# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1988 data_str548 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C12 H12 Cr O6' _chemical_formula_weight 304.22 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cr' 'Cr' 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M R3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' _cell_length_a 12.698(2) _cell_length_b 12.698(2) _cell_length_c 6.8580(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 957.6(3) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 22 _cell_measurement_theta_max 28 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.62 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.48 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.583 _exptl_crystal_density_method ? _exptl_crystal_F_000 468 _exptl_absorpt_coefficient_mu 0.915 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nicolet R3mV' _diffrn_measurement_method w-2t _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 432 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0087 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 25.04 _reflns_number_total 432 _reflns_number_observed 427 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Nicolet R3' _computing_cell_refinement 'Nicolet R3' _computing_data_reduction XDISK _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics XP _computing_publication_material CIFTAB _refine_special_details ; Refinement on F^2^ for ALL reflections except for 4 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0407P)^2^+1.0644P] 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 fixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(4) _refine_ls_number_reflns 428 _refine_ls_number_parameters 58 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0239 _refine_ls_R_factor_obs 0.0231 _refine_ls_wR_factor_all 0.0653 _refine_ls_wR_factor_obs 0.0586 _refine_ls_goodness_of_fit_all 1.026 _refine_ls_goodness_of_fit_obs 1.027 _refine_ls_restrained_S_all 1.137 _refine_ls_restrained_S_obs 1.026 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cr Cr 0.0000 0.0000 0.04602(4) 0.0289(2) Uani 1 d S . C1 C -0.0943(4) 0.0378(4) 0.2020(5) 0.0445(9) Uani 1 d . . C2 C 0.0681(3) 0.1278(3) -0.2048(4) 0.0311(6) Uani 1 d . . C3 C 0.1283(3) 0.0591(3) -0.2050(4) 0.0303(6) Uani 1 d . . C4 C 0.2653(3) 0.1259(3) -0.2147(5) 0.0393(7) Uani 1 d . . O1 O -0.1540(3) 0.0626(3) 0.2959(5) 0.0718(9) Uani 1 d . . O2 O 0.3166(2) 0.0533(3) -0.1681(4) 0.0472(6) Uani 1 d . . H1 H 0.1346 0.2280 -0.1828 0.080 Uiso 1 d . . H2 H 0.2918 0.1872 -0.1169 0.080 Uiso 1 d . . H3 H 0.2832 0.1552 -0.3509 0.080 Uiso 1 d . . H4 H 0.3171 0.0102 -0.2687 0.080 Uiso 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 Cr 0.0312(3) 0.0312(3) 0.0244(4) 0.000 0.000 0.01561(13) C1 0.049(2) 0.051(2) 0.034(2) 0.001(2) 0.007(2) 0.026(2) C2 0.034(2) 0.029(2) 0.0275(15) 0.0010(12) 0.0017(13) 0.0139(13) C3 0.0299(15) 0.035(2) 0.0254(13) 0.0005(12) -0.0003(11) 0.0157(13) C4 0.029(2) 0.044(2) 0.041(2) -0.0015(14) 0.0006(13) 0.0154(14) O1 0.085(2) 0.093(2) 0.059(2) -0.004(2) 0.022(2) 0.061(2) O2 0.0394(13) 0.068(2) 0.0442(12) -0.0094(12) -0.0085(10) 0.0340(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr C1 1.839(4) 3 ? Cr C1 1.839(4) . yes Cr C1 1.839(4) 2 ? Cr C2 2.222(3) 2 ? Cr C2 2.222(3) 3 ? Cr C2 2.222(3) . yes Cr C3 2.227(3) 3 ? Cr C3 2.227(3) 2 ? Cr C3 2.227(3) . yes C1 O1 1.152(5) . yes C2 C3 1.400(5) 2 ? C2 C3 1.419(5) . yes C3 C2 1.400(5) 3 ? C3 C4 1.508(4) . yes C4 O2 1.406(5) . yes 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 C1 Cr C1 89.6(2) 3 . ? C1 Cr C1 89.6(2) 3 2 ? C1 Cr C1 89.6(2) . 2 ? C1 Cr C2 160.93(14) 3 2 ? C1 Cr C2 94.6(2) . 2 ? C1 Cr C2 109.01(15) 2 2 ? C1 Cr C2 109.01(15) 3 3 ? C1 Cr C2 160.93(14) . 3 ? C1 Cr C2 94.6(2) 2 3 ? C2 Cr C2 66.50(12) 2 3 ? C1 Cr C2 94.6(2) 3 . ? C1 Cr C2 109.01(15) . . ? C1 Cr C2 160.93(14) 2 . ? C2 Cr C2 66.50(12) 2 . ? C2 Cr C2 66.50(12) 3 . ? C1 Cr C3 145.46(15) 3 3 ? C1 Cr C3 124.8(2) . 3 ? C1 Cr C3 87.40(14) 2 3 ? C2 Cr C3 36.68(12) 2 3 ? C2 Cr C3 37.21(12) 3 3 ? C2 Cr C3 78.65(11) . 3 ? C1 Cr C3 124.8(2) 3 2 ? C1 Cr C3 87.40(14) . 2 ? C1 Cr C3 145.46(15) 2 2 ? C2 Cr C3 37.21(12) 2 2 ? C2 Cr C3 78.65(11) 3 2 ? C2 Cr C3 36.68(12) . 2 ? C3 Cr C3 66.64(12) 3 2 ? C1 Cr C3 87.40(14) 3 . ? C1 Cr C3 145.46(15) . . ? C1 Cr C3 124.8(2) 2 . ? C2 Cr C3 78.65(11) 2 . ? C2 Cr C3 36.68(12) 3 . ? C2 Cr C3 37.21(12) . . ? C3 Cr C3 66.64(12) 3 . ? C3 Cr C3 66.64(12) 2 . ? O1 C1 Cr 178.4(4) . . ? C3 C2 C3 120.4(3) 2 . ? C3 C2 Cr 71.8(2) 2 . ? C3 C2 Cr 71.6(2) . . ? C2 C3 C2 119.6(3) 3 . ? C2 C3 C4 121.7(3) 3 . ? C2 C3 C4 118.6(3) . . ? C2 C3 Cr 71.5(2) 3 . ? C2 C3 Cr 71.2(2) . . ? C4 C3 Cr 131.9(2) . . ? O2 C4 C3 113.8(3) . . ? _refine_diff_density_max 0.459 _refine_diff_density_min -0.169 _refine_diff_density_rms 0.040 data_crbr2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H8 Br2 Cr O3' _chemical_formula_weight 399.99 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cr' 'Cr' 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 10.0413(3) _cell_length_b 12.5369(6) _cell_length_c 10.7044(5) _cell_angle_alpha 90.00 _cell_angle_beta 105.026(2) _cell_angle_gamma 90.00 _cell_volume 1301.47(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.041 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 7.010 _exptl_absorpt_correction_type Scalepack _exptl_absorpt_correction_T_min 0.3345 _exptl_absorpt_correction_T_max 0.5407 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '2o phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number n/a _diffrn_standards_interval_count n/a _diffrn_standards_interval_time n/a _diffrn_standards_decay_% 0 _diffrn_reflns_number 11366 _diffrn_reflns_av_R_equivalents 0.0577 _diffrn_reflns_av_sigmaI/netI 0.0649 _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 -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.80 _diffrn_reflns_theta_max 26.00 _reflns_number_total 2537 _reflns_number_gt 2249 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics RES2INS _computing_publication_material ? _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^)+(0.0468P)^2^+1.2809P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0045(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2537 _refine_ls_number_parameters 155 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0442 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.1009 _refine_ls_wR_factor_gt 0.0976 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _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 Br1 Br 1.35821(4) 0.54265(4) -0.13398(4) 0.02695(17) Uani 1 1 d . . . Br2 Br 0.93437(4) 0.21776(3) 0.15486(4) 0.02210(16) Uani 1 1 d . . . Cr1 Cr 0.91929(6) 0.33416(5) -0.29805(5) 0.01271(18) Uani 1 1 d . . . O1 O 0.7560(3) 0.1312(3) -0.3623(3) 0.0292(7) Uani 1 1 d . . . O2 O 0.6821(3) 0.4650(2) -0.4502(3) 0.0286(7) Uani 1 1 d . . . O3 O 1.0141(3) 0.3077(3) -0.5406(3) 0.0341(8) Uani 1 1 d . . . C1 C 0.8171(4) 0.2100(3) -0.3393(4) 0.0177(8) Uani 1 1 d . . . C2 C 0.7717(4) 0.4142(3) -0.3911(4) 0.0179(8) Uani 1 1 d . . . C3 C 0.9767(4) 0.3181(4) -0.4473(4) 0.0235(9) Uani 1 1 d . . . C4 C 0.9917(4) 0.4727(3) -0.1703(4) 0.0154(7) Uani 1 1 d . . . H4 H 0.9707 0.5462 -0.1854 0.018 Uiso 1 1 calc R . . C5 C 0.9073(4) 0.4082(3) -0.1127(3) 0.0168(8) Uani 1 1 d . . . H5 H 0.8309 0.4391 -0.0890 0.020 Uiso 1 1 calc R . . C6 C 0.9361(4) 0.2998(3) -0.0909(3) 0.0162(8) Uani 1 1 d . . . C7 C 1.0517(4) 0.2545(3) -0.1269(3) 0.0148(7) Uani 1 1 d . . . H7 H 1.0717 0.1807 -0.1128 0.018 Uiso 1 1 calc R . . C8 C 1.1348(4) 0.3176(3) -0.1823(3) 0.0151(7) Uani 1 1 d . . . H8 H 1.2117 0.2867 -0.2051 0.018 Uiso 1 1 calc R . . C9 C 1.1057(4) 0.4290(3) -0.2053(3) 0.0154(7) Uani 1 1 d . . . C10 C 1.1935(4) 0.4967(3) -0.2672(4) 0.0211(8) Uani 1 1 d . . . H10A H 1.1406 0.5599 -0.3081 0.025 Uiso 1 1 calc R . . H10B H 1.2213 0.4555 -0.3351 0.025 Uiso 1 1 calc R . . C11 C 0.8473(4) 0.2312(3) -0.0322(4) 0.0218(8) Uani 1 1 d . . . H11A H 0.8367 0.1599 -0.0732 0.026 Uiso 1 1 calc R . . H11B H 0.7546 0.2636 -0.0462 0.026 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 Br1 0.0207(2) 0.0310(3) 0.0284(3) -0.00054(17) 0.00493(18) -0.00932(16) Br2 0.0266(3) 0.0268(3) 0.0160(2) 0.00342(15) 0.01103(17) -0.00222(15) Cr1 0.0147(3) 0.0143(3) 0.0092(3) -0.0009(2) 0.0031(2) 0.0004(2) O1 0.0331(16) 0.0256(16) 0.0261(16) -0.0029(13) 0.0026(13) -0.0077(14) O2 0.0272(15) 0.0233(16) 0.0288(16) 0.0025(12) -0.0044(13) 0.0044(13) O3 0.0344(17) 0.059(2) 0.0116(14) 0.0022(14) 0.0107(12) 0.0121(16) C1 0.0220(18) 0.0168(19) 0.0142(18) 0.0013(14) 0.0045(15) 0.0004(15) C2 0.0243(19) 0.0161(19) 0.0134(17) -0.0026(14) 0.0053(15) -0.0043(16) C3 0.0222(19) 0.027(2) 0.0193(19) 0.0036(17) 0.0006(15) 0.0048(17) C4 0.0194(18) 0.0155(17) 0.0115(17) -0.0029(14) 0.0046(14) -0.0009(15) C5 0.0183(17) 0.019(2) 0.0127(17) -0.0053(14) 0.0044(14) -0.0023(15) C6 0.0179(17) 0.0208(19) 0.0101(17) -0.0015(14) 0.0039(14) -0.0019(15) C7 0.0171(17) 0.0156(18) 0.0098(16) 0.0000(14) -0.0001(14) 0.0020(15) C8 0.0147(16) 0.0202(18) 0.0099(16) -0.0013(14) 0.0021(13) -0.0001(15) C9 0.0155(17) 0.0201(19) 0.0098(16) -0.0002(14) 0.0019(13) -0.0053(15) C10 0.0194(18) 0.029(2) 0.0149(19) 0.0029(16) 0.0050(15) -0.0010(16) C11 0.024(2) 0.026(2) 0.0144(18) -0.0011(16) 0.0049(15) -0.0048(17) _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 Br1 C10 1.969(4) . ? Br2 C11 1.973(4) . ? Cr1 C3 1.845(4) . ? Cr1 C2 1.853(4) . ? Cr1 C1 1.854(4) . ? Cr1 C7 2.204(4) . ? Cr1 C8 2.208(4) . ? Cr1 C4 2.213(4) . ? Cr1 C6 2.222(4) . ? Cr1 C5 2.222(4) . ? Cr1 C9 2.222(4) . ? O1 C1 1.155(5) . ? O2 C2 1.149(5) . ? O3 C3 1.162(5) . ? C4 C9 1.405(5) . ? C4 C5 1.422(5) . ? C5 C6 1.397(6) . ? C6 C7 1.432(5) . ? C6 C11 1.490(5) . ? C7 C8 1.390(5) . ? C8 C9 1.434(5) . ? C9 C10 1.497(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Cr1 C2 88.85(17) . . ? C3 Cr1 C1 88.88(19) . . ? C2 Cr1 C1 90.61(17) . . ? C3 Cr1 C7 114.45(16) . . ? C2 Cr1 C7 156.70(16) . . ? C1 Cr1 C7 89.71(16) . . ? C3 Cr1 C8 89.70(16) . . ? C2 Cr1 C8 152.16(16) . . ? C1 Cr1 C8 117.16(16) . . ? C7 Cr1 C8 36.72(14) . . ? C3 Cr1 C4 119.60(17) . . ? C2 Cr1 C4 89.74(15) . . ? C1 Cr1 C4 151.52(15) . . ? C7 Cr1 C4 79.13(14) . . ? C8 Cr1 C4 67.03(14) . . ? C3 Cr1 C6 152.04(16) . . ? C2 Cr1 C6 118.99(15) . . ? C1 Cr1 C6 88.23(15) . . ? C7 Cr1 C6 37.74(14) . . ? C8 Cr1 C6 67.15(13) . . ? C4 Cr1 C6 66.92(14) . . ? C3 Cr1 C5 156.97(17) . . ? C2 Cr1 C5 91.84(15) . . ? C1 Cr1 C5 114.13(16) . . ? C7 Cr1 C5 66.92(14) . . ? C8 Cr1 C5 79.07(14) . . ? C4 Cr1 C5 37.41(13) . . ? C6 Cr1 C5 36.65(14) . . ? C3 Cr1 C9 91.67(16) . . ? C2 Cr1 C9 114.48(16) . . ? C1 Cr1 C9 154.92(16) . . ? C7 Cr1 C9 67.30(14) . . ? C8 Cr1 C9 37.79(14) . . ? C4 Cr1 C9 36.92(14) . . ? C6 Cr1 C9 79.65(14) . . ? C5 Cr1 C9 67.16(14) . . ? O1 C1 Cr1 178.1(4) . . ? O2 C2 Cr1 178.4(4) . . ? O3 C3 Cr1 179.4(4) . . ? C9 C4 C5 120.8(4) . . ? C9 C4 Cr1 71.9(2) . . ? C5 C4 Cr1 71.6(2) . . ? C6 C5 C4 120.3(3) . . ? C6 C5 Cr1 71.7(2) . . ? C4 C5 Cr1 71.0(2) . . ? C5 C6 C7 119.2(4) . . ? C5 C6 C11 120.8(4) . . ? C7 C6 C11 120.0(4) . . ? C5 C6 Cr1 71.6(2) . . ? C7 C6 Cr1 70.4(2) . . ? C11 C6 Cr1 129.3(3) . . ? C8 C7 C6 120.5(4) . . ? C8 C7 Cr1 71.8(2) . . ? C6 C7 Cr1 71.8(2) . . ? C7 C8 C9 120.6(3) . . ? C7 C8 Cr1 71.5(2) . . ? C9 C8 Cr1 71.7(2) . . ? C4 C9 C8 118.6(3) . . ? C4 C9 C10 120.7(4) . . ? C8 C9 C10 120.7(3) . . ? C4 C9 Cr1 71.2(2) . . ? C8 C9 Cr1 70.6(2) . . ? C10 C9 Cr1 129.0(2) . . ? C9 C10 Br1 109.0(3) . . ? C6 C11 Br2 108.7(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 Cr1 C1 O1 107(12) . . . . ? C2 Cr1 C1 O1 -164(12) . . . . ? C7 Cr1 C1 O1 -8(12) . . . . ? C8 Cr1 C1 O1 18(12) . . . . ? C4 Cr1 C1 O1 -74(12) . . . . ? C6 Cr1 C1 O1 -45(12) . . . . ? C5 Cr1 C1 O1 -72(12) . . . . ? C9 Cr1 C1 O1 15(12) . . . . ? C3 Cr1 C2 O2 -40(13) . . . . ? C1 Cr1 C2 O2 -129(13) . . . . ? C7 Cr1 C2 O2 140(13) . . . . ? C8 Cr1 C2 O2 47(13) . . . . ? C4 Cr1 C2 O2 79(13) . . . . ? C6 Cr1 C2 O2 143(13) . . . . ? C5 Cr1 C2 O2 117(13) . . . . ? C9 Cr1 C2 O2 51(13) . . . . ? C2 Cr1 C3 O3 168(100) . . . . ? C1 Cr1 C3 O3 -101(41) . . . . ? C7 Cr1 C3 O3 -12(41) . . . . ? C8 Cr1 C3 O3 16(41) . . . . ? C4 Cr1 C3 O3 79(41) . . . . ? C6 Cr1 C3 O3 -17(41) . . . . ? C5 Cr1 C3 O3 76(41) . . . . ? C9 Cr1 C3 O3 54(41) . . . . ? C3 Cr1 C4 C9 -45.5(3) . . . . ? C2 Cr1 C4 C9 -134.1(2) . . . . ? C1 Cr1 C4 C9 135.1(3) . . . . ? C7 Cr1 C4 C9 66.5(2) . . . . ? C8 Cr1 C4 C9 30.1(2) . . . . ? C6 Cr1 C4 C9 104.0(2) . . . . ? C5 Cr1 C4 C9 132.6(3) . . . . ? C3 Cr1 C4 C5 -178.1(2) . . . . ? C2 Cr1 C4 C5 93.4(2) . . . . ? C1 Cr1 C4 C5 2.6(4) . . . . ? C7 Cr1 C4 C5 -66.0(2) . . . . ? C8 Cr1 C4 C5 -102.4(2) . . . . ? C6 Cr1 C4 C5 -28.6(2) . . . . ? C9 Cr1 C4 C5 -132.6(3) . . . . ? C9 C4 C5 C6 -0.5(5) . . . . ? Cr1 C4 C5 C6 54.1(3) . . . . ? C9 C4 C5 Cr1 -54.6(3) . . . . ? C3 Cr1 C5 C6 -128.3(4) . . . . ? C2 Cr1 C5 C6 140.3(2) . . . . ? C1 Cr1 C5 C6 48.8(3) . . . . ? C7 Cr1 C5 C6 -29.9(2) . . . . ? C8 Cr1 C5 C6 -66.2(2) . . . . ? C4 Cr1 C5 C6 -132.6(3) . . . . ? C9 Cr1 C5 C6 -103.9(2) . . . . ? C3 Cr1 C5 C4 4.2(5) . . . . ? C2 Cr1 C5 C4 -87.2(2) . . . . ? C1 Cr1 C5 C4 -178.7(2) . . . . ? C7 Cr1 C5 C4 102.7(2) . . . . ? C8 Cr1 C5 C4 66.3(2) . . . . ? C6 Cr1 C5 C4 132.6(3) . . . . ? C9 Cr1 C5 C4 28.7(2) . . . . ? C4 C5 C6 C7 0.1(5) . . . . ? Cr1 C5 C6 C7 53.9(3) . . . . ? C4 C5 C6 C11 -179.2(3) . . . . ? Cr1 C5 C6 C11 -125.4(3) . . . . ? C4 C5 C6 Cr1 -53.8(3) . . . . ? C3 Cr1 C6 C5 139.1(4) . . . . ? C2 Cr1 C6 C5 -46.9(3) . . . . ? C1 Cr1 C6 C5 -136.6(2) . . . . ? C7 Cr1 C6 C5 131.6(3) . . . . ? C8 Cr1 C6 C5 102.8(2) . . . . ? C4 Cr1 C6 C5 29.1(2) . . . . ? C9 Cr1 C6 C5 65.4(2) . . . . ? C3 Cr1 C6 C7 7.6(5) . . . . ? C2 Cr1 C6 C7 -178.5(2) . . . . ? C1 Cr1 C6 C7 91.8(2) . . . . ? C8 Cr1 C6 C7 -28.8(2) . . . . ? C4 Cr1 C6 C7 -102.5(2) . . . . ? C5 Cr1 C6 C7 -131.6(3) . . . . ? C9 Cr1 C6 C7 -66.1(2) . . . . ? C3 Cr1 C6 C11 -105.7(5) . . . . ? C2 Cr1 C6 C11 68.2(4) . . . . ? C1 Cr1 C6 C11 -21.5(4) . . . . ? C7 Cr1 C6 C11 -113.3(5) . . . . ? C8 Cr1 C6 C11 -142.0(4) . . . . ? C4 Cr1 C6 C11 144.3(4) . . . . ? C5 Cr1 C6 C11 115.1(4) . . . . ? C9 Cr1 C6 C11 -179.4(4) . . . . ? C5 C6 C7 C8 0.4(5) . . . . ? C11 C6 C7 C8 179.7(3) . . . . ? Cr1 C6 C7 C8 54.8(3) . . . . ? C5 C6 C7 Cr1 -54.4(3) . . . . ? C11 C6 C7 Cr1 124.8(3) . . . . ? C3 Cr1 C7 C8 51.7(3) . . . . ? C2 Cr1 C7 C8 -128.8(4) . . . . ? C1 Cr1 C7 C8 140.4(2) . . . . ? C4 Cr1 C7 C8 -66.0(2) . . . . ? C6 Cr1 C7 C8 -132.1(3) . . . . ? C5 Cr1 C7 C8 -103.1(2) . . . . ? C9 Cr1 C7 C8 -29.3(2) . . . . ? C3 Cr1 C7 C6 -176.1(2) . . . . ? C2 Cr1 C7 C6 3.4(5) . . . . ? C1 Cr1 C7 C6 -87.5(2) . . . . ? C8 Cr1 C7 C6 132.1(3) . . . . ? C4 Cr1 C7 C6 66.2(2) . . . . ? C5 Cr1 C7 C6 29.0(2) . . . . ? C9 Cr1 C7 C6 102.8(2) . . . . ? C6 C7 C8 C9 -0.5(5) . . . . ? Cr1 C7 C8 C9 54.3(3) . . . . ? C6 C7 C8 Cr1 -54.9(3) . . . . ? C3 Cr1 C8 C7 -134.4(3) . . . . ? C2 Cr1 C8 C7 138.7(3) . . . . ? C1 Cr1 C8 C7 -45.8(3) . . . . ? C4 Cr1 C8 C7 103.0(2) . . . . ? C6 Cr1 C8 C7 29.5(2) . . . . ? C5 Cr1 C8 C7 65.9(2) . . . . ? C9 Cr1 C8 C7 132.5(3) . . . . ? C3 Cr1 C8 C9 93.1(2) . . . . ? C2 Cr1 C8 C9 6.2(4) . . . . ? C1 Cr1 C8 C9 -178.3(2) . . . . ? C7 Cr1 C8 C9 -132.5(3) . . . . ? C4 Cr1 C8 C9 -29.5(2) . . . . ? C6 Cr1 C8 C9 -103.0(2) . . . . ? C5 Cr1 C8 C9 -66.7(2) . . . . ? C5 C4 C9 C8 0.3(5) . . . . ? Cr1 C4 C9 C8 -54.1(3) . . . . ? C5 C4 C9 C10 179.3(3) . . . . ? Cr1 C4 C9 C10 124.9(3) . . . . ? C5 C4 C9 Cr1 54.5(3) . . . . ? C7 C8 C9 C4 0.2(5) . . . . ? Cr1 C8 C9 C4 54.4(3) . . . . ? C7 C8 C9 C10 -178.8(3) . . . . ? Cr1 C8 C9 C10 -124.6(3) . . . . ? C7 C8 C9 Cr1 -54.3(3) . . . . ? C3 Cr1 C9 C4 141.6(2) . . . . ? C2 Cr1 C9 C4 52.1(3) . . . . ? C1 Cr1 C9 C4 -127.5(4) . . . . ? C7 Cr1 C9 C4 -102.5(2) . . . . ? C8 Cr1 C9 C4 -131.0(3) . . . . ? C6 Cr1 C9 C4 -65.1(2) . . . . ? C5 Cr1 C9 C4 -29.0(2) . . . . ? C3 Cr1 C9 C8 -87.4(2) . . . . ? C2 Cr1 C9 C8 -176.8(2) . . . . ? C1 Cr1 C9 C8 3.6(5) . . . . ? C7 Cr1 C9 C8 28.5(2) . . . . ? C4 Cr1 C9 C8 131.0(3) . . . . ? C6 Cr1 C9 C8 65.9(2) . . . . ? C5 Cr1 C9 C8 102.0(2) . . . . ? C3 Cr1 C9 C10 26.9(4) . . . . ? C2 Cr1 C9 C10 -62.6(4) . . . . ? C1 Cr1 C9 C10 117.8(4) . . . . ? C7 Cr1 C9 C10 142.8(4) . . . . ? C8 Cr1 C9 C10 114.3(4) . . . . ? C4 Cr1 C9 C10 -114.7(4) . . . . ? C6 Cr1 C9 C10 -179.8(4) . . . . ? C5 Cr1 C9 C10 -143.7(4) . . . . ? C4 C9 C10 Br1 98.2(3) . . . . ? C8 C9 C10 Br1 -82.8(4) . . . . ? Cr1 C9 C10 Br1 -171.8(2) . . . . ? C5 C6 C11 Br2 -97.6(4) . . . . ? C7 C6 C11 Br2 83.1(4) . . . . ? Cr1 C6 C11 Br2 171.6(2) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.895 _refine_diff_density_min -1.138 _refine_diff_density_rms 0.165 data_mc444 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H18 Cr O5' _chemical_formula_weight 330.29 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cr' 'Cr' 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7270(7) _cell_length_b 11.9245(11) _cell_length_c 14.7140(10) _cell_angle_alpha 69.767(5) _cell_angle_beta 82.210(6) _cell_angle_gamma 84.463(5) _cell_volume 1421.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.543 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 688 _exptl_absorpt_coefficient_mu 0.823 _exptl_absorpt_correction_type Scalepack _exptl_absorpt_correction_T_min 0.7342 _exptl_absorpt_correction_T_max 0.9222 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 KappaCCD _diffrn_measurement_method '1o phi scans + omega to complete' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 10021 _diffrn_reflns_av_R_equivalents 0.0275 _diffrn_reflns_av_sigmaI/netI 0.0651 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6355 _reflns_number_gt 5205 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics RES2INS _computing_publication_material ? _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^)+(0.0382P)^2^+1.2563P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0093(15) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6355 _refine_ls_number_parameters 391 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0571 _refine_ls_R_factor_gt 0.0444 _refine_ls_wR_factor_ref 0.1210 _refine_ls_wR_factor_gt 0.1129 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.017 _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 0.84816(3) 0.82152(3) 0.44179(2) 0.01098(11) Uani 1 1 d . . . Cr2 Cr 0.33884(3) 0.82700(3) -0.05469(2) 0.01063(11) Uani 1 1 d . . . O10 O 0.50803(18) 0.70053(14) -0.31096(11) 0.0202(3) Uani 1 1 d . . . H10 H 0.4467 0.6966 -0.3490 0.024 Uiso 1 1 calc R . . O4 O 1.29362(17) 0.66622(14) 0.57652(11) 0.0200(3) Uani 1 1 d . . . O5 O 0.74904(19) 0.55985(14) 0.29748(12) 0.0225(4) Uani 1 1 d . . . H5 H 0.6750 0.5492 0.2709 0.027 Uiso 1 1 calc R . . O9 O 0.52770(19) 0.52917(14) 0.19613(11) 0.0234(4) Uani 1 1 d . . . H9 H 0.4855 0.4656 0.2307 0.028 Uiso 1 1 calc R . . O2 O 0.90921(19) 1.05936(14) 0.28715(12) 0.0234(4) Uani 1 1 d . . . O1 O 0.8242(2) 0.93904(15) 0.59391(12) 0.0234(4) Uani 1 1 d . . . C23 C 0.3134(2) 0.67304(18) -0.10229(15) 0.0132(4) Uani 1 1 d . . . O3 O 0.50641(18) 0.88343(16) 0.44373(14) 0.0280(4) Uani 1 1 d . . . O8 O -0.00213(18) 0.88913(17) -0.05213(14) 0.0301(4) Uani 1 1 d . . . C7 C 0.8336(2) 0.66911(18) 0.39215(15) 0.0133(4) Uani 1 1 d . . . O7 O 0.3942(2) 1.06550(14) -0.20969(12) 0.0258(4) Uani 1 1 d . . . C10 C 1.1714(2) 0.75637(19) 0.54652(15) 0.0141(4) Uani 1 1 d . . . H10A H 1.2166 0.8320 0.5030 0.017 Uiso 1 1 calc R . . H10B H 1.1143 0.7713 0.6045 0.017 Uiso 1 1 calc R . . C28 C 0.4488(2) 0.78985(19) -0.26794(15) 0.0155(4) Uani 1 1 d . . . H28A H 0.3437 0.8193 -0.2867 0.019 Uiso 1 1 calc R . . H28B H 0.5163 0.8585 -0.2928 0.019 Uiso 1 1 calc R . . C14 C 0.6883(2) 0.5420(2) 0.55180(16) 0.0182(4) Uani 1 1 d . . . H14A H 0.7100 0.4998 0.6192 0.027 Uiso 1 1 calc R . . H14B H 0.6774 0.4836 0.5201 0.027 Uiso 1 1 calc R . . H14C H 0.5919 0.5917 0.5515 0.027 Uiso 1 1 calc R . . C22 C 0.4421(2) 0.73826(18) -0.15806(14) 0.0123(4) Uani 1 1 d . . . C12 C 0.9863(3) 0.7762(2) 0.22826(15) 0.0190(4) Uani 1 1 d . . . H12A H 1.0715 0.7292 0.2056 0.028 Uiso 1 1 calc R . . H12B H 1.0104 0.8607 0.2038 0.028 Uiso 1 1 calc R . . H12C H 0.8906 0.7672 0.2040 0.028 Uiso 1 1 calc R . . C26 C 0.6817(2) 0.7438(2) 0.04207(16) 0.0181(4) Uani 1 1 d . . . H26A H 0.7604 0.6775 0.0542 0.027 Uiso 1 1 calc R . . H26B H 0.6370 0.7527 0.1042 0.027 Uiso 1 1 calc R . . H26C H 0.7295 0.8180 0.0002 0.027 Uiso 1 1 calc R . . O6 O 0.33438(19) 0.94761(15) 0.09406(12) 0.0225(3) Uani 1 1 d . . . C8 C 0.8206(2) 0.62105(18) 0.49699(15) 0.0129(4) Uani 1 1 d . . . C9 C 0.9307(2) 0.64791(18) 0.54744(14) 0.0124(4) Uani 1 1 d . . . C13 C 0.7048(2) 0.65323(19) 0.33852(16) 0.0162(4) Uani 1 1 d . . . H13A H 0.6093 0.6326 0.3842 0.019 Uiso 1 1 calc R . . H13B H 0.6826 0.7292 0.2859 0.019 Uiso 1 1 calc R . . C2 C 0.8837(2) 0.96788(19) 0.34755(16) 0.0155(4) Uani 1 1 d . . . C21 C 0.5679(2) 0.75503(18) -0.11080(14) 0.0128(4) Uani 1 1 d . . . C25 C 0.4115(2) 0.6198(2) 0.15870(15) 0.0162(4) Uani 1 1 d . . . H25A H 0.4245 0.6904 0.1771 0.019 Uiso 1 1 calc R . . H25B H 0.3079 0.5896 0.1877 0.019 Uiso 1 1 calc R . . C17 C 0.3717(2) 0.9743(2) -0.14978(16) 0.0166(4) Uani 1 1 d . . . C24 C 0.3059(2) 0.62893(18) 0.00231(15) 0.0126(4) Uani 1 1 d . . . C15 C 0.9120(2) 0.6017(2) 0.65803(15) 0.0178(4) Uani 1 1 d . . . H15A H 0.8051 0.6188 0.6821 0.027 Uiso 1 1 calc R . . H15B H 0.9831 0.6413 0.6818 0.027 Uiso 1 1 calc R . . H15C H 0.9357 0.5151 0.6816 0.027 Uiso 1 1 calc R . . C11 C 1.2243(2) 0.8157(2) 0.33278(15) 0.0174(4) Uani 1 1 d . . . H11A H 1.1984 0.9014 0.3026 0.026 Uiso 1 1 calc R . . H11B H 1.2634 0.7814 0.2819 0.026 Uiso 1 1 calc R . . H11C H 1.3040 0.8046 0.3766 0.026 Uiso 1 1 calc R . . C19 C 0.4220(2) 0.65620(18) 0.04881(14) 0.0126(4) Uani 1 1 d . . . C6 C 0.9649(2) 0.73198(18) 0.33888(15) 0.0138(4) Uani 1 1 d . . . C16 C 0.3371(2) 0.90103(19) 0.03656(15) 0.0146(4) Uani 1 1 d . . . C18 C 0.1291(3) 0.86467(19) -0.05342(16) 0.0178(4) Uani 1 1 d . . . C29 C 0.1845(2) 0.6481(2) -0.15071(16) 0.0179(4) Uani 1 1 d . . . H29A H 0.1990 0.6926 -0.2208 0.027 Uiso 1 1 calc R . . H29B H 0.0846 0.6733 -0.1226 0.027 Uiso 1 1 calc R . . H29C H 0.1866 0.5622 -0.1401 0.027 Uiso 1 1 calc R . . C1 C 0.8352(2) 0.89371(19) 0.53530(16) 0.0159(4) Uani 1 1 d . . . C4 C 1.0599(2) 0.71801(18) 0.49362(15) 0.0127(4) Uani 1 1 d . . . C3 C 0.6376(2) 0.85797(19) 0.44153(16) 0.0171(4) Uani 1 1 d . . . C30 C 0.1720(3) 0.5536(2) 0.06029(17) 0.0211(5) Uani 1 1 d . . . H30A H 0.0807 0.6061 0.0667 0.032 Uiso 1 1 calc R . . H30B H 0.2005 0.5054 0.1252 0.032 Uiso 1 1 calc R . . H30C H 0.1485 0.5006 0.0264 0.032 Uiso 1 1 calc R . . C5 C 1.0812(2) 0.75385(18) 0.39009(15) 0.0128(4) Uani 1 1 d . . . C20 C 0.5553(2) 0.71809(18) -0.00776(14) 0.0122(4) Uani 1 1 d . . . C27 C 0.7117(2) 0.8126(2) -0.17168(16) 0.0184(4) Uani 1 1 d . . . H27A H 0.6917 0.8996 -0.1977 0.028 Uiso 1 1 calc R . . H27B H 0.7393 0.7817 -0.2257 0.028 Uiso 1 1 calc R . . H27C H 0.7973 0.7939 -0.1311 0.028 Uiso 1 1 calc R . . H4 H 1.2587 0.5887 0.6189 0.022 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr1 0.01039(17) 0.01118(19) 0.01100(18) -0.00275(13) -0.00233(12) -0.00087(12) Cr2 0.01019(17) 0.01095(19) 0.01034(18) -0.00263(13) -0.00186(12) -0.00117(12) O10 0.0216(8) 0.0248(8) 0.0188(8) -0.0131(7) -0.0010(6) -0.0023(6) O4 0.0189(7) 0.0176(8) 0.0237(8) -0.0060(6) -0.0086(6) 0.0035(6) O5 0.0265(8) 0.0191(8) 0.0276(9) -0.0124(7) -0.0090(7) -0.0026(7) O9 0.0301(8) 0.0192(8) 0.0177(8) -0.0014(6) -0.0084(7) 0.0035(7) O2 0.0273(8) 0.0160(8) 0.0215(8) 0.0014(7) -0.0038(7) -0.0022(6) O1 0.0323(9) 0.0220(8) 0.0191(8) -0.0112(7) -0.0037(7) 0.0007(7) C23 0.0137(9) 0.0122(9) 0.0147(10) -0.0051(8) -0.0033(8) -0.0005(7) O3 0.0126(8) 0.0330(10) 0.0390(10) -0.0128(8) -0.0041(7) -0.0001(7) O8 0.0125(8) 0.0355(10) 0.0447(11) -0.0161(9) -0.0053(7) 0.0005(7) C7 0.0138(9) 0.0112(9) 0.0157(10) -0.0046(8) -0.0047(8) -0.0003(7) O7 0.0344(9) 0.0149(8) 0.0214(8) 0.0036(7) -0.0063(7) -0.0019(7) C10 0.0130(9) 0.0160(10) 0.0147(10) -0.0053(8) -0.0070(8) 0.0004(8) C28 0.0204(10) 0.0149(10) 0.0109(9) -0.0035(8) -0.0031(8) -0.0003(8) C14 0.0170(10) 0.0188(10) 0.0185(10) -0.0053(8) 0.0007(8) -0.0066(8) C22 0.0146(9) 0.0120(9) 0.0105(9) -0.0044(7) -0.0010(7) 0.0000(7) C12 0.0221(10) 0.0220(11) 0.0130(10) -0.0053(8) -0.0020(8) -0.0041(9) C26 0.0150(9) 0.0208(11) 0.0185(10) -0.0047(9) -0.0058(8) -0.0038(8) O6 0.0305(9) 0.0213(8) 0.0187(8) -0.0102(7) -0.0033(7) -0.0025(7) C8 0.0133(9) 0.0101(9) 0.0148(10) -0.0031(8) -0.0026(7) -0.0008(7) C9 0.0119(9) 0.0122(9) 0.0116(9) -0.0021(7) -0.0031(7) 0.0012(7) C13 0.0170(10) 0.0155(10) 0.0189(10) -0.0076(8) -0.0074(8) 0.0002(8) C2 0.0117(9) 0.0186(10) 0.0181(10) -0.0081(9) -0.0043(8) 0.0011(8) C21 0.0125(9) 0.0129(9) 0.0119(9) -0.0034(8) 0.0002(7) -0.0006(7) C25 0.0150(9) 0.0184(10) 0.0135(10) -0.0031(8) -0.0034(8) 0.0004(8) C17 0.0156(9) 0.0200(11) 0.0161(10) -0.0077(9) -0.0049(8) 0.0014(8) C24 0.0132(9) 0.0114(9) 0.0131(9) -0.0031(8) -0.0025(7) -0.0026(7) C15 0.0159(9) 0.0234(11) 0.0112(9) -0.0018(8) -0.0021(8) -0.0018(8) C11 0.0144(9) 0.0223(11) 0.0151(10) -0.0065(8) 0.0028(8) -0.0056(8) C19 0.0139(9) 0.0107(9) 0.0117(9) -0.0014(7) -0.0031(7) 0.0002(7) C6 0.0167(9) 0.0138(10) 0.0117(9) -0.0053(8) -0.0022(8) 0.0004(8) C16 0.0124(9) 0.0142(10) 0.0140(9) -0.0001(8) -0.0033(7) -0.0004(7) C18 0.0193(10) 0.0161(10) 0.0200(11) -0.0073(9) -0.0035(8) -0.0047(8) C29 0.0169(10) 0.0207(11) 0.0182(10) -0.0070(9) -0.0054(8) -0.0041(8) C1 0.0135(9) 0.0131(10) 0.0174(10) -0.0001(8) -0.0026(8) -0.0007(8) C4 0.0105(9) 0.0145(10) 0.0137(10) -0.0051(8) -0.0033(7) 0.0007(7) C3 0.0185(10) 0.0151(10) 0.0191(10) -0.0063(8) -0.0034(8) -0.0041(8) C30 0.0209(10) 0.0237(11) 0.0184(11) -0.0054(9) 0.0012(9) -0.0110(9) C5 0.0106(9) 0.0138(9) 0.0136(9) -0.0041(8) -0.0009(7) -0.0009(7) C20 0.0119(9) 0.0116(9) 0.0132(9) -0.0039(8) -0.0036(7) 0.0008(7) C27 0.0139(9) 0.0243(11) 0.0165(10) -0.0067(9) 0.0030(8) -0.0056(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 C2 1.838(2) . ? Cr1 C1 1.845(2) . ? Cr1 C3 1.847(2) . ? Cr1 C4 2.193(2) . ? Cr1 C7 2.200(2) . ? Cr1 C6 2.227(2) . ? Cr1 C9 2.238(2) . ? Cr1 C5 2.249(2) . ? Cr1 C8 2.269(2) . ? Cr2 C18 1.841(2) . ? Cr2 C16 1.842(2) . ? Cr2 C17 1.848(2) . ? Cr2 C22 2.192(2) . ? Cr2 C19 2.205(2) . ? Cr2 C23 2.218(2) . ? Cr2 C20 2.234(2) . ? Cr2 C24 2.249(2) . ? Cr2 C21 2.264(2) . ? O10 C28 1.440(3) . ? O4 C10 1.438(2) . ? O5 C13 1.440(3) . ? O9 C25 1.424(3) . ? O2 C2 1.163(3) . ? O1 C1 1.156(3) . ? C23 C22 1.420(3) . ? C23 C24 1.438(3) . ? C23 C29 1.513(3) . ? O3 C3 1.155(3) . ? O8 C18 1.154(3) . ? C7 C6 1.416(3) . ? C7 C8 1.440(3) . ? C7 C13 1.519(3) . ? O7 C17 1.153(3) . ? C10 C4 1.517(3) . ? C28 C22 1.513(3) . ? C14 C8 1.518(3) . ? C22 C21 1.440(3) . ? C12 C6 1.518(3) . ? C26 C20 1.513(3) . ? O6 C16 1.158(3) . ? C8 C9 1.412(3) . ? C9 C4 1.442(3) . ? C9 C15 1.518(3) . ? C21 C20 1.417(3) . ? C21 C27 1.512(3) . ? C25 C19 1.514(3) . ? C24 C19 1.416(3) . ? C24 C30 1.517(3) . ? C11 C5 1.508(3) . ? C19 C20 1.439(3) . ? C6 C5 1.436(3) . ? C4 C5 1.423(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Cr1 C1 88.94(9) . . ? C2 Cr1 C3 89.47(9) . . ? C1 Cr1 C3 85.24(9) . . ? C2 Cr1 C4 113.80(8) . . ? C1 Cr1 C4 91.18(8) . . ? C3 Cr1 C4 156.42(9) . . ? C2 Cr1 C7 117.23(9) . . ? C1 Cr1 C7 153.73(8) . . ? C3 Cr1 C7 92.28(8) . . ? C4 Cr1 C7 80.71(8) . . ? C2 Cr1 C6 89.51(8) . . ? C1 Cr1 C6 156.44(9) . . ? C3 Cr1 C6 118.26(9) . . ? C4 Cr1 C6 68.06(7) . . ? C7 Cr1 C6 37.31(7) . . ? C2 Cr1 C9 151.75(8) . . ? C1 Cr1 C9 90.76(8) . . ? C3 Cr1 C9 118.66(8) . . ? C4 Cr1 C9 37.96(7) . . ? C7 Cr1 C9 67.53(7) . . ? C6 Cr1 C9 79.72(7) . . ? C2 Cr1 C5 88.47(8) . . ? C1 Cr1 C5 119.03(8) . . ? C3 Cr1 C5 155.58(9) . . ? C4 Cr1 C5 37.36(7) . . ? C7 Cr1 C5 67.29(7) . . ? C6 Cr1 C5 37.41(7) . . ? C9 Cr1 C5 67.14(7) . . ? C2 Cr1 C8 154.66(9) . . ? C1 Cr1 C8 116.38(8) . . ? C3 Cr1 C8 93.60(8) . . ? C4 Cr1 C8 67.19(7) . . ? C7 Cr1 C8 37.56(7) . . ? C6 Cr1 C8 66.92(7) . . ? C9 Cr1 C8 36.51(7) . . ? C5 Cr1 C8 78.44(7) . . ? C18 Cr2 C16 87.06(9) . . ? C18 Cr2 C17 88.62(9) . . ? C16 Cr2 C17 87.76(9) . . ? C18 Cr2 C22 116.36(9) . . ? C16 Cr2 C22 156.40(8) . . ? C17 Cr2 C22 89.87(8) . . ? C18 Cr2 C19 119.13(9) . . ? C16 Cr2 C19 90.72(8) . . ? C17 Cr2 C19 152.10(8) . . ? C22 Cr2 C19 80.56(7) . . ? C18 Cr2 C23 90.91(9) . . ? C16 Cr2 C23 154.20(8) . . ? C17 Cr2 C23 117.92(9) . . ? C22 Cr2 C23 37.57(7) . . ? C19 Cr2 C23 67.93(7) . . ? C18 Cr2 C20 156.93(9) . . ? C16 Cr2 C20 91.87(8) . . ? C17 Cr2 C20 114.38(8) . . ? C22 Cr2 C20 67.85(7) . . ? C19 Cr2 C20 37.80(7) . . ? C23 Cr2 C20 80.11(7) . . ? C18 Cr2 C24 92.89(8) . . ? C16 Cr2 C24 116.83(8) . . ? C17 Cr2 C24 155.41(9) . . ? C22 Cr2 C24 67.51(7) . . ? C19 Cr2 C24 37.06(7) . . ? C23 Cr2 C24 37.56(7) . . ? C20 Cr2 C24 67.09(7) . . ? C18 Cr2 C21 153.96(9) . . ? C16 Cr2 C21 118.80(8) . . ? C17 Cr2 C21 89.47(8) . . ? C22 Cr2 C21 37.67(7) . . ? C19 Cr2 C21 67.02(7) . . ? C23 Cr2 C21 67.25(7) . . ? C20 Cr2 C21 36.71(7) . . ? C24 Cr2 C21 78.52(7) . . ? C22 C23 C24 119.40(18) . . ? C22 C23 C29 121.33(18) . . ? C24 C23 C29 119.27(18) . . ? C22 C23 Cr2 70.20(11) . . ? C24 C23 Cr2 72.40(12) . . ? C29 C23 Cr2 129.90(14) . . ? C6 C7 C8 120.43(18) . . ? C6 C7 C13 119.84(18) . . ? C8 C7 C13 119.72(18) . . ? C6 C7 Cr1 72.39(12) . . ? C8 C7 Cr1 73.80(12) . . ? C13 C7 Cr1 125.32(14) . . ? O4 C10 C4 111.17(17) . . ? O10 C28 C22 110.57(17) . . ? C23 C22 C21 120.43(18) . . ? C23 C22 C28 120.15(18) . . ? C21 C22 C28 119.42(17) . . ? C23 C22 Cr2 72.23(11) . . ? C21 C22 Cr2 73.89(11) . . ? C28 C22 Cr2 126.37(14) . . ? C9 C8 C7 119.75(18) . . ? C9 C8 C14 120.86(18) . . ? C7 C8 C14 119.39(18) . . ? C9 C8 Cr1 70.58(11) . . ? C7 C8 Cr1 68.63(11) . . ? C14 C8 Cr1 133.92(14) . . ? C8 C9 C4 119.82(18) . . ? C8 C9 C15 119.43(18) . . ? C4 C9 C15 120.75(18) . . ? C8 C9 Cr1 72.92(11) . . ? C4 C9 Cr1 69.31(11) . . ? C15 C9 Cr1 130.60(14) . . ? O5 C13 C7 110.36(17) . . ? O2 C2 Cr1 178.50(19) . . ? C20 C21 C22 119.72(17) . . ? C20 C21 C27 120.63(18) . . ? C22 C21 C27 119.66(17) . . ? C20 C21 Cr2 70.52(11) . . ? C22 C21 Cr2 68.44(11) . . ? C27 C21 Cr2 133.93(15) . . ? O9 C25 C19 110.70(17) . . ? O7 C17 Cr2 179.0(2) . . ? C19 C24 C23 119.92(18) . . ? C19 C24 C30 121.56(18) . . ? C23 C24 C30 118.53(18) . . ? C19 C24 Cr2 69.78(11) . . ? C23 C24 Cr2 70.04(11) . . ? C30 C24 Cr2 133.30(15) . . ? C24 C19 C20 120.44(18) . . ? C24 C19 C25 121.47(18) . . ? C20 C19 C25 118.08(18) . . ? C24 C19 Cr2 73.16(11) . . ? C20 C19 Cr2 72.19(11) . . ? C25 C19 Cr2 127.66(14) . . ? C7 C6 C5 119.61(18) . . ? C7 C6 C12 121.35(18) . . ? C5 C6 C12 119.04(18) . . ? C7 C6 Cr1 70.30(11) . . ? C5 C6 Cr1 72.09(11) . . ? C12 C6 Cr1 130.28(15) . . ? O6 C16 Cr2 179.29(18) . . ? O8 C18 Cr2 179.3(2) . . ? O1 C1 Cr1 178.80(19) . . ? C5 C4 C9 119.97(18) . . ? C5 C4 C10 119.64(18) . . ? C9 C4 C10 120.37(18) . . ? C5 C4 Cr1 73.44(11) . . ? C9 C4 Cr1 72.73(11) . . ? C10 C4 Cr1 124.35(14) . . ? O3 C3 Cr1 177.2(2) . . ? C4 C5 C6 119.84(18) . . ? C4 C5 C11 120.98(18) . . ? C6 C5 C11 119.17(18) . . ? C4 C5 Cr1 69.20(11) . . ? C6 C5 Cr1 70.49(11) . . ? C11 C5 Cr1 133.00(15) . . ? C21 C20 C19 119.61(18) . . ? C21 C20 C26 119.97(18) . . ? C19 C20 C26 120.42(18) . . ? C21 C20 Cr2 72.78(11) . . ? C19 C20 Cr2 70.00(11) . . ? C26 C20 Cr2 129.37(14) . . ? 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 C18 Cr2 C23 C22 135.03(13) . . . . ? C16 Cr2 C23 C22 -139.83(19) . . . . ? C17 Cr2 C23 C22 46.11(14) . . . . ? C19 Cr2 C23 C22 -103.71(13) . . . . ? C20 Cr2 C23 C22 -66.35(12) . . . . ? C24 Cr2 C23 C22 -131.41(17) . . . . ? C21 Cr2 C23 C22 -30.38(11) . . . . ? C18 Cr2 C23 C24 -93.56(13) . . . . ? C16 Cr2 C23 C24 -8.4(2) . . . . ? C17 Cr2 C23 C24 177.52(12) . . . . ? C22 Cr2 C23 C24 131.41(17) . . . . ? C19 Cr2 C23 C24 27.70(11) . . . . ? C20 Cr2 C23 C24 65.07(12) . . . . ? C21 Cr2 C23 C24 101.03(12) . . . . ? C18 Cr2 C23 C29 20.23(19) . . . . ? C16 Cr2 C23 C29 105.4(2) . . . . ? C17 Cr2 C23 C29 -68.7(2) . . . . ? C22 Cr2 C23 C29 -114.8(2) . . . . ? C19 Cr2 C23 C29 141.5(2) . . . . ? C20 Cr2 C23 C29 178.86(19) . . . . ? C24 Cr2 C23 C29 113.8(2) . . . . ? C21 Cr2 C23 C29 -145.2(2) . . . . ? C2 Cr1 C7 C6 46.27(14) . . . . ? C1 Cr1 C7 C6 -139.29(18) . . . . ? C3 Cr1 C7 C6 136.85(13) . . . . ? C4 Cr1 C7 C6 -65.80(12) . . . . ? C9 Cr1 C7 C6 -102.96(13) . . . . ? C5 Cr1 C7 C6 -29.38(11) . . . . ? C8 Cr1 C7 C6 -130.21(17) . . . . ? C2 Cr1 C7 C8 176.48(12) . . . . ? C1 Cr1 C7 C8 -9.1(2) . . . . ? C3 Cr1 C7 C8 -92.94(13) . . . . ? C4 Cr1 C7 C8 64.41(12) . . . . ? C6 Cr1 C7 C8 130.21(17) . . . . ? C9 Cr1 C7 C8 27.25(11) . . . . ? C5 Cr1 C7 C8 100.83(12) . . . . ? C2 Cr1 C7 C13 -68.25(19) . . . . ? C1 Cr1 C7 C13 106.2(2) . . . . ? C3 Cr1 C7 C13 22.33(18) . . . . ? C4 Cr1 C7 C13 179.68(18) . . . . ? C6 Cr1 C7 C13 -114.5(2) . . . . ? C9 Cr1 C7 C13 142.52(19) . . . . ? C5 Cr1 C7 C13 -143.90(19) . . . . ? C8 Cr1 C7 C13 115.3(2) . . . . ? C24 C23 C22 C21 3.1(3) . . . . ? C29 C23 C22 C21 -176.36(19) . . . . ? Cr2 C23 C22 C21 58.26(17) . . . . ? C24 C23 C22 C28 -177.42(18) . . . . ? C29 C23 C22 C28 3.1(3) . . . . ? Cr2 C23 C22 C28 -122.28(18) . . . . ? C24 C23 C22 Cr2 -55.14(17) . . . . ? C29 C23 C22 Cr2 125.38(19) . . . . ? O10 C28 C22 C23 -83.5(2) . . . . ? O10 C28 C22 C21 96.0(2) . . . . ? O10 C28 C22 Cr2 -172.90(13) . . . . ? C18 Cr2 C22 C23 -52.05(14) . . . . ? C16 Cr2 C22 C23 135.5(2) . . . . ? C17 Cr2 C22 C23 -140.45(13) . . . . ? C19 Cr2 C22 C23 65.87(12) . . . . ? C20 Cr2 C22 C23 103.02(13) . . . . ? C24 Cr2 C22 C23 29.66(11) . . . . ? C21 Cr2 C22 C23 130.25(17) . . . . ? C18 Cr2 C22 C21 177.70(12) . . . . ? C16 Cr2 C22 C21 5.2(3) . . . . ? C17 Cr2 C22 C21 89.30(12) . . . . ? C19 Cr2 C22 C21 -64.38(12) . . . . ? C23 Cr2 C22 C21 -130.25(17) . . . . ? C20 Cr2 C22 C21 -27.23(11) . . . . ? C24 Cr2 C22 C21 -100.59(12) . . . . ? C18 Cr2 C22 C28 62.72(19) . . . . ? C16 Cr2 C22 C28 -109.8(2) . . . . ? C17 Cr2 C22 C28 -25.68(18) . . . . ? C19 Cr2 C22 C28 -179.35(18) . . . . ? C23 Cr2 C22 C28 114.8(2) . . . . ? C20 Cr2 C22 C28 -142.21(19) . . . . ? C24 Cr2 C22 C28 144.43(19) . . . . ? C21 Cr2 C22 C28 -115.0(2) . . . . ? C6 C7 C8 C9 7.0(3) . . . . ? C13 C7 C8 C9 -172.41(18) . . . . ? Cr1 C7 C8 C9 -50.59(17) . . . . ? C6 C7 C8 C14 -173.03(19) . . . . ? C13 C7 C8 C14 7.6(3) . . . . ? Cr1 C7 C8 C14 129.39(18) . . . . ? C6 C7 C8 Cr1 57.59(17) . . . . ? C13 C7 C8 Cr1 -121.83(18) . . . . ? C2 Cr1 C8 C9 127.34(19) . . . . ? C1 Cr1 C8 C9 -49.81(14) . . . . ? C3 Cr1 C8 C9 -136.28(13) . . . . ? C4 Cr1 C8 C9 29.61(11) . . . . ? C7 Cr1 C8 C9 134.66(17) . . . . ? C6 Cr1 C8 C9 104.46(13) . . . . ? C5 Cr1 C8 C9 67.03(12) . . . . ? C2 Cr1 C8 C7 -7.3(2) . . . . ? C1 Cr1 C8 C7 175.53(12) . . . . ? C3 Cr1 C8 C7 89.06(13) . . . . ? C4 Cr1 C8 C7 -105.06(13) . . . . ? C6 Cr1 C8 C7 -30.20(11) . . . . ? C9 Cr1 C8 C7 -134.66(17) . . . . ? C5 Cr1 C8 C7 -67.63(12) . . . . ? C2 Cr1 C8 C14 -118.1(2) . . . . ? C1 Cr1 C8 C14 64.7(2) . . . . ? C3 Cr1 C8 C14 -21.7(2) . . . . ? C4 Cr1 C8 C14 144.2(2) . . . . ? C7 Cr1 C8 C14 -110.8(2) . . . . ? C6 Cr1 C8 C14 -141.0(2) . . . . ? C9 Cr1 C8 C14 114.6(2) . . . . ? C5 Cr1 C8 C14 -178.4(2) . . . . ? C7 C8 C9 C4 -3.3(3) . . . . ? C14 C8 C9 C4 176.78(18) . . . . ? Cr1 C8 C9 C4 -52.97(17) . . . . ? C7 C8 C9 C15 177.19(18) . . . . ? C14 C8 C9 C15 -2.8(3) . . . . ? Cr1 C8 C9 C15 127.47(18) . . . . ? C7 C8 C9 Cr1 49.72(17) . . . . ? C14 C8 C9 Cr1 -130.25(19) . . . . ? C2 Cr1 C9 C8 -134.03(18) . . . . ? C1 Cr1 C9 C8 136.81(12) . . . . ? C3 Cr1 C9 C8 51.82(14) . . . . ? C4 Cr1 C9 C8 -132.24(17) . . . . ? C7 Cr1 C9 C8 -27.98(11) . . . . ? C6 Cr1 C9 C8 -64.87(12) . . . . ? C5 Cr1 C9 C8 -101.78(13) . . . . ? C2 Cr1 C9 C4 -1.8(2) . . . . ? C1 Cr1 C9 C4 -90.95(13) . . . . ? C3 Cr1 C9 C4 -175.94(12) . . . . ? C7 Cr1 C9 C4 104.25(13) . . . . ? C6 Cr1 C9 C4 67.37(12) . . . . ? C5 Cr1 C9 C4 30.46(11) . . . . ? C8 Cr1 C9 C4 132.24(17) . . . . ? C2 Cr1 C9 C15 111.5(2) . . . . ? C1 Cr1 C9 C15 22.38(19) . . . . ? C3 Cr1 C9 C15 -62.6(2) . . . . ? C4 Cr1 C9 C15 113.3(2) . . . . ? C7 Cr1 C9 C15 -142.4(2) . . . . ? C6 Cr1 C9 C15 -179.30(19) . . . . ? C5 Cr1 C9 C15 143.8(2) . . . . ? C8 Cr1 C9 C15 -114.4(2) . . . . ? C6 C7 C13 O5 77.8(2) . . . . ? C8 C7 C13 O5 -102.8(2) . . . . ? Cr1 C7 C13 O5 166.62(13) . . . . ? C1 Cr1 C2 O2 125(8) . . . . ? C3 Cr1 C2 O2 -149(8) . . . . ? C4 Cr1 C2 O2 35(8) . . . . ? C7 Cr1 C2 O2 -57(8) . . . . ? C6 Cr1 C2 O2 -31(8) . . . . ? C9 Cr1 C2 O2 36(8) . . . . ? C5 Cr1 C2 O2 6(8) . . . . ? C8 Cr1 C2 O2 -52(8) . . . . ? C23 C22 C21 C20 -7.1(3) . . . . ? C28 C22 C21 C20 173.40(18) . . . . ? Cr2 C22 C21 C20 50.32(17) . . . . ? C23 C22 C21 C27 173.25(19) . . . . ? C28 C22 C21 C27 -6.2(3) . . . . ? Cr2 C22 C21 C27 -129.30(18) . . . . ? C23 C22 C21 Cr2 -57.45(17) . . . . ? C28 C22 C21 Cr2 123.08(18) . . . . ? C18 Cr2 C21 C20 -139.55(19) . . . . ? C16 Cr2 C21 C20 47.54(15) . . . . ? C17 Cr2 C21 C20 134.68(13) . . . . ? C22 Cr2 C21 C20 -134.84(18) . . . . ? C19 Cr2 C21 C20 -29.89(12) . . . . ? C23 Cr2 C21 C20 -104.54(13) . . . . ? C24 Cr2 C21 C20 -66.91(12) . . . . ? C18 Cr2 C21 C22 -4.7(2) . . . . ? C16 Cr2 C21 C22 -177.62(12) . . . . ? C17 Cr2 C21 C22 -90.48(13) . . . . ? C19 Cr2 C21 C22 104.95(13) . . . . ? C23 Cr2 C21 C22 30.30(11) . . . . ? C20 Cr2 C21 C22 134.84(18) . . . . ? C24 Cr2 C21 C22 67.93(12) . . . . ? C18 Cr2 C21 C27 106.3(3) . . . . ? C16 Cr2 C21 C27 -66.6(2) . . . . ? C17 Cr2 C21 C27 20.5(2) . . . . ? C22 Cr2 C21 C27 111.0(2) . . . . ? C19 Cr2 C21 C27 -144.1(2) . . . . ? C23 Cr2 C21 C27 141.3(2) . . . . ? C20 Cr2 C21 C27 -114.2(2) . . . . ? C24 Cr2 C21 C27 178.9(2) . . . . ? C18 Cr2 C17 O7 -148(12) . . . . ? C16 Cr2 C17 O7 125(12) . . . . ? C22 Cr2 C17 O7 -31(12) . . . . ? C19 Cr2 C17 O7 38(12) . . . . ? C23 Cr2 C17 O7 -58(12) . . . . ? C20 Cr2 C17 O7 34(12) . . . . ? C24 Cr2 C17 O7 -54(12) . . . . ? C21 Cr2 C17 O7 6(12) . . . . ? C22 C23 C24 C19 3.4(3) . . . . ? C29 C23 C24 C19 -177.13(18) . . . . ? Cr2 C23 C24 C19 -50.71(17) . . . . ? C22 C23 C24 C30 -176.63(19) . . . . ? C29 C23 C24 C30 2.9(3) . . . . ? Cr2 C23 C24 C30 129.28(19) . . . . ? C22 C23 C24 Cr2 54.09(17) . . . . ? C29 C23 C24 Cr2 -126.42(18) . . . . ? C18 Cr2 C24 C19 -137.90(13) . . . . ? C16 Cr2 C24 C19 -49.73(14) . . . . ? C17 Cr2 C24 C19 129.1(2) . . . . ? C22 Cr2 C24 C19 104.71(13) . . . . ? C23 Cr2 C24 C19 134.37(17) . . . . ? C20 Cr2 C24 C19 30.26(11) . . . . ? C21 Cr2 C24 C19 66.91(12) . . . . ? C18 Cr2 C24 C23 87.74(13) . . . . ? C16 Cr2 C24 C23 175.91(12) . . . . ? C17 Cr2 C24 C23 -5.3(2) . . . . ? C22 Cr2 C24 C23 -29.66(11) . . . . ? C19 Cr2 C24 C23 -134.37(17) . . . . ? C20 Cr2 C24 C23 -104.11(12) . . . . ? C21 Cr2 C24 C23 -67.46(12) . . . . ? C18 Cr2 C24 C30 -23.1(2) . . . . ? C16 Cr2 C24 C30 65.1(2) . . . . ? C17 Cr2 C24 C30 -116.1(2) . . . . ? C22 Cr2 C24 C30 -140.5(2) . . . . ? C19 Cr2 C24 C30 114.8(2) . . . . ? C23 Cr2 C24 C30 -110.8(2) . . . . ? C20 Cr2 C24 C30 145.0(2) . . . . ? C21 Cr2 C24 C30 -178.3(2) . . . . ? C23 C24 C19 C20 -5.9(3) . . . . ? C30 C24 C19 C20 174.10(19) . . . . ? Cr2 C24 C19 C20 -56.74(17) . . . . ? C23 C24 C19 C25 175.10(18) . . . . ? C30 C24 C19 C25 -4.9(3) . . . . ? Cr2 C24 C19 C25 124.28(19) . . . . ? C23 C24 C19 Cr2 50.83(17) . . . . ? C30 C24 C19 Cr2 -129.16(19) . . . . ? O9 C25 C19 C24 111.2(2) . . . . ? O9 C25 C19 C20 -67.8(2) . . . . ? O9 C25 C19 Cr2 -156.28(14) . . . . ? C18 Cr2 C19 C24 50.05(15) . . . . ? C16 Cr2 C19 C24 137.09(12) . . . . ? C17 Cr2 C19 C24 -136.36(19) . . . . ? C22 Cr2 C19 C24 -64.95(12) . . . . ? C23 Cr2 C19 C24 -28.05(11) . . . . ? C20 Cr2 C19 C24 -130.78(17) . . . . ? C21 Cr2 C19 C24 -101.71(13) . . . . ? C18 Cr2 C19 C20 -179.17(12) . . . . ? C16 Cr2 C19 C20 -92.13(13) . . . . ? C17 Cr2 C19 C20 -5.6(2) . . . . ? C22 Cr2 C19 C20 65.83(12) . . . . ? C23 Cr2 C19 C20 102.73(13) . . . . ? C24 Cr2 C19 C20 130.78(17) . . . . ? C21 Cr2 C19 C20 29.07(11) . . . . ? C18 Cr2 C19 C25 -67.0(2) . . . . ? C16 Cr2 C19 C25 19.99(18) . . . . ? C17 Cr2 C19 C25 106.6(2) . . . . ? C22 Cr2 C19 C25 177.96(19) . . . . ? C23 Cr2 C19 C25 -145.14(19) . . . . ? C20 Cr2 C19 C25 112.1(2) . . . . ? C24 Cr2 C19 C25 -117.1(2) . . . . ? C21 Cr2 C19 C25 141.20(19) . . . . ? C8 C7 C6 C5 -3.7(3) . . . . ? C13 C7 C6 C5 175.76(18) . . . . ? Cr1 C7 C6 C5 54.61(17) . . . . ? C8 C7 C6 C12 175.86(19) . . . . ? C13 C7 C6 C12 -4.7(3) . . . . ? Cr1 C7 C6 C12 -125.87(19) . . . . ? C8 C7 C6 Cr1 -58.27(17) . . . . ? C13 C7 C6 Cr1 121.14(18) . . . . ? C2 Cr1 C6 C7 -140.02(13) . . . . ? C1 Cr1 C6 C7 133.8(2) . . . . ? C3 Cr1 C6 C7 -50.88(14) . . . . ? C4 Cr1 C6 C7 103.98(13) . . . . ? C9 Cr1 C6 C7 66.24(12) . . . . ? C5 Cr1 C6 C7 131.85(17) . . . . ? C8 Cr1 C6 C7 30.40(11) . . . . ? C2 Cr1 C6 C5 88.13(13) . . . . ? C1 Cr1 C6 C5 1.9(3) . . . . ? C3 Cr1 C6 C5 177.27(12) . . . . ? C4 Cr1 C6 C5 -27.88(11) . . . . ? C7 Cr1 C6 C5 -131.85(17) . . . . ? C9 Cr1 C6 C5 -65.61(12) . . . . ? C8 Cr1 C6 C5 -101.45(13) . . . . ? C2 Cr1 C6 C12 -25.1(2) . . . . ? C1 Cr1 C6 C12 -111.3(2) . . . . ? C3 Cr1 C6 C12 64.0(2) . . . . ? C4 Cr1 C6 C12 -141.1(2) . . . . ? C7 Cr1 C6 C12 114.9(2) . . . . ? C9 Cr1 C6 C12 -178.9(2) . . . . ? C5 Cr1 C6 C12 -113.3(2) . . . . ? C8 Cr1 C6 C12 145.3(2) . . . . ? C18 Cr2 C16 O6 11(15) . . . . ? C17 Cr2 C16 O6 100(15) . . . . ? C22 Cr2 C16 O6 -175(100) . . . . ? C19 Cr2 C16 O6 -108(15) . . . . ? C23 Cr2 C16 O6 -75(15) . . . . ? C20 Cr2 C16 O6 -146(15) . . . . ? C24 Cr2 C16 O6 -80(15) . . . . ? C21 Cr2 C16 O6 -172(100) . . . . ? C16 Cr2 C18 O8 15(21) . . . . ? C17 Cr2 C18 O8 -73(21) . . . . ? C22 Cr2 C18 O8 -162(21) . . . . ? C19 Cr2 C18 O8 104(21) . . . . ? C23 Cr2 C18 O8 169(100) . . . . ? C20 Cr2 C18 O8 103(21) . . . . ? C24 Cr2 C18 O8 132(21) . . . . ? C21 Cr2 C18 O8 -159(21) . . . . ? C2 Cr1 C1 O1 97(9) . . . . ? C3 Cr1 C1 O1 8(9) . . . . ? C4 Cr1 C1 O1 -149(9) . . . . ? C7 Cr1 C1 O1 -78(9) . . . . ? C6 Cr1 C1 O1 -176(100) . . . . ? C9 Cr1 C1 O1 -111(9) . . . . ? C5 Cr1 C1 O1 -175(100) . . . . ? C8 Cr1 C1 O1 -84(9) . . . . ? C8 C9 C4 C5 -3.8(3) . . . . ? C15 C9 C4 C5 175.80(19) . . . . ? Cr1 C9 C4 C5 -58.41(17) . . . . ? C8 C9 C4 C10 174.84(18) . . . . ? C15 C9 C4 C10 -5.6(3) . . . . ? Cr1 C9 C4 C10 120.18(18) . . . . ? C8 C9 C4 Cr1 54.66(17) . . . . ? C15 C9 C4 Cr1 -125.79(19) . . . . ? O4 C10 C4 C5 -94.2(2) . . . . ? O4 C10 C4 C9 87.3(2) . . . . ? O4 C10 C4 Cr1 176.32(13) . . . . ? C2 Cr1 C4 C5 -51.26(14) . . . . ? C1 Cr1 C4 C5 -140.62(13) . . . . ? C3 Cr1 C4 C5 138.6(2) . . . . ? C7 Cr1 C4 C5 64.49(12) . . . . ? C6 Cr1 C4 C5 27.92(12) . . . . ? C9 Cr1 C4 C5 129.66(18) . . . . ? C8 Cr1 C4 C5 101.12(13) . . . . ? C2 Cr1 C4 C9 179.07(12) . . . . ? C1 Cr1 C4 C9 89.71(13) . . . . ? C3 Cr1 C4 C9 8.9(3) . . . . ? C7 Cr1 C4 C9 -65.17(12) . . . . ? C6 Cr1 C4 C9 -101.75(13) . . . . ? C5 Cr1 C4 C9 -129.66(18) . . . . ? C8 Cr1 C4 C9 -28.55(11) . . . . ? C2 Cr1 C4 C10 63.68(18) . . . . ? C1 Cr1 C4 C10 -25.68(17) . . . . ? C3 Cr1 C4 C10 -106.5(3) . . . . ? C7 Cr1 C4 C10 179.44(17) . . . . ? C6 Cr1 C4 C10 142.86(18) . . . . ? C9 Cr1 C4 C10 -115.4(2) . . . . ? C5 Cr1 C4 C10 114.9(2) . . . . ? C8 Cr1 C4 C10 -143.94(18) . . . . ? C2 Cr1 C3 O3 -80(4) . . . . ? C1 Cr1 C3 O3 9(4) . . . . ? C4 Cr1 C3 O3 91(4) . . . . ? C7 Cr1 C3 O3 162(4) . . . . ? C6 Cr1 C3 O3 -170(4) . . . . ? C9 Cr1 C3 O3 97(4) . . . . ? C5 Cr1 C3 O3 -166(4) . . . . ? C8 Cr1 C3 O3 125(4) . . . . ? C9 C4 C5 C6 7.1(3) . . . . ? C10 C4 C5 C6 -171.51(18) . . . . ? Cr1 C4 C5 C6 -50.97(17) . . . . ? C9 C4 C5 C11 -173.42(19) . . . . ? C10 C4 C5 C11 8.0(3) . . . . ? Cr1 C4 C5 C11 128.52(19) . . . . ? C9 C4 C5 Cr1 58.06(17) . . . . ? C10 C4 C5 Cr1 -120.54(18) . . . . ? C7 C6 C5 C4 -3.4(3) . . . . ? C12 C6 C5 C4 177.09(19) . . . . ? Cr1 C6 C5 C4 50.39(17) . . . . ? C7 C6 C5 C11 177.12(19) . . . . ? C12 C6 C5 C11 -2.4(3) . . . . ? Cr1 C6 C5 C11 -129.11(18) . . . . ? C7 C6 C5 Cr1 -53.77(17) . . . . ? C12 C6 C5 Cr1 126.70(19) . . . . ? C2 Cr1 C5 C4 134.44(13) . . . . ? C1 Cr1 C5 C4 46.50(15) . . . . ? C3 Cr1 C5 C4 -140.2(2) . . . . ? C7 Cr1 C5 C4 -105.07(13) . . . . ? C6 Cr1 C5 C4 -134.37(18) . . . . ? C9 Cr1 C5 C4 -30.92(12) . . . . ? C8 Cr1 C5 C4 -67.40(12) . . . . ? C2 Cr1 C5 C6 -91.19(13) . . . . ? C1 Cr1 C5 C6 -179.12(12) . . . . ? C3 Cr1 C5 C6 -5.8(3) . . . . ? C4 Cr1 C5 C6 134.37(18) . . . . ? C7 Cr1 C5 C6 29.30(11) . . . . ? C9 Cr1 C5 C6 103.45(13) . . . . ? C8 Cr1 C5 C6 66.97(12) . . . . ? C2 Cr1 C5 C11 20.9(2) . . . . ? C1 Cr1 C5 C11 -67.0(2) . . . . ? C3 Cr1 C5 C11 106.3(3) . . . . ? C4 Cr1 C5 C11 -113.5(2) . . . . ? C7 Cr1 C5 C11 141.4(2) . . . . ? C6 Cr1 C5 C11 112.1(2) . . . . ? C9 Cr1 C5 C11 -144.4(2) . . . . ? C8 Cr1 C5 C11 179.1(2) . . . . ? C22 C21 C20 C19 4.6(3) . . . . ? C27 C21 C20 C19 -175.79(18) . . . . ? Cr2 C21 C20 C19 53.99(17) . . . . ? C22 C21 C20 C26 -175.41(18) . . . . ? C27 C21 C20 C26 4.2(3) . . . . ? Cr2 C21 C20 C26 -126.00(19) . . . . ? C22 C21 C20 Cr2 -49.40(17) . . . . ? C27 C21 C20 Cr2 130.22(19) . . . . ? C24 C19 C20 C21 1.9(3) . . . . ? C25 C19 C20 C21 -179.09(18) . . . . ? Cr2 C19 C20 C21 -55.31(17) . . . . ? C24 C19 C20 C26 -178.11(18) . . . . ? C25 C19 C20 C26 0.9(3) . . . . ? Cr2 C19 C20 C26 124.68(18) . . . . ? C24 C19 C20 Cr2 57.21(17) . . . . ? C25 C19 C20 Cr2 -123.78(18) . . . . ? C18 Cr2 C20 C21 133.4(2) . . . . ? C16 Cr2 C20 C21 -139.70(13) . . . . ? C17 Cr2 C20 C21 -51.32(14) . . . . ? C22 Cr2 C20 C21 27.89(12) . . . . ? C19 Cr2 C20 C21 131.54(18) . . . . ? C23 Cr2 C20 C21 64.97(12) . . . . ? C24 Cr2 C20 C21 101.85(13) . . . . ? C18 Cr2 C20 C19 1.9(3) . . . . ? C16 Cr2 C20 C19 88.76(13) . . . . ? C17 Cr2 C20 C19 177.14(12) . . . . ? C22 Cr2 C20 C19 -103.65(13) . . . . ? C23 Cr2 C20 C19 -66.57(12) . . . . ? C24 Cr2 C20 C19 -29.69(11) . . . . ? C21 Cr2 C20 C19 -131.54(18) . . . . ? C18 Cr2 C20 C26 -111.6(3) . . . . ? C16 Cr2 C20 C26 -24.73(19) . . . . ? C17 Cr2 C20 C26 63.7(2) . . . . ? C22 Cr2 C20 C26 142.87(19) . . . . ? C19 Cr2 C20 C26 -113.5(2) . . . . ? C23 Cr2 C20 C26 179.95(19) . . . . ? C24 Cr2 C20 C26 -143.18(19) . . . . ? C21 Cr2 C20 C26 115.0(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O10 H10 O4 0.84 1.97 2.805(2) 171.8 1_454 O5 H5 O9 0.84 1.88 2.717(2) 172.4 . O9 H9 O10 0.84 1.92 2.697(2) 152.7 2_665 O4 H4 O5 0.97 1.77 2.719(2) 163.7 2_766 _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.601 _refine_diff_density_min -0.833 _refine_diff_density_rms 0.135 data_str560 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C10 H7 Br Cr O3' _chemical_formula_weight 307.07 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cr' 'Cr' 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 '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 6.7720(10) _cell_length_b 8.541(2) _cell_length_c 9.622(2) _cell_angle_alpha 83.31(3) _cell_angle_beta 88.37(3) _cell_angle_gamma 88.67(3) _cell_volume 552.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 20 _cell_measurement_theta_max 29 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.63 _exptl_crystal_size_min 0.48 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.846 _exptl_crystal_density_method ? _exptl_crystal_F_000 300 _exptl_absorpt_coefficient_mu 4.633 _exptl_absorpt_correction_type psi _exptl_absorpt_correction_T_min 0.322 _exptl_absorpt_correction_T_max 1.000 _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 'Nicolet R3mV ' _diffrn_measurement_method omega-2theta _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 2746 _diffrn_reflns_av_R_equivalents 0.0194 _diffrn_reflns_av_sigmaI/netI 0.0311 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.55 _reflns_number_total 2530 _reflns_number_observed 1904 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Nicolet R3' _computing_cell_refinement 'Nicolet R3' _computing_data_reduction XDISK _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics XP _computing_publication_material CIFTAB _refine_special_details ; Refinement on F^2^ for ALL reflections except for 5 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0880P)^2^+0.3430P] 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 'fixed thermal parameter' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2525 _refine_ls_number_parameters 136 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0655 _refine_ls_R_factor_obs 0.0464 _refine_ls_wR_factor_all 0.1487 _refine_ls_wR_factor_obs 0.1236 _refine_ls_goodness_of_fit_all 1.023 _refine_ls_goodness_of_fit_obs 1.051 _refine_ls_restrained_S_all 1.090 _refine_ls_restrained_S_obs 1.051 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cr Cr -0.41460(9) -0.34152(8) 0.73458(6) 0.0334(2) Uani 1 d . . Br Br 0.04026(8) 0.10108(6) 0.78902(5) 0.0550(2) Uani 1 d . . O1 O -0.7134(6) -0.2199(6) 0.5250(5) 0.0802(13) Uani 1 d . . O2 O -0.6235(8) -0.6471(6) 0.7784(5) 0.091(2) Uani 1 d . . O3 O -0.6763(7) -0.2322(6) 0.9607(5) 0.0792(13) Uani 1 d . . C1 C -0.5997(7) -0.2677(6) 0.6057(5) 0.0484(11) Uani 1 d . . C2 C -0.5436(8) -0.5298(7) 0.7623(5) 0.0539(12) Uani 1 d . . C3 C -0.5748(7) -0.2727(7) 0.8740(5) 0.0505(11) Uani 1 d . . C4 C -0.1520(7) -0.2996(6) 0.8551(5) 0.0448(10) Uani 1 d . . C5 C -0.1326(7) -0.4472(6) 0.8113(6) 0.0538(12) Uani 1 d . . C6 C -0.1481(7) -0.4692(6) 0.6705(6) 0.0555(13) Uani 1 d . . C7 C -0.1794(7) -0.3400(7) 0.5721(5) 0.0530(12) Uani 1 d . . C8 C -0.1971(7) -0.1899(5) 0.6141(5) 0.0431(10) Uani 1 d . . C9 C -0.1849(6) -0.1676(5) 0.7548(4) 0.0357(8) Uani 1 d . . C10 C -0.2118(8) -0.0076(6) 0.8000(6) 0.0530(12) Uani 1 d . . H4 H -0.0999 -0.2806 0.9864 0.080 Uiso 1 d . . H5 H -0.0518 -0.5142 0.8666 0.080 Uiso 1 d . . H6 H -0.1293 -0.5743 0.6376 0.080 Uiso 1 d . . H7 H -0.1540 -0.3600 0.5057 0.080 Uiso 1 d . . H8 H -0.1970 -0.0896 0.5653 0.080 Uiso 1 d . . H10 H -0.3088 0.0598 0.7162 0.080 Uiso 1 d . . H11 H -0.2516 -0.0121 0.8763 0.080 Uiso 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 Cr 0.0331(3) 0.0348(4) 0.0335(3) -0.0072(3) -0.0017(2) -0.0058(3) Br 0.0662(4) 0.0446(3) 0.0562(3) -0.0092(2) -0.0048(2) -0.0216(2) O1 0.064(2) 0.101(4) 0.073(3) 0.008(2) -0.029(2) -0.002(2) O2 0.100(3) 0.071(3) 0.101(4) 0.010(3) -0.023(3) -0.053(3) O3 0.075(3) 0.099(4) 0.063(3) -0.017(2) 0.020(2) 0.013(2) C1 0.043(2) 0.053(3) 0.049(3) -0.002(2) -0.006(2) -0.005(2) C2 0.050(3) 0.063(3) 0.051(3) -0.013(2) -0.005(2) -0.022(2) C3 0.045(2) 0.059(3) 0.048(3) -0.008(2) 0.003(2) -0.001(2) C4 0.042(2) 0.045(3) 0.048(2) -0.003(2) -0.010(2) -0.006(2) C5 0.042(2) 0.046(3) 0.072(3) 0.002(2) -0.014(2) 0.001(2) C6 0.043(2) 0.048(3) 0.081(4) -0.030(3) 0.002(2) 0.000(2) C7 0.051(3) 0.061(3) 0.052(3) -0.030(2) 0.011(2) -0.008(2) C8 0.044(2) 0.043(2) 0.042(2) -0.003(2) 0.005(2) -0.013(2) C9 0.036(2) 0.029(2) 0.043(2) -0.009(2) 0.001(2) -0.007(2) C10 0.055(3) 0.042(3) 0.065(3) -0.018(2) 0.001(2) -0.016(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr C2 1.837(5) . yes Cr C1 1.838(5) . yes Cr C3 1.842(5) . yes Cr C6 2.197(5) . yes Cr C7 2.199(5) . yes Cr C8 2.198(4) . yes Cr C5 2.203(5) . yes Cr C9 2.204(4) . yes Cr C4 2.209(4) . yes Br C10 1.956(5) . yes O1 C1 1.143(6) . ? O2 C2 1.142(6) . ? O3 C3 1.145(6) . ? C4 C5 1.377(7) . yes C4 C9 1.413(6) . yes C5 C6 1.397(8) . yes C6 C7 1.384(8) . yes C7 C8 1.391(7) . yes C8 C9 1.394(6) . yes C9 C10 1.488(6) . yes 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 Cr C1 89.0(2) . . ? C2 Cr C3 88.1(2) . . ? C1 Cr C3 89.4(2) . . ? C2 Cr C6 88.9(2) . . ? C1 Cr C6 120.6(2) . . ? C3 Cr C6 149.8(2) . . ? C2 Cr C7 112.5(2) . . ? C1 Cr C7 92.0(2) . . ? C3 Cr C7 159.4(2) . . ? C6 Cr C7 36.7(2) . . ? C2 Cr C8 149.1(2) . . ? C1 Cr C8 88.4(2) . . ? C3 Cr C8 122.7(2) . . ? C6 Cr C8 66.2(2) . . ? C7 Cr C8 36.9(2) . . ? C2 Cr C5 93.4(2) . . ? C1 Cr C5 157.3(2) . . ? C3 Cr C5 113.3(2) . . ? C6 Cr C5 37.0(2) . . ? C7 Cr C5 66.2(2) . . ? C8 Cr C5 77.9(2) . . ? C2 Cr C9 158.6(2) . . ? C1 Cr C9 112.3(2) . . ? C3 Cr C9 93.8(2) . . ? C6 Cr C9 78.8(2) . . ? C7 Cr C9 66.7(2) . . ? C8 Cr C9 36.9(2) . . ? C5 Cr C9 66.2(2) . . ? C2 Cr C4 121.4(2) . . ? C1 Cr C4 149.5(2) . . ? C3 Cr C4 89.7(2) . . ? C6 Cr C4 66.6(2) . . ? C7 Cr C4 78.8(2) . . ? C8 Cr C4 66.7(2) . . ? C5 Cr C4 36.4(2) . . ? C9 Cr C4 37.4(2) . . ? O1 C1 Cr 179.1(5) . . ? O2 C2 Cr 179.4(5) . . ? O3 C3 Cr 178.8(5) . . ? C5 C4 C9 119.2(5) . . ? C5 C4 Cr 71.6(3) . . ? C9 C4 Cr 71.1(2) . . ? C4 C5 C6 121.4(5) . . ? C4 C5 Cr 72.1(3) . . ? C6 C5 Cr 71.3(3) . . ? C7 C6 C5 119.6(5) . . ? C7 C6 Cr 71.7(3) . . ? C5 C6 Cr 71.7(3) . . ? C6 C7 C8 119.9(5) . . ? C6 C7 Cr 71.6(3) . . ? C8 C7 Cr 71.5(3) . . ? C7 C8 C9 120.7(4) . . ? C7 C8 Cr 71.6(3) . . ? C9 C8 Cr 71.7(2) . . ? C8 C9 C4 119.3(4) . . ? C8 C9 C10 120.6(4) . . ? C4 C9 C10 120.1(4) . . ? C8 C9 Cr 71.3(2) . . ? C4 C9 Cr 71.5(2) . . ? C10 C9 Cr 127.6(3) . . ? C9 C10 Br 110.4(3) . . ? _refine_diff_density_max 0.690 _refine_diff_density_min -0.713 _refine_diff_density_rms 0.129 data_str563 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C22 H20 Cr2 O10' _chemical_formula_weight 548.38 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cr' 'Cr' 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 12.882(3) _cell_length_b 13.217(3) _cell_length_c 14.087(3) _cell_angle_alpha 90.00 _cell_angle_beta 112.52(3) _cell_angle_gamma 90.00 _cell_volume 2215.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 29 _cell_measurement_theta_min 22 _cell_measurement_theta_max 29 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.82 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.644 _exptl_crystal_density_method ? _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 1.038 _exptl_absorpt_correction_type psi scans _exptl_absorpt_correction_T_min 0.744 _exptl_absorpt_correction_T_max 1.000 _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 Nicolet R3mV _diffrn_measurement_method omega-2theta _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 4084 _diffrn_reflns_av_R_equivalents 0.0191 _diffrn_reflns_av_sigmaI/netI 0.0147 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 25.05 _reflns_number_total 3903 _reflns_number_observed 3352 _reflns_observed_criterion >2sigma(I) _computing_data_collection Nicolet R3 _computing_cell_refinement Nicolet R3 _computing_data_reduction XDISK _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics XP _computing_publication_material CIFTAB _refine_special_details ; Refinement on F^2^ for ALL reflections except for 5 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0646P)^2^+1.4835P] 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 fixed thermal parameter _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3898 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0443 _refine_ls_R_factor_obs 0.0375 _refine_ls_wR_factor_all 0.1107 _refine_ls_wR_factor_obs 0.1014 _refine_ls_goodness_of_fit_all 1.027 _refine_ls_goodness_of_fit_obs 1.070 _refine_ls_restrained_S_all 1.077 _refine_ls_restrained_S_obs 1.070 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cr1 Cr 0.10049(3) 0.85694(3) 0.84948(3) 0.02559(13) Uani 1 d . . O1 O -0.0756(2) 1.0107(2) 0.7437(2) 0.0567(6) Uani 1 d . . O2 O 0.0571(2) 0.8908(2) 1.0406(2) 0.0535(5) Uani 1 d . . O3 O -0.0703(2) 0.6915(2) 0.7981(2) 0.0639(6) Uani 1 d . . O4 O 0.0648(2) 0.88623(15) 0.55191(14) 0.0469(5) Uani 1 d . . O5 O 0.3417(2) 0.64788(15) 1.0340(2) 0.0546(5) Uani 1 d . . C1 C -0.0095(2) 0.9514(2) 0.7850(2) 0.0356(6) Uani 1 d . . C2 C 0.0756(2) 0.8781(2) 0.9675(2) 0.0336(5) Uani 1 d . . C3 C -0.0056(2) 0.7556(2) 0.8173(2) 0.0386(6) Uani 1 d . . C4 C 0.1775(2) 0.8963(2) 0.7363(2) 0.0296(5) Uani 1 d . . C5 C 0.1758(2) 0.7913(2) 0.7453(2) 0.0311(5) Uani 1 d . . C6 C 0.2247(2) 0.7440(2) 0.8432(2) 0.0311(5) Uani 1 d . . C7 C 0.2778(2) 0.8014(2) 0.9320(2) 0.0309(5) Uani 1 d . . C8 C 0.2776(2) 0.9079(2) 0.9224(2) 0.0335(5) Uani 1 d . . C9 C 0.2288(2) 0.9551(2) 0.8273(2) 0.0320(5) Uani 1 d . . C10 C 0.1279(2) 0.9509(2) 0.6341(2) 0.0376(6) Uani 1 d . . C11 C 0.3340(2) 0.7548(2) 1.0372(2) 0.0428(6) Uani 1 d . . H1 H 0.1096 0.8585 0.5112 0.080 Uiso 1 d . . H2 H 0.4082 0.6416 1.0266 0.080 Uiso 1 d . . H5 H 0.1366 0.7339 0.6858 0.080 Uiso 1 d . . H6 H 0.2148 0.6553 0.8487 0.080 Uiso 1 d . . H8 H 0.3146 0.9400 0.9902 0.080 Uiso 1 d . . H9 H 0.2386 1.0342 0.8256 0.080 Uiso 1 d . . H10A H 0.1945 0.9760 0.6236 0.080 Uiso 1 d . . H10B H 0.0817 1.0172 0.6382 0.080 Uiso 1 d . . H11A H 0.2850 0.7830 1.0779 0.080 Uiso 1 d . . H11B H 0.4169 0.7827 1.0731 0.080 Uiso 1 d . . Cr2 Cr 0.08683(3) 0.64278(3) 1.32103(3) 0.02711(13) Uani 1 d . . O21 O -0.0866(2) 0.4808(2) 1.2374(2) 0.0739(8) Uani 1 d . . O22 O 0.0646(2) 0.6253(2) 1.5243(2) 0.0572(6) Uani 1 d . . O23 O -0.0912(2) 0.8026(2) 1.2604(2) 0.0581(6) Uani 1 d . . O24 O 0.2555(2) 0.8460(2) 1.5096(2) 0.0637(6) Uani 1 d . . O25 O 0.1866(2) 0.5190(2) 1.0650(2) 0.0648(6) Uani 1 d . . C21 C -0.0204(2) 0.5426(2) 1.2692(2) 0.0428(6) Uani 1 d . . C22 C 0.0723(2) 0.6316(2) 1.4455(2) 0.0367(6) Uani 1 d . . C23 C -0.0249(2) 0.7402(2) 1.2834(2) 0.0367(6) Uani 1 d . . C24 C 0.2583(2) 0.7057(2) 1.3984(2) 0.0316(5) Uani 1 d . . C25 C 0.2018(2) 0.7604(2) 1.3083(2) 0.0349(5) Uani 1 d . . C26 C 0.1548(2) 0.7101(2) 1.2132(2) 0.0386(6) Uani 1 d . . C27 C 0.1613(2) 0.6049(2) 1.2063(2) 0.0359(5) Uani 1 d . . C28 C 0.2187(2) 0.5494(2) 1.2979(2) 0.0347(5) Uani 1 d . . C29 C 0.2666(2) 0.5995(2) 1.3914(2) 0.0318(5) Uani 1 d . . C30 C 0.3107(2) 0.7564(2) 1.5019(2) 0.0491(7) Uani 1 d . . C31 C 0.1073(2) 0.5510(3) 1.1042(2) 0.0525(8) Uani 1 d . . H21 H 0.2830 0.9011 1.4818 0.080 Uiso 1 d . . H22 H 0.2274 0.5821 1.0592 0.080 Uiso 1 d . . H25 H 0.1932 0.8459 1.3135 0.080 Uiso 1 d . . H26 H 0.1116 0.7654 1.1546 0.080 Uiso 1 d . . H28 H 0.2233 0.4662 1.2956 0.080 Uiso 1 d . . H29 H 0.3075 0.5616 1.4551 0.080 Uiso 1 d . . H30A H 0.3884 0.7585 1.5133 0.080 Uiso 1 d . . H30B H 0.3011 0.6977 1.5607 0.080 Uiso 1 d . . H31A H 0.0640 0.4827 1.1103 0.080 Uiso 1 d . . H31B H 0.0421 0.6021 1.0502 0.080 Uiso 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 Cr1 0.0229(2) 0.0223(2) 0.0336(2) -0.00081(14) 0.0131(2) 0.00076(13) O1 0.0451(11) 0.0544(13) 0.0724(14) 0.0214(11) 0.0244(10) 0.0245(10) O2 0.0765(15) 0.0517(12) 0.0455(11) 0.0048(9) 0.0379(11) 0.0062(11) O3 0.0438(12) 0.0460(12) 0.109(2) -0.0204(12) 0.0372(12) -0.0179(10) O4 0.0489(11) 0.0500(11) 0.0385(10) -0.0022(8) 0.0129(9) -0.0041(9) O5 0.0514(12) 0.0459(12) 0.0657(14) 0.0204(9) 0.0214(10) 0.0122(9) C1 0.0324(12) 0.0372(14) 0.0428(13) 0.0019(11) 0.0205(11) 0.0005(11) C2 0.0335(13) 0.0268(12) 0.0422(14) 0.0034(10) 0.0162(11) 0.0015(10) C3 0.0291(12) 0.0341(13) 0.057(2) -0.0067(12) 0.0212(11) 0.0016(11) C4 0.0279(12) 0.0289(12) 0.0373(12) 0.0004(10) 0.0184(10) -0.0010(9) C5 0.0296(12) 0.0303(12) 0.0367(12) -0.0047(10) 0.0163(10) 0.0032(9) C6 0.0276(11) 0.0255(11) 0.0434(13) -0.0017(10) 0.0171(10) 0.0036(9) C7 0.0219(11) 0.0334(13) 0.0380(12) 0.0027(10) 0.0121(9) 0.0033(9) C8 0.0278(12) 0.0325(13) 0.0404(13) -0.0069(10) 0.0133(10) -0.0057(10) C9 0.0287(11) 0.0283(12) 0.0429(13) -0.0018(10) 0.0181(10) -0.0047(9) C10 0.0437(14) 0.0349(14) 0.0377(13) 0.0024(10) 0.0193(11) -0.0024(11) C11 0.0349(13) 0.047(2) 0.0416(14) 0.0066(12) 0.0095(11) 0.0034(12) Cr2 0.0239(2) 0.0244(2) 0.0356(2) 0.00136(14) 0.0143(2) 0.00090(13) O21 0.0532(13) 0.0605(15) 0.119(2) -0.0413(15) 0.0458(14) -0.0279(12) O22 0.0693(15) 0.0663(14) 0.0474(12) 0.0082(10) 0.0352(11) 0.0121(11) O23 0.0431(11) 0.0486(12) 0.089(2) 0.0209(11) 0.0323(11) 0.0192(10) O24 0.071(2) 0.0488(12) 0.085(2) -0.0267(11) 0.0457(14) -0.0105(11) O25 0.0678(14) 0.078(2) 0.0631(14) -0.0272(12) 0.0415(12) -0.0150(12) C21 0.0368(14) 0.0373(14) 0.063(2) -0.0119(12) 0.0280(13) -0.0022(12) C22 0.0337(13) 0.0328(13) 0.046(2) 0.0024(10) 0.0174(11) 0.0029(10) C23 0.0292(12) 0.0379(14) 0.0468(14) 0.0043(11) 0.0188(11) 0.0004(11) C24 0.0243(11) 0.0311(12) 0.0414(13) -0.0012(10) 0.0148(10) -0.0016(9) C25 0.0316(12) 0.0253(12) 0.0532(15) 0.0049(11) 0.0221(11) -0.0019(10) C26 0.0337(13) 0.0446(15) 0.0416(14) 0.0135(11) 0.0190(11) 0.0030(11) C27 0.0284(12) 0.0454(14) 0.0387(13) -0.0042(11) 0.0181(10) -0.0010(11) C28 0.0305(12) 0.0320(13) 0.0464(14) -0.0020(10) 0.0200(11) 0.0019(10) C29 0.0264(11) 0.0296(12) 0.0394(13) 0.0049(10) 0.0125(10) 0.0045(9) C30 0.0416(15) 0.050(2) 0.053(2) -0.0167(13) 0.0150(13) -0.0061(13) C31 0.043(2) 0.072(2) 0.045(2) -0.0169(14) 0.0188(13) -0.0043(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 C2 1.831(3) . yes Cr1 C3 1.842(3) . yes Cr1 C1 1.846(3) . yes Cr1 C6 2.215(2) . yes Cr1 C9 2.215(2) . yes Cr1 C8 2.218(2) . yes Cr1 C5 2.223(2) . yes Cr1 C4 2.238(2) . yes Cr1 C7 2.252(2) . yes O1 C1 1.139(3) . ? O2 C2 1.154(3) . ? O3 C3 1.145(3) . ? O4 C10 1.418(3) . yes O5 C11 1.418(4) . yes C4 C5 1.394(3) . yes C4 C9 1.426(3) . yes C4 C10 1.515(3) . yes C5 C6 1.423(3) . yes C6 C7 1.398(3) . yes C7 C8 1.414(4) . yes C7 C11 1.510(3) . yes C8 C9 1.391(4) . yes Cr2 C22 1.839(3) . ? Cr2 C21 1.850(3) . ? Cr2 C23 1.851(3) . ? Cr2 C25 2.202(2) . ? Cr2 C26 2.211(2) . ? Cr2 C29 2.217(2) . ? Cr2 C24 2.217(2) . ? Cr2 C28 2.223(2) . ? Cr2 C27 2.230(2) . ? O21 C21 1.141(3) . ? O22 C22 1.155(3) . ? O23 C23 1.141(3) . ? O24 C30 1.407(4) . ? O25 C31 1.400(3) . ? C24 C25 1.399(3) . ? C24 C29 1.414(3) . ? C24 C30 1.509(4) . ? C25 C26 1.409(4) . ? C26 C27 1.398(4) . ? C27 C28 1.421(4) . ? C27 C31 1.514(4) . ? C28 C29 1.391(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 C2 Cr1 C3 87.87(11) . . ? C2 Cr1 C1 88.61(11) . . ? C3 Cr1 C1 90.77(12) . . ? C2 Cr1 C6 121.29(10) . . ? C3 Cr1 C6 88.83(10) . . ? C1 Cr1 C6 150.05(10) . . ? C2 Cr1 C9 115.99(10) . . ? C3 Cr1 C9 156.12(10) . . ? C1 Cr1 C9 90.44(10) . . ? C6 Cr1 C9 78.45(9) . . ? C2 Cr1 C8 92.28(11) . . ? C3 Cr1 C8 150.43(10) . . ? C1 Cr1 C8 118.80(10) . . ? C6 Cr1 C8 65.96(9) . . ? C9 Cr1 C8 36.56(9) . . ? C2 Cr1 C5 158.69(10) . . ? C3 Cr1 C5 91.39(10) . . ? C1 Cr1 C5 112.70(10) . . ? C6 Cr1 C5 37.41(9) . . ? C9 Cr1 C5 66.26(9) . . ? C8 Cr1 C5 78.03(9) . . ? C2 Cr1 C4 152.99(10) . . ? C3 Cr1 C4 118.90(10) . . ? C1 Cr1 C4 87.61(10) . . ? C6 Cr1 C4 66.66(9) . . ? C9 Cr1 C4 37.35(9) . . ? C8 Cr1 C4 66.49(9) . . ? C5 Cr1 C4 36.42(9) . . ? C2 Cr1 C7 94.38(10) . . ? C3 Cr1 C7 113.61(10) . . ? C1 Cr1 C7 155.51(10) . . ? C6 Cr1 C7 36.46(9) . . ? C9 Cr1 C7 66.42(9) . . ? C8 Cr1 C7 36.88(9) . . ? C5 Cr1 C7 66.48(9) . . ? C4 Cr1 C7 78.74(9) . . ? O1 C1 Cr1 178.1(2) . . ? O2 C2 Cr1 178.3(2) . . ? O3 C3 Cr1 178.9(2) . . ? C5 C4 C9 118.6(2) . . ? C5 C4 C10 123.0(2) . . ? C9 C4 C10 118.4(2) . . ? C5 C4 Cr1 71.21(13) . . ? C9 C4 Cr1 70.48(13) . . ? C10 C4 Cr1 130.3(2) . . ? C4 C5 C6 120.6(2) . . ? C4 C5 Cr1 72.37(13) . . ? C6 C5 Cr1 70.98(13) . . ? C7 C6 C5 120.8(2) . . ? C7 C6 Cr1 73.21(13) . . ? C5 C6 Cr1 71.61(13) . . ? C6 C7 C8 118.2(2) . . ? C6 C7 C11 122.9(2) . . ? C8 C7 C11 118.9(2) . . ? C6 C7 Cr1 70.33(13) . . ? C8 C7 Cr1 70.25(13) . . ? C11 C7 Cr1 130.6(2) . . ? C9 C8 C7 121.5(2) . . ? C9 C8 Cr1 71.64(14) . . ? C7 C8 Cr1 72.88(13) . . ? C8 C9 C4 120.3(2) . . ? C8 C9 Cr1 71.80(14) . . ? C4 C9 Cr1 72.17(13) . . ? O4 C10 C4 113.0(2) . . ? O5 C11 C7 112.9(2) . . ? C22 Cr2 C21 89.18(12) . . ? C22 Cr2 C23 88.68(11) . . ? C21 Cr2 C23 90.20(12) . . ? C22 Cr2 C25 116.83(11) . . ? C21 Cr2 C25 153.82(12) . . ? C23 Cr2 C25 87.65(10) . . ? C22 Cr2 C26 154.07(11) . . ? C21 Cr2 C26 116.69(12) . . ? C23 Cr2 C26 89.59(10) . . ? C25 Cr2 C26 37.25(10) . . ? C22 Cr2 C29 91.33(11) . . ? C21 Cr2 C29 119.06(11) . . ? C23 Cr2 C29 150.73(11) . . ? C25 Cr2 C29 66.35(9) . . ? C26 Cr2 C29 77.89(9) . . ? C22 Cr2 C24 90.41(11) . . ? C21 Cr2 C24 156.24(11) . . ? C23 Cr2 C24 113.54(10) . . ? C25 Cr2 C24 36.92(9) . . ? C26 Cr2 C24 66.71(9) . . ? C29 Cr2 C24 37.19(9) . . ? C22 Cr2 C28 117.26(10) . . ? C21 Cr2 C28 92.38(10) . . ? C23 Cr2 C28 153.95(10) . . ? C25 Cr2 C28 78.74(9) . . ? C26 Cr2 C28 66.18(9) . . ? C29 Cr2 C28 36.50(9) . . ? C24 Cr2 C28 66.84(9) . . ? C22 Cr2 C27 154.45(10) . . ? C21 Cr2 C27 90.95(11) . . ? C23 Cr2 C27 116.86(11) . . ? C25 Cr2 C27 67.06(10) . . ? C26 Cr2 C27 36.70(10) . . ? C29 Cr2 C27 66.45(9) . . ? C24 Cr2 C27 79.42(9) . . ? C28 Cr2 C27 37.21(9) . . ? O21 C21 Cr2 179.9(2) . . ? O22 C22 Cr2 179.0(2) . . ? O23 C23 Cr2 177.7(2) . . ? C25 C24 C29 118.5(2) . . ? C25 C24 C30 122.1(2) . . ? C29 C24 C30 119.4(2) . . ? C25 C24 Cr2 70.94(13) . . ? C29 C24 Cr2 71.42(13) . . ? C30 C24 Cr2 129.4(2) . . ? C24 C25 C26 120.2(2) . . ? C24 C25 Cr2 72.14(13) . . ? C26 C25 Cr2 71.73(14) . . ? C27 C26 C25 121.4(2) . . ? C27 C26 Cr2 72.39(14) . . ? C25 C26 Cr2 71.02(14) . . ? C26 C27 C28 118.3(2) . . ? C26 C27 C31 121.0(2) . . ? C28 C27 C31 120.6(3) . . ? C26 C27 Cr2 70.91(14) . . ? C28 C27 Cr2 71.16(14) . . ? C31 C27 Cr2 128.7(2) . . ? C29 C28 C27 120.1(2) . . ? C29 C28 Cr2 71.51(14) . . ? C27 C28 Cr2 71.63(14) . . ? C28 C29 C24 121.4(2) . . ? C28 C29 Cr2 71.99(14) . . ? C24 C29 Cr2 71.39(13) . . ? O24 C30 C24 113.3(2) . . ? O25 C31 C27 112.2(2) . . ? _refine_diff_density_max 0.342 _refine_diff_density_min -0.655 _refine_diff_density_rms 0.084