# Supplementary Material (ESI) for Perkin Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 207/356 data_global #------------------------------------------------------------------------- #2 Person making the deposition _publ_contact_author 'Dr A.J. Blake' _publ_contact_author_email A.J.Blake@nottingham.ac.uk #------------------------------------------------------------------------- #3 Publication details # Provide these details if the structure has been published, # accepted or submitted for publication # The CCDC journal deposition number, eg. 182/357, # should be included only if it has been assigned by the journal loop_ _publ_author_name 'Alexander J. Blake' _journal_name_full 'JCS Perkin Trans. 1' _journal_volume ? _journal_page_first '?' _journal_page_last '?' _journal_year 1999 _ccdc_journal_depnumber '?' _publ_section_title ; The Asymmetrical Synthesis of Phosphorus- and Sulfur-Containing Tricarbonyl(eta-6-arene)chromium Complexes using the Chiral Base Approach by A. Ariffin, A.J. Blake, R.A. Ewin, W-S. Li & N.S. Simpkins ; data_(3) # Code CROTMS _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H23 Cr O4 P Si' _chemical_formula_weight 486.48 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' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 '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 tetragonal _symmetry_space_group_name_H-M P4(1)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+1/4' 'y+1/2, -x+1/2, z+3/4' '-x+1/2, y+1/2, -z+1/4' 'x+1/2, -y+1/2, -z+3/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 12.69(2) _cell_length_b 12.69(2) _cell_length_c 29.55(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4759(13) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 15 _cell_measurement_theta_min 12.5 _cell_measurement_theta_max 14.0 _exptl_crystal_description tablet _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.358 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2016 _exptl_absorpt_coefficient_mu 0.625 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.807 _exptl_absorpt_correction_T_max 0.862 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe Stadi-4 four-circle' _diffrn_measurement_method omega/theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 'variation +/-8.9' _diffrn_reflns_number 8953 _diffrn_reflns_av_R_equivalents 0.1235 _diffrn_reflns_av_sigmaI/netI 0.1199 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 25.01 _reflns_number_total 4185 _reflns_number_gt 3191 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STADI4 (Stoe & Cie, 1997a)' _computing_cell_refinement 'STADI4 (Stoe & Cie, 1997a)' _computing_data_reduction 'X-RED (Stoe & Cie, 1997b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1994)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.020P)^2^+5.09P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary 'difference Fourier' _atom_sites_solution_hydrogens 'introduced at calculated postions' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00022(7) _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 -0.04(4) _refine_ls_number_reflns 4185 _refine_ls_number_parameters 281 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0877 _refine_ls_R_factor_gt 0.0536 _refine_ls_wR_factor_ref 0.1081 _refine_ls_wR_factor_gt 0.0950 _refine_ls_goodness_of_fit_ref 1.160 _refine_ls_restrained_S_all 1.158 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr Cr 0.53072(6) 0.90187(6) 0.12473(3) 0.0215(2) Uani 1 d . . . C1 C 0.5415(4) 1.0736(3) 0.11337(15) 0.0180(11) Uani 1 d . . . C2 C 0.4418(4) 1.0542(4) 0.13646(17) 0.0212(11) Uani 1 d . . . C3 C 0.4487(4) 0.9964(4) 0.17744(18) 0.0265(12) Uani 1 d . . . H3 H 0.3870 0.9823 0.1933 0.032 Uiso 1 calc R . . C4 C 0.5446(4) 0.9596(4) 0.19510(17) 0.0265(11) Uani 1 d . . . H4 H 0.5447 0.9207 0.2218 0.032 Uiso 1 calc R . . C5 C 0.6391(4) 0.9805(4) 0.17343(18) 0.0256(12) Uani 1 d . . . H5 H 0.7027 0.9576 0.1856 0.031 Uiso 1 calc R . . C6 C 0.6361(3) 1.0373(4) 0.13244(17) 0.0218(11) Uani 1 d . . . HA H 0.6991 1.0513 0.1175 0.026 Uiso 1 calc R . . P P 0.54725(10) 1.14846(10) 0.06099(5) 0.0209(3) Uani 1 d . . . O O 0.4552(3) 1.1313(3) 0.03099(11) 0.0269(8) Uani 1 d . . . C7 C 0.5626(3) 1.2845(4) 0.07830(15) 0.0219(12) Uani 1 d D . . C8 C 0.5971(3) 1.3120(4) 0.12115(18) 0.0269(12) Uani 1 d D . . H8 H 0.6150 1.2596 0.1418 0.032 Uiso 1 calc R . . C9 C 0.6051(3) 1.4172(4) 0.13363(18) 0.0308(13) Uani 1 d D . . H9 H 0.6282 1.4351 0.1625 0.037 Uiso 1 calc R . . C10 C 0.5788(3) 1.4947(4) 0.10326(18) 0.0347(15) Uani 1 d D . . H10 H 0.5841 1.5652 0.1115 0.042 Uiso 1 calc R . . C11 C 0.5447(4) 1.4683(4) 0.0608(2) 0.0392(14) Uani 1 d D . . H11 H 0.5271 1.5210 0.0403 0.047 Uiso 1 calc R . . C12 C 0.5362(4) 1.3638(4) 0.04824(18) 0.0335(13) Uani 1 d D . . H12 H 0.5126 1.3467 0.0194 0.040 Uiso 1 calc R . . C13 C 0.6707(4) 1.1109(3) 0.03472(15) 0.0221(11) Uani 1 d D . . C14 C 0.7573(4) 1.1784(4) 0.03240(15) 0.0312(13) Uani 1 d D . . H14 H 0.7546 1.2438 0.0466 0.037 Uiso 1 calc R . . C15 C 0.8461(4) 1.1489(4) 0.00940(15) 0.0325(13) Uani 1 d D . . H15 H 0.9035 1.1943 0.0080 0.039 Uiso 1 calc R . . C16 C 0.8511(4) 1.0519(4) -0.01186(17) 0.0354(14) Uani 1 d D . . H16 H 0.9113 1.0323 -0.0276 0.043 Uiso 1 calc R . . C17 C 0.7655(4) 0.9844(4) -0.00941(17) 0.0297(13) Uani 1 d D . . H17 H 0.7690 0.9187 -0.0233 0.036 Uiso 1 calc R . . C18 C 0.6757(4) 1.0133(4) 0.01331(15) 0.0249(12) Uani 1 d D . . H18 H 0.6183 0.9678 0.0144 0.030 Uiso 1 calc R . . Si Si 0.30440(10) 1.10595(11) 0.12051(5) 0.0238(3) Uani 1 d . . . C19 C 0.3103(4) 1.2512(4) 0.1124(2) 0.0385(16) Uani 1 d . . . H19A H 0.2416 1.2770 0.1045 0.058 Uiso 1 calc R . . H19B H 0.3589 1.2674 0.0885 0.058 Uiso 1 calc R . . H19C H 0.3335 1.2840 0.1399 0.058 Uiso 1 calc R . . C20 C 0.2452(4) 1.0368(4) 0.07157(19) 0.0308(13) Uani 1 d . . . H20A H 0.1769 1.0659 0.0653 0.046 Uiso 1 calc R . . H20B H 0.2383 0.9632 0.0784 0.046 Uiso 1 calc R . . H20C H 0.2897 1.0454 0.0455 0.046 Uiso 1 calc R . . C21 C 0.2194(4) 1.0811(5) 0.1709(2) 0.0386(15) Uani 1 d . . . H21A H 0.1493 1.1058 0.1649 0.058 Uiso 1 calc R . . H21B H 0.2476 1.1179 0.1966 0.058 Uiso 1 calc R . . H21C H 0.2177 1.0069 0.1772 0.058 Uiso 1 calc R . . C22 C 0.6330(4) 0.8239(4) 0.0957(2) 0.0339(14) Uani 1 d . . . O22 O 0.6914(3) 0.7722(3) 0.07599(17) 0.0510(13) Uani 1 d . . . C23 C 0.4878(4) 0.7771(4) 0.1503(2) 0.0303(13) Uani 1 d . . . O23 O 0.4636(3) 0.6987(3) 0.16687(15) 0.0472(11) Uani 1 d . . . C24 C 0.4498(4) 0.8682(4) 0.07433(19) 0.0275(12) Uani 1 d . . . O24 O 0.4047(3) 0.8409(3) 0.04311(13) 0.0367(9) 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 0.0207(4) 0.0213(4) 0.0224(5) -0.0003(4) -0.0007(4) 0.0001(4) C1 0.022(2) 0.017(2) 0.015(3) -0.0054(17) -0.001(2) -0.003(2) C2 0.021(3) 0.021(3) 0.021(3) -0.011(2) 0.000(2) -0.003(2) C3 0.030(3) 0.026(3) 0.024(3) -0.004(2) 0.004(2) 0.001(2) C4 0.041(3) 0.022(3) 0.016(3) 0.003(2) -0.002(2) -0.001(2) C5 0.024(3) 0.025(3) 0.027(3) 0.002(2) -0.008(2) 0.003(2) C6 0.018(2) 0.019(2) 0.028(3) -0.003(2) 0.001(2) -0.006(2) P 0.0198(7) 0.0239(7) 0.0188(7) -0.0006(5) 0.0015(6) -0.0002(6) O 0.0242(19) 0.033(2) 0.023(2) -0.0030(15) -0.0036(16) -0.0021(16) C7 0.016(3) 0.026(3) 0.024(3) -0.002(2) 0.002(2) -0.002(2) C8 0.027(3) 0.025(3) 0.029(3) 0.000(2) 0.000(3) -0.006(2) C9 0.031(3) 0.037(3) 0.024(3) -0.009(2) 0.001(2) -0.006(3) C10 0.028(3) 0.020(3) 0.055(4) -0.002(3) 0.010(3) 0.002(2) C11 0.044(3) 0.028(3) 0.046(4) 0.007(3) -0.002(3) 0.013(3) C12 0.039(3) 0.033(3) 0.028(3) -0.002(3) 0.001(3) 0.008(3) C13 0.023(3) 0.028(3) 0.015(3) 0.001(2) -0.002(2) 0.004(2) C14 0.036(3) 0.028(3) 0.030(4) 0.001(2) 0.006(3) -0.005(2) C15 0.027(3) 0.043(3) 0.028(3) 0.003(3) 0.004(2) -0.007(3) C16 0.032(3) 0.038(3) 0.036(4) 0.003(3) 0.014(3) 0.010(3) C17 0.035(3) 0.029(3) 0.025(3) -0.004(2) 0.001(2) 0.006(2) C18 0.028(3) 0.028(3) 0.019(3) 0.001(2) 0.002(2) 0.001(2) Si 0.0188(7) 0.0249(7) 0.0278(9) -0.0062(7) 0.0020(6) 0.0001(6) C19 0.021(3) 0.031(3) 0.064(5) -0.011(3) 0.003(3) 0.006(2) C20 0.025(3) 0.034(3) 0.034(4) -0.008(3) -0.002(2) 0.004(3) C21 0.024(3) 0.046(4) 0.045(4) -0.001(3) 0.008(3) 0.007(3) C22 0.023(3) 0.025(3) 0.054(4) -0.005(3) -0.006(3) -0.003(2) O22 0.031(2) 0.051(3) 0.071(4) -0.027(2) -0.001(2) 0.011(2) C23 0.027(3) 0.031(3) 0.033(4) 0.002(3) -0.004(3) 0.005(2) O23 0.053(3) 0.034(2) 0.055(3) 0.013(2) -0.012(2) -0.011(2) C24 0.030(3) 0.023(3) 0.030(3) 0.001(2) 0.005(3) 0.000(2) O24 0.047(2) 0.035(2) 0.028(2) -0.0057(18) -0.008(2) -0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr C1 2.209(6) . ? Cr C2 2.265(6) . ? Cr C3 2.225(6) . ? Cr C4 2.212(6) . ? Cr C5 2.226(6) . ? Cr C6 2.190(6) . ? Cr C23 1.837(6) . ? Cr C22 1.843(6) . ? Cr C24 1.859(6) . ? C1 C2 1.459(7) . ? C2 C3 1.418(7) . ? C3 C4 1.404(7) . ? C4 C5 1.385(7) . ? C5 C6 1.410(7) . ? C1 C6 1.404(7) . ? C1 P 1.817(5) . ? P O 1.482(4) . ? P C7 1.811(6) . ? P C13 1.812(6) . ? C7 C12 1.383(6) . ? C7 C8 1.384(6) . ? C8 C9 1.389(6) . ? C9 C10 1.373(6) . ? C10 C11 1.369(7) . ? C11 C12 1.381(7) . ? C13 C18 1.392(6) . ? C13 C14 1.395(6) . ? C14 C15 1.369(7) . ? C15 C16 1.383(6) . ? C16 C17 1.385(6) . ? C17 C18 1.373(6) . ? C2 Si 1.922(6) . ? Si C20 1.851(6) . ? Si C19 1.860(6) . ? Si C21 1.865(6) . ? C22 O22 1.149(7) . ? C23 O23 1.150(6) . ? C24 O24 1.139(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C23 Cr C22 86.5(2) . . ? C23 Cr C24 88.2(2) . . ? C22 Cr C24 83.8(3) . . ? C23 Cr C6 144.6(2) . . ? C22 Cr C6 92.3(2) . . ? C24 Cr C6 127.0(2) . . ? C23 Cr C1 158.6(2) . . ? C22 Cr C1 114.5(2) . . ? C24 Cr C1 98.0(2) . . ? C6 Cr C1 37.21(17) . . ? C23 Cr C4 85.5(2) . . ? C22 Cr C4 124.0(2) . . ? C24 Cr C4 150.9(2) . . ? C6 Cr C4 66.02(19) . . ? C1 Cr C4 79.11(18) . . ? C23 Cr C3 92.2(2) . . ? C22 Cr C3 160.9(2) . . ? C24 Cr C3 115.2(2) . . ? C6 Cr C3 77.87(18) . . ? C1 Cr C3 66.64(18) . . ? C4 Cr C3 36.90(19) . . ? C23 Cr C5 107.6(2) . . ? C22 Cr C5 96.1(2) . . ? C24 Cr C5 164.2(2) . . ? C6 Cr C5 37.24(19) . . ? C1 Cr C5 67.54(19) . . ? C4 Cr C5 36.37(19) . . ? C3 Cr C5 66.1(2) . . ? C23 Cr C2 121.6(2) . . ? C22 Cr C2 151.6(2) . . ? C24 Cr C2 92.5(2) . . ? C6 Cr C2 67.59(16) . . ? C1 Cr C2 38.04(17) . . ? C4 Cr C2 67.24(19) . . ? C3 Cr C2 36.82(18) . . ? C5 Cr C2 80.02(17) . . ? C6 C1 C2 119.9(4) . . ? C6 C1 P 118.6(4) . . ? C2 C1 P 121.4(4) . . ? C6 C1 Cr 70.6(2) . . ? C2 C1 Cr 73.0(3) . . ? P C1 Cr 130.3(2) . . ? C3 C2 C1 115.7(4) . . ? C3 C2 Si 116.2(4) . . ? C1 C2 Si 127.9(4) . . ? C3 C2 Cr 70.1(3) . . ? C1 C2 Cr 68.9(2) . . ? Si C2 Cr 134.9(2) . . ? C4 C3 C2 122.9(5) . . ? C4 C3 Cr 71.0(3) . . ? C2 C3 Cr 73.1(3) . . ? C5 C4 C3 121.0(5) . . ? C5 C4 Cr 72.4(3) . . ? C3 C4 Cr 72.0(3) . . ? C4 C5 C6 118.1(5) . . ? C4 C5 Cr 71.2(3) . . ? C6 C5 Cr 70.0(3) . . ? C1 C6 C5 122.4(4) . . ? C1 C6 Cr 72.1(3) . . ? C5 C6 Cr 72.8(3) . . ? O P C7 113.2(2) . . ? O P C13 112.7(2) . . ? C7 P C13 106.17(19) . . ? O P C1 113.7(2) . . ? C7 P C1 105.2(2) . . ? C13 P C1 105.2(2) . . ? C12 C7 C8 118.7(5) . . ? C12 C7 P 119.1(4) . . ? C8 C7 P 122.2(3) . . ? C7 C8 C9 120.5(5) . . ? C10 C9 C8 119.8(5) . . ? C11 C10 C9 120.0(5) . . ? C10 C11 C12 120.4(5) . . ? C11 C12 C7 120.5(5) . . ? C18 C13 C14 119.2(5) . . ? C18 C13 P 117.9(3) . . ? C14 C13 P 122.7(4) . . ? C15 C14 C13 120.3(5) . . ? C14 C15 C16 120.5(5) . . ? C15 C16 C17 119.4(5) . . ? C18 C17 C16 120.7(5) . . ? C17 C18 C13 119.9(5) . . ? C20 Si C19 112.6(3) . . ? C20 Si C21 108.0(3) . . ? C19 Si C21 107.1(3) . . ? C20 Si C2 113.4(2) . . ? C19 Si C2 109.5(2) . . ? C21 Si C2 105.7(3) . . ? O22 C22 Cr 175.5(5) . . ? O23 C23 Cr 178.1(5) . . ? O24 C24 Cr 174.9(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -1.1(6) . . . . ? P C1 C2 C3 -178.9(3) . . . . ? C6 C1 C2 Si 173.9(3) . . . . ? P C1 C2 Si -3.9(6) . . . . ? C1 C2 C3 C4 -0.1(7) . . . . ? Si C2 C3 C4 -175.7(4) . . . . ? C2 C3 C4 C5 1.5(8) . . . . ? C3 C4 C5 C6 -1.7(7) . . . . ? C2 C1 C6 C5 0.9(7) . . . . ? P C1 C6 C5 178.8(4) . . . . ? C4 C5 C6 C1 0.5(7) . . . . ? C6 C1 P O 146.9(3) . . . . ? C2 C1 P O -35.3(4) . . . . ? C6 C1 P C7 -88.8(4) . . . . ? C2 C1 P C7 89.0(4) . . . . ? C6 C1 P C13 23.1(4) . . . . ? C2 C1 P C13 -159.1(3) . . . . ? O P C7 C12 -34.8(4) . . . . ? C13 P C7 C12 89.3(3) . . . . ? C1 P C7 C12 -159.5(3) . . . . ? O P C7 C8 143.2(3) . . . . ? C13 P C7 C8 -92.6(3) . . . . ? C1 P C7 C8 18.6(3) . . . . ? C12 C7 C8 C9 -0.1(2) . . . . ? P C7 C8 C9 -178.2(3) . . . . ? C7 C8 C9 C10 -0.1(2) . . . . ? C8 C9 C10 C11 0.0(5) . . . . ? C9 C10 C11 C12 0.2(6) . . . . ? C10 C11 C12 C7 -0.3(6) . . . . ? C8 C7 C12 C11 0.3(5) . . . . ? P C7 C12 C11 178.4(4) . . . . ? O P C13 C18 -47.8(4) . . . . ? C7 P C13 C18 -172.3(3) . . . . ? C1 P C13 C18 76.5(3) . . . . ? O P C13 C14 127.5(3) . . . . ? C7 P C13 C14 3.1(3) . . . . ? C1 P C13 C14 -108.1(3) . . . . ? C18 C13 C14 C15 -0.1(2) . . . . ? P C13 C14 C15 -175.4(3) . . . . ? C13 C14 C15 C16 0.1(2) . . . . ? C14 C15 C16 C17 -0.5(5) . . . . ? C15 C16 C17 C18 0.9(6) . . . . ? C16 C17 C18 C13 -0.9(6) . . . . ? C14 C13 C18 C17 0.5(5) . . . . ? P C13 C18 C17 176.0(4) . . . . ? C3 C2 Si C20 -109.3(4) . . . . ? C1 C2 Si C20 75.8(5) . . . . ? C3 C2 Si C19 124.0(4) . . . . ? C1 C2 Si C19 -51.0(5) . . . . ? C3 C2 Si C21 8.9(4) . . . . ? C1 C2 Si C21 -166.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.68 _refine_diff_density_min -0.39 _refine_diff_density_rms 0.07 #===END data_(21) # Code CRCOHP _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H21 Cr O4 P' _chemical_formula_sum 'C28 H21 Cr O4 P' _chemical_formula_weight 504.42 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' 'P' 'P' 0.1023 0.0942 '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 10.820(2) _cell_length_b 11.206(2) _cell_length_c 14.618(2) _cell_angle_alpha 75.33(2) _cell_angle_beta 86.12(2) _cell_angle_gamma 78.60(2) _cell_volume 1680.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 29 _cell_measurement_theta_min 13.5 _cell_measurement_theta_max 17.5 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.31 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 0.997 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 520 _exptl_absorpt_coefficient_mu 0.411 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.811 _exptl_absorpt_correction_T_max 0.885 _exptl_absorpt_process_details 'X-RED (Stoe & Cie, 1997b)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe Stadi-4 four-circle' _diffrn_measurement_method omega/theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% none _diffrn_reflns_number 10515 _diffrn_reflns_av_R_equivalents 0.023 _diffrn_reflns_av_sigmaI/netI 0.031 _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 -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 25.05 _reflns_number_total 5907 _reflns_number_gt 5017 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STADI4 (Stoe & Cie, 1997a)' _computing_cell_refinement STADI4 _computing_data_reduction 'X-RED (Stoe & Cie, 1997b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997); PLATON (Spek, 1998)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1994)' _computing_publication_material 'SHELXL-97, PLATON' _refine_special_details ; A region of poorly-defined solvent molecules was identified and all attempts to model this in terms of rational atomic sites and molecular geometry were unsuccessful. This problem was solved by applying the SQUEEZE procedure available as part of PLATON (Spek, 1998). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.048P)^2^+1.04P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary 'difference' _atom_sites_solution_hydrogens 'placed geometrically' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0033(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5907 _refine_ls_number_parameters 309 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0568 _refine_ls_R_factor_gt 0.0468 _refine_ls_wR_factor_ref 0.115 _refine_ls_wR_factor_gt 0.109 _refine_ls_goodness_of_fit_ref 1.12 _refine_ls_restrained_S_all 1.12 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr Cr 0.14048(4) 0.05864(4) 0.27371(3) 0.03098(14) Uani 1 1 d . . . C1 C 0.2978(3) 0.0979(2) 0.2737(2) 0.0404(6) Uani 1 1 d . . . O1 O 0.39553(19) 0.1251(2) 0.27168(18) 0.0625(6) Uani 1 1 d . . . C2 C 0.0781(3) 0.2268(3) 0.2293(2) 0.0473(7) Uani 1 1 d . . . O2 O 0.0398(2) 0.3330(2) 0.2015(2) 0.0741(8) Uani 1 1 d . . . C3 C 0.1146(3) 0.0810(3) 0.3942(2) 0.0516(8) Uani 1 1 d . . . O3 O 0.0965(3) 0.0965(3) 0.47018(19) 0.0834(9) Uani 1 1 d . . . C1B C 0.2281(2) -0.1290(2) 0.25143(17) 0.0264(5) Uani 1 1 d D . . C2B C 0.1355(2) -0.1437(2) 0.32326(18) 0.0299(5) Uani 1 1 d D . . H2B H 0.1622 -0.1887 0.3892 0.036 Uiso 1 1 calc R . . C3B C 0.0096(2) -0.0759(2) 0.30843(19) 0.0339(6) Uani 1 1 d D . . H3B H -0.0500 -0.0749 0.3637 0.041 Uiso 1 1 calc R . . C4B C -0.0237(2) 0.0062(2) 0.22128(19) 0.0326(6) Uani 1 1 d D . . H4B H -0.1068 0.0653 0.2146 0.039 Uiso 1 1 calc R . . C5B C 0.0685(2) 0.0223(2) 0.14846(18) 0.0305(5) Uani 1 1 d D . . H5B H 0.0487 0.0937 0.0914 0.037 Uiso 1 1 calc R . . C6B C 0.1943(2) -0.0432(2) 0.16128(17) 0.0260(5) Uani 1 1 d D . . C C 0.3597(2) -0.2073(2) 0.26786(17) 0.0278(5) Uani 1 1 d . . . H H 0.4225 -0.1541 0.2373 0.033 Uiso 1 1 calc R . . O O 0.38092(16) -0.24696(17) 0.36718(12) 0.0362(4) Uani 1 1 d . . . H1O H 0.4587 -0.2620 0.3769 0.054 Uiso 1 1 calc R . . C1P C 0.3739(2) -0.3187(2) 0.22415(17) 0.0295(5) Uani 1 1 d D . . C2P C 0.2899(2) -0.4015(2) 0.24851(19) 0.0403(6) Uani 1 1 d D . . H2P H 0.2236 -0.3886 0.2930 0.048 Uiso 1 1 calc R . . C3P C 0.3027(3) -0.5021(3) 0.2082(2) 0.0498(8) Uani 1 1 d D . . H3P H 0.2452 -0.5583 0.2255 0.060 Uiso 1 1 calc R . . C4P C 0.3975(3) -0.5219(3) 0.1437(2) 0.0510(8) Uani 1 1 d D . . H4P H 0.4053 -0.5914 0.1162 0.061 Uiso 1 1 calc R . . C5P C 0.4811(3) -0.4410(3) 0.1189(2) 0.0457(7) Uani 1 1 d D . . H5P H 0.5468 -0.4545 0.0741 0.055 Uiso 1 1 calc R . . C6P C 0.4699(2) -0.3398(2) 0.15916(19) 0.0369(6) Uani 1 1 d D . . H6P H 0.5284 -0.2845 0.1421 0.044 Uiso 1 1 calc R . . P P 0.31513(5) -0.01824(5) 0.06591(4) 0.02664(16) Uani 1 1 d . . . C7P C 0.2854(2) -0.1236(2) -0.00466(17) 0.0266(5) Uani 1 1 d D . . C8P C 0.1920(2) -0.19671(19) 0.01708(17) 0.0288(5) Uani 1 1 d D . . H8P H 0.1367 -0.1908 0.0697 0.035 Uiso 1 1 calc R . . C9P C 0.1796(2) -0.2781(2) -0.03789(19) 0.0343(6) Uani 1 1 d D . . H9P H 0.1159 -0.3279 -0.0224 0.041 Uiso 1 1 calc R . . C10P C 0.2587(2) -0.2872(2) -0.1146(2) 0.0395(6) Uani 1 1 d D . . H10 H 0.2498 -0.3430 -0.1520 0.047 Uiso 1 1 calc R . . C11P C 0.3517(2) -0.2144(2) -0.1371(2) 0.0403(6) Uani 1 1 d D . . H11 H 0.4061 -0.2201 -0.1903 0.048 Uiso 1 1 calc R . . C12P C 0.3656(2) -0.1337(2) -0.08247(19) 0.0339(6) Uani 1 1 d D . . H12 H 0.4300 -0.0848 -0.0980 0.041 Uiso 1 1 calc R . . C13P C 0.2428(2) 0.1369(2) -0.00637(17) 0.0295(5) Uani 1 1 d D . . C14P C 0.2608(2) 0.2413(2) 0.02264(19) 0.0391(6) Uani 1 1 d D . . H14 H 0.3105 0.2301 0.0764 0.047 Uiso 1 1 calc R . . C15P C 0.2067(3) 0.3614(2) -0.0264(2) 0.0483(7) Uani 1 1 d D . . H15 H 0.2187 0.4322 -0.0058 0.058 Uiso 1 1 calc R . . C16P C 0.1351(3) 0.3781(3) -0.1055(2) 0.0499(8) Uani 1 1 d D . . H16 H 0.0977 0.4602 -0.1391 0.060 Uiso 1 1 calc R . . C17P C 0.1187(3) 0.2753(3) -0.1349(2) 0.0482(7) Uani 1 1 d D . . H17 H 0.0710 0.2868 -0.1898 0.058 Uiso 1 1 calc R . . C18P C 0.1707(2) 0.1552(2) -0.08567(19) 0.0372(6) Uani 1 1 d D . . H18 H 0.1571 0.0849 -0.1061 0.045 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr 0.0247(2) 0.0270(2) 0.0454(3) -0.01431(18) 0.00134(17) -0.00818(16) C1 0.0352(15) 0.0355(14) 0.0587(18) -0.0251(13) 0.0026(13) -0.0096(12) O1 0.0369(12) 0.0750(16) 0.0952(18) -0.0441(14) 0.0074(11) -0.0293(11) C2 0.0310(14) 0.0357(16) 0.082(2) -0.0258(15) -0.0026(14) -0.0072(12) O2 0.0568(14) 0.0310(12) 0.133(2) -0.0221(13) -0.0187(15) 0.0030(10) C3 0.0525(18) 0.0575(19) 0.058(2) -0.0259(16) 0.0078(15) -0.0305(15) O3 0.104(2) 0.116(2) 0.0638(16) -0.0526(16) 0.0220(15) -0.0678(19) C1B 0.0243(12) 0.0220(11) 0.0364(13) -0.0092(10) -0.0037(10) -0.0087(9) C2B 0.0284(12) 0.0278(12) 0.0369(14) -0.0099(10) 0.0000(10) -0.0114(10) C3B 0.0294(13) 0.0338(13) 0.0447(15) -0.0163(12) 0.0045(11) -0.0138(11) C4B 0.0217(12) 0.0292(12) 0.0496(16) -0.0127(11) -0.0024(11) -0.0066(10) C5B 0.0244(12) 0.0252(12) 0.0430(14) -0.0074(10) -0.0044(10) -0.0068(9) C6B 0.0223(11) 0.0193(11) 0.0372(13) -0.0061(10) -0.0023(10) -0.0060(9) C 0.0254(12) 0.0268(12) 0.0308(13) -0.0042(10) -0.0052(10) -0.0059(9) O 0.0312(9) 0.0418(10) 0.0335(10) -0.0052(8) -0.0074(7) -0.0045(8) C1P 0.0254(12) 0.0240(12) 0.0357(13) -0.0040(10) -0.0104(10) 0.0025(9) C2P 0.0348(14) 0.0296(13) 0.0562(18) -0.0090(12) -0.0053(12) -0.0055(11) C3P 0.0431(17) 0.0311(14) 0.077(2) -0.0129(14) -0.0168(15) -0.0076(12) C4P 0.0542(19) 0.0332(15) 0.067(2) -0.0231(14) -0.0223(16) 0.0086(13) C5P 0.0457(17) 0.0389(15) 0.0501(17) -0.0177(13) -0.0089(13) 0.0097(13) C6P 0.0311(13) 0.0304(13) 0.0459(15) -0.0075(11) -0.0078(12) 0.0018(10) P 0.0214(3) 0.0229(3) 0.0358(3) -0.0046(2) -0.0037(2) -0.0066(2) C7P 0.0203(11) 0.0199(11) 0.0374(13) -0.0046(10) -0.0064(10) 0.0007(9) C8P 0.0229(11) 0.0212(11) 0.0400(14) -0.0037(10) -0.0046(10) -0.0021(9) C9P 0.0286(13) 0.0234(12) 0.0517(16) -0.0082(11) -0.0051(11) -0.0064(10) C10P 0.0361(14) 0.0269(13) 0.0587(18) -0.0191(12) -0.0067(13) 0.0000(11) C11P 0.0322(14) 0.0363(14) 0.0535(17) -0.0192(13) 0.0049(12) 0.0000(11) C12P 0.0239(12) 0.0294(13) 0.0493(16) -0.0116(11) 0.0016(11) -0.0052(10) C13P 0.0232(12) 0.0242(12) 0.0400(14) -0.0036(10) -0.0006(10) -0.0076(9) C14P 0.0408(15) 0.0281(13) 0.0504(16) -0.0063(12) -0.0070(12) -0.0131(11) C15P 0.0526(18) 0.0225(13) 0.069(2) -0.0068(13) -0.0024(15) -0.0110(12) C16P 0.0488(17) 0.0266(14) 0.063(2) 0.0058(13) -0.0019(15) -0.0018(12) C17P 0.0536(18) 0.0374(15) 0.0454(17) 0.0046(13) -0.0120(14) -0.0050(13) C18P 0.0390(15) 0.0310(13) 0.0407(15) -0.0055(11) -0.0062(12) -0.0072(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr C1 1.841(3) . ? Cr C2 1.834(3) . ? Cr C3 1.836(3) . ? Cr C1B 2.223(2) . ? Cr C2B 2.209(2) . ? Cr C3B 2.212(2) . ? Cr C4B 2.217(2) . ? Cr C5B 2.195(3) . ? Cr C6B 2.214(2) . ? C1 O1 1.153(3) . ? C2 O2 1.156(3) . ? C3 O3 1.166(4) . ? C1B C2B 1.403(3) . ? C2B C3B 1.424(3) . ? C3B C4B 1.391(4) . ? C4B C5B 1.411(4) . ? C5B C6B 1.414(3) . ? C6B C1B 1.442(3) . ? C1B C 1.517(3) . ? C6B P 1.852(2) . ? C O 1.427(3) . ? C C1P 1.519(3) . ? C1P C2P 1.391(4) . ? C2P C3P 1.379(4) . ? C3P C4P 1.370(5) . ? C4P C5P 1.373(4) . ? C5P C6P 1.386(4) . ? C6P C1P 1.385(4) . ? P C7P 1.837(2) . ? P C13P 1.842(2) . ? C7P C8P 1.395(3) . ? C8P C9P 1.390(3) . ? C9P C10P 1.377(4) . ? C10P C11P 1.389(4) . ? C11P C12P 1.384(4) . ? C12P C7P 1.398(3) . ? C13P C14P 1.392(3) . ? C14P C15P 1.388(4) . ? C15P C16P 1.389(4) . ? C16P C17P 1.373(4) . ? C17P C18P 1.382(4) . ? C18P C13P 1.390(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Cr C3 88.13(15) . . ? C2 Cr C1 88.16(12) . . ? C3 Cr C1 88.44(13) . . ? C2 Cr C5B 89.66(12) . . ? C3 Cr C5B 149.68(11) . . ? C1 Cr C5B 121.71(11) . . ? C2 Cr C2B 157.21(11) . . ? C3 Cr C2B 91.97(12) . . ? C1 Cr C2B 114.63(11) . . ? C5B Cr C2B 78.86(9) . . ? C2 Cr C3B 119.70(11) . . ? C3 Cr C3B 88.47(11) . . ? C1 Cr C3B 151.84(11) . . ? C5B Cr C3B 66.61(9) . . ? C2B Cr C3B 37.57(9) . . ? C2 Cr C6B 114.04(12) . . ? C3 Cr C6B 157.81(12) . . ? C1 Cr C6B 93.03(10) . . ? C5B Cr C6B 37.40(9) . . ? C2B Cr C6B 67.32(9) . . ? C3B Cr C6B 79.83(9) . . ? C2 Cr C4B 92.11(11) . . ? C3 Cr C4B 112.58(12) . . ? C1 Cr C4B 158.98(11) . . ? C5B Cr C4B 37.30(9) . . ? C2B Cr C4B 66.86(9) . . ? C3B Cr C4B 36.62(10) . . ? C6B Cr C4B 67.70(9) . . ? C2 Cr C1B 151.78(12) . . ? C3 Cr C1B 119.99(13) . . ? C1 Cr C1B 90.15(10) . . ? C5B Cr C1B 67.49(9) . . ? C2B Cr C1B 36.91(9) . . ? C3B Cr C1B 67.45(8) . . ? C6B Cr C1B 37.93(9) . . ? C4B Cr C1B 79.75(9) . . ? Cr C1 O1 178.2(3) . . ? Cr C2 O2 179.3(3) . . ? Cr C3 O3 178.9(4) . . ? C2B C1B C6B 119.0(2) . . ? C2B C1B C 119.9(2) . . ? C6B C1B C 121.0(2) . . ? C2B C1B Cr 71.00(12) . . ? C6B C1B Cr 70.67(12) . . ? C C1B Cr 132.70(15) . . ? C1B C2B C3B 121.2(2) . . ? C1B C2B Cr 72.09(12) . . ? C3B C2B Cr 71.33(12) . . ? C4B C3B C2B 120.0(2) . . ? C4B C3B Cr 71.86(14) . . ? C2B C3B Cr 71.10(12) . . ? C3B C4B C5B 119.5(2) . . ? C3B C4B Cr 71.52(13) . . ? C5B C4B Cr 70.53(13) . . ? C4B C5B C6B 121.8(2) . . ? C4B C5B Cr 72.17(14) . . ? C6B C5B Cr 72.00(14) . . ? C5B C6B C1B 118.5(2) . . ? C5B C6B P 121.28(18) . . ? C1B C6B P 120.17(17) . . ? C5B C6B Cr 70.60(14) . . ? C1B C6B Cr 71.40(13) . . ? P C6B Cr 128.59(11) . . ? O C C1B 108.73(19) . . ? O C C1P 111.35(19) . . ? C1B C C1P 110.03(18) . . ? C6P C1P C2P 118.7(2) . . ? C6P C1P C 121.0(2) . . ? C2P C1P C 120.4(2) . . ? C3P C2P C1P 120.2(3) . . ? C4P C3P C2P 120.8(3) . . ? C3P C4P C5P 119.8(3) . . ? C4P C5P C6P 120.1(3) . . ? C1P C6P C5P 120.5(3) . . ? C7P P C13P 101.92(11) . . ? C7P P C6B 100.97(10) . . ? C13P P C6B 100.70(10) . . ? C8P C7P C12P 118.9(2) . . ? C8P C7P P 124.08(19) . . ? C12P C7P P 117.00(17) . . ? C9P C8P C7P 120.3(2) . . ? C10P C9P C8P 120.5(2) . . ? C9P C10P C11P 119.7(2) . . ? C12P C11P C10P 120.4(3) . . ? C11P C12P C7P 120.3(2) . . ? C18P C13P C14P 118.9(2) . . ? C18P C13P P 124.34(19) . . ? C14P C13P P 116.79(19) . . ? C15P C14P C13P 120.5(3) . . ? C14P C15P C16P 119.9(3) . . ? C17P C16P C15P 119.7(3) . . ? C16P C17P C18P 120.8(3) . . ? C17P C18P C13P 120.3(3) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.28 _refine_diff_density_min -0.33 _refine_diff_density_rms 0.05 #===END data_(33) # Code CRTHPH _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H10 Cr O3 S' _chemical_formula_weight 286.26 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' 'S' 'S' 0.1246 0.1234 '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 6.581(6) _cell_length_b 8.758(9) _cell_length_c 10.333(8) _cell_angle_alpha 90.00 _cell_angle_beta 93.88(8) _cell_angle_gamma 90.00 _cell_volume 594.2(9) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 59 _cell_measurement_theta_min 12.4 _cell_measurement_theta_max 17.3 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.62 _exptl_crystal_size_mid 0.62 _exptl_crystal_size_min 0.44 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.600 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 292 _exptl_absorpt_coefficient_mu 1.129 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.5412 _exptl_absorpt_correction_T_max 0.6365 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe Stadi-4 four-circle' _diffrn_measurement_method omega/theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 'variation +/-2.3' _diffrn_reflns_number 2082 _diffrn_reflns_av_R_equivalents 0.0205 _diffrn_reflns_av_sigmaI/netI 0.0080 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 25.06 _reflns_number_total 1971 _reflns_number_gt 1952 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STADI4 (Stoe & Cie, 1997a)' _computing_cell_refinement 'STADI4 (Stoe & Cie, 1997a)' _computing_data_reduction 'X-RED (Stoe & Cie, 1997b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1994)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+0.5600P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.011(3) _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 1971 _refine_ls_number_parameters 155 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0287 _refine_ls_R_factor_gt 0.0283 _refine_ls_wR_factor_ref 0.0785 _refine_ls_wR_factor_gt 0.0777 _refine_ls_goodness_of_fit_ref 1.127 _refine_ls_restrained_S_all 1.127 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr Cr 0.03618(7) 0.72036(5) 0.74402(4) 0.01764(15) Uani 1 1 d . . . C1 C 0.2767(5) 1.0542(4) 0.6931(3) 0.0262(7) Uani 1 1 d . . . H1 H 0.1926 1.0640 0.6093 0.031 Uiso 1 1 calc R . . S2 S 0.14647(15) 1.15013(10) 0.82136(9) 0.0341(2) Uani 1 1 d . . . C3' C 0.2535(5) 0.8624(4) 0.8655(3) 0.0186(6) Uani 1 1 d . . . C3 C 0.2158(5) 1.0041(4) 0.9418(3) 0.0257(7) Uani 1 1 d . . . H3A H 0.3399 1.0342 0.9951 0.031 Uiso 1 1 calc R . . H3B H 0.1039 0.9876 0.9996 0.031 Uiso 1 1 calc R . . C4 C 0.2591(4) 0.7116(4) 0.9160(3) 0.0230(6) Uani 1 1 d . . . H4 H 0.2103 0.6913 1.0039 0.028 Uiso 1 1 calc R . . C5 C 0.2984(5) 0.5895(4) 0.8344(4) 0.0253(7) Uani 1 1 d . . . H5 H 0.2766 0.4827 0.8648 0.030 Uiso 1 1 calc R . . C6 C 0.3311(5) 0.6161(4) 0.7012(3) 0.0257(7) Uani 1 1 d . . . H6 H 0.3331 0.5278 0.6399 0.031 Uiso 1 1 calc R . . C7' C 0.2838(5) 0.8886(4) 0.7340(3) 0.0193(6) Uani 1 1 d . . . C7 C 0.3242(5) 0.7637(4) 0.6528(3) 0.0248(7) Uani 1 1 d . . . H7 H 0.3210 0.7798 0.5569 0.030 Uiso 1 1 calc R . . C8 C 0.4878(6) 1.1173(4) 0.6766(4) 0.0354(8) Uani 1 1 d . . . H8A H 0.5499 1.0618 0.6070 0.053 Uiso 1 1 calc R . . H8B H 0.5721 1.1050 0.7577 0.053 Uiso 1 1 calc R . . H8C H 0.4778 1.2260 0.6542 0.053 Uiso 1 1 calc R . . C9 C -0.1011(5) 0.8032(4) 0.6007(3) 0.0274(7) Uani 1 1 d . . . O9 O -0.1892(5) 0.8557(3) 0.5109(2) 0.0420(7) Uani 1 1 d . . . C10 C -0.1620(5) 0.7997(4) 0.8414(3) 0.0237(7) Uani 1 1 d . . . O10 O -0.2811(4) 0.8567(3) 0.9037(2) 0.0320(6) Uani 1 1 d . . . C11 C -0.1137(5) 0.5436(4) 0.7118(4) 0.0300(8) Uani 1 1 d . . . O11 O -0.2104(5) 0.4368(3) 0.6892(3) 0.0490(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr 0.0178(2) 0.0152(2) 0.0197(2) 0.00081(18) -0.00078(15) -0.0026(2) C1 0.0298(18) 0.0216(16) 0.0278(16) -0.0004(13) 0.0055(14) -0.0053(14) S2 0.0404(5) 0.0180(4) 0.0445(5) -0.0036(4) 0.0065(4) 0.0047(4) C3' 0.0119(15) 0.0232(15) 0.0204(14) -0.0042(11) -0.0018(11) -0.0017(12) C3 0.0250(17) 0.0252(17) 0.0268(16) -0.0095(13) -0.0002(13) -0.0013(14) C4 0.0192(13) 0.0271(15) 0.0224(13) 0.0055(15) -0.0019(10) -0.0011(16) C5 0.0187(17) 0.0186(15) 0.0374(19) 0.0053(13) -0.0065(14) -0.0019(13) C6 0.0205(16) 0.0218(17) 0.0346(18) -0.0085(13) -0.0003(14) 0.0008(14) C7' 0.0163(15) 0.0197(15) 0.0220(15) 0.0001(12) 0.0015(11) -0.0042(12) C7 0.0254(16) 0.0265(17) 0.0233(14) -0.0051(12) 0.0068(12) -0.0035(13) C8 0.034(2) 0.0262(18) 0.046(2) 0.0092(15) 0.0057(16) -0.0079(16) C9 0.0313(19) 0.0248(17) 0.0264(16) -0.0020(13) 0.0029(14) -0.0042(15) O9 0.0528(17) 0.0430(16) 0.0281(13) 0.0082(11) -0.0127(12) 0.0049(14) C10 0.0243(17) 0.0233(16) 0.0228(15) 0.0049(12) -0.0031(13) -0.0008(14) O10 0.0218(12) 0.0422(16) 0.0324(12) 0.0010(11) 0.0044(10) 0.0016(11) C11 0.0251(18) 0.0249(17) 0.039(2) 0.0010(14) -0.0021(15) -0.0028(16) O11 0.0385(17) 0.0254(14) 0.082(2) -0.0035(13) -0.0066(14) -0.0143(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr C9 1.831(4) . ? Cr C10 1.837(4) . ? Cr C11 1.854(4) . ? Cr C7' 2.205(3) . ? Cr C7 2.206(4) . ? Cr C6 2.217(4) . ? Cr C3' 2.220(4) . ? Cr C5 2.224(4) . ? Cr C4 2.227(4) . ? C1 C7' 1.510(5) . ? C1 C8 1.515(5) . ? C1 S2 1.830(4) . ? S2 C3 1.820(4) . ? C3' C7' 1.405(5) . ? C3' C4 1.420(5) . ? C3' C3 1.500(4) . ? C4 C5 1.397(5) . ? C5 C6 1.427(5) . ? C6 C7 1.386(5) . ? C7' C7 1.415(5) . ? C9 O9 1.156(4) . ? C10 O10 1.159(4) . ? C11 O11 1.146(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C9 Cr C10 87.90(16) . . ? C9 Cr C11 87.59(16) . . ? C10 Cr C11 91.47(16) . . ? C9 Cr C7' 91.33(15) . . ? C10 Cr C7' 109.10(15) . . ? C11 Cr C7' 159.36(14) . . ? C9 Cr C7 88.72(16) . . ? C10 Cr C7 146.23(14) . . ? C11 Cr C7 121.94(15) . . ? C7' Cr C7 37.42(12) . . ? C9 Cr C6 113.11(15) . . ? C10 Cr C6 158.28(13) . . ? C11 Cr C6 94.73(16) . . ? C7' Cr C6 66.80(15) . . ? C7 Cr C6 36.52(14) . . ? C9 Cr C3' 119.94(15) . . ? C10 Cr C3' 86.12(15) . . ? C11 Cr C3' 152.19(14) . . ? C7' Cr C3' 37.03(12) . . ? C7 Cr C3' 66.77(13) . . ? C6 Cr C3' 78.73(13) . . ? C9 Cr C5 150.46(15) . . ? C10 Cr C5 121.63(15) . . ? C11 Cr C5 91.91(16) . . ? C7' Cr C5 79.00(14) . . ? C7 Cr C5 66.63(14) . . ? C6 Cr C5 37.49(14) . . ? C3' Cr C5 66.39(14) . . ? C9 Cr C4 157.06(15) . . ? C10 Cr C4 91.70(14) . . ? C11 Cr C4 115.35(15) . . ? C7' Cr C4 67.14(13) . . ? C7 Cr C4 78.94(13) . . ? C6 Cr C4 66.85(14) . . ? C3' Cr C4 37.25(14) . . ? C5 Cr C4 36.57(14) . . ? C7' C1 C8 111.8(3) . . ? C7' C1 S2 104.2(2) . . ? C8 C1 S2 113.1(3) . . ? C3 S2 C1 93.69(17) . . ? C7' C3' C4 120.3(3) . . ? C7' C3' C3 114.4(3) . . ? C4 C3' C3 125.3(3) . . ? C7' C3' Cr 70.91(19) . . ? C4 C3' Cr 71.67(19) . . ? C3 C3' Cr 129.6(2) . . ? C3' C3 S2 105.4(2) . . ? C5 C4 C3' 119.5(3) . . ? C5 C4 Cr 71.59(19) . . ? C3' C4 Cr 71.08(17) . . ? C4 C5 C6 120.2(3) . . ? C4 C5 Cr 71.84(19) . . ? C6 C5 Cr 71.0(2) . . ? C7 C6 C5 119.8(3) . . ? C7 C6 Cr 71.3(2) . . ? C5 C6 Cr 71.5(2) . . ? C3' C7' C7 119.5(3) . . ? C3' C7' C1 115.0(3) . . ? C7 C7' C1 125.5(3) . . ? C3' C7' Cr 72.05(18) . . ? C7 C7' Cr 71.34(19) . . ? C1 C7' Cr 130.2(2) . . ? C6 C7 C7' 120.7(3) . . ? C6 C7 Cr 72.2(2) . . ? C7' C7 Cr 71.25(18) . . ? O9 C9 Cr 179.4(3) . . ? O10 C10 Cr 176.5(3) . . ? O11 C11 Cr 177.8(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C7' C1 S2 C3 24.1(3) . . . . ? C8 C1 S2 C3 -97.5(3) . . . . ? C9 Cr C3' C7' -44.1(2) . . . . ? C10 Cr C3' C7' -129.4(2) . . . . ? C11 Cr C3' C7' 144.8(3) . . . . ? C7 Cr C3' C7' 29.98(19) . . . . ? C6 Cr C3' C7' 66.3(2) . . . . ? C5 Cr C3' C7' 103.5(2) . . . . ? C4 Cr C3' C7' 132.7(3) . . . . ? C9 Cr C3' C4 -176.71(19) . . . . ? C10 Cr C3' C4 98.0(2) . . . . ? C11 Cr C3' C4 12.2(4) . . . . ? C7' Cr C3' C4 -132.7(3) . . . . ? C7 Cr C3' C4 -102.7(2) . . . . ? C6 Cr C3' C4 -66.4(2) . . . . ? C5 Cr C3' C4 -29.15(19) . . . . ? C9 Cr C3' C3 62.2(3) . . . . ? C10 Cr C3' C3 -23.1(3) . . . . ? C11 Cr C3' C3 -108.9(4) . . . . ? C7' Cr C3' C3 106.3(4) . . . . ? C7 Cr C3' C3 136.2(3) . . . . ? C6 Cr C3' C3 172.5(3) . . . . ? C5 Cr C3' C3 -150.2(3) . . . . ? C4 Cr C3' C3 -121.1(4) . . . . ? C7' C3' C3 S2 17.2(3) . . . . ? C4 C3' C3 S2 -162.5(3) . . . . ? Cr C3' C3 S2 -67.6(3) . . . . ? C1 S2 C3 C3' -23.9(2) . . . . ? C7' C3' C4 C5 1.1(5) . . . . ? C3 C3' C4 C5 -179.2(3) . . . . ? Cr C3' C4 C5 54.7(3) . . . . ? C7' C3' C4 Cr -53.6(3) . . . . ? C3 C3' C4 Cr 126.1(3) . . . . ? C9 Cr C4 C5 -124.2(4) . . . . ? C10 Cr C4 C5 147.2(2) . . . . ? C11 Cr C4 C5 54.8(2) . . . . ? C7' Cr C4 C5 -102.8(2) . . . . ? C7 Cr C4 C5 -65.5(2) . . . . ? C6 Cr C4 C5 -29.29(19) . . . . ? C3' Cr C4 C5 -131.5(3) . . . . ? C9 Cr C4 C3' 7.3(4) . . . . ? C10 Cr C4 C3' -81.3(2) . . . . ? C11 Cr C4 C3' -173.75(19) . . . . ? C7' Cr C4 C3' 28.73(18) . . . . ? C7 Cr C4 C3' 65.99(18) . . . . ? C6 Cr C4 C3' 102.2(2) . . . . ? C5 Cr C4 C3' 131.5(3) . . . . ? C3' C4 C5 C6 -0.5(5) . . . . ? Cr C4 C5 C6 54.0(3) . . . . ? C3' C4 C5 Cr -54.5(3) . . . . ? C9 Cr C5 C4 139.1(3) . . . . ? C10 Cr C5 C4 -39.5(2) . . . . ? C11 Cr C5 C4 -132.4(2) . . . . ? C7' Cr C5 C4 66.3(2) . . . . ? C7 Cr C5 C4 103.4(2) . . . . ? C6 Cr C5 C4 132.3(3) . . . . ? C3' Cr C5 C4 29.66(19) . . . . ? C9 Cr C5 C6 6.8(4) . . . . ? C10 Cr C5 C6 -171.8(2) . . . . ? C11 Cr C5 C6 95.3(2) . . . . ? C7' Cr C5 C6 -66.0(2) . . . . ? C7 Cr C5 C6 -28.93(19) . . . . ? C3' Cr C5 C6 -102.7(2) . . . . ? C4 Cr C5 C6 -132.3(3) . . . . ? C4 C5 C6 C7 0.2(5) . . . . ? Cr C5 C6 C7 54.5(3) . . . . ? C4 C5 C6 Cr -54.4(3) . . . . ? C9 Cr C6 C7 51.9(2) . . . . ? C10 Cr C6 C7 -112.6(4) . . . . ? C11 Cr C6 C7 141.3(2) . . . . ? C7' Cr C6 C7 -29.16(19) . . . . ? C3' Cr C6 C7 -66.0(2) . . . . ? C5 Cr C6 C7 -131.7(3) . . . . ? C4 Cr C6 C7 -103.1(2) . . . . ? C9 Cr C6 C5 -176.4(2) . . . . ? C10 Cr C6 C5 19.1(5) . . . . ? C11 Cr C6 C5 -87.0(2) . . . . ? C7' Cr C6 C5 102.6(2) . . . . ? C7 Cr C6 C5 131.7(3) . . . . ? C3' Cr C6 C5 65.7(2) . . . . ? C4 Cr C6 C5 28.6(2) . . . . ? C4 C3' C7' C7 -1.3(5) . . . . ? C3 C3' C7' C7 179.0(3) . . . . ? Cr C3' C7' C7 -55.3(3) . . . . ? C4 C3' C7' C1 -179.3(3) . . . . ? C3 C3' C7' C1 1.0(4) . . . . ? Cr C3' C7' C1 126.7(3) . . . . ? C4 C3' C7' Cr 54.0(3) . . . . ? C3 C3' C7' Cr -125.7(3) . . . . ? C8 C1 C7' C3' 104.0(3) . . . . ? S2 C1 C7' C3' -18.5(4) . . . . ? C8 C1 C7' C7 -73.8(4) . . . . ? S2 C1 C7' C7 163.7(3) . . . . ? C8 C1 C7' Cr -168.9(3) . . . . ? S2 C1 C7' Cr 68.6(3) . . . . ? C9 Cr C7' C3' 142.9(2) . . . . ? C10 Cr C7' C3' 54.7(2) . . . . ? C11 Cr C7' C3' -130.4(4) . . . . ? C7 Cr C7' C3' -130.9(3) . . . . ? C6 Cr C7' C3' -102.4(2) . . . . ? C5 Cr C7' C3' -65.2(2) . . . . ? C4 Cr C7' C3' -28.88(19) . . . . ? C9 Cr C7' C7 -86.2(2) . . . . ? C10 Cr C7' C7 -174.4(2) . . . . ? C11 Cr C7' C7 0.6(5) . . . . ? C6 Cr C7' C7 28.50(19) . . . . ? C3' Cr C7' C7 130.9(3) . . . . ? C5 Cr C7' C7 65.7(2) . . . . ? C4 Cr C7' C7 102.0(2) . . . . ? C9 Cr C7' C1 34.9(3) . . . . ? C10 Cr C7' C1 -53.3(3) . . . . ? C11 Cr C7' C1 121.6(4) . . . . ? C7 Cr C7' C1 121.1(4) . . . . ? C6 Cr C7' C1 149.6(3) . . . . ? C3' Cr C7' C1 -108.0(4) . . . . ? C5 Cr C7' C1 -173.2(3) . . . . ? C4 Cr C7' C1 -136.9(3) . . . . ? C5 C6 C7 C7' -0.4(5) . . . . ? Cr C6 C7 C7' 54.3(3) . . . . ? C5 C6 C7 Cr -54.6(3) . . . . ? C3' C7' C7 C6 1.0(5) . . . . ? C1 C7' C7 C6 178.7(3) . . . . ? Cr C7' C7 C6 -54.7(3) . . . . ? C3' C7' C7 Cr 55.7(3) . . . . ? C1 C7' C7 Cr -126.6(3) . . . . ? C9 Cr C7 C6 -133.6(2) . . . . ? C10 Cr C7 C6 142.1(2) . . . . ? C11 Cr C7 C6 -47.2(3) . . . . ? C7' Cr C7 C6 132.5(3) . . . . ? C3' Cr C7 C6 102.8(2) . . . . ? C5 Cr C7 C6 29.65(19) . . . . ? C4 Cr C7 C6 65.8(2) . . . . ? C9 Cr C7 C7' 93.9(2) . . . . ? C10 Cr C7 C7' 9.6(3) . . . . ? C11 Cr C7 C7' -179.8(2) . . . . ? C6 Cr C7 C7' -132.5(3) . . . . ? C3' Cr C7 C7' -29.69(19) . . . . ? C5 Cr C7 C7' -102.9(2) . . . . ? C4 Cr C7 C7' -66.7(2) . . . . ? C10 Cr C9 O9 -11(33) . . . . ? C11 Cr C9 O9 80(33) . . . . ? C7' Cr C9 O9 -120(33) . . . . ? C7 Cr C9 O9 -158(33) . . . . ? C6 Cr C9 O9 174(100) . . . . ? C3' Cr C9 O9 -96(33) . . . . ? C5 Cr C9 O9 170(100) . . . . ? C4 Cr C9 O9 -101(33) . . . . ? C9 Cr C10 O10 -90(5) . . . . ? C11 Cr C10 O10 -177(5) . . . . ? C7' Cr C10 O10 1(5) . . . . ? C7 Cr C10 O10 -5(5) . . . . ? C6 Cr C10 O10 76(5) . . . . ? C3' Cr C10 O10 31(5) . . . . ? C5 Cr C10 O10 90(5) . . . . ? C4 Cr C10 O10 67(5) . . . . ? C9 Cr C11 O11 -14(9) . . . . ? C10 Cr C11 O11 74(9) . . . . ? C7' Cr C11 O11 -101(9) . . . . ? C7 Cr C11 O11 -101(9) . . . . ? C6 Cr C11 O11 -127(9) . . . . ? C3' Cr C11 O11 158(9) . . . . ? C5 Cr C11 O11 -164(9) . . . . ? C4 Cr C11 O11 167(9) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.382 _refine_diff_density_min -0.273 _refine_diff_density_rms 0.069 #===END