# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1995 data_VG9833 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C61 H93 N2 O2 Cr' _chemical_formula_weight 938.37 _chemical_melting_point ? _chemical_compound_source ? 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' 'Cr' 'Cr' 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x, y, -z-1/2' '-x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z-1/2' _cell_length_a 25.231(3) _cell_length_b 10.1531(14) _cell_length_c 25.314(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.013(14) _cell_angle_gamma 90.00 _cell_volume 6484.7(20) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 5.25 _cell_measurement_theta_max 12.37 _exptl_crystal_description prisms _exptl_crystal_colour Orange/red _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.47 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.961 _exptl_crystal_density_method ? _exptl_crystal_F_000 2052 _exptl_absorpt_coefficient_mu 0.212 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 13.01 _diffrn_reflns_number 4350 _diffrn_reflns_av_R_equivalents 0.0220 _diffrn_reflns_av_sigmaI/netI 0.0824 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 22.50 _reflns_number_total 4236 _reflns_number_observed 2772 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 386 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1123P)^2^+5.4533P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3850 _refine_ls_number_parameters 321 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1340 _refine_ls_R_factor_obs 0.0832 _refine_ls_wR_factor_all 0.2684 _refine_ls_wR_factor_obs 0.2024 _refine_ls_goodness_of_fit_all 1.072 _refine_ls_goodness_of_fit_obs 1.172 _refine_ls_restrained_S_all 1.258 _refine_ls_restrained_S_obs 1.172 _refine_ls_shift/esd_max 0.074 _refine_ls_shift/esd_mean 0.002 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cr Cr 0.0000 0.13897(13) 0.2500 0.0400(4) Uani 1 d S . O O -0.05945(13) 0.1388(4) 0.29905(13) 0.0480(9) Uani 1 d . . N N -0.0516(2) 0.1957(5) 0.1904(2) 0.0453(11) Uani 1 d . . C1 C -0.0051(6) -0.0606(12) 0.2351(4) 0.051(3) Uani 0.50 d P -1 H1A H -0.0382(6) -0.0959(12) 0.2495(4) 0.062 Uiso 0.50 calc PR -1 H1B H -0.0046(6) -0.0768(12) 0.1969(4) 0.062 Uiso 0.50 calc PR -1 C2 C 0.0419(7) -0.1270(15) 0.2611(5) 0.073(4) Uani 0.50 d P -1 H2A H 0.0404(7) -0.2211(15) 0.2546(5) 0.110 Uiso 0.50 calc PR -1 H2B H 0.0410(7) -0.1107(15) 0.2988(5) 0.110 Uiso 0.50 calc PR -1 H2C H 0.0745(7) -0.0917(15) 0.2464(5) 0.110 Uiso 0.50 calc PR -1 C3 C -0.1108(2) 0.1398(6) 0.2918(2) 0.0450(12) Uani 1 d . . C4 C -0.1470(2) 0.0962(6) 0.3315(2) 0.0518(15) Uani 1 d . . C5 C -0.1997(2) 0.1149(6) 0.3227(2) 0.056(2) Uani 1 d . . H5A H -0.2230(2) 0.0887(6) 0.3497(2) 0.067 Uiso 1 calc R . C6 C -0.2227(2) 0.1695(6) 0.2771(2) 0.0544(15) Uani 1 d . . C7 C -0.1884(2) 0.2019(6) 0.2381(2) 0.0530(14) Uani 1 d . . H7A H -0.2017(2) 0.2362(6) 0.2063(2) 0.064 Uiso 1 calc R . C8 C -0.1329(2) 0.1853(5) 0.2441(2) 0.0415(12) Uani 1 d . . C9 C -0.1020(2) 0.2160(6) 0.1991(2) 0.0467(13) Uani 1 d . . H9A H -0.1205(2) 0.2570(6) 0.1713(2) 0.056 Uiso 1 calc R . C10 C -0.0359(2) 0.2280(6) 0.1363(2) 0.0518(15) Uani 1 d . . C11 C -0.0509(2) 0.1440(7) 0.0960(2) 0.059(2) Uani 1 d . . C12 C -0.0386(2) 0.1808(8) 0.0438(2) 0.068(2) Uani 1 d . . H12A H -0.0486(2) 0.1263(8) 0.0154(2) 0.082 Uiso 1 calc R . C13 C -0.0118(3) 0.2976(9) 0.0342(3) 0.081(2) Uani 1 d . . H13A H -0.0034(3) 0.3217(9) -0.0007(3) 0.098 Uiso 1 calc R . C14 C 0.0025(3) 0.3769(8) 0.0744(3) 0.075(2) Uani 1 d . . H14A H 0.0204(3) 0.4561(8) 0.0670(3) 0.089 Uiso 1 calc R . C15 C -0.0086(2) 0.3441(7) 0.1266(3) 0.059(2) Uani 1 d . . C16 C -0.1274(3) 0.0320(9) 0.3828(2) 0.074(2) Uani 1 d . . C17 C -0.0924(3) -0.0885(9) 0.3688(3) 0.094(3) Uani 1 d . . H17A H -0.1128(3) -0.1505(9) 0.3480(3) 0.142 Uiso 1 calc R . H17B H -0.0805(3) -0.1308(9) 0.4010(3) 0.142 Uiso 1 calc R . H17C H -0.0619(3) -0.0594(9) 0.3486(3) 0.142 Uiso 1 calc R . C18 C -0.0960(3) 0.1304(10) 0.4154(2) 0.091(3) Uani 1 d . . H18A H -0.0838(3) 0.0885(10) 0.4477(2) 0.137 Uiso 1 calc R . H18B H -0.1183(3) 0.2050(10) 0.4242(2) 0.137 Uiso 1 calc R . H18C H -0.0656(3) 0.1606(10) 0.3953(2) 0.137 Uiso 1 calc R . C19 C -0.1736(3) -0.0201(10) 0.4162(3) 0.099(3) Uani 1 d . . H19A H -0.1940(3) -0.0830(10) 0.3957(3) 0.148 Uiso 1 calc R . H19B H -0.1963(3) 0.0527(10) 0.4265(3) 0.148 Uiso 1 calc R . H19C H -0.1599(3) -0.0629(10) 0.4476(3) 0.148 Uiso 1 calc R . C20 C -0.2829(2) 0.1888(7) 0.2731(3) 0.070(2) Uani 1 d . . C21 C -0.3023(4) 0.2777(13) 0.3180(5) 0.134(4) Uani 1 d . . H21A H -0.2923(4) 0.2395(13) 0.3516(5) 0.201 Uiso 1 calc R . H21B H -0.3406(4) 0.2858(13) 0.3161(5) 0.201 Uiso 1 calc R . H21C H -0.2863(4) 0.3642(13) 0.3145(5) 0.201 Uiso 1 calc R . C22 C -0.3100(3) 0.0558(9) 0.2786(4) 0.098(3) Uani 1 d . . H22A H -0.2999(3) 0.0159(9) 0.3119(4) 0.147 Uiso 1 calc R . H22B H -0.2992(3) -0.0010(9) 0.2497(4) 0.147 Uiso 1 calc R . H22C H -0.3481(3) 0.0676(9) 0.2777(4) 0.147 Uiso 1 calc R . C23 C -0.2988(3) 0.2500(11) 0.2213(4) 0.115(4) Uani 1 d . . H23A H -0.2816(3) 0.3349(11) 0.2175(4) 0.173 Uiso 1 calc R . H23B H -0.3369(3) 0.2615(11) 0.2204(4) 0.173 Uiso 1 calc R . H23C H -0.2880(3) 0.1928(11) 0.1925(4) 0.173 Uiso 1 calc R . C24 C -0.0810(3) 0.0171(7) 0.1044(2) 0.066(2) Uani 1 d . . H24A H -0.0829(3) 0.0014(7) 0.1429(2) 0.080 Uiso 1 calc R . C25 C -0.1381(3) 0.0275(10) 0.0837(3) 0.096(3) Uani 1 d . . H25A H -0.1564(3) -0.0553(10) 0.0897(3) 0.143 Uiso 1 calc R . H25B H -0.1376(3) 0.0467(10) 0.0462(3) 0.143 Uiso 1 calc R . H25C H -0.1564(3) 0.0975(10) 0.1023(3) 0.143 Uiso 1 calc R . C26 C -0.0535(3) -0.1014(8) 0.0796(3) 0.081(2) Uani 1 d . . H26A H -0.0743(3) -0.1801(8) 0.0861(3) 0.122 Uiso 1 calc R . H26B H -0.0186(3) -0.1119(8) 0.0950(3) 0.122 Uiso 1 calc R . H26C H -0.0501(3) -0.0878(8) 0.0418(3) 0.122 Uiso 1 calc R . C27 C 0.0055(3) 0.4387(7) 0.1711(3) 0.077(2) Uani 1 d . . H27A H 0.0006(3) 0.3903(7) 0.2047(3) 0.093 Uiso 1 calc R . C28 C -0.0327(4) 0.5556(10) 0.1721(5) 0.134(4) Uani 1 d . . H28A H -0.0231(4) 0.6146(10) 0.2007(5) 0.201 Uiso 1 calc R . H28B H -0.0686(4) 0.5240(10) 0.1774(5) 0.201 Uiso 1 calc R . H28C H -0.0307(4) 0.6024(10) 0.1387(5) 0.201 Uiso 1 calc R . C29 C 0.0635(4) 0.4835(11) 0.1693(4) 0.118(3) Uani 1 d . . H29A H 0.0704(4) 0.5434(11) 0.1983(4) 0.177 Uiso 1 calc R . H29B H 0.0703(4) 0.5282(11) 0.1361(4) 0.177 Uiso 1 calc R . H29C H 0.0866(4) 0.4074(11) 0.1722(4) 0.177 Uiso 1 calc R . C31 C -0.1690(11) 0.3985(31) 0.0689(11) 0.147(9) Uiso 0.50 d P . C32 C -0.1712(17) 0.4995(42) 0.0271(20) 0.156(13) Uiso 0.38 d P . C33 C -0.1309(19) 0.5808(48) 0.0361(18) 0.150(14) Uiso 0.32 d P . C34 C -0.2004(19) 0.5002(48) -0.0889(18) 0.151(15) Uiso 0.30 d P . C35 C -0.1960(30) 0.4677(72) -0.0214(27) 0.156(23) Uiso 0.24 d P . C36 C -0.1406(28) 0.4869(76) 0.0691(27) 0.166(22) Uiso 0.24 d P . C37 C -0.2223(27) 0.6146(70) -0.0385(26) 0.152(21) Uiso 0.21 d P . C38 C -0.1560(40) 0.3972(111) -0.0339(39) 0.159(34) Uiso 0.16 d P . C39 C -0.1651(51) 0.4720(125) -0.0128(53) 0.151(36) Uiso 0.15 d P . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr 0.0363(6) 0.0443(7) 0.0393(7) 0.000 -0.0065(5) 0.000 O 0.039(2) 0.063(2) 0.042(2) 0.001(2) -0.0086(14) -0.006(2) N 0.041(3) 0.056(3) 0.039(2) 0.003(2) -0.006(2) 0.001(2) C1 0.066(8) 0.048(6) 0.040(9) -0.003(4) -0.009(8) -0.011(7) C2 0.103(11) 0.055(8) 0.062(8) -0.001(7) -0.019(7) 0.007(9) C3 0.038(3) 0.049(3) 0.048(3) -0.003(3) -0.007(2) -0.002(3) C4 0.046(3) 0.067(4) 0.042(3) -0.006(3) -0.004(2) -0.014(3) C5 0.051(3) 0.065(4) 0.051(3) 0.000(3) 0.003(3) -0.014(3) C6 0.045(3) 0.057(4) 0.061(4) 0.003(3) 0.000(3) -0.003(3) C7 0.045(3) 0.054(3) 0.060(4) 0.001(3) -0.007(3) 0.004(3) C8 0.038(3) 0.045(3) 0.041(3) 0.000(2) -0.001(2) -0.001(2) C9 0.042(3) 0.051(3) 0.047(3) 0.006(3) -0.010(2) 0.006(3) C10 0.039(3) 0.068(4) 0.048(3) 0.013(3) -0.006(2) 0.004(3) C11 0.047(3) 0.085(4) 0.045(3) 0.013(3) -0.006(2) -0.004(3) C12 0.057(4) 0.105(6) 0.043(3) 0.018(3) -0.002(3) -0.001(4) C13 0.074(5) 0.111(6) 0.059(4) 0.045(5) 0.004(3) 0.015(5) C14 0.070(4) 0.076(5) 0.078(5) 0.035(4) 0.007(3) 0.006(4) C15 0.047(3) 0.057(4) 0.074(4) 0.020(3) 0.006(3) 0.004(3) C16 0.057(4) 0.114(6) 0.051(3) 0.020(4) -0.010(3) -0.024(4) C17 0.093(6) 0.101(6) 0.089(5) 0.042(5) -0.030(4) -0.003(5) C18 0.086(5) 0.149(8) 0.038(3) -0.003(4) -0.012(3) -0.034(5) C19 0.076(5) 0.162(9) 0.058(4) 0.043(5) -0.011(3) -0.043(5) C20 0.041(3) 0.081(5) 0.089(5) 0.013(4) 0.001(3) 0.003(3) C21 0.073(6) 0.165(11) 0.165(10) -0.046(9) 0.013(6) 0.035(6) C22 0.047(4) 0.115(7) 0.132(7) 0.020(6) -0.010(4) -0.008(4) C23 0.045(4) 0.164(10) 0.138(8) 0.054(7) -0.005(4) 0.014(5) C24 0.075(4) 0.089(5) 0.035(3) 0.002(3) -0.013(3) -0.010(4) C25 0.070(5) 0.128(8) 0.089(5) -0.008(5) -0.006(4) -0.019(5) C26 0.091(5) 0.086(6) 0.066(4) -0.007(4) -0.010(4) -0.013(4) C27 0.076(5) 0.060(4) 0.096(5) 0.018(4) 0.000(4) -0.003(4) C28 0.124(8) 0.092(7) 0.186(11) -0.038(8) -0.008(8) 0.029(6) C29 0.101(7) 0.103(7) 0.150(9) 0.000(7) -0.023(6) -0.026(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr O 1.947(3) . ? Cr O 1.947(3) 6_556 ? Cr C1 2.065(12) 6_556 ? Cr C1 2.065(12) . ? Cr N 2.073(4) 6_556 ? Cr N 2.073(4) . ? O C3 1.310(6) . ? N C9 1.308(7) . ? N C10 1.463(7) . ? C1 C2 1.51(2) . ? C3 C8 1.407(7) . ? C3 C4 1.429(8) . ? C4 C5 1.362(8) . ? C4 C16 1.534(9) . ? C5 C6 1.404(8) . ? C6 C7 1.353(8) . ? C6 C20 1.535(8) . ? C7 C8 1.417(8) . ? C8 C9 1.416(7) . ? C10 C11 1.384(9) . ? C10 C15 1.387(9) . ? C11 C12 1.408(8) . ? C11 C24 1.510(10) . ? C12 C13 1.388(11) . ? C13 C14 1.346(11) . ? C14 C15 1.393(9) . ? C15 C27 1.522(10) . ? C16 C18 1.520(10) . ? C16 C19 1.536(9) . ? C16 C17 1.550(12) . ? C20 C23 1.505(11) . ? C20 C22 1.520(11) . ? C20 C21 1.532(12) . ? C24 C26 1.525(10) . ? C24 C25 1.536(10) . ? C27 C28 1.530(12) . ? C27 C29 1.534(11) . ? C31 C36 1.15(7) . ? C31 C32 1.48(5) . ? C32 C39 1.06(12) . ? C32 C36 1.32(7) . ? C32 C33 1.33(5) . ? C32 C35 1.42(8) . ? C32 C38 1.90(11) . ? C33 C36 1.29(8) . ? C33 C39 1.87(14) . ? C34 C35 1.74(8) . ? C34 C37 1.81(8) . ? C35 C39 0.81(12) . ? C35 C38 1.28(12) . ? C35 C37 1.69(9) . ? C38 C39 0.96(14) . ? 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 O Cr O 179.9(3) . 6_556 ? O Cr C1 86.0(4) . 6_556 ? O Cr C1 93.9(4) 6_556 6_556 ? O Cr C1 93.9(4) . . ? O Cr C1 86.0(4) 6_556 . ? C1 Cr C1 22.3(5) 6_556 . ? O Cr N 91.15(15) . 6_556 ? O Cr N 88.88(15) 6_556 6_556 ? C1 Cr N 95.8(3) 6_556 6_556 ? C1 Cr N 116.4(3) . 6_556 ? O Cr N 88.88(15) . . ? O Cr N 91.15(15) 6_556 . ? C1 Cr N 116.4(3) 6_556 . ? C1 Cr N 95.8(3) . . ? N Cr N 147.8(3) 6_556 . ? C3 O Cr 132.3(3) . . ? C9 N C10 112.6(4) . . ? C9 N Cr 122.2(4) . . ? C10 N Cr 125.0(3) . . ? C2 C1 Cr 108.0(8) . . ? O C3 C8 121.0(5) . . ? O C3 C4 122.1(5) . . ? C8 C3 C4 116.9(4) . . ? C5 C4 C3 117.7(5) . . ? C5 C4 C16 120.9(5) . . ? C3 C4 C16 121.4(5) . . ? C4 C5 C6 126.4(5) . . ? C7 C6 C5 115.5(5) . . ? C7 C6 C20 123.5(6) . . ? C5 C6 C20 120.9(5) . . ? C6 C7 C8 121.6(5) . . ? C3 C8 C9 123.0(5) . . ? C3 C8 C7 121.4(5) . . ? C9 C8 C7 115.6(5) . . ? N C9 C8 129.5(5) . . ? C11 C10 C15 121.9(5) . . ? C11 C10 N 118.6(5) . . ? C15 C10 N 119.4(5) . . ? C10 C11 C12 118.0(6) . . ? C10 C11 C24 124.0(5) . . ? C12 C11 C24 118.0(6) . . ? C13 C12 C11 119.9(7) . . ? C14 C13 C12 120.6(6) . . ? C13 C14 C15 121.4(7) . . ? C10 C15 C14 118.1(7) . . ? C10 C15 C27 121.4(6) . . ? C14 C15 C27 120.4(6) . . ? C18 C16 C4 110.4(6) . . ? C18 C16 C19 108.9(6) . . ? C4 C16 C19 111.6(5) . . ? C18 C16 C17 110.2(6) . . ? C4 C16 C17 109.0(6) . . ? C19 C16 C17 106.7(7) . . ? C23 C20 C22 109.1(7) . . ? C23 C20 C21 108.5(8) . . ? C22 C20 C21 108.1(7) . . ? C23 C20 C6 112.0(6) . . ? C22 C20 C6 109.0(6) . . ? C21 C20 C6 110.0(6) . . ? C11 C24 C26 112.7(6) . . ? C11 C24 C25 111.4(6) . . ? C26 C24 C25 110.0(6) . . ? C15 C27 C28 110.7(7) . . ? C15 C27 C29 112.8(7) . . ? C28 C27 C29 111.8(8) . . ? C36 C31 C32 58.8(39) . . ? C39 C32 C36 131.3(93) . . ? C39 C32 C33 102.5(83) . . ? C36 C32 C33 58.4(39) . . ? C39 C32 C35 34.5(72) . . ? C36 C32 C35 159.3(58) . . ? C33 C32 C35 128.9(53) . . ? C39 C32 C31 119.7(81) . . ? C36 C32 C31 48.2(36) . . ? C33 C32 C31 106.3(40) . . ? C35 C32 C31 118.7(44) . . ? C39 C32 C38 18.5(79) . . ? C36 C32 C38 119.0(50) . . ? C33 C32 C38 108.9(47) . . ? C35 C32 C38 42.2(44) . . ? C31 C32 C38 101.3(39) . . ? C36 C33 C32 60.5(40) . . ? C36 C33 C39 84.6(54) . . ? C32 C33 C39 33.6(40) . . ? C35 C34 C37 56.7(33) . . ? C39 C35 C38 48.4(100) . . ? C39 C35 C32 47.8(100) . . ? C38 C35 C32 89.5(73) . . ? C39 C35 C37 113.5(100) . . ? C38 C35 C37 137.9(72) . . ? C32 C35 C37 101.2(52) . . ? C39 C35 C34 108.4(100) . . ? C38 C35 C34 85.1(61) . . ? C32 C35 C34 146.6(57) . . ? C37 C35 C34 63.7(37) . . ? C31 C36 C33 133.8(70) . . ? C31 C36 C32 73.0(48) . . ? C33 C36 C32 61.2(41) . . ? C35 C37 C34 59.6(36) . . ? C39 C38 C35 39.3(89) . . ? C39 C38 C32 20.6(87) . . ? C35 C38 C32 48.3(55) . . ? C35 C39 C38 92.2(100) . . ? C35 C39 C32 97.7(100) . . ? C38 C39 C32 140.8(100) . . ? C35 C39 C33 130.9(100) . . ? C38 C39 C33 136.6(100) . . ? C32 C39 C33 43.9(61) . . ? _refine_diff_density_max 0.313 _refine_diff_density_min -0.347 _refine_diff_density_rms 0.056 data_VG9870 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C58 H82 N4 O2 Cl Cr' _chemical_formula_weight 954.73 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cr' 'Cr' 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 22.829(3) _cell_length_b 12.704(2) _cell_length_c 20.164(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.726(11) _cell_angle_gamma 90.00 _cell_volume 5847.4(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 20 _cell_measurement_theta_min 4.83 _cell_measurement_theta_max 12.48 _exptl_crystal_description prisms _exptl_crystal_colour 'Deep orange' _exptl_crystal_size_max 0.77 _exptl_crystal_size_mid 0.77 _exptl_crystal_size_min 0.38 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.084 _exptl_crystal_density_method ? _exptl_crystal_F_000 2060 _exptl_absorpt_coefficient_mu 0.282 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 26.89 _diffrn_reflns_number 10501 _diffrn_reflns_av_R_equivalents 0.0351 _diffrn_reflns_av_sigmaI/netI 0.0943 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10176 _reflns_number_observed 5565 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1513 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0739P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8663 _refine_ls_number_parameters 619 _refine_ls_number_restraints 108 _refine_ls_R_factor_all 0.1378 _refine_ls_R_factor_obs 0.0652 _refine_ls_wR_factor_all 0.1811 _refine_ls_wR_factor_obs 0.1413 _refine_ls_goodness_of_fit_all 1.005 _refine_ls_goodness_of_fit_obs 1.113 _refine_ls_restrained_S_all 1.050 _refine_ls_restrained_S_obs 1.138 _refine_ls_shift/esd_max 0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cr Cr 0.19871(3) 0.53024(5) 0.46100(3) 0.0367(2) Uani 1 d . . Cl Cl 0.10641(5) 0.46933(11) 0.43048(5) 0.0551(3) Uani 1 d . . O1 O 0.23785(14) 0.4263(2) 0.4087(2) 0.0537(8) Uani 1 d . . O2 O 0.27395(13) 0.5918(2) 0.48627(14) 0.0465(7) Uani 1 d . . N1 N 0.2004(2) 0.4292(3) 0.5436(2) 0.0439(8) Uani 1 d . . N2 N 0.19659(14) 0.6386(3) 0.3825(2) 0.0375(7) Uani 1 d . . C1 C 0.2697(2) 0.3452(4) 0.4266(3) 0.0543(12) Uani 1 d . . C2 C 0.3051(2) 0.2906(4) 0.3793(3) 0.0654(15) Uani 1 d . . C3 C 0.3370(3) 0.2052(5) 0.4018(4) 0.088(2) Uani 1 d . . H3A H 0.3594(3) 0.1697(5) 0.3708(4) 0.106 Uiso 1 calc R . C4 C 0.3389(3) 0.1671(6) 0.4665(4) 0.094(2) Uani 1 d . . C5 C 0.3036(3) 0.2183(5) 0.5116(3) 0.079(2) Uani 1 d . . H5A H 0.3022(3) 0.1945(5) 0.5552(3) 0.095 Uiso 1 calc R . C6 C 0.2697(2) 0.3064(4) 0.4921(3) 0.0608(13) Uani 1 d . . C7 C 0.2333(2) 0.3473(4) 0.5438(3) 0.0561(12) Uani 1 d . . H7A H 0.2337(2) 0.3088(4) 0.5831(3) 0.067 Uiso 1 calc R . C8 C 0.1631(2) 0.4365(4) 0.6020(2) 0.0485(11) Uani 1 d . . C9 C 0.1130(2) 0.3733(4) 0.6048(2) 0.0602(13) Uani 1 d . . C10 C 0.0772(3) 0.3843(6) 0.6604(3) 0.086(2) Uani 1 d . . H10A H 0.0434(3) 0.3440(6) 0.6632(3) 0.103 Uiso 1 calc R . C11 C 0.0907(3) 0.4522(6) 0.7103(3) 0.084(2) Uani 1 d . . H11A H 0.0658(3) 0.4589(6) 0.7461(3) 0.101 Uiso 1 calc R . C12 C 0.1409(3) 0.5109(5) 0.7078(2) 0.071(2) Uani 1 d . . H12A H 0.1501(3) 0.5561(5) 0.7427(2) 0.085 Uiso 1 calc R . C13 C 0.1785(2) 0.5042(4) 0.6540(2) 0.0546(12) Uani 1 d . . C14 C 0.3056(3) 0.3210(5) 0.3050(4) 0.089(2) Uani 1 d . . C15 C 0.2457(4) 0.2973(7) 0.2740(4) 0.108(3) Uani 1 d . . H15A H 0.2368(4) 0.2239(7) 0.2794(4) 0.161 Uiso 1 calc R . H15B H 0.2461(4) 0.3142(7) 0.2276(4) 0.161 Uiso 1 calc R . H15C H 0.2163(4) 0.3388(7) 0.2955(4) 0.161 Uiso 1 calc R . C16 C 0.3192(4) 0.4368(6) 0.2963(4) 0.126(3) Uani 1 d U . H16A H 0.3569(4) 0.4522(6) 0.3157(4) 0.189 Uiso 1 calc R . H16B H 0.2898(4) 0.4782(6) 0.3177(4) 0.189 Uiso 1 calc R . H16C H 0.3196(4) 0.4536(6) 0.2498(4) 0.189 Uiso 1 calc R . C17 C 0.3509(3) 0.2567(7) 0.2668(4) 0.118(3) Uani 1 d . . H17A H 0.3428(3) 0.1830(7) 0.2719(4) 0.177 Uiso 1 calc R . H17B H 0.3895(3) 0.2718(7) 0.2839(4) 0.177 Uiso 1 calc R . H17C H 0.3489(3) 0.2750(7) 0.2206(4) 0.177 Uiso 1 calc R . C18 C 0.3785(4) 0.0738(6) 0.4868(5) 0.127(3) Uani 1 d D . C19 C 0.4427(4) 0.1076(11) 0.4655(9) 0.151(6) Uani 0.70 d PDU 1 H19A H 0.4428(4) 0.1227(11) 0.4188(9) 0.226 Uiso 0.70 calc PR 1 H19B H 0.4696(4) 0.0512(11) 0.4749(9) 0.226 Uiso 0.70 calc PR 1 H19C H 0.4544(4) 0.1692(11) 0.4898(9) 0.226 Uiso 0.70 calc PR 1 C20 C 0.3632(6) -0.0219(8) 0.4454(7) 0.127(5) Uani 0.70 d PDU 1 H20A H 0.3629(6) -0.0032(8) 0.3993(7) 0.190 Uiso 0.70 calc PR 1 H20B H 0.3252(6) -0.0473(8) 0.4575(7) 0.190 Uiso 0.70 calc PR 1 H20C H 0.3918(6) -0.0761(8) 0.4533(7) 0.190 Uiso 0.70 calc PR 1 C21 C 0.3798(6) 0.0507(11) 0.5599(6) 0.132(5) Uani 0.70 d PDU 1 H21A H 0.3897(6) 0.1137(11) 0.5839(6) 0.198 Uiso 0.70 calc PR 1 H21B H 0.4086(6) -0.0026(11) 0.5692(6) 0.198 Uiso 0.70 calc PR 1 H21C H 0.3420(6) 0.0263(11) 0.5733(6) 0.198 Uiso 0.70 calc PR 1 C19' C 0.4312(15) 0.1099(39) 0.5258(21) 0.214(23) Uiso 0.30 d PD 2 H19D H 0.4188(15) 0.1517(39) 0.5627(21) 0.321 Uiso 0.30 calc PR 2 H19E H 0.4559(15) 0.1512(39) 0.4979(21) 0.321 Uiso 0.30 calc PR 2 H19F H 0.4525(15) 0.0497(39) 0.5419(21) 0.321 Uiso 0.30 calc PR 2 C20' C 0.3936(21) 0.0070(37) 0.4273(17) 0.214(29) Uiso 0.30 d PD 2 H20D H 0.3583(21) -0.0135(37) 0.4045(17) 0.321 Uiso 0.30 calc PR 2 H20E H 0.4144(21) -0.0547(37) 0.4419(17) 0.321 Uiso 0.30 calc PR 2 H20F H 0.4178(21) 0.0468(37) 0.3979(17) 0.321 Uiso 0.30 calc PR 2 C21' C 0.3395(18) 0.0044(33) 0.5334(19) 0.196(20) Uiso 0.30 d PD 2 H21D H 0.3055(18) -0.0193(33) 0.5092(19) 0.294 Uiso 0.30 calc PR 2 H21E H 0.3275(18) 0.0456(33) 0.5707(19) 0.294 Uiso 0.30 calc PR 2 H21F H 0.3616(18) -0.0553(33) 0.5486(19) 0.294 Uiso 0.30 calc PR 2 C22 C 0.0969(3) 0.2920(5) 0.5544(3) 0.078(2) Uani 1 d . . H22A H 0.1202(3) 0.3046(5) 0.5148(3) 0.093 Uiso 1 calc R . C23 C 0.1117(5) 0.1807(6) 0.5804(4) 0.127(3) Uani 1 d . . H23A H 0.1009(5) 0.1295(6) 0.5474(4) 0.191 Uiso 1 calc R . H23B H 0.0903(5) 0.1674(6) 0.6202(4) 0.191 Uiso 1 calc R . H23C H 0.1529(5) 0.1760(6) 0.5897(4) 0.191 Uiso 1 calc R . C24 C 0.0315(3) 0.2988(7) 0.5341(4) 0.109(3) Uani 1 d . . H24A H 0.0227(3) 0.2455(7) 0.5018(4) 0.164 Uiso 1 calc R . H24B H 0.0235(3) 0.3669(7) 0.5154(4) 0.164 Uiso 1 calc R . H24C H 0.0077(3) 0.2884(7) 0.5724(4) 0.164 Uiso 1 calc R . C25 C 0.2355(2) 0.5638(4) 0.6559(2) 0.0584(13) Uani 1 d . . H25A H 0.2516(2) 0.5642(4) 0.6111(2) 0.070 Uiso 1 calc R . C26 C 0.2281(3) 0.6774(5) 0.6781(3) 0.088(2) Uani 1 d . . H26A H 0.2655(3) 0.7120(5) 0.6785(3) 0.132 Uiso 1 calc R . H26B H 0.2121(3) 0.6788(5) 0.7219(3) 0.132 Uiso 1 calc R . H26C H 0.2020(3) 0.7132(5) 0.6480(3) 0.132 Uiso 1 calc R . C27 C 0.2788(3) 0.5073(6) 0.7015(3) 0.095(2) Uani 1 d . . H27A H 0.3152(3) 0.5452(6) 0.7028(3) 0.142 Uiso 1 calc R . H27B H 0.2854(3) 0.4374(6) 0.6852(3) 0.142 Uiso 1 calc R . H27C H 0.2631(3) 0.5035(6) 0.7454(3) 0.142 Uiso 1 calc R . C31 C 0.3158(2) 0.6238(4) 0.4462(2) 0.0463(10) Uani 1 d . . C32 C 0.3760(2) 0.6286(5) 0.4682(2) 0.0576(12) Uani 1 d . . C33 C 0.4172(2) 0.6562(5) 0.4222(3) 0.070(2) Uani 1 d . . H33A H 0.4563(2) 0.6548(5) 0.4359(3) 0.084 Uiso 1 calc R . C34 C 0.4057(2) 0.6861(5) 0.3573(3) 0.070(2) Uani 1 d . . C35 C 0.3480(2) 0.6904(4) 0.3386(3) 0.0593(13) Uani 1 d . . H35A H 0.3381(2) 0.7148(4) 0.2964(3) 0.071 Uiso 1 calc R . C36 C 0.3031(2) 0.6588(4) 0.3818(2) 0.0482(11) Uani 1 d . . C37 C 0.2444(2) 0.6734(4) 0.3575(2) 0.0455(10) Uani 1 d . . H37A H 0.2404(2) 0.7129(4) 0.3188(2) 0.055 Uiso 1 calc R . C38 C 0.1443(2) 0.6850(3) 0.3516(2) 0.0409(9) Uani 1 d . . C39 C 0.1263(2) 0.7836(4) 0.3741(2) 0.0489(11) Uani 1 d . . C40 C 0.0777(2) 0.8287(4) 0.3425(3) 0.0561(12) Uani 1 d . . H40A H 0.0640(2) 0.8935(4) 0.3571(3) 0.067 Uiso 1 calc R . C41 C 0.0498(2) 0.7804(4) 0.2906(3) 0.0599(13) Uani 1 d . . H41A H 0.0180(2) 0.8131(4) 0.2698(3) 0.072 Uiso 1 calc R . C42 C 0.0684(2) 0.6837(4) 0.2689(2) 0.0567(12) Uani 1 d . . H42A H 0.0488(2) 0.6512(4) 0.2338(2) 0.068 Uiso 1 calc R . C43 C 0.1165(2) 0.6329(4) 0.2988(2) 0.0456(10) Uani 1 d . . C44 C 0.3926(2) 0.6062(6) 0.5407(3) 0.076(2) Uani 1 d . . C45 C 0.3614(3) 0.6847(6) 0.5841(3) 0.088(2) Uani 1 d . . H45A H 0.3720(3) 0.7548(6) 0.5712(3) 0.132 Uiso 1 calc R . H45B H 0.3726(3) 0.6734(6) 0.6296(3) 0.132 Uiso 1 calc R . H45C H 0.3198(3) 0.6757(6) 0.5791(3) 0.132 Uiso 1 calc R . C46 C 0.3772(3) 0.4926(5) 0.5593(3) 0.082(2) Uani 1 d . . H46A H 0.3977(3) 0.4449(5) 0.5309(3) 0.124 Uiso 1 calc R . H46B H 0.3358(3) 0.4821(5) 0.5541(3) 0.124 Uiso 1 calc R . H46C H 0.3885(3) 0.4798(5) 0.6046(3) 0.124 Uiso 1 calc R . C47 C 0.4595(3) 0.6185(8) 0.5535(4) 0.114(3) Uani 1 d U . H47A H 0.4803(3) 0.5693(8) 0.5264(4) 0.171 Uiso 1 calc R . H47B H 0.4682(3) 0.6049(8) 0.5994(4) 0.171 Uiso 1 calc R . H47C H 0.4712(3) 0.6889(8) 0.5426(4) 0.171 Uiso 1 calc R . C48 C 0.4556(2) 0.7115(6) 0.3086(3) 0.093(2) Uani 1 d D . C49 C 0.4929(6) 0.6109(11) 0.2997(7) 0.127(5) Uani 0.60 d PDU 1 H49A H 0.5052(6) 0.5850(11) 0.3424(7) 0.190 Uiso 0.60 calc PR 1 H49B H 0.5267(6) 0.6270(11) 0.2738(7) 0.190 Uiso 0.60 calc PR 1 H49C H 0.4698(6) 0.5581(11) 0.2774(7) 0.190 Uiso 0.60 calc PR 1 C50 C 0.4984(6) 0.7894(12) 0.3432(7) 0.125(5) Uani 0.60 d PDU 1 H50A H 0.5112(6) 0.7606(12) 0.3850(7) 0.188 Uiso 0.60 calc PR 1 H50B H 0.4789(6) 0.8552(12) 0.3505(7) 0.188 Uiso 0.60 calc PR 1 H50C H 0.5318(6) 0.8007(12) 0.3155(7) 0.188 Uiso 0.60 calc PR 1 C51 C 0.4360(5) 0.7534(13) 0.2458(6) 0.115(4) Uani 0.60 d PDU 1 H51A H 0.4131(5) 0.8156(13) 0.2531(6) 0.173 Uiso 0.60 calc PR 1 H51B H 0.4125(5) 0.7018(13) 0.2230(6) 0.173 Uiso 0.60 calc PR 1 H51C H 0.4693(5) 0.7708(13) 0.2194(6) 0.173 Uiso 0.60 calc PR 1 C49' C 0.5139(8) 0.6765(18) 0.3309(11) 0.117(7) Uiso 0.40 d PD 2 H49D H 0.5126(8) 0.6029(18) 0.3415(11) 0.175 Uiso 0.40 calc PR 2 H49E H 0.5256(8) 0.7158(18) 0.3695(11) 0.175 Uiso 0.40 calc PR 2 H49F H 0.5415(8) 0.6881(18) 0.2962(11) 0.175 Uiso 0.40 calc PR 2 C50' C 0.4518(10) 0.8262(13) 0.2903(12) 0.127(8) Uiso 0.40 d PD 2 H50D H 0.4125(10) 0.8427(13) 0.2764(12) 0.190 Uiso 0.40 calc PR 2 H50E H 0.4783(10) 0.8406(13) 0.2548(12) 0.190 Uiso 0.40 calc PR 2 H50F H 0.4623(10) 0.8684(13) 0.3281(12) 0.190 Uiso 0.40 calc PR 2 C51' C 0.4416(9) 0.6517(16) 0.2412(9) 0.107(6) Uiso 0.40 d PD 2 H51D H 0.4036(9) 0.6725(16) 0.2249(9) 0.160 Uiso 0.40 calc PR 2 H51E H 0.4420(9) 0.5771(16) 0.2489(9) 0.160 Uiso 0.40 calc PR 2 H51F H 0.4707(9) 0.6693(16) 0.2091(9) 0.160 Uiso 0.40 calc PR 2 C52 C 0.1586(3) 0.8441(4) 0.4276(3) 0.0626(13) Uani 1 d . . H52A H 0.1837(3) 0.7943(4) 0.4518(3) 0.075 Uiso 1 calc R . C53 C 0.1985(3) 0.9287(5) 0.3969(3) 0.087(2) Uani 1 d . . H53A H 0.2186(3) 0.9663(5) 0.4317(3) 0.131 Uiso 1 calc R . H53B H 0.1751(3) 0.9769(5) 0.3712(3) 0.131 Uiso 1 calc R . H53C H 0.2266(3) 0.8954(5) 0.3688(3) 0.131 Uiso 1 calc R . C54 C 0.1175(4) 0.8952(5) 0.4775(3) 0.093(2) Uani 1 d . . H54A H 0.1402(4) 0.9325(5) 0.5103(3) 0.140 Uiso 1 calc R . H54B H 0.0947(4) 0.8417(5) 0.4988(3) 0.140 Uiso 1 calc R . H54C H 0.0918(4) 0.9435(5) 0.4549(3) 0.140 Uiso 1 calc R . C55 C 0.1378(2) 0.5295(4) 0.2713(2) 0.0538(11) Uani 1 d . . H55A H 0.1640(2) 0.4973(4) 0.3045(2) 0.065 Uiso 1 calc R . C56 C 0.0875(3) 0.4520(5) 0.2569(3) 0.073(2) Uani 1 d . . H56A H 0.1032(3) 0.3876(5) 0.2395(3) 0.109 Uiso 1 calc R . H56B H 0.0610(3) 0.4824(5) 0.2249(3) 0.109 Uiso 1 calc R . H56C H 0.0670(3) 0.4375(5) 0.2971(3) 0.109 Uiso 1 calc R . C57 C 0.1732(3) 0.5481(5) 0.2081(3) 0.0719(15) Uani 1 d . . H57A H 0.1865(3) 0.4818(5) 0.1911(3) 0.108 Uiso 1 calc R . H57B H 0.2063(3) 0.5920(5) 0.2182(3) 0.108 Uiso 1 calc R . H57C H 0.1488(3) 0.5821(5) 0.1754(3) 0.108 Uiso 1 calc R . N60 N 0.1519(2) 0.6338(3) 0.5209(2) 0.0512(9) Uani 1 d . . C61 C 0.1160(3) 0.6597(5) 0.5560(3) 0.0640(14) Uani 1 d . . C62 C 0.0705(3) 0.6872(7) 0.6025(3) 0.112(3) Uani 1 d . . H62A H 0.0383(3) 0.6392(7) 0.5975(3) 0.168 Uiso 1 d R . H62B H 0.0572(3) 0.7576(7) 0.5938(3) 0.168 Uiso 1 d R . H62C H 0.0858(3) 0.6830(7) 0.6470(3) 0.168 Uiso 1 d R . N70 N 0.0282(4) 0.3818(8) 0.8756(4) 0.134(3) Uani 1 d . . C71 C 0.0723(5) 0.3435(8) 0.8755(5) 0.109(3) Uani 1 d . . C72 C 0.1287(6) 0.2966(7) 0.8730(6) 0.153(5) Uani 1 d . . H72A H 0.1482(6) 0.3192(7) 0.8335(6) 0.230 Uiso 1 d R . H72B H 0.1248(6) 0.2213(7) 0.8725(6) 0.230 Uiso 1 d R . H72C H 0.1512(6) 0.3176(7) 0.9113(6) 0.230 Uiso 1 d 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 Cr 0.0409(3) 0.0347(3) 0.0346(3) -0.0011(3) 0.0044(2) 0.0061(3) Cl 0.0540(6) 0.0611(7) 0.0502(6) 0.0058(6) -0.0003(5) -0.0109(6) O1 0.066(2) 0.046(2) 0.050(2) -0.0048(14) 0.015(2) 0.018(2) O2 0.044(2) 0.056(2) 0.039(2) 0.0042(14) -0.0006(13) -0.0007(14) N1 0.050(2) 0.041(2) 0.041(2) 0.001(2) 0.004(2) 0.006(2) N2 0.041(2) 0.035(2) 0.036(2) 0.0012(14) 0.0000(14) 0.0009(14) C1 0.051(3) 0.041(2) 0.071(3) -0.010(2) 0.008(2) 0.008(2) C2 0.053(3) 0.061(3) 0.083(4) -0.022(3) 0.016(3) 0.009(3) C3 0.059(3) 0.078(4) 0.127(6) -0.044(4) 0.007(4) 0.026(3) C4 0.084(4) 0.075(4) 0.123(6) -0.025(4) -0.019(4) 0.041(4) C5 0.087(4) 0.057(3) 0.093(4) -0.008(3) -0.012(3) 0.034(3) C6 0.063(3) 0.046(3) 0.074(4) -0.007(2) -0.002(3) 0.017(2) C7 0.069(3) 0.044(3) 0.055(3) 0.003(2) 0.000(2) 0.013(2) C8 0.057(3) 0.049(3) 0.039(2) 0.012(2) 0.009(2) 0.007(2) C9 0.071(3) 0.066(3) 0.044(3) 0.011(2) 0.006(2) -0.012(3) C10 0.087(4) 0.112(5) 0.060(4) 0.007(4) 0.024(3) -0.030(4) C11 0.086(4) 0.115(5) 0.053(3) 0.008(4) 0.028(3) 0.002(4) C12 0.085(4) 0.087(4) 0.039(2) -0.003(3) 0.007(2) 0.006(3) C13 0.067(3) 0.061(3) 0.036(2) 0.006(2) 0.002(2) 0.012(2) C14 0.102(5) 0.075(4) 0.092(5) -0.032(4) 0.042(4) 0.007(4) C15 0.112(6) 0.115(6) 0.096(5) -0.019(5) 0.011(4) 0.030(5) C16 0.182(9) 0.092(6) 0.106(6) -0.014(5) 0.072(6) -0.008(5) C17 0.106(5) 0.137(7) 0.112(6) -0.058(5) 0.047(5) 0.015(5) C18 0.107(6) 0.094(5) 0.179(10) -0.035(6) -0.030(6) 0.062(5) C19 0.076(7) 0.156(11) 0.220(14) 0.036(11) -0.015(8) 0.054(7) C20 0.145(10) 0.061(6) 0.173(11) -0.010(7) -0.001(9) 0.052(7) C21 0.136(9) 0.106(9) 0.153(11) 0.028(8) -0.025(8) 0.063(8) C22 0.093(4) 0.078(4) 0.062(3) 0.015(3) 0.008(3) -0.027(3) C23 0.218(11) 0.064(4) 0.099(6) 0.016(4) -0.005(6) -0.045(5) C24 0.095(5) 0.155(8) 0.078(5) 0.003(5) 0.008(4) -0.054(5) C25 0.067(3) 0.066(3) 0.043(2) -0.004(2) -0.001(2) 0.006(2) C26 0.105(5) 0.078(4) 0.081(4) -0.031(4) 0.004(4) -0.010(4) C27 0.077(4) 0.128(7) 0.078(4) 0.021(4) -0.014(3) 0.006(4) C31 0.041(2) 0.049(3) 0.049(3) -0.001(2) -0.002(2) 0.001(2) C32 0.044(3) 0.078(3) 0.051(3) 0.008(3) -0.008(2) 0.001(2) C33 0.037(2) 0.103(5) 0.071(4) 0.012(3) -0.007(2) -0.006(3) C34 0.041(3) 0.103(4) 0.067(3) 0.019(3) 0.007(2) -0.007(3) C35 0.050(3) 0.076(3) 0.052(3) 0.016(3) 0.002(2) -0.005(2) C36 0.043(2) 0.053(3) 0.049(3) 0.001(2) -0.001(2) 0.001(2) C37 0.046(2) 0.050(2) 0.040(2) 0.009(2) -0.003(2) -0.004(2) C38 0.037(2) 0.045(2) 0.041(2) 0.009(2) 0.000(2) 0.001(2) C39 0.054(3) 0.046(2) 0.047(2) 0.010(2) 0.004(2) 0.004(2) C40 0.054(3) 0.049(3) 0.065(3) 0.017(2) 0.009(2) 0.011(2) C41 0.043(2) 0.074(3) 0.062(3) 0.024(3) 0.002(2) 0.007(2) C42 0.049(3) 0.072(3) 0.050(3) 0.011(2) -0.003(2) -0.008(2) C43 0.039(2) 0.056(3) 0.042(2) 0.007(2) 0.003(2) -0.005(2) C44 0.051(3) 0.118(5) 0.060(3) 0.013(3) -0.012(3) -0.011(3) C45 0.093(4) 0.111(5) 0.059(4) -0.001(4) -0.013(3) -0.030(4) C46 0.065(3) 0.108(5) 0.074(4) 0.029(4) -0.012(3) 0.010(3) C47 0.064(4) 0.192(9) 0.086(5) 0.037(5) -0.029(3) -0.031(5) C48 0.045(3) 0.148(7) 0.086(4) 0.045(5) 0.008(3) -0.005(4) C49 0.122(8) 0.138(9) 0.122(8) 0.009(7) 0.062(7) 0.019(7) C50 0.106(7) 0.151(9) 0.120(8) -0.002(7) 0.036(7) -0.054(7) C51 0.087(6) 0.162(9) 0.098(7) 0.039(7) 0.025(6) -0.014(7) C52 0.084(4) 0.040(2) 0.063(3) -0.001(2) -0.001(3) 0.011(2) C53 0.110(5) 0.060(3) 0.093(5) -0.002(3) -0.013(4) -0.017(3) C54 0.143(6) 0.064(4) 0.073(4) -0.009(3) -0.003(4) 0.026(4) C55 0.058(3) 0.059(3) 0.044(2) -0.002(2) -0.006(2) -0.007(2) C56 0.086(4) 0.067(4) 0.064(3) -0.007(3) -0.005(3) -0.021(3) C57 0.087(4) 0.072(4) 0.057(3) -0.006(3) 0.014(3) -0.003(3) N60 0.062(2) 0.047(2) 0.045(2) 0.000(2) 0.002(2) 0.015(2) C61 0.069(3) 0.075(4) 0.048(3) 0.004(3) 0.002(3) 0.031(3) C62 0.109(5) 0.161(8) 0.068(4) 0.007(4) 0.029(4) 0.077(5) N70 0.133(6) 0.155(8) 0.112(6) 0.040(5) -0.025(6) -0.075(7) C71 0.137(8) 0.102(7) 0.089(5) 0.013(5) -0.003(6) -0.061(7) C72 0.214(13) 0.072(5) 0.175(11) 0.017(6) 0.062(10) -0.013(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 Cr O1 1.917(3) . ? Cr O2 1.949(3) . ? Cr N60 2.089(4) . ? Cr N2 2.098(3) . ? Cr N1 2.102(4) . ? Cr Cl 2.3204(13) . ? O1 C1 1.310(6) . ? O2 C31 1.323(5) . ? N1 C7 1.283(6) . ? N1 C8 1.466(5) . ? N2 C37 1.287(5) . ? N2 C38 1.463(5) . ? C1 C6 1.409(8) . ? C1 C2 1.437(7) . ? C2 C3 1.381(9) . ? C2 C14 1.547(10) . ? C3 C4 1.391(11) . ? C4 C5 1.385(9) . ? C4 C18 1.543(9) . ? C5 C6 1.413(7) . ? C6 C7 1.438(7) . ? C8 C13 1.398(7) . ? C8 C9 1.398(7) . ? C9 C10 1.404(8) . ? C9 C22 1.491(8) . ? C10 C11 1.356(9) . ? C11 C12 1.369(9) . ? C12 C13 1.395(7) . ? C13 C25 1.505(7) . ? C14 C16 1.514(10) . ? C14 C15 1.528(11) . ? C14 C17 1.534(8) . ? C18 C19' 1.50(2) . ? C18 C21 1.502(13) . ? C18 C20' 1.51(2) . ? C18 C20 1.513(12) . ? C18 C21' 1.57(2) . ? C18 C19 1.591(13) . ? C22 C23 1.543(10) . ? C22 C24 1.544(10) . ? C25 C27 1.521(8) . ? C25 C26 1.521(8) . ? C31 C36 1.399(7) . ? C31 C32 1.440(6) . ? C32 C33 1.376(7) . ? C32 C44 1.533(7) . ? C33 C34 1.385(8) . ? C34 C35 1.367(7) . ? C34 C48 1.547(7) . ? C35 C36 1.412(7) . ? C36 C37 1.432(6) . ? C38 C39 1.395(6) . ? C38 C43 1.399(6) . ? C39 C40 1.397(7) . ? C39 C52 1.508(7) . ? C40 C41 1.364(8) . ? C41 C42 1.374(8) . ? C42 C43 1.402(7) . ? C43 C55 1.509(7) . ? C44 C45 1.511(10) . ? C44 C46 1.532(9) . ? C44 C47 1.552(8) . ? C48 C51 1.441(12) . ? C48 C49' 1.467(15) . ? C48 C50' 1.51(2) . ? C48 C49 1.547(12) . ? C48 C50 1.551(12) . ? C48 C51' 1.586(15) . ? C52 C54 1.529(8) . ? C52 C53 1.544(8) . ? C55 C57 1.537(7) . ? C55 C56 1.538(7) . ? N60 C61 1.138(6) . ? C61 C62 1.451(8) . ? N70 C71 1.117(13) . ? C71 C72 1.420(14) . ? 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 Cr O2 90.26(14) . . ? O1 Cr N60 175.4(2) . . ? O2 Cr N60 92.96(15) . . ? O1 Cr N2 92.48(13) . . ? O2 Cr N2 86.90(13) . . ? N60 Cr N2 90.91(14) . . ? O1 Cr N1 90.62(14) . . ? O2 Cr N1 91.76(14) . . ? N60 Cr N1 86.06(14) . . ? N2 Cr N1 176.62(14) . . ? O1 Cr Cl 93.01(11) . . ? O2 Cr Cl 175.83(10) . . ? N60 Cr Cl 83.92(12) . . ? N2 Cr Cl 90.37(10) . . ? N1 Cr Cl 90.79(11) . . ? C1 O1 Cr 130.7(3) . . ? C31 O2 Cr 127.1(3) . . ? C7 N1 C8 113.3(4) . . ? C7 N1 Cr 120.2(3) . . ? C8 N1 Cr 126.4(3) . . ? C37 N2 C38 112.8(3) . . ? C37 N2 Cr 120.6(3) . . ? C38 N2 Cr 126.6(2) . . ? O1 C1 C6 121.8(4) . . ? O1 C1 C2 120.8(5) . . ? C6 C1 C2 117.4(5) . . ? C3 C2 C1 117.3(6) . . ? C3 C2 C14 120.3(5) . . ? C1 C2 C14 122.3(5) . . ? C2 C3 C4 126.3(6) . . ? C5 C4 C3 116.1(6) . . ? C5 C4 C18 122.1(8) . . ? C3 C4 C18 121.8(7) . . ? C4 C5 C6 120.7(7) . . ? C1 C6 C5 122.1(5) . . ? C1 C6 C7 124.0(4) . . ? C5 C6 C7 113.8(5) . . ? N1 C7 C6 129.3(5) . . ? C13 C8 C9 121.5(4) . . ? C13 C8 N1 119.9(4) . . ? C9 C8 N1 118.6(4) . . ? C8 C9 C10 117.3(5) . . ? C8 C9 C22 124.5(5) . . ? C10 C9 C22 118.1(5) . . ? C11 C10 C9 121.8(6) . . ? C10 C11 C12 120.1(5) . . ? C11 C12 C13 121.3(5) . . ? C12 C13 C8 117.9(5) . . ? C12 C13 C25 119.4(5) . . ? C8 C13 C25 122.6(4) . . ? C16 C14 C15 109.2(8) . . ? C16 C14 C17 108.6(6) . . ? C15 C14 C17 107.2(6) . . ? C16 C14 C2 111.1(6) . . ? C15 C14 C2 109.2(6) . . ? C17 C14 C2 111.5(7) . . ? C19' C18 C20' 113.5(18) . . ? C21 C18 C20 112.7(10) . . ? C19' C18 C4 111.6(21) . . ? C21 C18 C4 114.5(7) . . ? C20' C18 C4 111.1(23) . . ? C20 C18 C4 109.9(7) . . ? C19' C18 C21' 108.3(17) . . ? C20' C18 C21' 107.2(16) . . ? C4 C18 C21' 104.7(19) . . ? C21 C18 C19 108.1(9) . . ? C20 C18 C19 106.0(9) . . ? C4 C18 C19 105.1(8) . . ? C9 C22 C23 110.6(5) . . ? C9 C22 C24 111.8(6) . . ? C23 C22 C24 110.4(6) . . ? C13 C25 C27 109.4(5) . . ? C13 C25 C26 112.7(5) . . ? C27 C25 C26 110.1(5) . . ? O2 C31 C36 121.5(4) . . ? O2 C31 C32 121.2(4) . . ? C36 C31 C32 117.3(4) . . ? C33 C32 C31 117.5(4) . . ? C33 C32 C44 121.8(4) . . ? C31 C32 C44 120.7(4) . . ? C32 C33 C34 125.7(5) . . ? C35 C34 C33 116.3(5) . . ? C35 C34 C48 122.1(5) . . ? C33 C34 C48 121.6(5) . . ? C34 C35 C36 121.6(5) . . ? C31 C36 C35 121.3(4) . . ? C31 C36 C37 122.7(4) . . ? C35 C36 C37 115.8(4) . . ? N2 C37 C36 128.0(4) . . ? C39 C38 C43 122.7(4) . . ? C39 C38 N2 117.6(4) . . ? C43 C38 N2 119.6(4) . . ? C38 C39 C40 117.0(4) . . ? C38 C39 C52 123.2(4) . . ? C40 C39 C52 119.7(4) . . ? C41 C40 C39 121.8(5) . . ? C40 C41 C42 120.2(5) . . ? C41 C42 C43 121.3(5) . . ? C38 C43 C42 117.0(4) . . ? C38 C43 C55 123.1(4) . . ? C42 C43 C55 119.8(4) . . ? C45 C44 C46 111.6(5) . . ? C45 C44 C32 108.5(5) . . ? C46 C44 C32 110.7(5) . . ? C45 C44 C47 107.9(6) . . ? C46 C44 C47 106.4(6) . . ? C32 C44 C47 111.8(5) . . ? C49' C48 C50' 114.6(12) . . ? C51 C48 C49 111.6(9) . . ? C51 C48 C34 114.3(6) . . ? C49' C48 C34 114.5(10) . . ? C50' C48 C34 108.5(11) . . ? C49 C48 C34 108.2(7) . . ? C51 C48 C50 110.3(9) . . ? C49 C48 C50 103.6(8) . . ? C34 C48 C50 108.2(7) . . ? C49' C48 C51' 106.8(11) . . ? C50' C48 C51' 104.1(10) . . ? C34 C48 C51' 107.6(9) . . ? C39 C52 C54 112.9(5) . . ? C39 C52 C53 110.7(5) . . ? C54 C52 C53 109.8(5) . . ? C43 C55 C57 110.3(4) . . ? C43 C55 C56 112.5(4) . . ? C57 C55 C56 109.9(4) . . ? C61 N60 Cr 156.8(5) . . ? N60 C61 C62 176.9(6) . . ? N70 C71 C72 177.8(11) . . ? _refine_diff_density_max 0.302 _refine_diff_density_min -0.323 _refine_diff_density_rms 0.050