# 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_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email ymu@jlu.edu.cn _publ_contact_author_name 'Ying Mu' loop_ _publ_author_name 'Mingtai Sun' 'Tieqi Xu' 'Wei Gao' 'Yang Liu' QiaolinWu 'Ying Mu' 'Ling Ye' data_complex_1 _database_code_depnum_ccdc_archive 'CCDC 756686' #TrackingRef '- combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H33 Cl Cr N O' _chemical_formula_weight 426.95 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 7.9630(16) _cell_length_b 8.3667(17) _cell_length_c 19.261(4) _cell_angle_alpha 84.11(3) _cell_angle_beta 86.97(3) _cell_angle_gamma 63.57(3) _cell_volume 1143.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5185 _cell_measurement_theta_min 3.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.241 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 454 _exptl_absorpt_coefficient_mu 0.629 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11336 _diffrn_reflns_av_R_equivalents 0.0693 _diffrn_reflns_av_sigmaI/netI 0.0930 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5185 _reflns_number_gt 3015 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0525P)^2^+0.6594P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.011(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5185 _refine_ls_number_parameters 254 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1208 _refine_ls_R_factor_gt 0.0629 _refine_ls_wR_factor_ref 0.1537 _refine_ls_wR_factor_gt 0.1265 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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 0.62743(8) 0.49450(8) 0.29057(3) 0.0370(2) Uani 1 1 d . . . Cl1 Cl 0.45076(14) 0.36834(15) 0.35163(5) 0.0547(3) Uani 1 1 d . . . O1 O 0.4473(3) 0.6332(3) 0.21888(12) 0.0444(6) Uani 1 1 d . . . N1 N 0.5277(4) 0.7168(4) 0.34498(14) 0.0414(7) Uani 1 1 d . . . C1 C 0.9297(5) 0.3513(5) 0.3268(2) 0.0425(9) Uani 1 1 d . . . C2 C 0.8838(5) 0.2237(5) 0.3017(2) 0.0459(9) Uani 1 1 d . . . C3 C 0.8361(5) 0.2773(5) 0.2302(2) 0.0482(10) Uani 1 1 d . . . C4 C 0.8581(5) 0.4348(6) 0.21132(19) 0.0455(9) Uani 1 1 d . . . C5 C 0.9131(5) 0.4837(5) 0.2715(2) 0.0424(9) Uani 1 1 d . . . C6 C 1.0030(5) 0.3388(6) 0.3983(2) 0.0598(12) Uani 1 1 d . . . H6A H 0.9448 0.2851 0.4315 0.090 Uiso 1 1 calc R . . H6B H 0.9748 0.4566 0.4104 0.090 Uiso 1 1 calc R . . H6C H 1.1364 0.2665 0.3987 0.090 Uiso 1 1 calc R . . C7 C 0.8925(6) 0.0580(5) 0.3409(3) 0.0691(13) Uani 1 1 d . . . H7A H 1.0106 -0.0412 0.3318 0.104 Uiso 1 1 calc R . . H7B H 0.7923 0.0353 0.3262 0.104 Uiso 1 1 calc R . . H7C H 0.8801 0.0727 0.3900 0.104 Uiso 1 1 calc R . . C8 C 0.7838(7) 0.1768(7) 0.1822(3) 0.0792(15) Uani 1 1 d . . . H8A H 0.6877 0.2603 0.1510 0.119 Uiso 1 1 calc R . . H8B H 0.7380 0.1011 0.2092 0.119 Uiso 1 1 calc R . . H8C H 0.8921 0.1045 0.1558 0.119 Uiso 1 1 calc R . . C9 C 0.8310(6) 0.5313(8) 0.1398(2) 0.0723(14) Uani 1 1 d . . . H9A H 0.7727 0.6582 0.1435 0.108 Uiso 1 1 calc R . . H9B H 0.7523 0.5009 0.1133 0.108 Uiso 1 1 calc R . . H9C H 0.9505 0.4966 0.1168 0.108 Uiso 1 1 calc R . . C10 C 0.9616(6) 0.6353(6) 0.2735(3) 0.0650(12) Uani 1 1 d . . . H10A H 1.0900 0.5983 0.2593 0.097 Uiso 1 1 calc R . . H10B H 0.9448 0.6710 0.3202 0.097 Uiso 1 1 calc R . . H10C H 0.8814 0.7345 0.2425 0.097 Uiso 1 1 calc R . . C11 C 0.4014(5) 0.8012(5) 0.19684(18) 0.0396(8) Uani 1 1 d . . . C12 C 0.3462(5) 0.8635(6) 0.12651(19) 0.0469(10) Uani 1 1 d . . . C13 C 0.3000(6) 1.0398(6) 0.1045(2) 0.0567(11) Uani 1 1 d . . . H13 H 0.2650 1.0796 0.0582 0.068 Uiso 1 1 calc R . . C14 C 0.3029(6) 1.1603(6) 0.1475(2) 0.0588(11) Uani 1 1 d . . . H14 H 0.2721 1.2780 0.1305 0.071 Uiso 1 1 calc R . . C15 C 0.3523(5) 1.1030(6) 0.2160(2) 0.0534(10) Uani 1 1 d . . . H15 H 0.3506 1.1838 0.2462 0.064 Uiso 1 1 calc R . . C16 C 0.4051(5) 0.9245(5) 0.24099(19) 0.0435(9) Uani 1 1 d . . . C17 C 0.4498(5) 0.8761(5) 0.31437(18) 0.0433(9) Uani 1 1 d . . . H17 H 0.4190 0.9699 0.3422 0.052 Uiso 1 1 calc R . . C18 C 0.3391(6) 0.7364(6) 0.07797(19) 0.0586(11) Uani 1 1 d . . . H18 H 0.4187 0.6145 0.0980 0.070 Uiso 1 1 calc R . . C19 C 0.4164(9) 0.7575(9) 0.0054(2) 0.0975(19) Uani 1 1 d . . . H19A H 0.3343 0.8712 -0.0178 0.146 Uiso 1 1 calc R . . H19B H 0.4248 0.6631 -0.0212 0.146 Uiso 1 1 calc R . . H19C H 0.5388 0.7514 0.0093 0.146 Uiso 1 1 calc R . . C20 C 0.1429(9) 0.7533(10) 0.0736(3) 0.108(2) Uani 1 1 d . . . H20A H 0.1006 0.7296 0.1194 0.163 Uiso 1 1 calc R . . H20B H 0.1432 0.6685 0.0436 0.163 Uiso 1 1 calc R . . H20C H 0.0602 0.8724 0.0552 0.163 Uiso 1 1 calc R . . C21 C 0.5419(5) 0.6984(6) 0.42223(18) 0.0486(10) Uani 1 1 d . . . H21 H 0.6140 0.5705 0.4366 0.058 Uiso 1 1 calc R . . C22 C 0.6469(7) 0.7942(7) 0.4481(2) 0.0723(14) Uani 1 1 d . . . H22A H 0.7668 0.7550 0.4252 0.109 Uiso 1 1 calc R . . H22B H 0.6645 0.7668 0.4976 0.109 Uiso 1 1 calc R . . H22C H 0.5756 0.9212 0.4379 0.109 Uiso 1 1 calc R . . C23 C 0.3483(6) 0.7576(7) 0.4554(2) 0.0712(14) Uani 1 1 d . . . H23A H 0.2748 0.8838 0.4438 0.107 Uiso 1 1 calc R . . H23B H 0.3602 0.7336 0.5051 0.107 Uiso 1 1 calc R . . H23C H 0.2877 0.6930 0.4381 0.107 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 0.0387(3) 0.0387(4) 0.0345(3) -0.0054(2) -0.0018(2) -0.0174(3) Cl1 0.0546(6) 0.0671(7) 0.0505(6) 0.0011(5) 0.0010(5) -0.0357(5) O1 0.0530(15) 0.0429(16) 0.0358(13) -0.0014(12) -0.0086(11) -0.0194(12) N1 0.0441(17) 0.047(2) 0.0327(15) -0.0075(14) -0.0025(13) -0.0191(15) C1 0.0330(19) 0.044(2) 0.049(2) -0.0006(18) -0.0058(16) -0.0151(16) C2 0.041(2) 0.033(2) 0.063(3) -0.0064(18) -0.0001(18) -0.0144(17) C3 0.042(2) 0.049(2) 0.057(2) -0.022(2) 0.0058(18) -0.0204(18) C4 0.039(2) 0.054(2) 0.045(2) -0.0063(18) 0.0073(16) -0.0214(18) C5 0.0358(19) 0.040(2) 0.056(2) -0.0090(18) 0.0030(16) -0.0201(16) C6 0.043(2) 0.069(3) 0.061(3) -0.005(2) -0.0098(19) -0.018(2) C7 0.067(3) 0.033(2) 0.099(4) 0.003(2) -0.009(3) -0.015(2) C8 0.076(3) 0.088(4) 0.088(4) -0.046(3) 0.007(3) -0.042(3) C9 0.057(3) 0.105(4) 0.048(3) 0.005(3) 0.004(2) -0.033(3) C10 0.064(3) 0.056(3) 0.086(3) -0.010(3) 0.006(2) -0.037(2) C11 0.0356(19) 0.044(2) 0.0364(19) -0.0044(17) 0.0003(15) -0.0153(16) C12 0.045(2) 0.058(3) 0.038(2) 0.0000(19) -0.0011(16) -0.0236(19) C13 0.058(3) 0.062(3) 0.044(2) 0.010(2) -0.0096(19) -0.023(2) C14 0.061(3) 0.048(3) 0.060(3) 0.010(2) -0.001(2) -0.020(2) C15 0.056(2) 0.046(2) 0.057(3) -0.007(2) 0.002(2) -0.021(2) C16 0.039(2) 0.043(2) 0.043(2) -0.0066(18) 0.0012(16) -0.0130(17) C17 0.046(2) 0.044(2) 0.038(2) -0.0102(18) -0.0006(16) -0.0172(18) C18 0.075(3) 0.069(3) 0.034(2) -0.002(2) -0.0084(19) -0.034(2) C19 0.143(5) 0.120(5) 0.046(3) -0.019(3) 0.015(3) -0.073(4) C20 0.117(5) 0.154(6) 0.098(4) -0.041(4) 0.004(4) -0.094(5) C21 0.055(2) 0.051(2) 0.0321(19) -0.0095(17) -0.0049(16) -0.0152(19) C22 0.090(3) 0.077(3) 0.051(3) -0.018(2) -0.016(2) -0.033(3) C23 0.067(3) 0.091(4) 0.040(2) -0.007(2) 0.008(2) -0.022(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 O1 1.926(3) . ? Cr1 N1 2.046(3) . ? Cr1 C3 2.227(4) . ? Cr1 C4 2.236(3) . ? Cr1 C5 2.248(3) . ? Cr1 C1 2.270(4) . ? Cr1 C2 2.275(4) . ? Cr1 Cl1 2.3172(13) . ? O1 C11 1.313(4) . ? N1 C17 1.284(5) . ? N1 C21 1.485(4) . ? C1 C2 1.407(5) . ? C1 C5 1.423(5) . ? C1 C6 1.498(5) . ? C2 C3 1.422(5) . ? C2 C7 1.483(6) . ? C3 C4 1.415(5) . ? C3 C8 1.498(6) . ? C4 C5 1.418(5) . ? C4 C9 1.498(6) . ? C5 C10 1.486(5) . ? C11 C16 1.414(5) . ? C11 C12 1.419(5) . ? C12 C13 1.377(6) . ? C12 C18 1.507(6) . ? C13 C14 1.378(6) . ? C14 C15 1.372(6) . ? C15 C16 1.398(5) . ? C16 C17 1.448(5) . ? C18 C20 1.511(7) . ? C18 C19 1.523(6) . ? C21 C23 1.520(6) . ? C21 C22 1.521(6) . ? 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 88.66(12) . . ? O1 Cr1 C3 100.49(13) . . ? N1 Cr1 C3 156.49(14) . . ? O1 Cr1 C4 89.58(13) . . ? N1 Cr1 C4 122.67(14) . . ? C3 Cr1 C4 36.96(14) . . ? O1 Cr1 C5 114.50(13) . . ? N1 Cr1 C5 94.77(13) . . ? C3 Cr1 C5 61.72(14) . . ? C4 Cr1 C5 36.87(13) . . ? O1 Cr1 C1 149.67(13) . . ? N1 Cr1 C1 100.94(13) . . ? C3 Cr1 C1 60.94(14) . . ? C4 Cr1 C1 60.95(14) . . ? C5 Cr1 C1 36.70(13) . . ? O1 Cr1 C2 136.38(13) . . ? N1 Cr1 C2 133.72(14) . . ? C3 Cr1 C2 36.82(14) . . ? C4 Cr1 C2 61.25(15) . . ? C5 Cr1 C2 61.23(14) . . ? C1 Cr1 C2 36.07(14) . . ? O1 Cr1 Cl1 97.47(9) . . ? N1 Cr1 Cl1 95.10(9) . . ? C3 Cr1 Cl1 104.98(12) . . ? C4 Cr1 Cl1 141.80(12) . . ? C5 Cr1 Cl1 146.68(11) . . ? C1 Cr1 Cl1 110.06(11) . . ? C2 Cr1 Cl1 89.49(11) . . ? C11 O1 Cr1 125.4(2) . . ? C17 N1 C21 117.5(3) . . ? C17 N1 Cr1 121.9(2) . . ? C21 N1 Cr1 120.5(2) . . ? C2 C1 C5 109.0(3) . . ? C2 C1 C6 125.1(4) . . ? C5 C1 C6 125.6(4) . . ? C2 C1 Cr1 72.1(2) . . ? C5 C1 Cr1 70.8(2) . . ? C6 C1 Cr1 127.9(3) . . ? C1 C2 C3 107.4(3) . . ? C1 C2 C7 126.9(4) . . ? C3 C2 C7 125.6(4) . . ? C1 C2 Cr1 71.8(2) . . ? C3 C2 Cr1 69.7(2) . . ? C7 C2 Cr1 126.1(3) . . ? C4 C3 C2 108.2(3) . . ? C4 C3 C8 126.2(4) . . ? C2 C3 C8 125.5(4) . . ? C4 C3 Cr1 71.9(2) . . ? C2 C3 Cr1 73.4(2) . . ? C8 C3 Cr1 123.5(3) . . ? C3 C4 C5 108.3(3) . . ? C3 C4 C9 125.7(4) . . ? C5 C4 C9 126.0(4) . . ? C3 C4 Cr1 71.2(2) . . ? C5 C4 Cr1 72.04(19) . . ? C9 C4 Cr1 123.3(3) . . ? C4 C5 C1 107.1(3) . . ? C4 C5 C10 125.7(4) . . ? C1 C5 C10 126.9(4) . . ? C4 C5 Cr1 71.1(2) . . ? C1 C5 Cr1 72.5(2) . . ? C10 C5 Cr1 126.1(3) . . ? O1 C11 C16 122.2(3) . . ? O1 C11 C12 119.8(3) . . ? C16 C11 C12 118.0(4) . . ? C13 C12 C11 118.8(4) . . ? C13 C12 C18 121.7(4) . . ? C11 C12 C18 119.5(4) . . ? C12 C13 C14 123.3(4) . . ? C15 C14 C13 118.7(4) . . ? C14 C15 C16 120.6(4) . . ? C15 C16 C11 120.6(4) . . ? C15 C16 C17 117.2(4) . . ? C11 C16 C17 122.0(4) . . ? N1 C17 C16 126.7(3) . . ? C12 C18 C20 111.2(4) . . ? C12 C18 C19 113.0(4) . . ? C20 C18 C19 110.7(4) . . ? N1 C21 C23 110.2(3) . . ? N1 C21 C22 112.9(3) . . ? C23 C21 C22 112.2(4) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.405 _refine_diff_density_min -0.587 _refine_diff_density_rms 0.073 #===END data_complex_2 _database_code_depnum_ccdc_archive 'CCDC 756687' #TrackingRef '- combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H35 Cl Cr N O' _chemical_formula_weight 440.98 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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.4593(19) _cell_length_b 12.206(2) _cell_length_c 21.386(4) _cell_angle_alpha 90.00 _cell_angle_beta 102.19(3) _cell_angle_gamma 90.00 _cell_volume 2413.6(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5494 _cell_measurement_theta_min 3.08 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.214 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 940 _exptl_absorpt_coefficient_mu 0.598 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9317 _exptl_absorpt_correction_T_max 0.9371 _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 'Rigaku R-AXIS RAPID IP diffractometer' _diffrn_measurement_method 'Oscillation scans' _diffrn_detector_area_resol_mean '100x100 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21508 _diffrn_reflns_av_R_equivalents 0.1268 _diffrn_reflns_av_sigmaI/netI 0.1662 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5494 _reflns_number_gt 3033 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAPID AUTO' _computing_cell_refinement 'RAPID AUTO' _computing_data_reduction 'RAPID AUTO' _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^)+(0.1197P)^2^+0.8577P] 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 5494 _refine_ls_number_parameters 263 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1406 _refine_ls_R_factor_gt 0.0925 _refine_ls_wR_factor_ref 0.2666 _refine_ls_wR_factor_gt 0.2336 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3422(6) 0.6002(4) 0.1580(2) 0.0691(14) Uani 1 1 d . . . C2 C 0.2720(7) 0.6845(5) 0.1860(2) 0.0749(16) Uani 1 1 d . . . C3 C 0.2194(6) 0.7632(4) 0.1378(3) 0.0675(14) Uani 1 1 d . . . C4 C 0.2614(5) 0.7283(4) 0.0814(2) 0.0550(11) Uani 1 1 d . . . C5 C 0.3346(5) 0.6287(4) 0.0935(2) 0.0569(12) Uani 1 1 d . . . C6 C 0.4034(9) 0.4958(5) 0.1899(3) 0.111(3) Uani 1 1 d . . . H6A H 0.3421 0.4355 0.1727 0.166 Uiso 1 1 calc R . . H6B H 0.4086 0.5010 0.2351 0.166 Uiso 1 1 calc R . . H6C H 0.4986 0.4841 0.1821 0.166 Uiso 1 1 calc R . . C7 C 0.2411(9) 0.6875(8) 0.2530(3) 0.122(3) Uani 1 1 d . . . H7A H 0.2556 0.7606 0.2698 0.183 Uiso 1 1 calc R . . H7B H 0.3053 0.6382 0.2802 0.183 Uiso 1 1 calc R . . H7C H 0.1428 0.6657 0.2513 0.183 Uiso 1 1 calc R . . C8 C 0.1286(7) 0.8604(6) 0.1456(3) 0.103(2) Uani 1 1 d . . . H8A H 0.1538 0.9207 0.1214 0.154 Uiso 1 1 calc R . . H8B H 0.1452 0.8802 0.1900 0.154 Uiso 1 1 calc R . . H8C H 0.0283 0.8425 0.1306 0.154 Uiso 1 1 calc R . . C9 C 0.2218(6) 0.7850(5) 0.0171(3) 0.0806(17) Uani 1 1 d . . . H9A H 0.2989 0.8331 0.0121 0.121 Uiso 1 1 calc R . . H9B H 0.1348 0.8266 0.0149 0.121 Uiso 1 1 calc R . . H9C H 0.2066 0.7311 -0.0163 0.121 Uiso 1 1 calc R . . C10 C 0.3914(7) 0.5611(5) 0.0454(3) 0.0799(17) Uani 1 1 d . . . H10A H 0.3213 0.5064 0.0278 0.120 Uiso 1 1 calc R . . H10B H 0.4798 0.5260 0.0661 0.120 Uiso 1 1 calc R . . H10C H 0.4094 0.6076 0.0118 0.120 Uiso 1 1 calc R . . C11 C 0.7083(6) 0.7147(4) 0.0922(2) 0.0559(12) Uani 1 1 d . . . C12 C 0.7765(5) 0.6455(4) 0.1432(2) 0.0561(11) Uani 1 1 d . . . C13 C 0.8928(6) 0.5771(5) 0.1356(3) 0.0733(15) Uani 1 1 d . . . H13 H 0.9361 0.5316 0.1691 0.088 Uiso 1 1 calc R . . C14 C 0.9426(6) 0.5766(5) 0.0800(3) 0.0789(16) Uani 1 1 d . . . H14 H 1.0148 0.5284 0.0741 0.095 Uiso 1 1 calc R . . C15 C 0.8815(6) 0.6510(5) 0.0324(3) 0.0714(14) Uani 1 1 d . . . H15 H 0.9189 0.6536 -0.0045 0.086 Uiso 1 1 calc R . . C16 C 0.7684(6) 0.7215(4) 0.0363(2) 0.0588(12) Uani 1 1 d . . . C17 C 0.7450(6) 0.6509(4) 0.2053(2) 0.0672(14) Uani 1 1 d . . . H17 H 0.8084 0.6142 0.2377 0.081 Uiso 1 1 calc R . . C18 C 0.7128(6) 0.8073(5) -0.0160(2) 0.0669(14) Uani 1 1 d . . . C19 C 0.5579(6) 0.7842(6) -0.0491(3) 0.0842(18) Uani 1 1 d . . . H19A H 0.4967 0.7898 -0.0188 0.126 Uiso 1 1 calc R . . H19B H 0.5512 0.7117 -0.0669 0.126 Uiso 1 1 calc R . . H19C H 0.5276 0.8366 -0.0828 0.126 Uiso 1 1 calc R . . C20 C 0.7245(9) 0.9212(5) 0.0125(3) 0.116(3) Uani 1 1 d . . . H20A H 0.6882 0.9736 -0.0205 0.175 Uiso 1 1 calc R . . H20B H 0.8239 0.9371 0.0309 0.175 Uiso 1 1 calc R . . H20C H 0.6686 0.9250 0.0450 0.175 Uiso 1 1 calc R . . C21 C 0.8021(8) 0.8076(8) -0.0685(3) 0.116(3) Uani 1 1 d . . . H21A H 0.7619 0.8599 -0.1010 0.175 Uiso 1 1 calc R . . H21B H 0.7998 0.7360 -0.0872 0.175 Uiso 1 1 calc R . . H21C H 0.9004 0.8272 -0.0501 0.175 Uiso 1 1 calc R . . C22 C 0.6426(8) 0.7187(6) 0.2914(2) 0.0874(19) Uani 1 1 d . . . H22 H 0.5480 0.7472 0.2953 0.105 Uiso 1 1 calc R . . C23 C 0.7544(9) 0.8074(6) 0.3152(3) 0.115(3) Uani 1 1 d . . . H23A H 0.8492 0.7802 0.3142 0.172 Uiso 1 1 calc R . . H23B H 0.7504 0.8272 0.3582 0.172 Uiso 1 1 calc R . . H23C H 0.7341 0.8706 0.2881 0.172 Uiso 1 1 calc R . . C24 C 0.6695(9) 0.6130(7) 0.3306(3) 0.112(3) Uani 1 1 d . . . H24A H 0.5996 0.5589 0.3121 0.168 Uiso 1 1 calc R . . H24B H 0.6609 0.6275 0.3738 0.168 Uiso 1 1 calc R . . H24C H 0.7650 0.5864 0.3306 0.168 Uiso 1 1 calc R . . Cl Cl 0.47620(17) 0.93769(11) 0.18983(7) 0.0784(5) Uani 1 1 d . . . Cr Cr 0.46545(8) 0.75723(6) 0.15476(3) 0.0509(3) Uani 1 1 d . . . N N 0.6381(5) 0.7010(4) 0.22156(17) 0.0635(11) Uani 1 1 d . . . O O 0.5940(4) 0.7732(3) 0.09668(15) 0.0581(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.090(4) 0.057(3) 0.058(3) 0.001(2) 0.013(3) -0.021(3) C2 0.089(4) 0.091(4) 0.049(3) -0.012(3) 0.024(3) -0.027(3) C3 0.057(3) 0.071(4) 0.074(3) -0.018(3) 0.013(2) -0.008(3) C4 0.051(3) 0.058(3) 0.053(3) -0.0038(19) 0.005(2) -0.013(2) C5 0.068(3) 0.052(3) 0.049(2) -0.0074(19) 0.009(2) -0.012(2) C6 0.167(7) 0.063(4) 0.091(5) 0.020(3) 0.004(4) -0.025(4) C7 0.143(7) 0.170(8) 0.064(4) -0.025(4) 0.046(4) -0.048(6) C8 0.077(4) 0.098(5) 0.134(6) -0.039(4) 0.026(4) 0.011(4) C9 0.069(4) 0.095(4) 0.068(3) 0.016(3) -0.007(3) -0.003(3) C10 0.091(4) 0.068(4) 0.083(4) -0.028(3) 0.025(3) -0.014(3) C11 0.061(3) 0.047(2) 0.053(3) 0.0004(19) 0.000(2) -0.008(2) C12 0.049(3) 0.055(3) 0.060(3) 0.003(2) 0.002(2) -0.004(2) C13 0.064(3) 0.063(3) 0.086(4) 0.003(3) -0.001(3) 0.005(3) C14 0.065(4) 0.079(4) 0.093(4) -0.007(3) 0.017(3) -0.004(3) C15 0.067(4) 0.081(4) 0.069(3) -0.007(3) 0.021(3) -0.008(3) C16 0.057(3) 0.065(3) 0.052(3) 0.000(2) 0.006(2) -0.009(2) C17 0.067(3) 0.067(3) 0.061(3) 0.013(2) -0.003(2) 0.008(3) C18 0.066(3) 0.078(4) 0.054(3) 0.008(2) 0.006(2) -0.017(3) C19 0.067(4) 0.109(5) 0.069(4) 0.010(3) -0.004(3) -0.014(3) C20 0.189(9) 0.070(4) 0.081(4) 0.020(3) 0.008(5) -0.030(5) C21 0.094(5) 0.174(8) 0.089(5) 0.042(5) 0.038(4) 0.008(5) C22 0.105(5) 0.112(5) 0.038(3) 0.002(3) -0.003(3) 0.020(4) C23 0.153(7) 0.109(5) 0.063(4) -0.019(4) -0.019(4) 0.012(5) C24 0.148(7) 0.132(6) 0.052(3) 0.024(4) 0.012(4) 0.007(5) Cl 0.0892(11) 0.0555(8) 0.0810(9) -0.0172(6) -0.0038(7) -0.0041(7) Cr 0.0604(5) 0.0489(5) 0.0399(4) -0.0029(3) 0.0029(3) -0.0027(3) N 0.075(3) 0.065(3) 0.043(2) 0.0027(17) -0.0018(18) 0.003(2) O 0.057(2) 0.062(2) 0.0528(19) 0.0089(14) 0.0074(14) 0.0063(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C5 1.410(6) . ? C1 C2 1.424(8) . ? C1 C6 1.502(8) . ? C1 Cr 2.253(5) . ? C2 C3 1.420(8) . ? C2 C7 1.523(7) . ? C2 Cr 2.258(5) . ? C3 C4 1.413(7) . ? C3 C8 1.495(8) . ? C3 Cr 2.279(5) . ? C4 C5 1.396(7) . ? C4 C9 1.513(7) . ? C4 Cr 2.243(5) . ? C5 C10 1.503(7) . ? C5 Cr 2.241(4) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 O 1.316(6) . ? C11 C12 1.422(6) . ? C11 C16 1.430(7) . ? C12 C13 1.418(7) . ? C12 C17 1.422(7) . ? C13 C14 1.370(8) . ? C13 H13 0.9300 . ? C14 C15 1.396(8) . ? C14 H14 0.9300 . ? C15 C16 1.388(7) . ? C15 H15 0.9300 . ? C16 C18 1.543(7) . ? C17 N 1.291(7) . ? C17 H17 0.9300 . ? C18 C20 1.512(8) . ? C18 C19 1.513(7) . ? C18 C21 1.541(8) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 N 1.501(6) . ? C22 C23 1.523(10) . ? C22 C24 1.530(9) . ? C22 H22 0.9800 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? Cl Cr 2.3222(15) . ? Cr O 1.923(3) . ? Cr N 2.048(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 C1 C2 107.4(5) . . ? C5 C1 C6 126.0(5) . . ? C2 C1 C6 126.4(5) . . ? C5 C1 Cr 71.3(3) . . ? C2 C1 Cr 71.8(3) . . ? C6 C1 Cr 125.7(4) . . ? C3 C2 C1 107.9(4) . . ? C3 C2 C7 124.1(6) . . ? C1 C2 C7 127.7(6) . . ? C3 C2 Cr 72.6(3) . . ? C1 C2 Cr 71.4(3) . . ? C7 C2 Cr 126.7(4) . . ? C4 C3 C2 107.3(5) . . ? C4 C3 C8 127.4(6) . . ? C2 C3 C8 125.2(6) . . ? C4 C3 Cr 70.4(3) . . ? C2 C3 Cr 70.9(3) . . ? C8 C3 Cr 126.8(4) . . ? C5 C4 C3 108.8(4) . . ? C5 C4 C9 125.8(5) . . ? C3 C4 C9 125.2(5) . . ? C5 C4 Cr 71.8(3) . . ? C3 C4 Cr 73.2(3) . . ? C9 C4 Cr 125.1(3) . . ? C4 C5 C1 108.5(4) . . ? C4 C5 C10 125.9(4) . . ? C1 C5 C10 125.6(5) . . ? C4 C5 Cr 71.9(3) . . ? C1 C5 Cr 72.2(3) . . ? C10 C5 Cr 123.4(4) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O C11 C12 120.9(4) . . ? O C11 C16 120.4(4) . . ? C12 C11 C16 118.7(5) . . ? C13 C12 C11 119.9(5) . . ? C13 C12 C17 117.0(4) . . ? C11 C12 C17 122.6(5) . . ? C14 C13 C12 121.3(5) . . ? C14 C13 H13 119.3 . . ? C12 C13 H13 119.3 . . ? C13 C14 C15 117.8(5) . . ? C13 C14 H14 121.1 . . ? C15 C14 H14 121.1 . . ? C16 C15 C14 124.3(5) . . ? C16 C15 H15 117.8 . . ? C14 C15 H15 117.8 . . ? C15 C16 C11 117.5(5) . . ? C15 C16 C18 121.7(5) . . ? C11 C16 C18 120.7(5) . . ? N C17 C12 127.1(4) . . ? N C17 H17 116.4 . . ? C12 C17 H17 116.4 . . ? C20 C18 C19 109.9(6) . . ? C20 C18 C21 106.7(5) . . ? C19 C18 C21 106.6(5) . . ? C20 C18 C16 110.3(4) . . ? C19 C18 C16 111.2(4) . . ? C21 C18 C16 112.0(5) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N C22 C23 107.8(5) . . ? N C22 C24 113.0(5) . . ? C23 C22 C24 113.1(5) . . ? N C22 H22 107.6 . . ? C23 C22 H22 107.6 . . ? C24 C22 H22 107.6 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O Cr N 87.96(16) . . ? O Cr C5 92.30(16) . . ? N Cr C5 115.70(18) . . ? O Cr C4 97.60(16) . . ? N Cr C4 151.25(18) . . ? C5 Cr C4 36.27(18) . . ? O Cr C1 120.57(18) . . ? N Cr C1 92.00(19) . . ? C5 Cr C1 36.58(16) . . ? C4 Cr C1 60.88(18) . . ? O Cr C2 153.32(17) . . ? N Cr C2 103.8(2) . . ? C5 Cr C2 61.04(18) . . ? C4 Cr C2 60.89(19) . . ? C1 Cr C2 36.8(2) . . ? O Cr C3 131.11(18) . . ? N Cr C3 139.4(2) . . ? C5 Cr C3 60.68(19) . . ? C4 Cr C3 36.39(18) . . ? C1 Cr C3 61.0(2) . . ? C2 Cr C3 36.5(2) . . ? O Cr Cl 96.99(11) . . ? N Cr Cl 96.81(13) . . ? C5 Cr Cl 146.48(14) . . ? C4 Cr Cl 110.35(13) . . ? C1 Cr Cl 141.71(16) . . ? C2 Cr Cl 105.08(17) . . ? C3 Cr Cl 89.69(14) . . ? C17 N C22 118.5(4) . . ? C17 N Cr 121.7(3) . . ? C22 N Cr 119.8(4) . . ? C11 O Cr 129.3(3) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.772 _refine_diff_density_min -0.644 _refine_diff_density_rms 0.083 #===END data_complex_3 _database_code_depnum_ccdc_archive 'CCDC 756688' #TrackingRef '- combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H37 Cl Cr N O' _chemical_formula_weight 455.01 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)/n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.4568(19) _cell_length_b 12.286(3) _cell_length_c 21.323(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.68(3) _cell_angle_gamma 90.00 _cell_volume 2434.5(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5531 _cell_measurement_theta_min 3.05 _cell_measurement_theta_max 27.46 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.241 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 972 _exptl_absorpt_coefficient_mu 0.595 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21973 _diffrn_reflns_av_R_equivalents 0.0685 _diffrn_reflns_av_sigmaI/netI 0.0622 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 27.46 _reflns_number_total 5531 _reflns_number_gt 3369 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0644P)^2^+0.7793P] 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 5531 _refine_ls_number_parameters 273 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1027 _refine_ls_R_factor_gt 0.0555 _refine_ls_wR_factor_ref 0.1453 _refine_ls_wR_factor_gt 0.1263 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 0.45411(5) 0.74802(4) 0.15662(2) 0.03290(15) Uani 1 1 d . . . Cl1 Cl 0.45379(10) 0.56507(7) 0.18410(5) 0.0583(3) Uani 1 1 d . . . O1 O 0.5823(2) 0.72609(16) 0.09702(9) 0.0408(5) Uani 1 1 d . . . N1 N 0.6311(3) 0.8022(2) 0.22262(11) 0.0408(6) Uani 1 1 d . . . C1 C 0.3254(4) 0.9006(3) 0.16595(18) 0.0574(9) Uani 1 1 d . . . C2 C 0.3398(4) 0.8855(3) 0.10146(18) 0.0557(10) Uani 1 1 d . . . C3 C 0.2649(4) 0.7902(3) 0.07956(15) 0.0513(9) Uani 1 1 d . . . C4 C 0.2086(3) 0.7464(3) 0.12915(17) 0.0513(8) Uani 1 1 d . . . C5 C 0.2441(4) 0.8121(3) 0.18253(16) 0.0520(9) Uani 1 1 d . . . C6 C 0.3745(6) 0.9973(4) 0.2066(3) 0.117(2) Uani 1 1 d . . . H6A H 0.3818 0.9783 0.2507 0.176 Uiso 1 1 calc R . . H6B H 0.3063 1.0554 0.1961 0.176 Uiso 1 1 calc R . . H6C H 0.4669 1.0205 0.1991 0.176 Uiso 1 1 calc R . . C7 C 0.4124(5) 0.9629(4) 0.0631(3) 0.117(2) Uani 1 1 d . . . H7A H 0.4541 0.9227 0.0324 0.175 Uiso 1 1 calc R . . H7B H 0.4866 1.0019 0.0910 0.175 Uiso 1 1 calc R . . H7C H 0.3429 1.0135 0.0412 0.175 Uiso 1 1 calc R . . C8 C 0.2391(5) 0.7478(5) 0.0122(2) 0.108(2) Uani 1 1 d . . . H8A H 0.2746 0.6746 0.0119 0.163 Uiso 1 1 calc R . . H8B H 0.2883 0.7932 -0.0135 0.163 Uiso 1 1 calc R . . H8C H 0.1377 0.7486 -0.0049 0.163 Uiso 1 1 calc R . . C9 C 0.1140(5) 0.6468(4) 0.1254(3) 0.1020(18) Uani 1 1 d . . . H9A H 0.0152 0.6688 0.1209 0.153 Uiso 1 1 calc R . . H9B H 0.1406 0.6045 0.1636 0.153 Uiso 1 1 calc R . . H9C H 0.1259 0.6037 0.0892 0.153 Uiso 1 1 calc R . . C10 C 0.1815(5) 0.7998(5) 0.2424(2) 0.1014(18) Uani 1 1 d . . . H10A H 0.2130 0.8592 0.2708 0.152 Uiso 1 1 calc R . . H10B H 0.2135 0.7323 0.2630 0.152 Uiso 1 1 calc R . . H10C H 0.0784 0.8000 0.2314 0.152 Uiso 1 1 calc R . . C16 C 0.7587(3) 0.8580(2) 0.13704(14) 0.0388(7) Uani 1 1 d . . . C15 C 0.8717(3) 0.9258(3) 0.12637(17) 0.0503(8) Uani 1 1 d . . . H15 H 0.9137 0.9740 0.1580 0.060 Uiso 1 1 calc R . . C14 C 0.9202(4) 0.9217(3) 0.07002(18) 0.0556(9) Uani 1 1 d . . . H14 H 0.9891 0.9708 0.0615 0.067 Uiso 1 1 calc R . . C13 C 0.8651(3) 0.8432(3) 0.02593(16) 0.0476(8) Uani 1 1 d . . . H13 H 0.9028 0.8387 -0.0113 0.057 Uiso 1 1 calc R . . C12 C 0.7569(3) 0.7705(2) 0.03344(14) 0.0390(7) Uani 1 1 d . . . C11 C 0.6942(3) 0.7836(2) 0.08917(14) 0.0373(7) Uani 1 1 d . . . C17 C 0.7316(3) 0.8527(3) 0.20090(15) 0.0442(7) Uani 1 1 d . . . H17 H 0.7959 0.8913 0.2311 0.053 Uiso 1 1 calc R . . C18 C 0.6602(4) 0.7847(3) 0.29477(15) 0.0524(9) Uani 1 1 d . . . C19 C 0.5237(4) 0.7451(4) 0.31512(18) 0.0733(12) Uani 1 1 d . . . H19A H 0.4863 0.6836 0.2895 0.110 Uiso 1 1 calc R . . H19B H 0.4536 0.8024 0.3095 0.110 Uiso 1 1 calc R . . H19C H 0.5448 0.7241 0.3592 0.110 Uiso 1 1 calc R . . C20 C 0.7096(5) 0.8892(4) 0.33081(19) 0.0844(14) Uani 1 1 d . . . H20A H 0.7073 0.8796 0.3753 0.127 Uiso 1 1 calc R . . H20B H 0.6467 0.9478 0.3141 0.127 Uiso 1 1 calc R . . H20C H 0.8061 0.9059 0.3258 0.127 Uiso 1 1 calc R . . C21 C 0.7727(4) 0.6967(4) 0.30819(19) 0.0725(12) Uani 1 1 d . . . H21A H 0.7800 0.6718 0.3514 0.109 Uiso 1 1 calc R . . H21B H 0.8639 0.7252 0.3024 0.109 Uiso 1 1 calc R . . H21C H 0.7458 0.6370 0.2794 0.109 Uiso 1 1 calc R . . C22 C 0.7102(3) 0.6787(3) -0.01457(15) 0.0454(8) Uani 1 1 d . . . C23 C 0.8061(5) 0.6709(4) -0.0646(2) 0.0859(15) Uani 1 1 d . . . H23A H 0.7726 0.6131 -0.0939 0.129 Uiso 1 1 calc R . . H23B H 0.9034 0.6564 -0.0440 0.129 Uiso 1 1 calc R . . H23C H 0.8027 0.7385 -0.0875 0.129 Uiso 1 1 calc R . . C24 C 0.7215(5) 0.5696(3) 0.0203(2) 0.0822(13) Uani 1 1 d . . . H24A H 0.6618 0.5708 0.0522 0.123 Uiso 1 1 calc R . . H24B H 0.8196 0.5570 0.0405 0.123 Uiso 1 1 calc R . . H24C H 0.6902 0.5123 -0.0097 0.123 Uiso 1 1 calc R . . C25 C 0.5568(4) 0.6947(5) -0.0490(2) 0.0898(15) Uani 1 1 d . . . H25A H 0.5338 0.6411 -0.0821 0.135 Uiso 1 1 calc R . . H25B H 0.5466 0.7662 -0.0675 0.135 Uiso 1 1 calc R . . H25C H 0.4926 0.6871 -0.0193 0.135 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 0.0316(2) 0.0376(3) 0.0302(2) 0.0008(2) 0.00770(17) 0.0012(2) Cl1 0.0638(6) 0.0417(4) 0.0714(6) 0.0107(4) 0.0180(5) 0.0045(4) O1 0.0347(11) 0.0511(12) 0.0390(12) -0.0081(9) 0.0135(9) -0.0068(9) N1 0.0397(14) 0.0504(15) 0.0317(13) -0.0046(11) 0.0051(11) 0.0019(12) C1 0.056(2) 0.0469(19) 0.063(2) -0.0106(17) -0.0044(18) 0.0195(17) C2 0.0455(19) 0.059(2) 0.065(2) 0.0315(18) 0.0181(17) 0.0176(17) C3 0.0409(18) 0.073(2) 0.0368(18) 0.0006(16) -0.0007(14) 0.0188(17) C4 0.0302(16) 0.056(2) 0.065(2) 0.0090(18) 0.0014(15) 0.0035(16) C5 0.0434(19) 0.068(2) 0.048(2) 0.0108(17) 0.0155(16) 0.0173(18) C6 0.127(5) 0.057(3) 0.153(5) -0.043(3) -0.013(4) 0.023(3) C7 0.079(3) 0.116(4) 0.165(5) 0.100(4) 0.046(3) 0.026(3) C8 0.071(3) 0.193(6) 0.053(3) -0.031(3) -0.011(2) 0.052(3) C9 0.052(3) 0.090(3) 0.153(5) 0.022(3) -0.011(3) -0.017(2) C10 0.070(3) 0.179(5) 0.063(3) 0.030(3) 0.032(2) 0.043(3) C16 0.0312(15) 0.0444(17) 0.0407(17) -0.0007(13) 0.0061(13) 0.0014(13) C15 0.0431(18) 0.0479(18) 0.059(2) -0.0025(16) 0.0074(16) -0.0065(15) C14 0.047(2) 0.054(2) 0.069(2) 0.0109(18) 0.0202(18) -0.0079(17) C13 0.0452(18) 0.057(2) 0.0443(19) 0.0089(15) 0.0176(15) 0.0034(16) C12 0.0349(15) 0.0461(18) 0.0375(16) 0.0068(13) 0.0104(13) 0.0053(14) C11 0.0308(15) 0.0437(16) 0.0369(16) 0.0047(12) 0.0054(12) 0.0049(13) C17 0.0402(17) 0.0482(18) 0.0431(18) -0.0092(14) 0.0045(14) -0.0025(15) C18 0.053(2) 0.075(2) 0.0272(16) -0.0054(15) 0.0037(14) -0.0041(18) C19 0.063(2) 0.120(4) 0.0393(19) 0.004(2) 0.0149(17) -0.006(2) C20 0.104(4) 0.105(3) 0.042(2) -0.020(2) 0.006(2) -0.016(3) C21 0.060(2) 0.108(3) 0.048(2) 0.018(2) 0.0051(19) 0.014(2) C22 0.0428(18) 0.058(2) 0.0379(18) 0.0003(15) 0.0146(14) 0.0033(15) C23 0.083(3) 0.119(4) 0.067(3) -0.033(3) 0.042(2) -0.020(3) C24 0.120(4) 0.058(2) 0.072(3) -0.016(2) 0.027(3) -0.004(2) C25 0.062(3) 0.128(4) 0.072(3) -0.034(3) -0.008(2) 0.009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 O1 1.9311(19) . ? Cr1 N1 2.087(3) . ? Cr1 C2 2.222(3) . ? Cr1 C3 2.254(3) . ? Cr1 C1 2.264(3) . ? Cr1 C4 2.287(3) . ? Cr1 C5 2.297(3) . ? Cr1 Cl1 2.3229(10) . ? O1 C11 1.309(3) . ? N1 C17 1.290(4) . ? N1 C18 1.527(4) . ? C1 C5 1.415(5) . ? C1 C2 1.419(5) . ? C1 C6 1.493(5) . ? C2 C3 1.403(5) . ? C2 C7 1.501(5) . ? C3 C4 1.379(5) . ? C3 C8 1.505(5) . ? C4 C5 1.386(5) . ? C4 C9 1.509(5) . ? C5 C10 1.510(5) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C16 C15 1.407(4) . ? C16 C11 1.420(4) . ? C16 C17 1.433(4) . ? C15 C14 1.364(5) . ? C15 H15 0.9300 . ? C14 C13 1.380(5) . ? C14 H14 0.9300 . ? C13 C12 1.390(4) . ? C13 H13 0.9300 . ? C12 C11 1.432(4) . ? C12 C22 1.532(4) . ? C17 H17 0.9300 . ? C18 C21 1.506(5) . ? C18 C19 1.517(5) . ? C18 C20 1.524(5) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C25 1.513(5) . ? C22 C23 1.526(4) . ? C22 C24 1.527(5) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 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 88.01(9) . . ? O1 Cr1 C2 93.50(11) . . ? N1 Cr1 C2 111.42(13) . . ? O1 Cr1 C3 93.59(10) . . ? N1 Cr1 C3 147.95(13) . . ? C2 Cr1 C3 36.54(14) . . ? O1 Cr1 C1 125.92(12) . . ? N1 Cr1 C1 93.06(12) . . ? C2 Cr1 C1 36.86(13) . . ? C3 Cr1 C1 60.45(13) . . ? O1 Cr1 C4 124.18(11) . . ? N1 Cr1 C4 145.60(12) . . ? C2 Cr1 C4 59.99(13) . . ? C3 Cr1 C4 35.34(12) . . ? C1 Cr1 C4 59.55(13) . . ? O1 Cr1 C5 151.94(11) . . ? N1 Cr1 C5 110.46(12) . . ? C2 Cr1 C5 60.60(12) . . ? C3 Cr1 C5 59.45(12) . . ? C1 Cr1 C5 36.12(13) . . ? C4 Cr1 C5 35.18(12) . . ? O1 Cr1 Cl1 93.52(7) . . ? N1 Cr1 Cl1 100.21(8) . . ? C2 Cr1 Cl1 147.80(11) . . ? C3 Cr1 Cl1 111.62(11) . . ? C1 Cr1 Cl1 138.88(11) . . ? C4 Cr1 Cl1 90.42(9) . . ? C5 Cr1 Cl1 103.26(9) . . ? C11 O1 Cr1 129.05(18) . . ? C17 N1 C18 115.0(3) . . ? C17 N1 Cr1 117.6(2) . . ? C18 N1 Cr1 127.3(2) . . ? C5 C1 C2 107.2(3) . . ? C5 C1 C6 126.3(4) . . ? C2 C1 C6 126.3(4) . . ? C5 C1 Cr1 73.22(18) . . ? C2 C1 Cr1 69.94(18) . . ? C6 C1 Cr1 126.6(3) . . ? C3 C2 C1 107.4(3) . . ? C3 C2 C7 126.9(4) . . ? C1 C2 C7 125.6(4) . . ? C3 C2 Cr1 72.97(19) . . ? C1 C2 Cr1 73.20(18) . . ? C7 C2 Cr1 122.9(3) . . ? C4 C3 C2 108.3(3) . . ? C4 C3 C8 125.4(4) . . ? C2 C3 C8 126.1(4) . . ? C4 C3 Cr1 73.65(19) . . ? C2 C3 Cr1 70.49(19) . . ? C8 C3 Cr1 125.7(3) . . ? C3 C4 C5 109.5(3) . . ? C3 C4 C9 125.8(4) . . ? C5 C4 C9 124.6(4) . . ? C3 C4 Cr1 71.00(19) . . ? C5 C4 Cr1 72.82(19) . . ? C9 C4 Cr1 125.8(3) . . ? C4 C5 C1 107.6(3) . . ? C4 C5 C10 124.2(4) . . ? C1 C5 C10 127.2(4) . . ? C4 C5 Cr1 72.00(18) . . ? C1 C5 Cr1 70.66(18) . . ? C10 C5 Cr1 131.3(3) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C15 C16 C11 120.2(3) . . ? C15 C16 C17 117.1(3) . . ? C11 C16 C17 121.7(3) . . ? C14 C15 C16 120.7(3) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C15 C14 C13 118.7(3) . . ? C15 C14 H14 120.7 . . ? C13 C14 H14 120.7 . . ? C14 C13 C12 124.3(3) . . ? C14 C13 H13 117.8 . . ? C12 C13 H13 117.8 . . ? C13 C12 C11 116.7(3) . . ? C13 C12 C22 121.5(3) . . ? C11 C12 C22 121.7(3) . . ? O1 C11 C16 120.3(3) . . ? O1 C11 C12 120.9(3) . . ? C16 C11 C12 118.7(3) . . ? N1 C17 C16 129.5(3) . . ? N1 C17 H17 115.3 . . ? C16 C17 H17 115.3 . . ? C21 C18 C19 108.9(3) . . ? C21 C18 C20 111.7(3) . . ? C19 C18 C20 108.9(3) . . ? C21 C18 N1 106.4(3) . . ? C19 C18 N1 109.2(3) . . ? C20 C18 N1 111.7(3) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C25 C22 C23 108.0(3) . . ? C25 C22 C24 109.0(4) . . ? C23 C22 C24 106.8(3) . . ? C25 C22 C12 111.1(3) . . ? C23 C22 C12 112.2(3) . . ? C24 C22 C12 109.6(3) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.407 _refine_diff_density_min -0.387 _refine_diff_density_rms 0.061 #===END data_complex_4 _database_code_depnum_ccdc_archive 'CCDC 756690' #TrackingRef '- combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H43 Cl Cr N O' _chemical_formula_weight 497.08 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 11.921(2) _cell_length_b 19.965(4) _cell_length_c 13.056(3) _cell_angle_alpha 90.00 _cell_angle_beta 113.69(3) _cell_angle_gamma 90.00 _cell_volume 2845.5(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6367 _cell_measurement_theta_min 3.16 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.160 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1068 _exptl_absorpt_coefficient_mu 0.514 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID IP diffractometer' _diffrn_measurement_method 'Oscillation scans' _diffrn_detector_area_resol_mean '100x100 microns' _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 27139 _diffrn_reflns_av_R_equivalents 0.0753 _diffrn_reflns_av_sigmaI/netI 0.0614 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6367 _reflns_number_gt 4064 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAPID AUTO' _computing_cell_refinement 'RAPID AUTO' _computing_data_reduction 'RAPID AUTO' _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^)+(0.0752P)^2^+1.0966P] 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 6367 _refine_ls_number_parameters 302 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1043 _refine_ls_R_factor_gt 0.0610 _refine_ls_wR_factor_ref 0.1606 _refine_ls_wR_factor_gt 0.1415 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.109 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1882(4) 0.5323(2) 0.2677(3) 0.0537(9) Uani 1 1 d . . . C2 C 0.2980(4) 0.5645(2) 0.3374(4) 0.0586(10) Uani 1 1 d . . . C3 C 0.3192(4) 0.5479(2) 0.4502(3) 0.0578(10) Uani 1 1 d . . . C4 C 0.2230(4) 0.50549(18) 0.4471(3) 0.0540(10) Uani 1 1 d . . . C5 C 0.1453(4) 0.49500(18) 0.3350(3) 0.0539(9) Uani 1 1 d . . . C6 C 0.1327(5) 0.5328(3) 0.1411(3) 0.0864(16) Uani 1 1 d . . . H6A H 0.1600 0.4940 0.1140 0.130 Uiso 1 1 calc R . . H6B H 0.1581 0.5725 0.1149 0.130 Uiso 1 1 calc R . . H6C H 0.0450 0.5321 0.1142 0.130 Uiso 1 1 calc R . . C7 C 0.3802(5) 0.6023(3) 0.2959(5) 0.0958(17) Uani 1 1 d . . . H7A H 0.4110 0.5724 0.2557 0.144 Uiso 1 1 calc R . . H7B H 0.4475 0.6210 0.3584 0.144 Uiso 1 1 calc R . . H7C H 0.3347 0.6377 0.2472 0.144 Uiso 1 1 calc R . . C8 C 0.4276(5) 0.5664(3) 0.5546(4) 0.107(2) Uani 1 1 d . . . H8A H 0.3998 0.5827 0.6096 0.161 Uiso 1 1 calc R . . H8B H 0.4741 0.6006 0.5378 0.161 Uiso 1 1 calc R . . H8C H 0.4782 0.5276 0.5833 0.161 Uiso 1 1 calc R . . C9 C 0.2111(6) 0.4732(3) 0.5465(4) 0.0976(18) Uani 1 1 d . . . H9A H 0.1317 0.4530 0.5235 0.146 Uiso 1 1 calc R . . H9B H 0.2209 0.5066 0.6024 0.146 Uiso 1 1 calc R . . H9C H 0.2731 0.4395 0.5770 0.146 Uiso 1 1 calc R . . C10 C 0.0328(5) 0.4514(2) 0.2944(5) 0.0854(15) Uani 1 1 d . . . H10A H 0.0568 0.4053 0.3089 0.128 Uiso 1 1 calc R . . H10B H -0.0120 0.4578 0.2155 0.128 Uiso 1 1 calc R . . H10C H -0.0180 0.4632 0.3330 0.128 Uiso 1 1 calc R . . C11 C -0.0859(3) 0.63007(16) 0.1792(2) 0.0348(7) Uani 1 1 d . . . C12 C -0.2013(3) 0.60558(17) 0.1055(3) 0.0404(7) Uani 1 1 d . . . C13 C -0.2545(3) 0.63226(18) -0.0001(3) 0.0445(8) Uani 1 1 d . . . H13 H -0.3296 0.6150 -0.0484 0.053 Uiso 1 1 calc R . . C14 C -0.2029(3) 0.68397(18) -0.0400(3) 0.0429(8) Uani 1 1 d . . . C15 C -0.0932(3) 0.70924(17) 0.0343(3) 0.0422(8) Uani 1 1 d . . . H15 H -0.0573 0.7446 0.0120 0.051 Uiso 1 1 calc R . . C16 C -0.0333(3) 0.68336(16) 0.1429(2) 0.0367(7) Uani 1 1 d . . . C17 C 0.0739(3) 0.71890(16) 0.2174(2) 0.0391(7) Uani 1 1 d . . . H17 H 0.0903 0.7592 0.1906 0.047 Uiso 1 1 calc R . . C18 C -0.2669(3) 0.55210(19) 0.1431(3) 0.0523(9) Uani 1 1 d . . . H18 H -0.2129 0.5394 0.2197 0.063 Uiso 1 1 calc R . . C19 C -0.2923(5) 0.4897(2) 0.0721(4) 0.0837(15) Uani 1 1 d . . . H19A H -0.3530 0.4994 -0.0013 0.126 Uiso 1 1 calc R . . H19B H -0.3219 0.4551 0.1058 0.126 Uiso 1 1 calc R . . H19C H -0.2182 0.4751 0.0667 0.126 Uiso 1 1 calc R . . C20 C -0.3858(4) 0.5789(3) 0.1461(4) 0.0820(14) Uani 1 1 d . . . H20A H -0.3684 0.6182 0.1922 0.123 Uiso 1 1 calc R . . H20B H -0.4213 0.5452 0.1764 0.123 Uiso 1 1 calc R . . H20C H -0.4421 0.5900 0.0716 0.123 Uiso 1 1 calc R . . C21 C -0.2693(3) 0.7122(2) -0.1578(3) 0.0570(10) Uani 1 1 d . . . C25 C 0.2366(3) 0.75751(17) 0.3834(3) 0.0451(8) Uani 1 1 d . . . C26 C 0.3399(4) 0.7276(2) 0.4834(3) 0.0639(11) Uani 1 1 d . . . H26A H 0.3875 0.6984 0.4582 0.096 Uiso 1 1 calc R . . H26B H 0.3066 0.7027 0.5275 0.096 Uiso 1 1 calc R . . H26C H 0.3911 0.7629 0.5279 0.096 Uiso 1 1 calc R . . C27 C 0.2926(4) 0.7952(2) 0.3143(3) 0.0686(12) Uani 1 1 d . . . H27A H 0.3574 0.8236 0.3624 0.103 Uiso 1 1 calc R . . H27B H 0.2308 0.8221 0.2592 0.103 Uiso 1 1 calc R . . H27C H 0.3250 0.7637 0.2776 0.103 Uiso 1 1 calc R . . C28 C 0.1628(4) 0.8044(2) 0.4234(4) 0.0702(12) Uani 1 1 d . . . H28A H 0.2155 0.8388 0.4693 0.105 Uiso 1 1 calc R . . H28B H 0.1276 0.7797 0.4662 0.105 Uiso 1 1 calc R . . H28C H 0.0987 0.8246 0.3600 0.105 Uiso 1 1 calc R . . Cl1 Cl 0.11304(9) 0.63424(5) 0.53231(7) 0.0556(3) Uani 1 1 d . . . Cr1 Cr 0.13939(5) 0.60530(3) 0.37207(4) 0.03551(17) Uani 1 1 d . . . N1 N 0.1505(2) 0.70191(13) 0.3171(2) 0.0368(6) Uani 1 1 d . . . O1 O -0.0326(2) 0.60493(11) 0.28031(17) 0.0418(5) Uani 1 1 d . . . C22 C -0.1929(5) 0.7562(3) -0.1942(4) 0.0955(17) Uani 1 1 d U . . H22A H -0.2388 0.7701 -0.2700 0.143 Uiso 1 1 calc R . . H22B H -0.1211 0.7324 -0.1895 0.143 Uiso 1 1 calc R . . H22C H -0.1689 0.7950 -0.1467 0.143 Uiso 1 1 calc R . . C23 C -0.3798(6) 0.7489(4) -0.1638(6) 0.140(2) Uani 1 1 d U . . H23A H -0.3556 0.7869 -0.1147 0.210 Uiso 1 1 calc R . . H23B H -0.4300 0.7198 -0.1414 0.210 Uiso 1 1 calc R . . H23C H -0.4254 0.7639 -0.2391 0.210 Uiso 1 1 calc R . . C24 C -0.3176(8) 0.6552(4) -0.2425(5) 0.150(3) Uani 1 1 d U . . H24A H -0.3589 0.6735 -0.3162 0.225 Uiso 1 1 calc R . . H24B H -0.3739 0.6284 -0.2243 0.225 Uiso 1 1 calc R . . H24C H -0.2504 0.6278 -0.2402 0.225 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.065(3) 0.050(2) 0.052(2) -0.0034(17) 0.0300(19) 0.0088(19) C2 0.058(2) 0.046(2) 0.086(3) 0.003(2) 0.043(2) 0.0092(19) C3 0.049(2) 0.050(2) 0.062(2) -0.0026(18) 0.0091(18) 0.0198(18) C4 0.065(3) 0.041(2) 0.057(2) 0.0114(16) 0.0263(19) 0.0155(18) C5 0.063(3) 0.037(2) 0.065(2) -0.0037(17) 0.030(2) 0.0028(17) C6 0.128(4) 0.085(4) 0.057(3) -0.012(2) 0.047(3) 0.021(3) C7 0.093(4) 0.074(3) 0.160(5) 0.004(3) 0.091(4) -0.001(3) C8 0.079(4) 0.088(4) 0.100(4) -0.011(3) -0.022(3) 0.027(3) C9 0.150(5) 0.077(3) 0.081(3) 0.041(3) 0.062(3) 0.041(3) C10 0.089(4) 0.048(3) 0.120(4) -0.013(3) 0.043(3) -0.013(2) C11 0.0327(16) 0.0373(17) 0.0339(16) -0.0008(13) 0.0129(13) 0.0005(13) C12 0.0391(18) 0.0425(19) 0.0411(17) -0.0017(14) 0.0175(14) -0.0067(15) C13 0.0329(17) 0.054(2) 0.0402(18) -0.0027(15) 0.0082(14) -0.0092(15) C14 0.0359(18) 0.049(2) 0.0391(17) 0.0044(15) 0.0104(14) -0.0008(15) C15 0.0357(17) 0.0445(19) 0.0435(18) 0.0090(14) 0.0130(14) 0.0016(15) C16 0.0312(16) 0.0384(18) 0.0376(16) 0.0007(13) 0.0108(13) -0.0036(14) C17 0.0355(17) 0.0368(18) 0.0407(17) 0.0049(13) 0.0107(14) -0.0027(14) C18 0.048(2) 0.060(2) 0.0474(19) -0.0024(16) 0.0175(16) -0.0232(18) C19 0.107(4) 0.055(3) 0.099(3) -0.011(2) 0.052(3) -0.030(3) C20 0.069(3) 0.090(4) 0.107(4) -0.010(3) 0.056(3) -0.026(3) C21 0.0382(19) 0.071(3) 0.047(2) 0.0165(18) 0.0007(16) -0.0016(18) C25 0.0369(18) 0.0419(19) 0.0462(19) -0.0009(15) 0.0059(15) -0.0091(15) C26 0.055(2) 0.057(3) 0.056(2) 0.0013(18) -0.0025(18) -0.0123(19) C27 0.058(2) 0.073(3) 0.062(2) 0.005(2) 0.011(2) -0.029(2) C28 0.063(3) 0.052(3) 0.085(3) -0.021(2) 0.019(2) -0.007(2) Cl1 0.0721(7) 0.0579(6) 0.0430(5) -0.0073(4) 0.0295(4) -0.0032(5) Cr1 0.0387(3) 0.0348(3) 0.0327(3) 0.0012(2) 0.0139(2) 0.0006(2) N1 0.0315(14) 0.0380(15) 0.0384(14) 0.0003(11) 0.0113(11) -0.0030(11) O1 0.0398(12) 0.0448(13) 0.0370(12) 0.0047(10) 0.0114(10) -0.0066(10) C22 0.076(3) 0.124(4) 0.076(3) 0.046(3) 0.019(2) -0.013(3) C23 0.112(4) 0.173(5) 0.143(4) 0.075(4) 0.059(3) 0.044(4) C24 0.195(5) 0.136(4) 0.080(3) 0.007(3) 0.014(3) -0.032(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 C1 C5 1.396(5) . ? C1 C2 1.413(6) . ? C1 C6 1.513(5) . ? C1 Cr1 2.226(4) . ? C2 C3 1.428(6) . ? C2 C7 1.501(6) . ? C2 Cr1 2.265(4) . ? C3 C4 1.413(6) . ? C3 C8 1.499(6) . ? C3 Cr1 2.279(4) . ? C4 C5 1.398(5) . ? C4 C9 1.506(6) . ? C4 Cr1 2.267(3) . ? C5 C10 1.505(6) . ? C5 Cr1 2.262(4) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 O1 1.314(4) . ? C11 C16 1.410(4) . ? C11 C12 1.412(4) . ? C12 C13 1.372(5) . ? C12 C18 1.517(5) . ? C13 C14 1.404(5) . ? C13 H13 0.9300 . ? C14 C15 1.374(4) . ? C14 C21 1.527(5) . ? C15 C16 1.405(4) . ? C15 H15 0.9300 . ? C16 C17 1.444(4) . ? C17 N1 1.299(4) . ? C17 H17 0.9300 . ? C18 C19 1.508(6) . ? C18 C20 1.530(6) . ? C18 H18 0.9800 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C22 1.476(6) . ? C21 C23 1.483(7) . ? C21 C24 1.529(8) . ? C25 C26 1.511(5) . ? C25 C28 1.514(5) . ? C25 C27 1.520(5) . ? C25 N1 1.523(4) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? Cl1 Cr1 2.3103(10) . ? Cr1 O1 1.914(2) . ? Cr1 N1 2.081(3) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 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 C5 C1 C2 108.4(3) . . ? C5 C1 C6 125.5(4) . . ? C2 C1 C6 125.9(4) . . ? C5 C1 Cr1 73.3(2) . . ? C2 C1 Cr1 73.1(2) . . ? C6 C1 Cr1 123.8(3) . . ? C1 C2 C3 107.1(4) . . ? C1 C2 C7 124.5(4) . . ? C3 C2 C7 128.1(4) . . ? C1 C2 Cr1 70.2(2) . . ? C3 C2 Cr1 72.2(2) . . ? C7 C2 Cr1 127.5(3) . . ? C4 C3 C2 107.6(3) . . ? C4 C3 C8 124.5(4) . . ? C2 C3 C8 127.7(5) . . ? C4 C3 Cr1 71.4(2) . . ? C2 C3 Cr1 71.1(2) . . ? C8 C3 Cr1 126.5(3) . . ? C5 C4 C3 108.0(3) . . ? C5 C4 C9 125.9(4) . . ? C3 C4 C9 126.0(4) . . ? C5 C4 Cr1 71.8(2) . . ? C3 C4 Cr1 72.3(2) . . ? C9 C4 Cr1 124.8(3) . . ? C1 C5 C4 108.8(3) . . ? C1 C5 C10 125.9(4) . . ? C4 C5 C10 125.3(4) . . ? C1 C5 Cr1 70.5(2) . . ? C4 C5 Cr1 72.2(2) . . ? C10 C5 Cr1 122.6(3) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O1 C11 C16 121.7(3) . . ? O1 C11 C12 119.9(3) . . ? C16 C11 C12 118.4(3) . . ? C13 C12 C11 118.7(3) . . ? C13 C12 C18 120.6(3) . . ? C11 C12 C18 120.7(3) . . ? C12 C13 C14 124.3(3) . . ? C12 C13 H13 117.9 . . ? C14 C13 H13 117.9 . . ? C15 C14 C13 116.3(3) . . ? C15 C14 C21 122.4(3) . . ? C13 C14 C21 121.2(3) . . ? C14 C15 C16 122.0(3) . . ? C14 C15 H15 119.0 . . ? C16 C15 H15 119.0 . . ? C15 C16 C11 120.2(3) . . ? C15 C16 C17 116.9(3) . . ? C11 C16 C17 122.5(3) . . ? N1 C17 C16 128.5(3) . . ? N1 C17 H17 115.8 . . ? C16 C17 H17 115.8 . . ? C19 C18 C12 112.6(3) . . ? C19 C18 C20 110.1(4) . . ? C12 C18 C20 111.4(3) . . ? C19 C18 H18 107.5 . . ? C12 C18 H18 107.5 . . ? C20 C18 H18 107.5 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C23 109.8(5) . . ? C22 C21 C14 114.1(3) . . ? C23 C21 C14 109.0(4) . . ? C22 C21 C24 108.2(5) . . ? C23 C21 C24 105.1(5) . . ? C14 C21 C24 110.3(4) . . ? C26 C25 C28 109.3(3) . . ? C26 C25 C27 107.9(3) . . ? C28 C25 C27 110.7(3) . . ? C26 C25 N1 109.4(3) . . ? C28 C25 N1 107.2(3) . . ? C27 C25 N1 112.3(3) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O1 Cr1 N1 89.34(10) . . ? O1 Cr1 C1 95.28(13) . . ? N1 Cr1 C1 109.10(12) . . ? O1 Cr1 C5 88.84(12) . . ? N1 Cr1 C5 144.78(12) . . ? C1 Cr1 C5 36.23(14) . . ? O1 Cr1 C2 130.06(13) . . ? N1 Cr1 C2 95.21(12) . . ? C1 Cr1 C2 36.66(14) . . ? C5 Cr1 C2 60.44(15) . . ? O1 Cr1 C4 116.20(13) . . ? N1 Cr1 C4 152.36(13) . . ? C1 Cr1 C4 60.73(14) . . ? C5 Cr1 C4 35.96(13) . . ? C2 Cr1 C4 60.81(14) . . ? O1 Cr1 C3 148.94(13) . . ? N1 Cr1 C3 116.20(14) . . ? C1 Cr1 C3 60.95(14) . . ? C5 Cr1 C3 60.12(14) . . ? C2 Cr1 C3 36.65(15) . . ? C4 Cr1 C3 36.23(14) . . ? O1 Cr1 Cl1 93.82(8) . . ? N1 Cr1 Cl1 97.54(8) . . ? C1 Cr1 Cl1 151.88(10) . . ? C5 Cr1 Cl1 117.67(10) . . ? C2 Cr1 Cl1 134.33(12) . . ? C4 Cr1 Cl1 91.42(10) . . ? C3 Cr1 Cl1 99.56(11) . . ? C17 N1 C25 114.9(3) . . ? C17 N1 Cr1 118.1(2) . . ? C25 N1 Cr1 126.96(19) . . ? C11 O1 Cr1 126.3(2) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 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 C5 C1 C2 C3 -2.1(4) . . . . ? C6 C1 C2 C3 -176.8(4) . . . . ? Cr1 C1 C2 C3 63.2(3) . . . . ? C5 C1 C2 C7 172.1(4) . . . . ? C6 C1 C2 C7 -2.6(6) . . . . ? Cr1 C1 C2 C7 -122.6(4) . . . . ? C5 C1 C2 Cr1 -65.3(3) . . . . ? C6 C1 C2 Cr1 119.9(4) . . . . ? C1 C2 C3 C4 0.6(4) . . . . ? C7 C2 C3 C4 -173.3(4) . . . . ? Cr1 C2 C3 C4 62.5(3) . . . . ? C1 C2 C3 C8 176.0(4) . . . . ? C7 C2 C3 C8 2.1(7) . . . . ? Cr1 C2 C3 C8 -122.1(4) . . . . ? C1 C2 C3 Cr1 -61.9(3) . . . . ? C7 C2 C3 Cr1 124.2(4) . . . . ? C2 C3 C4 C5 1.1(4) . . . . ? C8 C3 C4 C5 -174.5(4) . . . . ? Cr1 C3 C4 C5 63.4(3) . . . . ? C2 C3 C4 C9 177.1(4) . . . . ? C8 C3 C4 C9 1.5(6) . . . . ? Cr1 C3 C4 C9 -120.6(4) . . . . ? C2 C3 C4 Cr1 -62.3(3) . . . . ? C8 C3 C4 Cr1 122.1(4) . . . . ? C2 C1 C5 C4 2.8(4) . . . . ? C6 C1 C5 C4 177.6(4) . . . . ? Cr1 C1 C5 C4 -62.4(3) . . . . ? C2 C1 C5 C10 -178.1(4) . . . . ? C6 C1 C5 C10 -3.3(6) . . . . ? Cr1 C1 C5 C10 116.7(4) . . . . ? C2 C1 C5 Cr1 65.2(3) . . . . ? C6 C1 C5 Cr1 -120.0(4) . . . . ? C3 C4 C5 C1 -2.4(4) . . . . ? C9 C4 C5 C1 -178.4(4) . . . . ? Cr1 C4 C5 C1 61.4(3) . . . . ? C3 C4 C5 C10 178.5(4) . . . . ? C9 C4 C5 C10 2.4(6) . . . . ? Cr1 C4 C5 C10 -117.8(4) . . . . ? C3 C4 C5 Cr1 -63.7(3) . . . . ? C9 C4 C5 Cr1 120.3(4) . . . . ? O1 C11 C12 C13 -179.4(3) . . . . ? C16 C11 C12 C13 3.3(5) . . . . ? O1 C11 C12 C18 2.2(5) . . . . ? C16 C11 C12 C18 -175.1(3) . . . . ? C11 C12 C13 C14 -1.5(5) . . . . ? C18 C12 C13 C14 176.9(3) . . . . ? C12 C13 C14 C15 -1.3(5) . . . . ? C12 C13 C14 C21 -178.5(4) . . . . ? C13 C14 C15 C16 2.2(5) . . . . ? C21 C14 C15 C16 179.4(3) . . . . ? C14 C15 C16 C11 -0.4(5) . . . . ? C14 C15 C16 C17 -173.0(3) . . . . ? O1 C11 C16 C15 -179.7(3) . . . . ? C12 C11 C16 C15 -2.4(5) . . . . ? O1 C11 C16 C17 -7.5(5) . . . . ? C12 C11 C16 C17 169.8(3) . . . . ? C15 C16 C17 N1 -173.1(3) . . . . ? C11 C16 C17 N1 14.4(6) . . . . ? C13 C12 C18 C19 60.6(5) . . . . ? C11 C12 C18 C19 -121.0(4) . . . . ? C13 C12 C18 C20 -63.7(4) . . . . ? C11 C12 C18 C20 114.7(4) . . . . ? C15 C14 C21 C22 14.4(6) . . . . ? C13 C14 C21 C22 -168.5(4) . . . . ? C15 C14 C21 C23 -108.7(5) . . . . ? C13 C14 C21 C23 68.4(6) . . . . ? C15 C14 C21 C24 136.4(5) . . . . ? C13 C14 C21 C24 -46.5(6) . . . . ? C5 C1 Cr1 O1 -80.8(2) . . . . ? C2 C1 Cr1 O1 163.4(2) . . . . ? C6 C1 Cr1 O1 41.2(4) . . . . ? C5 C1 Cr1 N1 -171.9(2) . . . . ? C2 C1 Cr1 N1 72.3(2) . . . . ? C6 C1 Cr1 N1 -50.0(4) . . . . ? C2 C1 Cr1 C5 -115.8(3) . . . . ? C6 C1 Cr1 C5 121.9(5) . . . . ? C5 C1 Cr1 C2 115.8(3) . . . . ? C6 C1 Cr1 C2 -122.3(5) . . . . ? C5 C1 Cr1 C4 36.4(2) . . . . ? C2 C1 Cr1 C4 -79.4(2) . . . . ? C6 C1 Cr1 C4 158.3(4) . . . . ? C5 C1 Cr1 C3 78.1(3) . . . . ? C2 C1 Cr1 C3 -37.7(2) . . . . ? C6 C1 Cr1 C3 -160.0(4) . . . . ? C5 C1 Cr1 Cl1 27.6(4) . . . . ? C2 C1 Cr1 Cl1 -88.2(3) . . . . ? C6 C1 Cr1 Cl1 149.5(3) . . . . ? C1 C5 Cr1 O1 100.6(2) . . . . ? C4 C5 Cr1 O1 -141.2(2) . . . . ? C10 C5 Cr1 O1 -20.3(4) . . . . ? C1 C5 Cr1 N1 13.4(4) . . . . ? C4 C5 Cr1 N1 131.5(2) . . . . ? C10 C5 Cr1 N1 -107.5(4) . . . . ? C4 C5 Cr1 C1 118.2(3) . . . . ? C10 C5 Cr1 C1 -120.8(4) . . . . ? C1 C5 Cr1 C2 -38.2(2) . . . . ? C4 C5 Cr1 C2 80.0(3) . . . . ? C10 C5 Cr1 C2 -159.0(4) . . . . ? C1 C5 Cr1 C4 -118.2(3) . . . . ? C10 C5 Cr1 C4 121.0(5) . . . . ? C1 C5 Cr1 C3 -80.6(3) . . . . ? C4 C5 Cr1 C3 37.6(2) . . . . ? C10 C5 Cr1 C3 158.6(4) . . . . ? C1 C5 Cr1 Cl1 -165.7(2) . . . . ? C4 C5 Cr1 Cl1 -47.5(3) . . . . ? C10 C5 Cr1 Cl1 73.4(4) . . . . ? C1 C2 Cr1 O1 -21.8(3) . . . . ? C3 C2 Cr1 O1 -138.1(2) . . . . ? C7 C2 Cr1 O1 97.1(4) . . . . ? C1 C2 Cr1 N1 -115.3(2) . . . . ? C3 C2 Cr1 N1 128.3(2) . . . . ? C7 C2 Cr1 N1 3.5(4) . . . . ? C3 C2 Cr1 C1 -116.3(3) . . . . ? C7 C2 Cr1 C1 118.9(5) . . . . ? C1 C2 Cr1 C5 37.7(2) . . . . ? C3 C2 Cr1 C5 -78.6(3) . . . . ? C7 C2 Cr1 C5 156.6(5) . . . . ? C1 C2 Cr1 C4 79.2(2) . . . . ? C3 C2 Cr1 C4 -37.1(2) . . . . ? C7 C2 Cr1 C4 -161.9(5) . . . . ? C1 C2 Cr1 C3 116.3(3) . . . . ? C7 C2 Cr1 C3 -124.8(5) . . . . ? C1 C2 Cr1 Cl1 138.8(2) . . . . ? C3 C2 Cr1 Cl1 22.5(3) . . . . ? C7 C2 Cr1 Cl1 -102.3(4) . . . . ? C5 C4 Cr1 O1 44.2(3) . . . . ? C3 C4 Cr1 O1 160.7(2) . . . . ? C9 C4 Cr1 O1 -77.3(4) . . . . ? C5 C4 Cr1 N1 -111.5(3) . . . . ? C3 C4 Cr1 N1 5.0(4) . . . . ? C9 C4 Cr1 N1 127.0(4) . . . . ? C5 C4 Cr1 C1 -36.7(2) . . . . ? C3 C4 Cr1 C1 79.8(2) . . . . ? C9 C4 Cr1 C1 -158.2(5) . . . . ? C3 C4 Cr1 C5 116.5(3) . . . . ? C9 C4 Cr1 C5 -121.5(5) . . . . ? C5 C4 Cr1 C2 -78.9(3) . . . . ? C3 C4 Cr1 C2 37.6(2) . . . . ? C9 C4 Cr1 C2 159.6(5) . . . . ? C5 C4 Cr1 C3 -116.5(3) . . . . ? C9 C4 Cr1 C3 122.0(5) . . . . ? C5 C4 Cr1 Cl1 139.2(2) . . . . ? C3 C4 Cr1 Cl1 -104.3(2) . . . . ? C9 C4 Cr1 Cl1 17.7(4) . . . . ? C4 C3 Cr1 O1 -35.1(4) . . . . ? C2 C3 Cr1 O1 81.8(3) . . . . ? C8 C3 Cr1 O1 -154.7(4) . . . . ? C4 C3 Cr1 N1 -177.4(2) . . . . ? C2 C3 Cr1 N1 -60.5(3) . . . . ? C8 C3 Cr1 N1 62.9(5) . . . . ? C4 C3 Cr1 C1 -79.1(2) . . . . ? C2 C3 Cr1 C1 37.7(2) . . . . ? C8 C3 Cr1 C1 161.2(5) . . . . ? C4 C3 Cr1 C5 -37.3(2) . . . . ? C2 C3 Cr1 C5 79.6(3) . . . . ? C8 C3 Cr1 C5 -157.0(5) . . . . ? C4 C3 Cr1 C2 -116.9(3) . . . . ? C8 C3 Cr1 C2 123.5(6) . . . . ? C2 C3 Cr1 C4 116.9(3) . . . . ? C8 C3 Cr1 C4 -119.6(5) . . . . ? C4 C3 Cr1 Cl1 79.2(2) . . . . ? C2 C3 Cr1 Cl1 -163.9(2) . . . . ? C8 C3 Cr1 Cl1 -40.4(5) . . . . ? C16 C17 N1 C25 -166.7(3) . . . . ? C16 C17 N1 Cr1 10.8(5) . . . . ? C26 C25 N1 C17 -165.8(3) . . . . ? C28 C25 N1 C17 75.8(4) . . . . ? C27 C25 N1 C17 -45.9(4) . . . . ? C26 C25 N1 Cr1 17.0(4) . . . . ? C28 C25 N1 Cr1 -101.4(3) . . . . ? C27 C25 N1 Cr1 136.9(3) . . . . ? O1 Cr1 N1 C17 -29.8(2) . . . . ? C1 Cr1 N1 C17 65.6(3) . . . . ? C5 Cr1 N1 C17 57.3(3) . . . . ? C2 Cr1 N1 C17 100.4(3) . . . . ? C4 Cr1 N1 C17 128.6(3) . . . . ? C3 Cr1 N1 C17 131.9(2) . . . . ? Cl1 Cr1 N1 C17 -123.6(2) . . . . ? O1 Cr1 N1 C25 147.4(3) . . . . ? C1 Cr1 N1 C25 -117.3(3) . . . . ? C5 Cr1 N1 C25 -125.6(3) . . . . ? C2 Cr1 N1 C25 -82.5(3) . . . . ? C4 Cr1 N1 C25 -54.3(4) . . . . ? C3 Cr1 N1 C25 -51.0(3) . . . . ? Cl1 Cr1 N1 C25 53.6(3) . . . . ? C16 C11 O1 Cr1 -26.8(4) . . . . ? C12 C11 O1 Cr1 155.9(2) . . . . ? N1 Cr1 O1 C11 39.5(3) . . . . ? C1 Cr1 O1 C11 -69.6(3) . . . . ? C5 Cr1 O1 C11 -105.3(3) . . . . ? C2 Cr1 O1 C11 -56.8(3) . . . . ? C4 Cr1 O1 C11 -129.5(3) . . . . ? C3 Cr1 O1 C11 -107.3(3) . . . . ? Cl1 Cr1 O1 C11 137.0(2) . . . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.582 _refine_diff_density_min -0.501 _refine_diff_density_rms 0.059 #===END data_complex_6 _database_code_depnum_ccdc_archive 'CCDC 756691' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H49 Cl Cr N O' _chemical_formula_weight 575.19 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' 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 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 29.846(6) _cell_length_b 8.7377(17) _cell_length_c 26.532(5) _cell_angle_alpha 90.00 _cell_angle_beta 113.53(3) _cell_angle_gamma 90.00 _cell_volume 6344(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7248 _cell_measurement_theta_min 3.07 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.205 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2472 _exptl_absorpt_coefficient_mu 0.471 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID IP diffractometer' _diffrn_measurement_method 'Oscillation scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28394 _diffrn_reflns_av_R_equivalents 0.0973 _diffrn_reflns_av_sigmaI/netI 0.0871 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7248 _reflns_number_gt 4536 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAPID AUTO' _computing_cell_refinement 'RAPID AUTO' _computing_data_reduction 'RAPID AUTO' _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^)+(0.0681P)^2^+89.9510P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00031(14) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7248 _refine_ls_number_parameters 385 _refine_ls_number_restraints 120 _refine_ls_R_factor_all 0.1499 _refine_ls_R_factor_gt 0.1017 _refine_ls_wR_factor_ref 0.2873 _refine_ls_wR_factor_gt 0.2678 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.109 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1732(3) 0.3646(8) 0.5302(3) 0.0438(17) Uani 1 1 d . . . C2 C 0.1242(3) 0.3727(9) 0.5243(3) 0.0454(18) Uani 1 1 d . . . C3 C 0.1114(3) 0.5286(9) 0.5273(3) 0.0469(17) Uani 1 1 d . . . C4 C 0.1531(3) 0.6159(8) 0.5337(3) 0.0447(17) Uani 1 1 d . . . C5 C 0.1912(3) 0.5194(9) 0.5364(3) 0.0432(16) Uani 1 1 d . . . C6 C 0.1992(4) 0.2231(10) 0.5269(4) 0.071(3) Uani 1 1 d . . . H6A H 0.1878 0.1390 0.5419 0.107 Uiso 1 1 calc R . . H6B H 0.2337 0.2365 0.5476 0.107 Uiso 1 1 calc R . . H6C H 0.1931 0.2022 0.4892 0.107 Uiso 1 1 calc R . . C7 C 0.0904(4) 0.2385(12) 0.5146(4) 0.082(3) Uani 1 1 d . . . H7A H 0.0952 0.1693 0.4891 0.122 Uiso 1 1 calc R . . H7B H 0.0572 0.2738 0.4999 0.122 Uiso 1 1 calc R . . H7C H 0.0973 0.1865 0.5488 0.122 Uiso 1 1 calc R . . C8 C 0.0629(3) 0.5860(13) 0.5230(4) 0.081(3) Uani 1 1 d . . . H8A H 0.0663 0.6886 0.5371 0.121 Uiso 1 1 calc R . . H8B H 0.0508 0.5211 0.5441 0.121 Uiso 1 1 calc R . . H8C H 0.0402 0.5853 0.4852 0.121 Uiso 1 1 calc R . . C9 C 0.1534(4) 0.7898(10) 0.5308(4) 0.074(3) Uani 1 1 d . . . H9A H 0.1865 0.8254 0.5423 0.111 Uiso 1 1 calc R . . H9B H 0.1393 0.8315 0.5546 0.111 Uiso 1 1 calc R . . H9C H 0.1347 0.8222 0.4937 0.111 Uiso 1 1 calc R . . C10 C 0.2418(3) 0.5608(12) 0.5408(4) 0.070(3) Uani 1 1 d . . . H10A H 0.2457 0.6699 0.5432 0.105 Uiso 1 1 calc R . . H10B H 0.2461 0.5242 0.5089 0.105 Uiso 1 1 calc R . . H10C H 0.2657 0.5144 0.5732 0.105 Uiso 1 1 calc R . . C11 C 0.1230(2) 0.4288(7) 0.6857(2) 0.0325(14) Uani 1 1 d . . . C12 C 0.1489(2) 0.5546(7) 0.7180(3) 0.0348(14) Uani 1 1 d . . . C13 C 0.1448(3) 0.5933(9) 0.7673(3) 0.0438(17) Uani 1 1 d . . . H13 H 0.1628 0.6754 0.7877 0.053 Uiso 1 1 calc R . . C14 C 0.1152(3) 0.5142(9) 0.7860(3) 0.0430(17) Uani 1 1 d . A . C15 C 0.0902(3) 0.3911(8) 0.7540(3) 0.0404(16) Uani 1 1 d . . . H15 H 0.0699 0.3365 0.7665 0.048 Uiso 1 1 calc R . . C16 C 0.0923(2) 0.3409(8) 0.7054(2) 0.0334(14) Uani 1 1 d . . . C17 C 0.1834(2) 0.6466(7) 0.7048(3) 0.0364(15) Uani 1 1 d . . . H17 H 0.1984 0.7255 0.7292 0.044 Uiso 1 1 calc R . . C18 C 0.2356(3) 0.7387(8) 0.6649(3) 0.0460(18) Uani 1 1 d . . . H18 H 0.2365 0.7323 0.6284 0.055 Uiso 1 1 calc R . . C19 C 0.2268(3) 0.9041(9) 0.6742(4) 0.065(2) Uani 1 1 d . . . H19A H 0.1933 0.9297 0.6526 0.097 Uiso 1 1 calc R . . H19B H 0.2477 0.9680 0.6636 0.097 Uiso 1 1 calc R . . H19C H 0.2339 0.9199 0.7125 0.097 Uiso 1 1 calc R . . C20 C 0.2845(3) 0.6817(10) 0.7058(4) 0.061(2) Uani 1 1 d . . . H20A H 0.2841 0.6787 0.7419 0.091 Uiso 1 1 calc R . . H20B H 0.3098 0.7494 0.7060 0.091 Uiso 1 1 calc R . . H20C H 0.2904 0.5807 0.6956 0.091 Uiso 1 1 calc R . . C21 C 0.1109(3) 0.5555(10) 0.8404(3) 0.063(2) Uani 1 1 d DU . . C25 C 0.0650(2) 0.1974(8) 0.6760(3) 0.0339(14) Uani 1 1 d . . . C26 C 0.0275(3) 0.2354(8) 0.6185(3) 0.0421(16) Uani 1 1 d . . . H26A H 0.0439 0.2807 0.5972 0.050 Uiso 1 1 calc R . . H26B H 0.0044 0.3097 0.6212 0.050 Uiso 1 1 calc R . . C27 C 0.1004(3) 0.0786(8) 0.6703(3) 0.0481(18) Uani 1 1 d . . . H27A H 0.1244 0.0514 0.7065 0.058 Uiso 1 1 calc R . . H27B H 0.1176 0.1220 0.6494 0.058 Uiso 1 1 calc R . . C28 C 0.0370(3) 0.1212(10) 0.7071(3) 0.055(2) Uani 1 1 d . . . H28A H 0.0598 0.0950 0.7439 0.065 Uiso 1 1 calc R . . H28B H 0.0134 0.1930 0.7101 0.065 Uiso 1 1 calc R . . C29 C 0.0107(3) -0.0220(10) 0.6780(4) 0.060(2) Uani 1 1 d . . . H29 H -0.0061 -0.0666 0.6996 0.072 Uiso 1 1 calc R . . C30 C 0.0726(3) -0.0654(9) 0.6412(4) 0.056(2) Uani 1 1 d . . . H30 H 0.0958 -0.1399 0.6378 0.067 Uiso 1 1 calc R . . C31 C -0.0002(3) 0.0918(10) 0.5892(3) 0.055(2) Uani 1 1 d . . . H31 H -0.0238 0.1187 0.5522 0.066 Uiso 1 1 calc R . . C32 C 0.0358(3) -0.0248(10) 0.5851(3) 0.058(2) Uani 1 1 d . . . H32A H 0.0184 -0.1162 0.5669 0.069 Uiso 1 1 calc R . . H32B H 0.0524 0.0168 0.5633 0.069 Uiso 1 1 calc R . . C33 C -0.0269(3) 0.0155(11) 0.6218(4) 0.063(2) Uani 1 1 d . . . H33A H -0.0513 0.0846 0.6246 0.076 Uiso 1 1 calc R . . H33B H -0.0433 -0.0770 0.6033 0.076 Uiso 1 1 calc R . . C35 C 0.0456(4) -0.1368(10) 0.6738(4) 0.070(3) Uani 1 1 d . . . H35A H 0.0282 -0.2279 0.6553 0.084 Uiso 1 1 calc R . . H35B H 0.0688 -0.1657 0.7102 0.084 Uiso 1 1 calc R . . Cl1 Cl 0.23482(8) 0.3054(2) 0.65813(8) 0.0556(6) Uani 1 1 d . . . Cr1 Cr 0.17090(4) 0.46315(11) 0.60802(4) 0.0293(3) Uani 1 1 d . . . N1 N 0.19573(19) 0.6341(6) 0.6644(2) 0.0328(12) Uani 1 1 d . . . O1 O 0.12582(17) 0.3956(5) 0.63864(18) 0.0409(11) Uani 1 1 d . . . C22A C 0.1386(6) 0.6954(18) 0.8675(7) 0.081(4) Uani 0.678(15) 1 d PDU A 1 H22A H 0.1337 0.7155 0.9005 0.122 Uiso 0.678(15) 1 calc PR A 1 H22B H 0.1272 0.7810 0.8430 0.122 Uiso 0.678(15) 1 calc PR A 1 H22C H 0.1728 0.6798 0.8765 0.122 Uiso 0.678(15) 1 calc PR A 1 C23A C 0.0562(5) 0.571(2) 0.8292(6) 0.073(4) Uani 0.678(15) 1 d PDU A 1 H23A H 0.0528 0.5860 0.8633 0.110 Uiso 0.678(15) 1 calc PR A 1 H23B H 0.0392 0.4802 0.8116 0.110 Uiso 0.678(15) 1 calc PR A 1 H23C H 0.0427 0.6578 0.8057 0.110 Uiso 0.678(15) 1 calc PR A 1 C24A C 0.1260(7) 0.4195(18) 0.8796(6) 0.086(4) Uani 0.678(15) 1 d PDU A 1 H24A H 0.1596 0.3947 0.8882 0.130 Uiso 0.678(15) 1 calc PR A 1 H24B H 0.1058 0.3330 0.8625 0.130 Uiso 0.678(15) 1 calc PR A 1 H24C H 0.1220 0.4450 0.9127 0.130 Uiso 0.678(15) 1 calc PR A 1 C22B C 0.1166(13) 0.733(2) 0.8475(14) 0.067(6) Uani 0.322(15) 1 d PDU A 2 H22D H 0.1027 0.7667 0.8725 0.101 Uiso 0.322(15) 1 calc PR A 2 H22E H 0.1000 0.7815 0.8125 0.101 Uiso 0.322(15) 1 calc PR A 2 H22F H 0.1506 0.7593 0.8618 0.101 Uiso 0.322(15) 1 calc PR A 2 C23B C 0.0712(12) 0.477(4) 0.8522(16) 0.089(7) Uani 0.322(15) 1 d PDU A 2 H23D H 0.0785 0.4828 0.8908 0.134 Uiso 0.322(15) 1 calc PR A 2 H23E H 0.0694 0.3710 0.8415 0.134 Uiso 0.322(15) 1 calc PR A 2 H23F H 0.0405 0.5255 0.8319 0.134 Uiso 0.322(15) 1 calc PR A 2 C24B C 0.1592(10) 0.490(4) 0.8851(12) 0.085(7) Uani 0.322(15) 1 d PDU A 2 H24D H 0.1864 0.5505 0.8861 0.127 Uiso 0.322(15) 1 calc PR A 2 H24E H 0.1634 0.3862 0.8764 0.127 Uiso 0.322(15) 1 calc PR A 2 H24F H 0.1573 0.4942 0.9204 0.127 Uiso 0.322(15) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.063(5) 0.041(4) 0.033(3) -0.007(3) 0.025(3) -0.007(3) C2 0.052(4) 0.058(5) 0.028(3) -0.010(3) 0.019(3) -0.015(4) C3 0.044(4) 0.057(5) 0.033(4) 0.007(3) 0.008(3) 0.009(4) C4 0.062(5) 0.040(4) 0.030(3) 0.008(3) 0.016(3) 0.002(4) C5 0.049(4) 0.048(4) 0.035(4) 0.001(3) 0.020(3) -0.003(3) C6 0.104(8) 0.057(5) 0.072(6) -0.010(5) 0.056(6) 0.008(5) C7 0.097(8) 0.093(7) 0.057(6) -0.033(5) 0.034(5) -0.054(6) C8 0.049(5) 0.105(8) 0.074(7) 0.014(6) 0.008(5) 0.022(5) C9 0.103(8) 0.046(5) 0.056(5) 0.014(4) 0.014(5) 0.005(5) C10 0.075(6) 0.079(7) 0.073(6) 0.000(5) 0.049(5) -0.021(5) C11 0.030(3) 0.038(4) 0.028(3) -0.005(3) 0.009(3) -0.001(3) C12 0.037(3) 0.035(3) 0.032(3) -0.004(3) 0.013(3) -0.004(3) C13 0.044(4) 0.046(4) 0.036(4) -0.015(3) 0.011(3) -0.005(3) C14 0.042(4) 0.059(5) 0.031(3) -0.008(3) 0.017(3) -0.002(3) C15 0.041(4) 0.052(4) 0.033(3) -0.003(3) 0.020(3) -0.006(3) C16 0.034(3) 0.040(4) 0.027(3) -0.001(3) 0.012(3) -0.003(3) C17 0.039(4) 0.034(3) 0.033(3) -0.010(3) 0.012(3) -0.004(3) C18 0.050(4) 0.037(4) 0.055(4) -0.010(3) 0.025(4) -0.014(3) C19 0.071(6) 0.034(4) 0.091(7) -0.005(4) 0.035(5) -0.014(4) C20 0.038(4) 0.067(6) 0.069(6) -0.005(4) 0.013(4) -0.017(4) C21 0.071(4) 0.072(4) 0.053(4) -0.008(3) 0.032(3) -0.002(3) C25 0.034(3) 0.040(4) 0.033(3) -0.006(3) 0.019(3) -0.008(3) C26 0.037(4) 0.046(4) 0.043(4) -0.001(3) 0.016(3) 0.001(3) C27 0.035(4) 0.042(4) 0.062(5) -0.003(3) 0.015(3) -0.003(3) C28 0.058(5) 0.069(5) 0.046(4) -0.010(4) 0.030(4) -0.023(4) C29 0.069(6) 0.065(5) 0.061(5) -0.007(4) 0.041(5) -0.025(5) C30 0.056(5) 0.037(4) 0.075(6) -0.011(4) 0.028(4) -0.008(4) C31 0.050(5) 0.062(5) 0.048(4) -0.006(4) 0.014(4) -0.009(4) C32 0.061(5) 0.053(5) 0.061(5) -0.021(4) 0.028(4) -0.016(4) C33 0.048(5) 0.068(6) 0.081(6) -0.014(5) 0.034(5) -0.005(4) C35 0.083(7) 0.051(5) 0.071(6) 0.006(4) 0.025(5) -0.016(5) Cl1 0.0626(13) 0.0450(11) 0.0486(11) 0.0072(8) 0.0109(9) 0.0198(9) Cr1 0.0341(5) 0.0294(5) 0.0255(5) -0.0003(4) 0.0129(4) -0.0009(4) N1 0.035(3) 0.029(3) 0.034(3) 0.001(2) 0.014(2) -0.001(2) O1 0.046(3) 0.046(3) 0.035(2) -0.014(2) 0.021(2) -0.014(2) C22A 0.087(6) 0.086(5) 0.075(6) -0.016(4) 0.037(4) -0.005(4) C23A 0.078(5) 0.081(6) 0.071(5) -0.011(4) 0.041(4) 0.003(4) C24A 0.093(6) 0.088(5) 0.076(6) 0.008(4) 0.031(4) -0.001(4) C22B 0.069(8) 0.072(6) 0.064(8) -0.006(5) 0.030(5) 0.004(4) C23B 0.088(7) 0.092(8) 0.091(9) 0.002(5) 0.039(5) -0.006(5) C24B 0.087(7) 0.086(8) 0.080(8) 0.003(5) 0.032(5) 0.004(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.406(10) . ? C1 C5 1.441(10) . ? C1 C6 1.482(11) . ? C1 Cr1 2.263(7) . ? C2 C3 1.426(11) . ? C2 C7 1.502(11) . ? C2 Cr1 2.242(7) . ? C3 C4 1.413(11) . ? C3 C8 1.493(11) . ? C3 Cr1 2.243(7) . ? C4 C5 1.393(10) . ? C4 C9 1.521(11) . ? C4 Cr1 2.262(7) . ? C5 C10 1.511(11) . ? C5 Cr1 2.267(7) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 O1 1.317(7) . ? C11 C12 1.417(9) . ? C11 C16 1.444(9) . ? C12 C13 1.403(9) . ? C12 C17 1.455(9) . ? C13 C14 1.363(10) . ? C13 H13 0.9300 . ? C14 C15 1.389(10) . ? C14 C21 1.540(10) . ? C15 C16 1.387(9) . ? C15 H15 0.9300 . ? C16 C25 1.528(9) . ? C17 N1 1.268(8) . ? C17 H17 0.9300 . ? C18 N1 1.496(8) . ? C18 C19 1.507(10) . ? C18 C20 1.514(11) . ? C18 H18 0.9800 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C22A 1.490(14) . ? C21 C23B 1.509(18) . ? C21 C24A 1.524(13) . ? C21 C23A 1.545(13) . ? C21 C22B 1.562(18) . ? C21 C24B 1.562(18) . ? C25 C26 1.526(9) . ? C25 C27 1.531(10) . ? C25 C28 1.539(9) . ? C26 C31 1.532(10) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C30 1.536(10) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.514(11) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C35 1.483(13) . ? C29 C33 1.502(12) . ? C29 H29 0.9800 . ? C30 C32 1.497(12) . ? C30 C35 1.530(12) . ? C30 H30 0.9800 . ? C31 C32 1.515(12) . ? C31 C33 1.543(12) . ? C31 H31 0.9800 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? Cl1 Cr1 2.298(2) . ? Cr1 O1 1.921(5) . ? Cr1 N1 2.033(5) . ? C22A H22A 0.9600 . ? C22A H22B 0.9600 . ? C22A H22C 0.9600 . ? C23A H23A 0.9600 . ? C23A H23B 0.9600 . ? C23A H23C 0.9600 . ? C24A H24A 0.9600 . ? C24A H24B 0.9600 . ? C24A H24C 0.9600 . ? C22B H22D 0.9600 . ? C22B H22E 0.9600 . ? C22B H22F 0.9600 . ? C23B H23D 0.9600 . ? C23B H23E 0.9600 . ? C23B H23F 0.9600 . ? C24B H24D 0.9600 . ? C24B H24E 0.9600 . ? C24B H24F 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 C2 C1 C5 106.8(7) . . ? C2 C1 C6 125.6(7) . . ? C5 C1 C6 127.5(7) . . ? C2 C1 Cr1 71.0(4) . . ? C5 C1 Cr1 71.6(4) . . ? C6 C1 Cr1 125.3(6) . . ? C1 C2 C3 109.5(7) . . ? C1 C2 C7 125.2(8) . . ? C3 C2 C7 125.3(8) . . ? C1 C2 Cr1 72.6(4) . . ? C3 C2 Cr1 71.5(4) . . ? C7 C2 Cr1 123.6(5) . . ? C4 C3 C2 106.1(7) . . ? C4 C3 C8 127.6(8) . . ? C2 C3 C8 126.3(8) . . ? C4 C3 Cr1 72.4(4) . . ? C2 C3 Cr1 71.4(4) . . ? C8 C3 Cr1 122.2(6) . . ? C5 C4 C3 110.0(7) . . ? C5 C4 C9 125.9(8) . . ? C3 C4 C9 123.8(8) . . ? C5 C4 Cr1 72.3(4) . . ? C3 C4 Cr1 71.0(4) . . ? C9 C4 Cr1 129.0(5) . . ? C4 C5 C1 107.6(7) . . ? C4 C5 C10 128.9(7) . . ? C1 C5 C10 123.3(7) . . ? C4 C5 Cr1 71.9(4) . . ? C1 C5 Cr1 71.3(4) . . ? C10 C5 Cr1 125.4(5) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O1 C11 C12 121.2(6) . . ? O1 C11 C16 121.0(6) . . ? C12 C11 C16 117.8(6) . . ? C13 C12 C11 121.4(6) . . ? C13 C12 C17 115.1(6) . . ? C11 C12 C17 123.4(6) . . ? C14 C13 C12 122.0(6) . . ? C14 C13 H13 119.0 . . ? C12 C13 H13 119.0 . . ? C13 C14 C15 115.9(6) . . ? C13 C14 C21 122.1(7) . . ? C15 C14 C21 122.0(7) . . ? C16 C15 C14 127.0(7) . . ? C16 C15 H15 116.5 . . ? C14 C15 H15 116.5 . . ? C15 C16 C11 116.0(6) . . ? C15 C16 C25 121.4(6) . . ? C11 C16 C25 122.6(5) . . ? N1 C17 C12 128.9(6) . . ? N1 C17 H17 115.6 . . ? C12 C17 H17 115.6 . . ? N1 C18 C19 113.4(6) . . ? N1 C18 C20 109.9(6) . . ? C19 C18 C20 112.2(7) . . ? N1 C18 H18 107.0 . . ? C19 C18 H18 107.0 . . ? C20 C18 H18 107.0 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22A C21 C23B 127.2(18) . . ? C22A C21 C24A 110.8(11) . . ? C23B C21 C24A 62.8(16) . . ? C22A C21 C14 114.0(9) . . ? C23B C21 C14 116.9(16) . . ? C24A C21 C14 110.1(9) . . ? C22A C21 C23A 111.1(11) . . ? C23B C21 C23A 39.0(15) . . ? C24A C21 C23A 101.7(10) . . ? C14 C21 C23A 108.5(8) . . ? C22A C21 C22B 27.8(12) . . ? C23B C21 C22B 119(2) . . ? C24A C21 C22B 134.7(16) . . ? C14 C21 C22B 107.5(14) . . ? C23A C21 C22B 89.4(15) . . ? C22A C21 C24B 76.5(16) . . ? C23B C21 C24B 104(2) . . ? C24A C21 C24B 42.8(14) . . ? C14 C21 C24B 103.3(14) . . ? C23A C21 C24B 139.6(16) . . ? C22B C21 C24B 104.3(19) . . ? C26 C25 C16 111.1(6) . . ? C26 C25 C27 108.0(6) . . ? C16 C25 C27 111.0(5) . . ? C26 C25 C28 106.9(6) . . ? C16 C25 C28 112.1(5) . . ? C27 C25 C28 107.6(6) . . ? C25 C26 C31 111.2(6) . . ? C25 C26 H26A 109.4 . . ? C31 C26 H26A 109.4 . . ? C25 C26 H26B 109.4 . . ? C31 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? C25 C27 C30 110.5(6) . . ? C25 C27 H27A 109.6 . . ? C30 C27 H27A 109.6 . . ? C25 C27 H27B 109.6 . . ? C30 C27 H27B 109.6 . . ? H27A C27 H27B 108.1 . . ? C29 C28 C25 111.5(6) . . ? C29 C28 H28A 109.3 . . ? C25 C28 H28A 109.3 . . ? C29 C28 H28B 109.3 . . ? C25 C28 H28B 109.3 . . ? H28A C28 H28B 108.0 . . ? C35 C29 C33 110.0(7) . . ? C35 C29 C28 111.1(7) . . ? C33 C29 C28 110.8(8) . . ? C35 C29 H29 108.2 . . ? C33 C29 H29 108.2 . . ? C28 C29 H29 108.2 . . ? C32 C30 C35 108.4(7) . . ? C32 C30 C27 109.9(7) . . ? C35 C30 C27 110.5(7) . . ? C32 C30 H30 109.3 . . ? C35 C30 H30 109.3 . . ? C27 C30 H30 109.3 . . ? C32 C31 C26 109.5(6) . . ? C32 C31 C33 106.8(7) . . ? C26 C31 C33 111.2(7) . . ? C32 C31 H31 109.7 . . ? C26 C31 H31 109.7 . . ? C33 C31 H31 109.7 . . ? C30 C32 C31 110.4(7) . . ? C30 C32 H32A 109.6 . . ? C31 C32 H32A 109.6 . . ? C30 C32 H32B 109.6 . . ? C31 C32 H32B 109.6 . . ? H32A C32 H32B 108.1 . . ? C29 C33 C31 107.6(7) . . ? C29 C33 H33A 110.2 . . ? C31 C33 H33A 110.2 . . ? C29 C33 H33B 110.2 . . ? C31 C33 H33B 110.2 . . ? H33A C33 H33B 108.5 . . ? C29 C35 C30 108.1(7) . . ? C29 C35 H35A 110.1 . . ? C30 C35 H35A 110.1 . . ? C29 C35 H35B 110.1 . . ? C30 C35 H35B 110.1 . . ? H35A C35 H35B 108.4 . . ? O1 Cr1 N1 91.5(2) . . ? O1 Cr1 C2 92.8(2) . . ? N1 Cr1 C2 152.6(3) . . ? O1 Cr1 C3 93.5(2) . . ? N1 Cr1 C3 115.6(3) . . ? C2 Cr1 C3 37.1(3) . . ? O1 Cr1 C4 126.1(3) . . ? N1 Cr1 C4 95.6(2) . . ? C2 Cr1 C4 60.5(3) . . ? C3 Cr1 C4 36.6(3) . . ? O1 Cr1 C1 123.4(2) . . ? N1 Cr1 C1 144.7(2) . . ? C2 Cr1 C1 36.4(3) . . ? C3 Cr1 C1 61.8(3) . . ? C4 Cr1 C1 60.7(3) . . ? O1 Cr1 C5 152.6(2) . . ? N1 Cr1 C5 108.5(2) . . ? C2 Cr1 C5 60.9(3) . . ? C3 Cr1 C5 61.3(3) . . ? C4 Cr1 C5 35.8(3) . . ? C1 Cr1 C5 37.1(3) . . ? O1 Cr1 Cl1 97.51(17) . . ? N1 Cr1 Cl1 92.31(16) . . ? C2 Cr1 Cl1 113.9(2) . . ? C3 Cr1 Cl1 149.7(2) . . ? C4 Cr1 Cl1 135.2(2) . . ? C1 Cr1 Cl1 88.8(2) . . ? C5 Cr1 Cl1 100.2(2) . . ? C17 N1 C18 116.0(6) . . ? C17 N1 Cr1 122.8(5) . . ? C18 N1 Cr1 120.6(4) . . ? C11 O1 Cr1 130.8(4) . . ? C21 C22A H22A 109.5 . . ? C21 C22A H22B 109.5 . . ? C21 C22A H22C 109.5 . . ? C21 C23A H23A 109.5 . . ? C21 C23A H23B 109.5 . . ? C21 C23A H23C 109.5 . . ? C21 C24A H24A 109.5 . . ? C21 C24A H24B 109.5 . . ? C21 C24A H24C 109.5 . . ? C21 C22B H22D 109.5 . . ? C21 C22B H22E 109.5 . . ? H22D C22B H22E 109.5 . . ? C21 C22B H22F 109.5 . . ? H22D C22B H22F 109.5 . . ? H22E C22B H22F 109.5 . . ? C21 C23B H23D 109.5 . . ? C21 C23B H23E 109.5 . . ? H23D C23B H23E 109.5 . . ? C21 C23B H23F 109.5 . . ? H23D C23B H23F 109.5 . . ? H23E C23B H23F 109.5 . . ? C21 C24B H24D 109.5 . . ? C21 C24B H24E 109.5 . . ? H24D C24B H24E 109.5 . . ? C21 C24B H24F 109.5 . . ? H24D C24B H24F 109.5 . . ? H24E C24B H24F 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 C5 C1 C2 C3 -0.7(8) . . . . ? C6 C1 C2 C3 -177.2(7) . . . . ? Cr1 C1 C2 C3 62.4(5) . . . . ? C5 C1 C2 C7 177.7(7) . . . . ? C6 C1 C2 C7 1.1(12) . . . . ? Cr1 C1 C2 C7 -119.3(8) . . . . ? C5 C1 C2 Cr1 -63.1(5) . . . . ? C6 C1 C2 Cr1 120.4(8) . . . . ? C1 C2 C3 C4 1.6(8) . . . . ? C7 C2 C3 C4 -176.8(7) . . . . ? Cr1 C2 C3 C4 64.7(5) . . . . ? C1 C2 C3 C8 -179.9(7) . . . . ? C7 C2 C3 C8 1.7(12) . . . . ? Cr1 C2 C3 C8 -116.8(8) . . . . ? C1 C2 C3 Cr1 -63.1(5) . . . . ? C7 C2 C3 Cr1 118.5(7) . . . . ? C2 C3 C4 C5 -1.9(8) . . . . ? C8 C3 C4 C5 179.6(8) . . . . ? Cr1 C3 C4 C5 62.1(5) . . . . ? C2 C3 C4 C9 171.3(7) . . . . ? C8 C3 C4 C9 -7.2(12) . . . . ? Cr1 C3 C4 C9 -124.8(7) . . . . ? C2 C3 C4 Cr1 -64.0(5) . . . . ? C8 C3 C4 Cr1 117.5(8) . . . . ? C3 C4 C5 C1 1.5(8) . . . . ? C9 C4 C5 C1 -171.5(7) . . . . ? Cr1 C4 C5 C1 62.8(5) . . . . ? C3 C4 C5 C10 177.4(7) . . . . ? C9 C4 C5 C10 4.4(12) . . . . ? Cr1 C4 C5 C10 -121.3(8) . . . . ? C3 C4 C5 Cr1 -61.3(5) . . . . ? C9 C4 C5 Cr1 125.7(8) . . . . ? C2 C1 C5 C4 -0.5(8) . . . . ? C6 C1 C5 C4 176.0(7) . . . . ? Cr1 C1 C5 C4 -63.2(5) . . . . ? C2 C1 C5 C10 -176.6(7) . . . . ? C6 C1 C5 C10 -0.2(12) . . . . ? Cr1 C1 C5 C10 120.7(7) . . . . ? C2 C1 C5 Cr1 62.7(5) . . . . ? C6 C1 C5 Cr1 -120.8(8) . . . . ? O1 C11 C12 C13 177.9(6) . . . . ? C16 C11 C12 C13 -0.3(10) . . . . ? O1 C11 C12 C17 -5.8(10) . . . . ? C16 C11 C12 C17 176.1(6) . . . . ? C11 C12 C13 C14 -1.2(11) . . . . ? C17 C12 C13 C14 -177.8(7) . . . . ? C12 C13 C14 C15 1.3(11) . . . . ? C12 C13 C14 C21 179.5(7) . . . . ? C13 C14 C15 C16 0.1(12) . . . . ? C21 C14 C15 C16 -178.1(7) . . . . ? C14 C15 C16 C11 -1.5(11) . . . . ? C14 C15 C16 C25 176.4(7) . . . . ? O1 C11 C16 C15 -176.7(6) . . . . ? C12 C11 C16 C15 1.5(9) . . . . ? O1 C11 C16 C25 5.5(10) . . . . ? C12 C11 C16 C25 -176.3(6) . . . . ? C13 C12 C17 N1 177.2(7) . . . . ? C11 C12 C17 N1 0.6(11) . . . . ? C13 C14 C21 C22A 4.6(14) . . . . ? C15 C14 C21 C22A -177.3(10) . . . . ? C13 C14 C21 C23B 170.5(19) . . . . ? C15 C14 C21 C23B -11(2) . . . . ? C13 C14 C21 C24A -120.6(11) . . . . ? C15 C14 C21 C24A 57.5(12) . . . . ? C13 C14 C21 C23A 128.9(10) . . . . ? C15 C14 C21 C23A -53.0(12) . . . . ? C13 C14 C21 C22B 33.6(17) . . . . ? C15 C14 C21 C22B -148.4(15) . . . . ? C13 C14 C21 C24B -76.4(17) . . . . ? C15 C14 C21 C24B 101.7(17) . . . . ? C15 C16 C25 C26 119.0(7) . . . . ? C11 C16 C25 C26 -63.3(8) . . . . ? C15 C16 C25 C27 -120.9(7) . . . . ? C11 C16 C25 C27 56.8(8) . . . . ? C15 C16 C25 C28 -0.5(9) . . . . ? C11 C16 C25 C28 177.2(6) . . . . ? C16 C25 C26 C31 -179.7(6) . . . . ? C27 C25 C26 C31 58.4(7) . . . . ? C28 C25 C26 C31 -57.1(8) . . . . ? C26 C25 C27 C30 -58.4(8) . . . . ? C16 C25 C27 C30 179.6(6) . . . . ? C28 C25 C27 C30 56.6(8) . . . . ? C26 C25 C28 C29 58.8(9) . . . . ? C16 C25 C28 C29 -179.2(7) . . . . ? C27 C25 C28 C29 -56.9(9) . . . . ? C25 C28 C29 C35 60.5(9) . . . . ? C25 C28 C29 C33 -62.2(9) . . . . ? C25 C27 C30 C32 59.8(9) . . . . ? C25 C27 C30 C35 -59.8(9) . . . . ? C25 C26 C31 C32 -58.9(8) . . . . ? C25 C26 C31 C33 59.0(8) . . . . ? C35 C30 C32 C31 61.6(9) . . . . ? C27 C30 C32 C31 -59.3(9) . . . . ? C26 C31 C32 C30 58.6(9) . . . . ? C33 C31 C32 C30 -62.0(8) . . . . ? C35 C29 C33 C31 -64.2(9) . . . . ? C28 C29 C33 C31 59.1(9) . . . . ? C32 C31 C33 C29 61.6(9) . . . . ? C26 C31 C33 C29 -57.8(9) . . . . ? C33 C29 C35 C30 63.2(9) . . . . ? C28 C29 C35 C30 -60.0(9) . . . . ? C32 C30 C35 C29 -60.6(9) . . . . ? C27 C30 C35 C29 59.9(9) . . . . ? C1 C2 Cr1 O1 -149.7(4) . . . . ? C3 C2 Cr1 O1 92.1(4) . . . . ? C7 C2 Cr1 O1 -28.5(8) . . . . ? C1 C2 Cr1 N1 111.8(6) . . . . ? C3 C2 Cr1 N1 -6.4(8) . . . . ? C7 C2 Cr1 N1 -127.0(8) . . . . ? C1 C2 Cr1 C3 118.3(6) . . . . ? C7 C2 Cr1 C3 -120.6(9) . . . . ? C1 C2 Cr1 C4 79.7(5) . . . . ? C3 C2 Cr1 C4 -38.6(4) . . . . ? C7 C2 Cr1 C4 -159.1(9) . . . . ? C3 C2 Cr1 C1 -118.3(6) . . . . ? C7 C2 Cr1 C1 121.2(10) . . . . ? C1 C2 Cr1 C5 38.4(4) . . . . ? C3 C2 Cr1 C5 -79.9(5) . . . . ? C7 C2 Cr1 C5 159.6(9) . . . . ? C1 C2 Cr1 Cl1 -50.2(5) . . . . ? C3 C2 Cr1 Cl1 -168.4(4) . . . . ? C7 C2 Cr1 Cl1 71.0(8) . . . . ? C4 C3 Cr1 O1 155.6(4) . . . . ? C2 C3 Cr1 O1 -90.0(4) . . . . ? C8 C3 Cr1 O1 31.8(8) . . . . ? C4 C3 Cr1 N1 62.3(5) . . . . ? C2 C3 Cr1 N1 176.7(4) . . . . ? C8 C3 Cr1 N1 -61.5(8) . . . . ? C4 C3 Cr1 C2 -114.4(6) . . . . ? C8 C3 Cr1 C2 121.8(9) . . . . ? C2 C3 Cr1 C4 114.4(6) . . . . ? C8 C3 Cr1 C4 -123.8(10) . . . . ? C4 C3 Cr1 C1 -78.0(5) . . . . ? C2 C3 Cr1 C1 36.4(4) . . . . ? C8 C3 Cr1 C1 158.1(8) . . . . ? C4 C3 Cr1 C5 -35.6(4) . . . . ? C2 C3 Cr1 C5 78.8(5) . . . . ? C8 C3 Cr1 C5 -159.4(9) . . . . ? C4 C3 Cr1 Cl1 -93.1(6) . . . . ? C2 C3 Cr1 Cl1 21.3(7) . . . . ? C8 C3 Cr1 Cl1 143.1(6) . . . . ? C5 C4 Cr1 O1 -150.0(4) . . . . ? C3 C4 Cr1 O1 -30.7(5) . . . . ? C9 C4 Cr1 O1 87.8(9) . . . . ? C5 C4 Cr1 N1 114.0(4) . . . . ? C3 C4 Cr1 N1 -126.6(4) . . . . ? C9 C4 Cr1 N1 -8.1(8) . . . . ? C5 C4 Cr1 C2 -80.2(5) . . . . ? C3 C4 Cr1 C2 39.1(4) . . . . ? C9 C4 Cr1 C2 157.6(9) . . . . ? C5 C4 Cr1 C3 -119.3(6) . . . . ? C9 C4 Cr1 C3 118.5(10) . . . . ? C5 C4 Cr1 C1 -38.2(4) . . . . ? C3 C4 Cr1 C1 81.1(5) . . . . ? C9 C4 Cr1 C1 -160.4(9) . . . . ? C3 C4 Cr1 C5 119.3(6) . . . . ? C9 C4 Cr1 C5 -122.2(10) . . . . ? C5 C4 Cr1 Cl1 15.0(6) . . . . ? C3 C4 Cr1 Cl1 134.3(4) . . . . ? C9 C4 Cr1 Cl1 -107.1(8) . . . . ? C2 C1 Cr1 O1 37.2(5) . . . . ? C5 C1 Cr1 O1 153.0(4) . . . . ? C6 C1 Cr1 O1 -83.5(8) . . . . ? C2 C1 Cr1 N1 -132.3(5) . . . . ? C5 C1 Cr1 N1 -16.4(7) . . . . ? C6 C1 Cr1 N1 107.0(7) . . . . ? C5 C1 Cr1 C2 115.9(6) . . . . ? C6 C1 Cr1 C2 -120.7(9) . . . . ? C2 C1 Cr1 C3 -37.1(5) . . . . ? C5 C1 Cr1 C3 78.8(5) . . . . ? C6 C1 Cr1 C3 -157.8(8) . . . . ? C2 C1 Cr1 C4 -79.0(5) . . . . ? C5 C1 Cr1 C4 36.9(4) . . . . ? C6 C1 Cr1 C4 160.3(8) . . . . ? C2 C1 Cr1 C5 -115.9(6) . . . . ? C6 C1 Cr1 C5 123.4(9) . . . . ? C2 C1 Cr1 Cl1 135.4(4) . . . . ? C5 C1 Cr1 Cl1 -108.7(4) . . . . ? C6 C1 Cr1 Cl1 14.7(7) . . . . ? C4 C5 Cr1 O1 61.2(7) . . . . ? C1 C5 Cr1 O1 -55.3(7) . . . . ? C10 C5 Cr1 O1 -173.4(6) . . . . ? C4 C5 Cr1 N1 -73.4(5) . . . . ? C1 C5 Cr1 N1 170.1(4) . . . . ? C10 C5 Cr1 N1 52.0(7) . . . . ? C4 C5 Cr1 C2 78.9(5) . . . . ? C1 C5 Cr1 C2 -37.6(4) . . . . ? C10 C5 Cr1 C2 -155.7(8) . . . . ? C4 C5 Cr1 C3 36.3(4) . . . . ? C1 C5 Cr1 C3 -80.2(5) . . . . ? C10 C5 Cr1 C3 161.7(8) . . . . ? C1 C5 Cr1 C4 -116.5(6) . . . . ? C10 C5 Cr1 C4 125.4(9) . . . . ? C4 C5 Cr1 C1 116.5(6) . . . . ? C10 C5 Cr1 C1 -118.1(9) . . . . ? C4 C5 Cr1 Cl1 -169.3(4) . . . . ? C1 C5 Cr1 Cl1 74.2(4) . . . . ? C10 C5 Cr1 Cl1 -43.9(7) . . . . ? C12 C17 N1 C18 -174.9(7) . . . . ? C12 C17 N1 Cr1 -3.6(10) . . . . ? C19 C18 N1 C17 -50.5(9) . . . . ? C20 C18 N1 C17 76.0(8) . . . . ? C19 C18 N1 Cr1 138.0(6) . . . . ? C20 C18 N1 Cr1 -95.5(7) . . . . ? O1 Cr1 N1 C17 7.8(6) . . . . ? C2 Cr1 N1 C17 106.7(7) . . . . ? C3 Cr1 N1 C17 102.4(6) . . . . ? C4 Cr1 N1 C17 134.4(6) . . . . ? C1 Cr1 N1 C17 179.0(5) . . . . ? C5 Cr1 N1 C17 168.7(5) . . . . ? Cl1 Cr1 N1 C17 -89.7(5) . . . . ? O1 Cr1 N1 C18 178.7(5) . . . . ? C2 Cr1 N1 C18 -82.5(7) . . . . ? C3 Cr1 N1 C18 -86.7(5) . . . . ? C4 Cr1 N1 C18 -54.7(5) . . . . ? C1 Cr1 N1 C18 -10.1(7) . . . . ? C5 Cr1 N1 C18 -20.4(5) . . . . ? Cl1 Cr1 N1 C18 81.1(5) . . . . ? C12 C11 O1 Cr1 14.8(9) . . . . ? C16 C11 O1 Cr1 -167.1(5) . . . . ? N1 Cr1 O1 C11 -14.0(6) . . . . ? C2 Cr1 O1 C11 -166.9(6) . . . . ? C3 Cr1 O1 C11 -129.8(6) . . . . ? C4 Cr1 O1 C11 -112.1(6) . . . . ? C1 Cr1 O1 C11 172.0(5) . . . . ? C5 Cr1 O1 C11 -151.5(6) . . . . ? Cl1 Cr1 O1 C11 78.5(6) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.601 _refine_diff_density_min -0.448 _refine_diff_density_rms 0.106 #===END