# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Prof. Xiao-Bing Lu' _publ_contact_author_email lxb-1999@163.com _publ_section_title ; Binuclear Half-metallocene Chromium(III) Complexes Mediated Ethylene Polymerization with Alkylaluminum as Cocatalyst ; loop_ _publ_author_name 'Tieqi Xu' 'Yu Pan' 'Xiao-Bing Lu' # Attachment '- complex 1.cif' data_cr2 _database_code_depnum_ccdc_archive 'CCDC 757579' #TrackingRef '- complex 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H60 Cl6 Cr2 N2 O2' _chemical_formula_weight 1037.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 '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 p21/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 16.312(4) _cell_length_b 12.288(4) _cell_length_c 29.792(6) _cell_angle_alpha 90.00 _cell_angle_beta 120.392(10) _cell_angle_gamma 90.00 _cell_volume 5151(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 30003 _cell_measurement_theta_min 2.08 _cell_measurement_theta_max 27.53 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.338 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2160 _exptl_absorpt_coefficient_mu 0.772 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.937 _exptl_absorpt_correction_T_max 0.951 _exptl_absorpt_process_details 'ABSCOR by T.Higashi 8 March, 1995' _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 'Bruker Smart Apex CCD' _diffrn_measurement_method \w-2\q _diffrn_detector_area_resol_mean 0.01 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 30003 _diffrn_reflns_av_R_equivalents 0.1294 _diffrn_reflns_av_sigmaI/netI 0.1573 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 27.53 _reflns_number_total 9789 _reflns_number_gt 3882 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0671P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9789 _refine_ls_number_parameters 572 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.2003 _refine_ls_R_factor_gt 0.0715 _refine_ls_wR_factor_ref 0.1936 _refine_ls_wR_factor_gt 0.1480 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr1 Cr 0.28146(7) 0.23983(7) 0.08885(4) 0.0415(3) Uani 1 1 d . . . Cr2 Cr 0.79184(7) 0.37605(7) 0.18357(4) 0.0437(3) Uani 1 1 d . . . Cl1 Cl 0.21718(14) 0.11748(14) 0.12107(7) 0.0720(6) Uani 1 1 d . . . Cl2 Cl 0.92608(14) 0.27773(16) 0.24011(8) 0.0782(6) Uani 1 1 d . . . O1 O 0.4118(3) 0.2064(3) 0.13290(15) 0.0501(12) Uani 1 1 d . . . O2 O 0.7012(3) 0.2913(3) 0.18935(17) 0.0485(12) Uani 1 1 d . . . N1 N 0.2748(4) 0.1249(4) 0.03731(18) 0.0439(14) Uani 1 1 d . . . N2 N 0.8052(4) 0.4762(4) 0.24131(19) 0.0410(14) Uani 1 1 d . . . C1 C 0.4714(4) 0.1366(4) 0.1317(2) 0.0399(16) Uani 1 1 d . . . C2 C 0.4417(4) 0.0649(4) 0.0884(2) 0.0385(16) Uani 1 1 d . . . C3 C 0.5069(5) -0.0064(4) 0.0876(2) 0.0479(18) Uani 1 1 d . . . H3A H 0.4871 -0.0520 0.0590 0.058 Uiso 1 1 calc R . . C4 C 0.5999(5) -0.0122(5) 0.1277(3) 0.0462(17) Uani 1 1 d . . . C5 C 0.6661(6) -0.0869(5) 0.1265(3) 0.064(2) Uani 1 1 d . . . H5A H 0.6461 -0.1341 0.0984 0.077 Uiso 1 1 calc R . . C6 C 0.7571(6) -0.0892(5) 0.1655(3) 0.069(2) Uani 1 1 d . . . H6A H 0.8003 -0.1360 0.1639 0.083 Uiso 1 1 calc R . . C7 C 0.7869(5) -0.0207(5) 0.2091(3) 0.062(2) Uani 1 1 d . . . H7A H 0.8496 -0.0241 0.2363 0.075 Uiso 1 1 calc R . . C8 C 0.7264(5) 0.0497(5) 0.2121(2) 0.0470(18) Uani 1 1 d . . . H8A H 0.7481 0.0935 0.2414 0.056 Uiso 1 1 calc R . . C9 C 0.6300(4) 0.0583(4) 0.1712(2) 0.0392(16) Uani 1 1 d . . . C10 C 0.5648(4) 0.1339(4) 0.1728(2) 0.0336(15) Uani 1 1 d . . . C11 C 0.6641(4) 0.2958(4) 0.2196(2) 0.0362(16) Uani 1 1 d . . . C12 C 0.6898(4) 0.3816(4) 0.2572(2) 0.0352(15) Uani 1 1 d . . . C13 C 0.6470(4) 0.3865(4) 0.2871(2) 0.0378(16) Uani 1 1 d . . . H13A H 0.6637 0.4431 0.3110 0.045 Uiso 1 1 calc R . . C14 C 0.5800(4) 0.3109(4) 0.2834(2) 0.0353(15) Uani 1 1 d . . . C15 C 0.5336(5) 0.3221(5) 0.3122(2) 0.0476(18) Uani 1 1 d . . . H15A H 0.5481 0.3808 0.3347 0.057 Uiso 1 1 calc R . . C16 C 0.4680(5) 0.2477(5) 0.3073(2) 0.0505(18) Uani 1 1 d . . . H16A H 0.4380 0.2548 0.3266 0.061 Uiso 1 1 calc R . . C17 C 0.4459(5) 0.1601(5) 0.2729(3) 0.0522(19) Uani 1 1 d . . . H17A H 0.4010 0.1092 0.2697 0.063 Uiso 1 1 calc R . . C18 C 0.4881(4) 0.1481(4) 0.2444(2) 0.0437(18) Uani 1 1 d . . . H18A H 0.4728 0.0880 0.2226 0.052 Uiso 1 1 calc R . . C19 C 0.5561(4) 0.2252(4) 0.2468(2) 0.0344(16) Uani 1 1 d . . . C20 C 0.5971(4) 0.2181(4) 0.2150(2) 0.0329(15) Uani 1 1 d . . . C21 C 0.3453(5) 0.0645(5) 0.0447(2) 0.0489(18) Uani 1 1 d . . . H21A H 0.3325 0.0142 0.0186 0.059 Uiso 1 1 calc R . . C22 C 0.7601(4) 0.4641(4) 0.2662(2) 0.0406(17) Uani 1 1 d . . . H22A H 0.7743 0.5135 0.2928 0.049 Uiso 1 1 calc R . . C23 C 0.1795(5) 0.0991(5) -0.0098(2) 0.058(2) Uani 1 1 d . . . H23A H 0.1339 0.1521 -0.0106 0.070 Uiso 1 1 calc R . . C24 C 0.1812(6) 0.1126(6) -0.0599(3) 0.086(3) Uani 1 1 d . . . H24A H 0.2197 0.1743 -0.0569 0.129 Uiso 1 1 calc R . . H24B H 0.1176 0.1238 -0.0883 0.129 Uiso 1 1 calc R . . H24C H 0.2073 0.0484 -0.0662 0.129 Uiso 1 1 calc R . . C25 C 0.1443(5) -0.0155(6) -0.0051(3) 0.088(3) Uani 1 1 d . . . H25A H 0.0814 -0.0274 -0.0340 0.132 Uiso 1 1 calc R . . H25B H 0.1434 -0.0200 0.0268 0.132 Uiso 1 1 calc R . . H25C H 0.1865 -0.0699 -0.0052 0.132 Uiso 1 1 calc R . . C26 C 0.8791(5) 0.5642(5) 0.2619(3) 0.057(2) Uani 1 1 d . . . H26A H 0.9045 0.5689 0.2384 0.068 Uiso 1 1 calc R . . C27 C 0.8369(5) 0.6749(5) 0.2614(3) 0.081(3) Uani 1 1 d . . . H27A H 0.7809 0.6867 0.2282 0.121 Uiso 1 1 calc R . . H27B H 0.8827 0.7307 0.2677 0.121 Uiso 1 1 calc R . . H27C H 0.8206 0.6772 0.2882 0.121 Uiso 1 1 calc R . . C28 C 0.9612(5) 0.5357(7) 0.3153(3) 0.099(3) Uani 1 1 d . . . H28A H 1.0154 0.5792 0.3226 0.149 Uiso 1 1 calc R . . H28B H 0.9767 0.4601 0.3161 0.149 Uiso 1 1 calc R . . H28C H 0.9434 0.5496 0.3409 0.149 Uiso 1 1 calc R . . C29 C 0.3294(5) 0.4136(5) 0.1048(3) 0.0489(19) Uani 1 1 d . . . C30 C 0.2765(5) 0.3976(5) 0.0500(3) 0.0518(19) Uani 1 1 d . . . C31 C 0.1820(5) 0.3732(5) 0.0375(3) 0.0518(19) Uani 1 1 d . . . C32 C 0.1795(5) 0.3691(5) 0.0831(3) 0.0526(19) Uani 1 1 d . . . C33 C 0.2723(5) 0.3948(5) 0.1256(3) 0.0492(18) Uani 1 1 d . . . C34 C 0.4329(5) 0.4452(6) 0.1348(3) 0.084(3) Uani 1 1 d . . . H34A H 0.4388 0.5221 0.1316 0.126 Uiso 1 1 calc R . . H34B H 0.4668 0.4066 0.1212 0.126 Uiso 1 1 calc R . . H34C H 0.4590 0.4269 0.1709 0.126 Uiso 1 1 calc R . . C35 C 0.3116(6) 0.4128(6) 0.0126(3) 0.092(3) Uani 1 1 d . . . H35A H 0.2638 0.4492 -0.0181 0.138 Uiso 1 1 calc R . . H35B H 0.3249 0.3431 0.0032 0.138 Uiso 1 1 calc R . . H35C H 0.3685 0.4559 0.0287 0.138 Uiso 1 1 calc R . . C36 C 0.0978(5) 0.3666(6) -0.0173(3) 0.086(3) Uani 1 1 d . . . H36A H 0.0736 0.4384 -0.0295 0.129 Uiso 1 1 calc R . . H36B H 0.0489 0.3227 -0.0174 0.129 Uiso 1 1 calc R . . H36C H 0.1173 0.3344 -0.0397 0.129 Uiso 1 1 calc R . . C37 C 0.0929(6) 0.3487(6) 0.0873(3) 0.096(3) Uani 1 1 d . . . H37A H 0.0535 0.4125 0.0765 0.144 Uiso 1 1 calc R . . H37B H 0.1119 0.3319 0.1227 0.144 Uiso 1 1 calc R . . H37C H 0.0579 0.2885 0.0654 0.144 Uiso 1 1 calc R . . C38 C 0.3020(6) 0.3992(6) 0.1824(3) 0.090(3) Uani 1 1 d . . . H38A H 0.3192 0.4724 0.1948 0.135 Uiso 1 1 calc R . . H38B H 0.3556 0.3521 0.2018 0.135 Uiso 1 1 calc R . . H38C H 0.2502 0.3758 0.1866 0.135 Uiso 1 1 calc R . . C39 C 0.6883(5) 0.3711(7) 0.0974(3) 0.061(2) Uani 1 1 d . . . C40 C 0.7116(6) 0.4785(6) 0.1132(3) 0.066(2) Uani 1 1 d . . . C41 C 0.8051(7) 0.4966(6) 0.1298(3) 0.065(2) Uani 1 1 d . . . C42 C 0.8437(6) 0.3984(8) 0.1276(3) 0.068(2) Uani 1 1 d U . . C43 C 0.7715(7) 0.3184(6) 0.1079(3) 0.065(2) Uani 1 1 d . . . C44 C 0.5924(6) 0.3205(8) 0.0746(3) 0.123(4) Uani 1 1 d . . . H44A H 0.5565 0.3359 0.0380 0.184 Uiso 1 1 calc R . . H44B H 0.5599 0.3500 0.0912 0.184 Uiso 1 1 calc R . . H44C H 0.5990 0.2432 0.0799 0.184 Uiso 1 1 calc R . . C45 C 0.6404(7) 0.5674(7) 0.1071(4) 0.125(4) Uani 1 1 d U . . H45A H 0.5914 0.5728 0.0713 0.188 Uiso 1 1 calc R . . H45B H 0.6728 0.6359 0.1186 0.188 Uiso 1 1 calc R . . H45C H 0.6124 0.5491 0.1278 0.188 Uiso 1 1 calc R . . C46 C 0.8582(7) 0.6044(7) 0.1439(3) 0.126(4) Uani 1 1 d U . . H46A H 0.8392 0.6457 0.1128 0.188 Uiso 1 1 calc R . . H46B H 0.9254 0.5909 0.1612 0.188 Uiso 1 1 calc R . . H46C H 0.8436 0.6447 0.1666 0.188 Uiso 1 1 calc R . . C47 C 0.9445(6) 0.3784(8) 0.1403(4) 0.123(4) Uani 1 1 d U . . H47A H 0.9496 0.3934 0.1102 0.185 Uiso 1 1 calc R . . H47B H 0.9612 0.3039 0.1505 0.185 Uiso 1 1 calc R . . H47C H 0.9868 0.4253 0.1683 0.185 Uiso 1 1 calc R . . C48 C 0.7799(7) 0.1986(7) 0.0996(3) 0.118(3) Uani 1 1 d U . . H48A H 0.7688 0.1873 0.0650 0.177 Uiso 1 1 calc R . . H48B H 0.7337 0.1587 0.1038 0.177 Uiso 1 1 calc R . . H48C H 0.8425 0.1736 0.1245 0.177 Uiso 1 1 calc R . . Cl3 Cl 0.3621(2) 0.7255(2) 0.04799(12) 0.1498(12) Uani 1 1 d . . . Cl4 Cl 0.1684(2) 0.6730(2) 0.01470(13) 0.1506(12) Uani 1 1 d . . . C49 C 0.2782(7) 0.7047(8) 0.0680(4) 0.124(4) Uani 1 1 d . . . H49A H 0.2992 0.6458 0.0931 0.149 Uiso 1 1 calc R . . H49B H 0.2730 0.7701 0.0846 0.149 Uiso 1 1 calc R . . Cl5 Cl 0.09776(19) 0.84141(19) 0.10505(10) 0.1156(9) Uani 1 1 d . . . Cl6 Cl 0.1347(3) 0.6215(3) 0.13994(13) 0.1979(17) Uani 1 1 d U . . C50 C 0.1056(8) 0.7405(7) 0.1479(4) 0.135(4) Uani 1 1 d . . . H50A H 0.1515 0.7640 0.1829 0.161 Uiso 1 1 calc R . . H50B H 0.0444 0.7356 0.1459 0.161 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 Cr1 0.0422(7) 0.0441(6) 0.0360(6) -0.0007(4) 0.0182(5) 0.0036(5) Cr2 0.0441(7) 0.0486(6) 0.0472(6) 0.0053(5) 0.0296(6) 0.0037(5) Cl1 0.0923(16) 0.0680(11) 0.0704(13) 0.0146(9) 0.0519(12) -0.0016(11) Cl2 0.0719(14) 0.0942(14) 0.0704(13) 0.0240(10) 0.0374(12) 0.0346(11) O1 0.038(3) 0.058(3) 0.041(3) -0.0133(19) 0.010(2) 0.009(2) O2 0.056(3) 0.050(2) 0.055(3) -0.010(2) 0.040(3) -0.014(2) N1 0.044(3) 0.047(3) 0.035(3) -0.010(2) 0.016(3) -0.004(3) N2 0.038(4) 0.050(3) 0.041(3) -0.001(2) 0.025(3) -0.004(2) C1 0.040(4) 0.038(3) 0.047(4) -0.006(3) 0.025(4) 0.002(3) C2 0.038(4) 0.043(3) 0.035(4) -0.005(3) 0.019(3) -0.002(3) C3 0.054(5) 0.038(3) 0.058(4) -0.014(3) 0.034(4) -0.001(3) C4 0.046(5) 0.042(4) 0.062(5) -0.003(3) 0.035(4) 0.003(3) C5 0.078(6) 0.053(4) 0.083(6) -0.005(4) 0.056(5) 0.021(4) C6 0.076(6) 0.058(5) 0.083(6) 0.005(4) 0.047(5) 0.026(4) C7 0.055(5) 0.064(5) 0.064(5) 0.010(4) 0.027(4) 0.018(4) C8 0.046(5) 0.048(4) 0.053(4) 0.007(3) 0.028(4) 0.010(3) C9 0.041(4) 0.036(3) 0.053(4) 0.004(3) 0.033(4) 0.001(3) C10 0.034(4) 0.033(3) 0.040(4) 0.000(2) 0.023(3) 0.004(3) C11 0.024(4) 0.047(4) 0.038(4) 0.006(3) 0.017(3) 0.004(3) C12 0.028(4) 0.043(3) 0.035(3) -0.004(3) 0.017(3) -0.003(3) C13 0.038(4) 0.033(3) 0.041(4) -0.001(3) 0.019(3) 0.002(3) C14 0.038(4) 0.040(3) 0.036(4) -0.002(3) 0.025(3) -0.007(3) C15 0.047(5) 0.056(4) 0.046(4) -0.010(3) 0.028(4) -0.010(3) C16 0.051(5) 0.075(5) 0.048(4) -0.006(3) 0.042(4) -0.006(4) C17 0.054(5) 0.057(4) 0.058(5) 0.001(3) 0.037(4) -0.011(3) C18 0.043(5) 0.041(4) 0.047(4) -0.005(3) 0.023(4) -0.004(3) C19 0.031(4) 0.039(3) 0.036(4) 0.000(2) 0.019(3) 0.004(3) C20 0.033(4) 0.033(3) 0.032(3) 0.000(2) 0.016(3) 0.003(3) C21 0.066(5) 0.050(4) 0.042(4) -0.011(3) 0.036(4) -0.008(4) C22 0.032(4) 0.040(3) 0.039(4) -0.007(3) 0.010(3) 0.000(3) C23 0.051(5) 0.077(5) 0.040(4) -0.010(3) 0.017(4) 0.005(4) C24 0.095(7) 0.093(6) 0.047(5) -0.008(4) 0.019(5) -0.006(5) C25 0.077(6) 0.086(6) 0.089(6) -0.020(5) 0.034(5) -0.037(5) C26 0.053(5) 0.070(5) 0.059(5) -0.002(3) 0.037(4) -0.026(4) C27 0.096(7) 0.055(5) 0.101(6) -0.012(4) 0.057(6) -0.027(4) C28 0.061(6) 0.125(7) 0.076(6) 0.011(5) 0.007(5) -0.027(5) C29 0.043(5) 0.045(4) 0.055(5) -0.004(3) 0.022(4) 0.006(3) C30 0.060(5) 0.044(4) 0.053(5) 0.006(3) 0.030(4) 0.005(3) C31 0.052(5) 0.043(4) 0.050(5) 0.004(3) 0.019(4) 0.006(3) C32 0.045(5) 0.055(4) 0.074(6) 0.009(4) 0.042(5) 0.017(3) C33 0.056(5) 0.051(4) 0.047(4) 0.004(3) 0.030(4) 0.018(3) C34 0.058(6) 0.066(5) 0.103(7) -0.008(4) 0.023(5) -0.013(4) C35 0.124(8) 0.094(6) 0.084(6) 0.010(5) 0.071(6) -0.023(5) C36 0.067(6) 0.074(5) 0.070(5) 0.000(4) -0.001(5) 0.010(4) C37 0.082(7) 0.088(6) 0.135(9) 0.009(5) 0.068(7) 0.031(5) C38 0.125(8) 0.084(6) 0.062(5) -0.005(4) 0.048(6) 0.027(5) C39 0.047(5) 0.095(6) 0.040(4) 0.010(4) 0.020(4) -0.008(5) C40 0.069(6) 0.067(5) 0.066(5) 0.020(4) 0.038(5) 0.032(5) C41 0.086(7) 0.072(5) 0.046(5) 0.007(4) 0.041(5) -0.020(5) C42 0.050(5) 0.111(6) 0.062(5) 0.015(4) 0.042(4) 0.017(4) C43 0.096(7) 0.059(5) 0.056(5) 0.004(4) 0.050(5) 0.012(5) C44 0.078(7) 0.183(10) 0.085(7) 0.002(7) 0.025(6) -0.037(7) C45 0.146(7) 0.129(6) 0.110(6) 0.027(5) 0.072(6) 0.061(6) C46 0.165(8) 0.129(7) 0.091(6) 0.009(5) 0.070(6) -0.049(6) C47 0.096(7) 0.184(8) 0.122(7) 0.025(6) 0.080(6) 0.012(6) C48 0.163(8) 0.092(6) 0.102(6) -0.007(5) 0.070(6) 0.021(5) Cl3 0.157(3) 0.150(3) 0.114(2) 0.0052(18) 0.048(2) -0.035(2) Cl4 0.137(3) 0.118(2) 0.154(3) -0.0152(19) 0.042(2) -0.0047(19) C49 0.136(10) 0.114(8) 0.110(8) 0.018(6) 0.052(8) 0.003(7) Cl5 0.125(2) 0.0941(17) 0.113(2) -0.0014(14) 0.0502(18) -0.0095(15) Cl6 0.274(4) 0.118(2) 0.131(3) 0.0219(19) 0.050(3) 0.061(3) C50 0.192(12) 0.090(7) 0.110(8) -0.024(6) 0.068(8) -0.042(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 O1 1.894(4) . ? Cr1 N1 2.049(5) . ? Cr1 C30 2.238(6) . ? Cr1 C33 2.239(6) . ? Cr1 C29 2.240(6) . ? Cr1 C32 2.244(6) . ? Cr1 C31 2.268(6) . ? Cr1 Cl1 2.302(2) . ? Cr2 O2 1.887(4) . ? Cr2 N2 2.036(5) . ? Cr2 C40 2.217(7) . ? Cr2 C43 2.222(7) . ? Cr2 C42 2.234(8) . ? Cr2 C39 2.249(7) . ? Cr2 C41 2.271(7) . ? Cr2 Cl2 2.315(2) . ? O1 C1 1.310(6) . ? O2 C11 1.316(7) . ? N1 C21 1.290(7) . ? N1 C23 1.511(7) . ? N2 C22 1.291(7) . ? N2 C26 1.500(7) . ? C1 C10 1.391(7) . ? C1 C2 1.430(7) . ? C2 C3 1.388(7) . ? C2 C21 1.448(8) . ? C3 C4 1.379(8) . ? C3 H3A 0.9300 . ? C4 C9 1.424(8) . ? C4 C5 1.432(8) . ? C5 C6 1.346(9) . ? C5 H5A 0.9300 . ? C6 C7 1.411(9) . ? C6 H6A 0.9300 . ? C7 C8 1.349(8) . ? C7 H7A 0.9300 . ? C8 C9 1.425(8) . ? C8 H8A 0.9300 . ? C9 C10 1.429(7) . ? C10 C20 1.503(7) . ? C11 C20 1.404(8) . ? C11 C12 1.438(8) . ? C12 C13 1.384(8) . ? C12 C22 1.450(8) . ? C13 C14 1.395(8) . ? C13 H13A 0.9300 . ? C14 C15 1.409(8) . ? C14 C19 1.422(7) . ? C15 C16 1.359(8) . ? C15 H15A 0.9300 . ? C16 C17 1.402(8) . ? C16 H16A 0.9300 . ? C17 C18 1.344(8) . ? C17 H17A 0.9300 . ? C18 C19 1.434(8) . ? C18 H18A 0.9300 . ? C19 C20 1.411(8) . ? C21 H21A 0.9300 . ? C22 H22A 0.9300 . ? C23 C24 1.515(9) . ? C23 C25 1.553(9) . ? C23 H23A 0.9800 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C27 1.521(9) . ? C26 C28 1.514(9) . ? C26 H26A 0.9800 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C33 1.376(9) . ? C29 C30 1.422(8) . ? C29 C34 1.508(8) . ? C30 C31 1.422(9) . ? C30 C35 1.500(9) . ? C31 C32 1.381(9) . ? C31 C36 1.514(9) . ? C32 C33 1.434(9) . ? C32 C37 1.501(9) . ? C33 C38 1.505(9) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 C43 1.389(9) . ? C39 C40 1.388(10) . ? C39 C44 1.490(10) . ? C40 C41 1.364(9) . ? C40 C45 1.538(10) . ? C41 C42 1.377(10) . ? C41 C46 1.521(10) . ? C42 C43 1.414(10) . ? C42 C47 1.510(10) . ? C43 C48 1.511(10) . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? Cl3 C49 1.766(10) . ? Cl4 C49 1.733(10) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? Cl5 C50 1.738(9) . ? Cl6 C50 1.592(9) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? 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 Cr1 N1 89.13(19) . . ? O1 Cr1 C30 106.3(2) . . ? N1 Cr1 C30 103.6(2) . . ? O1 Cr1 C33 100.1(2) . . ? N1 Cr1 C33 164.1(2) . . ? C30 Cr1 C33 61.5(2) . . ? O1 Cr1 C29 84.9(2) . . ? N1 Cr1 C29 134.1(3) . . ? C30 Cr1 C29 37.0(2) . . ? C33 Cr1 C29 35.8(2) . . ? O1 Cr1 C32 137.3(2) . . ? N1 Cr1 C32 132.5(2) . . ? C30 Cr1 C32 61.0(3) . . ? C33 Cr1 C32 37.3(2) . . ? C29 Cr1 C32 60.5(3) . . ? O1 Cr1 C31 142.5(2) . . ? N1 Cr1 C31 104.1(2) . . ? C30 Cr1 C31 36.8(2) . . ? C33 Cr1 C31 60.9(2) . . ? C29 Cr1 C31 60.5(2) . . ? C32 Cr1 C31 35.6(2) . . ? O1 Cr1 Cl1 99.06(14) . . ? N1 Cr1 Cl1 89.98(15) . . ? C30 Cr1 Cl1 151.2(2) . . ? C33 Cr1 Cl1 101.2(2) . . ? C29 Cr1 Cl1 135.9(2) . . ? C32 Cr1 Cl1 91.0(2) . . ? C31 Cr1 Cl1 115.6(2) . . ? O2 Cr2 N2 90.6(2) . . ? O2 Cr2 C40 106.5(3) . . ? N2 Cr2 C40 102.4(2) . . ? O2 Cr2 C43 101.2(3) . . ? N2 Cr2 C43 161.3(2) . . ? C40 Cr2 C43 60.5(3) . . ? O2 Cr2 C42 138.2(3) . . ? N2 Cr2 C42 129.6(3) . . ? C40 Cr2 C42 59.4(3) . . ? C43 Cr2 C42 37.0(3) . . ? O2 Cr2 C39 85.3(2) . . ? N2 Cr2 C39 132.7(3) . . ? C40 Cr2 C39 36.2(3) . . ? C43 Cr2 C39 36.2(2) . . ? C42 Cr2 C39 60.1(3) . . ? O2 Cr2 C41 141.6(3) . . ? N2 Cr2 C41 101.2(2) . . ? C40 Cr2 C41 35.3(2) . . ? C43 Cr2 C41 60.7(3) . . ? C42 Cr2 C41 35.6(3) . . ? C39 Cr2 C41 59.8(3) . . ? O2 Cr2 Cl2 98.18(14) . . ? N2 Cr2 Cl2 92.49(15) . . ? C40 Cr2 Cl2 150.8(2) . . ? C43 Cr2 Cl2 99.9(2) . . ? C42 Cr2 Cl2 91.8(2) . . ? C39 Cr2 Cl2 134.8(2) . . ? C41 Cr2 Cl2 117.4(3) . . ? C1 O1 Cr1 135.3(4) . . ? C11 O2 Cr2 133.8(4) . . ? C21 N1 C23 116.6(5) . . ? C21 N1 Cr1 124.3(4) . . ? C23 N1 Cr1 118.7(4) . . ? C22 N2 C26 115.0(5) . . ? C22 N2 Cr2 124.6(4) . . ? C26 N2 Cr2 120.1(4) . . ? O1 C1 C10 119.3(5) . . ? O1 C1 C2 120.7(5) . . ? C10 C1 C2 119.9(6) . . ? C3 C2 C1 119.5(6) . . ? C3 C2 C21 118.4(5) . . ? C1 C2 C21 122.1(6) . . ? C4 C3 C2 122.3(6) . . ? C4 C3 H3A 118.8 . . ? C2 C3 H3A 118.8 . . ? C3 C4 C9 118.6(6) . . ? C3 C4 C5 121.6(6) . . ? C9 C4 C5 119.8(6) . . ? C6 C5 C4 120.5(7) . . ? C6 C5 H5A 119.7 . . ? C4 C5 H5A 119.7 . . ? C5 C6 C7 119.9(7) . . ? C5 C6 H6A 120.0 . . ? C7 C6 H6A 120.0 . . ? C8 C7 C6 121.4(7) . . ? C8 C7 H7A 119.3 . . ? C6 C7 H7A 119.3 . . ? C7 C8 C9 121.3(6) . . ? C7 C8 H8A 119.4 . . ? C9 C8 H8A 119.4 . . ? C4 C9 C8 117.1(6) . . ? C4 C9 C10 120.4(6) . . ? C8 C9 C10 122.5(5) . . ? C1 C10 C9 119.3(5) . . ? C1 C10 C20 118.9(5) . . ? C9 C10 C20 121.5(5) . . ? O2 C11 C20 120.5(6) . . ? O2 C11 C12 120.7(6) . . ? C20 C11 C12 118.7(6) . . ? C13 C12 C11 119.4(6) . . ? C13 C12 C22 117.4(5) . . ? C11 C12 C22 123.2(6) . . ? C12 C13 C14 123.3(6) . . ? C12 C13 H13A 118.3 . . ? C14 C13 H13A 118.3 . . ? C13 C14 C15 121.7(6) . . ? C13 C14 C19 117.0(6) . . ? C15 C14 C19 121.2(6) . . ? C16 C15 C14 120.3(6) . . ? C16 C15 H15A 119.8 . . ? C14 C15 H15A 119.8 . . ? C15 C16 C17 119.6(7) . . ? C15 C16 H16A 120.2 . . ? C17 C16 H16A 120.2 . . ? C18 C17 C16 121.4(6) . . ? C18 C17 H17A 119.3 . . ? C16 C17 H17A 119.3 . . ? C17 C18 C19 121.9(6) . . ? C17 C18 H18A 119.1 . . ? C19 C18 H18A 119.1 . . ? C20 C19 C14 121.5(6) . . ? C20 C19 C18 123.0(6) . . ? C14 C19 C18 115.5(6) . . ? C11 C20 C19 120.1(5) . . ? C11 C20 C10 118.4(6) . . ? C19 C20 C10 121.3(5) . . ? N1 C21 C2 128.3(6) . . ? N1 C21 H21A 115.8 . . ? C2 C21 H21A 115.8 . . ? N2 C22 C12 127.0(6) . . ? N2 C22 H22A 116.5 . . ? C12 C22 H22A 116.5 . . ? C24 C23 N1 111.7(6) . . ? C24 C23 C25 112.3(6) . . ? N1 C23 C25 111.1(5) . . ? C24 C23 H23A 107.1 . . ? N1 C23 H23A 107.1 . . ? C25 C23 H23A 107.1 . . ? 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 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N2 C26 C27 112.0(5) . . ? N2 C26 C28 111.3(5) . . ? C27 C26 C28 111.8(6) . . ? N2 C26 H26A 107.1 . . ? C27 C26 H26A 107.1 . . ? C28 C26 H26A 107.1 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C33 C29 C30 109.8(6) . . ? C33 C29 C34 125.8(7) . . ? C30 C29 C34 124.3(8) . . ? C33 C29 Cr1 72.1(4) . . ? C30 C29 Cr1 71.4(3) . . ? C34 C29 Cr1 122.5(4) . . ? C29 C30 C31 106.1(7) . . ? C29 C30 C35 126.6(7) . . ? C31 C30 C35 127.1(7) . . ? C29 C30 Cr1 71.6(4) . . ? C31 C30 Cr1 72.8(4) . . ? C35 C30 Cr1 124.4(5) . . ? C32 C31 C30 108.6(6) . . ? C32 C31 C36 126.6(7) . . ? C30 C31 C36 124.4(7) . . ? C32 C31 Cr1 71.2(4) . . ? C30 C31 Cr1 70.5(4) . . ? C36 C31 Cr1 129.6(4) . . ? C31 C32 C33 108.5(7) . . ? C31 C32 C37 125.9(8) . . ? C33 C32 C37 125.5(8) . . ? C31 C32 Cr1 73.1(4) . . ? C33 C32 Cr1 71.2(4) . . ? C37 C32 Cr1 124.6(5) . . ? C29 C33 C32 106.9(6) . . ? C29 C33 C38 126.5(7) . . ? C32 C33 C38 126.6(8) . . ? C29 C33 Cr1 72.2(4) . . ? C32 C33 Cr1 71.5(4) . . ? C38 C33 Cr1 121.1(4) . . ? C29 C34 H34A 109.5 . . ? C29 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C29 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C30 C35 H35A 109.5 . . ? C30 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C30 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C31 C36 H36A 109.5 . . ? C31 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C31 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C33 C38 H38A 109.5 . . ? C33 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C33 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C43 C39 C40 107.3(7) . . ? C43 C39 C44 126.1(8) . . ? C40 C39 C44 126.5(9) . . ? C43 C39 Cr2 70.9(4) . . ? C40 C39 Cr2 70.6(4) . . ? C44 C39 Cr2 122.8(5) . . ? C41 C40 C39 110.0(7) . . ? C41 C40 C45 124.5(8) . . ? C39 C40 C45 125.1(9) . . ? C41 C40 Cr2 74.5(4) . . ? C39 C40 Cr2 73.1(4) . . ? C45 C40 Cr2 124.4(5) . . ? C40 C41 C42 107.1(7) . . ? C40 C41 C46 128.2(9) . . ? C42 C41 C46 124.5(9) . . ? C40 C41 Cr2 70.1(4) . . ? C42 C41 Cr2 70.7(4) . . ? C46 C41 Cr2 128.2(5) . . ? C41 C42 C43 109.0(7) . . ? C41 C42 C47 126.6(9) . . ? C43 C42 C47 124.3(9) . . ? C41 C42 Cr2 73.7(4) . . ? C43 C42 Cr2 71.0(4) . . ? C47 C42 Cr2 124.7(6) . . ? C39 C43 C42 106.4(7) . . ? C39 C43 C48 125.2(9) . . ? C42 C43 C48 128.3(9) . . ? C39 C43 Cr2 72.9(4) . . ? C42 C43 Cr2 72.0(4) . . ? C48 C43 Cr2 119.9(5) . . ? C39 C44 H44A 109.5 . . ? C39 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C39 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C40 C45 H45A 109.5 . . ? C40 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C40 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C41 C46 H46A 109.5 . . ? C41 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C41 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C42 C47 H47A 109.5 . . ? C42 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C42 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C43 C48 H48A 109.5 . . ? C43 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C43 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? Cl4 C49 Cl3 110.0(6) . . ? Cl4 C49 H49A 109.7 . . ? Cl3 C49 H49A 109.7 . . ? Cl4 C49 H49B 109.7 . . ? Cl3 C49 H49B 109.7 . . ? H49A C49 H49B 108.2 . . ? Cl6 C50 Cl5 117.5(6) . . ? Cl6 C50 H50A 107.9 . . ? Cl5 C50 H50A 107.9 . . ? Cl6 C50 H50B 107.9 . . ? Cl5 C50 H50B 107.9 . . ? H50A C50 H50B 107.2 . . ? _diffrn_measured_fraction_theta_max 0.824 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.854 _refine_diff_density_max 0.510 _refine_diff_density_min -0.509 _refine_diff_density_rms 0.074 # Attachment '- complex 3.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 821440' #TrackingRef '- complex 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H76 Cl2 Cr2 N2 O2' _chemical_formula_weight 1104.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 '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 P21/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 18.076(5) _cell_length_b 18.047(5) _cell_length_c 23.103(4) _cell_angle_alpha 90.00 _cell_angle_beta 125.714(14) _cell_angle_gamma 90.00 _cell_volume 6119(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 29922 _cell_measurement_theta_min 1.77 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.199 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2336 _exptl_absorpt_coefficient_mu 0.485 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.916 _exptl_absorpt_correction_T_max 0.939 _exptl_absorpt_process_details 'ABSCOR by T.Higashi 8 March, 1995' _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 'Bruker Smart Apex CCD' _diffrn_measurement_method \w-2\q _diffrn_detector_area_resol_mean 0.01 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 29922 _diffrn_reflns_av_R_equivalents 0.1491 _diffrn_reflns_av_sigmaI/netI 0.2055 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10750 _reflns_number_gt 4123 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0611P)^2^+6.9558P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10750 _refine_ls_number_parameters 685 _refine_ls_number_restraints 258 _refine_ls_R_factor_all 0.2369 _refine_ls_R_factor_gt 0.0940 _refine_ls_wR_factor_ref 0.2245 _refine_ls_wR_factor_gt 0.1695 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.004 _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 Cr1 Cr 0.17783(8) -0.48425(7) -0.13190(6) 0.0497(4) Uani 1 1 d . . . Cr2 Cr 0.33263(8) -0.43037(7) -0.33670(6) 0.0488(4) Uani 1 1 d . . . Cl1 Cl 0.14438(14) -0.60181(13) -0.11357(12) 0.0682(7) Uani 1 1 d . . . Cl2 Cl 0.39835(15) -0.37427(13) -0.22810(11) 0.0657(7) Uani 1 1 d . . . O1 O 0.2052(3) -0.5133(3) -0.1967(2) 0.0458(13) Uani 1 1 d . . . O2 O 0.2952(3) -0.5191(3) -0.3162(2) 0.0468(14) Uani 1 1 d . . . N1 N 0.0428(4) -0.4679(4) -0.2216(3) 0.0486(17) Uani 1 1 d . . . N2 N 0.4535(4) -0.4880(4) -0.3004(3) 0.0453(17) Uani 1 1 d . . . C1 C 0.1568(5) -0.5549(4) -0.2529(4) 0.0360(19) Uani 1 1 d . . . C2 C 0.0587(5) -0.5572(4) -0.2944(4) 0.042(2) Uani 1 1 d . . . C3 C 0.0100(5) -0.6003(4) -0.3537(4) 0.047(2) Uani 1 1 d . . . H3 H -0.0532 -0.6010 -0.3794 0.056 Uiso 1 1 calc R . . C4 C 0.0511(5) -0.6434(4) -0.3777(4) 0.0402(19) Uani 1 1 d . . . C5 C 0.0007(5) -0.6889(5) -0.4385(4) 0.054(2) Uani 1 1 d . . . H5 H -0.0623 -0.6912 -0.4635 0.065 Uiso 1 1 calc R . . C6 C 0.0425(6) -0.7298(5) -0.4613(4) 0.064(3) Uani 1 1 d . . . H6 H 0.0085 -0.7607 -0.5008 0.076 Uiso 1 1 calc R . . C7 C 0.1373(6) -0.7248(5) -0.4247(4) 0.063(3) Uani 1 1 d . . . H7 H 0.1658 -0.7510 -0.4413 0.075 Uiso 1 1 calc R . . C8 C 0.1881(5) -0.6821(4) -0.3654(4) 0.049(2) Uani 1 1 d . . . H8 H 0.2510 -0.6805 -0.3416 0.059 Uiso 1 1 calc R . . C9 C 0.1480(5) -0.6401(4) -0.3388(3) 0.041(2) Uani 1 1 d . . . C10 C 0.1998(5) -0.5975(4) -0.2757(3) 0.0348(18) Uani 1 1 d . . . C11 C 0.3444(5) -0.5566(4) -0.2562(4) 0.0367(19) Uani 1 1 d . . . C12 C 0.4412(5) -0.5607(4) -0.2173(4) 0.0373(19) Uani 1 1 d . . . C13 C 0.4915(5) -0.5994(4) -0.1544(4) 0.041(2) Uani 1 1 d . . . H13 H 0.5545 -0.6013 -0.1299 0.049 Uiso 1 1 calc R . . C14 C 0.4517(5) -0.6361(4) -0.1257(4) 0.0364(18) Uani 1 1 d . . . C15 C 0.5034(5) -0.6747(4) -0.0605(4) 0.048(2) Uani 1 1 d . . . H15 H 0.5666 -0.6748 -0.0340 0.058 Uiso 1 1 calc R . . C16 C 0.4613(6) -0.7115(5) -0.0362(4) 0.062(3) Uani 1 1 d . . . H16 H 0.4956 -0.7376 0.0065 0.074 Uiso 1 1 calc R . . C17 C 0.3667(6) -0.7104(5) -0.0750(4) 0.060(2) Uani 1 1 d . . . H17 H 0.3385 -0.7354 -0.0576 0.072 Uiso 1 1 calc R . . C18 C 0.3153(5) -0.6738(4) -0.1374(4) 0.046(2) Uani 1 1 d . . . H18 H 0.2523 -0.6741 -0.1620 0.056 Uiso 1 1 calc R . . C19 C 0.3541(5) -0.6350(4) -0.1663(4) 0.0388(19) Uani 1 1 d . . . C20 C 0.3009(5) -0.5966(4) -0.2321(3) 0.0338(18) Uani 1 1 d . . . C21 C 0.0095(5) -0.5077(4) -0.2779(4) 0.049(2) Uani 1 1 d . . . H21 H -0.0532 -0.5045 -0.3121 0.059 Uiso 1 1 calc R . . C22 C 0.4870(5) -0.5316(4) -0.2470(4) 0.044(2) Uani 1 1 d . . . H22 H 0.5472 -0.5462 -0.2249 0.052 Uiso 1 1 calc R . . C23 C -0.0229(5) -0.4148(6) -0.2259(4) 0.060(3) Uani 1 1 d . . . C24 C -0.0678(6) -0.4356(7) -0.1967(5) 0.076(3) Uani 1 1 d . . . C25 C -0.1276(7) -0.3821(8) -0.1992(6) 0.095(4) Uani 1 1 d . . . H25 H -0.1593 -0.3925 -0.1797 0.114 Uiso 1 1 calc R . . C26 C -0.1376(8) -0.3147(8) -0.2310(7) 0.102(4) Uani 1 1 d . . . H26 H -0.1763 -0.2797 -0.2323 0.123 Uiso 1 1 calc R . . C27 C -0.0945(7) -0.2974(6) -0.2601(6) 0.095(4) Uani 1 1 d . . . H27 H -0.1039 -0.2510 -0.2810 0.114 Uiso 1 1 calc R . . C28 C -0.0360(6) -0.3469(6) -0.2598(5) 0.067(3) Uani 1 1 d . . . C29 C -0.0669(8) -0.5152(8) -0.1724(6) 0.108(4) Uani 1 1 d U . . H29 H -0.0109 -0.5390 -0.1606 0.130 Uiso 1 1 calc R . . C30 C 0.0080(7) -0.3277(6) -0.2964(5) 0.085(3) Uani 1 1 d U . . H30 H 0.0615 -0.3596 -0.2770 0.102 Uiso 1 1 calc R . . C31 C -0.1456(10) -0.5605(8) -0.2294(7) 0.165(6) Uani 1 1 d U . . H31A H -0.2013 -0.5406 -0.2396 0.248 Uiso 1 1 calc R . . H31B H -0.1385 -0.6108 -0.2135 0.248 Uiso 1 1 calc R . . H31C H -0.1474 -0.5591 -0.2718 0.248 Uiso 1 1 calc R . . C32 C -0.0631(10) -0.5142(9) -0.1057(8) 0.184(6) Uani 1 1 d U . . H32A H -0.0209 -0.4769 -0.0739 0.277 Uiso 1 1 calc R . . H32B H -0.0436 -0.5618 -0.0830 0.277 Uiso 1 1 calc R . . H32C H -0.1226 -0.5033 -0.1177 0.277 Uiso 1 1 calc R . . C33 C -0.0568(7) -0.3418(6) -0.3764(5) 0.118(4) Uani 1 1 d U . . H33A H -0.1106 -0.3122 -0.3962 0.177 Uiso 1 1 calc R . . H33B H -0.0733 -0.3932 -0.3847 0.177 Uiso 1 1 calc R . . H33C H -0.0273 -0.3288 -0.3986 0.177 Uiso 1 1 calc R . . C34 C 0.0402(7) -0.2459(6) -0.2845(6) 0.118(4) Uani 1 1 d U . . H34A H -0.0117 -0.2137 -0.3056 0.177 Uiso 1 1 calc R . . H34B H 0.0713 -0.2374 -0.3062 0.177 Uiso 1 1 calc R . . H34C H 0.0808 -0.2361 -0.2343 0.177 Uiso 1 1 calc R . . C35 C 0.5076(6) -0.4813(6) -0.3286(5) 0.065(3) Uani 1 1 d U . . C36 C 0.4998(8) -0.5396(8) -0.3721(6) 0.100(4) Uani 1 1 d U . . C37 C 0.5512(10) -0.5330(9) -0.3999(7) 0.143(5) Uani 1 1 d U . . H37 H 0.5482 -0.5690 -0.4300 0.171 Uiso 1 1 calc R . . C38 C 0.6048(9) -0.4728(10) -0.3815(7) 0.131(5) Uani 1 1 d U . . H38 H 0.6393 -0.4705 -0.3995 0.157 Uiso 1 1 calc R . . C39 C 0.6142(8) -0.4156(7) -0.3401(6) 0.109(4) Uani 1 1 d U . . H39 H 0.6516 -0.3753 -0.3312 0.131 Uiso 1 1 calc R . . C40 C 0.5629(6) -0.4204(6) -0.3105(5) 0.073(3) Uani 1 1 d U . . C41 C 0.4398(10) -0.6088(8) -0.3889(7) 0.134(5) Uani 1 1 d U . . H41 H 0.3985 -0.5987 -0.3754 0.161 Uiso 1 1 calc R . . C42 C 0.5741(6) -0.3647(6) -0.2589(5) 0.082(3) Uani 1 1 d U . . H42 H 0.5163 -0.3604 -0.2643 0.098 Uiso 1 1 calc R . . C43 C 0.5046(12) -0.6698(9) -0.3418(8) 0.211(7) Uani 1 1 d U . . H43A H 0.5302 -0.6586 -0.2929 0.317 Uiso 1 1 calc R . . H43B H 0.5526 -0.6735 -0.3480 0.317 Uiso 1 1 calc R . . H43C H 0.4723 -0.7159 -0.3547 0.317 Uiso 1 1 calc R . . C44 C 0.3833(10) -0.6288(8) -0.4683(7) 0.192(7) Uani 1 1 d U . . H44A H 0.4231 -0.6442 -0.4807 0.288 Uiso 1 1 calc R . . H44B H 0.3490 -0.5862 -0.4961 0.288 Uiso 1 1 calc R . . H44C H 0.3422 -0.6684 -0.4777 0.288 Uiso 1 1 calc R . . C45 C 0.5989(7) -0.2883(6) -0.2719(6) 0.128(4) Uani 1 1 d U . . H45A H 0.5598 -0.2769 -0.3218 0.192 Uiso 1 1 calc R . . H45B H 0.6612 -0.2886 -0.2562 0.192 Uiso 1 1 calc R . . H45C H 0.5914 -0.2515 -0.2457 0.192 Uiso 1 1 calc R . . C46 C 0.6478(7) -0.3866(6) -0.1825(5) 0.109(4) Uani 1 1 d U . . H46A H 0.7048 -0.3916 -0.1765 0.163 Uiso 1 1 calc R . . H46B H 0.6320 -0.4329 -0.1719 0.163 Uiso 1 1 calc R . . H46C H 0.6532 -0.3491 -0.1508 0.163 Uiso 1 1 calc R . . C47 C 0.3059(5) -0.4801(5) -0.0202(4) 0.052(2) Uani 1 1 d U . . C48 C 0.3204(5) -0.4400(5) -0.0643(4) 0.050(2) Uani 1 1 d U . . C49 C 0.2597(6) -0.3808(5) -0.0943(4) 0.054(2) Uani 1 1 d U . . C50 C 0.2085(6) -0.3803(5) -0.0656(4) 0.059(2) Uani 1 1 d U . . C51 C 0.2345(6) -0.4434(5) -0.0216(4) 0.062(2) Uani 1 1 d U . . C52 C 0.3562(6) -0.5483(5) 0.0225(4) 0.079(3) Uani 1 1 d U . . H52A H 0.4080 -0.5340 0.0689 0.119 Uiso 1 1 calc R . . H52B H 0.3764 -0.5759 -0.0014 0.119 Uiso 1 1 calc R . . H52C H 0.3163 -0.5786 0.0272 0.119 Uiso 1 1 calc R . . C53 C 0.3881(5) -0.4591(5) -0.0801(4) 0.062(3) Uani 1 1 d U . . H53A H 0.4031 -0.5108 -0.0708 0.093 Uiso 1 1 calc R . . H53B H 0.4423 -0.4300 -0.0502 0.093 Uiso 1 1 calc R . . H53C H 0.3620 -0.4487 -0.1292 0.093 Uiso 1 1 calc R . . C54 C 0.2597(6) -0.3230(5) -0.1404(5) 0.086(3) Uani 1 1 d U . . H54A H 0.3127 -0.2923 -0.1121 0.129 Uiso 1 1 calc R . . H54B H 0.2059 -0.2931 -0.1615 0.129 Uiso 1 1 calc R . . H54C H 0.2604 -0.3465 -0.1773 0.129 Uiso 1 1 calc R . . C55 C 0.1427(6) -0.3215(5) -0.0761(5) 0.092(3) Uani 1 1 d U . . H55A H 0.1092 -0.3033 -0.1242 0.138 Uiso 1 1 calc R . . H55B H 0.1758 -0.2814 -0.0436 0.138 Uiso 1 1 calc R . . H55C H 0.1012 -0.3422 -0.0674 0.138 Uiso 1 1 calc R . . C56 C 0.2010(7) -0.4649(6) 0.0219(5) 0.104(4) Uani 1 1 d U . . H56A H 0.1815 -0.5157 0.0124 0.156 Uiso 1 1 calc R . . H56B H 0.1507 -0.4338 0.0096 0.156 Uiso 1 1 calc R . . H56C H 0.2493 -0.4591 0.0716 0.156 Uiso 1 1 calc R . . C57 C 0.2902(6) -0.3287(6) -0.4042(5) 0.075(3) Uani 1 1 d U . . C58 C 0.2875(7) -0.3866(7) -0.4438(5) 0.081(3) Uani 1 1 d U . . C59 C 0.2236(8) -0.4345(6) -0.4519(5) 0.087(3) Uani 1 1 d U . . C60 C 0.1868(6) -0.4077(7) -0.4204(6) 0.084(3) Uani 1 1 d U . . C61 C 0.2275(7) -0.3414(6) -0.3894(5) 0.074(3) Uani 1 1 d U . . C62 C 0.3464(8) -0.2571(6) -0.3819(6) 0.132(4) Uani 1 1 d U . . H62A H 0.3731 -0.2528 -0.4075 0.198 Uiso 1 1 calc R . . H62B H 0.3938 -0.2585 -0.3316 0.198 Uiso 1 1 calc R . . H62C H 0.3075 -0.2153 -0.3926 0.198 Uiso 1 1 calc R . . C63 C 0.3399(9) -0.3883(8) -0.4748(6) 0.168(6) Uani 1 1 d U . . H63A H 0.3956 -0.3610 -0.4447 0.252 Uiso 1 1 calc R . . H63B H 0.3043 -0.3663 -0.5214 0.252 Uiso 1 1 calc R . . H63C H 0.3538 -0.4387 -0.4783 0.252 Uiso 1 1 calc R . . C64 C 0.1911(10) -0.5081(9) -0.4911(7) 0.194(7) Uani 1 1 d U . . H64A H 0.1981 -0.5461 -0.4591 0.291 Uiso 1 1 calc R . . H64B H 0.2266 -0.5206 -0.5084 0.291 Uiso 1 1 calc R . . H64C H 0.1280 -0.5042 -0.5306 0.291 Uiso 1 1 calc R . . C65 C 0.1138(9) -0.4418(8) -0.4138(7) 0.160(5) Uani 1 1 d U . . H65A H 0.0558 -0.4194 -0.4483 0.241 Uiso 1 1 calc R . . H65B H 0.1299 -0.4331 -0.3668 0.241 Uiso 1 1 calc R . . H65C H 0.1101 -0.4942 -0.4224 0.241 Uiso 1 1 calc R . . C66 C 0.2075(8) -0.2892(7) -0.3491(6) 0.150(5) Uani 1 1 d U . . H66A H 0.1655 -0.3122 -0.3420 0.226 Uiso 1 1 calc R . . H66B H 0.1812 -0.2443 -0.3760 0.226 Uiso 1 1 calc R . . H66C H 0.2630 -0.2778 -0.3037 0.226 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 Cr1 0.0366(8) 0.0548(10) 0.0475(8) -0.0079(7) 0.0188(6) 0.0007(7) Cr2 0.0439(8) 0.0442(9) 0.0447(7) 0.0101(7) 0.0181(6) -0.0025(7) Cl1 0.0573(14) 0.0605(17) 0.0802(16) 0.0041(13) 0.0364(13) -0.0028(11) Cl2 0.0721(16) 0.0589(17) 0.0593(14) -0.0018(12) 0.0344(12) -0.0006(12) O1 0.034(3) 0.048(4) 0.046(3) -0.011(3) 0.018(3) -0.005(3) O2 0.034(3) 0.048(4) 0.045(3) 0.013(3) 0.015(3) -0.003(3) N1 0.034(4) 0.047(5) 0.055(4) -0.003(4) 0.020(3) 0.004(3) N2 0.042(4) 0.050(5) 0.045(4) 0.000(4) 0.026(3) -0.004(3) C1 0.033(5) 0.029(5) 0.034(4) 0.003(4) 0.013(4) -0.001(4) C2 0.033(5) 0.039(6) 0.041(4) 0.001(4) 0.013(4) 0.004(4) C3 0.028(4) 0.049(6) 0.039(5) 0.007(4) 0.006(4) -0.001(4) C4 0.042(5) 0.034(5) 0.029(4) 0.000(4) 0.012(4) -0.003(4) C5 0.038(5) 0.053(6) 0.050(5) 0.001(5) 0.014(4) -0.005(4) C6 0.064(7) 0.055(7) 0.050(5) -0.022(5) 0.021(5) -0.013(5) C7 0.064(6) 0.057(7) 0.055(6) -0.011(5) 0.028(5) 0.002(5) C8 0.043(5) 0.042(6) 0.053(5) -0.010(4) 0.023(4) -0.008(4) C9 0.033(5) 0.050(6) 0.030(4) 0.008(4) 0.013(4) 0.005(4) C10 0.033(4) 0.028(5) 0.031(4) 0.000(4) 0.012(4) -0.003(3) C11 0.037(5) 0.028(5) 0.040(4) 0.005(4) 0.019(4) 0.005(4) C12 0.033(5) 0.038(5) 0.036(4) -0.004(4) 0.018(4) -0.003(4) C13 0.029(4) 0.032(5) 0.043(5) -0.003(4) 0.011(4) 0.000(4) C14 0.039(5) 0.025(5) 0.036(4) -0.004(4) 0.017(4) -0.002(4) C15 0.040(5) 0.046(6) 0.046(5) 0.008(4) 0.018(4) 0.005(4) C16 0.064(6) 0.056(7) 0.049(5) 0.022(5) 0.024(5) 0.000(5) C17 0.053(6) 0.064(7) 0.055(5) 0.022(5) 0.027(5) 0.001(5) C18 0.042(5) 0.041(6) 0.052(5) 0.008(4) 0.026(4) -0.002(4) C19 0.039(5) 0.035(5) 0.040(4) -0.005(4) 0.021(4) -0.002(4) C20 0.030(4) 0.032(5) 0.032(4) -0.001(4) 0.014(4) -0.001(3) C21 0.022(4) 0.047(6) 0.057(5) -0.001(5) 0.011(4) 0.002(4) C22 0.035(5) 0.041(6) 0.044(5) 0.007(4) 0.017(4) 0.002(4) C23 0.030(5) 0.083(8) 0.050(5) -0.011(5) 0.014(4) 0.009(5) C24 0.051(6) 0.102(10) 0.083(7) 0.001(6) 0.043(6) 0.016(6) C25 0.063(7) 0.139(12) 0.098(9) -0.007(8) 0.055(7) 0.013(8) C26 0.072(8) 0.100(11) 0.128(11) -0.032(8) 0.054(8) 0.018(8) C27 0.060(7) 0.079(9) 0.133(10) -0.030(7) 0.049(7) 0.000(6) C28 0.044(6) 0.066(8) 0.074(7) -0.001(6) 0.025(5) 0.019(5) C29 0.092(7) 0.142(9) 0.123(7) 0.035(7) 0.081(6) 0.038(6) C30 0.075(6) 0.064(7) 0.105(7) 0.003(5) 0.047(5) 0.013(5) C31 0.177(9) 0.142(9) 0.190(9) 0.007(7) 0.115(8) 0.012(7) C32 0.184(10) 0.228(11) 0.179(9) 0.037(8) 0.128(8) -0.002(8) C33 0.124(8) 0.109(8) 0.110(7) -0.002(6) 0.062(6) 0.001(6) C34 0.093(7) 0.088(8) 0.147(8) 0.021(6) 0.056(6) 0.006(6) C35 0.065(5) 0.066(6) 0.060(5) 0.010(5) 0.034(4) 0.001(5) C36 0.114(7) 0.122(8) 0.095(6) -0.001(6) 0.079(6) 0.008(6) C37 0.166(9) 0.159(10) 0.129(8) -0.006(7) 0.102(7) 0.010(7) C38 0.138(9) 0.162(10) 0.127(8) 0.014(7) 0.098(7) -0.004(7) C39 0.109(7) 0.118(8) 0.116(7) 0.024(6) 0.075(6) -0.012(6) C40 0.061(5) 0.090(7) 0.072(6) 0.027(5) 0.042(5) 0.006(5) C41 0.162(9) 0.133(9) 0.114(8) -0.027(7) 0.084(7) 0.003(7) C42 0.063(6) 0.073(7) 0.093(6) 0.032(5) 0.036(5) -0.018(5) C43 0.243(11) 0.192(11) 0.195(10) -0.006(8) 0.125(8) 0.028(8) C44 0.224(11) 0.179(10) 0.168(9) -0.035(8) 0.112(8) 0.001(8) C45 0.120(6) 0.116(6) 0.131(6) 0.015(4) 0.064(4) -0.013(4) C46 0.112(7) 0.109(8) 0.095(7) 0.023(6) 0.055(6) -0.015(6) C47 0.035(4) 0.060(6) 0.052(5) -0.005(4) 0.021(4) 0.004(4) C48 0.035(4) 0.057(6) 0.042(4) -0.008(4) 0.013(4) -0.003(4) C49 0.051(5) 0.049(6) 0.045(4) -0.009(4) 0.018(4) -0.002(4) C50 0.055(5) 0.053(6) 0.053(5) -0.018(4) 0.022(4) 0.005(4) C51 0.057(5) 0.070(6) 0.055(5) -0.019(4) 0.031(4) -0.007(4) C52 0.074(6) 0.072(6) 0.069(5) -0.002(5) 0.029(4) 0.004(5) C53 0.046(5) 0.076(6) 0.062(5) -0.018(4) 0.030(4) -0.006(4) C54 0.074(6) 0.071(7) 0.087(6) -0.007(5) 0.032(5) -0.005(5) C55 0.074(6) 0.089(7) 0.097(6) -0.036(5) 0.041(5) 0.012(5) C56 0.110(7) 0.132(8) 0.093(6) -0.018(6) 0.072(6) -0.008(6) C57 0.062(6) 0.066(7) 0.069(6) 0.029(5) 0.022(5) -0.009(5) C58 0.083(6) 0.104(8) 0.060(5) 0.037(5) 0.044(5) 0.032(6) C59 0.089(5) 0.069(5) 0.069(5) 0.005(4) 0.027(4) -0.001(4) C60 0.051(5) 0.074(7) 0.086(6) 0.052(5) 0.017(5) -0.008(5) C61 0.067(6) 0.074(7) 0.065(5) 0.021(5) 0.029(5) 0.022(5) C62 0.125(6) 0.115(6) 0.133(6) 0.016(4) 0.062(4) -0.012(4) C63 0.192(10) 0.202(10) 0.128(8) 0.051(7) 0.104(7) 0.048(8) C64 0.200(8) 0.178(8) 0.178(8) -0.003(4) 0.095(5) 0.006(4) C65 0.149(7) 0.156(7) 0.165(7) 0.028(4) 0.084(5) -0.009(4) C66 0.144(8) 0.150(9) 0.140(8) 0.006(7) 0.072(7) 0.056(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 O1 1.905(5) . ? Cr1 N1 2.106(6) . ? Cr1 C49 2.220(8) . ? Cr1 C48 2.240(7) . ? Cr1 C51 2.246(8) . ? Cr1 C47 2.247(7) . ? Cr1 C50 2.276(8) . ? Cr1 Cl1 2.312(3) . ? Cr2 O2 1.902(5) . ? Cr2 N2 2.102(6) . ? Cr2 C60 2.214(9) . ? Cr2 C59 2.203(10) . ? Cr2 C61 2.229(9) . ? Cr2 C58 2.247(9) . ? Cr2 C57 2.234(9) . ? Cr2 Cl2 2.292(2) . ? O1 C1 1.299(8) . ? O2 C11 1.318(7) . ? N1 C21 1.288(9) . ? N1 C23 1.483(10) . ? N2 C22 1.279(8) . ? N2 C35 1.463(10) . ? C1 C10 1.396(9) . ? C1 C2 1.443(9) . ? C2 C3 1.361(9) . ? C2 C21 1.458(10) . ? C3 C4 1.395(10) . ? C3 H3 0.9300 . ? C4 C5 1.409(10) . ? C4 C9 1.427(9) . ? C5 C6 1.363(10) . ? C5 H5 0.9300 . ? C6 C7 1.404(10) . ? C6 H6 0.9300 . ? C7 C8 1.359(10) . ? C7 H7 0.9300 . ? C8 C9 1.414(9) . ? C8 H8 0.9300 . ? C9 C10 1.414(9) . ? C10 C20 1.486(9) . ? C11 C20 1.399(9) . ? C11 C12 1.429(9) . ? C12 C13 1.374(9) . ? C12 C22 1.446(9) . ? C13 C14 1.396(9) . ? C13 H13 0.9300 . ? C14 C15 1.409(9) . ? C14 C19 1.436(9) . ? C15 C16 1.355(10) . ? C15 H15 0.9300 . ? C16 C17 1.392(10) . ? C16 H16 0.9300 . ? C17 C18 1.347(9) . ? C17 H17 0.9300 . ? C18 C19 1.406(9) . ? C18 H18 0.9300 . ? C19 C20 1.417(9) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.377(12) . ? C23 C28 1.398(12) . ? C24 C25 1.425(13) . ? C24 C29 1.539(14) . ? C25 C26 1.379(14) . ? C25 H25 0.9300 . ? C26 C27 1.328(14) . ? C26 H26 0.9300 . ? C27 C28 1.383(12) . ? C27 H27 0.9300 . ? C28 C30 1.502(12) . ? C29 C32 1.501(14) . ? C29 C31 1.497(15) . ? C29 H29 0.9800 . ? C30 C33 1.524(12) . ? C30 C34 1.550(13) . ? C30 H30 0.9800 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 C40 1.376(12) . ? C35 C36 1.405(13) . ? C36 C37 1.408(15) . ? C36 C41 1.547(15) . ? C37 C38 1.348(16) . ? C37 H37 0.9300 . ? C38 C39 1.351(15) . ? C38 H38 0.9300 . ? C39 C40 1.441(12) . ? C39 H39 0.9300 . ? C40 C42 1.480(13) . ? C41 C43 1.509(17) . ? C41 C44 1.533(14) . ? C41 H41 0.9800 . ? C42 C46 1.516(11) . ? C42 C45 1.534(12) . ? C42 H42 0.9800 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 C48 1.393(10) . ? C47 C51 1.435(10) . ? C47 C52 1.507(11) . ? C48 C49 1.393(10) . ? C48 C53 1.506(10) . ? C49 C50 1.416(11) . ? C49 C54 1.490(11) . ? C50 C51 1.412(11) . ? C50 C55 1.505(11) . ? C51 C56 1.496(11) . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C57 C58 1.370(13) . ? C57 C61 1.380(12) . ? C57 C62 1.535(13) . ? C58 C59 1.365(14) . ? C58 C63 1.486(13) . ? C59 C60 1.332(13) . ? C59 C64 1.519(16) . ? C60 C61 1.367(13) . ? C60 C65 1.542(14) . ? C61 C66 1.511(13) . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? C65 H65A 0.9600 . ? C65 H65B 0.9600 . ? C65 H65C 0.9600 . ? C66 H66A 0.9600 . ? C66 H66B 0.9600 . ? C66 H66C 0.9600 . ? 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 Cr1 N1 87.1(2) . . ? O1 Cr1 C49 96.9(3) . . ? N1 Cr1 C49 113.1(3) . . ? O1 Cr1 C48 85.7(3) . . ? N1 Cr1 C48 146.8(3) . . ? C49 Cr1 C48 36.4(3) . . ? O1 Cr1 C51 145.8(3) . . ? N1 Cr1 C51 124.7(3) . . ? C49 Cr1 C51 61.4(3) . . ? C48 Cr1 C51 61.0(3) . . ? O1 Cr1 C47 110.2(3) . . ? N1 Cr1 C47 161.9(3) . . ? C49 Cr1 C47 61.2(3) . . ? C48 Cr1 C47 36.2(3) . . ? C51 Cr1 C47 37.3(3) . . ? O1 Cr1 C50 133.0(3) . . ? N1 Cr1 C50 103.5(3) . . ? C49 Cr1 C50 36.7(3) . . ? C48 Cr1 C50 60.5(3) . . ? C51 Cr1 C50 36.4(3) . . ? C47 Cr1 C50 61.1(3) . . ? O1 Cr1 Cl1 96.17(17) . . ? N1 Cr1 Cl1 91.86(19) . . ? C49 Cr1 Cl1 152.4(2) . . ? C48 Cr1 Cl1 121.1(2) . . ? C51 Cr1 Cl1 95.1(3) . . ? C47 Cr1 Cl1 91.4(2) . . ? C50 Cr1 Cl1 128.3(3) . . ? O2 Cr2 N2 85.5(2) . . ? O2 Cr2 C60 87.6(3) . . ? N2 Cr2 C60 150.4(4) . . ? O2 Cr2 C59 94.3(4) . . ? N2 Cr2 C59 117.0(4) . . ? C60 Cr2 C59 35.1(4) . . ? O2 Cr2 C61 115.4(3) . . ? N2 Cr2 C61 158.5(4) . . ? C60 Cr2 C61 35.8(3) . . ? C59 Cr2 C61 59.2(4) . . ? O2 Cr2 C58 128.0(4) . . ? N2 Cr2 C58 103.8(3) . . ? C60 Cr2 C58 59.4(4) . . ? C59 Cr2 C58 35.7(4) . . ? C61 Cr2 C58 60.0(4) . . ? O2 Cr2 C57 146.9(3) . . ? N2 Cr2 C57 122.6(4) . . ? C60 Cr2 C57 59.3(3) . . ? C59 Cr2 C57 58.9(4) . . ? C61 Cr2 C57 36.0(3) . . ? C58 Cr2 C57 35.6(3) . . ? O2 Cr2 Cl2 97.60(16) . . ? N2 Cr2 Cl2 91.61(17) . . ? C60 Cr2 Cl2 117.8(4) . . ? C59 Cr2 Cl2 149.8(3) . . ? C61 Cr2 Cl2 90.7(3) . . ? C58 Cr2 Cl2 132.3(4) . . ? C57 Cr2 Cl2 98.6(3) . . ? C1 O1 Cr1 127.7(4) . . ? C11 O2 Cr2 125.2(4) . . ? C21 N1 C23 114.1(6) . . ? C21 N1 Cr1 120.4(5) . . ? C23 N1 Cr1 125.4(5) . . ? C22 N2 C35 114.7(7) . . ? C22 N2 Cr2 119.1(5) . . ? C35 N2 Cr2 126.2(5) . . ? O1 C1 C10 119.8(6) . . ? O1 C1 C2 122.0(7) . . ? C10 C1 C2 118.2(7) . . ? C3 C2 C1 120.4(7) . . ? C3 C2 C21 118.6(7) . . ? C1 C2 C21 120.6(7) . . ? C2 C3 C4 122.6(7) . . ? C2 C3 H3 118.7 . . ? C4 C3 H3 118.7 . . ? C3 C4 C5 122.4(7) . . ? C3 C4 C9 118.0(7) . . ? C5 C4 C9 119.6(7) . . ? C6 C5 C4 121.3(8) . . ? C6 C5 H5 119.4 . . ? C4 C5 H5 119.4 . . ? C5 C6 C7 119.3(8) . . ? C5 C6 H6 120.3 . . ? C7 C6 H6 120.3 . . ? C8 C7 C6 120.9(8) . . ? C8 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? C7 C8 C9 121.7(8) . . ? C7 C8 H8 119.1 . . ? C9 C8 H8 119.1 . . ? C10 C9 C8 122.7(7) . . ? C10 C9 C4 120.1(7) . . ? C8 C9 C4 117.2(7) . . ? C1 C10 C9 120.6(7) . . ? C1 C10 C20 118.3(6) . . ? C9 C10 C20 121.1(6) . . ? O2 C11 C20 119.6(6) . . ? O2 C11 C12 120.9(6) . . ? C20 C11 C12 119.4(6) . . ? C13 C12 C11 120.1(7) . . ? C13 C12 C22 118.6(7) . . ? C11 C12 C22 121.0(7) . . ? C12 C13 C14 122.6(7) . . ? C12 C13 H13 118.7 . . ? C14 C13 H13 118.7 . . ? C13 C14 C15 122.6(7) . . ? C13 C14 C19 117.4(6) . . ? C15 C14 C19 120.0(7) . . ? C16 C15 C14 120.3(7) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C15 C16 C17 120.1(8) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C18 C17 C16 121.1(8) . . ? C18 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? C17 C18 C19 122.0(7) . . ? C17 C18 H18 119.0 . . ? C19 C18 H18 119.0 . . ? C20 C19 C18 122.6(7) . . ? C20 C19 C14 120.9(7) . . ? C18 C19 C14 116.5(7) . . ? C11 C20 C19 119.4(6) . . ? C11 C20 C10 119.4(6) . . ? C19 C20 C10 121.2(6) . . ? N1 C21 C2 127.5(7) . . ? N1 C21 H21 116.3 . . ? C2 C21 H21 116.3 . . ? N2 C22 C12 126.9(7) . . ? N2 C22 H22 116.5 . . ? C12 C22 H22 116.5 . . ? C24 C23 C28 123.9(9) . . ? C24 C23 N1 118.0(9) . . ? C28 C23 N1 118.1(8) . . ? C23 C24 C25 116.5(11) . . ? C23 C24 C29 123.4(9) . . ? C25 C24 C29 119.5(10) . . ? C26 C25 C24 118.6(11) . . ? C26 C25 H25 120.7 . . ? C24 C25 H25 120.7 . . ? C27 C26 C25 123.1(11) . . ? C27 C26 H26 118.5 . . ? C25 C26 H26 118.5 . . ? C26 C27 C28 121.2(12) . . ? C26 C27 H27 119.4 . . ? C28 C27 H27 119.4 . . ? C27 C28 C23 116.6(10) . . ? C27 C28 C30 120.3(11) . . ? C23 C28 C30 123.1(9) . . ? C32 C29 C24 110.4(11) . . ? C32 C29 C31 111.1(11) . . ? C24 C29 C31 112.7(10) . . ? C32 C29 H29 107.5 . . ? C24 C29 H29 107.5 . . ? C31 C29 H29 107.5 . . ? C28 C30 C33 111.1(9) . . ? C28 C30 C34 112.7(9) . . ? C33 C30 C34 108.5(9) . . ? C28 C30 H30 108.1 . . ? C33 C30 H30 108.1 . . ? C34 C30 H30 108.1 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C30 C34 H34A 109.5 . . ? C30 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C30 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C40 C35 C36 124.6(10) . . ? C40 C35 N2 119.1(9) . . ? C36 C35 N2 116.3(9) . . ? C37 C36 C35 116.4(12) . . ? C37 C36 C41 120.5(13) . . ? C35 C36 C41 123.1(10) . . ? C38 C37 C36 118.0(14) . . ? C38 C37 H37 121.0 . . ? C36 C37 H37 121.0 . . ? C37 C38 C39 127.5(14) . . ? C37 C38 H38 116.2 . . ? C39 C38 H38 116.2 . . ? C38 C39 C40 116.2(12) . . ? C38 C39 H39 121.9 . . ? C40 C39 H39 121.9 . . ? C35 C40 C39 117.3(11) . . ? C35 C40 C42 121.4(9) . . ? C39 C40 C42 121.2(11) . . ? C43 C41 C36 105.8(12) . . ? C43 C41 C44 112.7(12) . . ? C36 C41 C44 111.7(12) . . ? C43 C41 H41 108.9 . . ? C36 C41 H41 108.9 . . ? C44 C41 H41 108.9 . . ? C40 C42 C46 112.0(9) . . ? C40 C42 C45 111.8(9) . . ? C46 C42 C45 107.7(8) . . ? C40 C42 H42 108.4 . . ? C46 C42 H42 108.4 . . ? C45 C42 H42 108.4 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C42 C45 H45A 109.5 . . ? C42 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C42 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C42 C46 H46A 109.5 . . ? C42 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C42 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C48 C47 C51 107.2(8) . . ? C48 C47 C52 127.2(8) . . ? C51 C47 C52 125.6(8) . . ? C48 C47 Cr1 71.7(4) . . ? C51 C47 Cr1 71.3(4) . . ? C52 C47 Cr1 123.2(6) . . ? C47 C48 C49 109.4(8) . . ? C47 C48 C53 125.8(8) . . ? C49 C48 C53 124.8(8) . . ? C47 C48 Cr1 72.2(5) . . ? C49 C48 Cr1 71.0(5) . . ? C53 C48 Cr1 121.1(5) . . ? C48 C49 C50 108.2(8) . . ? C48 C49 C54 124.3(9) . . ? C50 C49 C54 127.0(8) . . ? C48 C49 Cr1 72.6(5) . . ? C50 C49 Cr1 73.8(5) . . ? C54 C49 Cr1 125.9(5) . . ? C49 C50 C51 107.4(8) . . ? C49 C50 C55 126.8(9) . . ? C51 C50 C55 125.7(9) . . ? C49 C50 Cr1 69.5(5) . . ? C51 C50 Cr1 70.6(5) . . ? C55 C50 Cr1 127.8(6) . . ? C47 C51 C50 107.7(8) . . ? C47 C51 C56 125.2(9) . . ? C50 C51 C56 126.8(9) . . ? C47 C51 Cr1 71.4(4) . . ? C50 C51 Cr1 73.0(5) . . ? C56 C51 Cr1 125.6(6) . . ? C47 C52 H52A 109.5 . . ? C47 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C47 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C48 C53 H53A 109.5 . . ? C48 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C48 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C49 C54 H54A 109.5 . . ? C49 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C49 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C50 C55 H55A 109.5 . . ? C50 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C50 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C51 C56 H56A 109.5 . . ? C51 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C51 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C58 C57 C61 108.9(9) . . ? C58 C57 C62 128.7(12) . . ? C61 C57 C62 122.4(12) . . ? C58 C57 Cr2 72.7(6) . . ? C61 C57 Cr2 71.8(5) . . ? C62 C57 Cr2 124.5(6) . . ? C57 C58 C59 105.9(10) . . ? C57 C58 C63 123.6(13) . . ? C59 C58 C63 130.3(14) . . ? C57 C58 Cr2 71.7(5) . . ? C59 C58 Cr2 70.4(6) . . ? C63 C58 Cr2 126.8(7) . . ? C60 C59 C58 110.3(11) . . ? C60 C59 C64 120.1(14) . . ? C58 C59 C64 129.7(14) . . ? C60 C59 Cr2 72.9(6) . . ? C58 C59 Cr2 73.9(6) . . ? C64 C59 Cr2 120.8(8) . . ? C61 C60 C59 108.4(10) . . ? C61 C60 C65 121.9(13) . . ? C59 C60 C65 129.7(13) . . ? C61 C60 Cr2 72.6(6) . . ? C59 C60 Cr2 72.0(6) . . ? C65 C60 Cr2 119.5(7) . . ? C60 C61 C57 106.6(10) . . ? C60 C61 C66 128.3(12) . . ? C57 C61 C66 125.1(12) . . ? C60 C61 Cr2 71.5(6) . . ? C57 C61 Cr2 72.2(6) . . ? C66 C61 Cr2 123.2(7) . . ? C57 C62 H62A 109.5 . . ? C57 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C57 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C58 C63 H63A 109.5 . . ? C58 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C58 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C59 C64 H64A 109.5 . . ? C59 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C59 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C60 C65 H65A 109.5 . . ? C60 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C60 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C61 C66 H66A 109.5 . . ? C61 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C61 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Cr1 O1 C1 -41.8(6) . . . . ? C49 Cr1 O1 C1 -154.7(6) . . . . ? C48 Cr1 O1 C1 170.6(6) . . . . ? C51 Cr1 O1 C1 158.2(6) . . . . ? C47 Cr1 O1 C1 143.5(6) . . . . ? C50 Cr1 O1 C1 -147.6(6) . . . . ? Cl1 Cr1 O1 C1 49.8(6) . . . . ? N2 Cr2 O2 C11 49.1(6) . . . . ? C60 Cr2 O2 C11 -159.7(7) . . . . ? C59 Cr2 O2 C11 165.8(6) . . . . ? C61 Cr2 O2 C11 -136.4(6) . . . . ? C58 Cr2 O2 C11 153.1(6) . . . . ? C57 Cr2 O2 C11 -160.7(8) . . . . ? Cl2 Cr2 O2 C11 -42.0(6) . . . . ? O1 Cr1 N1 C21 30.9(6) . . . . ? C49 Cr1 N1 C21 127.1(6) . . . . ? C48 Cr1 N1 C21 108.4(7) . . . . ? C51 Cr1 N1 C21 -162.7(6) . . . . ? C47 Cr1 N1 C21 -165.5(9) . . . . ? C50 Cr1 N1 C21 164.5(6) . . . . ? Cl1 Cr1 N1 C21 -65.2(6) . . . . ? O1 Cr1 N1 C23 -152.2(7) . . . . ? C49 Cr1 N1 C23 -56.0(8) . . . . ? C48 Cr1 N1 C23 -74.7(9) . . . . ? C51 Cr1 N1 C23 14.2(8) . . . . ? C47 Cr1 N1 C23 11.4(13) . . . . ? C50 Cr1 N1 C23 -18.5(8) . . . . ? Cl1 Cr1 N1 C23 111.7(7) . . . . ? O2 Cr2 N2 C22 -38.4(6) . . . . ? C60 Cr2 N2 C22 -115.4(7) . . . . ? C59 Cr2 N2 C22 -130.9(6) . . . . ? C61 Cr2 N2 C22 155.0(9) . . . . ? C58 Cr2 N2 C22 -166.5(6) . . . . ? C57 Cr2 N2 C22 160.3(6) . . . . ? Cl2 Cr2 N2 C22 59.1(6) . . . . ? O2 Cr2 N2 C35 144.4(7) . . . . ? C60 Cr2 N2 C35 67.4(9) . . . . ? C59 Cr2 N2 C35 51.9(8) . . . . ? C61 Cr2 N2 C35 -22.2(12) . . . . ? C58 Cr2 N2 C35 16.3(8) . . . . ? C57 Cr2 N2 C35 -16.9(8) . . . . ? Cl2 Cr2 N2 C35 -118.1(7) . . . . ? Cr1 O1 C1 C10 -151.1(5) . . . . ? Cr1 O1 C1 C2 30.5(9) . . . . ? O1 C1 C2 C3 178.7(7) . . . . ? C10 C1 C2 C3 0.3(11) . . . . ? O1 C1 C2 C21 5.4(11) . . . . ? C10 C1 C2 C21 -173.1(7) . . . . ? C1 C2 C3 C4 -0.3(12) . . . . ? C21 C2 C3 C4 173.1(7) . . . . ? C2 C3 C4 C5 178.9(7) . . . . ? C2 C3 C4 C9 -1.6(11) . . . . ? C3 C4 C5 C6 179.1(8) . . . . ? C9 C4 C5 C6 -0.4(12) . . . . ? C4 C5 C6 C7 -1.8(13) . . . . ? C5 C6 C7 C8 2.7(13) . . . . ? C6 C7 C8 C9 -1.3(13) . . . . ? C7 C8 C9 C10 177.5(7) . . . . ? C7 C8 C9 C4 -0.9(11) . . . . ? C3 C4 C9 C10 3.7(10) . . . . ? C5 C4 C9 C10 -176.8(7) . . . . ? C3 C4 C9 C8 -177.8(7) . . . . ? C5 C4 C9 C8 1.7(10) . . . . ? O1 C1 C10 C9 -176.6(6) . . . . ? C2 C1 C10 C9 1.8(10) . . . . ? O1 C1 C10 C20 3.1(10) . . . . ? C2 C1 C10 C20 -178.5(6) . . . . ? C8 C9 C10 C1 177.8(7) . . . . ? C4 C9 C10 C1 -3.8(10) . . . . ? C8 C9 C10 C20 -1.9(11) . . . . ? C4 C9 C10 C20 176.5(6) . . . . ? Cr2 O2 C11 C20 149.4(5) . . . . ? Cr2 O2 C11 C12 -34.3(9) . . . . ? O2 C11 C12 C13 179.3(7) . . . . ? C20 C11 C12 C13 -4.4(10) . . . . ? O2 C11 C12 C22 -7.7(11) . . . . ? C20 C11 C12 C22 168.6(7) . . . . ? C11 C12 C13 C14 0.1(11) . . . . ? C22 C12 C13 C14 -173.0(7) . . . . ? C12 C13 C14 C15 -178.7(7) . . . . ? C12 C13 C14 C19 2.7(11) . . . . ? C13 C14 C15 C16 -177.7(7) . . . . ? C19 C14 C15 C16 0.8(11) . . . . ? C14 C15 C16 C17 -1.1(13) . . . . ? C15 C16 C17 C18 0.7(13) . . . . ? C16 C17 C18 C19 0.0(13) . . . . ? C17 C18 C19 C20 179.6(7) . . . . ? C17 C18 C19 C14 -0.3(11) . . . . ? C13 C14 C19 C20 -1.4(10) . . . . ? C15 C14 C19 C20 -180.0(7) . . . . ? C13 C14 C19 C18 178.5(7) . . . . ? C15 C14 C19 C18 0.0(10) . . . . ? O2 C11 C20 C19 -178.0(6) . . . . ? C12 C11 C20 C19 5.6(10) . . . . ? O2 C11 C20 C10 1.4(10) . . . . ? C12 C11 C20 C10 -174.9(6) . . . . ? C18 C19 C20 C11 177.3(7) . . . . ? C14 C19 C20 C11 -2.8(10) . . . . ? C18 C19 C20 C10 -2.2(11) . . . . ? C14 C19 C20 C10 177.7(6) . . . . ? C1 C10 C20 C11 -104.9(8) . . . . ? C9 C10 C20 C11 74.8(9) . . . . ? C1 C10 C20 C19 74.5(9) . . . . ? C9 C10 C20 C19 -105.8(8) . . . . ? C23 N1 C21 C2 171.0(8) . . . . ? Cr1 N1 C21 C2 -11.7(11) . . . . ? C3 C2 C21 N1 173.6(8) . . . . ? C1 C2 C21 N1 -13.0(12) . . . . ? C35 N2 C22 C12 -166.6(7) . . . . ? Cr2 N2 C22 C12 15.9(10) . . . . ? C13 C12 C22 N2 -172.0(7) . . . . ? C11 C12 C22 N2 15.0(12) . . . . ? C21 N1 C23 C24 96.4(9) . . . . ? Cr1 N1 C23 C24 -80.7(9) . . . . ? C21 N1 C23 C28 -83.2(9) . . . . ? Cr1 N1 C23 C28 99.7(8) . . . . ? C28 C23 C24 C25 -3.0(14) . . . . ? N1 C23 C24 C25 177.5(8) . . . . ? C28 C23 C24 C29 168.1(9) . . . . ? N1 C23 C24 C29 -11.5(13) . . . . ? C23 C24 C25 C26 1.0(15) . . . . ? C29 C24 C25 C26 -170.4(10) . . . . ? C24 C25 C26 C27 0.5(18) . . . . ? C25 C26 C27 C28 -0.2(18) . . . . ? C26 C27 C28 C23 -1.6(15) . . . . ? C26 C27 C28 C30 176.7(10) . . . . ? C24 C23 C28 C27 3.3(13) . . . . ? N1 C23 C28 C27 -177.2(7) . . . . ? C24 C23 C28 C30 -174.9(9) . . . . ? N1 C23 C28 C30 4.6(12) . . . . ? C23 C24 C29 C32 142.6(10) . . . . ? C25 C24 C29 C32 -46.7(14) . . . . ? C23 C24 C29 C31 -92.6(12) . . . . ? C25 C24 C29 C31 78.2(13) . . . . ? C27 C28 C30 C33 -81.2(12) . . . . ? C23 C28 C30 C33 97.0(11) . . . . ? C27 C28 C30 C34 40.8(13) . . . . ? C23 C28 C30 C34 -141.0(9) . . . . ? C22 N2 C35 C40 -100.4(9) . . . . ? Cr2 N2 C35 C40 76.9(9) . . . . ? C22 N2 C35 C36 78.5(10) . . . . ? Cr2 N2 C35 C36 -104.2(9) . . . . ? C40 C35 C36 C37 -1.7(16) . . . . ? N2 C35 C36 C37 179.4(9) . . . . ? C40 C35 C36 C41 177.4(10) . . . . ? N2 C35 C36 C41 -1.5(15) . . . . ? C35 C36 C37 C38 1.5(19) . . . . ? C41 C36 C37 C38 -177.6(12) . . . . ? C36 C37 C38 C39 -2(2) . . . . ? C37 C38 C39 C40 2(2) . . . . ? C36 C35 C40 C39 1.9(15) . . . . ? N2 C35 C40 C39 -179.3(8) . . . . ? C36 C35 C40 C42 -174.1(9) . . . . ? N2 C35 C40 C42 4.7(13) . . . . ? C38 C39 C40 C35 -1.8(15) . . . . ? C38 C39 C40 C42 174.2(10) . . . . ? C37 C36 C41 C43 76.8(15) . . . . ? C35 C36 C41 C43 -102.2(13) . . . . ? C37 C36 C41 C44 -46.1(17) . . . . ? C35 C36 C41 C44 134.8(12) . . . . ? C35 C40 C42 C46 85.7(11) . . . . ? C39 C40 C42 C46 -90.2(11) . . . . ? C35 C40 C42 C45 -153.5(9) . . . . ? C39 C40 C42 C45 30.7(13) . . . . ? O1 Cr1 C47 C48 50.2(5) . . . . ? N1 Cr1 C47 C48 -112.3(10) . . . . ? C49 Cr1 C47 C48 -36.5(5) . . . . ? C51 Cr1 C47 C48 -116.1(8) . . . . ? C50 Cr1 C47 C48 -78.6(6) . . . . ? Cl1 Cr1 C47 C48 147.4(5) . . . . ? O1 Cr1 C47 C51 166.4(5) . . . . ? N1 Cr1 C47 C51 3.9(13) . . . . ? C49 Cr1 C47 C51 79.7(6) . . . . ? C48 Cr1 C47 C51 116.1(8) . . . . ? C50 Cr1 C47 C51 37.5(5) . . . . ? Cl1 Cr1 C47 C51 -96.5(5) . . . . ? O1 Cr1 C47 C52 -72.7(7) . . . . ? N1 Cr1 C47 C52 124.8(9) . . . . ? C49 Cr1 C47 C52 -159.4(8) . . . . ? C48 Cr1 C47 C52 -122.9(9) . . . . ? C51 Cr1 C47 C52 120.9(10) . . . . ? C50 Cr1 C47 C52 158.4(8) . . . . ? Cl1 Cr1 C47 C52 24.4(7) . . . . ? C51 C47 C48 C49 -1.3(9) . . . . ? C52 C47 C48 C49 179.9(7) . . . . ? Cr1 C47 C48 C49 61.6(6) . . . . ? C51 C47 C48 C53 -178.8(7) . . . . ? C52 C47 C48 C53 2.4(13) . . . . ? Cr1 C47 C48 C53 -115.9(7) . . . . ? C51 C47 C48 Cr1 -62.9(5) . . . . ? C52 C47 C48 Cr1 118.3(8) . . . . ? O1 Cr1 C48 C47 -133.6(5) . . . . ? N1 Cr1 C48 C47 148.4(5) . . . . ? C49 Cr1 C48 C47 118.6(7) . . . . ? C51 Cr1 C48 C47 38.4(5) . . . . ? C50 Cr1 C48 C47 80.4(5) . . . . ? Cl1 Cr1 C48 C47 -39.0(6) . . . . ? O1 Cr1 C48 C49 107.7(5) . . . . ? N1 Cr1 C48 C49 29.8(8) . . . . ? C51 Cr1 C48 C49 -80.2(5) . . . . ? C47 Cr1 C48 C49 -118.6(7) . . . . ? C50 Cr1 C48 C49 -38.3(5) . . . . ? Cl1 Cr1 C48 C49 -157.7(4) . . . . ? O1 Cr1 C48 C53 -12.1(7) . . . . ? N1 Cr1 C48 C53 -90.1(8) . . . . ? C49 Cr1 C48 C53 -119.8(9) . . . . ? C51 Cr1 C48 C53 160.0(8) . . . . ? C47 Cr1 C48 C53 121.5(9) . . . . ? C50 Cr1 C48 C53 -158.1(8) . . . . ? Cl1 Cr1 C48 C53 82.5(7) . . . . ? C47 C48 C49 C50 3.4(9) . . . . ? C53 C48 C49 C50 -179.1(7) . . . . ? Cr1 C48 C49 C50 65.7(6) . . . . ? C47 C48 C49 C54 175.6(7) . . . . ? C53 C48 C49 C54 -6.8(12) . . . . ? Cr1 C48 C49 C54 -122.0(8) . . . . ? C47 C48 C49 Cr1 -62.4(6) . . . . ? C53 C48 C49 Cr1 115.2(7) . . . . ? O1 Cr1 C49 C48 -73.1(5) . . . . ? N1 Cr1 C49 C48 -162.8(5) . . . . ? C51 Cr1 C49 C48 79.0(5) . . . . ? C47 Cr1 C49 C48 36.2(5) . . . . ? C50 Cr1 C49 C48 115.6(7) . . . . ? Cl1 Cr1 C49 C48 44.5(8) . . . . ? O1 Cr1 C49 C50 171.3(5) . . . . ? N1 Cr1 C49 C50 81.6(5) . . . . ? C48 Cr1 C49 C50 -115.6(7) . . . . ? C51 Cr1 C49 C50 -36.6(5) . . . . ? C47 Cr1 C49 C50 -79.4(5) . . . . ? Cl1 Cr1 C49 C50 -71.1(8) . . . . ? O1 Cr1 C49 C54 47.0(8) . . . . ? N1 Cr1 C49 C54 -42.7(8) . . . . ? C48 Cr1 C49 C54 120.1(10) . . . . ? C51 Cr1 C49 C54 -160.9(9) . . . . ? C47 Cr1 C49 C54 156.3(9) . . . . ? C50 Cr1 C49 C54 -124.3(10) . . . . ? Cl1 Cr1 C49 C54 164.6(5) . . . . ? C48 C49 C50 C51 -4.2(9) . . . . ? C54 C49 C50 C51 -176.1(7) . . . . ? Cr1 C49 C50 C51 60.8(6) . . . . ? C48 C49 C50 C55 172.5(8) . . . . ? C54 C49 C50 C55 0.5(13) . . . . ? Cr1 C49 C50 C55 -122.6(8) . . . . ? C48 C49 C50 Cr1 -64.9(6) . . . . ? C54 C49 C50 Cr1 123.1(8) . . . . ? O1 Cr1 C50 C49 -11.8(6) . . . . ? N1 Cr1 C50 C49 -110.6(5) . . . . ? C48 Cr1 C50 C49 37.9(5) . . . . ? C51 Cr1 C50 C49 118.0(7) . . . . ? C47 Cr1 C50 C49 79.6(5) . . . . ? Cl1 Cr1 C50 C49 146.0(4) . . . . ? O1 Cr1 C50 C51 -129.8(5) . . . . ? N1 Cr1 C50 C51 131.4(5) . . . . ? C49 Cr1 C50 C51 -118.0(7) . . . . ? C48 Cr1 C50 C51 -80.1(5) . . . . ? C47 Cr1 C50 C51 -38.4(5) . . . . ? Cl1 Cr1 C50 C51 27.9(6) . . . . ? O1 Cr1 C50 C55 109.5(9) . . . . ? N1 Cr1 C50 C55 10.7(9) . . . . ? C49 Cr1 C50 C55 121.3(11) . . . . ? C48 Cr1 C50 C55 159.2(10) . . . . ? C51 Cr1 C50 C55 -120.7(11) . . . . ? C47 Cr1 C50 C55 -159.1(10) . . . . ? Cl1 Cr1 C50 C55 -92.7(9) . . . . ? C48 C47 C51 C50 -1.3(9) . . . . ? C52 C47 C51 C50 177.5(7) . . . . ? Cr1 C47 C51 C50 -64.4(6) . . . . ? C48 C47 C51 C56 -176.0(8) . . . . ? C52 C47 C51 C56 2.9(13) . . . . ? Cr1 C47 C51 C56 120.9(9) . . . . ? C48 C47 C51 Cr1 63.1(5) . . . . ? C52 C47 C51 Cr1 -118.0(8) . . . . ? C49 C50 C51 C47 3.4(9) . . . . ? C55 C50 C51 C47 -173.3(8) . . . . ? Cr1 C50 C51 C47 63.4(5) . . . . ? C49 C50 C51 C56 177.9(8) . . . . ? C55 C50 C51 C56 1.2(14) . . . . ? Cr1 C50 C51 C56 -122.1(9) . . . . ? C49 C50 C51 Cr1 -60.1(5) . . . . ? C55 C50 C51 Cr1 123.3(8) . . . . ? O1 Cr1 C51 C47 -23.2(9) . . . . ? N1 Cr1 C51 C47 -178.5(5) . . . . ? C49 Cr1 C51 C47 -79.1(6) . . . . ? C48 Cr1 C51 C47 -37.3(5) . . . . ? C50 Cr1 C51 C47 -116.0(8) . . . . ? Cl1 Cr1 C51 C47 85.7(5) . . . . ? O1 Cr1 C51 C50 92.8(7) . . . . ? N1 Cr1 C51 C50 -62.5(6) . . . . ? C49 Cr1 C51 C50 36.9(5) . . . . ? C48 Cr1 C51 C50 78.7(5) . . . . ? C47 Cr1 C51 C50 116.0(8) . . . . ? Cl1 Cr1 C51 C50 -158.3(5) . . . . ? O1 Cr1 C51 C56 -143.7(7) . . . . ? N1 Cr1 C51 C56 60.9(10) . . . . ? C49 Cr1 C51 C56 160.4(10) . . . . ? C48 Cr1 C51 C56 -157.8(10) . . . . ? C47 Cr1 C51 C56 -120.5(11) . . . . ? C50 Cr1 C51 C56 123.5(11) . . . . ? Cl1 Cr1 C51 C56 -34.9(8) . . . . ? O2 Cr2 C57 C58 -78.1(10) . . . . ? N2 Cr2 C57 C58 66.0(7) . . . . ? C60 Cr2 C57 C58 -79.2(7) . . . . ? C59 Cr2 C57 C58 -38.1(6) . . . . ? C61 Cr2 C57 C58 -117.3(9) . . . . ? Cl2 Cr2 C57 C58 163.5(6) . . . . ? O2 Cr2 C57 C61 39.2(11) . . . . ? N2 Cr2 C57 C61 -176.7(6) . . . . ? C60 Cr2 C57 C61 38.1(6) . . . . ? C59 Cr2 C57 C61 79.2(7) . . . . ? C58 Cr2 C57 C61 117.3(9) . . . . ? Cl2 Cr2 C57 C61 -79.2(6) . . . . ? O2 Cr2 C57 C62 156.4(8) . . . . ? N2 Cr2 C57 C62 -59.5(12) . . . . ? C60 Cr2 C57 C62 155.3(13) . . . . ? C59 Cr2 C57 C62 -163.6(14) . . . . ? C61 Cr2 C57 C62 117.2(14) . . . . ? C58 Cr2 C57 C62 -125.5(14) . . . . ? Cl2 Cr2 C57 C62 38.0(11) . . . . ? C61 C57 C58 C59 -0.7(11) . . . . ? C62 C57 C58 C59 -176.8(9) . . . . ? Cr2 C57 C58 C59 62.5(7) . . . . ? C61 C57 C58 C63 174.3(9) . . . . ? C62 C57 C58 C63 -1.8(16) . . . . ? Cr2 C57 C58 C63 -122.5(10) . . . . ? C61 C57 C58 Cr2 -63.1(6) . . . . ? C62 C57 C58 Cr2 120.7(10) . . . . ? O2 Cr2 C58 C57 137.3(6) . . . . ? N2 Cr2 C58 C57 -127.6(6) . . . . ? C60 Cr2 C58 C57 78.9(7) . . . . ? C59 Cr2 C58 C57 115.1(10) . . . . ? C61 Cr2 C58 C57 37.1(6) . . . . ? Cl2 Cr2 C58 C57 -22.4(8) . . . . ? O2 Cr2 C58 C59 22.2(9) . . . . ? N2 Cr2 C58 C59 117.3(7) . . . . ? C60 Cr2 C58 C59 -36.2(7) . . . . ? C61 Cr2 C58 C59 -78.0(7) . . . . ? C57 Cr2 C58 C59 -115.1(10) . . . . ? Cl2 Cr2 C58 C59 -137.5(7) . . . . ? O2 Cr2 C58 C63 -104.0(12) . . . . ? N2 Cr2 C58 C63 -8.9(13) . . . . ? C60 Cr2 C58 C63 -162.4(15) . . . . ? C59 Cr2 C58 C63 -126.2(17) . . . . ? C61 Cr2 C58 C63 155.8(15) . . . . ? C57 Cr2 C58 C63 118.7(16) . . . . ? Cl2 Cr2 C58 C63 96.3(12) . . . . ? C57 C58 C59 C60 1.1(12) . . . . ? C63 C58 C59 C60 -173.5(10) . . . . ? Cr2 C58 C59 C60 64.4(8) . . . . ? C57 C58 C59 C64 179.7(11) . . . . ? C63 C58 C59 C64 5(2) . . . . ? Cr2 C58 C59 C64 -116.9(12) . . . . ? C57 C58 C59 Cr2 -63.3(7) . . . . ? C63 C58 C59 Cr2 122.1(11) . . . . ? O2 Cr2 C59 C60 79.6(7) . . . . ? N2 Cr2 C59 C60 166.7(6) . . . . ? C61 Cr2 C59 C60 -37.5(6) . . . . ? C58 Cr2 C59 C60 -117.7(10) . . . . ? C57 Cr2 C59 C60 -79.8(7) . . . . ? Cl2 Cr2 C59 C60 -33.5(13) . . . . ? O2 Cr2 C59 C58 -162.6(7) . . . . ? N2 Cr2 C59 C58 -75.5(8) . . . . ? C60 Cr2 C59 C58 117.7(10) . . . . ? C61 Cr2 C59 C58 80.2(7) . . . . ? C57 Cr2 C59 C58 38.0(6) . . . . ? Cl2 Cr2 C59 C58 84.3(11) . . . . ? O2 Cr2 C59 C64 -35.6(12) . . . . ? N2 Cr2 C59 C64 51.5(13) . . . . ? C60 Cr2 C59 C64 -115.3(16) . . . . ? C61 Cr2 C59 C64 -152.8(14) . . . . ? C58 Cr2 C59 C64 127.0(16) . . . . ? C57 Cr2 C59 C64 165.0(15) . . . . ? Cl2 Cr2 C59 C64 -148.7(8) . . . . ? C58 C59 C60 C61 -1.1(12) . . . . ? C64 C59 C60 C61 -179.9(9) . . . . ? Cr2 C59 C60 C61 64.0(7) . . . . ? C58 C59 C60 C65 -178.7(10) . . . . ? C64 C59 C60 C65 2.4(17) . . . . ? Cr2 C59 C60 C65 -113.7(11) . . . . ? C58 C59 C60 Cr2 -65.0(8) . . . . ? C64 C59 C60 Cr2 116.2(10) . . . . ? O2 Cr2 C60 C61 142.3(7) . . . . ? N2 Cr2 C60 C61 -141.2(7) . . . . ? C59 Cr2 C60 C61 -116.7(10) . . . . ? C58 Cr2 C60 C61 -79.9(7) . . . . ? C57 Cr2 C60 C61 -38.3(6) . . . . ? Cl2 Cr2 C60 C61 45.0(7) . . . . ? O2 Cr2 C60 C59 -100.9(8) . . . . ? N2 Cr2 C60 C59 -24.5(11) . . . . ? C61 Cr2 C60 C59 116.7(10) . . . . ? C58 Cr2 C60 C59 36.9(7) . . . . ? C57 Cr2 C60 C59 78.5(7) . . . . ? Cl2 Cr2 C60 C59 161.7(7) . . . . ? O2 Cr2 C60 C65 25.0(11) . . . . ? N2 Cr2 C60 C65 101.5(12) . . . . ? C59 Cr2 C60 C65 126.0(15) . . . . ? C61 Cr2 C60 C65 -117.3(15) . . . . ? C58 Cr2 C60 C65 162.8(14) . . . . ? C57 Cr2 C60 C65 -155.6(14) . . . . ? Cl2 Cr2 C60 C65 -72.3(11) . . . . ? C59 C60 C61 C57 0.6(11) . . . . ? C65 C60 C61 C57 178.5(9) . . . . ? Cr2 C60 C61 C57 64.2(6) . . . . ? C59 C60 C61 C66 178.3(9) . . . . ? C65 C60 C61 C66 -3.8(15) . . . . ? Cr2 C60 C61 C66 -118.1(10) . . . . ? C59 C60 C61 Cr2 -63.5(7) . . . . ? C65 C60 C61 Cr2 114.4(9) . . . . ? C58 C57 C61 C60 0.0(10) . . . . ? C62 C57 C61 C60 176.5(8) . . . . ? Cr2 C57 C61 C60 -63.7(6) . . . . ? C58 C57 C61 C66 -177.8(9) . . . . ? C62 C57 C61 C66 -1.3(14) . . . . ? Cr2 C57 C61 C66 118.5(9) . . . . ? C58 C57 C61 Cr2 63.7(7) . . . . ? C62 C57 C61 Cr2 -119.8(9) . . . . ? O2 Cr2 C61 C60 -42.5(8) . . . . ? N2 Cr2 C61 C60 122.6(10) . . . . ? C59 Cr2 C61 C60 36.7(6) . . . . ? C58 Cr2 C61 C60 78.3(7) . . . . ? C57 Cr2 C61 C60 115.0(9) . . . . ? Cl2 Cr2 C61 C60 -141.3(7) . . . . ? O2 Cr2 C61 C57 -157.6(6) . . . . ? N2 Cr2 C61 C57 7.6(13) . . . . ? C60 Cr2 C61 C57 -115.0(9) . . . . ? C59 Cr2 C61 C57 -78.3(7) . . . . ? C58 Cr2 C61 C57 -36.7(6) . . . . ? Cl2 Cr2 C61 C57 103.7(6) . . . . ? O2 Cr2 C61 C66 81.6(10) . . . . ? N2 Cr2 C61 C66 -113.2(11) . . . . ? C60 Cr2 C61 C66 124.2(14) . . . . ? C59 Cr2 C61 C66 160.9(13) . . . . ? C58 Cr2 C61 C66 -157.5(13) . . . . ? C57 Cr2 C61 C66 -120.8(14) . . . . ? Cl2 Cr2 C61 C66 -17.1(10) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.629 _refine_diff_density_min -0.424 _refine_diff_density_rms 0.071 # Attachment '- complex 5.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 821441' #TrackingRef '- complex 5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H41 Cl Cr N O2' _chemical_formula_weight 667.20 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 8.6023(7) _cell_length_b 12.9253(11) _cell_length_c 16.4342(14) _cell_angle_alpha 69.8440(10) _cell_angle_beta 83.356(2) _cell_angle_gamma 79.470(2) _cell_volume 1683.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9250 _cell_measurement_theta_min 1.70 _cell_measurement_theta_max 26.04 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.316 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 702 _exptl_absorpt_coefficient_mu 0.456 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.936 _exptl_absorpt_correction_T_max 0.955 _exptl_absorpt_process_details 'ABSCOR by T.Higashi 8 March, 1995' _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 'Bruker Smart Apex CCD' _diffrn_measurement_method \w-2\q _diffrn_detector_area_resol_mean 0.01 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 9250 _diffrn_reflns_av_R_equivalents 0.0229 _diffrn_reflns_av_sigmaI/netI 0.0596 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 26.04 _reflns_number_total 6500 _reflns_number_gt 4503 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0705P)^2^+0.1228P] 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 6500 _refine_ls_number_parameters 421 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0840 _refine_ls_R_factor_gt 0.0513 _refine_ls_wR_factor_ref 0.1355 _refine_ls_wR_factor_gt 0.1202 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _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 Cr1 Cr 0.73595(5) 0.62238(4) 0.16982(3) 0.02931(15) Uani 1 1 d . . . Cl1 Cl 1.00359(9) 0.62932(8) 0.13658(5) 0.0508(2) Uani 1 1 d . . . O1 O 0.7009(2) 0.72548(16) 0.23281(12) 0.0360(5) Uani 1 1 d . . . O2 O 0.3796(2) 0.90720(18) 0.35192(13) 0.0392(5) Uani 1 1 d . . . N1 N 0.7777(3) 0.49279(19) 0.28495(15) 0.0302(5) Uani 1 1 d . . . C1 C 0.7219(3) 0.7162(2) 0.31306(17) 0.0287(6) Uani 1 1 d . . . C11 C 0.6268(3) 0.9208(2) 0.27570(18) 0.0289(6) Uani 1 1 d . . . C21 C 0.7944(3) 0.5063(2) 0.35765(18) 0.0307(6) Uani 1 1 d . . . H21 H 0.8238 0.4417 0.4037 0.037 Uiso 1 1 calc R . . C3 C 0.7935(3) 0.6017(2) 0.46001(17) 0.0299(6) Uani 1 1 d . . . H3 H 0.8293 0.5323 0.4995 0.036 Uiso 1 1 calc R . . C20 C 0.7251(3) 0.9793(2) 0.20508(17) 0.0281(6) Uani 1 1 d . . . C8 C 0.6731(3) 0.8929(3) 0.45688(19) 0.0336(7) Uani 1 1 d . . . H8 H 0.6358 0.9628 0.4185 0.040 Uiso 1 1 calc R . . C9 C 0.7078(3) 0.8001(2) 0.42689(17) 0.0267(6) Uani 1 1 d . . . C2 C 0.7731(3) 0.6095(2) 0.37583(17) 0.0283(6) Uani 1 1 d . . . C12 C 0.4713(3) 0.9680(2) 0.28443(18) 0.0318(7) Uani 1 1 d . . . C26 C 0.7965(3) 0.3779(2) 0.28959(18) 0.0320(7) Uani 1 1 d . . . C10 C 0.6889(3) 0.8103(2) 0.33895(17) 0.0268(6) Uani 1 1 d . . . C4 C 0.7622(3) 0.6942(2) 0.48779(17) 0.0295(6) Uani 1 1 d . . . C19 C 0.8850(3) 0.9359(3) 0.18906(18) 0.0345(7) Uani 1 1 d . . . H19 H 0.9291 0.8667 0.2259 0.041 Uiso 1 1 calc R . . C33 C 0.6364(3) 0.5506(3) 0.08258(19) 0.0358(7) Uani 1 1 d . . . C15 C 0.6643(3) 1.0863(2) 0.14781(18) 0.0332(7) Uani 1 1 d . . . C32 C 0.5114(3) 0.5819(3) 0.13823(19) 0.0385(7) Uani 1 1 d . . . C27 C 0.9147(4) 0.3373(3) 0.23852(19) 0.0406(8) Uani 1 1 d . . . H27 H 0.9807 0.3841 0.2002 0.049 Uiso 1 1 calc R . . C5 C 0.7827(4) 0.6853(3) 0.57498(19) 0.0391(7) Uani 1 1 d . . . H5 H 0.8197 0.6163 0.6146 0.047 Uiso 1 1 calc R . . C35 C 0.6157(4) 0.7390(3) 0.05483(18) 0.0353(7) Uani 1 1 d . . . C36 C 0.4967(3) 0.6984(3) 0.11890(19) 0.0380(7) Uani 1 1 d . . . C14 C 0.5058(4) 1.1324(3) 0.16341(19) 0.0381(7) Uani 1 1 d . . . H14 H 0.4659 1.2037 0.1282 0.046 Uiso 1 1 calc R . . C13 C 0.4116(3) 1.0750(3) 0.2284(2) 0.0376(7) Uani 1 1 d . . . H13 H 0.3069 1.1059 0.2364 0.045 Uiso 1 1 calc R . . C16 C 0.7615(4) 1.1436(3) 0.07691(19) 0.0393(7) Uani 1 1 d . . . H16 H 0.7206 1.2130 0.0391 0.047 Uiso 1 1 calc R . . C17 C 0.9127(4) 1.0987(3) 0.0638(2) 0.0441(8) Uani 1 1 d . . . H17 H 0.9755 1.1370 0.0172 0.053 Uiso 1 1 calc R . . C34 C 0.6989(3) 0.6480(3) 0.03038(18) 0.0347(7) Uani 1 1 d . . . C31 C 0.6961(4) 0.3087(3) 0.3443(2) 0.0444(8) Uani 1 1 d . . . H31 H 0.6150 0.3368 0.3771 0.053 Uiso 1 1 calc R . . C7 C 0.6934(4) 0.8818(3) 0.5408(2) 0.0428(8) Uani 1 1 d . . . H7 H 0.6705 0.9441 0.5587 0.051 Uiso 1 1 calc R . . C18 C 0.9749(4) 0.9939(3) 0.1206(2) 0.0424(8) Uani 1 1 d . . . H18 H 1.0794 0.9636 0.1113 0.051 Uiso 1 1 calc R . . C29 C 0.8354(4) 0.1563(3) 0.3010(2) 0.0511(9) Uani 1 1 d . . . H29 H 0.8498 0.0816 0.3054 0.061 Uiso 1 1 calc R . . C38 C 0.6802(4) 0.4370(3) 0.0726(2) 0.0520(9) Uani 1 1 d . . . H38A H 0.6160 0.4317 0.0306 0.078 Uiso 1 1 calc R . . H38B H 0.6627 0.3807 0.1274 0.078 Uiso 1 1 calc R . . H38C H 0.7899 0.4263 0.0534 0.078 Uiso 1 1 calc R . . C28 C 0.9329(4) 0.2254(3) 0.2456(2) 0.0456(8) Uani 1 1 d . . . H28 H 1.0126 0.1972 0.2122 0.055 Uiso 1 1 calc R . . C23 C 0.1400(4) 0.8345(3) 0.4136(2) 0.0545(10) Uani 1 1 d . . . H23A H 0.0264 0.8571 0.4187 0.065 Uiso 1 1 calc R . . H23B H 0.1816 0.8233 0.4689 0.065 Uiso 1 1 calc R . . C6 C 0.7487(4) 0.7767(3) 0.6008(2) 0.0470(8) Uani 1 1 d . . . H6 H 0.7618 0.7700 0.6578 0.056 Uiso 1 1 calc R . . C22 C 0.2106(3) 0.9286(3) 0.3452(2) 0.0456(8) Uani 1 1 d . . . H22A H 0.1855 0.9332 0.2879 0.055 Uiso 1 1 calc R . . H22B H 0.1673 0.9989 0.3540 0.055 Uiso 1 1 calc R . . C30 C 0.7156(4) 0.1969(3) 0.3506(2) 0.0540(9) Uani 1 1 d . . . H30 H 0.6485 0.1501 0.3878 0.065 Uiso 1 1 calc R . . C40 C 0.6458(4) 0.8582(3) 0.0206(2) 0.0522(9) Uani 1 1 d . . . H40A H 0.5552 0.9054 -0.0087 0.078 Uiso 1 1 calc R . . H40B H 0.7370 0.8641 -0.0195 0.078 Uiso 1 1 calc R . . H40C H 0.6644 0.8808 0.0680 0.078 Uiso 1 1 calc R . . C39 C 0.8268(4) 0.6529(3) -0.0404(2) 0.0547(10) Uani 1 1 d . . . H39A H 0.7798 0.6715 -0.0948 0.082 Uiso 1 1 calc R . . H39B H 0.8932 0.5817 -0.0281 0.082 Uiso 1 1 calc R . . H39C H 0.8892 0.7088 -0.0435 0.082 Uiso 1 1 calc R . . C41 C 0.3749(4) 0.7698(4) 0.1585(2) 0.0627(11) Uani 1 1 d . . . H41A H 0.3257 0.7231 0.2101 0.094 Uiso 1 1 calc R . . H41B H 0.2960 0.8107 0.1176 0.094 Uiso 1 1 calc R . . H41C H 0.4256 0.8210 0.1729 0.094 Uiso 1 1 calc R . . C37 C 0.4067(4) 0.5051(4) 0.2013(3) 0.0652(11) Uani 1 1 d . . . H37A H 0.3796 0.5274 0.2517 0.098 Uiso 1 1 calc R . . H37B H 0.4620 0.4300 0.2181 0.098 Uiso 1 1 calc R . . H37C H 0.3119 0.5089 0.1741 0.098 Uiso 1 1 calc R . . C25 C 0.3406(4) 0.6626(3) 0.4065(3) 0.0647(11) Uani 1 1 d . . . H25A H 0.4096 0.7077 0.3646 0.097 Uiso 1 1 calc R . . H25B H 0.3482 0.5924 0.3973 0.097 Uiso 1 1 calc R . . H25C H 0.3712 0.6499 0.4640 0.097 Uiso 1 1 calc R . . C24 C 0.1711(4) 0.7223(3) 0.3967(3) 0.0598(10) Uani 1 1 d . . . H24A H 0.1021 0.6735 0.4365 0.072 Uiso 1 1 calc R . . H24B H 0.1423 0.7352 0.3383 0.072 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 Cr1 0.0335(3) 0.0296(3) 0.0262(3) -0.0117(2) -0.00606(18) -0.0006(2) Cl1 0.0337(4) 0.0593(6) 0.0500(5) -0.0046(4) -0.0052(4) -0.0084(4) O1 0.0577(13) 0.0230(11) 0.0287(11) -0.0099(9) -0.0121(9) -0.0013(10) O2 0.0294(11) 0.0431(13) 0.0427(12) -0.0103(11) -0.0055(9) -0.0051(10) N1 0.0362(13) 0.0249(13) 0.0326(13) -0.0140(11) -0.0021(10) -0.0033(11) C1 0.0316(15) 0.0282(16) 0.0274(15) -0.0095(12) -0.0051(12) -0.0047(13) C11 0.0347(16) 0.0250(15) 0.0327(15) -0.0170(13) -0.0065(12) -0.0010(13) C21 0.0363(16) 0.0247(15) 0.0295(15) -0.0067(13) -0.0046(12) -0.0034(13) C3 0.0339(15) 0.0254(16) 0.0286(15) -0.0058(13) -0.0013(12) -0.0068(13) C20 0.0364(16) 0.0259(15) 0.0247(14) -0.0106(12) -0.0054(12) -0.0054(13) C8 0.0334(16) 0.0337(17) 0.0367(16) -0.0158(14) -0.0032(13) -0.0041(14) C9 0.0235(14) 0.0307(16) 0.0283(14) -0.0128(13) -0.0008(11) -0.0046(12) C2 0.0294(15) 0.0259(15) 0.0307(15) -0.0106(13) -0.0017(12) -0.0043(13) C12 0.0362(16) 0.0321(17) 0.0307(15) -0.0150(13) -0.0055(13) -0.0031(14) C26 0.0407(17) 0.0260(16) 0.0310(15) -0.0122(13) -0.0111(13) 0.0015(14) C10 0.0276(14) 0.0247(15) 0.0292(15) -0.0097(12) -0.0034(11) -0.0038(12) C4 0.0302(15) 0.0349(17) 0.0264(14) -0.0134(13) 0.0005(12) -0.0071(13) C19 0.0399(17) 0.0294(17) 0.0338(16) -0.0106(14) -0.0039(13) -0.0032(14) C33 0.0366(16) 0.0380(18) 0.0383(17) -0.0200(15) -0.0144(13) 0.0030(14) C15 0.0448(17) 0.0304(17) 0.0291(15) -0.0149(13) -0.0084(13) -0.0034(14) C32 0.0310(16) 0.048(2) 0.0387(17) -0.0154(16) -0.0090(13) -0.0053(15) C27 0.0466(18) 0.0381(19) 0.0345(17) -0.0127(15) -0.0076(14) 0.0047(16) C5 0.0450(18) 0.0419(19) 0.0301(16) -0.0139(14) -0.0042(13) -0.0002(15) C35 0.0433(17) 0.0317(17) 0.0325(16) -0.0143(14) -0.0152(13) 0.0053(14) C36 0.0349(16) 0.048(2) 0.0382(17) -0.0266(16) -0.0100(13) 0.0054(15) C14 0.0493(19) 0.0289(17) 0.0343(17) -0.0096(14) -0.0148(14) 0.0043(15) C13 0.0331(16) 0.0369(18) 0.0439(18) -0.0176(15) -0.0100(14) 0.0050(14) C16 0.059(2) 0.0279(17) 0.0298(16) -0.0086(14) -0.0074(14) -0.0037(16) C17 0.054(2) 0.046(2) 0.0313(17) -0.0112(16) 0.0039(15) -0.0134(17) C34 0.0399(17) 0.0378(18) 0.0264(15) -0.0137(14) -0.0072(13) 0.0034(15) C31 0.052(2) 0.0359(19) 0.051(2) -0.0229(16) 0.0040(16) -0.0082(17) C7 0.0477(19) 0.045(2) 0.0442(19) -0.0287(17) -0.0035(15) 0.0008(16) C18 0.0435(18) 0.043(2) 0.0398(18) -0.0165(16) 0.0029(14) -0.0022(16) C29 0.067(2) 0.0338(19) 0.061(2) -0.0243(18) -0.0209(19) 0.0000(18) C38 0.065(2) 0.039(2) 0.060(2) -0.0272(18) -0.0309(18) 0.0094(18) C28 0.057(2) 0.040(2) 0.0435(19) -0.0248(17) -0.0135(16) 0.0125(17) C23 0.0308(17) 0.077(3) 0.055(2) -0.022(2) 0.0032(15) -0.0083(18) C6 0.058(2) 0.055(2) 0.0338(17) -0.0240(17) -0.0068(15) -0.0028(18) C22 0.0345(17) 0.050(2) 0.053(2) -0.0194(18) -0.0066(15) -0.0019(16) C30 0.061(2) 0.038(2) 0.068(2) -0.0229(19) 0.0011(19) -0.0140(18) C40 0.074(2) 0.0344(19) 0.048(2) -0.0126(16) -0.0242(18) 0.0040(18) C39 0.055(2) 0.068(3) 0.0362(18) -0.0194(18) 0.0017(16) 0.0036(19) C41 0.048(2) 0.085(3) 0.065(2) -0.050(2) -0.0103(18) 0.020(2) C37 0.045(2) 0.083(3) 0.066(3) -0.018(2) -0.0047(18) -0.020(2) C25 0.051(2) 0.060(3) 0.077(3) -0.016(2) 0.011(2) -0.014(2) C24 0.045(2) 0.056(2) 0.069(3) -0.005(2) 0.0040(18) -0.0178(19) _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 Cr1 O1 1.9157(19) . ? Cr1 N1 2.066(2) . ? Cr1 C35 2.198(3) . ? Cr1 C36 2.234(3) . ? Cr1 C32 2.250(3) . ? Cr1 C34 2.252(3) . ? Cr1 C33 2.267(3) . ? Cr1 Cl1 2.3147(9) . ? O1 C1 1.313(3) . ? O2 C12 1.376(3) . ? O2 C22 1.439(3) . ? N1 C21 1.293(3) . ? N1 C26 1.440(3) . ? C1 C10 1.394(4) . ? C1 C2 1.437(4) . ? C11 C12 1.378(4) . ? C11 C20 1.427(4) . ? C11 C10 1.495(4) . ? C21 C2 1.440(4) . ? C3 C2 1.382(4) . ? C3 C4 1.393(4) . ? C20 C19 1.418(4) . ? C20 C15 1.423(4) . ? C8 C7 1.366(4) . ? C8 C9 1.418(4) . ? C9 C4 1.423(4) . ? C9 C10 1.431(4) . ? C12 C13 1.412(4) . ? C26 C31 1.379(4) . ? C26 C27 1.387(4) . ? C4 C5 1.426(4) . ? C19 C18 1.363(4) . ? C33 C34 1.417(4) . ? C33 C32 1.423(4) . ? C33 C38 1.508(4) . ? C15 C14 1.417(4) . ? C15 C16 1.419(4) . ? C32 C36 1.412(4) . ? C32 C37 1.507(5) . ? C27 C28 1.391(4) . ? C5 C6 1.360(4) . ? C35 C36 1.413(4) . ? C35 C34 1.417(4) . ? C35 C40 1.507(4) . ? C36 C41 1.509(4) . ? C14 C13 1.350(4) . ? C16 C17 1.349(4) . ? C17 C18 1.404(4) . ? C34 C39 1.498(4) . ? C31 C30 1.392(4) . ? C7 C6 1.411(5) . ? C29 C28 1.366(5) . ? C29 C30 1.379(5) . ? C23 C22 1.510(5) . ? C23 C24 1.539(5) . ? C25 C24 1.519(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 O1 Cr1 N1 89.33(8) . . ? O1 Cr1 C35 94.89(9) . . ? N1 Cr1 C35 160.74(10) . . ? O1 Cr1 C36 86.56(10) . . ? N1 Cr1 C36 124.80(11) . . ? C35 Cr1 C36 37.17(11) . . ? O1 Cr1 C32 113.69(10) . . ? N1 Cr1 C32 99.01(10) . . ? C35 Cr1 C32 62.11(12) . . ? C36 Cr1 C32 36.69(11) . . ? O1 Cr1 C34 130.86(10) . . ? N1 Cr1 C34 139.04(10) . . ? C35 Cr1 C34 37.10(10) . . ? C36 Cr1 C34 61.21(10) . . ? C32 Cr1 C34 61.33(11) . . ? O1 Cr1 C33 147.45(10) . . ? N1 Cr1 C33 105.97(10) . . ? C35 Cr1 C33 61.80(11) . . ? C36 Cr1 C33 61.04(10) . . ? C32 Cr1 C33 36.72(10) . . ? C34 Cr1 C33 36.54(11) . . ? O1 Cr1 Cl1 96.59(7) . . ? N1 Cr1 Cl1 92.41(7) . . ? C35 Cr1 Cl1 105.71(9) . . ? C36 Cr1 Cl1 142.74(9) . . ? C32 Cr1 Cl1 147.57(8) . . ? C34 Cr1 Cl1 90.46(8) . . ? C33 Cr1 Cl1 110.91(8) . . ? C1 O1 Cr1 133.76(18) . . ? C12 O2 C22 118.2(2) . . ? C21 N1 C26 114.1(2) . . ? C21 N1 Cr1 123.98(19) . . ? C26 N1 Cr1 121.83(17) . . ? O1 C1 C10 119.8(3) . . ? O1 C1 C2 120.9(2) . . ? C10 C1 C2 119.2(2) . . ? C12 C11 C20 118.6(3) . . ? C12 C11 C10 120.1(3) . . ? C20 C11 C10 121.4(2) . . ? N1 C21 C2 127.7(3) . . ? C2 C3 C4 122.3(3) . . ? C19 C20 C15 117.3(3) . . ? C19 C20 C11 122.7(3) . . ? C15 C20 C11 120.0(2) . . ? C7 C8 C9 121.5(3) . . ? C8 C9 C4 117.7(2) . . ? C8 C9 C10 122.3(3) . . ? C4 C9 C10 120.1(2) . . ? C3 C2 C1 119.9(2) . . ? C3 C2 C21 116.7(3) . . ? C1 C2 C21 123.2(2) . . ? O2 C12 C11 116.6(3) . . ? O2 C12 C13 122.1(3) . . ? C11 C12 C13 121.3(3) . . ? C31 C26 C27 120.2(3) . . ? C31 C26 N1 119.9(2) . . ? C27 C26 N1 119.9(3) . . ? C1 C10 C9 120.1(3) . . ? C1 C10 C11 119.8(2) . . ? C9 C10 C11 120.0(2) . . ? C3 C4 C9 118.5(2) . . ? C3 C4 C5 121.9(3) . . ? C9 C4 C5 119.6(3) . . ? C18 C19 C20 121.0(3) . . ? C34 C33 C32 107.9(3) . . ? C34 C33 C38 125.7(3) . . ? C32 C33 C38 125.9(3) . . ? C34 C33 Cr1 71.13(16) . . ? C32 C33 Cr1 70.97(16) . . ? C38 C33 Cr1 129.4(2) . . ? C14 C15 C16 121.7(3) . . ? C14 C15 C20 118.3(3) . . ? C16 C15 C20 120.0(3) . . ? C36 C32 C33 107.5(3) . . ? C36 C32 C37 126.7(3) . . ? C33 C32 C37 125.6(3) . . ? C36 C32 Cr1 71.07(17) . . ? C33 C32 Cr1 72.31(16) . . ? C37 C32 Cr1 125.5(2) . . ? C26 C27 C28 118.9(3) . . ? C6 C5 C4 120.7(3) . . ? C36 C35 C34 107.6(3) . . ? C36 C35 C40 125.0(3) . . ? C34 C35 C40 127.4(3) . . ? C36 C35 Cr1 72.80(17) . . ? C34 C35 Cr1 73.49(17) . . ? C40 C35 Cr1 119.1(2) . . ? C32 C36 C35 108.7(3) . . ? C32 C36 C41 126.7(3) . . ? C35 C36 C41 124.7(3) . . ? C32 C36 Cr1 72.24(17) . . ? C35 C36 Cr1 70.03(16) . . ? C41 C36 Cr1 124.0(2) . . ? C13 C14 C15 121.3(3) . . ? C14 C13 C12 120.3(3) . . ? C17 C16 C15 120.7(3) . . ? C16 C17 C18 119.9(3) . . ? C35 C34 C33 108.1(3) . . ? C35 C34 C39 126.7(3) . . ? C33 C34 C39 125.2(3) . . ? C35 C34 Cr1 69.41(15) . . ? C33 C34 Cr1 72.33(16) . . ? C39 C34 Cr1 125.7(2) . . ? C26 C31 C30 120.3(3) . . ? C8 C7 C6 120.6(3) . . ? C19 C18 C17 121.2(3) . . ? C28 C29 C30 120.3(3) . . ? C29 C28 C27 121.0(3) . . ? C22 C23 C24 115.5(3) . . ? C5 C6 C7 120.0(3) . . ? O2 C22 C23 108.4(3) . . ? C29 C30 C31 119.4(3) . . ? C25 C24 C23 115.1(3) . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 26.04 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.426 _refine_diff_density_min -0.300 _refine_diff_density_rms 0.065 # Attachment '- complex 6.cif' data_cr3 _database_code_depnum_ccdc_archive 'CCDC 821442' #TrackingRef '- complex 6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H53 Cl Cr N O2' _chemical_formula_weight 751.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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 P21/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 11.6666(16) _cell_length_b 20.495(3) _cell_length_c 17.050(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.581(2) _cell_angle_gamma 90.00 _cell_volume 4072.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 23798 _cell_measurement_theta_min 1.55 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.225 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1596 _exptl_absorpt_coefficient_mu 0.385 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.800 _exptl_absorpt_correction_T_max 0.900 _exptl_absorpt_process_details 'ABSCOR by T.Higashi 8 March, 1995' _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 'Bruker Smart Apex CCD' _diffrn_measurement_method \w-2\q _diffrn_detector_area_resol_mean 0.01 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 23798 _diffrn_reflns_av_R_equivalents 0.0712 _diffrn_reflns_av_sigmaI/netI 0.0809 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7158 _reflns_number_gt 4080 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0700P)^2^+4.6320P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7158 _refine_ls_number_parameters 469 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.1369 _refine_ls_R_factor_gt 0.0731 _refine_ls_wR_factor_ref 0.1916 _refine_ls_wR_factor_gt 0.1623 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.080 _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 Cr1 Cr 0.32699(7) 0.26289(4) 0.33418(4) 0.0434(2) Uani 1 1 d . . . Cl1 Cl 0.32818(11) 0.20929(7) 0.21465(7) 0.0544(4) Uani 1 1 d . . . N1 N 0.1508(3) 0.28501(18) 0.3178(2) 0.0403(9) Uani 1 1 d . . . O1 O 0.3587(3) 0.34761(16) 0.29307(18) 0.0504(9) Uani 1 1 d . . . O2 O 0.4323(5) 0.5253(2) 0.2792(3) 0.1124(18) Uani 1 1 d . . . C21 C 0.1187(4) 0.3234(2) 0.2615(3) 0.0459(12) Uani 1 1 d . . . H21A H 0.0401 0.3249 0.2500 0.055 Uiso 1 1 calc R . . C2 C 0.1876(4) 0.3647(2) 0.2132(3) 0.0403(12) Uani 1 1 d . . . C1 C 0.3062(4) 0.3766(2) 0.2331(3) 0.0407(11) Uani 1 1 d . . . C10 C 0.3651(4) 0.4222(2) 0.1891(3) 0.0422(12) Uani 1 1 d . . . C9 C 0.3093(4) 0.4562(2) 0.1263(3) 0.0409(12) Uani 1 1 d . . . C8 C 0.3653(5) 0.5029(2) 0.0809(3) 0.0494(13) Uani 1 1 d . . . H8A H 0.4423 0.5120 0.0925 0.059 Uiso 1 1 calc R . . C7 C 0.3095(5) 0.5350(2) 0.0202(3) 0.0530(14) Uani 1 1 d . . . H7A H 0.3486 0.5656 -0.0086 0.064 Uiso 1 1 calc R . . C6 C 0.1946(5) 0.5220(3) 0.0014(3) 0.0626(16) Uani 1 1 d . . . H6A H 0.1570 0.5439 -0.0400 0.075 Uiso 1 1 calc R . . C5 C 0.1372(5) 0.4771(3) 0.0437(3) 0.0598(15) Uani 1 1 d . . . H5A H 0.0606 0.4685 0.0303 0.072 Uiso 1 1 calc R . . C4 C 0.1916(4) 0.4432(2) 0.1075(3) 0.0438(12) Uani 1 1 d . . . C3 C 0.1338(4) 0.3986(2) 0.1526(3) 0.0465(13) Uani 1 1 d . . . H3A H 0.0561 0.3915 0.1413 0.056 Uiso 1 1 calc R . . C26 C 0.0561(4) 0.2611(3) 0.3638(3) 0.0487(13) Uani 1 1 d . . . C27 C 0.0143(5) 0.1981(3) 0.3526(3) 0.0552(14) Uani 1 1 d . . . C28 C -0.0761(5) 0.1794(4) 0.3976(4) 0.0794(19) Uani 1 1 d . . . H28A H -0.1061 0.1377 0.3906 0.095 Uiso 1 1 calc R . . C29 C -0.1223(7) 0.2186(5) 0.4505(5) 0.105(3) Uani 1 1 d . . . H29A H -0.1817 0.2034 0.4802 0.126 Uiso 1 1 calc R . . C30 C -0.0823(6) 0.2806(4) 0.4610(4) 0.096(2) Uani 1 1 d . . . H30A H -0.1164 0.3079 0.4968 0.116 Uiso 1 1 calc R . . C31 C 0.0113(5) 0.3041(3) 0.4179(3) 0.0665(16) Uani 1 1 d . . . C32 C 0.0574(5) 0.1549(3) 0.2910(4) 0.0742(18) Uani 1 1 d . . . H32A H 0.1394 0.1639 0.2870 0.089 Uiso 1 1 calc R . . C33 C 0.0551(6) 0.3730(3) 0.4311(4) 0.0790(19) Uani 1 1 d . . . H33A H 0.1324 0.3753 0.4111 0.095 Uiso 1 1 calc R . . C34 C 0.0446(6) 0.0821(3) 0.3096(5) 0.111(3) Uani 1 1 d U . . H34A H 0.0815 0.0728 0.3598 0.166 Uiso 1 1 calc R . . H34B H 0.0797 0.0567 0.2699 0.166 Uiso 1 1 calc R . . H34C H -0.0354 0.0712 0.3107 0.166 Uiso 1 1 calc R . . C35 C -0.0006(8) 0.1694(4) 0.2120(4) 0.118(3) Uani 1 1 d . . . H35A H 0.0074 0.2150 0.2003 0.178 Uiso 1 1 calc R . . H35B H -0.0805 0.1586 0.2131 0.178 Uiso 1 1 calc R . . H35C H 0.0345 0.1440 0.1723 0.178 Uiso 1 1 calc R . . C37 C -0.0196(7) 0.4221(4) 0.3848(4) 0.102(2) Uani 1 1 d . . . H37A H -0.0247 0.4096 0.3305 0.153 Uiso 1 1 calc R . . H37B H 0.0140 0.4647 0.3898 0.153 Uiso 1 1 calc R . . H37C H -0.0950 0.4227 0.4051 0.153 Uiso 1 1 calc R . . C36 C 0.0641(7) 0.3923(4) 0.5186(4) 0.110(3) Uani 1 1 d . . . H36A H 0.1112 0.3611 0.5472 0.165 Uiso 1 1 calc R . . H36B H -0.0111 0.3928 0.5393 0.165 Uiso 1 1 calc R . . H36C H 0.0979 0.4348 0.5239 0.165 Uiso 1 1 calc R . . C11 C 0.4893(5) 0.4343(3) 0.2102(3) 0.0617(16) Uani 1 1 d . . . C12 C 0.5206(6) 0.4875(4) 0.2549(4) 0.087(2) Uani 1 1 d . . . C13 C 0.6318(8) 0.5001(4) 0.2803(5) 0.109(3) Uani 1 1 d U . . H13A H 0.6506 0.5344 0.3142 0.130 Uiso 1 1 calc R . . C14 C 0.7112(7) 0.4599(5) 0.2532(5) 0.098(2) Uani 1 1 d U . . H14A H 0.7873 0.4706 0.2657 0.118 Uiso 1 1 calc R . . C15 C 0.6924(7) 0.4037(5) 0.2082(5) 0.097(2) Uani 1 1 d U . . C16 C 0.7707(8) 0.3571(5) 0.1823(5) 0.119(3) Uani 1 1 d U . . H16A H 0.8479 0.3652 0.1944 0.143 Uiso 1 1 calc R . . C17 C 0.7461(7) 0.3027(5) 0.1422(5) 0.114(3) Uani 1 1 d U . . H17A H 0.8033 0.2731 0.1306 0.136 Uiso 1 1 calc R . . C18 C 0.6275(7) 0.2911(5) 0.1171(4) 0.113(3) Uani 1 1 d . . . H18A H 0.6072 0.2547 0.0871 0.136 Uiso 1 1 calc R . . C19 C 0.5458(5) 0.3350(4) 0.1387(4) 0.0760(19) Uani 1 1 d . . . H19A H 0.4695 0.3273 0.1235 0.091 Uiso 1 1 calc R . . C20 C 0.5735(5) 0.3912(4) 0.1831(4) 0.0734(19) Uani 1 1 d . . . C22 C 0.4524(8) 0.5697(4) 0.3445(5) 0.128(3) Uani 1 1 d U . . H22A H 0.5027 0.6050 0.3299 0.154 Uiso 1 1 calc R . . H22B H 0.4877 0.5470 0.3892 0.154 Uiso 1 1 calc R . . C23 C 0.3317(9) 0.5970(5) 0.3649(6) 0.140(3) Uani 1 1 d U . . H23A H 0.3408 0.6320 0.4028 0.168 Uiso 1 1 calc R . . H23B H 0.2928 0.6143 0.3179 0.168 Uiso 1 1 calc R . . C24 C 0.2622(9) 0.5433(6) 0.3980(7) 0.161(4) Uani 1 1 d U . . H24A H 0.1825 0.5567 0.3986 0.193 Uiso 1 1 calc R . . H24B H 0.2664 0.5050 0.3649 0.193 Uiso 1 1 calc R . . C25 C 0.3048(12) 0.5267(6) 0.4793(9) 0.208(5) Uani 1 1 d U . . H25A H 0.2590 0.4922 0.4995 0.312 Uiso 1 1 calc R . . H25B H 0.2994 0.5645 0.5122 0.312 Uiso 1 1 calc R . . H25C H 0.3833 0.5129 0.4785 0.312 Uiso 1 1 calc R . . C38 C 0.4837(5) 0.2087(3) 0.3794(3) 0.0603(15) Uani 1 1 d . . . C39 C 0.3846(5) 0.1796(3) 0.4115(3) 0.0570(15) Uani 1 1 d . . . C40 C 0.3333(5) 0.2256(3) 0.4586(3) 0.0576(15) Uani 1 1 d . . . C41 C 0.3973(5) 0.2848(3) 0.4547(3) 0.0605(15) Uani 1 1 d . . . C42 C 0.4903(5) 0.2724(3) 0.4063(3) 0.0631(16) Uani 1 1 d . . . C43 C 0.5673(5) 0.1753(3) 0.3285(4) 0.088(2) Uani 1 1 d . . . H43A H 0.6271 0.1556 0.3609 0.132 Uiso 1 1 calc R . . H43B H 0.6001 0.2068 0.2943 0.132 Uiso 1 1 calc R . . H43C H 0.5282 0.1423 0.2976 0.132 Uiso 1 1 calc R . . C44 C 0.3482(5) 0.1097(3) 0.4001(4) 0.0794(19) Uani 1 1 d . . . H44A H 0.3842 0.0832 0.4406 0.119 Uiso 1 1 calc R . . H44B H 0.3707 0.0947 0.3497 0.119 Uiso 1 1 calc R . . H44C H 0.2663 0.1066 0.4027 0.119 Uiso 1 1 calc R . . C45 C 0.2350(5) 0.2137(3) 0.5106(3) 0.0752(18) Uani 1 1 d . . . H45A H 0.2639 0.1977 0.5606 0.113 Uiso 1 1 calc R . . H45B H 0.1840 0.1820 0.4867 0.113 Uiso 1 1 calc R . . H45C H 0.1943 0.2538 0.5179 0.113 Uiso 1 1 calc R . . C46 C 0.3748(6) 0.3460(3) 0.4984(4) 0.089(2) Uani 1 1 d . . . H46A H 0.4141 0.3444 0.5491 0.133 Uiso 1 1 calc R . . H46B H 0.2938 0.3505 0.5048 0.133 Uiso 1 1 calc R . . H46C H 0.4020 0.3827 0.4695 0.133 Uiso 1 1 calc R . . C47 C 0.5817(5) 0.3215(3) 0.3871(4) 0.085(2) Uani 1 1 d . . . H47A H 0.6450 0.3180 0.4248 0.128 Uiso 1 1 calc R . . H47B H 0.5502 0.3648 0.3887 0.128 Uiso 1 1 calc R . . H47C H 0.6079 0.3130 0.3355 0.128 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 Cr1 0.0465(5) 0.0465(5) 0.0367(4) 0.0106(4) -0.0029(3) 0.0018(4) Cl1 0.0536(8) 0.0627(9) 0.0472(7) -0.0013(6) 0.0047(6) 0.0122(7) N1 0.047(2) 0.044(2) 0.031(2) 0.0063(18) 0.0077(18) 0.0036(19) O1 0.055(2) 0.052(2) 0.0429(19) 0.0164(16) -0.0123(16) -0.0050(17) O2 0.119(4) 0.083(4) 0.130(4) -0.033(3) -0.054(4) 0.000(3) C21 0.036(3) 0.062(3) 0.040(3) 0.000(3) 0.006(2) 0.012(2) C2 0.040(3) 0.042(3) 0.040(3) 0.008(2) 0.013(2) 0.011(2) C1 0.052(3) 0.036(3) 0.034(3) -0.001(2) -0.001(2) 0.003(2) C10 0.047(3) 0.038(3) 0.040(3) 0.003(2) -0.006(2) -0.002(2) C9 0.057(3) 0.034(3) 0.032(3) 0.000(2) 0.001(2) 0.002(2) C8 0.058(3) 0.041(3) 0.049(3) 0.002(2) -0.002(3) -0.008(3) C7 0.075(4) 0.040(3) 0.044(3) 0.012(2) 0.005(3) 0.002(3) C6 0.063(4) 0.064(4) 0.061(4) 0.025(3) 0.001(3) 0.019(3) C5 0.049(3) 0.071(4) 0.059(3) 0.026(3) 0.005(3) 0.014(3) C4 0.047(3) 0.041(3) 0.044(3) 0.009(2) 0.005(2) 0.020(2) C3 0.031(3) 0.058(3) 0.051(3) 0.016(3) 0.005(2) 0.011(2) C26 0.046(3) 0.062(3) 0.038(3) 0.010(3) 0.007(2) 0.006(3) C27 0.053(3) 0.062(4) 0.050(3) 0.014(3) 0.000(3) -0.003(3) C28 0.068(4) 0.094(5) 0.077(4) 0.022(4) 0.010(4) -0.024(4) C29 0.097(6) 0.132(8) 0.090(6) 0.007(5) 0.041(5) -0.031(5) C30 0.082(5) 0.127(7) 0.083(5) -0.003(5) 0.047(4) 0.000(5) C31 0.060(4) 0.083(5) 0.058(4) 0.003(3) 0.018(3) 0.002(3) C32 0.063(4) 0.065(4) 0.094(5) -0.007(4) 0.008(4) -0.012(3) C33 0.084(5) 0.083(5) 0.072(4) -0.018(4) 0.023(4) 0.010(4) C34 0.091(5) 0.075(5) 0.166(7) -0.011(5) 0.003(5) -0.011(4) C35 0.156(8) 0.128(7) 0.070(5) -0.027(5) 0.000(5) -0.042(6) C37 0.114(6) 0.093(6) 0.102(6) -0.011(5) 0.029(5) 0.024(5) C36 0.131(7) 0.121(7) 0.080(5) -0.036(5) 0.032(5) 0.010(5) C11 0.061(4) 0.064(4) 0.057(3) 0.031(3) -0.023(3) -0.019(3) C12 0.066(5) 0.095(6) 0.096(5) 0.026(4) -0.041(4) -0.024(4) C13 0.099(5) 0.102(5) 0.122(6) 0.025(5) -0.027(5) -0.028(5) C14 0.075(5) 0.116(6) 0.102(5) 0.027(5) -0.006(4) -0.035(5) C15 0.085(5) 0.117(6) 0.089(5) 0.046(4) 0.009(4) 0.014(5) C16 0.105(4) 0.138(5) 0.115(4) 0.023(4) 0.007(4) 0.009(4) C17 0.081(5) 0.159(7) 0.104(5) 0.026(5) 0.037(4) 0.058(5) C18 0.085(6) 0.167(8) 0.088(5) -0.001(5) 0.022(4) 0.059(6) C19 0.055(4) 0.111(6) 0.063(4) 0.010(4) 0.014(3) 0.022(4) C20 0.025(3) 0.116(6) 0.078(4) 0.029(4) -0.002(3) -0.010(4) C22 0.145(7) 0.119(6) 0.117(6) -0.026(5) -0.030(5) -0.049(5) C23 0.157(7) 0.120(6) 0.142(7) -0.035(6) -0.010(6) 0.025(6) C24 0.133(7) 0.170(8) 0.179(8) -0.016(7) 0.010(6) -0.006(6) C25 0.212(9) 0.172(8) 0.241(10) 0.008(8) 0.023(8) -0.014(7) C38 0.051(4) 0.073(4) 0.055(3) 0.022(3) -0.014(3) 0.009(3) C39 0.060(4) 0.055(4) 0.055(3) 0.023(3) -0.012(3) 0.003(3) C40 0.066(4) 0.069(4) 0.036(3) 0.020(3) -0.007(3) -0.002(3) C41 0.076(4) 0.062(4) 0.042(3) 0.015(3) -0.019(3) -0.009(3) C42 0.057(4) 0.081(5) 0.050(3) 0.023(3) -0.018(3) -0.012(3) C43 0.060(4) 0.104(5) 0.101(5) 0.033(4) -0.001(4) 0.023(4) C44 0.078(4) 0.060(4) 0.099(5) 0.032(4) -0.006(4) 0.012(3) C45 0.090(5) 0.091(5) 0.044(3) 0.020(3) 0.001(3) -0.004(4) C46 0.119(6) 0.088(5) 0.058(4) -0.008(4) -0.016(4) -0.016(4) C47 0.068(4) 0.101(5) 0.084(5) 0.033(4) -0.026(3) -0.029(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 O1 1.915(3) . ? Cr1 N1 2.111(4) . ? Cr1 C41 2.224(5) . ? Cr1 C42 2.229(5) . ? Cr1 C39 2.242(5) . ? Cr1 C38 2.246(5) . ? Cr1 C40 2.253(5) . ? Cr1 Cl1 2.3157(15) . ? N1 C21 1.285(6) . ? N1 C26 1.467(6) . ? O1 C1 1.311(5) . ? O2 C12 1.367(9) . ? O2 C22 1.449(8) . ? C21 C2 1.449(6) . ? C21 H21A 0.9300 . ? C2 C3 1.374(6) . ? C2 C1 1.430(6) . ? C1 C10 1.398(6) . ? C10 C9 1.411(6) . ? C10 C11 1.498(7) . ? C9 C8 1.410(6) . ? C9 C4 1.421(7) . ? C8 C7 1.366(7) . ? C8 H8A 0.9300 . ? C7 C6 1.390(7) . ? C7 H7A 0.9300 . ? C6 C5 1.363(7) . ? C6 H6A 0.9300 . ? C5 C4 1.418(6) . ? C5 H5A 0.9300 . ? C4 C3 1.387(6) . ? C3 H3A 0.9300 . ? C26 C27 1.391(7) . ? C26 C31 1.393(7) . ? C27 C28 1.385(8) . ? C27 C32 1.480(8) . ? C28 C29 1.340(9) . ? C28 H28A 0.9300 . ? C29 C30 1.362(10) . ? C29 H29A 0.9300 . ? C30 C31 1.428(8) . ? C30 H30A 0.9300 . ? C31 C33 1.516(8) . ? C32 C35 1.508(9) . ? C32 C34 1.534(9) . ? C32 H32A 0.9800 . ? C33 C37 1.527(9) . ? C33 C36 1.542(9) . ? C33 H33A 0.9800 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C11 C12 1.372(9) . ? C11 C20 1.414(9) . ? C12 C13 1.373(9) . ? C13 C14 1.338(11) . ? C13 H13A 0.9300 . ? C14 C15 1.397(11) . ? C14 H14A 0.9300 . ? C15 C16 1.405(11) . ? C15 C20 1.456(9) . ? C16 C17 1.333(11) . ? C16 H16A 0.9300 . ? C17 C18 1.448(11) . ? C17 H17A 0.9300 . ? C18 C19 1.372(9) . ? C18 H18A 0.9300 . ? C19 C20 1.408(9) . ? C19 H19A 0.9300 . ? C22 C23 1.568(12) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.493(13) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.491(15) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C38 C42 1.385(8) . ? C38 C39 1.431(7) . ? C38 C43 1.500(8) . ? C39 C40 1.391(7) . ? C39 C44 1.505(8) . ? C40 C41 1.428(7) . ? C40 C45 1.501(7) . ? C41 C42 1.416(8) . ? C41 C46 1.489(8) . ? C42 C47 1.513(8) . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? 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 Cr1 N1 87.72(14) . . ? O1 Cr1 C41 94.93(18) . . ? N1 Cr1 C41 113.3(2) . . ? O1 Cr1 C42 87.01(18) . . ? N1 Cr1 C42 149.0(2) . . ? C41 Cr1 C42 37.1(2) . . ? O1 Cr1 C39 147.99(18) . . ? N1 Cr1 C39 120.38(18) . . ? C41 Cr1 C39 61.4(2) . . ? C42 Cr1 C39 61.0(2) . . ? O1 Cr1 C38 113.96(19) . . ? N1 Cr1 C38 157.56(19) . . ? C41 Cr1 C38 61.4(2) . . ? C42 Cr1 C38 36.1(2) . . ? C39 Cr1 C38 37.20(19) . . ? O1 Cr1 C40 130.83(19) . . ? N1 Cr1 C40 100.81(18) . . ? C41 Cr1 C40 37.19(19) . . ? C42 Cr1 C40 61.3(2) . . ? C39 Cr1 C40 36.05(19) . . ? C38 Cr1 C40 61.1(2) . . ? O1 Cr1 Cl1 95.68(11) . . ? N1 Cr1 Cl1 91.72(11) . . ? C41 Cr1 Cl1 153.18(17) . . ? C42 Cr1 Cl1 119.23(19) . . ? C39 Cr1 Cl1 98.22(16) . . ? C38 Cr1 Cl1 91.76(17) . . ? C40 Cr1 Cl1 131.79(16) . . ? C21 N1 C26 113.7(4) . . ? C21 N1 Cr1 118.6(3) . . ? C26 N1 Cr1 127.6(3) . . ? C1 O1 Cr1 127.2(3) . . ? C12 O2 C22 119.4(6) . . ? N1 C21 C2 129.2(4) . . ? N1 C21 H21A 115.4 . . ? C2 C21 H21A 115.4 . . ? C3 C2 C1 119.8(4) . . ? C3 C2 C21 118.5(4) . . ? C1 C2 C21 121.3(4) . . ? O1 C1 C10 119.8(4) . . ? O1 C1 C2 121.4(4) . . ? C10 C1 C2 118.7(4) . . ? C1 C10 C9 121.1(4) . . ? C1 C10 C11 118.4(4) . . ? C9 C10 C11 120.5(4) . . ? C8 C9 C10 122.9(5) . . ? C8 C9 C4 118.0(4) . . ? C10 C9 C4 119.1(4) . . ? C7 C8 C9 121.8(5) . . ? C7 C8 H8A 119.1 . . ? C9 C8 H8A 119.1 . . ? C8 C7 C6 120.3(5) . . ? C8 C7 H7A 119.8 . . ? C6 C7 H7A 119.8 . . ? C5 C6 C7 119.9(5) . . ? C5 C6 H6A 120.0 . . ? C7 C6 H6A 120.0 . . ? C6 C5 C4 121.6(5) . . ? C6 C5 H5A 119.2 . . ? C4 C5 H5A 119.2 . . ? C3 C4 C5 122.4(5) . . ? C3 C4 C9 119.2(4) . . ? C5 C4 C9 118.4(5) . . ? C2 C3 C4 122.2(5) . . ? C2 C3 H3A 118.9 . . ? C4 C3 H3A 118.9 . . ? C27 C26 C31 122.5(5) . . ? C27 C26 N1 120.3(5) . . ? C31 C26 N1 117.2(5) . . ? C28 C27 C26 116.9(6) . . ? C28 C27 C32 121.3(6) . . ? C26 C27 C32 121.6(5) . . ? C29 C28 C27 123.1(7) . . ? C29 C28 H28A 118.4 . . ? C27 C28 H28A 118.4 . . ? C28 C29 C30 120.1(7) . . ? C28 C29 H29A 119.9 . . ? C30 C29 H29A 119.9 . . ? C29 C30 C31 120.8(7) . . ? C29 C30 H30A 119.6 . . ? C31 C30 H30A 119.6 . . ? C26 C31 C30 116.5(6) . . ? C26 C31 C33 123.6(5) . . ? C30 C31 C33 119.9(6) . . ? C27 C32 C35 111.3(6) . . ? C27 C32 C34 113.3(6) . . ? C35 C32 C34 109.5(6) . . ? C27 C32 H32A 107.5 . . ? C35 C32 H32A 107.5 . . ? C34 C32 H32A 107.5 . . ? C31 C33 C37 110.9(6) . . ? C31 C33 C36 113.0(6) . . ? C37 C33 C36 110.2(6) . . ? C31 C33 H33A 107.5 . . ? C37 C33 H33A 107.5 . . ? C36 C33 H33A 107.5 . . ? 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 . . ? C32 C35 H35A 109.5 . . ? C32 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C32 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C37 H37A 109.5 . . ? C33 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C33 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C12 C11 C20 120.4(6) . . ? C12 C11 C10 119.7(6) . . ? C20 C11 C10 119.9(5) . . ? O2 C12 C11 115.7(6) . . ? O2 C12 C13 120.8(8) . . ? C11 C12 C13 123.3(8) . . ? C14 C13 C12 115.8(9) . . ? C14 C13 H13A 122.1 . . ? C12 C13 H13A 122.1 . . ? C13 C14 C15 127.1(8) . . ? C13 C14 H14A 116.4 . . ? C15 C14 H14A 116.4 . . ? C14 C15 C16 130.1(9) . . ? C14 C15 C20 115.5(8) . . ? C16 C15 C20 114.4(9) . . ? C17 C16 C15 127.0(9) . . ? C17 C16 H16A 116.5 . . ? C15 C16 H16A 116.5 . . ? C16 C17 C18 117.9(8) . . ? C16 C17 H17A 121.0 . . ? C18 C17 H17A 121.0 . . ? C19 C18 C17 118.7(8) . . ? C19 C18 H18A 120.7 . . ? C17 C18 H18A 120.7 . . ? C18 C19 C20 122.3(7) . . ? C18 C19 H19A 118.9 . . ? C20 C19 H19A 118.9 . . ? C19 C20 C11 122.7(5) . . ? C19 C20 C15 119.6(7) . . ? C11 C20 C15 117.5(7) . . ? O2 C22 C23 106.1(7) . . ? O2 C22 H22A 110.5 . . ? C23 C22 H22A 110.5 . . ? O2 C22 H22B 110.5 . . ? C23 C22 H22B 110.5 . . ? H22A C22 H22B 108.7 . . ? C24 C23 C22 109.3(8) . . ? C24 C23 H23A 109.8 . . ? C22 C23 H23A 109.8 . . ? C24 C23 H23B 109.8 . . ? C22 C23 H23B 109.8 . . ? H23A C23 H23B 108.3 . . ? C25 C24 C23 110.8(10) . . ? C25 C24 H24A 109.5 . . ? C23 C24 H24A 109.5 . . ? C25 C24 H24B 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 108.1 . . ? 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 . . ? C42 C38 C39 107.5(5) . . ? C42 C38 C43 126.4(6) . . ? C39 C38 C43 126.1(6) . . ? C42 C38 Cr1 71.3(3) . . ? C39 C38 Cr1 71.2(3) . . ? C43 C38 Cr1 124.5(4) . . ? C40 C39 C38 108.3(5) . . ? C40 C39 C44 126.4(5) . . ? C38 C39 C44 125.2(6) . . ? C40 C39 Cr1 72.4(3) . . ? C38 C39 Cr1 71.6(3) . . ? C44 C39 Cr1 125.0(4) . . ? C39 C40 C41 108.0(5) . . ? C39 C40 C45 126.3(5) . . ? C41 C40 C45 125.4(6) . . ? C39 C40 Cr1 71.5(3) . . ? C41 C40 Cr1 70.3(3) . . ? C45 C40 Cr1 128.2(4) . . ? C42 C41 C40 106.9(5) . . ? C42 C41 C46 126.8(6) . . ? C40 C41 C46 126.1(6) . . ? C42 C41 Cr1 71.7(3) . . ? C40 C41 Cr1 72.5(3) . . ? C46 C41 Cr1 124.5(4) . . ? C38 C42 C41 109.2(5) . . ? C38 C42 C47 125.8(6) . . ? C41 C42 C47 125.0(6) . . ? C38 C42 Cr1 72.6(3) . . ? C41 C42 Cr1 71.3(3) . . ? C47 C42 Cr1 122.1(4) . . ? C38 C43 H43A 109.5 . . ? C38 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C38 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C39 C44 H44A 109.5 . . ? C39 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C39 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C40 C45 H45A 109.5 . . ? C40 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C40 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C41 C46 H46A 109.5 . . ? C41 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C41 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C42 C47 H47A 109.5 . . ? C42 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C42 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Cr1 N1 C21 30.5(4) . . . . ? C41 Cr1 N1 C21 124.9(4) . . . . ? C42 Cr1 N1 C21 110.9(5) . . . . ? C39 Cr1 N1 C21 -165.7(4) . . . . ? C38 Cr1 N1 C21 -163.9(5) . . . . ? C40 Cr1 N1 C21 161.7(4) . . . . ? Cl1 Cr1 N1 C21 -65.1(4) . . . . ? O1 Cr1 N1 C26 -149.9(4) . . . . ? C41 Cr1 N1 C26 -55.5(4) . . . . ? C42 Cr1 N1 C26 -69.6(5) . . . . ? C39 Cr1 N1 C26 13.9(5) . . . . ? C38 Cr1 N1 C26 15.6(7) . . . . ? C40 Cr1 N1 C26 -18.7(4) . . . . ? Cl1 Cr1 N1 C26 114.5(4) . . . . ? N1 Cr1 O1 C1 -41.7(4) . . . . ? C41 Cr1 O1 C1 -154.8(4) . . . . ? C42 Cr1 O1 C1 168.9(4) . . . . ? C39 Cr1 O1 C1 165.3(4) . . . . ? C38 Cr1 O1 C1 144.3(4) . . . . ? C40 Cr1 O1 C1 -144.0(4) . . . . ? Cl1 Cr1 O1 C1 49.8(4) . . . . ? C26 N1 C21 C2 168.1(5) . . . . ? Cr1 N1 C21 C2 -12.2(7) . . . . ? N1 C21 C2 C3 175.8(5) . . . . ? N1 C21 C2 C1 -11.6(8) . . . . ? Cr1 O1 C1 C10 -152.0(3) . . . . ? Cr1 O1 C1 C2 30.9(6) . . . . ? C3 C2 C1 O1 176.4(4) . . . . ? C21 C2 C1 O1 3.9(7) . . . . ? C3 C2 C1 C10 -0.8(7) . . . . ? C21 C2 C1 C10 -173.3(4) . . . . ? O1 C1 C10 C9 -177.3(4) . . . . ? C2 C1 C10 C9 0.0(7) . . . . ? O1 C1 C10 C11 2.9(7) . . . . ? C2 C1 C10 C11 -179.9(5) . . . . ? C1 C10 C9 C8 179.6(4) . . . . ? C11 C10 C9 C8 -0.5(7) . . . . ? C1 C10 C9 C4 -0.4(7) . . . . ? C11 C10 C9 C4 179.5(5) . . . . ? C10 C9 C8 C7 179.8(5) . . . . ? C4 C9 C8 C7 -0.2(7) . . . . ? C9 C8 C7 C6 -0.2(8) . . . . ? C8 C7 C6 C5 0.1(8) . . . . ? C7 C6 C5 C4 0.6(8) . . . . ? C6 C5 C4 C3 178.2(5) . . . . ? C6 C5 C4 C9 -1.0(8) . . . . ? C8 C9 C4 C3 -178.4(4) . . . . ? C10 C9 C4 C3 1.5(7) . . . . ? C8 C9 C4 C5 0.8(7) . . . . ? C10 C9 C4 C5 -179.2(4) . . . . ? C1 C2 C3 C4 2.0(7) . . . . ? C21 C2 C3 C4 174.7(4) . . . . ? C5 C4 C3 C2 178.4(5) . . . . ? C9 C4 C3 C2 -2.4(7) . . . . ? C21 N1 C26 C27 102.8(5) . . . . ? Cr1 N1 C26 C27 -76.8(5) . . . . ? C21 N1 C26 C31 -77.2(6) . . . . ? Cr1 N1 C26 C31 103.2(5) . . . . ? C31 C26 C27 C28 0.7(8) . . . . ? N1 C26 C27 C28 -179.3(5) . . . . ? C31 C26 C27 C32 175.6(5) . . . . ? N1 C26 C27 C32 -4.5(8) . . . . ? C26 C27 C28 C29 -0.9(9) . . . . ? C32 C27 C28 C29 -175.7(7) . . . . ? C27 C28 C29 C30 1.5(12) . . . . ? C28 C29 C30 C31 -2.0(13) . . . . ? C27 C26 C31 C30 -1.2(8) . . . . ? N1 C26 C31 C30 178.8(5) . . . . ? C27 C26 C31 C33 -179.9(5) . . . . ? N1 C26 C31 C33 0.1(8) . . . . ? C29 C30 C31 C26 1.8(11) . . . . ? C29 C30 C31 C33 -179.4(7) . . . . ? C28 C27 C32 C35 92.7(7) . . . . ? C26 C27 C32 C35 -81.9(7) . . . . ? C28 C27 C32 C34 -31.1(8) . . . . ? C26 C27 C32 C34 154.3(6) . . . . ? C26 C31 C33 C37 97.3(7) . . . . ? C30 C31 C33 C37 -81.5(7) . . . . ? C26 C31 C33 C36 -138.5(6) . . . . ? C30 C31 C33 C36 42.7(9) . . . . ? C1 C10 C11 C12 -99.4(6) . . . . ? C9 C10 C11 C12 80.8(7) . . . . ? C1 C10 C11 C20 81.4(6) . . . . ? C9 C10 C11 C20 -98.5(6) . . . . ? C22 O2 C12 C11 161.4(6) . . . . ? C22 O2 C12 C13 -13.1(11) . . . . ? C20 C11 C12 O2 -178.9(5) . . . . ? C10 C11 C12 O2 1.9(8) . . . . ? C20 C11 C12 C13 -4.5(10) . . . . ? C10 C11 C12 C13 176.3(6) . . . . ? O2 C12 C13 C14 179.6(7) . . . . ? C11 C12 C13 C14 5.5(11) . . . . ? C12 C13 C14 C15 -6.3(12) . . . . ? C13 C14 C15 C16 -175.2(8) . . . . ? C13 C14 C15 C20 5.5(12) . . . . ? C14 C15 C16 C17 176.7(8) . . . . ? C20 C15 C16 C17 -4.0(12) . . . . ? C15 C16 C17 C18 4.5(14) . . . . ? C16 C17 C18 C19 -2.8(12) . . . . ? C17 C18 C19 C20 1.1(10) . . . . ? C18 C19 C20 C11 -175.5(6) . . . . ? C18 C19 C20 C15 -0.7(10) . . . . ? C12 C11 C20 C19 178.3(6) . . . . ? C10 C11 C20 C19 -2.5(8) . . . . ? C12 C11 C20 C15 3.4(8) . . . . ? C10 C11 C20 C15 -177.4(5) . . . . ? C14 C15 C20 C19 -178.8(6) . . . . ? C16 C15 C20 C19 1.8(9) . . . . ? C14 C15 C20 C11 -3.7(9) . . . . ? C16 C15 C20 C11 176.9(6) . . . . ? C12 O2 C22 C23 -171.7(7) . . . . ? O2 C22 C23 C24 68.2(10) . . . . ? C22 C23 C24 C25 73.0(12) . . . . ? O1 Cr1 C38 C42 45.0(4) . . . . ? N1 Cr1 C38 C42 -119.2(5) . . . . ? C41 Cr1 C38 C42 -37.3(3) . . . . ? C39 Cr1 C38 C42 -116.7(5) . . . . ? C40 Cr1 C38 C42 -79.9(4) . . . . ? Cl1 Cr1 C38 C42 142.0(3) . . . . ? O1 Cr1 C38 C39 161.7(3) . . . . ? N1 Cr1 C38 C39 -2.5(7) . . . . ? C41 Cr1 C38 C39 79.4(4) . . . . ? C42 Cr1 C38 C39 116.7(5) . . . . ? C40 Cr1 C38 C39 36.8(3) . . . . ? Cl1 Cr1 C38 C39 -101.3(3) . . . . ? O1 Cr1 C38 C43 -76.9(6) . . . . ? N1 Cr1 C38 C43 118.9(6) . . . . ? C41 Cr1 C38 C43 -159.2(6) . . . . ? C42 Cr1 C38 C43 -121.9(7) . . . . ? C39 Cr1 C38 C43 121.4(7) . . . . ? C40 Cr1 C38 C43 158.2(6) . . . . ? Cl1 Cr1 C38 C43 20.1(5) . . . . ? C42 C38 C39 C40 -1.0(6) . . . . ? C43 C38 C39 C40 176.9(5) . . . . ? Cr1 C38 C39 C40 -63.5(4) . . . . ? C42 C38 C39 C44 -177.2(5) . . . . ? C43 C38 C39 C44 0.8(8) . . . . ? Cr1 C38 C39 C44 120.3(5) . . . . ? C42 C38 C39 Cr1 62.5(4) . . . . ? C43 C38 C39 Cr1 -119.5(5) . . . . ? O1 Cr1 C39 C40 84.1(5) . . . . ? N1 Cr1 C39 C40 -64.2(4) . . . . ? C41 Cr1 C39 C40 37.5(3) . . . . ? C42 Cr1 C39 C40 80.0(4) . . . . ? C38 Cr1 C39 C40 116.9(5) . . . . ? Cl1 Cr1 C39 C40 -161.0(3) . . . . ? O1 Cr1 C39 C38 -32.8(6) . . . . ? N1 Cr1 C39 C38 178.9(3) . . . . ? C41 Cr1 C39 C38 -79.4(4) . . . . ? C42 Cr1 C39 C38 -36.9(3) . . . . ? C40 Cr1 C39 C38 -116.9(5) . . . . ? Cl1 Cr1 C39 C38 82.0(3) . . . . ? O1 Cr1 C39 C44 -153.3(4) . . . . ? N1 Cr1 C39 C44 58.4(6) . . . . ? C41 Cr1 C39 C44 160.0(6) . . . . ? C42 Cr1 C39 C44 -157.4(6) . . . . ? C38 Cr1 C39 C44 -120.5(7) . . . . ? C40 Cr1 C39 C44 122.5(7) . . . . ? Cl1 Cr1 C39 C44 -38.5(5) . . . . ? C38 C39 C40 C41 1.8(6) . . . . ? C44 C39 C40 C41 177.9(5) . . . . ? Cr1 C39 C40 C41 -61.2(3) . . . . ? C38 C39 C40 C45 -172.7(5) . . . . ? C44 C39 C40 C45 3.3(9) . . . . ? Cr1 C39 C40 C45 124.3(5) . . . . ? C38 C39 C40 Cr1 63.0(3) . . . . ? C44 C39 C40 Cr1 -120.9(5) . . . . ? O1 Cr1 C40 C39 -135.8(3) . . . . ? N1 Cr1 C40 C39 127.8(3) . . . . ? C41 Cr1 C40 C39 -117.8(5) . . . . ? C42 Cr1 C40 C39 -79.3(4) . . . . ? C38 Cr1 C40 C39 -38.0(3) . . . . ? Cl1 Cr1 C40 C39 25.6(4) . . . . ? O1 Cr1 C40 C41 -18.0(4) . . . . ? N1 Cr1 C40 C41 -114.4(4) . . . . ? C42 Cr1 C40 C41 38.5(3) . . . . ? C39 Cr1 C40 C41 117.8(5) . . . . ? C38 Cr1 C40 C41 79.8(4) . . . . ? Cl1 Cr1 C40 C41 143.4(3) . . . . ? O1 Cr1 C40 C45 102.1(5) . . . . ? N1 Cr1 C40 C45 5.7(6) . . . . ? C41 Cr1 C40 C45 120.1(7) . . . . ? C42 Cr1 C40 C45 158.6(6) . . . . ? C39 Cr1 C40 C45 -122.1(7) . . . . ? C38 Cr1 C40 C45 -160.1(6) . . . . ? Cl1 Cr1 C40 C45 -96.5(6) . . . . ? C39 C40 C41 C42 -1.9(6) . . . . ? C45 C40 C41 C42 172.7(5) . . . . ? Cr1 C40 C41 C42 -63.8(3) . . . . ? C39 C40 C41 C46 -177.7(5) . . . . ? C45 C40 C41 C46 -3.1(9) . . . . ? Cr1 C40 C41 C46 120.3(6) . . . . ? C39 C40 C41 Cr1 61.9(4) . . . . ? C45 C40 C41 Cr1 -123.4(5) . . . . ? O1 Cr1 C41 C42 -78.4(4) . . . . ? N1 Cr1 C41 C42 -168.0(3) . . . . ? C39 Cr1 C41 C42 78.8(4) . . . . ? C38 Cr1 C41 C42 36.3(3) . . . . ? C40 Cr1 C41 C42 115.2(5) . . . . ? Cl1 Cr1 C41 C42 34.6(6) . . . . ? O1 Cr1 C41 C40 166.4(3) . . . . ? N1 Cr1 C41 C40 76.8(4) . . . . ? C42 Cr1 C41 C40 -115.2(5) . . . . ? C39 Cr1 C41 C40 -36.4(3) . . . . ? C38 Cr1 C41 C40 -78.9(4) . . . . ? Cl1 Cr1 C41 C40 -80.6(5) . . . . ? O1 Cr1 C41 C46 44.2(5) . . . . ? N1 Cr1 C41 C46 -45.5(6) . . . . ? C42 Cr1 C41 C46 122.6(7) . . . . ? C39 Cr1 C41 C46 -158.6(6) . . . . ? C38 Cr1 C41 C46 158.8(6) . . . . ? C40 Cr1 C41 C46 -122.2(7) . . . . ? Cl1 Cr1 C41 C46 157.2(4) . . . . ? C39 C38 C42 C41 -0.2(6) . . . . ? C43 C38 C42 C41 -178.1(5) . . . . ? Cr1 C38 C42 C41 62.3(4) . . . . ? C39 C38 C42 C47 -179.9(5) . . . . ? C43 C38 C42 C47 2.1(9) . . . . ? Cr1 C38 C42 C47 -117.5(5) . . . . ? C39 C38 C42 Cr1 -62.4(3) . . . . ? C43 C38 C42 Cr1 119.6(5) . . . . ? C40 C41 C42 C38 1.3(6) . . . . ? C46 C41 C42 C38 177.1(5) . . . . ? Cr1 C41 C42 C38 -63.1(4) . . . . ? C40 C41 C42 C47 -179.0(5) . . . . ? C46 C41 C42 C47 -3.2(8) . . . . ? Cr1 C41 C42 C47 116.6(5) . . . . ? C40 C41 C42 Cr1 64.4(3) . . . . ? C46 C41 C42 Cr1 -119.8(5) . . . . ? O1 Cr1 C42 C38 -139.7(4) . . . . ? N1 Cr1 C42 C38 139.7(4) . . . . ? C41 Cr1 C42 C38 118.1(5) . . . . ? C39 Cr1 C42 C38 38.1(3) . . . . ? C40 Cr1 C42 C38 79.5(4) . . . . ? Cl1 Cr1 C42 C38 -44.9(4) . . . . ? O1 Cr1 C42 C41 102.2(3) . . . . ? N1 Cr1 C42 C41 21.7(6) . . . . ? C39 Cr1 C42 C41 -80.0(4) . . . . ? C38 Cr1 C42 C41 -118.1(5) . . . . ? C40 Cr1 C42 C41 -38.6(3) . . . . ? Cl1 Cr1 C42 C41 -162.9(3) . . . . ? O1 Cr1 C42 C47 -17.9(6) . . . . ? N1 Cr1 C42 C47 -98.5(6) . . . . ? C41 Cr1 C42 C47 -120.1(7) . . . . ? C39 Cr1 C42 C47 159.9(7) . . . . ? C38 Cr1 C42 C47 121.8(7) . . . . ? C40 Cr1 C42 C47 -158.7(7) . . . . ? Cl1 Cr1 C42 C47 76.9(6) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.452 _refine_diff_density_min -0.356 _refine_diff_density_rms 0.064