 C14 N2 C49 157.4(6) . . . . ? C13 C14 N2 C49 -17.3(11) . . . . ? C1 C14 N2 Cr1 -17.2(8) . . . . ? C13 C14 N2 Cr1 168.1(6) . . . . ? C50 C49 N2 C14 112.2(8) . . . . ? C54 C49 N2 C14 -69.3(9) . . . . ? C50 C49 N2 Cr1 -73.8(8) . . . . ? C54 C49 N2 Cr1 104.8(7) . . . . ? N1 Cr1 N2 C14 19.9(5) . . . . ? Cl4 Cr1 N2 C14 -72.7(5) . . . . ? Cl3 Cr1 N2 C14 114.8(5) . . . . ? Cl1 Cr1 N2 C14 55(4) . . . . ? Cl2 Cr1 N2 C14 -165.9(4) . . . . ? N1 Cr1 N2 C49 -154.6(6) . . . . ? Cl4 Cr1 N2 C49 112.8(5) . . . . ? Cl3 Cr1 N2 C49 -59.7(5) . . . . ? Cl1 Cr1 N2 C49 -120(4) . . . . ? Cl2 Cr1 N2 C49 19.6(6) . . . . ? C14 C1 N1 C61 -158.2(7) . . . . ? C2 C1 N1 C61 20.9(11) . . . . ? C14 C1 N1 Cr1 15.0(8) . . . . ? C2 C1 N1 Cr1 -165.9(6) . . . . ? C66 C61 N1 C1 -110.8(9) . . . . ? C62 C61 N1 C1 71.6(10) . . . . ? C66 C61 N1 Cr1 76.5(8) . . . . ? C62 C61 N1 Cr1 -101.2(7) . . . . ? N2 Cr1 N1 C1 -18.9(5) . . . . ? Cl4 Cr1 N1 C1 72.9(5) . . . . ? Cl3 Cr1 N1 C1 -113.4(5) . . . . ? Cl1 Cr1 N1 C1 162.8(5) . . . . ? Cl2 Cr1 N1 C1 -142.2(15) . . . . ? N2 Cr1 N1 C61 154.6(6) . . . . ? Cl4 Cr1 N1 C61 -113.6(6) . . . . ? Cl3 Cr1 N1 C61 60.1(6) . . . . ? Cl1 Cr1 N1 C61 -23.6(6) . . . . ? Cl2 Cr1 N1 C61 31(2) . . . . ? C70 C69 O1 C72 13.4(9) . . . . ? C70 C69 O1 Cr2 -165.1(5) . . . . ? C71 C72 O1 C69 10.7(10) . . . . ? C71 C72 O1 Cr2 -170.8(6) . . . . ? N3 Cr2 O1 C69 34.6(6) . . . . ? N4 Cr2 O1 C69 -45.4(6) . . . . ? Cl2 Cr2 O1 C69 152.4(6) . . . . ? Cl1 Cr2 O1 C69 -140.4(6) . . . . ? Cl3 Cr2 O1 C69 135.7(6) . . . . ? N3 Cr2 O1 C72 -143.7(6) . . . . ? N4 Cr2 O1 C72 136.4(6) . . . . ? Cl2 Cr2 O1 C72 -25.9(11) . . . . ? Cl1 Cr2 O1 C72 41.3(6) . . . . ? Cl3 Cr2 O1 C72 -42.6(6) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.620 _refine_diff_density_min -1.252 _refine_diff_density_rms 0.105