# Copyright The Royal Societ of Chemistry, 1999 # CCDC Number: 440/106 # Supplementary crystallographic data for manuscript # "pi-Bonded organometallic building blocks for supramolecular # chemistry," by Reinaldo Atencio, Lee Brammer,* Shiyue Fang, # and F. Christopher Pigge. # # Data for compound 1 # ------------------- data_l5898_complex_1 _publ_contact_author_name 'Lee Brammer' _publ_contact_author_address ; Department of Chemistry University of Missouri-St.Louis 8001 Natural Bridge Road St. Louis, MO 63121-4499 USA ; _publ_contact_author_phone '+1-314-516-5345' _publ_contact_author_fax '+1-314-516-5342' _publ_contact_author_email 'lee.brammer@umsl.edu' _publ_section_title ; pi-Bonded organometallic building blocks for supramolecular chemistry. ; _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C10 H6 Cr O5' _chemical_formula_weight 258.15 _chemical_melting_point ? _chemical_compound_source 'synthesis' 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 7.0349(3) _cell_length_b 7.2332(3) _cell_length_c 11.1518(5) _cell_angle_alpha 88.7100(10) _cell_angle_beta 81.7330(10) _cell_angle_gamma 63.0120(10) _cell_volume 499.82(4) _cell_formula_units_Z 2 _cell_measurement_temperature 208(2) _cell_measurement_reflns_used 3326 _cell_measurement_theta_min 1.85 _cell_measurement_theta_max 29.30 _exptl_crystal_description plates _exptl_crystal_colour orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.715 _exptl_crystal_density_method ? _exptl_crystal_F_000 260 _exptl_absorpt_coefficient_mu 1.145 _exptl_absorpt_correction_type 'empirical: (SADABS)' _exptl_absorpt_correction_T_min 0.610590 _exptl_absorpt_correction_T_max 0.843461 _exptl_absorpt_process_details ; Absorption correction was based upon symmetry equivalent and repeated intensity measurements using the program SADABS (Sheldrick, 1995), which is based upon the method of Blessing (Blessing, 1995). ; _exptl_special_details ; Data were collected with a Siemens SMART CCD-based diffractometer using /w-scans of width 0.3 deg. and 25s duration at a crystal-to-detector distance of 4.908 cm. Intensity decay over the course of the data collection was evaluated by recollecting the first 50 frames of data at the end of the experiment. No significant decay was noted. ; _diffrn_ambient_temperature 208(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART' _diffrn_measurement_method '\w-scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 5785 _diffrn_reflns_av_R_equivalents 0.0380 _diffrn_reflns_av_sigmaI/netI 0.0547 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 29.31 _reflns_number_total 2437 _reflns_number_observed 1868 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART (Siemens, 1994)' _computing_cell_refinement 'SAINT (Siemens, 1994)' _computing_data_reduction 'SAINT (Siemens, 1994)' _computing_structure_solution 'SHELXTL (Siemens, 1994)' _computing_structure_refinement 'SHELXTL (Siemens, 1994)' _computing_molecular_graphics 'SHELXTL (Siemens, 1994)' _computing_publication_material 'SHELXTL (Siemens, 1994)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 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^)+(0.0440P)^2^+0.5303P] 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 ; Arene hydrogen atoms were included in the final cycles in their calculated positions; the carboxyl hydrogen was located directly from a difference map. All hydrogen atoms were refined using riding models. ; _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2437 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0732 _refine_ls_R_factor_obs 0.0449 _refine_ls_wR_factor_all 0.1158 _refine_ls_wR_factor_obs 0.0981 _refine_ls_goodness_of_fit_all 1.058 _refine_ls_goodness_of_fit_obs 1.032 _refine_ls_restrained_S_all 1.058 _refine_ls_restrained_S_obs 1.032 _refine_ls_shift/esd_max 0.002 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cr Cr 0.18733(8) 0.13063(7) 0.21501(4) 0.0270(2) Uani 1 d . . O1 O -0.3657(3) 0.5841(3) 0.3815(2) 0.0407(6) Uani 1 d . . H1 H -0.5212(3) 0.6357(3) 0.4268(2) 0.049 Uiso 1 d R . O2 O -0.2465(4) 0.3219(4) 0.5058(2) 0.0403(6) Uani 1 d . . O10 O -0.0856(4) -0.0809(4) 0.2984(2) 0.0401(6) Uani 1 d . . C10 C 0.0231(5) -0.0032(4) 0.2652(3) 0.0286(6) Uani 1 d . . C1 C -0.2149(5) 0.4250(5) 0.4215(3) 0.0294(6) Uani 1 d . . C2 C 0.0096(5) 0.3665(4) 0.3618(3) 0.0277(6) Uani 1 d . . C9 C 0.4017(6) -0.1199(6) 0.1408(3) 0.0420(8) Uani 1 d . . O9 O 0.5298(5) -0.2772(4) 0.0967(3) 0.0676(9) Uani 1 d . . C3 C 0.1852(5) 0.1990(5) 0.4063(3) 0.0319(7) Uani 1 d . . H3 H 0.1600(5) 0.1332(5) 0.4760(3) 0.038 Uiso 1 calc R . O8 O -0.0039(6) 0.2264(5) -0.0154(3) 0.0695(9) Uani 1 d . . C6 C 0.2606(5) 0.3996(5) 0.1979(3) 0.0349(7) Uani 1 d . . H6 H 0.2866(5) 0.4679(5) 0.1295(3) 0.042 Uiso 1 calc R . C7 C 0.0475(5) 0.4652(5) 0.2575(3) 0.0304(7) Uani 1 d . . H7 H -0.0686(5) 0.5745(5) 0.2276(3) 0.036 Uiso 1 calc R . C8 C 0.0706(6) 0.1884(5) 0.0729(3) 0.0419(8) Uani 1 d . . C5 C 0.4325(5) 0.2334(5) 0.2403(3) 0.0378(8) Uani 1 d . . H5 H 0.5736(5) 0.1877(5) 0.1991(3) 0.045 Uiso 1 calc R . C4 C 0.3949(5) 0.1330(5) 0.3456(3) 0.0360(7) Uani 1 d . . H4 H 0.5113(5) 0.0223(5) 0.3745(3) 0.043 Uiso 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 Cr 0.0299(3) 0.0280(3) 0.0212(3) 0.0035(2) -0.0013(2) -0.0123(2) O1 0.0292(11) 0.0357(12) 0.0445(14) 0.0085(10) -0.0001(10) -0.0056(10) O2 0.0347(12) 0.0424(13) 0.0336(13) 0.0087(10) 0.0042(10) -0.0117(10) O10 0.0403(13) 0.0383(12) 0.0448(14) 0.0037(10) -0.0003(11) -0.0223(11) C10 0.0302(15) 0.0271(14) 0.0218(15) -0.0007(11) -0.0038(11) -0.0073(12) C1 0.0318(15) 0.0294(15) 0.0230(15) -0.0022(12) -0.0020(12) -0.0109(12) C2 0.0330(15) 0.0276(14) 0.0212(14) -0.0044(11) -0.0001(12) -0.0134(12) C9 0.044(2) 0.044(2) 0.033(2) 0.0024(15) 0.0062(15) -0.019(2) O9 0.064(2) 0.046(2) 0.062(2) -0.0145(14) 0.0245(15) -0.0076(14) C3 0.035(2) 0.040(2) 0.0209(15) 0.0018(12) -0.0042(12) -0.0168(14) O8 0.121(3) 0.065(2) 0.042(2) 0.0221(14) -0.046(2) -0.051(2) C6 0.042(2) 0.037(2) 0.032(2) 0.0045(13) -0.0022(14) -0.0240(15) C7 0.033(2) 0.0256(14) 0.033(2) 0.0014(12) -0.0033(13) -0.0141(12) C8 0.062(2) 0.034(2) 0.036(2) 0.0071(14) -0.012(2) -0.026(2) C5 0.032(2) 0.050(2) 0.036(2) 0.0050(15) -0.0021(13) -0.0230(15) C4 0.031(2) 0.046(2) 0.032(2) 0.0063(14) -0.0085(13) -0.0182(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 Cr C10 1.841(3) . ? Cr C8 1.843(4) . ? Cr C9 1.863(4) . ? Cr C2 2.180(3) . ? Cr C7 2.192(3) . ? Cr C3 2.196(3) . ? Cr C4 2.212(3) . ? Cr C5 2.218(3) . ? Cr C6 2.225(3) . ? O1 C1 1.285(4) . ? O1 H1 1.03 . ? O2 C1 1.245(4) . ? O10 C10 1.156(4) . ? C1 C2 1.490(4) . ? C2 C7 1.407(4) . ? C2 C3 1.425(4) . ? C9 O9 1.148(4) . ? C3 C4 1.396(4) . ? C3 H3 0.94 . ? O8 C8 1.151(4) . ? C6 C5 1.397(5) . ? C6 C7 1.413(4) . ? C6 H6 0.94 . ? C7 H7 0.94 . ? C5 C4 1.423(5) . ? C5 H5 0.94 . ? C4 H4 0.94 . ? 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 C10 Cr C8 89.40(14) . . ? C10 Cr C9 88.50(14) . . ? C8 Cr C9 88.5(2) . . ? C10 Cr C2 90.32(12) . . ? C8 Cr C2 114.74(14) . . ? C9 Cr C2 156.70(14) . . ? C10 Cr C7 118.32(12) . . ? C8 Cr C7 89.07(13) . . ? C9 Cr C7 153.04(14) . . ? C2 Cr C7 37.53(11) . . ? C10 Cr C3 88.80(13) . . ? C8 Cr C3 152.65(14) . . ? C9 Cr C3 118.69(14) . . ? C2 Cr C3 38.00(11) . . ? C7 Cr C3 68.00(12) . . ? C10 Cr C4 114.60(13) . . ? C8 Cr C4 156.00(14) . . ? C9 Cr C4 91.97(15) . . ? C2 Cr C4 67.47(12) . . ? C7 Cr C4 79.71(12) . . ? C3 Cr C4 36.93(11) . . ? C10 Cr C5 152.02(13) . . ? C8 Cr C5 118.55(14) . . ? C9 Cr C5 90.82(15) . . ? C2 Cr C5 79.50(12) . . ? C7 Cr C5 67.00(12) . . ? C3 Cr C5 67.15(12) . . ? C4 Cr C5 37.46(12) . . ? C10 Cr C6 155.55(12) . . ? C8 Cr C6 91.40(14) . . ? C9 Cr C6 115.95(14) . . ? C2 Cr C6 67.23(12) . . ? C7 Cr C6 37.29(11) . . ? C3 Cr C6 79.41(12) . . ? C4 Cr C6 66.88(12) . . ? C5 Cr C6 36.65(12) . . ? C1 O1 H1 117.6(2) . . ? O10 C10 Cr 177.7(3) . . ? O2 C1 O1 124.0(3) . . ? O2 C1 C2 119.6(3) . . ? O1 C1 C2 116.4(3) . . ? C7 C2 C3 120.1(3) . . ? C7 C2 C1 120.5(3) . . ? C3 C2 C1 119.2(3) . . ? C7 C2 Cr 71.7(2) . . ? C3 C2 Cr 71.6(2) . . ? C1 C2 Cr 125.2(2) . . ? O9 C9 Cr 177.8(3) . . ? C4 C3 C2 119.6(3) . . ? C4 C3 Cr 72.1(2) . . ? C2 C3 Cr 70.4(2) . . ? C4 C3 H3 120.2(2) . . ? C2 C3 H3 120.2(2) . . ? Cr C3 H3 129.74(8) . . ? C5 C6 C7 120.1(3) . . ? C5 C6 Cr 71.4(2) . . ? C7 C6 Cr 70.1(2) . . ? C5 C6 H6 120.0(2) . . ? C7 C6 H6 120.0(2) . . ? Cr C6 H6 131.35(9) . . ? C2 C7 C6 119.8(3) . . ? C2 C7 Cr 70.8(2) . . ? C6 C7 Cr 72.6(2) . . ? C2 C7 H7 120.1(2) . . ? C6 C7 H7 120.1(2) . . ? Cr C7 H7 128.76(8) . . ? O8 C8 Cr 179.3(3) . . ? C6 C5 C4 120.3(3) . . ? C6 C5 Cr 72.0(2) . . ? C4 C5 Cr 71.0(2) . . ? C6 C5 H5 119.9(2) . . ? C4 C5 H5 119.9(2) . . ? Cr C5 H5 129.61(9) . . ? C3 C4 C5 120.0(3) . . ? C3 C4 Cr 70.9(2) . . ? C5 C4 Cr 71.5(2) . . ? C3 C4 H4 120.0(2) . . ? C5 C4 H4 120.0(2) . . ? Cr C4 H4 130.06(9) . . ? _refine_diff_density_max 0.591 _refine_diff_density_min -0.482 _refine_diff_density_rms 0.088 #==END #=============================================================================# # Data for compound 2 # ------------------- data_l15198_complex_2 _publ_contact_author_name 'Lee Brammer' _publ_contact_author_address ; Department of Chemistry University of Missouri-St.Louis 8001 Natural Bridge Road St. Louis, MO 63121-4499 USA ; _publ_contact_author_phone '+1-314-516-5345' _publ_contact_author_fax '+1-314-516-5342' _publ_contact_author_email 'lee.brammer@umsl.edu' _publ_section_title ; pi-Bonded organometallic building blocks for supramolecular chemistry. ; _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C20 H24 Cr O10' _chemical_formula_weight 476.39 _chemical_melting_point ? _chemical_compound_source 'synthesis' 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 11.6029(3) _cell_length_b 13.0537(2) _cell_length_c 15.2638(2) _cell_angle_alpha 87.472(1) _cell_angle_beta 75.734(1) _cell_angle_gamma 86.752(1) _cell_volume 2235.89(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5704 _cell_measurement_theta_min 1.81 _cell_measurement_theta_max 29.66 _exptl_crystal_description Irregular _exptl_crystal_colour orange _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.415 _exptl_crystal_density_method ? _exptl_crystal_F_000 992 _exptl_absorpt_coefficient_mu 0.564 _exptl_absorpt_correction_type 'empirical: SADABS' _exptl_absorpt_correction_T_min 0.473050 _exptl_absorpt_correction_T_max 0.894453 _exptl_absorpt_process_details ; Absorption correction was based upon symmetry equivalent and repeated intensity measurements using the program SADABS (Sheldrick, 1995), which is based upon the method of Blessing (Blessing, 1995). ; _exptl_special_details ; Data were collected with a Siemens SMART CCD-based diffractometer using /w-scans of width 0.3 deg. and 50s duration at a crystal-to-detector distance of 4.942 cm. Intensity decay over the course of the data collection was evaluated by recollecting the first 50 frames of data at the end of the experiment. No significant decay was noted. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART' _diffrn_measurement_method '\w-scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 18389 _diffrn_reflns_av_R_equivalents 0.1250 _diffrn_reflns_av_sigmaI/netI 0.1370 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 22.50 _reflns_number_total 5833 _reflns_number_observed 3651 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART (Siemens, 1994)' _computing_cell_refinement 'SAINT (Siemens, 1994)' _computing_data_reduction 'SAINT (Siemens, 1994)' _computing_structure_solution 'SHELXTL (Siemens, 1994)' _computing_structure_refinement 'SHELXTL (Siemens, 1994)' _computing_molecular_graphics 'SHELXTL (Siemens, 1994)' _computing_publication_material 'SHELXTL (Siemens, 1994)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 326 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^)+(0.1281P)^2^+10.8240P] 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 ; Arene hydrogen atoms were included in calculated positions, whereas carboxyl hydrogen atoms were located directly from the difference map. Both types were then refined by using riding models. ; _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5507 _refine_ls_number_parameters 559 _refine_ls_number_restraints 108 _refine_ls_R_factor_all 0.1643 _refine_ls_R_factor_obs 0.1101 _refine_ls_wR_factor_all 0.3001 _refine_ls_wR_factor_obs 0.2674 _refine_ls_goodness_of_fit_all 1.145 _refine_ls_goodness_of_fit_obs 1.328 _refine_ls_restrained_S_all 1.151 _refine_ls_restrained_S_obs 1.307 _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 Cr1 Cr 0.8851(2) 0.44189(13) 0.29278(11) 0.0230(5) Uani 1 d . . O132 O 0.8660(6) 0.2342(5) 0.4905(4) 0.026(2) Uani 1 d . . H132 H 0.8129(6) 0.1858(5) 0.5465(4) 0.031 Uiso 1 d R . O153 O 1.1950(7) 0.3830(6) 0.1168(5) 0.033(2) Uani 1 d . . O133 O 0.8024(7) 0.3819(6) 0.5606(5) 0.031(2) Uani 1 d . . O152 O 1.1421(7) 0.2371(6) 0.1922(5) 0.035(2) Uani 1 d . . H152 H 1.1793(7) 0.1957(6) 0.1377(5) 0.042 Uiso 1 d R . O173 O 0.9306(7) 0.7135(6) 0.4031(5) 0.038(2) Uani 1 d . . O172 O 1.0466(7) 0.7106(6) 0.2624(5) 0.037(2) Uani 1 d . . H172 H 1.0332(7) 0.7858(6) 0.2544(5) 0.044 Uiso 1 d R . O10 O 0.6341(8) 0.5263(7) 0.3657(6) 0.050(3) Uani 1 d U . O11 O 0.7806(8) 0.2491(7) 0.2493(7) 0.056(3) Uani 1 d U . O12 O 0.8739(10) 0.5373(9) 0.1108(7) 0.071(3) Uani 1 d U . O105 O 0.0516(7) 0.9143(6) 0.2270(5) 0.038(2) Uani 1 d . . C10 C 0.7294(11) 0.4949(10) 0.3403(8) 0.035(3) Uani 1 d U . C11 C 0.8190(11) 0.3228(12) 0.2648(8) 0.041(3) Uani 1 d U . C12 C 0.8775(11) 0.4996(10) 0.1798(8) 0.038(3) Uani 1 d U . C13 C 0.9386(9) 0.3896(8) 0.4155(6) 0.019(2) Uani 1 d U . C14 C 1.0077(9) 0.3359(8) 0.3409(6) 0.021(2) Uani 1 d U . H14 H 1.0107(9) 0.2630(8) 0.3423(6) 0.025 Uiso 1 calc R . C15 C 1.0729(9) 0.3906(8) 0.2637(7) 0.021(2) Uani 1 d U . C16 C 1.0649(9) 0.4967(8) 0.2634(7) 0.021(2) Uani 1 d U . H16 H 1.1078(9) 0.5328(8) 0.2112(7) 0.025 Uiso 1 calc R . C17 C 0.9959(9) 0.5554(8) 0.3369(7) 0.021(2) Uani 1 d U . C18 C 0.9297(9) 0.4963(8) 0.4124(7) 0.021(2) Uani 1 d U . H18A H 0.8783(9) 0.5311(8) 0.4615(7) 0.025 Uiso 1 calc R . C131 C 0.8598(9) 0.3338(8) 0.4963(7) 0.021(3) Uani 1 d . . C151 C 1.1424(10) 0.3343(9) 0.1834(7) 0.023(3) Uani 1 d . . C171 C 0.9843(10) 0.6666(8) 0.3383(7) 0.025(3) Uani 1 d . . C101 C 0.0133(16) 0.7417(14) -0.0072(11) 0.084(6) Uani 1 d . . H30G H -0.0663(16) 0.7300(14) -0.0150(11) 0.127 Uiso 1 calc R . H30H H 0.0466(16) 0.6782(14) 0.0155(11) 0.127 Uiso 1 calc R . H30I H 0.0650(16) 0.7625(14) -0.0655(11) 0.127 Uiso 1 calc R . C102 C 0.0048(14) 0.8237(12) 0.0583(9) 0.059(4) Uani 1 d . . H30E H -0.0494(14) 0.8026(12) 0.1163(9) 0.070 Uiso 1 calc R . H30F H -0.0311(14) 0.8868(12) 0.0355(9) 0.070 Uiso 1 calc R . C103 C 0.1230(13) 0.8490(11) 0.0761(8) 0.051(4) Uani 1 d . . H30C H 0.1556(13) 0.7873(11) 0.1035(8) 0.061 Uiso 1 calc R . H30D H 0.1793(13) 0.8641(11) 0.0174(8) 0.061 Uiso 1 calc R . C104 C 0.1187(12) 0.9365(11) 0.1358(9) 0.052(4) Uani 1 d . . H30A H 0.2008(12) 0.9524(11) 0.1367(9) 0.063 Uiso 1 calc R . H30B H 0.0817(12) 0.9978(11) 0.1112(9) 0.063 Uiso 1 calc R . C106 C 0.0407(12) 0.9998(9) 0.2832(9) 0.041(3) Uani 1 d . . H30J H -0.0018(12) 1.0577(9) 0.2584(9) 0.049 Uiso 1 calc R . H30K H 0.1210(12) 1.0217(9) 0.2830(9) 0.049 Uiso 1 calc R . C107 C -0.0258(12) 0.9751(10) 0.3787(9) 0.045(4) Uani 1 d . . H30L H -0.0155(12) 1.0312(10) 0.4174(9) 0.054 Uiso 1 calc R . H30M H 0.0113(12) 0.9116(10) 0.3998(9) 0.054 Uiso 1 calc R . C108 C -0.1572(12) 0.9605(11) 0.3931(10) 0.052(4) Uani 1 d . . H30N H -0.1688(12) 0.9048(11) 0.3546(10) 0.062 Uiso 1 calc R . H30O H -0.1960(12) 1.0244(11) 0.3743(10) 0.062 Uiso 1 calc R . C109 C -0.2161(13) 0.9337(11) 0.4917(9) 0.056(4) Uani 1 d . . H30P H -0.3012(13) 0.9249(11) 0.4982(9) 0.085 Uiso 1 calc R . H30Q H -0.2061(13) 0.9893(11) 0.5299(9) 0.085 Uiso 1 calc R . H30R H -0.1790(13) 0.8698(11) 0.5102(9) 0.085 Uiso 1 calc R . Cr2 Cr 0.5886(2) 0.91291(13) 0.21254(11) 0.0238(5) Uani 1 d . . O233 O 0.7217(7) 0.8548(5) -0.0520(5) 0.035(2) Uani 1 d . . O253 O 0.2646(7) 0.8492(6) 0.3627(5) 0.037(2) Uani 1 d . . O232 O 0.6639(7) 0.7071(6) 0.0227(5) 0.034(2) Uani 1 d . . H232 H 0.6991(7) 0.6611(6) -0.0190(5) 0.041 Uiso 1 d R . O252 O 0.3453(7) 0.7026(6) 0.3000(5) 0.035(2) Uani 1 d . . H252 H 0.2931(7) 0.6555(6) 0.3543(5) 0.042 Uiso 1 d R . O272 O 0.4047(7) 1.1740(6) 0.2266(5) 0.039(2) Uani 1 d . . H272 H 0.4017(7) 1.2501(6) 0.2343(5) 0.046 Uiso 1 d R . O273 O 0.5339(8) 1.1873(6) 0.0895(5) 0.041(2) Uani 1 d . . O20 O 0.8138(9) 1.0305(7) 0.1600(6) 0.056(3) Uani 1 d U . O22 O 0.5450(9) 0.9966(9) 0.3998(6) 0.070(3) Uani 1 d U . O21 O 0.7345(9) 0.7308(8) 0.2651(7) 0.064(3) Uani 1 d U . O205 O 0.3632(8) 1.3612(6) 0.2777(5) 0.041(2) Uani 1 d . . C20 C 0.7301(11) 0.9842(9) 0.1790(8) 0.031(3) Uani 1 d U . C21 C 0.6777(12) 0.7994(10) 0.2457(8) 0.039(3) Uani 1 d U . C22 C 0.5634(11) 0.9636(10) 0.3293(8) 0.040(3) Uani 1 d U . C23 C 0.5669(10) 0.8610(8) 0.0837(7) 0.025(2) Uani 1 d U . C24 C 0.4925(9) 0.8049(8) 0.1558(7) 0.024(2) Uani 1 d U . H24 H 0.4990(9) 0.7320(8) 0.1581(7) 0.029 Uiso 1 calc R . C25 C 0.4088(9) 0.8581(8) 0.2241(7) 0.021(2) Uani 1 d U . C26 C 0.4035(9) 0.9664(8) 0.2238(7) 0.023(2) Uani 1 d U . H26 H 0.3509(9) 1.0016(8) 0.2719(7) 0.028 Uiso 1 calc R . C27 C 0.4767(9) 1.0226(8) 0.1514(6) 0.021(2) Uani 1 d U . C28 C 0.5582(10) 0.9674(8) 0.0831(7) 0.025(2) Uani 1 d U . H28 H 0.6087(10) 1.0045(8) 0.0352(7) 0.030 Uiso 1 calc R . C231 C 0.6577(10) 0.8035(9) 0.0126(7) 0.021(3) Uani 1 d . . C251 C 0.3328(9) 0.8015(9) 0.3022(7) 0.027(3) Uani 1 d . . C271 C 0.4770(10) 1.1356(9) 0.1518(7) 0.027(3) Uani 1 d . . C201 C 0.5530(14) 1.2689(13) 0.4900(11) 0.078(5) Uani 1 d . . H20P H 0.6192(14) 1.2177(13) 0.4742(11) 0.117 Uiso 1 calc R . H20Q H 0.5015(14) 1.2504(13) 0.5491(11) 0.117 Uiso 1 calc R . H20R H 0.5845(14) 1.3365(13) 0.4927(11) 0.117 Uiso 1 calc R . C202 C 0.4812(12) 1.2725(12) 0.4185(10) 0.058(4) Uani 1 d . . H20I H 0.5343(12) 1.2896(12) 0.3588(10) 0.070 Uiso 1 calc R . H20J H 0.4514(12) 1.2036(12) 0.4152(10) 0.070 Uiso 1 calc R . C203 C 0.3776(11) 1.3494(11) 0.4375(9) 0.044(3) Uani 1 d . . H20A H 0.3291(11) 1.3361(11) 0.4997(9) 0.053 Uiso 1 calc R . H20B H 0.4085(11) 1.4189(11) 0.4354(9) 0.053 Uiso 1 calc R . C204 C 0.2991(11) 1.3485(11) 0.3737(8) 0.044(4) Uani 1 d . . H20C H 0.2586(11) 1.2827(11) 0.3822(8) 0.053 Uiso 1 calc R . H20D H 0.2369(11) 1.4045(11) 0.3888(8) 0.053 Uiso 1 calc R . C206 C 0.3890(12) 1.4660(10) 0.2510(9) 0.045(4) Uani 1 d . . H20G H 0.4338(12) 1.4951(10) 0.2907(9) 0.054 Uiso 1 calc R . H20H H 0.3144(12) 1.5082(10) 0.2548(9) 0.054 Uiso 1 calc R . C207 C 0.4638(13) 1.4642(10) 0.1533(10) 0.053(4) Uani 1 d . . H20N H 0.4253(13) 1.4215(10) 0.1178(10) 0.064 Uiso 1 calc R . H20O H 0.4658(13) 1.5349(10) 0.1268(10) 0.064 Uiso 1 calc R . C208 C 0.5890(12) 1.4229(12) 0.1455(8) 0.052(4) Uani 1 d . . H20E H 0.5876(12) 1.3537(12) 0.1748(8) 0.062 Uiso 1 calc R . H20F H 0.6297(12) 1.4680(12) 0.1776(8) 0.062 Uiso 1 calc R . C209 C 0.6599(14) 1.4164(12) 0.0449(10) 0.066(5) Uani 1 d . . H20K H 0.7411(14) 1.3892(12) 0.0421(10) 0.099 Uiso 1 calc R . H20L H 0.6626(14) 1.4851(12) 0.0160(10) 0.099 Uiso 1 calc R . H20M H 0.6205(14) 1.3709(12) 0.0133(10) 0.099 Uiso 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 0.0201(10) 0.0291(11) 0.0156(10) 0.0000(8) 0.0048(8) -0.0069(8) O132 0.027(5) 0.023(5) 0.017(4) 0.008(3) 0.016(3) -0.003(3) O153 0.036(5) 0.037(5) 0.016(4) 0.000(4) 0.012(4) -0.011(4) O133 0.034(5) 0.030(5) 0.015(4) 0.000(4) 0.021(4) -0.011(4) O152 0.037(5) 0.030(5) 0.027(5) 0.000(4) 0.018(4) -0.008(4) O173 0.046(5) 0.026(5) 0.036(5) -0.003(4) 0.005(4) -0.003(4) O172 0.047(5) 0.023(4) 0.027(5) 0.002(4) 0.017(4) -0.007(4) O10 0.028(6) 0.060(6) 0.064(6) -0.022(5) -0.013(5) 0.010(5) O11 0.049(6) 0.041(6) 0.081(7) -0.014(5) -0.016(5) -0.020(5) O12 0.073(8) 0.097(9) 0.048(7) 0.033(6) -0.023(6) -0.033(6) O105 0.046(6) 0.036(5) 0.024(5) 0.003(4) 0.010(4) -0.016(4) C10 0.020(8) 0.054(9) 0.031(7) 0.005(6) -0.004(6) -0.004(7) C11 0.029(8) 0.065(10) 0.021(7) -0.006(7) 0.009(6) 0.009(7) C12 0.042(8) 0.048(8) 0.026(7) 0.019(6) -0.011(6) -0.015(7) C13 0.015(5) 0.027(5) 0.013(5) -0.001(4) 0.003(4) -0.008(4) C14 0.018(5) 0.028(5) 0.014(5) 0.001(4) 0.002(4) -0.002(4) C15 0.016(5) 0.030(5) 0.012(4) -0.001(4) 0.010(4) -0.010(4) C16 0.014(5) 0.032(5) 0.011(4) 0.002(4) 0.011(4) -0.006(4) C17 0.013(5) 0.035(5) 0.013(4) 0.000(4) 0.001(4) -0.005(4) C18 0.014(5) 0.032(5) 0.015(5) -0.005(4) 0.003(4) -0.009(4) C131 0.019(6) 0.027(7) 0.013(6) 0.003(5) 0.003(5) 0.001(5) C151 0.017(6) 0.028(7) 0.024(7) 0.000(5) -0.003(5) -0.004(5) C171 0.026(7) 0.026(7) 0.017(6) 0.002(5) 0.011(5) -0.008(5) C101 0.074(13) 0.113(16) 0.059(11) 0.001(11) 0.001(9) -0.019(11) C102 0.060(11) 0.084(12) 0.030(8) -0.002(8) -0.004(7) -0.020(9) C103 0.052(10) 0.066(10) 0.025(7) 0.011(7) 0.009(7) -0.011(8) C104 0.037(8) 0.068(10) 0.045(9) 0.010(8) 0.005(7) -0.021(7) C106 0.038(8) 0.023(7) 0.065(10) 0.012(7) -0.016(7) -0.010(6) C107 0.049(9) 0.044(8) 0.045(8) -0.003(7) -0.018(7) -0.003(7) C108 0.046(9) 0.044(9) 0.061(10) -0.011(7) -0.001(8) -0.012(7) C109 0.059(10) 0.057(10) 0.050(9) -0.012(7) -0.007(8) 0.002(8) Cr2 0.0223(11) 0.0287(11) 0.0140(10) 0.0025(8) 0.0077(8) -0.0031(8) O233 0.045(5) 0.024(4) 0.020(4) 0.005(4) 0.026(4) -0.009(4) O253 0.035(5) 0.037(5) 0.024(5) 0.001(4) 0.020(4) -0.004(4) O232 0.050(6) 0.020(5) 0.017(4) -0.006(3) 0.024(4) 0.002(4) O252 0.035(5) 0.024(5) 0.028(5) 0.001(4) 0.026(4) -0.010(4) O272 0.048(6) 0.026(5) 0.035(5) -0.005(4) 0.003(4) 0.001(4) O273 0.055(6) 0.031(5) 0.028(5) 0.006(4) 0.008(4) -0.011(4) O20 0.044(6) 0.060(6) 0.060(6) 0.012(5) 0.001(5) -0.034(5) O22 0.056(7) 0.121(9) 0.035(6) -0.034(6) -0.015(5) 0.018(6) O21 0.054(7) 0.043(6) 0.087(8) 0.018(6) -0.013(6) 0.017(5) O205 0.047(6) 0.032(5) 0.042(5) -0.006(4) -0.006(4) -0.002(4) C20 0.026(7) 0.036(7) 0.029(7) 0.005(6) -0.007(6) -0.001(6) C21 0.035(8) 0.039(8) 0.034(8) 0.000(6) 0.011(6) -0.014(7) C22 0.036(8) 0.062(9) 0.021(7) -0.008(7) -0.004(6) 0.004(7) C23 0.024(5) 0.026(5) 0.017(5) 0.000(4) 0.009(4) -0.007(4) C24 0.023(5) 0.024(5) 0.019(5) 0.004(4) 0.005(4) -0.003(4) C25 0.018(5) 0.022(5) 0.015(5) 0.000(4) 0.009(4) -0.004(4) C26 0.021(5) 0.031(5) 0.010(4) -0.006(4) 0.012(4) 0.003(4) C27 0.024(5) 0.029(5) 0.006(4) 0.002(4) 0.005(4) -0.001(4) C28 0.028(5) 0.031(5) 0.010(5) 0.004(4) 0.008(4) -0.008(4) C231 0.026(7) 0.024(7) 0.012(6) -0.011(5) -0.003(5) 0.004(5) C251 0.014(6) 0.033(8) 0.025(7) 0.001(6) 0.012(5) -0.001(5) C271 0.029(7) 0.033(7) 0.016(6) 0.002(6) 0.000(6) -0.001(6) C201 0.051(11) 0.095(13) 0.088(13) 0.030(10) -0.019(10) -0.013(10) C202 0.034(9) 0.081(11) 0.060(10) 0.000(8) -0.014(8) -0.003(8) C203 0.033(8) 0.063(9) 0.039(8) -0.016(7) -0.011(6) -0.003(7) C204 0.025(7) 0.056(9) 0.048(9) -0.020(7) -0.002(7) 0.005(6) C206 0.038(8) 0.037(8) 0.059(9) -0.012(7) -0.004(7) -0.013(6) C207 0.053(10) 0.037(8) 0.083(12) 0.013(8) -0.038(9) -0.021(7) C208 0.045(9) 0.072(10) 0.036(8) 0.014(7) -0.004(7) -0.021(8) C209 0.066(11) 0.067(11) 0.055(10) 0.013(8) 0.004(8) -0.021(9) _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 C12 1.871(12) . ? Cr1 C10 1.878(13) . ? Cr1 C11 1.88(2) . ? Cr1 C14 2.163(11) . ? Cr1 C18 2.174(10) . ? Cr1 C16 2.178(10) . ? Cr1 C13 2.184(10) . ? Cr1 C15 2.185(11) . ? Cr1 C17 2.244(10) . ? O132 C131 1.304(12) . ? O153 C151 1.221(12) . ? O133 C131 1.220(12) . ? O152 C151 1.270(13) . ? O173 C171 1.202(12) . ? O172 C171 1.331(12) . ? O10 C10 1.136(14) . ? O11 C11 1.141(15) . ? O12 C12 1.153(13) . ? O105 C106 1.418(14) . ? O105 C104 1.443(14) . ? C13 C18 1.390(14) . ? C13 C14 1.410(14) . ? C13 C131 1.526(14) . ? C14 C15 1.421(14) . ? C15 C16 1.382(14) . ? C15 C151 1.490(15) . ? C16 C17 1.433(14) . ? C17 C18 1.437(14) . ? C17 C171 1.451(15) . ? C101 C102 1.48(2) . ? C102 C103 1.52(2) . ? C103 C104 1.48(2) . ? C106 C107 1.50(2) . ? C107 C108 1.51(2) . ? C108 C109 1.53(2) . ? Cr2 C22 1.877(13) . ? Cr2 C21 1.88(2) . ? Cr2 C20 1.882(13) . ? Cr2 C28 2.174(11) . ? Cr2 C24 2.178(11) . ? Cr2 C23 2.184(11) . ? Cr2 C26 2.189(11) . ? Cr2 C25 2.207(10) . ? Cr2 C27 2.208(11) . ? O233 C231 1.268(12) . ? O253 C251 1.226(12) . ? O232 C231 1.261(12) . ? O252 C251 1.292(13) . ? O272 C271 1.337(13) . ? O273 C271 1.217(13) . ? O20 C20 1.142(13) . ? O22 C22 1.144(13) . ? O21 C21 1.153(14) . ? O205 C206 1.437(14) . ? O205 C204 1.478(14) . ? C23 C28 1.386(15) . ? C23 C24 1.423(14) . ? C23 C231 1.507(14) . ? C24 C25 1.414(14) . ? C25 C26 1.410(14) . ? C25 C251 1.491(14) . ? C26 C27 1.420(14) . ? C27 C28 1.415(14) . ? C27 C271 1.48(2) . ? C201 C202 1.53(2) . ? C202 C203 1.50(2) . ? C203 C204 1.49(2) . ? C206 C207 1.53(2) . ? C207 C208 1.50(2) . ? C208 C209 1.56(2) . ? 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 C12 Cr1 C10 88.8(5) . . ? C12 Cr1 C11 89.2(5) . . ? C10 Cr1 C11 88.0(5) . . ? C12 Cr1 C14 134.9(5) . . ? C10 Cr1 C14 135.4(4) . . ? C11 Cr1 C14 84.8(5) . . ? C12 Cr1 C18 135.4(5) . . ? C10 Cr1 C18 87.4(5) . . ? C11 Cr1 C18 135.1(5) . . ? C14 Cr1 C18 68.1(4) . . ? C12 Cr1 C16 86.2(5) . . ? C10 Cr1 C16 137.4(5) . . ? C11 Cr1 C16 134.1(4) . . ? C14 Cr1 C16 67.4(4) . . ? C18 Cr1 C16 67.7(4) . . ? C12 Cr1 C13 165.6(5) . . ? C10 Cr1 C13 101.6(4) . . ? C11 Cr1 C13 100.9(5) . . ? C14 Cr1 C13 37.8(4) . . ? C18 Cr1 C13 37.2(4) . . ? C16 Cr1 C13 79.4(4) . . ? C12 Cr1 C15 100.1(5) . . ? C10 Cr1 C15 168.1(5) . . ? C11 Cr1 C15 99.9(5) . . ? C14 Cr1 C15 38.1(4) . . ? C18 Cr1 C15 80.7(4) . . ? C16 Cr1 C15 36.9(4) . . ? C13 Cr1 C15 68.3(4) . . ? C12 Cr1 C17 100.5(5) . . ? C10 Cr1 C17 102.5(5) . . ? C11 Cr1 C17 165.7(5) . . ? C14 Cr1 C17 80.9(4) . . ? C18 Cr1 C17 37.9(4) . . ? C16 Cr1 C17 37.8(4) . . ? C13 Cr1 C17 67.8(4) . . ? C15 Cr1 C17 68.2(4) . . ? C106 O105 C104 112.2(9) . . ? O10 C10 Cr1 177.2(11) . . ? O11 C11 Cr1 178.0(12) . . ? O12 C12 Cr1 178.2(11) . . ? C18 C13 C14 120.2(9) . . ? C18 C13 C131 117.9(9) . . ? C14 C13 C131 121.5(9) . . ? C18 C13 Cr1 71.0(6) . . ? C14 C13 Cr1 70.3(6) . . ? C131 C13 Cr1 125.2(7) . . ? C13 C14 C15 120.1(10) . . ? C13 C14 Cr1 71.9(6) . . ? C15 C14 Cr1 71.8(6) . . ? C16 C15 C14 118.4(9) . . ? C16 C15 C151 121.2(9) . . ? C14 C15 C151 120.3(10) . . ? C16 C15 Cr1 71.3(6) . . ? C14 C15 Cr1 70.1(6) . . ? C151 C15 Cr1 127.3(7) . . ? C15 C16 C17 124.0(9) . . ? C15 C16 Cr1 71.8(6) . . ? C17 C16 Cr1 73.6(6) . . ? C16 C17 C18 115.3(10) . . ? C16 C17 C171 125.4(9) . . ? C18 C17 C171 119.3(9) . . ? C16 C17 Cr1 68.6(6) . . ? C18 C17 Cr1 68.4(6) . . ? C171 C17 Cr1 130.6(8) . . ? C13 C18 C17 121.9(9) . . ? C13 C18 Cr1 71.8(6) . . ? C17 C18 Cr1 73.7(6) . . ? O133 C131 O132 125.6(9) . . ? O133 C131 C13 120.2(10) . . ? O132 C131 C13 114.1(9) . . ? O153 C151 O152 125.8(10) . . ? O153 C151 C15 119.2(10) . . ? O152 C151 C15 115.0(10) . . ? O173 C171 O172 123.9(10) . . ? O173 C171 C17 123.6(9) . . ? O172 C171 C17 112.4(9) . . ? C101 C102 C103 114.5(13) . . ? C104 C103 C102 115.6(12) . . ? O105 C104 C103 111.8(10) . . ? O105 C106 C107 111.8(9) . . ? C106 C107 C108 115.8(11) . . ? C107 C108 C109 111.9(12) . . ? C22 Cr2 C21 90.0(5) . . ? C22 Cr2 C20 88.6(5) . . ? C21 Cr2 C20 88.3(5) . . ? C22 Cr2 C28 137.0(5) . . ? C21 Cr2 C28 132.3(5) . . ? C20 Cr2 C28 85.9(5) . . ? C22 Cr2 C24 131.9(5) . . ? C21 Cr2 C24 87.6(5) . . ? C20 Cr2 C24 139.2(4) . . ? C28 Cr2 C24 67.7(4) . . ? C22 Cr2 C23 164.8(5) . . ? C21 Cr2 C23 99.7(5) . . ? C20 Cr2 C23 103.3(4) . . ? C28 Cr2 C23 37.1(4) . . ? C24 Cr2 C23 38.1(4) . . ? C22 Cr2 C26 84.3(5) . . ? C21 Cr2 C26 140.3(5) . . ? C20 Cr2 C26 130.6(5) . . ? C28 Cr2 C26 67.9(4) . . ? C24 Cr2 C26 68.3(4) . . ? C23 Cr2 C26 80.7(4) . . ? C22 Cr2 C25 98.2(5) . . ? C21 Cr2 C25 105.6(5) . . ? C20 Cr2 C25 164.4(4) . . ? C28 Cr2 C25 79.4(4) . . ? C24 Cr2 C25 37.6(4) . . ? C23 Cr2 C25 67.9(4) . . ? C26 Cr2 C25 37.4(4) . . ? C22 Cr2 C27 101.5(5) . . ? C21 Cr2 C27 167.2(5) . . ? C20 Cr2 C27 97.5(4) . . ? C28 Cr2 C27 37.7(4) . . ? C24 Cr2 C27 80.6(4) . . ? C23 Cr2 C27 67.9(4) . . ? C26 Cr2 C27 37.7(4) . . ? C25 Cr2 C27 67.5(4) . . ? C206 O205 C204 113.1(9) . . ? O20 C20 Cr2 177.6(11) . . ? O21 C21 Cr2 178.5(11) . . ? O22 C22 Cr2 177.7(11) . . ? C28 C23 C24 119.2(9) . . ? C28 C23 C231 121.5(9) . . ? C24 C23 C231 119.2(10) . . ? C28 C23 Cr2 71.1(6) . . ? C24 C23 Cr2 70.7(6) . . ? C231 C23 Cr2 127.5(8) . . ? C25 C24 C23 119.7(10) . . ? C25 C24 Cr2 72.3(6) . . ? C23 C24 Cr2 71.2(6) . . ? C26 C25 C24 120.3(9) . . ? C26 C25 C251 118.6(9) . . ? C24 C25 C251 120.8(9) . . ? C26 C25 Cr2 70.6(6) . . ? C24 C25 Cr2 70.1(6) . . ? C251 C25 Cr2 127.6(8) . . ? C25 C26 C27 120.0(9) . . ? C25 C26 Cr2 72.0(6) . . ? C27 C26 Cr2 71.9(6) . . ? C28 C27 C26 118.4(10) . . ? C28 C27 C271 120.3(9) . . ? C26 C27 C271 121.0(9) . . ? C28 C27 Cr2 69.9(6) . . ? C26 C27 Cr2 70.4(6) . . ? C271 C27 Cr2 126.3(7) . . ? C23 C28 C27 122.2(10) . . ? C23 C28 Cr2 71.8(6) . . ? C27 C28 Cr2 72.5(6) . . ? O232 C231 O233 125.2(9) . . ? O232 C231 C23 116.6(9) . . ? O233 C231 C23 118.2(10) . . ? O253 C251 O252 124.6(10) . . ? O253 C251 C25 119.9(10) . . ? O252 C251 C25 115.4(9) . . ? O273 C271 O272 124.4(11) . . ? O273 C271 C27 123.3(10) . . ? O272 C271 C27 112.3(9) . . ? C203 C202 C201 113.0(13) . . ? C204 C203 C202 114.5(11) . . ? O205 C204 C203 113.7(10) . . ? O205 C206 C207 106.3(10) . . ? C208 C207 C206 113.1(11) . . ? C207 C208 C209 111.5(12) . . ? _refine_diff_density_max 1.461 _refine_diff_density_min -0.760 _refine_diff_density_rms 0.137 #==END