# Supplementary Material (ESI) for Perkin Transactions # This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 207 _publ_requested_journal 'Perkin Transactions 1' loop_ _publ_author_name 'Tan, Yen-Ling' 'White, Andrew J. P.' 'Widdowson, David' 'Willhelm, Rene' 'Williams, D.' _publ_contact_author_name 'Dr David Widdowson' _publ_contact_author_address ; Chemistry Imperial College Dept of Chemistry Imperial College London SW7 2AZ UNITED KINGDOM ; _publ_contact_author_email 'D.WIDDOWSON@IC.AC.UK' _publ_section_title ; Dilithiation of arenetricarbonylchromium(0) complexes with enantioselective quench: application to chiral biaryl synthesis ; data_dw9902 _database_code_CSD 172233 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C9 H11 B O4' _chemical_formula_weight 193.99 _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' 0.0181 0.0091 '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' 'B' 'B' 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 '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 5.666(2) _cell_length_b 8.4652(10) _cell_length_c 10.4672(9) _cell_angle_alpha 109.348(7) _cell_angle_beta 98.654(14) _cell_angle_gamma 95.745(12) _cell_volume 462.23(15) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 28 _cell_measurement_theta_min 9.15 _cell_measurement_theta_max 55.40 _exptl_crystal_description plates _exptl_crystal_colour Clear _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.394 _exptl_crystal_density_method ? _exptl_crystal_F_000 204 _exptl_absorpt_coefficient_mu 0.897 _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 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4/RA' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1662 _diffrn_reflns_av_R_equivalents 0.0147 _diffrn_reflns_av_sigmaI/netI 0.0135 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 4.57 _diffrn_reflns_theta_max 63.84 _reflns_number_total 1493 _reflns_number_observed 1356 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 44 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^)+(0.0750P)^2^+0.0839P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0782(97) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1449 _refine_ls_number_parameters 132 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0482 _refine_ls_R_factor_obs 0.0429 _refine_ls_wR_factor_all 0.1225 _refine_ls_wR_factor_obs 0.1153 _refine_ls_goodness_of_fit_all 1.077 _refine_ls_goodness_of_fit_obs 1.097 _refine_ls_restrained_S_all 1.107 _refine_ls_restrained_S_obs 1.096 _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 O1 O -0.2885(2) -0.0040(2) 0.86574(14) 0.0594(4) Uani 1 d D . H1 H -0.2395(53) -0.0667(33) 0.9156(27) 0.105(9) Uiso 1 d D . B1 B -0.1256(3) 0.1260(2) 0.8731(2) 0.0413(4) Uani 1 d . . O2 O 0.0992(2) 0.16826(14) 0.96039(11) 0.0454(4) Uani 1 d . . C3 C 0.2362(3) 0.3145(2) 0.9505(2) 0.0415(4) Uani 1 d . . H3A H 0.3840(3) 0.2867(2) 0.9186(2) 0.050 Uiso 1 calc R . H3B H 0.2780(3) 0.4054(2) 1.0397(2) 0.050 Uiso 1 calc R . C4 C 0.0748(3) 0.3666(2) 0.84804(15) 0.0375(4) Uani 1 d . . C5 C 0.1293(3) 0.5042(2) 0.8080(2) 0.0414(4) Uani 1 d . . H5A H 0.2760(3) 0.5773(2) 0.8448(2) 0.050 Uiso 1 calc R . C6 C -0.0446(3) 0.5282(2) 0.7105(2) 0.0417(4) Uani 1 d . . C7 C -0.2645(3) 0.4166(2) 0.6549(2) 0.0424(4) Uani 1 d . . H7A H -0.3782(3) 0.4342(2) 0.5891(2) 0.051 Uiso 1 calc R . C8 C -0.3133(3) 0.2810(2) 0.69708(15) 0.0375(4) Uani 1 d . . C9 C -0.1416(3) 0.2546(2) 0.79707(15) 0.0375(4) Uani 1 d . . O10 O -0.0187(2) 0.6570(2) 0.66094(13) 0.0572(4) Uani 1 d . . C10 C 0.1995(4) 0.7756(2) 0.7140(2) 0.0605(5) Uani 1 d . . H10A H 0.1955(4) 0.8597(2) 0.6710(2) 0.091 Uiso 1 calc R . H10B H 0.3343(4) 0.7175(2) 0.6947(2) 0.091 Uiso 1 calc R . H10C H 0.2162(4) 0.8296(2) 0.8120(2) 0.091 Uiso 1 calc R . O11 O -0.5213(2) 0.16673(14) 0.64881(12) 0.0483(4) Uani 1 d . . C11 C -0.6897(3) 0.1765(2) 0.5366(2) 0.0529(5) Uani 1 d . . H11A H -0.8275(3) 0.0892(2) 0.5129(2) 0.079 Uiso 1 calc R . H11B H -0.6137(3) 0.1613(2) 0.4582(2) 0.079 Uiso 1 calc R . H11C H -0.7410(3) 0.2855(2) 0.5632(2) 0.079 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 O1 0.0531(8) 0.0572(8) 0.0713(9) 0.0419(7) -0.0126(6) -0.0052(6) B1 0.0406(9) 0.0424(10) 0.0416(9) 0.0194(7) -0.0003(7) 0.0073(8) O2 0.0436(7) 0.0469(7) 0.0484(7) 0.0272(5) -0.0052(5) 0.0046(5) C3 0.0378(8) 0.0462(9) 0.0420(8) 0.0221(7) -0.0017(6) 0.0050(7) C4 0.0373(8) 0.0418(8) 0.0339(8) 0.0158(6) 0.0018(6) 0.0081(6) C5 0.0392(8) 0.0437(9) 0.0401(8) 0.0173(7) 0.0008(6) 0.0021(7) C6 0.0486(9) 0.0401(8) 0.0397(8) 0.0199(7) 0.0049(7) 0.0078(7) C7 0.0450(9) 0.0460(9) 0.0374(8) 0.0203(7) -0.0027(7) 0.0100(7) C8 0.0364(8) 0.0397(8) 0.0344(8) 0.0134(6) 0.0004(6) 0.0054(6) C9 0.0378(8) 0.0397(8) 0.0355(8) 0.0155(6) 0.0023(6) 0.0084(7) O10 0.0645(8) 0.0524(8) 0.0596(8) 0.0363(6) -0.0038(6) -0.0019(6) C10 0.0691(13) 0.0499(11) 0.0640(12) 0.0289(9) 0.0068(9) -0.0056(9) O11 0.0414(7) 0.0524(7) 0.0489(7) 0.0245(5) -0.0083(5) 0.0000(5) C11 0.0429(9) 0.0629(11) 0.0471(10) 0.0208(8) -0.0087(7) 0.0044(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 O1 B1 1.337(2) . ? B1 O2 1.388(2) . ? B1 C9 1.548(2) . ? O2 C3 1.436(2) . ? C3 C4 1.511(2) . ? C4 C5 1.385(2) . ? C4 C9 1.387(2) . ? C5 C6 1.389(2) . ? C6 O10 1.359(2) . ? C6 C7 1.402(2) . ? C7 C8 1.378(2) . ? C8 O11 1.360(2) . ? C8 C9 1.409(2) . ? O10 C10 1.422(2) . ? O11 C11 1.428(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 O1 B1 O2 121.93(15) . . ? O1 B1 C9 130.20(15) . . ? O2 B1 C9 107.86(14) . . ? B1 O2 C3 110.62(12) . . ? O2 C3 C4 105.84(12) . . ? C5 C4 C9 123.74(14) . . ? C5 C4 C3 126.40(14) . . ? C9 C4 C3 109.86(14) . . ? C4 C5 C6 117.08(15) . . ? O10 C6 C5 124.2(2) . . ? O10 C6 C7 114.73(14) . . ? C5 C6 C7 121.07(15) . . ? C8 C7 C6 120.38(14) . . ? O11 C8 C7 124.35(14) . . ? O11 C8 C9 115.79(13) . . ? C7 C8 C9 119.85(15) . . ? C4 C9 C8 117.87(14) . . ? C4 C9 B1 105.78(13) . . ? C8 C9 B1 136.35(15) . . ? C6 O10 C10 117.59(14) . . ? C8 O11 C11 118.01(13) . . ? _refine_diff_density_max 0.202 _refine_diff_density_min -0.171 _refine_diff_density_rms 0.041 data_DW9903 _database_code_CSD 172234 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C24 H20 O6 Cr' _chemical_formula_weight 456.40 _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 Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.8222(14) _cell_length_b 11.509(2) _cell_length_c 17.707(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2205.5(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 20 _cell_measurement_theta_min 4.95 _cell_measurement_theta_max 12.43 _exptl_crystal_description prisms _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.93 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.375 _exptl_crystal_density_method ? _exptl_crystal_F_000 944 _exptl_absorpt_coefficient_mu 0.556 _exptl_absorpt_correction_type 'Face-indexed numerical' _exptl_absorpt_correction_T_min 0.6988 _exptl_absorpt_correction_T_max 0.9026 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 8.73 _diffrn_reflns_number 4418 _diffrn_reflns_av_R_equivalents 0.0224 _diffrn_reflns_av_sigmaI/netI 0.0479 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3866 _reflns_number_observed 3525 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 68 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^)+(0.0539P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0040(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(2) _refine_ls_number_reflns 3798 _refine_ls_number_parameters 261 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0442 _refine_ls_R_factor_obs 0.0383 _refine_ls_wR_factor_all 0.0940 _refine_ls_wR_factor_obs 0.0899 _refine_ls_goodness_of_fit_all 1.032 _refine_ls_goodness_of_fit_obs 1.048 _refine_ls_restrained_S_all 1.043 _refine_ls_restrained_S_obs 1.048 _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 Cr Cr 0.13366(4) 0.28720(4) -0.19808(2) 0.03191(13) Uani 1 d . . C1 C 0.1816(3) 0.1029(2) -0.1639(2) 0.0337(6) Uani 1 d . . C2 C 0.1530(2) 0.1686(2) -0.09789(15) 0.0305(5) Uani 1 d . . C3 C 0.0388(3) 0.2262(3) -0.09545(15) 0.0341(5) Uani 1 d . . H3A H 0.0184(3) 0.2687(3) -0.05258(15) 0.041 Uiso 1 calc R . C4 C -0.0460(2) 0.2216(3) -0.1557(2) 0.0398(6) Uani 1 d . . H4A H -0.1222(2) 0.2586(3) -0.1522(2) 0.048 Uiso 1 calc R . C5 C -0.0134(3) 0.1606(3) -0.2206(2) 0.0409(6) Uani 1 d . . H5A H -0.0671(3) 0.1597(3) -0.2616(2) 0.049 Uiso 1 calc R . C6 C 0.0987(3) 0.1008(3) -0.2251(2) 0.0412(7) Uani 1 d . . H6A H 0.1186(3) 0.0595(3) -0.2686(2) 0.049 Uiso 1 calc R . O7 O 0.2924(2) 0.0477(2) -0.16364(14) 0.0438(5) Uani 1 d . . C8 C 0.3243(4) -0.0281(4) -0.2252(2) 0.0592(9) Uani 1 d . . H8A H 0.3096(4) 0.0118(4) -0.2726(2) 0.071 Uiso 1 calc R . H8B H 0.4117(4) -0.0465(4) -0.2224(2) 0.071 Uiso 1 calc R . O9 O 0.2578(3) -0.1285(3) -0.2238(2) 0.0782(10) Uani 1 d . . C10 C 0.2871(7) -0.1991(4) -0.1615(4) 0.102(2) Uani 1 d . . H10A H 0.2379(7) -0.2685(4) -0.1631(4) 0.152 Uiso 1 calc R . H10B H 0.2702(7) -0.1575(4) -0.1157(4) 0.152 Uiso 1 calc R . H10C H 0.3731(7) -0.2193(4) -0.1633(4) 0.152 Uiso 1 calc R . C11 C 0.2379(3) 0.1627(3) -0.0281(2) 0.0339(6) Uani 1 d . . O12 O 0.3634(2) 0.1841(2) -0.04836(12) 0.0447(5) Uani 1 d D . H12A H 0.3837(48) 0.1385(35) -0.0878(18) 0.073(14) Uiso 1 d D . C13 C 0.1098(2) -0.0134(2) 0.0094(2) 0.0656(11) Uani 1 d G . H13A H 0.0404(2) 0.0229(2) -0.0106(2) 0.079 Uiso 1 calc R . C14 C 0.0993(3) -0.1231(3) 0.0418(2) 0.093(2) Uani 1 d G . H14A H 0.0230(3) -0.1601(4) 0.0433(3) 0.111 Uiso 1 calc R . C15 C 0.2030(4) -0.1774(2) 0.0717(2) 0.096(2) Uani 1 d G . H15A H 0.1961(5) -0.2508(2) 0.0933(3) 0.116 Uiso 1 calc R . C16 C 0.3172(3) -0.1221(2) 0.0694(2) 0.086(2) Uani 1 d G . H16A H 0.3865(4) -0.1585(3) 0.0894(3) 0.104 Uiso 1 calc R . C17 C 0.3276(2) -0.0125(2) 0.0371(2) 0.0630(11) Uani 1 d G . H17A H 0.4039(2) 0.0245(3) 0.0355(2) 0.076 Uiso 1 calc R . C18 C 0.2239(2) 0.0419(2) 0.00711(13) 0.0430(7) Uani 1 d G . C19 C 0.1411(2) 0.2425(2) 0.09369(11) 0.0451(7) Uani 1 d G . H19A H 0.1126(2) 0.1685(2) 0.10565(11) 0.054 Uiso 1 calc R . C20 C 0.1178(2) 0.3350(2) 0.14212(10) 0.0593(9) Uani 1 d G . H20A H 0.0736(3) 0.3229(3) 0.18648(13) 0.071 Uiso 1 calc R . C21 C 0.1604(2) 0.4455(2) 0.12425(13) 0.0682(12) Uani 1 d G . H21A H 0.1448(4) 0.5074(2) 0.1567(2) 0.082 Uiso 1 calc R . C22 C 0.2265(3) 0.46357(14) 0.05795(14) 0.0621(10) Uani 1 d G . H22A H 0.2550(4) 0.5375(2) 0.0460(2) 0.075 Uiso 1 calc R . C23 C 0.2498(2) 0.3711(2) 0.00952(10) 0.0468(7) Uani 1 d G . H23A H 0.2940(3) 0.3832(2) -0.03484(13) 0.056 Uiso 1 calc R . C24 C 0.2071(2) 0.26055(14) 0.02739(10) 0.0368(6) Uani 1 d G . C25 C 0.2963(3) 0.3099(3) -0.2197(2) 0.0592(10) Uani 1 d . . O25 O 0.3993(3) 0.3249(4) -0.2342(3) 0.111(2) Uani 1 d . . C26 C 0.1287(4) 0.4338(3) -0.1579(2) 0.0522(8) Uani 1 d . . O26 O 0.1262(5) 0.5263(2) -0.1327(2) 0.0862(11) Uani 1 d . . C27 C 0.0921(3) 0.3478(3) -0.2913(2) 0.0421(6) Uani 1 d . . O27 O 0.0657(3) 0.3831(2) -0.34925(13) 0.0625(7) Uani 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 0.0324(2) 0.0307(2) 0.0327(2) 0.0042(2) -0.0010(2) -0.0007(2) C1 0.0361(13) 0.0307(13) 0.0344(13) -0.0005(11) 0.0042(11) -0.0012(11) C2 0.0323(14) 0.0293(11) 0.0300(12) 0.0020(9) -0.0015(10) -0.0038(10) C3 0.0335(12) 0.0367(14) 0.0321(12) 0.0012(12) 0.0040(10) -0.0013(12) C4 0.0288(12) 0.049(2) 0.0421(14) 0.0056(14) -0.0022(10) -0.0036(13) C5 0.0408(15) 0.0446(15) 0.0372(14) 0.0030(12) -0.0089(11) -0.0078(13) C6 0.050(2) 0.0367(14) 0.0367(13) -0.0045(11) -0.0021(12) -0.0043(12) O7 0.0442(12) 0.0369(11) 0.0504(12) -0.0097(9) 0.0005(9) 0.0101(9) C8 0.063(2) 0.062(2) 0.053(2) -0.014(2) 0.006(2) 0.017(2) O9 0.082(2) 0.054(2) 0.099(2) -0.034(2) -0.024(2) 0.0122(15) C10 0.119(5) 0.044(2) 0.142(5) -0.005(3) -0.024(4) -0.009(3) C11 0.0328(13) 0.0343(13) 0.0346(13) 0.0014(11) -0.0039(11) 0.0022(11) O12 0.0299(9) 0.0525(12) 0.0517(11) -0.0076(9) -0.0036(10) 0.0018(10) C13 0.077(3) 0.054(2) 0.066(2) 0.020(2) -0.004(2) -0.015(2) C14 0.132(5) 0.063(3) 0.083(3) 0.023(2) -0.007(3) -0.030(3) C15 0.183(7) 0.041(2) 0.064(3) 0.016(2) -0.019(3) 0.006(3) C16 0.145(5) 0.049(2) 0.066(2) 0.005(2) -0.031(3) 0.031(3) C17 0.089(3) 0.047(2) 0.053(2) 0.000(2) -0.022(2) 0.018(2) C18 0.059(2) 0.0350(15) 0.0355(13) 0.0034(12) -0.0073(13) 0.0022(14) C19 0.0373(13) 0.057(2) 0.0406(14) -0.0033(12) -0.0035(13) -0.0011(13) C20 0.046(2) 0.084(3) 0.048(2) -0.023(2) -0.0003(15) 0.005(2) C21 0.065(2) 0.072(2) 0.068(2) -0.036(2) -0.010(2) 0.009(2) C22 0.074(2) 0.044(2) 0.068(2) -0.017(2) -0.010(2) -0.003(2) C23 0.054(2) 0.039(2) 0.047(2) -0.0044(13) -0.0067(14) -0.0031(14) C24 0.0341(13) 0.040(2) 0.0358(13) -0.0032(11) -0.0082(10) 0.0024(11) C25 0.043(2) 0.058(2) 0.077(2) 0.032(2) -0.001(2) -0.0042(15) O25 0.041(2) 0.130(3) 0.161(4) 0.083(3) 0.011(2) -0.007(2) C26 0.079(2) 0.036(2) 0.0412(15) 0.0082(12) -0.013(2) -0.004(2) O26 0.160(4) 0.0358(13) 0.063(2) -0.0013(12) -0.023(2) 0.003(2) C27 0.0473(15) 0.0413(14) 0.038(2) 0.0035(12) 0.0012(12) 0.0026(12) O27 0.087(2) 0.063(2) 0.0374(12) 0.0140(11) -0.0030(12) 0.0096(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 C25 1.820(4) . ? Cr C26 1.832(3) . ? Cr C27 1.848(3) . ? Cr C5 2.194(3) . ? Cr C3 2.202(3) . ? Cr C4 2.217(3) . ? Cr C6 2.230(3) . ? Cr C2 2.248(3) . ? Cr C1 2.266(3) . ? C1 O7 1.357(4) . ? C1 C6 1.406(4) . ? C1 C2 1.427(4) . ? C2 C3 1.403(4) . ? C2 C11 1.541(4) . ? C3 C4 1.408(4) . ? C4 C5 1.393(5) . ? C5 C6 1.397(5) . ? O7 C8 1.438(4) . ? C8 O9 1.362(6) . ? O9 C10 1.406(7) . ? C11 O12 1.425(4) . ? C11 C24 1.532(3) . ? C11 C18 1.532(3) . ? C13 C14 1.39 . ? C13 C18 1.39 . ? C14 C15 1.39 . ? C15 C16 1.39 . ? C16 C17 1.39 . ? C17 C18 1.39 . ? C19 C20 1.39 . ? C19 C24 1.39 . ? C20 C21 1.39 . ? C21 C22 1.39 . ? C22 C23 1.39 . ? C23 C24 1.39 . ? C25 O25 1.157(5) . ? C26 O26 1.154(4) . ? C27 O27 1.140(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 C25 Cr C26 88.7(2) . . ? C25 Cr C27 89.6(2) . . ? C26 Cr C27 89.52(13) . . ? C25 Cr C5 139.3(2) . . ? C26 Cr C5 131.4(2) . . ? C27 Cr C5 84.93(13) . . ? C25 Cr C3 132.07(14) . . ? C26 Cr C3 87.71(14) . . ? C27 Cr C3 138.09(12) . . ? C5 Cr C3 66.43(11) . . ? C25 Cr C4 165.52(14) . . ? C26 Cr C4 99.0(2) . . ? C27 Cr C4 102.57(12) . . ? C5 Cr C4 36.81(12) . . ? C3 Cr C4 37.15(10) . . ? C25 Cr C6 104.9(2) . . ? C26 Cr C6 164.6(2) . . ? C27 Cr C6 97.50(13) . . ? C5 Cr C6 36.81(12) . . ? C3 Cr C6 77.93(11) . . ? C4 Cr C6 66.19(12) . . ? C25 Cr C2 99.37(13) . . ? C26 Cr C2 104.81(11) . . ? C27 Cr C2 163.13(12) . . ? C5 Cr C2 78.93(10) . . ? C3 Cr C2 36.73(10) . . ? C4 Cr C2 66.90(10) . . ? C6 Cr C2 66.48(10) . . ? C25 Cr C1 88.22(14) . . ? C26 Cr C1 139.96(12) . . ? C27 Cr C1 130.36(12) . . ? C5 Cr C1 65.98(11) . . ? C3 Cr C1 65.66(11) . . ? C4 Cr C1 77.97(11) . . ? C6 Cr C1 36.43(11) . . ? C2 Cr C1 36.85(10) . . ? O7 C1 C6 124.0(3) . . ? O7 C1 C2 115.9(3) . . ? C6 C1 C2 120.1(3) . . ? O7 C1 Cr 129.9(2) . . ? C6 C1 Cr 70.4(2) . . ? C2 C1 Cr 70.9(2) . . ? C3 C2 C1 117.8(2) . . ? C3 C2 C11 121.4(2) . . ? C1 C2 C11 120.3(2) . . ? C3 C2 Cr 69.87(15) . . ? C1 C2 Cr 72.3(2) . . ? C11 C2 Cr 135.6(2) . . ? C2 C3 C4 122.2(3) . . ? C2 C3 Cr 73.40(15) . . ? C4 C3 Cr 72.0(2) . . ? C5 C4 C3 118.6(3) . . ? C5 C4 Cr 70.7(2) . . ? C3 C4 Cr 70.9(2) . . ? C4 C5 C6 121.0(3) . . ? C4 C5 Cr 72.5(2) . . ? C6 C5 Cr 73.0(2) . . ? C5 C6 C1 120.1(3) . . ? C5 C6 Cr 70.2(2) . . ? C1 C6 Cr 73.2(2) . . ? C1 O7 C8 119.6(3) . . ? O9 C8 O7 112.0(3) . . ? C8 O9 C10 112.6(4) . . ? O12 C11 C24 104.0(2) . . ? O12 C11 C18 110.7(2) . . ? C24 C11 C18 112.6(2) . . ? O12 C11 C2 111.0(2) . . ? C24 C11 C2 110.6(2) . . ? C18 C11 C2 107.9(2) . . ? C14 C13 C18 120.0 . . ? C15 C14 C13 120.0 . . ? C14 C15 C16 120.0 . . ? C17 C16 C15 120.0 . . ? C18 C17 C16 120.0 . . ? C17 C18 C13 120.0 . . ? C17 C18 C11 118.9(2) . . ? C13 C18 C11 121.1(2) . . ? C20 C19 C24 120.0 . . ? C19 C20 C21 120.0 . . ? C22 C21 C20 120.0 . . ? C21 C22 C23 120.0 . . ? C24 C23 C22 120.0 . . ? C23 C24 C19 120.0 . . ? C23 C24 C11 117.0(2) . . ? C19 C24 C11 123.0(2) . . ? O25 C25 Cr 179.2(4) . . ? O26 C26 Cr 179.7(5) . . ? O27 C27 Cr 178.7(3) . . ? _refine_diff_density_max 0.402 _refine_diff_density_min -0.311 _refine_diff_density_rms 0.047 data_DW9904 _database_code_CSD 172235 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C26 H24 O8 Cr' _chemical_formula_weight 516.45 _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' 0.0181 0.0091 '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' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cr' 'Cr' -0.1635 2.4439 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P3(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' _cell_length_a 12.5356(15) _cell_length_b 12.5356(15) _cell_length_c 13.273(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1806.3(4) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 27 _cell_measurement_theta_min 1.26 _cell_measurement_theta_max 22.38 _exptl_crystal_description rhombs _exptl_crystal_colour Orange _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.424 _exptl_crystal_density_method ? _exptl_crystal_F_000 804 _exptl_absorpt_coefficient_mu 4.332 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.5995 _exptl_absorpt_correction_T_max 0.8799 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2203 _diffrn_reflns_av_R_equivalents 0.0972 _diffrn_reflns_av_sigmaI/netI 0.2220 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 4.07 _diffrn_reflns_theta_max 63.90 _reflns_number_total 2052 _reflns_number_observed 1033 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 311 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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0008(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(2) _refine_ls_number_reflns 1741 _refine_ls_number_parameters 321 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1980 _refine_ls_R_factor_obs 0.0879 _refine_ls_wR_factor_all 0.1789 _refine_ls_wR_factor_obs 0.1245 _refine_ls_goodness_of_fit_all 1.051 _refine_ls_goodness_of_fit_obs 1.271 _refine_ls_restrained_S_all 1.207 _refine_ls_restrained_S_obs 1.269 _refine_ls_shift/esd_max -0.020 _refine_ls_shift/esd_mean 0.003 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 0.0858(3) 0.3399(3) 0.8209(9) 0.0351(7) Uani 1 d . . C1 C -0.1274(17) 0.2422(16) 0.8288(15) 0.032(4) Uani 1 d . . C2 C -0.0688(20) 0.3085(18) 0.9191(19) 0.047(6) Uani 1 d . . C3 C 0.0166(18) 0.4329(17) 0.9139(17) 0.041(5) Uani 1 d . . H3A H 0.0502(18) 0.4771(17) 0.9730(17) 0.050 Uiso 1 calc R . C4 C 0.0535(17) 0.4940(17) 0.8196(18) 0.045(5) Uani 1 d . . H4A H 0.1111(17) 0.5776(17) 0.8175(18) 0.054 Uiso 1 calc R . C5 C 0.0055(19) 0.4314(18) 0.7325(18) 0.043(5) Uani 1 d . . H5A H 0.0293(19) 0.4717(18) 0.6708(18) 0.051 Uiso 1 calc R . C6 C -0.0802(19) 0.3053(20) 0.7368(16) 0.043(5) Uani 1 d . . H6A H -0.1072(19) 0.2613(20) 0.6768(16) 0.052 Uiso 1 calc R . O7 O -0.2171(11) 0.1229(12) 0.8356(12) 0.043(3) Uani 1 d . . C8 C -0.2760(19) 0.0560(21) 0.7437(16) 0.060(7) Uani 1 d . . H8A H -0.3472(19) -0.0226(21) 0.7609(16) 0.072 Uiso 1 calc R . H8B H -0.3042(19) 0.1026(21) 0.7047(16) 0.072 Uiso 1 calc R . O9 O -0.1973(15) 0.0371(14) 0.6881(14) 0.068(5) Uani 1 d . . C10 C -0.1696(27) -0.0511(24) 0.7260(20) 0.102(11) Uani 1 d . . H10A H -0.1130(27) -0.0579(24) 0.6814(20) 0.153 Uiso 1 calc R . H10B H -0.2439(27) -0.1294(24) 0.7309(20) 0.153 Uiso 1 calc R . H10C H -0.1330(27) -0.0261(24) 0.7915(20) 0.153 Uiso 1 calc R . C11 C -0.1146(16) 0.2417(20) 1.0233(16) 0.043(5) Uani 1 d . . O12 O -0.1224(12) 0.1221(12) 1.0200 0.047(3) Uani 1 d D . H12 H -0.1375(203) 0.0822(164) 0.9608(76) 0.079(82) Uiso 1 d D . C13 C -0.2428(15) 0.2231(16) 1.0477(15) 0.034(4) Uani 1 d . . C14 C -0.2924(19) 0.2861(19) 1.0081(18) 0.052(5) Uani 1 d . . H14A H -0.2475(19) 0.3451(19) 0.9594(18) 0.062 Uiso 1 calc R . C15 C -0.4094(16) 0.2686(19) 1.0358(18) 0.051(6) Uani 1 d . . H15A H -0.4384(16) 0.3174(19) 1.0078(18) 0.062 Uiso 1 calc R . C16 C -0.4760(22) 0.1827(22) 1.1012(19) 0.062(6) Uani 1 d . . C17 C -0.4320(19) 0.1147(23) 1.1466(17) 0.066(8) Uani 1 d . . H17A H -0.4791(19) 0.0562(23) 1.1949(17) 0.079 Uiso 1 calc R . C18 C -0.3146(23) 0.1335(21) 1.1199(17) 0.064(7) Uani 1 d . . H18A H -0.2848(23) 0.0867(21) 1.1501(17) 0.076 Uiso 1 calc R . O19 O -0.5911(14) 0.1506(20) 1.1355(15) 0.094(7) Uani 1 d . . C20 C -0.6572(24) 0.1949(26) 1.0813(25) 0.106(12) Uani 1 d . . H20A H -0.7269(24) 0.1845(26) 1.1194(25) 0.159 Uiso 1 d R . H20B H -0.6850(24) 0.1495(26) 1.0195(25) 0.159 Uiso 1 d R . H20C H -0.6041(24) 0.2807(26) 1.0666(25) 0.159 Uiso 1 d R . C21 C -0.0258(17) 0.3046(16) 1.1038(16) 0.035(4) Uani 1 d . . C22 C -0.0261(20) 0.3988(18) 1.1675(16) 0.048(5) Uani 1 d . . H22A H -0.0883(20) 0.4181(18) 1.1596(16) 0.058 Uiso 1 calc R . C23 C 0.0620(16) 0.4590(18) 1.2380(16) 0.046(5) Uani 1 d . . H23A H 0.0552(16) 0.5142(18) 1.2806(16) 0.055 Uiso 1 calc R . C24 C 0.1631(19) 0.4411(18) 1.2492(18) 0.046(5) Uani 1 d . . C25 C 0.1671(17) 0.3538(19) 1.1910(15) 0.041(5) Uani 1 d . . H25A H 0.2298(17) 0.3355(19) 1.1996(15) 0.049 Uiso 1 calc R . C26 C 0.0764(15) 0.2923(15) 1.1183(16) 0.035(4) Uani 1 d . . H26A H 0.0856(15) 0.2383(15) 1.0760(16) 0.042 Uiso 1 calc R . O27 O 0.2560(14) 0.4985(14) 1.3166(14) 0.070(5) Uani 1 d . . C28 C 0.2559(25) 0.5823(26) 1.3854(22) 0.106(12) Uani 1 d . . H28A H 0.2672(25) 0.6551(26) 1.3519(22) 0.159 Uiso 1 d R . H28B H 0.3220(25) 0.6040(26) 1.4322(22) 0.159 Uiso 1 d R . H28C H 0.1789(25) 0.5443(26) 1.4210(22) 0.159 Uiso 1 d R . C29 C 0.0846(17) 0.1978(17) 0.8582(15) 0.036(5) Uani 1 d . . O29 O 0.0867(16) 0.1100(14) 0.8835(14) 0.075(5) Uani 1 d . . C30 C 0.2326(18) 0.4250(18) 0.8887(15) 0.044(5) Uani 1 d . . O30 O 0.3246(14) 0.4740(17) 0.9331(16) 0.087(6) Uani 1 d . . C31 C 0.1729(20) 0.3481(24) 0.7092(17) 0.060(7) Uani 1 d . . O31 O 0.2186(16) 0.3454(15) 0.6324(15) 0.078(5) Uani 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 0.034(2) 0.038(2) 0.0346(13) 0.004(2) 0.001(2) 0.019(2) C1 0.028(10) 0.029(11) 0.033(10) -0.001(8) -0.004(7) 0.009(9) C2 0.052(14) 0.027(11) 0.061(13) -0.003(10) 0.008(11) 0.020(11) C3 0.052(14) 0.025(11) 0.040(10) -0.008(9) -0.009(10) 0.013(10) C4 0.035(11) 0.019(10) 0.065(13) 0.006(10) -0.015(11) 0.002(9) C5 0.054(14) 0.038(13) 0.046(11) 0.005(10) -0.009(11) 0.030(12) C6 0.053(14) 0.065(16) 0.023(9) -0.018(10) -0.025(9) 0.038(13) O7 0.035(7) 0.045(9) 0.031(7) -0.003(6) -0.001(6) 0.007(7) C8 0.055(15) 0.085(18) 0.033(10) -0.037(11) -0.028(10) 0.029(13) O9 0.086(12) 0.049(10) 0.057(9) -0.010(8) 0.015(9) 0.024(9) C10 0.180(34) 0.095(23) 0.068(18) -0.003(16) 0.035(19) 0.096(24) C11 0.036(11) 0.056(13) 0.032(9) 0.018(10) 0.003(8) 0.020(10) O12 0.057(9) 0.035(8) 0.041(7) 0.000(7) -0.008(7) 0.018(7) C13 0.026(10) 0.037(11) 0.041(10) -0.005(8) -0.006(8) 0.017(9) C14 0.043(13) 0.058(15) 0.055(12) 0.007(12) 0.004(11) 0.026(12) C15 0.015(10) 0.063(15) 0.071(14) 0.021(12) 0.014(9) 0.015(10) C16 0.062(16) 0.071(18) 0.063(15) -0.018(13) -0.016(12) 0.041(15) C17 0.039(13) 0.106(22) 0.043(12) 0.039(13) 0.009(10) 0.029(14) C18 0.093(19) 0.058(14) 0.053(14) 0.009(12) 0.033(13) 0.047(15) O19 0.036(9) 0.176(20) 0.084(12) 0.011(13) 0.018(9) 0.064(12) C20 0.059(18) 0.114(25) 0.173(32) 0.030(22) 0.054(19) 0.065(18) C21 0.036(11) 0.027(10) 0.045(9) 0.006(8) -0.022(8) 0.017(9) C22 0.055(15) 0.041(13) 0.064(12) 0.006(11) -0.016(11) 0.036(12) C23 0.027(11) 0.065(15) 0.048(11) -0.032(10) -0.012(9) 0.025(11) C24 0.046(13) 0.039(12) 0.052(11) 0.006(9) 0.015(10) 0.020(10) C25 0.033(11) 0.063(14) 0.043(10) -0.005(10) -0.009(9) 0.038(11) C26 0.027(10) 0.032(10) 0.047(10) -0.011(8) -0.006(8) 0.016(9) O27 0.065(10) 0.082(12) 0.065(9) -0.044(9) -0.043(8) 0.040(9) C28 0.097(23) 0.137(29) 0.116(24) -0.078(22) -0.044(19) 0.083(23) C29 0.050(12) 0.041(12) 0.033(9) 0.016(8) -0.005(8) 0.035(10) O29 0.111(15) 0.076(12) 0.075(11) 0.033(9) 0.027(10) 0.073(12) C30 0.045(13) 0.047(13) 0.024(9) -0.007(8) -0.015(9) 0.010(11) O30 0.037(9) 0.115(15) 0.081(12) -0.016(10) -0.030(8) 0.017(10) C31 0.045(14) 0.093(19) 0.038(12) 0.001(12) -0.013(10) 0.033(14) O31 0.107(15) 0.077(12) 0.060(11) 0.030(9) 0.039(10) 0.054(12) _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 C31 1.81(2) . ? Cr C29 1.84(2) . ? Cr C30 1.84(2) . ? Cr C3 2.16(2) . ? Cr C4 2.16(2) . ? Cr C5 2.20(2) . ? Cr C6 2.21(2) . ? Cr C2 2.20(2) . ? Cr C1 2.32(2) . ? C1 O7 1.35(2) . ? C1 C6 1.41(2) . ? C1 C2 1.43(2) . ? C2 C3 1.38(3) . ? C2 C11 1.57(3) . ? C3 C4 1.42(3) . ? C4 C5 1.36(2) . ? C5 C6 1.40(3) . ? O7 C8 1.45(2) . ? C8 O9 1.34(2) . ? O9 C10 1.41(3) . ? C11 O12 1.45(2) . ? C11 C21 1.46(2) . ? C11 C13 1.54(2) . ? C13 C14 1.33(3) . ? C13 C18 1.41(3) . ? C14 C15 1.42(3) . ? C15 C16 1.31(3) . ? C16 C17 1.36(3) . ? C16 O19 1.37(3) . ? C17 C18 1.41(3) . ? O19 C20 1.40(3) . ? C21 C26 1.38(2) . ? C21 C22 1.45(2) . ? C22 C23 1.35(2) . ? C23 C24 1.40(2) . ? C24 C25 1.36(3) . ? C24 O27 1.36(2) . ? C25 C26 1.39(2) . ? O27 C28 1.39(2) . ? C29 O29 1.16(2) . ? C30 O30 1.16(2) . ? C31 O31 1.18(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 C31 Cr C29 89.4(10) . . ? C31 Cr C30 88.2(9) . . ? C29 Cr C30 87.2(9) . . ? C31 Cr C3 146.2(10) . . ? C29 Cr C3 123.9(8) . . ? C30 Cr C3 87.8(8) . . ? C31 Cr C4 108.6(10) . . ? C29 Cr C4 162.0(8) . . ? C30 Cr C4 93.7(8) . . ? C3 Cr C4 38.3(7) . . ? C31 Cr C5 87.3(9) . . ? C29 Cr C5 149.4(8) . . ? C30 Cr C5 123.0(8) . . ? C3 Cr C5 67.1(7) . . ? C4 Cr C5 36.2(6) . . ? C31 Cr C6 94.5(8) . . ? C29 Cr C6 113.3(8) . . ? C30 Cr C6 159.3(8) . . ? C3 Cr C6 78.5(7) . . ? C4 Cr C6 65.9(7) . . ? C5 Cr C6 37.0(7) . . ? C31 Cr C2 161.0(9) . . ? C29 Cr C2 95.0(8) . . ? C30 Cr C2 110.5(8) . . ? C3 Cr C2 37.0(7) . . ? C4 Cr C2 67.8(7) . . ? C5 Cr C2 79.5(7) . . ? C6 Cr C2 66.7(8) . . ? C31 Cr C1 124.7(8) . . ? C29 Cr C1 91.5(7) . . ? C30 Cr C1 147.1(7) . . ? C3 Cr C1 65.8(7) . . ? C4 Cr C1 77.9(6) . . ? C5 Cr C1 66.0(7) . . ? C6 Cr C1 36.3(6) . . ? C2 Cr C1 36.9(6) . . ? O7 C1 C6 124.0(16) . . ? O7 C1 C2 119.2(16) . . ? C6 C1 C2 116.6(16) . . ? O7 C1 Cr 133.5(13) . . ? C6 C1 Cr 67.4(10) . . ? C2 C1 Cr 67.1(11) . . ? C3 C2 C1 119.7(19) . . ? C3 C2 C11 121.1(19) . . ? C1 C2 C11 118.9(17) . . ? C3 C2 Cr 69.7(12) . . ? C1 C2 Cr 76.0(12) . . ? C11 C2 Cr 132.2(14) . . ? C2 C3 C4 120.8(18) . . ? C2 C3 Cr 73.3(12) . . ? C4 C3 Cr 71.1(12) . . ? C5 C4 C3 120.6(17) . . ? C5 C4 Cr 73.6(12) . . ? C3 C4 Cr 70.6(11) . . ? C4 C5 C6 119.1(17) . . ? C4 C5 Cr 70.2(12) . . ? C6 C5 Cr 71.6(11) . . ? C5 C6 C1 122.5(16) . . ? C5 C6 Cr 71.4(11) . . ? C1 C6 Cr 76.3(10) . . ? C1 O7 C8 119.0(14) . . ? O9 C8 O7 110.9(16) . . ? C8 O9 C10 115.7(18) . . ? O12 C11 C21 102.7(15) . . ? O12 C11 C13 108.8(15) . . ? C21 C11 C13 112.7(16) . . ? O12 C11 C2 110.0(15) . . ? C21 C11 C2 112.4(17) . . ? C13 C11 C2 110.0(15) . . ? C14 C13 C18 116.0(19) . . ? C14 C13 C11 126.0(18) . . ? C18 C13 C11 117.9(17) . . ? C13 C14 C15 124.0(20) . . ? C16 C15 C14 118.9(21) . . ? C15 C16 C17 121.1(23) . . ? C15 C16 O19 127.4(22) . . ? C17 C16 O19 111.5(23) . . ? C16 C17 C18 119.8(21) . . ? C13 C18 C17 120.1(21) . . ? C16 O19 C20 117.2(20) . . ? C26 C21 C22 112.9(16) . . ? C26 C21 C11 122.9(18) . . ? C22 C21 C11 123.6(17) . . ? C23 C22 C21 121.4(18) . . ? C22 C23 C24 122.4(19) . . ? C25 C24 O27 115.7(18) . . ? C25 C24 C23 118.0(20) . . ? O27 C24 C23 126.2(18) . . ? C24 C25 C26 119.3(18) . . ? C21 C26 C25 125.6(17) . . ? C24 O27 C28 120.6(18) . . ? O29 C29 Cr 178.0(17) . . ? O30 C30 Cr 177.0(19) . . ? O31 C31 Cr 173.5(20) . . ? _refine_diff_density_max 0.377 _refine_diff_density_min -0.345 _refine_diff_density_rms 0.084 data_DW9905 _database_code_CSD 172236 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C12 H10 O6 Cr' _chemical_formula_weight 302.20 _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 P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 6.6813(6) _cell_length_b 13.750(2) _cell_length_c 7.4108(6) _cell_angle_alpha 90.00 _cell_angle_beta 106.179(6) _cell_angle_gamma 90.00 _cell_volume 653.85(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 21 _cell_measurement_theta_min 4.83 _cell_measurement_theta_max 12.99 _exptl_crystal_description blocks _exptl_crystal_colour Orange _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.535 _exptl_crystal_density_method ? _exptl_crystal_F_000 308 _exptl_absorpt_coefficient_mu 0.893 _exptl_absorpt_correction_type Ellipsoidal _exptl_absorpt_correction_T_min 0.6738 _exptl_absorpt_correction_T_max 0.7766 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 6.54 _diffrn_reflns_number 1685 _diffrn_reflns_av_R_equivalents 0.0379 _diffrn_reflns_av_sigmaI/netI 0.0574 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.86 _diffrn_reflns_theta_max 27.50 _reflns_number_total 1559 _reflns_number_observed 1367 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 42 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^)+(0.0313P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0021(32) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.05(4) _refine_ls_number_reflns 1517 _refine_ls_number_parameters 173 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0498 _refine_ls_R_factor_obs 0.0396 _refine_ls_wR_factor_all 0.0972 _refine_ls_wR_factor_obs 0.0900 _refine_ls_goodness_of_fit_all 1.043 _refine_ls_goodness_of_fit_obs 1.056 _refine_ls_restrained_S_all 1.065 _refine_ls_restrained_S_obs 1.055 _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 0.19615(11) -0.00579(5) 0.02503(9) 0.0402(2) Uani 1 d . . C1 C 0.4973(7) 0.0654(3) 0.1889(7) 0.0370(9) Uani 1 d . . C2 C 0.5320(8) -0.0348(3) 0.1569(8) 0.0407(10) Uani 1 d . . C3 C 0.4737(10) -0.0705(4) -0.0311(8) 0.0510(12) Uani 1 d . . H3A H 0.4973(10) -0.1354(4) -0.0534(8) 0.061 Uiso 1 calc R . C4 C 0.3827(8) -0.0103(6) -0.1810(6) 0.0535(12) Uani 1 d . . H4A H 0.3512(8) -0.0341(6) -0.3031(6) 0.064 Uiso 1 calc R . C5 C 0.3380(8) 0.0864(4) -0.1482(7) 0.0485(11) Uani 1 d . . H5A H 0.2690(8) 0.1254(4) -0.2489(7) 0.058 Uiso 1 calc R . C6 C 0.3961(8) 0.1260(4) 0.0356(7) 0.0432(10) Uani 1 d . . H6A H 0.3684(8) 0.1908(4) 0.0555(7) 0.052 Uiso 1 calc R . O7 O 0.5577(6) 0.0939(3) 0.3705(5) 0.0462(8) Uani 1 d . . C8 C 0.5059(10) 0.1898(4) 0.4155(8) 0.0501(12) Uani 1 d . . H8A H 0.3590(10) 0.2011(4) 0.3560(8) 0.060 Uiso 1 calc R . H8B H 0.5283(10) 0.1943(4) 0.5503(8) 0.060 Uiso 1 calc R . O9 O 0.6206(7) 0.2619(3) 0.3595(6) 0.0581(10) Uani 1 d . . C10 C 0.8356(11) 0.2624(5) 0.4668(11) 0.072(2) Uani 1 d . . H10A H 0.9076(11) 0.3135(5) 0.4224(11) 0.109 Uiso 1 calc R . H10B H 0.8979(11) 0.2010(5) 0.4527(11) 0.109 Uiso 1 calc R . H10C H 0.8452(11) 0.2730(5) 0.5969(11) 0.109 Uiso 1 calc R . C11 C 0.6213(10) -0.1022(4) 0.3152(9) 0.0527(13) Uani 1 d . . H11A H 0.6420(10) -0.0796(4) 0.4372(9) 0.063 Uiso 1 calc R . O11 O 0.6679(9) -0.1845(3) 0.2928(8) 0.0727(14) Uani 1 d . . C12 C 0.1063(8) 0.0097(5) 0.2362(7) 0.0514(14) Uani 1 d . . O12 O 0.0509(8) 0.0215(4) 0.3688(6) 0.078(2) Uani 1 d . . C13 C 0.0709(14) -0.1271(6) -0.0102(11) 0.077(2) Uani 1 d . . O13 O -0.0163(16) -0.1994(6) -0.0366(14) 0.141(4) Uani 1 d . . C14 C -0.0496(11) 0.0456(8) -0.1147(11) 0.097(3) Uani 1 d . . O14 O -0.2039(9) 0.0782(8) -0.2079(11) 0.158(4) Uani 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 0.0379(3) 0.0425(3) 0.0384(3) 0.0032(4) 0.0078(2) -0.0087(4) C1 0.037(2) 0.028(2) 0.045(2) 0.001(2) 0.009(2) -0.001(2) C2 0.038(2) 0.030(2) 0.052(3) 0.000(2) 0.010(2) 0.001(2) C3 0.062(3) 0.037(2) 0.059(3) -0.008(2) 0.026(3) -0.003(2) C4 0.063(3) 0.058(3) 0.043(2) -0.010(3) 0.020(2) -0.013(4) C5 0.051(3) 0.054(3) 0.039(2) 0.010(2) 0.008(2) -0.011(2) C6 0.044(2) 0.035(2) 0.048(2) 0.009(2) 0.007(2) -0.001(2) O7 0.053(2) 0.037(2) 0.042(2) -0.0014(14) 0.002(2) -0.002(2) C8 0.061(3) 0.039(2) 0.049(2) -0.005(2) 0.012(2) 0.004(2) O9 0.073(3) 0.037(2) 0.054(2) -0.002(2) 0.001(2) -0.003(2) C10 0.072(4) 0.058(4) 0.082(4) -0.004(3) 0.012(3) -0.017(3) C11 0.055(3) 0.038(2) 0.062(3) 0.005(2) 0.012(3) 0.004(2) O11 0.083(3) 0.040(2) 0.098(4) 0.014(2) 0.029(3) 0.015(2) C12 0.042(2) 0.059(4) 0.054(2) 0.003(3) 0.016(2) -0.005(3) O12 0.081(3) 0.101(5) 0.062(2) -0.008(2) 0.034(2) -0.003(3) C13 0.090(5) 0.075(5) 0.075(4) -0.015(4) 0.037(4) -0.044(4) O13 0.184(8) 0.094(5) 0.175(8) -0.046(5) 0.099(7) -0.088(6) C14 0.043(3) 0.162(9) 0.077(4) 0.059(5) 0.002(3) -0.021(4) O14 0.046(3) 0.267(11) 0.141(6) 0.125(7) -0.004(3) -0.004(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr C14 1.822(7) . ? Cr C12 1.838(5) . ? Cr C13 1.851(7) . ? Cr C5 2.198(5) . ? Cr C3 2.198(6) . ? Cr C2 2.220(5) . ? Cr C4 2.224(5) . ? Cr C6 2.240(5) . ? Cr C1 2.263(5) . ? C1 O7 1.351(6) . ? C1 C6 1.419(6) . ? C1 C2 1.428(7) . ? C2 C3 1.425(8) . ? C2 C11 1.483(8) . ? C3 C4 1.382(9) . ? C4 C5 1.398(10) . ? C5 C6 1.417(7) . ? O7 C8 1.426(6) . ? C8 O9 1.386(7) . ? O9 C10 1.435(8) . ? C11 O11 1.196(7) . ? C12 O12 1.154(6) . ? C13 O13 1.142(9) . ? C14 O14 1.159(9) . ? 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 C14 Cr C12 89.0(3) . . ? C14 Cr C13 88.2(5) . . ? C12 Cr C13 89.0(3) . . ? C14 Cr C5 84.9(3) . . ? C12 Cr C5 136.6(3) . . ? C13 Cr C5 133.5(3) . . ? C14 Cr C3 136.3(3) . . ? C12 Cr C3 134.5(2) . . ? C13 Cr C3 88.9(3) . . ? C5 Cr C3 66.3(2) . . ? C14 Cr C2 163.8(3) . . ? C12 Cr C2 100.1(2) . . ? C13 Cr C2 105.2(3) . . ? C5 Cr C2 79.2(2) . . ? C3 Cr C2 37.6(2) . . ? C14 Cr C4 102.1(3) . . ? C12 Cr C4 165.0(2) . . ? C13 Cr C4 101.3(3) . . ? C5 Cr C4 36.9(3) . . ? C3 Cr C4 36.4(2) . . ? C2 Cr C4 66.8(2) . . ? C14 Cr C6 98.1(3) . . ? C12 Cr C6 102.1(2) . . ? C13 Cr C6 167.3(3) . . ? C5 Cr C6 37.2(2) . . ? C3 Cr C6 78.9(2) . . ? C2 Cr C6 67.1(2) . . ? C4 Cr C6 66.7(2) . . ? C14 Cr C1 131.5(3) . . ? C12 Cr C1 86.9(2) . . ? C13 Cr C1 139.9(3) . . ? C5 Cr C1 66.4(2) . . ? C3 Cr C1 66.8(2) . . ? C2 Cr C1 37.1(2) . . ? C4 Cr C1 78.2(2) . . ? C6 Cr C1 36.7(2) . . ? O7 C1 C6 124.8(4) . . ? O7 C1 C2 115.3(4) . . ? C6 C1 C2 119.8(5) . . ? O7 C1 Cr 129.4(4) . . ? C6 C1 Cr 70.7(3) . . ? C2 C1 Cr 69.8(3) . . ? C3 C2 C1 118.7(5) . . ? C3 C2 C11 119.9(5) . . ? C1 C2 C11 121.3(5) . . ? C3 C2 Cr 70.4(3) . . ? C1 C2 Cr 73.1(3) . . ? C11 C2 Cr 126.5(4) . . ? C4 C3 C2 121.3(5) . . ? C4 C3 Cr 72.8(3) . . ? C2 C3 Cr 72.0(3) . . ? C3 C4 C5 119.8(5) . . ? C3 C4 Cr 70.8(3) . . ? C5 C4 Cr 70.5(3) . . ? C4 C5 C6 121.2(5) . . ? C4 C5 Cr 72.6(3) . . ? C6 C5 Cr 73.0(3) . . ? C5 C6 C1 119.1(5) . . ? C5 C6 Cr 69.8(3) . . ? C1 C6 Cr 72.5(3) . . ? C1 O7 C8 118.5(4) . . ? O9 C8 O7 113.6(5) . . ? C8 O9 C10 112.9(5) . . ? O11 C11 C2 122.9(6) . . ? O12 C12 Cr 178.5(6) . . ? O13 C13 Cr 176.3(10) . . ? O14 C14 Cr 178.1(8) . . ? _refine_diff_density_max 0.226 _refine_diff_density_min -0.240 _refine_diff_density_rms 0.056 data_DW9907 _database_code_CSD 172237 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C30 H42 O9 Si Cr' _chemical_formula_weight 626.73 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cr' 'Cr' -0.1635 2.4439 '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 8.3515(13) _cell_length_b 10.1419(12) _cell_length_c 20.393(2) _cell_angle_alpha 91.132(9) _cell_angle_beta 91.211(10) _cell_angle_gamma 110.571(10) _cell_volume 1616.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 22 _cell_measurement_theta_min 10.57 _cell_measurement_theta_max 24.01 _exptl_crystal_description 'platy needles' _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.288 _exptl_crystal_density_method ? _exptl_crystal_F_000 664 _exptl_absorpt_coefficient_mu 3.679 _exptl_absorpt_correction_type 'Lamina [0 0 1]' _exptl_absorpt_correction_T_min 0.5198 _exptl_absorpt_correction_T_max 1.0000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4781 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_sigmaI/netI 0.0570 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 4.34 _diffrn_reflns_theta_max 59.99 _reflns_number_total 4429 _reflns_number_observed 3284 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 304 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^)+(0.0896P)^2^+0.1521P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4125 _refine_ls_number_parameters 403 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0828 _refine_ls_R_factor_obs 0.0576 _refine_ls_wR_factor_all 0.1625 _refine_ls_wR_factor_obs 0.1421 _refine_ls_goodness_of_fit_all 1.031 _refine_ls_goodness_of_fit_obs 1.088 _refine_ls_restrained_S_all 1.056 _refine_ls_restrained_S_obs 1.087 _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 0.03746(9) 0.24937(7) 0.25596(4) 0.0535(2) Uani 1 d . . Si Si 0.3835(2) 0.74116(15) 0.37994(6) 0.0672(4) Uani 1 d . . C1 C -0.1294(5) 0.2728(4) 0.1703(2) 0.0542(9) Uani 1 d . . C2 C 0.0298(5) 0.3805(4) 0.1665(2) 0.0491(9) Uani 1 d . . C3 C 0.0957(5) 0.4661(4) 0.2239(2) 0.0528(9) Uani 1 d . . H3A H 0.2047(5) 0.5342(4) 0.2233(2) 0.063 Uiso 1 calc R . C4 C 0.0028(5) 0.4516(5) 0.2811(2) 0.0567(10) Uani 1 d . . C5 C -0.1561(6) 0.3411(5) 0.2830(3) 0.0639(12) Uani 1 d . . H5A H -0.2191(6) 0.3292(5) 0.3209(3) 0.077 Uiso 1 calc R . C6 C -0.2207(5) 0.2500(5) 0.2298(3) 0.0599(11) Uani 1 d . . H6A H -0.3230(5) 0.1744(5) 0.2327(3) 0.072 Uiso 1 calc R . O7 O -0.1923(4) 0.1908(3) 0.1146(2) 0.0659(8) Uani 1 d . . C8 C -0.3723(6) 0.1152(6) 0.1093(3) 0.082(2) Uani 1 d . . H8A H -0.4312(6) 0.1744(6) 0.1270(3) 0.099 Uiso 1 calc R . H8B H -0.4053(6) 0.0969(6) 0.0632(3) 0.099 Uiso 1 calc R . O9 O -0.4248(6) -0.0069(4) 0.1400(3) 0.1028(15) Uani 1 d . . C10 C -0.3776(11) -0.1151(8) 0.1097(6) 0.132(3) Uani 1 d . . H10A H -0.4199(11) -0.1992(8) 0.1345(6) 0.198 Uiso 1 calc R . H10B H -0.2552(11) -0.0851(8) 0.1081(6) 0.198 Uiso 1 calc R . H10C H -0.4259(11) -0.1341(8) 0.0658(6) 0.198 Uiso 1 calc R . C11 C 0.1206(5) 0.4212(4) 0.1033(2) 0.0508(9) Uani 1 d . . C12 C 0.1451(5) 0.5579(4) 0.0817(2) 0.0510(9) Uani 1 d . . C13 C 0.2207(6) 0.6057(5) 0.0233(2) 0.0572(10) Uani 1 d . . H13A H 0.2369(6) 0.6969(5) 0.0105(2) 0.069 Uiso 1 calc R . C14 C 0.2724(5) 0.5159(5) -0.0164(2) 0.0569(10) Uani 1 d . . C15 C 0.2539(6) 0.3831(5) 0.0037(2) 0.0586(10) Uani 1 d . . H15A H 0.2933(6) 0.3252(5) -0.0223(2) 0.070 Uiso 1 calc R . C16 C 0.1767(5) 0.3340(5) 0.0626(2) 0.0539(9) Uani 1 d . . O17 O 0.0843(4) 0.6386(3) 0.1219(2) 0.0636(8) Uani 1 d . . C18 C 0.1144(7) 0.7802(5) 0.1051(3) 0.0693(12) Uani 1 d . . H18A H 0.0651(7) 0.8238(5) 0.1372(3) 0.104 Uiso 1 calc R . H18B H 0.0631(7) 0.7819(5) 0.0627(3) 0.104 Uiso 1 calc R . H18C H 0.2354(7) 0.8307(5) 0.1040(3) 0.104 Uiso 1 calc R . O19 O 0.3430(5) 0.5727(4) -0.0741(2) 0.0743(9) Uani 1 d . . C20 C 0.3747(8) 0.4807(6) -0.1215(3) 0.0807(15) Uani 1 d . . H20A H 0.4239(8) 0.5329(6) -0.1594(3) 0.121 Uiso 1 calc R . H20B H 0.2689(8) 0.4072(6) -0.1342(3) 0.121 Uiso 1 calc R . H20C H 0.4525(8) 0.4398(6) -0.1030(3) 0.121 Uiso 1 calc R . C21 C 0.1617(7) 0.1866(5) 0.0801(3) 0.0698(13) Uani 1 d . . H21A H 0.1933(7) 0.1877(5) 0.1262(3) 0.084 Uiso 0.60 calc PR 1 H21B H 0.0424(7) 0.1267(5) 0.0748(3) 0.084 Uiso 0.60 calc PR 1 H21C H 0.1319(7) 0.1741(5) 0.1253(3) 0.084 Uiso 0.40 d PR 2 H21D H 0.2719(7) 0.1780(5) 0.0762(3) 0.084 Uiso 0.40 d PR 2 O22 O 0.2522(18) 0.1290(12) 0.0470(5) 0.145(5) Uani 0.60 d P 1 H22A H 0.3203(220) 0.1119(246) 0.0720(21) 0.217 Uiso 0.60 calc PR 1 O22' O 0.0524(16) 0.0833(13) 0.0445(6) 0.100(3) Uiso 0.40 d P 2 H22B H -0.0455(18) 0.0745(173) 0.0543(87) 0.150 Uiso 0.40 calc PR 2 C23 C 0.0713(6) 0.5479(6) 0.3399(3) 0.0718(13) Uani 1 d . . H23A H 0.0329(6) 0.6276(6) 0.3375(3) 0.086 Uiso 1 calc R . H23B H 0.0268(6) 0.4979(6) 0.3794(3) 0.086 Uiso 1 calc R . O24 O 0.2508(4) 0.5968(4) 0.3434(2) 0.0713(9) Uani 1 d . . C25 C 0.3474(14) 0.8960(8) 0.3397(4) 0.121(3) Uani 1 d . . H25A H 0.2350(14) 0.8915(8) 0.3548(4) 0.145 Uiso 1 calc R . C26 C 0.3284(19) 0.8885(10) 0.2712(5) 0.168(5) Uani 1 d . . H26A H 0.2506(19) 0.7968(10) 0.2575(5) 0.253 Uiso 1 calc R . H26B H 0.4375(19) 0.9046(10) 0.2522(5) 0.253 Uiso 1 calc R . H26C H 0.2839(19) 0.9589(10) 0.2569(5) 0.253 Uiso 1 calc R . C27 C 0.4685(15) 1.0374(8) 0.3670(5) 0.139(4) Uani 1 d . . H27A H 0.4753(15) 1.0350(8) 0.4140(5) 0.209 Uiso 1 calc R . H27B H 0.4266(15) 1.1104(8) 0.3545(5) 0.209 Uiso 1 calc R . H27C H 0.5802(15) 1.0562(8) 0.3498(5) 0.209 Uiso 1 calc R . C28 C 0.5953(24) 0.7012(23) 0.3779(9) 0.100(5) Uani 0.50 d PD 1 H28A H 0.5875(24) 0.6220(23) 0.4060(9) 0.120 Uiso 0.50 calc PR 1 C29 C 0.6154(36) 0.6624(36) 0.3057(16) 0.135(12) Uani 0.50 d PD 1 H29A H 0.5184(36) 0.5820(36) 0.2916(16) 0.203 Uiso 0.50 calc PR 1 H29B H 0.7178(36) 0.6406(36) 0.3020(16) 0.203 Uiso 0.50 calc PR 1 H29C H 0.6226(36) 0.7406(36) 0.2787(16) 0.203 Uiso 0.50 calc PR 1 C30 C 0.7548(50) 0.8316(46) 0.3985(24) 0.138(11) Uani 0.50 d PD 1 H30A H 0.7457(50) 0.8582(46) 0.4433(24) 0.207 Uiso 0.50 calc PR 1 H30B H 0.7609(50) 0.9086(46) 0.3708(24) 0.207 Uiso 0.50 calc PR 1 H30C H 0.8563(50) 0.8087(46) 0.3941(24) 0.207 Uiso 0.50 calc PR 1 C28' C 0.5997(20) 0.7573(21) 0.3528(9) 0.086(4) Uani 0.50 d PD 2 H28B H 0.6332(20) 0.8255(21) 0.3178(9) 0.104 Uiso 0.50 calc PR 2 C29' C 0.6207(61) 0.6188(40) 0.3295(26) 0.204(27) Uani 0.50 d PD 2 H29D H 0.5458(61) 0.5800(40) 0.2922(26) 0.306 Uiso 0.50 calc PR 2 H29E H 0.5923(61) 0.5529(40) 0.3643(26) 0.306 Uiso 0.50 calc PR 2 H29F H 0.7370(61) 0.6375(40) 0.3176(26) 0.306 Uiso 0.50 calc PR 2 C30' C 0.7246(62) 0.8137(70) 0.4132(25) 0.220(35) Uani 0.50 d PD 2 H30D H 0.7159(62) 0.9004(70) 0.4295(25) 0.330 Uiso 0.50 calc PR 2 H30E H 0.8397(62) 0.8301(70) 0.4003(25) 0.330 Uiso 0.50 calc PR 2 H30F H 0.6950(62) 0.7455(70) 0.4470(25) 0.330 Uiso 0.50 calc PR 2 C31 C 0.3418(11) 0.7481(9) 0.4694(3) 0.108(2) Uani 1 d . . H31A H 0.4352(11) 0.8289(9) 0.4888(3) 0.129 Uiso 1 calc R . C32 C 0.1787(13) 0.7716(13) 0.4841(5) 0.161(5) Uani 1 d . . H32A H 0.1759(13) 0.8535(13) 0.4620(5) 0.241 Uiso 1 calc R . H32B H 0.1727(13) 0.7854(13) 0.5306(5) 0.241 Uiso 1 calc R . H32C H 0.0831(13) 0.6909(13) 0.4691(5) 0.241 Uiso 1 calc R . C33 C 0.3469(21) 0.6194(14) 0.5040(5) 0.188(6) Uani 1 d . . H33A H 0.4515(21) 0.6047(14) 0.4945(5) 0.282 Uiso 1 calc R . H33B H 0.2514(21) 0.5386(14) 0.4891(5) 0.282 Uiso 1 calc R . H33C H 0.3410(21) 0.6331(14) 0.5505(5) 0.282 Uiso 1 calc R . C34 C -0.0260(7) 0.0583(6) 0.2387(3) 0.0754(14) Uani 1 d . . O34 O -0.0653(7) -0.0600(5) 0.2272(3) 0.116(2) Uani 1 d . . C35 C 0.2613(6) 0.2690(5) 0.2458(3) 0.0722(13) Uani 1 d . . O35 O 0.4019(5) 0.2796(5) 0.2388(3) 0.112(2) Uani 1 d . . C36 C 0.0717(8) 0.2155(7) 0.3429(3) 0.088(2) Uani 1 d . . O36 O 0.0964(9) 0.1965(8) 0.3965(2) 0.138(2) Uani 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 0.0453(4) 0.0546(4) 0.0580(4) -0.0001(3) 0.0147(3) 0.0137(3) Si 0.0653(7) 0.0747(8) 0.0520(7) -0.0092(6) 0.0024(6) 0.0132(6) C1 0.046(2) 0.052(2) 0.063(2) -0.008(2) 0.003(2) 0.015(2) C2 0.040(2) 0.045(2) 0.062(2) -0.006(2) 0.007(2) 0.014(2) C3 0.047(2) 0.048(2) 0.060(2) -0.005(2) 0.007(2) 0.012(2) C4 0.050(2) 0.059(2) 0.062(2) -0.008(2) 0.011(2) 0.020(2) C5 0.051(2) 0.064(3) 0.076(3) -0.010(2) 0.022(2) 0.019(2) C6 0.036(2) 0.058(2) 0.080(3) -0.004(2) 0.011(2) 0.009(2) O7 0.049(2) 0.062(2) 0.076(2) -0.014(2) 0.0027(15) 0.0069(13) C8 0.052(3) 0.071(3) 0.112(4) -0.024(3) -0.008(3) 0.009(2) O9 0.081(3) 0.068(2) 0.140(4) -0.026(2) 0.021(3) 0.003(2) C10 0.116(6) 0.074(4) 0.192(10) -0.050(5) -0.008(6) 0.021(4) C11 0.043(2) 0.054(2) 0.053(2) -0.007(2) 0.001(2) 0.015(2) C12 0.046(2) 0.052(2) 0.054(2) -0.010(2) 0.001(2) 0.017(2) C13 0.058(2) 0.053(2) 0.059(2) -0.002(2) 0.003(2) 0.019(2) C14 0.053(2) 0.065(3) 0.053(2) -0.002(2) 0.006(2) 0.020(2) C15 0.060(2) 0.060(2) 0.057(2) -0.006(2) 0.010(2) 0.023(2) C16 0.049(2) 0.057(2) 0.055(2) -0.011(2) 0.002(2) 0.018(2) O17 0.073(2) 0.057(2) 0.067(2) -0.0054(14) 0.0129(15) 0.0302(15) C18 0.076(3) 0.058(3) 0.079(3) -0.009(2) 0.004(2) 0.031(2) O19 0.088(2) 0.075(2) 0.063(2) 0.005(2) 0.024(2) 0.032(2) C20 0.090(4) 0.085(3) 0.064(3) 0.001(3) 0.026(3) 0.026(3) C21 0.085(3) 0.054(2) 0.072(3) -0.006(2) 0.021(3) 0.026(2) O22 0.244(12) 0.141(7) 0.121(6) 0.056(6) 0.100(8) 0.150(9) C23 0.063(3) 0.074(3) 0.068(3) -0.018(2) 0.021(2) 0.011(2) O24 0.061(2) 0.076(2) 0.071(2) -0.018(2) 0.003(2) 0.018(2) C25 0.161(8) 0.081(4) 0.100(5) -0.012(4) -0.028(5) 0.021(4) C26 0.263(14) 0.099(6) 0.117(7) 0.012(5) -0.061(8) 0.033(7) C27 0.191(9) 0.077(4) 0.115(6) -0.003(4) -0.028(6) 0.006(5) C28 0.078(9) 0.118(14) 0.103(13) 0.016(10) -0.010(9) 0.032(10) C29 0.086(13) 0.150(20) 0.173(22) -0.041(19) 0.051(14) 0.044(13) C30 0.057(13) 0.164(22) 0.165(23) -0.026(17) -0.004(14) 0.006(12) C28' 0.059(7) 0.111(12) 0.084(10) 0.002(8) -0.004(7) 0.025(8) C29' 0.134(24) 0.175(33) 0.331(67) -0.062(38) -0.016(30) 0.092(25) C30' 0.078(23) 0.349(76) 0.215(49) -0.061(47) -0.016(27) 0.059(31) C31 0.124(6) 0.121(6) 0.061(3) -0.018(3) 0.009(3) 0.023(4) C32 0.140(8) 0.200(11) 0.119(7) -0.067(7) 0.045(6) 0.032(7) C33 0.282(17) 0.189(11) 0.090(6) 0.050(7) 0.025(8) 0.076(11) C34 0.070(3) 0.068(3) 0.088(4) 0.004(3) 0.022(3) 0.023(2) O34 0.130(4) 0.061(3) 0.153(5) -0.014(3) 0.022(3) 0.028(2) C35 0.057(3) 0.068(3) 0.095(4) 0.020(3) 0.019(3) 0.025(2) O35 0.060(2) 0.116(3) 0.174(5) 0.050(3) 0.035(3) 0.041(2) C36 0.091(4) 0.096(4) 0.084(4) 0.000(3) 0.024(3) 0.042(3) O36 0.173(6) 0.201(6) 0.060(3) 0.029(3) 0.024(3) 0.089(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr C35 1.826(5) . ? Cr C34 1.845(6) . ? Cr C36 1.847(7) . ? Cr C3 2.194(4) . ? Cr C5 2.204(4) . ? Cr C6 2.213(4) . ? Cr C4 2.222(4) . ? Cr C1 2.279(5) . ? Cr C2 2.291(4) . ? Si O24 1.646(3) . ? Si C28' 1.85(2) . ? Si C31 1.870(6) . ? Si C25 1.898(9) . ? Si C28 1.95(2) . ? C1 O7 1.374(5) . ? C1 C2 1.398(6) . ? C1 C6 1.425(6) . ? C2 C3 1.422(6) . ? C2 C11 1.500(6) . ? C3 C4 1.396(6) . ? C4 C5 1.406(6) . ? C4 C23 1.501(7) . ? C5 C6 1.381(7) . ? O7 C8 1.428(6) . ? C8 O9 1.333(8) . ? O9 C10 1.425(9) . ? C11 C16 1.403(6) . ? C11 C12 1.408(6) . ? C12 O17 1.372(5) . ? C12 C13 1.377(6) . ? C13 C14 1.391(6) . ? C14 O19 1.371(6) . ? C14 C15 1.374(7) . ? C15 C16 1.392(6) . ? C16 C21 1.506(7) . ? O17 C18 1.418(6) . ? O19 C20 1.423(6) . ? C21 O22 1.298(9) . ? C21 O22' 1.314(13) . ? C23 O24 1.403(6) . ? C25 C26 1.401(12) . ? C25 C27 1.521(10) . ? C28 C29 1.54(2) . ? C28 C30 1.55(2) . ? C28' C29' 1.54(3) . ? C28' C30' 1.56(3) . ? C31 C32 1.497(13) . ? C31 C33 1.509(14) . ? C34 O34 1.145(7) . ? C35 O35 1.153(6) . ? C36 O36 1.141(8) . ? 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 C35 Cr C34 89.8(2) . . ? C35 Cr C36 86.1(3) . . ? C34 Cr C36 88.2(3) . . ? C35 Cr C3 89.4(2) . . ? C34 Cr C3 151.6(2) . . ? C36 Cr C3 120.1(2) . . ? C35 Cr C5 149.7(2) . . ? C34 Cr C5 120.2(2) . . ? C36 Cr C5 90.9(2) . . ? C3 Cr C5 66.2(2) . . ? C35 Cr C6 158.5(2) . . ? C34 Cr C6 92.7(2) . . ? C36 Cr C6 115.3(2) . . ? C3 Cr C6 78.4(2) . . ? C5 Cr C6 36.5(2) . . ? C35 Cr C4 112.9(2) . . ? C34 Cr C4 157.2(2) . . ? C36 Cr C4 92.5(2) . . ? C3 Cr C4 36.9(2) . . ? C5 Cr C4 37.0(2) . . ? C6 Cr C4 66.5(2) . . ? C35 Cr C1 121.7(2) . . ? C34 Cr C1 91.4(2) . . ? C36 Cr C1 152.2(2) . . ? C3 Cr C1 65.2(2) . . ? C5 Cr C1 65.4(2) . . ? C6 Cr C1 37.0(2) . . ? C4 Cr C1 77.5(2) . . ? C35 Cr C2 93.6(2) . . ? C34 Cr C2 114.9(2) . . ? C36 Cr C2 156.9(2) . . ? C3 Cr C2 36.9(2) . . ? C5 Cr C2 77.8(2) . . ? C6 Cr C2 66.0(2) . . ? C4 Cr C2 66.3(2) . . ? C1 Cr C2 35.63(15) . . ? O24 Si C28' 105.9(6) . . ? O24 Si C31 111.7(3) . . ? C28' Si C31 120.0(6) . . ? O24 Si C25 107.2(3) . . ? C28' Si C25 102.6(7) . . ? C31 Si C25 108.6(4) . . ? O24 Si C28 100.1(6) . . ? C31 Si C28 103.8(6) . . ? C25 Si C28 125.1(7) . . ? O7 C1 C2 117.0(4) . . ? O7 C1 C6 122.1(4) . . ? C2 C1 C6 120.9(4) . . ? O7 C1 Cr 131.6(3) . . ? C2 C1 Cr 72.7(3) . . ? C6 C1 Cr 69.0(3) . . ? C1 C2 C3 117.4(4) . . ? C1 C2 C11 123.0(4) . . ? C3 C2 C11 119.0(3) . . ? C1 C2 Cr 71.7(3) . . ? C3 C2 Cr 67.8(2) . . ? C11 C2 Cr 138.8(3) . . ? C4 C3 C2 122.4(4) . . ? C4 C3 Cr 72.7(3) . . ? C2 C3 Cr 75.3(2) . . ? C3 C4 C5 118.1(4) . . ? C3 C4 C23 121.5(4) . . ? C5 C4 C23 120.4(4) . . ? C3 C4 Cr 70.5(2) . . ? C5 C4 Cr 70.8(2) . . ? C23 C4 Cr 128.6(4) . . ? C6 C5 C4 121.4(4) . . ? C6 C5 Cr 72.1(2) . . ? C4 C5 Cr 72.2(2) . . ? C5 C6 C1 119.5(4) . . ? C5 C6 Cr 71.4(3) . . ? C1 C6 Cr 74.1(2) . . ? C1 O7 C8 117.7(4) . . ? O9 C8 O7 114.7(5) . . ? C8 O9 C10 114.5(6) . . ? C16 C11 C12 117.3(4) . . ? C16 C11 C2 126.0(4) . . ? C12 C11 C2 116.6(3) . . ? O17 C12 C13 122.2(4) . . ? O17 C12 C11 115.7(4) . . ? C13 C12 C11 122.1(4) . . ? C12 C13 C14 119.1(4) . . ? O19 C14 C15 125.2(4) . . ? O19 C14 C13 114.6(4) . . ? C15 C14 C13 120.2(4) . . ? C14 C15 C16 120.7(4) . . ? C15 C16 C11 120.4(4) . . ? C15 C16 C21 116.6(4) . . ? C11 C16 C21 123.0(4) . . ? C12 O17 C18 118.5(4) . . ? C14 O19 C20 117.6(4) . . ? O22 C21 C16 117.0(6) . . ? O22' C21 C16 116.6(7) . . ? O24 C23 C4 111.2(4) . . ? C23 O24 Si 128.6(3) . . ? C26 C25 C27 114.1(8) . . ? C26 C25 Si 116.4(7) . . ? C27 C25 Si 112.6(6) . . ? C29 C28 C30 107.6(22) . . ? C29 C28 Si 106.0(16) . . ? C30 C28 Si 112.5(23) . . ? C29' C28' C30' 106.5(26) . . ? C29' C28' Si 115.6(22) . . ? C30' C28' Si 106.9(24) . . ? C32 C31 C33 109.7(9) . . ? C32 C31 Si 114.2(6) . . ? C33 C31 Si 112.3(6) . . ? O34 C34 Cr 179.3(6) . . ? O35 C35 Cr 179.0(6) . . ? O36 C36 Cr 178.5(7) . . ? _refine_diff_density_max 0.384 _refine_diff_density_min -0.239 _refine_diff_density_rms 0.051