#------------------------------------------------------------------------------ #$Date: 2015-04-02 12:22:18 +0100 (Thu, 02 Apr 2015) $ #$Revision: 134621 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/89/2008984.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2008984 loop_ _publ_author_name 'Rickard, Clifton E. F.' 'Singh, Yogendra' 'Woodgate, Paul D.' 'Zhao, Zhongde' _publ_section_title ; Tricarbonylchromium complexes of four methyl 4,6-O-[(\h^6^-phenyl)alkylidene]-\a-D-glucopyranosides ; _journal_issue 9 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1475 _journal_page_last 1479 _journal_paper_doi 10.1107/S0108270199007313 _journal_volume 55 _journal_year 1999 _chemical_formula_iupac '[Cr (C17 H22 O6) (C O)3]' _chemical_formula_sum 'C20 H22 Cr O9' _chemical_formula_weight 458.38 _chemical_name_systematic ; Tricarbonyl{(R)-methyl 2,3-O-(1-methylethylidene)-4,6-O-[(\h^6^- phenyl)methylene]-\a-D-glucopyranoside}chromium(0). ; _space_group_IT_number 4 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _audit_creation_method SHELXL97 _cell_angle_alpha 90.00 _cell_angle_beta 101.65 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 7.75930(10) _cell_length_b 27.9746(3) _cell_length_c 10.20640(10) _cell_measurement_reflns_used 8192 _cell_measurement_temperature 203(2) _cell_measurement_theta_max 26 _cell_measurement_theta_min 2 _cell_volume 2169.80(4) _computing_cell_refinement SMART _computing_data_collection 'SMART (Siemens, 1994a)' _computing_data_reduction 'SAINT (Siemens, 1994a)' _computing_molecular_graphics 'SHELXTL (Siemens, 1994b)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1990)' _diffrn_ambient_temperature 203(2) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Siemens SMART CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.019 _diffrn_reflns_av_sigmaI/netI 0.037 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 13078 _diffrn_reflns_theta_full 25.99 _diffrn_reflns_theta_max 26 _diffrn_reflns_theta_min 1.46 _diffrn_standards_decay_% 0 _exptl_absorpt_coefficient_mu 0.574 _exptl_absorpt_correction_T_max 0.889 _exptl_absorpt_correction_T_min 0.833 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Blessing, 1995)' _exptl_crystal_colour Yellow _exptl_crystal_density_diffrn 1.403 _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'Irregular fragment' _exptl_crystal_F_000 952 _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.21 _refine_diff_density_max 0.367 _refine_diff_density_min -0.259 _refine_ls_abs_structure_details 'Flack (1983)' _refine_ls_abs_structure_Flack 0.016(16) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 546 _refine_ls_number_reflns 7411 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.035 _refine_ls_R_factor_all 0.041 _refine_ls_R_factor_gt 0.035 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0341P)^2^+0.5820P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.084 _reflns_number_gt 6642 _reflns_number_total 7411 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file ta1240.cif _[local]_cod_data_source_block 3 _[local]_cod_cif_authors_sg_H-M 'P 21' _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w = 1/[\s^2^(Fo^2^)+(0.0341P)^2^+0.5820P] where P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w = 1/[\s^2^(Fo^2^)+(0.0341P)^2^+0.5820P] where P=(Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_cell_volume 2169.78(4) _cod_database_code 2008984 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Cr1 0.89411(6) 0.941793(15) 0.93644(5) 0.04280(13) Uani d . 1 . . Cr O1 0.6432(3) 1.14520(8) 1.5011(2) 0.0625(6) Uani d . 1 . . O O2 0.3034(3) 1.10221(9) 1.5125(2) 0.0592(6) Uani d . 1 . . O O3 0.3260(3) 1.02814(8) 1.4087(2) 0.0511(5) Uani d . 1 . . O O4 0.5829(3) 1.01528(7) 1.2124(2) 0.0417(5) Uani d . 1 . . O O5 0.5577(3) 1.14660(7) 1.2626(2) 0.0496(5) Uani d . 1 . . O O6 0.7624(3) 1.05443(7) 1.0847(2) 0.0514(5) Uani d . 1 . . O O7 1.1810(4) 1.01576(12) 0.9957(4) 0.0967(10) Uani d . 1 . . O O8 0.7828(4) 0.98914(12) 0.6660(3) 0.0902(9) Uani d . 1 . . O O9 1.1917(8) 0.8854(2) 0.8537(6) 0.0677(15) Uiso d P 0.50 . . O O9A 1.1236(10) 0.8797(3) 0.7996(8) 0.099(2) Uiso d P 0.50 . . O C1 0.5025(5) 1.14961(11) 1.3916(3) 0.0521(8) Uani d . 1 . . C H1 0.4421 1.1805 1.3974 0.063 Uiso calc R 1 . . H C2 0.3733(4) 1.10897(12) 1.3927(3) 0.0474(7) Uani d . 1 . . C H2 0.2736 1.1131 1.3159 0.057 Uiso calc R 1 . . H C3 0.4584(4) 1.06020(10) 1.3800(3) 0.0402(6) Uani d . 1 . . C H3 0.5679 1.0569 1.4487 0.048 Uiso calc R 1 . . H C4 0.5001(4) 1.05927(10) 1.2411(3) 0.0400(6) Uani d . 1 . . C H4 0.3920 1.0651 1.1727 0.048 Uiso calc R 1 . . H C5 0.6330(4) 1.10047(10) 1.2404(3) 0.0428(7) Uani d . 1 . . C H5 0.7374 1.0947 1.3122 0.051 Uiso calc R 1 . . H C6 0.6913(5) 1.10157(12) 1.1057(4) 0.0531(8) Uani d . 1 . . C H6A 0.5909 1.1089 1.0335 0.064 Uiso calc R 1 . . H H6B 0.7814 1.1262 1.1067 0.064 Uiso calc R 1 . . H C7 0.6332(4) 1.01842(11) 1.0838(3) 0.0419(6) Uani d . 1 . . C H7 0.5283 1.0257 1.0138 0.050 Uiso calc R 1 . . H C8 0.7590(7) 1.18593(18) 1.5186(5) 0.1037(17) Uani d . 1 . . C H8A 0.8302 1.1855 1.4507 0.124 Uiso calc R 1 . . H H8B 0.8350 1.1847 1.6066 0.124 Uiso calc R 1 . . H H8C 0.6898 1.2151 1.5104 0.124 Uiso calc R 1 . . H C9 0.2491(4) 1.05219(13) 1.5117(3) 0.0498(8) Uani d . 1 . . C C10 0.3208(6) 1.03178(16) 1.6503(4) 0.0719(11) Uani d . 1 . . C H10A 0.2826 0.9989 1.6538 0.086 Uiso calc R 1 . . H H10B 0.2772 1.0505 1.7167 0.086 Uiso calc R 1 . . H H10C 0.4484 1.0330 1.6686 0.086 Uiso calc R 1 . . H C11 0.0505(5) 1.04809(17) 1.4676(4) 0.0741(11) Uani d . 1 . . C H11A 0.0161 1.0148 1.4691 0.089 Uiso calc R 1 . . H H11B 0.0146 1.0606 1.3775 0.089 Uiso calc R 1 . . H H11C -0.0059 1.0663 1.5280 0.089 Uiso calc R 1 . . H C12 0.7024(4) 0.96907(11) 1.0592(3) 0.0445(7) Uani d . 1 . . C C13 0.6104(5) 0.94059(15) 0.9544(4) 0.0625(9) Uani d . 1 . . C H13 0.5114 0.9529 0.8954 0.075 Uiso calc R 1 . . H C14 0.6690(7) 0.89227(17) 0.9381(5) 0.0872(16) Uani d . 1 . . C H14 0.6081 0.8727 0.8691 0.105 Uiso calc R 1 . . H C15 0.8182(8) 0.87501(14) 1.0269(6) 0.0929(17) Uani d . 1 . . C H15 0.8580 0.8438 1.0156 0.112 Uiso calc R 1 . . H C16 0.9074(7) 0.90264(14) 1.1301(4) 0.0811(14) Uani d . 1 . . C H16 1.0046 0.8899 1.1899 0.097 Uiso calc R 1 . . H C17 0.8534(5) 0.95036(12) 1.1465(3) 0.0574(9) Uani d . 1 . . C H17 0.9174 0.9696 1.2150 0.069 Uiso calc R 1 . . H C18 1.0689(5) 0.98760(13) 0.9741(4) 0.0581(9) Uani d . 1 . . C C19 0.8250(4) 0.97055(13) 0.7697(4) 0.0551(8) Uani d . 1 . . C C20 1.0541(6) 0.90564(14) 0.8701(5) 0.0775(13) Uani d . 1 . . C Cr2 1.60859(6) 1.354939(16) 0.57794(5) 0.04230(12) Uani d . 1 . . Cr O1' 0.9512(3) 1.14792(7) 0.8828(2) 0.0511(5) Uani d . 1 . . O O2' 1.0329(3) 1.18929(8) 1.1560(2) 0.0542(6) Uani d . 1 . . O O3' 1.1277(3) 1.26486(8) 1.1025(2) 0.0487(6) Uani d . 1 . . O O4' 1.3039(3) 1.27987(7) 0.8564(2) 0.0429(5) Uani d . 1 . . O O5' 1.2600(3) 1.14790(7) 0.8884(2) 0.0520(5) Uani d . 1 . . O O6' 1.4255(3) 1.24179(8) 0.6891(2) 0.0580(6) Uani d . 1 . . O O7' 1.5448(5) 1.30298(15) 0.3130(3) 0.1052(12) Uani d . 1 . . O O8' 1.8858(5) 1.41690(12) 0.4903(4) 0.1126(12) Uani d . 1 . . O O9' 1.9013(4) 1.28491(11) 0.6784(4) 0.0965(10) Uani d . 1 . . O C1' 1.1203(4) 1.14390(11) 0.9629(3) 0.0477(7) Uani d . 1 . . C H1' 1.1306 1.1129 1.0105 0.057 Uiso calc R 1 . . H C2' 1.1513(4) 1.18460(11) 1.0658(3) 0.0431(7) Uani d . 1 . . C H2' 1.2722 1.1813 1.1195 0.052 Uiso calc R 1 . . H C3' 1.1381(4) 1.23278(10) 0.9943(3) 0.0381(6) Uani d . 1 . . C H3' 1.0280 1.2343 0.9257 0.046 Uiso calc R 1 . . H C4' 1.2954(4) 1.23576(10) 0.9284(3) 0.0409(6) Uani d . 1 . . C H4' 1.4054 1.2310 0.9955 0.049 Uiso calc R 1 . . H C5' 1.2694(4) 1.19430(10) 0.8244(3) 0.0438(7) Uani d . 1 . . C H5' 1.1583 1.1997 0.7590 0.053 Uiso calc R 1 . . H C6' 1.4218(5) 1.19457(12) 0.7502(4) 0.0617(9) Uani d . 1 . . C H6'1 1.5331 1.1884 0.8127 0.074 Uiso calc R 1 . . H H6'2 1.4045 1.1697 0.6812 0.074 Uiso calc R 1 . . H C7' 1.4466(4) 1.27864(11) 0.7868(3) 0.0454(7) Uani d . 1 . . C H7' 1.5587 1.2739 0.8517 0.055 Uiso calc R 1 . . H C8' 0.8934(6) 1.10552(13) 0.8056(4) 0.0684(10) Uani d . 1 . . C H8'1 0.7780 1.1111 0.7503 0.082 Uiso calc R 1 . . H H8'2 0.8872 1.0790 0.8657 0.082 Uiso calc R 1 . . H H8'3 0.9763 1.0980 0.7491 0.082 Uiso calc R 1 . . H C9' 1.0144(4) 1.24069(12) 1.1795(3) 0.0505(8) Uani d . 1 . . C C10' 0.8216(5) 1.25339(15) 1.1284(4) 0.0715(11) Uani d . 1 . . C H10D 0.8033 1.2870 1.1452 0.086 Uiso calc R 1 . . H H10E 0.7486 1.2341 1.1744 0.086 Uiso calc R 1 . . H H10F 0.7901 1.2472 1.0330 0.086 Uiso calc R 1 . . H C11' 1.0828(6) 1.25313(16) 1.3264(4) 0.0787(13) Uani d . 1 . . C H11D 1.0638 1.2869 1.3405 0.094 Uiso calc R 1 . . H H11E 1.2077 1.2461 1.3504 0.094 Uiso calc R 1 . . H H11F 1.0205 1.2343 1.3818 0.094 Uiso calc R 1 . . H C12' 1.4477(4) 1.32728(11) 0.7201(3) 0.0419(7) Uani d . 1 . . C C13' 1.5607(4) 1.36428(11) 0.7850(3) 0.0499(8) Uani d . 1 . . C H13' 1.6365 1.3582 0.8675 0.060 Uiso calc R 1 . . H C14' 1.5587(5) 1.40987(12) 0.7254(4) 0.0563(9) Uani d . 1 . . C H14' 1.6332 1.4341 0.7682 0.068 Uiso calc R 1 . . H C15' 1.4445(5) 1.41908(13) 0.6013(4) 0.0604(9) Uani d . 1 . . C H15' 1.4446 1.4494 0.5616 0.072 Uiso calc R 1 . . H C16' 1.3319(5) 1.38361(13) 0.5373(4) 0.0590(9) Uani d . 1 . . C H16' 1.2551 1.3901 0.4556 0.071 Uiso calc R 1 . . H C17' 1.3343(4) 1.33727(11) 0.5970(3) 0.0493(8) Uani d . 1 . . C H17' 1.2593 1.3132 0.5536 0.059 Uiso calc R 1 . . H C18' 1.5704(5) 1.32322(15) 0.4146(4) 0.0629(9) Uani d . 1 . . C C19' 1.7769(5) 1.39370(14) 0.5218(4) 0.0676(10) Uani d . 1 . . C C20' 1.7887(5) 1.31179(12) 0.6397(4) 0.0553(8) Uani d . 1 . . C loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cr1 0.0528(3) 0.0320(2) 0.0498(3) -0.0028(2) 0.0250(2) -0.0050(2) O1 0.0835(17) 0.0418(13) 0.0582(14) -0.0136(12) 0.0050(13) -0.0038(10) O2 0.0787(16) 0.0485(13) 0.0594(14) 0.0055(12) 0.0356(12) -0.0088(11) O3 0.0583(13) 0.0452(13) 0.0586(13) -0.0008(11) 0.0325(10) -0.0072(10) O4 0.0505(12) 0.0313(10) 0.0494(11) 0.0046(9) 0.0245(9) -0.0025(9) O5 0.0679(14) 0.0315(11) 0.0514(12) 0.0115(10) 0.0173(11) 0.0037(9) O6 0.0554(13) 0.0364(11) 0.0715(15) 0.0018(10) 0.0348(11) 0.0002(10) O7 0.0712(18) 0.086(2) 0.125(3) -0.0340(17) 0.0017(17) -0.0057(19) O8 0.095(2) 0.112(3) 0.0601(17) -0.0020(18) 0.0070(15) 0.0116(16) C1 0.071(2) 0.0323(16) 0.0550(19) 0.0089(15) 0.0182(16) -0.0014(13) C2 0.0571(19) 0.0420(17) 0.0451(16) 0.0135(15) 0.0149(14) -0.0030(13) C3 0.0439(15) 0.0337(15) 0.0444(15) 0.0046(12) 0.0124(13) -0.0005(12) C4 0.0427(15) 0.0354(15) 0.0445(16) 0.0084(12) 0.0147(12) 0.0008(12) C5 0.0468(16) 0.0324(15) 0.0509(17) 0.0078(12) 0.0135(13) 0.0037(12) C6 0.060(2) 0.0366(17) 0.070(2) 0.0020(15) 0.0298(17) 0.0040(15) C7 0.0452(16) 0.0417(16) 0.0429(16) 0.0024(13) 0.0182(13) 0.0004(12) C8 0.126(4) 0.084(3) 0.092(3) -0.047(3) 0.001(3) 0.007(3) C9 0.0546(19) 0.056(2) 0.0435(17) 0.0055(16) 0.0222(14) -0.0036(14) C10 0.086(3) 0.076(3) 0.057(2) 0.013(2) 0.022(2) 0.0030(19) C11 0.059(2) 0.094(3) 0.075(3) 0.012(2) 0.0257(19) -0.017(2) C12 0.0549(19) 0.0385(16) 0.0479(17) -0.0023(14) 0.0286(14) -0.0021(13) C13 0.0539(19) 0.067(2) 0.075(2) -0.0226(18) 0.0321(17) -0.020(2) C14 0.097(3) 0.066(3) 0.121(4) -0.048(3) 0.074(3) -0.051(3) C15 0.139(4) 0.033(2) 0.140(4) 0.000(2) 0.107(4) 0.006(2) C16 0.133(4) 0.051(2) 0.075(3) 0.034(2) 0.059(3) 0.018(2) C17 0.077(2) 0.053(2) 0.0486(18) 0.0190(17) 0.0273(16) 0.0035(14) C18 0.0525(19) 0.060(2) 0.061(2) -0.0046(17) 0.0094(16) 0.0020(16) C19 0.056(2) 0.057(2) 0.055(2) -0.0084(16) 0.0167(16) -0.0090(16) C20 0.101(3) 0.046(2) 0.107(3) 0.021(2) 0.073(3) 0.010(2) Cr2 0.0476(3) 0.0364(3) 0.0466(3) -0.0006(2) 0.0184(2) 0.0008(2) O1' 0.0606(13) 0.0389(12) 0.0525(12) -0.0074(10) 0.0083(11) -0.0021(10) O2' 0.0702(15) 0.0452(13) 0.0535(13) -0.0093(11) 0.0272(11) 0.0017(10) O3' 0.0652(14) 0.0378(12) 0.0508(12) -0.0122(10) 0.0300(11) -0.0094(9) O4' 0.0521(12) 0.0329(10) 0.0484(12) -0.0039(9) 0.0209(10) -0.0025(9) O5' 0.0651(14) 0.0333(11) 0.0638(14) 0.0046(10) 0.0277(11) 0.0021(10) O6' 0.0860(16) 0.0412(12) 0.0573(14) -0.0037(12) 0.0392(12) -0.0035(10) O7' 0.105(2) 0.148(3) 0.0644(19) 0.007(2) 0.0212(17) -0.041(2) O8' 0.106(2) 0.085(2) 0.171(3) -0.0264(19) 0.084(2) 0.021(2) O9' 0.0684(18) 0.077(2) 0.131(3) 0.0206(16) -0.0115(18) 0.0024(19) C1' 0.0616(19) 0.0305(15) 0.0531(17) 0.0006(14) 0.0162(15) 0.0047(12) C2' 0.0511(17) 0.0374(16) 0.0411(16) -0.0040(14) 0.0097(13) 0.0052(12) C3' 0.0459(16) 0.0328(15) 0.0373(15) -0.0032(12) 0.0124(12) -0.0028(11) C4' 0.0461(16) 0.0352(15) 0.0429(16) -0.0025(13) 0.0124(13) 0.0000(12) C5' 0.0560(18) 0.0291(14) 0.0497(17) 0.0021(13) 0.0186(14) -0.0022(12) C6' 0.089(3) 0.0379(18) 0.069(2) 0.0019(18) 0.044(2) -0.0055(15) C7' 0.0495(17) 0.0443(17) 0.0450(16) -0.0025(14) 0.0154(13) -0.0025(13) C8' 0.097(3) 0.049(2) 0.059(2) -0.018(2) 0.014(2) -0.0129(17) C9' 0.059(2) 0.0485(19) 0.0496(18) -0.0148(15) 0.0233(15) -0.0045(14) C10' 0.063(2) 0.066(3) 0.091(3) -0.0016(19) 0.028(2) 0.004(2) C11' 0.101(3) 0.090(3) 0.049(2) -0.033(3) 0.026(2) -0.0159(19) C12' 0.0436(16) 0.0447(17) 0.0408(15) -0.0017(13) 0.0168(13) -0.0016(12) C13' 0.0608(18) 0.049(2) 0.0438(16) -0.0032(15) 0.0199(14) -0.0083(13) C14' 0.067(2) 0.0409(19) 0.068(2) -0.0081(16) 0.0315(18) -0.0158(15) C15' 0.076(2) 0.0391(18) 0.074(2) 0.0098(17) 0.0337(19) 0.0042(16) C16' 0.056(2) 0.059(2) 0.062(2) 0.0108(17) 0.0115(17) 0.0097(17) C17' 0.0435(16) 0.0497(19) 0.0573(19) -0.0035(13) 0.0162(14) -0.0038(14) C18' 0.061(2) 0.077(3) 0.053(2) 0.0111(19) 0.0177(17) -0.0055(18) C19' 0.075(3) 0.050(2) 0.085(3) 0.0016(19) 0.034(2) 0.0067(19) C20' 0.054(2) 0.048(2) 0.063(2) -0.0041(16) 0.0119(16) -0.0061(16) 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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C20 Cr1 C18 86.35(19) C20 Cr1 C19 89.55(18) C18 Cr1 C19 87.38(15) C20 Cr1 C15 86.89(16) C18 Cr1 C15 138.0(2) C19 Cr1 C15 133.9(2) C20 Cr1 C14 104.46(19) C18 Cr1 C14 166.12(16) C19 Cr1 C14 101.2(2) C15 Cr1 C14 36.80(19) C20 Cr1 C17 130.44(18) C18 Cr1 C17 88.05(15) C19 Cr1 C17 139.31(14) C15 Cr1 C17 65.85(16) C14 Cr1 C17 78.33(16) C20 Cr1 C16 98.15(17) C18 Cr1 C16 104.70(18) C19 Cr1 C16 165.99(18) C15 Cr1 C16 35.91(19) C14 Cr1 C16 65.6(2) C17 Cr1 C16 36.90(13) C20 Cr1 C13 140.33(18) C18 Cr1 C13 133.10(15) C19 Cr1 C13 88.58(15) C15 Cr1 C13 66.78(18) C14 Cr1 C13 37.68(17) C17 Cr1 C13 66.04(14) C16 Cr1 C13 78.01(17) C20 Cr1 C12 163.85(15) C18 Cr1 C12 100.82(14) C19 Cr1 C12 105.11(13) C15 Cr1 C12 78.09(13) C14 Cr1 C12 66.55(13) C17 Cr1 C12 36.78(12) C16 Cr1 C12 66.13(13) C13 Cr1 C12 36.37(12) C1 O1 C8 113.3(3) C2 O2 C9 106.1(2) C3 O3 C9 105.6(2) C7 O4 C4 110.2(2) C5 O5 C1 113.0(2) C7 O6 C6 110.7(2) O9A O9 C20 71.4(9) O9 O9A C20 75.7(9) O1 C1 O5 112.9(3) O1 C1 C2 109.8(3) O5 C1 C2 106.1(2) O2 C2 C1 117.7(3) O2 C2 C3 101.3(2) C1 C2 C3 111.7(3) O3 C3 C4 118.4(3) O3 C3 C2 101.6(2) C4 C3 C2 105.7(2) O4 C4 C3 113.0(2) O4 C4 C5 108.0(2) C3 C4 C5 105.1(2) O5 C5 C6 108.9(2) O5 C5 C4 111.8(2) C6 C5 C4 109.7(3) O6 C6 C5 107.6(2) O6 C7 O4 110.9(2) O6 C7 C12 111.9(2) O4 C7 C12 105.3(2) O2 C9 O3 106.5(2) O2 C9 C11 110.4(3) O3 C9 C11 106.7(3) O2 C9 C10 107.6(3) O3 C9 C10 111.6(3) C11 C9 C10 113.9(3) C13 C12 C17 119.7(3) C13 C12 C7 119.9(3) C17 C12 C7 120.3(3) C13 C12 Cr1 71.20(18) C17 C12 Cr1 70.85(17) C7 C12 Cr1 133.8(2) C12 C13 C14 119.6(4) C12 C13 Cr1 72.43(18) C14 C13 Cr1 70.6(2) C15 C14 C13 119.0(4) C15 C14 Cr1 71.0(2) C13 C14 Cr1 71.7(2) C16 C15 C14 121.6(4) C16 C15 Cr1 73.1(2) C14 C15 Cr1 72.2(2) C15 C16 C17 120.3(5) C15 C16 Cr1 71.0(2) C17 C16 Cr1 71.5(2) C16 C17 C12 119.9(4) C16 C17 Cr1 71.6(2) C12 C17 Cr1 72.37(17) O7 C18 Cr1 178.3(4) O8 C19 Cr1 179.1(3) O9A C20 O9 32.9(4) O9A C20 Cr1 163.3(6) O9 C20 Cr1 163.8(5) C20' Cr2 C18' 88.12(16) C20' Cr2 C19' 87.52(16) C18' Cr2 C19' 89.83(18) C20' Cr2 C17' 119.46(14) C18' Cr2 C17' 89.44(15) C19' Cr2 C17' 152.96(15) C20' Cr2 C13' 90.71(14) C18' Cr2 C13' 151.34(15) C19' Cr2 C13' 118.74(16) C17' Cr2 C13' 66.39(12) C20' Cr2 C12' 92.01(14) C18' Cr2 C12' 114.10(15) C19' Cr2 C12' 156.05(15) C17' Cr2 C12' 36.78(11) C13' Cr2 C12' 37.31(11) C20' Cr2 C14' 115.99(15) C18' Cr2 C14' 155.88(15) C19' Cr2 C14' 91.96(15) C17' Cr2 C14' 78.22(12) C13' Cr2 C14' 36.80(12) C12' Cr2 C14' 66.79(11) C20' Cr2 C15' 152.72(15) C18' Cr2 C15' 119.12(16) C19' Cr2 C15' 90.87(15) C17' Cr2 C15' 66.15(13) C13' Cr2 C15' 66.35(13) C12' Cr2 C15' 78.71(12) C14' Cr2 C15' 36.82(13) C20' Cr2 C16' 156.68(14) C18' Cr2 C16' 91.81(15) C19' Cr2 C16' 115.80(15) C17' Cr2 C16' 37.23(12) C13' Cr2 C16' 78.33(13) C12' Cr2 C16' 66.79(12) C14' Cr2 C16' 65.86(14) C15' Cr2 C16' 36.17(13) C1' O1' C8' 113.8(3) C2' O2' C9' 106.9(2) C3' O3' C9' 105.0(2) C7' O4' C4' 110.5(2) C1' O5' C5' 114.4(2) C7' O6' C6' 111.4(2) O1' C1' O5' 113.5(2) O1' C1' C2' 109.8(2) O5' C1' C2' 105.7(2) O2' C2' C3' 103.7(2) O2' C2' C1' 118.4(3) C3' C2' C1' 110.0(2) O3' C3' C4' 118.9(2) O3' C3' C2' 101.1(2) C4' C3' C2' 106.2(2) O4' C4' C3' 113.4(2) O4' C4' C5' 107.6(2) C3' C4' C5' 104.9(2) O5' C5' C6' 109.8(2) O5' C5' C4' 111.6(2) C6' C5' C4' 109.1(3) O6' C6' C5' 107.4(3) O6' C7' O4' 112.0(2) O6' C7' C12' 110.2(2) O4' C7' C12' 106.0(2) O3' C9' O2' 106.0(2) O3' C9' C10' 111.4(3) O2' C9' C10' 107.1(3) O3' C9' C11' 107.2(3) O2' C9' C11' 110.9(3) C10' C9' C11' 114.0(3) C17' C12' C13' 118.9(3) C17' C12' C7' 121.1(3) C13' C12' C7' 119.9(3) C17' C12' Cr2 71.48(17) C13' C12' Cr2 71.30(16) C7' C12' Cr2 130.9(2) C14' C13' C12' 120.2(3) C14' C13' Cr2 71.81(18) C12' C13' Cr2 71.39(16) C15' C14' C13' 120.0(3) C15' C14' Cr2 71.64(19) C13' C14' Cr2 71.40(17) C16' C15' C14' 120.6(3) C16' C15' Cr2 72.3(2) C14' C15' Cr2 71.53(19) C15' C16' C17' 119.5(3) C15' C16' Cr2 71.5(2) C17' C16' Cr2 70.7(2) C12' C17' C16' 120.7(3) C12' C17' Cr2 71.74(17) C16' C17' Cr2 72.1(2) O7' C18' Cr2 179.1(4) O8' C19' Cr2 177.6(4) O9' C20' Cr2 179.9(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cr1 C20 . 1.833(4) ? Cr1 C18 . 1.849(4) ? Cr1 C19 . 1.861(4) ? Cr1 C15 . 2.216(4) ? Cr1 C14 . 2.232(4) ? Cr1 C17 . 2.242(3) ? Cr1 C16 . 2.243(4) ? Cr1 C13 . 2.246(3) ? Cr1 C12 . 2.262(3) ? O1 C1 . 1.401(4) ? O1 C8 . 1.440(5) ? O2 C2 . 1.447(4) ? O2 C9 . 1.461(4) ? O3 C3 . 1.437(4) ? O3 C9 . 1.472(4) ? O4 C7 . 1.445(3) ? O4 C4 . 1.445(3) ? O5 C5 . 1.453(3) ? O5 C1 . 1.467(4) ? O6 C7 . 1.420(4) ? O6 C6 . 1.462(4) ? O7 C18 . 1.161(4) ? O8 C19 . 1.165(4) ? O9 O9A . 0.701(8) ? O9 C20 . 1.249(7) ? O9A C20 . 1.222(8) ? C1 C2 . 1.518(5) ? C2 C3 . 1.533(4) ? C3 C4 . 1.518(4) ? C4 C5 . 1.547(4) ? C5 C6 . 1.531(4) ? C7 C12 . 1.521(4) ? C9 C11 . 1.520(5) ? C9 C10 . 1.523(5) ? C12 C13 . 1.407(5) ? C12 C17 . 1.421(5) ? C13 C14 . 1.446(6) ? C14 C15 . 1.404(7) ? C15 C16 . 1.375(7) ? C16 C17 . 1.419(5) ? Cr2 C20' . 1.858(4) ? Cr2 C18' . 1.859(4) ? Cr2 C19' . 1.874(4) ? Cr2 C17' . 2.231(3) ? Cr2 C13' . 2.234(3) ? Cr2 C12' . 2.235(3) ? Cr2 C14' . 2.239(3) ? Cr2 C15' . 2.240(3) ? Cr2 C16' . 2.250(4) ? O1' C1' . 1.403(4) ? O1' C8' . 1.444(4) ? O2' C2' . 1.433(4) ? O2' C9' . 1.470(4) ? O3' C3' . 1.438(3) ? O3' C9' . 1.459(4) ? O4' C7' . 1.432(4) ? O4' C4' . 1.444(3) ? O5' C1' . 1.449(4) ? O5' C5' . 1.462(4) ? O6' C7' . 1.420(4) ? O6' C6' . 1.463(4) ? O7' C18' . 1.162(4) ? O8' C19' . 1.161(5) ? O9' C20' . 1.160(4) ? C1' C2' . 1.534(4) ? C2' C3' . 1.526(4) ? C3' C4' . 1.510(4) ? C4' C5' . 1.557(4) ? C5' C6' . 1.527(4) ? C7' C12' . 1.522(4) ? C9' C10' . 1.523(5) ? C9' C11' . 1.526(5) ? C12' C17' . 1.409(4) ? C12' C13' . 1.429(4) ? C13' C14' . 1.412(5) ? C14' C15' . 1.415(5) ? C15' C16' . 1.394(5) ? C16' C17' . 1.431(5) ?