data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Peter Roesky' _publ_contact_author_address ; Institut fur Anorganische Chemie Engesserstr. 15 Karlsruhe D-76199 ; _publ_contact_author_email roesky@kit.edu loop_ _publ_author_name P.Roesky B.Murugesapandian # Attachment '- deposit.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 778877' #TrackingRef '- deposit.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H17 Cr Na2 O11, C10 H5 Cr O5' _chemical_formula_sum 'C20 H22 Cr2 Na2 O16' _chemical_formula_weight 668.36 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' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.4827(13) _cell_length_b 12.585(3) _cell_length_c 33.012(7) _cell_angle_alpha 90.00 _cell_angle_beta 92.82(3) _cell_angle_gamma 90.00 _cell_volume 2690.1(9) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 9769 _cell_measurement_theta_min 1.73 _cell_measurement_theta_max 29.58 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.650 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 0.915 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8171 _exptl_absorpt_correction_T_max 0.9471 _exptl_absorpt_process_details 'STOE X-RED & X-SHAPE' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 IPDS 2' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24978 _diffrn_reflns_av_R_equivalents 0.0793 _diffrn_reflns_av_sigmaI/netI 0.0686 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 29.16 _reflns_number_total 7236 _reflns_number_gt 4972 _reflns_threshold_expression >2\s(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA, PLATON (A.L.Spek, 2005)' _computing_data_reduction 'STOE X-RED, PLATON (A.L.Spek, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e/3' _computing_publication_material 'X-STEP32, Microsoft Word' _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^ > 2\s(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^)+(0.0327P)^2^+2.8593P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7236 _refine_ls_number_parameters 409 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0978 _refine_ls_R_factor_gt 0.0591 _refine_ls_wR_factor_ref 0.1163 _refine_ls_wR_factor_gt 0.1047 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.3645(5) -0.1150(3) 0.14144(9) 0.0236(6) Uani 1 1 d . . . C2 C 1.3919(5) -0.2038(3) 0.11658(10) 0.0274(7) Uani 1 1 d . . . H2 H 1.4036 -0.2727 0.1282 0.033 Uiso 1 1 calc R . . C3 C 1.4020(5) -0.1903(3) 0.07406(10) 0.0308(7) Uani 1 1 d . . . H3 H 1.4238 -0.2502 0.0573 0.037 Uiso 1 1 calc R . . C4 C 1.3803(5) -0.0895(3) 0.05665(10) 0.0328(8) Uani 1 1 d . . . H4 H 1.3834 -0.0812 0.0281 0.039 Uiso 1 1 calc R . . C5 C 1.3536(5) 0.0000(3) 0.08169(10) 0.0316(7) Uani 1 1 d . . . H5 H 1.3400 0.0686 0.0699 0.038 Uiso 1 1 calc R . . C6 C 1.3470(5) -0.0119(3) 0.12372(10) 0.0270(7) Uani 1 1 d . . . H6 H 1.3309 0.0486 0.1404 0.032 Uiso 1 1 calc R . . C7 C 1.3445(5) -0.1291(3) 0.18662(9) 0.0243(6) Uani 1 1 d . . . C8 C 0.9324(5) -0.0602(3) 0.05494(10) 0.0323(7) Uani 1 1 d . . . C9 C 0.9310(5) -0.0814(3) 0.13427(10) 0.0319(7) Uani 1 1 d . . . C10 C 0.9676(6) -0.2443(3) 0.08734(11) 0.0331(8) Uani 1 1 d . . . C11 C 0.8263(5) 0.3180(3) 0.10247(9) 0.0271(7) Uani 1 1 d . . . C12 C 0.8090(5) 0.4204(3) 0.08611(10) 0.0289(7) Uani 1 1 d . . . H12 H 0.7883 0.4794 0.1034 0.035 Uiso 1 1 calc R . . C13 C 0.8223(5) 0.4364(3) 0.04395(11) 0.0344(8) Uani 1 1 d . . . H13 H 0.8116 0.5061 0.0330 0.041 Uiso 1 1 calc R . . C14 C 0.8510(6) 0.3503(3) 0.01850(11) 0.0370(8) Uani 1 1 d . . . H14 H 0.8610 0.3616 -0.0098 0.044 Uiso 1 1 calc R . . C15 C 0.8655(6) 0.2459(3) 0.03444(10) 0.0345(8) Uani 1 1 d . . . H15 H 0.8851 0.1872 0.0170 0.041 Uiso 1 1 calc R . . C16 C 0.8506(5) 0.2300(3) 0.07626(10) 0.0300(7) Uani 1 1 d . . . H16 H 0.8568 0.1601 0.0871 0.036 Uiso 1 1 calc R . . C17 C 0.8316(5) 0.2978(3) 0.14797(10) 0.0325(8) Uani 1 1 d . . . C18 C 1.2632(5) 0.2929(3) 0.10967(11) 0.0333(8) Uani 1 1 d . . . C19 C 1.2854(6) 0.2972(4) 0.03092(12) 0.0454(10) Uani 1 1 d . . . C20 C 1.2498(6) 0.4708(3) 0.07282(11) 0.0369(8) Uani 1 1 d . . . O1 O 1.3309(4) -0.22162(19) 0.20007(7) 0.0351(6) Uani 1 1 d . . . O2 O 1.3417(4) -0.04590(19) 0.20795(7) 0.0310(5) Uani 1 1 d . . . O3 O 0.8207(4) -0.0249(3) 0.03002(9) 0.0471(7) Uani 1 1 d . . . O4 O 0.8269(4) -0.0622(3) 0.16058(8) 0.0478(7) Uani 1 1 d . . . O5 O 0.8768(5) -0.3222(2) 0.08262(10) 0.0529(8) Uani 1 1 d . . . O6 O 0.8504(4) 0.2043(2) 0.15917(8) 0.0434(7) Uani 1 1 d . . . O7 O 0.8216(4) 0.3785(2) 0.17086(7) 0.0421(7) Uani 1 1 d . . . O8 O 1.3634(4) 0.2594(3) 0.13660(9) 0.0495(7) Uani 1 1 d . . . O9 O 1.3959(5) 0.2628(4) 0.00805(11) 0.0805(13) Uani 1 1 d . . . O10 O 1.3451(5) 0.5482(2) 0.07625(11) 0.0589(9) Uani 1 1 d . . . O11 O 1.2925(5) -0.0915(3) 0.28755(10) 0.0485(8) Uani 1 1 d . . . O12 O 1.3975(4) -0.3646(2) 0.27779(8) 0.0315(5) Uani 1 1 d . . . O13 O 0.9664(6) -0.3525(4) 0.18896(11) 0.0586(9) Uani 1 1 d . . . O14 O 0.7981(4) -0.1615(2) 0.24931(9) 0.0371(6) Uani 1 1 d . . . O15 O 0.8858(4) -0.3787(3) 0.28124(8) 0.0355(6) Uani 1 1 d . . . O16 O 0.5188(5) -0.4633(2) 0.18181(10) 0.0471(7) Uani 1 1 d . . . Na1 Na 1.1238(2) -0.25175(13) 0.25845(5) 0.0439(4) Uani 1 1 d . . . Na2 Na 0.6374(2) -0.32820(11) 0.22423(4) 0.0313(3) Uani 1 1 d . . . Cr1 Cr 1.11012(8) -0.11805(4) 0.094489(15) 0.02353(12) Uani 1 1 d . . . Cr2 Cr 1.09981(8) 0.34674(4) 0.066999(15) 0.02463(12) Uani 1 1 d . . . H11A H 1.328(9) -0.074(4) 0.2646(18) 0.073(18) Uiso 1 1 d . . . H11B H 1.410(9) -0.093(4) 0.3001(17) 0.067(17) Uiso 1 1 d . . . H12A H 1.353(7) -0.428(4) 0.2827(12) 0.037(11) Uiso 1 1 d . . . H12B H 1.450(8) -0.340(4) 0.2959(16) 0.065(18) Uiso 1 1 d . . . H13A H 1.049(11) -0.318(6) 0.181(2) 0.09(3) Uiso 1 1 d . . . H13B H 0.985(13) -0.415(7) 0.182(3) 0.14(4) Uiso 1 1 d . . . H14A H 0.793(9) -0.111(5) 0.2361(17) 0.069(18) Uiso 1 1 d . . . H14B H 0.752(10) -0.150(5) 0.273(2) 0.09(2) Uiso 1 1 d . . . H15A H 0.826(9) -0.363(5) 0.3012(18) 0.09(2) Uiso 1 1 d . . . H15B H 0.949(8) -0.439(4) 0.2863(15) 0.063(16) Uiso 1 1 d . . . H16A H 0.431(8) -0.498(4) 0.1916(15) 0.054(15) Uiso 1 1 d . . . H16B H 0.617(9) -0.518(5) 0.1736(16) 0.073(17) Uiso 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 C1 0.0208(14) 0.0261(16) 0.0238(14) -0.0006(12) -0.0017(11) -0.0012(13) C2 0.0250(15) 0.0295(17) 0.0278(16) -0.0006(13) 0.0013(13) 0.0039(14) C3 0.0262(16) 0.038(2) 0.0280(16) -0.0071(14) 0.0050(13) 0.0018(15) C4 0.0291(17) 0.046(2) 0.0240(16) 0.0032(14) 0.0044(13) -0.0023(16) C5 0.0315(18) 0.0320(19) 0.0309(17) 0.0082(14) -0.0012(14) -0.0088(15) C6 0.0302(17) 0.0222(16) 0.0282(16) 0.0001(12) -0.0013(13) -0.0039(13) C7 0.0236(14) 0.0232(16) 0.0259(14) 0.0014(12) -0.0027(11) 0.0016(13) C8 0.0297(17) 0.037(2) 0.0305(17) 0.0051(14) 0.0012(14) -0.0019(16) C9 0.0281(17) 0.038(2) 0.0298(17) -0.0016(14) -0.0014(13) 0.0011(15) C10 0.0326(17) 0.034(2) 0.0331(18) -0.0008(14) 0.0020(14) 0.0022(16) C11 0.0235(15) 0.0338(18) 0.0239(15) 0.0018(13) 0.0015(12) -0.0005(14) C12 0.0258(16) 0.0297(17) 0.0314(17) 0.0011(13) 0.0028(13) 0.0043(14) C13 0.0319(18) 0.037(2) 0.0335(18) 0.0125(15) -0.0029(14) 0.0011(16) C14 0.0348(18) 0.051(2) 0.0247(16) 0.0071(15) -0.0027(14) -0.0069(18) C15 0.0342(18) 0.041(2) 0.0276(17) -0.0078(15) -0.0021(14) -0.0079(16) C16 0.0292(16) 0.0320(18) 0.0288(16) 0.0008(13) 0.0026(13) -0.0060(15) C17 0.0269(16) 0.046(2) 0.0246(16) 0.0031(14) 0.0033(13) 0.0029(16) C18 0.0284(17) 0.0341(19) 0.0376(19) 0.0016(15) 0.0043(14) 0.0003(15) C19 0.0312(19) 0.069(3) 0.037(2) -0.0124(19) 0.0055(16) -0.0043(19) C20 0.0319(19) 0.038(2) 0.040(2) 0.0072(16) -0.0031(15) -0.0006(17) O1 0.0482(15) 0.0261(13) 0.0310(13) 0.0018(10) 0.0006(11) 0.0039(12) O2 0.0430(14) 0.0257(12) 0.0243(11) -0.0020(9) 0.0010(10) 0.0001(11) O3 0.0397(15) 0.060(2) 0.0411(15) 0.0199(14) -0.0061(12) 0.0011(14) O4 0.0350(14) 0.072(2) 0.0379(15) -0.0122(14) 0.0140(12) 0.0013(14) O5 0.0526(18) 0.0317(16) 0.074(2) -0.0057(14) -0.0003(16) -0.0135(14) O6 0.0426(15) 0.0565(18) 0.0315(14) 0.0186(12) 0.0051(11) 0.0086(14) O7 0.0388(14) 0.0617(19) 0.0257(12) -0.0056(12) 0.0015(10) 0.0098(14) O8 0.0397(15) 0.0582(19) 0.0491(17) 0.0164(14) -0.0127(13) 0.0048(14) O9 0.0424(18) 0.144(4) 0.057(2) -0.046(2) 0.0184(16) 0.001(2) O10 0.0518(19) 0.0372(17) 0.086(2) 0.0076(16) -0.0163(17) -0.0154(15) O11 0.0470(17) 0.066(2) 0.0329(15) 0.0145(14) 0.0097(13) 0.0216(16) O12 0.0315(13) 0.0299(15) 0.0329(13) 0.0015(11) 0.0007(10) -0.0040(11) O13 0.064(2) 0.058(2) 0.056(2) -0.0045(17) 0.0277(17) -0.013(2) O14 0.0398(15) 0.0393(16) 0.0321(14) 0.0043(12) 0.0017(11) 0.0054(13) O15 0.0324(13) 0.0440(16) 0.0305(13) 0.0072(12) 0.0056(11) 0.0087(12) O16 0.0507(18) 0.0372(17) 0.0547(18) -0.0107(14) 0.0174(15) -0.0061(15) Na1 0.0283(7) 0.0425(9) 0.0615(10) 0.0165(8) 0.0098(7) 0.0039(7) Na2 0.0333(7) 0.0296(7) 0.0310(7) 0.0007(5) 0.0018(5) 0.0004(6) Cr1 0.0230(2) 0.0252(3) 0.0226(2) -0.0001(2) 0.00193(18) -0.0007(2) Cr2 0.0245(3) 0.0278(3) 0.0217(2) -0.0003(2) 0.00223(18) -0.0013(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 C2 1.403(4) . ? C1 C6 1.425(5) . ? C1 C7 1.514(4) . ? C1 Cr1 2.207(3) . ? C2 C3 1.419(5) . ? C2 Cr1 2.214(3) . ? C3 C4 1.396(5) . ? C3 Cr1 2.234(3) . ? C4 C5 1.413(5) . ? C4 Cr1 2.230(3) . ? C5 C6 1.398(5) . ? C5 Cr1 2.223(3) . ? C6 Cr1 2.220(3) . ? C7 O1 1.251(4) . ? C7 O2 1.262(4) . ? C8 O3 1.158(4) . ? C8 Cr1 1.847(4) . ? C9 O4 1.151(4) . ? C9 Cr1 1.854(4) . ? C10 O5 1.151(4) . ? C10 Cr1 1.847(4) . ? C11 C12 1.400(5) . ? C11 C16 1.419(5) . ? C11 C17 1.522(5) . ? C11 Cr2 2.202(3) . ? C12 C13 1.413(5) . ? C12 Cr2 2.220(3) . ? C13 C14 1.389(6) . ? C13 Cr2 2.226(4) . ? C14 C15 1.417(5) . ? C14 Cr2 2.217(4) . ? C15 C16 1.403(5) . ? C15 Cr2 2.216(4) . ? C16 Cr2 2.216(3) . ? C17 O6 1.237(5) . ? C17 O7 1.270(5) . ? C18 O8 1.155(4) . ? C18 Cr2 1.849(4) . ? C19 O9 1.150(5) . ? C19 Cr2 1.843(4) . ? C20 O10 1.156(5) . ? C20 Cr2 1.844(4) . ? O1 Na1 2.432(3) . ? O1 Na2 2.496(3) 1_655 ? O11 Na1 2.466(4) . ? O12 Na1 2.337(3) . ? O12 Na2 2.455(3) 1_655 ? O13 Na2 2.499(4) . ? O13 Na1 2.772(5) . ? O14 Na1 2.404(3) . ? O14 Na2 2.467(3) . ? O15 Na1 2.369(3) . ? O15 Na2 2.498(3) . ? O16 Na2 2.310(3) . ? Na1 Na2 3.434(2) . ? Na1 Na2 3.696(2) 1_655 ? Na2 O12 2.455(3) 1_455 ? Na2 O1 2.496(3) 1_455 ? Na2 Na1 3.696(2) 1_455 ? 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 C1 C6 119.6(3) . . ? C2 C1 C7 120.2(3) . . ? C6 C1 C7 120.2(3) . . ? C2 C1 Cr1 71.75(18) . . ? C6 C1 Cr1 71.71(18) . . ? C7 C1 Cr1 126.3(2) . . ? C1 C2 C3 119.8(3) . . ? C1 C2 Cr1 71.23(18) . . ? C3 C2 Cr1 72.16(19) . . ? C4 C3 C2 120.5(3) . . ? C4 C3 Cr1 71.6(2) . . ? C2 C3 Cr1 70.64(18) . . ? C3 C4 C5 119.7(3) . . ? C3 C4 Cr1 71.92(19) . . ? C5 C4 Cr1 71.24(19) . . ? C6 C5 C4 120.4(3) . . ? C6 C5 Cr1 71.53(19) . . ? C4 C5 Cr1 71.8(2) . . ? C5 C6 C1 120.0(3) . . ? C5 C6 Cr1 71.78(19) . . ? C1 C6 Cr1 70.74(18) . . ? O1 C7 O2 124.8(3) . . ? O1 C7 C1 118.0(3) . . ? O2 C7 C1 117.2(3) . . ? O3 C8 Cr1 179.4(4) . . ? O4 C9 Cr1 175.9(3) . . ? O5 C10 Cr1 179.1(4) . . ? C12 C11 C16 119.5(3) . . ? C12 C11 C17 122.2(3) . . ? C16 C11 C17 118.2(3) . . ? C12 C11 Cr2 72.25(19) . . ? C16 C11 Cr2 71.79(19) . . ? C17 C11 Cr2 124.9(2) . . ? C11 C12 C13 120.2(3) . . ? C11 C12 Cr2 70.86(19) . . ? C13 C12 Cr2 71.7(2) . . ? C14 C13 C12 120.1(3) . . ? C14 C13 Cr2 71.4(2) . . ? C12 C13 Cr2 71.26(19) . . ? C13 C14 C15 120.4(3) . . ? C13 C14 Cr2 72.1(2) . . ? C15 C14 Cr2 71.3(2) . . ? C16 C15 C14 119.4(3) . . ? C16 C15 Cr2 71.5(2) . . ? C14 C15 Cr2 71.4(2) . . ? C15 C16 C11 120.2(3) . . ? C15 C16 Cr2 71.6(2) . . ? C11 C16 Cr2 70.73(19) . . ? O6 C17 O7 126.2(3) . . ? O6 C17 C11 116.8(3) . . ? O7 C17 C11 117.0(3) . . ? O8 C18 Cr2 179.2(3) . . ? O9 C19 Cr2 177.2(4) . . ? O10 C20 Cr2 179.4(4) . . ? C7 O1 Na1 118.5(2) . . ? C7 O1 Na2 123.0(2) . 1_655 ? Na1 O1 Na2 97.17(10) . 1_655 ? Na1 O12 Na2 100.90(11) . 1_655 ? Na2 O13 Na1 81.15(11) . . ? Na1 O14 Na2 89.64(11) . . ? Na1 O15 Na2 89.70(10) . . ? O12 Na1 O15 90.04(11) . . ? O12 Na1 O14 166.40(12) . . ? O15 Na1 O14 77.11(11) . . ? O12 Na1 O1 82.54(10) . . ? O15 Na1 O1 138.60(13) . . ? O14 Na1 O1 110.03(12) . . ? O12 Na1 O11 94.29(12) . . ? O15 Na1 O11 135.31(12) . . ? O14 Na1 O11 91.85(12) . . ? O1 Na1 O11 85.98(10) . . ? O12 Na1 O13 101.03(13) . . ? O15 Na1 O13 74.64(12) . . ? O14 Na1 O13 80.04(12) . . ? O1 Na1 O13 67.08(11) . . ? O11 Na1 O13 146.59(13) . . ? O12 Na1 Na2 126.29(10) . . ? O15 Na1 Na2 46.67(7) . . ? O14 Na1 Na2 45.93(8) . . ? O1 Na1 Na2 108.46(9) . . ? O11 Na1 Na2 137.69(9) . . ? O13 Na1 Na2 45.96(8) . . ? O12 Na1 Na2 40.72(7) . 1_655 ? O15 Na1 Na2 122.14(10) . 1_655 ? O14 Na1 Na2 152.10(10) . 1_655 ? O1 Na1 Na2 42.07(7) . 1_655 ? O11 Na1 Na2 86.74(8) . 1_655 ? O13 Na1 Na2 85.89(9) . 1_655 ? Na2 Na1 Na2 130.77(7) . 1_655 ? O16 Na2 O12 95.46(12) . 1_455 ? O16 Na2 O14 162.11(13) . . ? O12 Na2 O14 100.91(11) 1_455 . ? O16 Na2 O1 88.04(12) . 1_455 ? O12 Na2 O1 78.92(10) 1_455 1_455 ? O14 Na2 O1 88.08(10) . 1_455 ? O16 Na2 O15 116.89(13) . . ? O12 Na2 O15 79.50(10) 1_455 . ? O14 Na2 O15 73.62(11) . . ? O1 Na2 O15 148.34(11) 1_455 . ? O16 Na2 O13 83.89(14) . . ? O12 Na2 O13 153.95(13) 1_455 . ? O14 Na2 O13 84.54(13) . . ? O1 Na2 O13 126.98(13) 1_455 . ? O15 Na2 O13 77.67(12) . . ? O16 Na2 Na1 132.72(11) . . ? O12 Na2 Na1 114.81(9) 1_455 . ? O14 Na2 Na1 44.43(8) . . ? O1 Na2 Na1 131.18(8) 1_455 . ? O15 Na2 Na1 43.63(7) . . ? O13 Na2 Na1 52.89(10) . . ? O16 Na2 Na1 95.67(10) . 1_455 ? O12 Na2 Na1 38.39(7) 1_455 1_455 ? O14 Na2 Na1 92.74(8) . 1_455 ? O1 Na2 Na1 40.76(7) 1_455 1_455 ? O15 Na2 Na1 113.14(8) . 1_455 ? O13 Na2 Na1 167.66(11) . 1_455 ? Na1 Na2 Na1 130.77(7) . 1_455 ? C10 Cr1 C8 87.58(16) . . ? C10 Cr1 C9 88.71(16) . . ? C8 Cr1 C9 90.69(16) . . ? C10 Cr1 C1 117.17(14) . . ? C8 Cr1 C1 155.18(15) . . ? C9 Cr1 C1 88.31(13) . . ? C10 Cr1 C2 91.29(15) . . ? C8 Cr1 C2 154.21(14) . . ? C9 Cr1 C2 115.05(14) . . ? C1 Cr1 C2 37.01(12) . . ? C10 Cr1 C6 154.70(14) . . ? C8 Cr1 C6 117.66(15) . . ? C9 Cr1 C6 89.22(14) . . ? C1 Cr1 C6 37.55(12) . . ? C2 Cr1 C6 66.93(13) . . ? C10 Cr1 C5 154.94(15) . . ? C8 Cr1 C5 91.51(14) . . ? C9 Cr1 C5 116.34(15) . . ? C1 Cr1 C5 66.97(12) . . ? C2 Cr1 C5 78.83(13) . . ? C6 Cr1 C5 36.69(12) . . ? C10 Cr1 C4 117.95(15) . . ? C8 Cr1 C4 91.17(14) . . ? C9 Cr1 C4 153.33(16) . . ? C1 Cr1 C4 79.07(12) . . ? C2 Cr1 C4 66.72(13) . . ? C6 Cr1 C4 66.49(13) . . ? C5 Cr1 C4 37.01(13) . . ? C10 Cr1 C3 92.14(15) . . ? C8 Cr1 C3 117.07(14) . . ? C9 Cr1 C3 152.24(14) . . ? C1 Cr1 C3 66.70(12) . . ? C2 Cr1 C3 37.20(12) . . ? C6 Cr1 C3 78.34(13) . . ? C5 Cr1 C3 66.09(14) . . ? C4 Cr1 C3 36.46(13) . . ? C19 Cr2 C20 89.78(19) . . ? C19 Cr2 C18 90.03(18) . . ? C20 Cr2 C18 87.21(16) . . ? C19 Cr2 C11 148.93(17) . . ? C20 Cr2 C11 121.17(16) . . ? C18 Cr2 C11 88.91(14) . . ? C19 Cr2 C16 111.62(17) . . ? C20 Cr2 C16 158.61(16) . . ? C18 Cr2 C16 92.65(15) . . ? C11 Cr2 C16 37.48(12) . . ? C19 Cr2 C15 86.94(16) . . ? C20 Cr2 C15 151.70(15) . . ? C18 Cr2 C15 120.86(16) . . ? C11 Cr2 C15 67.26(13) . . ? C16 Cr2 C15 36.90(13) . . ? C19 Cr2 C14 90.87(16) . . ? C20 Cr2 C14 114.79(15) . . ? C18 Cr2 C14 157.98(16) . . ? C11 Cr2 C14 79.11(13) . . ? C16 Cr2 C14 66.65(13) . . ? C15 Cr2 C14 37.29(14) . . ? C19 Cr2 C12 156.29(16) . . ? C20 Cr2 C12 93.87(16) . . ? C18 Cr2 C12 113.53(14) . . ? C11 Cr2 C12 36.90(12) . . ? C16 Cr2 C12 66.60(14) . . ? C15 Cr2 C12 78.80(14) . . ? C14 Cr2 C12 66.35(14) . . ? C19 Cr2 C13 119.55(17) . . ? C20 Cr2 C13 91.13(16) . . ? C18 Cr2 C13 150.39(15) . . ? C11 Cr2 C13 66.83(13) . . ? C16 Cr2 C13 78.51(14) . . ? C15 Cr2 C13 66.50(15) . . ? C14 Cr2 C13 36.44(14) . . ? C12 Cr2 C13 37.07(12) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 29.16 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.350 _refine_diff_density_min -0.684 _refine_diff_density_rms 0.082 #============================================================================== data_4 _database_code_depnum_ccdc_archive 'CCDC 778878' #TrackingRef '- deposit.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21.50 H18 Cr2 K2 O12.50' _chemical_formula_sum 'C21.50 H18 Cr2 K2 O12.50' _chemical_formula_weight 658.56 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' K K 0.2009 0.2494 '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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 18.956(4) _cell_length_b 7.1076(14) _cell_length_c 20.170(4) _cell_angle_alpha 90.00 _cell_angle_beta 113.79(3) _cell_angle_gamma 90.00 _cell_volume 2486.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 4367 _cell_measurement_theta_min 1.91 _cell_measurement_theta_max 29.11 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.162 _exptl_crystal_size_mid 0.109 _exptl_crystal_size_min 0.038 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.759 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1332 _exptl_absorpt_coefficient_mu 1.275 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8213 _exptl_absorpt_correction_T_max 0.9493 _exptl_absorpt_process_details 'STOE X-RED & X-SHAPE' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 IPDS 2' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10444 _diffrn_reflns_av_R_equivalents 0.0947 _diffrn_reflns_av_sigmaI/netI 0.1345 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 25.02 _reflns_number_total 4384 _reflns_number_gt 2431 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA, PLATON (A.L.Spek, 2005)' _computing_data_reduction 'STOE X-RED, PLATON (A.L.Spek, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e/3' _computing_publication_material 'X-STEP32, Microsoft Word' _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^)+(0.0614P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4384 _refine_ls_number_parameters 346 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1419 _refine_ls_R_factor_gt 0.0736 _refine_ls_wR_factor_ref 0.1596 _refine_ls_wR_factor_gt 0.1389 _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_restrained_S_all 0.993 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.2421(5) 0.1458(11) 0.0213(4) 0.0287(19) Uani 1 1 d . . . C2 C -0.3110(4) 0.2487(10) 0.0061(4) 0.0255(19) Uani 1 1 d . . . H2 H -0.3307 0.3271 -0.0356 0.031 Uiso 1 1 calc R . . C3 C -0.3493(5) 0.2364(11) 0.0506(4) 0.0280(19) Uani 1 1 d . . . H3 H -0.3946 0.3090 0.0398 0.034 Uiso 1 1 calc R . . C4 C -0.3230(5) 0.1178(11) 0.1128(5) 0.034(2) Uani 1 1 d . . . H4 H -0.3502 0.1106 0.1433 0.040 Uiso 1 1 calc R . . C5 C -0.2560(5) 0.0120(12) 0.1279(5) 0.034(2) Uani 1 1 d . . . H5 H -0.2381 -0.0706 0.1683 0.040 Uiso 1 1 calc R . . C6 C -0.2146(5) 0.0272(11) 0.0831(5) 0.033(2) Uani 1 1 d . . . H6 H -0.1684 -0.0422 0.0946 0.040 Uiso 1 1 calc R . . C7 C -0.1971(5) 0.1734(15) -0.0256(5) 0.041(2) Uani 1 1 d . . . C8 C -0.1841(5) 0.4983(12) 0.0873(5) 0.031(2) Uani 1 1 d . . . C9 C -0.2618(5) 0.4920(12) 0.1669(5) 0.032(2) Uani 1 1 d . . . C10 C -0.1397(5) 0.2960(10) 0.2002(4) 0.0250(11) Uani 1 1 d . . . C11 C -0.1420(4) 0.3517(10) -0.3701(4) 0.0220(17) Uani 1 1 d . . . C12 C -0.4211(4) 0.9721(10) -0.1471(5) 0.0230(17) Uani 1 1 d . . . H12 H -0.4355 1.0520 -0.1883 0.028 Uiso 1 1 calc R . . C13 C -0.4639(5) 0.9758(10) -0.1034(4) 0.0243(18) Uani 1 1 d . . . H13 H -0.5073 1.0565 -0.1157 0.029 Uiso 1 1 calc R . . C14 C -0.4419(5) 0.8600(9) -0.0420(4) 0.0250(18) Uani 1 1 d . . . H14 H -0.4706 0.8613 -0.0127 0.030 Uiso 1 1 calc R . . C15 C -0.3766(5) 0.7408(10) -0.0238(4) 0.0240(18) Uani 1 1 d . . . H15 H -0.3606 0.6654 0.0187 0.029 Uiso 1 1 calc R . . C16 C -0.3362(5) 0.7342(10) -0.0678(4) 0.0254(18) Uani 1 1 d . . . H16 H -0.2937 0.6508 -0.0564 0.030 Uiso 1 1 calc R . . C17 C -0.1860(4) 0.3424(11) -0.3218(4) 0.0254(17) Uani 1 1 d . . . C18 C -0.4333(5) 0.4969(11) -0.1872(5) 0.0274(19) Uani 1 1 d . . . C19 C -0.5080(4) 0.5014(11) -0.1043(4) 0.0231(18) Uani 1 1 d . . . C20 C -0.5497(5) 0.7149(9) -0.2192(5) 0.0250(11) Uani 1 1 d . . . O1 O -0.1410(4) 0.0600(9) -0.0143(4) 0.0498(17) Uani 1 1 d . A . O2 O -0.2168(4) 0.3044(12) -0.0697(3) 0.0535(18) Uani 1 1 d . . . O3 O -0.1549(4) -0.3854(8) 0.0652(4) 0.0430(16) Uani 1 1 d . . . O4 O -0.0831(3) 0.2869(8) 0.2518(3) 0.0428(16) Uani 1 1 d . . . O5 O -0.2823(4) 0.6000(9) 0.1973(4) 0.0436(16) Uani 1 1 d . . . O6 O -0.1704(3) 0.4665(8) -0.2730(3) 0.0340(14) Uani 1 1 d . . . O7 O -0.2349(3) 0.2141(7) -0.3341(3) 0.0321(13) Uani 1 1 d . . . O8 O -0.6051(3) 0.7309(8) -0.2696(3) 0.0447(17) Uani 1 1 d . . . O9 O -0.5388(3) 0.3902(8) -0.0836(3) 0.0327(14) Uani 1 1 d . . . O10 O -0.4174(3) 0.3846(8) -0.2198(3) 0.0360(15) Uani 1 1 d . . . O11 O -0.3616(4) 0.5383(13) -0.3445(4) 0.070(2) Uani 1 1 d . . . O12 O -0.0529(9) -0.421(3) -0.1514(8) 0.087(6) Uani 0.50 1 d PD A 1 C21 C -0.0211(15) -0.583(4) -0.1542(13) 0.087(6) Uani 0.50 1 d PD A 1 H21A H 0.0338 -0.5794 -0.1221 0.130 Uiso 0.50 1 calc PR A 1 H21B H -0.0270 -0.6069 -0.2040 0.130 Uiso 0.50 1 calc PR A 1 H21C H -0.0464 -0.6833 -0.1386 0.130 Uiso 0.50 1 calc PR A 1 O13 O 0.0284(10) -0.337(2) 0.0217(10) 0.109(7) Uani 0.50 1 d PD . 2 C22 C 0.0203(12) -0.232(3) 0.0846(12) 0.109(7) Uani 0.50 1 d PD B 2 H22A H -0.0078 -0.1137 0.0667 0.163 Uiso 0.50 1 calc PR B 2 H22B H 0.0716 -0.2039 0.1219 0.163 Uiso 0.50 1 calc PR B 2 H22C H -0.0081 -0.3101 0.1054 0.163 Uiso 0.50 1 calc PR B 2 O14 O 0.0018(8) -0.161(3) -0.0894(9) 0.085(5) Uani 0.50 1 d PD A 3 C23 C 0.0178(12) 0.013(4) -0.1234(14) 0.085(5) Uani 0.50 1 d PD A 3 H23A H -0.0238 0.0322 -0.1713 0.127 Uiso 0.50 1 calc PR A 3 H23B H 0.0668 -0.0017 -0.1284 0.127 Uiso 0.50 1 calc PR A 3 H23C H 0.0209 0.1221 -0.0926 0.127 Uiso 0.50 1 calc PR A 3 K1 K -0.26996(11) 0.3325(3) -0.21566(10) 0.0317(4) Uani 1 1 d . . . K2 K -0.12259(13) -0.3186(4) -0.05589(14) 0.0585(7) Uani 1 1 d D . . Cr1 Cr -0.22975(7) 0.31407(18) 0.11771(6) 0.0234(3) Uani 1 1 d . . . Cr2 Cr -0.45939(7) 0.68171(18) -0.13687(6) 0.0197(3) 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 C1 0.036(5) 0.023(4) 0.025(4) -0.005(3) 0.009(4) 0.003(3) C2 0.033(4) 0.016(4) 0.022(4) -0.009(3) 0.005(4) 0.000(3) C3 0.030(4) 0.020(4) 0.029(4) -0.002(3) 0.007(4) -0.001(3) C4 0.037(5) 0.021(4) 0.046(6) -0.007(4) 0.019(4) -0.011(3) C5 0.048(5) 0.022(4) 0.028(5) 0.003(3) 0.012(4) -0.004(4) C6 0.038(5) 0.024(4) 0.029(5) -0.004(4) 0.005(4) 0.006(4) C7 0.047(5) 0.050(5) 0.029(5) -0.016(5) 0.019(4) -0.004(5) C8 0.045(5) 0.021(4) 0.029(5) -0.002(4) 0.017(4) 0.005(4) C9 0.045(5) 0.030(5) 0.025(5) 0.001(4) 0.017(4) -0.004(4) C10 0.040(3) 0.007(2) 0.033(3) -0.001(2) 0.020(3) -0.002(2) C11 0.034(4) 0.017(4) 0.021(4) 0.000(3) 0.016(3) 0.002(3) C12 0.031(4) 0.009(3) 0.039(5) -0.001(3) 0.024(4) -0.002(3) C13 0.039(5) 0.007(3) 0.036(5) -0.003(3) 0.025(4) 0.004(3) C14 0.048(5) 0.010(4) 0.030(4) -0.006(3) 0.031(4) -0.005(3) C15 0.037(4) 0.016(4) 0.021(4) -0.002(3) 0.014(4) 0.001(3) C16 0.031(4) 0.021(4) 0.031(4) 0.001(3) 0.019(4) -0.005(3) C17 0.033(4) 0.021(4) 0.028(4) -0.008(3) 0.018(3) -0.002(3) C18 0.027(4) 0.026(4) 0.035(5) 0.006(4) 0.018(4) -0.001(3) C19 0.029(4) 0.021(4) 0.021(4) -0.009(3) 0.012(4) 0.001(3) C20 0.040(3) 0.007(2) 0.033(3) -0.001(2) 0.020(3) -0.002(2) O1 0.061(4) 0.039(4) 0.060(5) -0.004(3) 0.035(4) 0.013(3) O2 0.062(4) 0.074(5) 0.033(4) 0.007(4) 0.028(3) 0.012(4) O3 0.065(4) 0.029(3) 0.043(4) 0.003(3) 0.029(3) -0.004(3) O4 0.037(3) 0.036(4) 0.040(4) 0.005(3) -0.001(3) -0.001(3) O5 0.059(4) 0.035(3) 0.049(4) -0.014(3) 0.035(4) 0.000(3) O6 0.050(4) 0.027(3) 0.036(3) -0.009(3) 0.028(3) -0.001(3) O7 0.047(3) 0.022(3) 0.041(3) -0.014(2) 0.033(3) -0.010(3) O8 0.044(4) 0.035(4) 0.036(4) 0.009(3) -0.003(3) 0.002(3) O9 0.045(3) 0.021(3) 0.042(4) 0.004(3) 0.028(3) -0.007(3) O10 0.052(4) 0.022(3) 0.045(4) -0.013(3) 0.031(3) -0.001(3) O11 0.067(5) 0.099(6) 0.053(5) 0.021(4) 0.032(4) 0.008(5) O12 0.061(10) 0.17(2) 0.030(6) -0.016(11) 0.018(7) -0.021(10) C21 0.061(10) 0.17(2) 0.030(6) -0.016(11) 0.018(7) -0.021(10) O13 0.081(9) 0.046(8) 0.124(14) -0.022(8) -0.036(10) 0.013(7) C22 0.081(9) 0.046(8) 0.124(14) -0.022(8) -0.036(10) 0.013(7) O14 0.032(6) 0.148(16) 0.083(10) -0.022(11) 0.032(6) -0.013(9) C23 0.032(6) 0.148(16) 0.083(10) -0.022(11) 0.032(6) -0.013(9) K1 0.0472(10) 0.0251(9) 0.0336(10) 0.0026(8) 0.0276(8) 0.0034(9) K2 0.0532(13) 0.0623(14) 0.0737(16) 0.0295(14) 0.0397(12) 0.0216(13) Cr1 0.0322(7) 0.0145(6) 0.0229(7) -0.0015(6) 0.0105(5) 0.0027(6) Cr2 0.0290(6) 0.0123(6) 0.0220(6) 0.0013(5) 0.0145(5) 0.0005(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 C1 C2 1.418(11) . ? C1 C6 1.419(11) . ? C1 C7 1.520(12) . ? C1 Cr1 2.214(8) . ? C2 C3 1.367(12) . ? C2 Cr1 2.205(8) . ? C3 C4 1.424(12) . ? C3 Cr1 2.190(8) . ? C4 C5 1.400(12) . ? C4 Cr1 2.223(8) . ? C5 C6 1.418(13) . ? C5 Cr1 2.232(8) . ? C6 Cr1 2.211(8) . ? C7 O2 1.236(12) . ? C7 O1 1.279(11) . ? C8 O3 1.178(10) 1_565 ? C8 Cr1 1.808(9) . ? C9 O5 1.145(10) . ? C9 Cr1 1.854(9) . ? C10 O4 1.156(9) . ? C10 Cr1 1.846(8) . ? C11 C12 1.396(10) 2_444 ? C11 C16 1.421(11) 2_444 ? C11 C17 1.519(10) . ? C11 Cr2 2.225(7) 2_444 ? C12 C11 1.396(10) 2_454 ? C12 C13 1.418(11) . ? C12 Cr2 2.225(7) . ? C13 C14 1.404(11) . ? C13 Cr2 2.209(7) . ? C14 C15 1.420(11) . ? C14 Cr2 2.206(7) . ? C15 C16 1.389(11) . ? C15 Cr2 2.226(8) . ? C16 C11 1.421(10) 2_454 ? C16 Cr2 2.216(8) . ? C17 O7 1.251(9) . ? C17 O6 1.265(9) . ? C17 K1 3.141(8) . ? C18 O10 1.150(10) . ? C18 Cr2 1.845(9) . ? C19 O9 1.157(9) . ? C19 Cr2 1.846(9) . ? C20 O8 1.134(9) . ? C20 Cr2 1.858(8) . ? O1 K2 2.881(7) . ? O2 K1 2.708(6) . ? O2 K2 3.170(9) 1_565 ? O3 C8 1.178(10) 1_545 ? O3 K2 2.788(7) . ? O6 K1 2.751(6) . ? O6 K1 2.809(6) 2_454 ? O7 K2 2.728(6) 2_454 ? O7 K1 2.853(6) . ? O7 K1 2.881(6) 2_444 ? O10 K1 2.787(6) . ? O11 K1 2.876(8) . ? O11 K1 3.102(9) 2_454 ? O11 K2 3.174(9) 2_454 ? O12 C21 1.311(18) . ? O12 K2 2.835(18) . ? O13 C22 1.531(18) . ? O13 K2 2.654(16) . ? O13 K2 2.946(16) 3_545 ? O14 C23 1.504(18) . ? O14 K2 2.925(16) . ? K1 O6 2.809(6) 2_444 ? K1 O7 2.881(6) 2_454 ? K1 O11 3.102(9) 2_444 ? K1 K1 3.9959(17) 2_444 ? K1 K1 3.9959(17) 2_454 ? K1 K2 4.132(4) 1_565 ? K2 O7 2.728(6) 2_444 ? K2 O13 2.946(16) 3_545 ? K2 O2 3.170(9) 1_545 ? K2 O11 3.174(9) 2_444 ? K2 K1 4.132(4) 1_545 ? K2 K1 4.355(3) 2_444 ? K2 K2 4.988(4) 3_545 ? Cr2 C11 2.225(7) 2_454 ? 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 C1 C6 118.4(8) . . ? C2 C1 C7 119.9(8) . . ? C6 C1 C7 121.6(8) . . ? C2 C1 Cr1 70.9(4) . . ? C6 C1 Cr1 71.2(5) . . ? C7 C1 Cr1 126.1(6) . . ? C3 C2 C1 120.8(8) . . ? C3 C2 Cr1 71.3(5) . . ? C1 C2 Cr1 71.7(4) . . ? C2 C3 C4 121.8(8) . . ? C2 C3 Cr1 72.5(5) . . ? C4 C3 Cr1 72.4(5) . . ? C5 C4 C3 118.3(9) . . ? C5 C4 Cr1 72.0(5) . . ? C3 C4 Cr1 69.9(5) . . ? C4 C5 C6 120.5(8) . . ? C4 C5 Cr1 71.3(5) . . ? C6 C5 Cr1 70.6(5) . . ? C5 C6 C1 120.2(8) . . ? C5 C6 Cr1 72.2(5) . . ? C1 C6 Cr1 71.4(5) . . ? O2 C7 O1 126.2(9) . . ? O2 C7 C1 117.5(8) . . ? O1 C7 C1 116.3(9) . . ? O3 C8 Cr1 177.6(7) 1_565 . ? O5 C9 Cr1 179.0(8) . . ? O4 C10 Cr1 179.2(7) . . ? C12 C11 C16 119.7(7) 2_444 2_444 ? C12 C11 C17 120.3(7) 2_444 . ? C16 C11 C17 120.0(7) 2_444 . ? C12 C11 Cr2 71.7(4) 2_444 2_444 ? C16 C11 Cr2 71.0(4) 2_444 2_444 ? C17 C11 Cr2 128.3(5) . 2_444 ? C11 C12 C13 120.3(7) 2_454 . ? C11 C12 Cr2 71.7(4) 2_454 . ? C13 C12 Cr2 70.7(4) . . ? C14 C13 C12 119.8(7) . . ? C14 C13 Cr2 71.4(4) . . ? C12 C13 Cr2 72.0(4) . . ? C13 C14 C15 119.7(7) . . ? C13 C14 Cr2 71.6(4) . . ? C15 C14 Cr2 72.1(4) . . ? C16 C15 C14 120.2(7) . . ? C16 C15 Cr2 71.4(5) . . ? C14 C15 Cr2 70.6(4) . . ? C15 C16 C11 120.3(7) . 2_454 ? C15 C16 Cr2 72.2(5) . . ? C11 C16 Cr2 71.7(4) 2_454 . ? O7 C17 O6 125.9(7) . . ? O7 C17 C11 117.3(6) . . ? O6 C17 C11 116.9(7) . . ? O7 C17 K1 65.3(4) . . ? O6 C17 K1 60.6(4) . . ? C11 C17 K1 177.1(5) . . ? O10 C18 Cr2 178.4(7) . . ? O9 C19 Cr2 179.1(7) . . ? O8 C20 Cr2 178.4(6) . . ? C7 O1 K2 136.6(6) . . ? C7 O2 K1 135.2(6) . . ? C7 O2 K2 125.3(6) . 1_565 ? K1 O2 K2 89.0(2) . 1_565 ? C8 O3 K2 138.9(6) 1_545 . ? C17 O6 K1 95.8(5) . . ? C17 O6 K1 128.5(5) . 2_454 ? K1 O6 K1 91.89(17) . 2_454 ? C17 O7 K2 129.4(5) . 2_454 ? C17 O7 K1 91.3(4) . . ? K2 O7 K1 102.54(19) 2_454 . ? C17 O7 K1 134.4(5) . 2_444 ? K2 O7 K1 94.87(17) 2_454 2_444 ? K1 O7 K1 88.35(16) . 2_444 ? C18 O10 K1 124.5(6) . . ? K1 O11 K1 83.8(2) . 2_454 ? K1 O11 K2 91.9(2) . 2_454 ? K1 O11 K2 129.9(3) 2_454 2_454 ? C21 O12 K2 127.0(17) . . ? C22 O13 K2 91.2(10) . . ? C22 O13 K2 117.7(12) . 3_545 ? K2 O13 K2 125.9(6) . 3_545 ? C23 O14 K2 138.6(12) . . ? O2 K1 O6 117.7(2) . . ? O2 K1 O10 88.3(2) . . ? O6 K1 O10 142.30(19) . . ? O2 K1 O6 88.9(2) . 2_444 ? O6 K1 O6 127.47(17) . 2_444 ? O10 K1 O6 75.80(17) . 2_444 ? O2 K1 O7 141.1(2) . . ? O6 K1 O7 47.07(16) . . ? O10 K1 O7 125.71(18) . . ? O6 K1 O7 83.15(17) 2_444 . ? O2 K1 O11 147.6(2) . . ? O6 K1 O11 73.2(2) . . ? O10 K1 O11 70.9(2) . . ? O6 K1 O11 108.7(2) 2_444 . ? O7 K1 O11 69.7(2) . . ? O2 K1 O7 75.2(2) . 2_454 ? O6 K1 O7 83.67(16) . 2_454 ? O10 K1 O7 77.05(16) . 2_454 ? O6 K1 O7 148.82(17) 2_444 2_454 ? O7 K1 O7 125.74(16) . 2_454 ? O11 K1 O7 76.0(2) . 2_454 ? O2 K1 O11 68.7(2) . 2_444 ? O6 K1 O11 79.5(2) . 2_444 ? O10 K1 O11 137.7(2) . 2_444 ? O6 K1 O11 69.0(2) 2_444 2_444 ? O7 K1 O11 72.94(19) . 2_444 ? O11 K1 O11 142.53(13) . 2_444 ? O7 K1 O11 126.21(19) 2_454 2_444 ? O2 K1 C17 132.4(2) . . ? O6 K1 C17 23.62(17) . . ? O10 K1 C17 138.9(2) . . ? O6 K1 C17 105.26(19) 2_444 . ? O7 K1 C17 23.46(17) . . ? O11 K1 C17 70.1(2) . . ? O7 K1 C17 105.23(18) 2_454 . ? O11 K1 C17 74.5(2) 2_444 . ? O2 K1 K1 105.79(18) . 2_444 ? O6 K1 K1 84.51(13) . 2_444 ? O10 K1 K1 115.82(13) . 2_444 ? O6 K1 K1 43.48(12) 2_444 2_444 ? O7 K1 K1 46.11(12) . 2_444 ? O11 K1 K1 105.6(2) . 2_444 ? O7 K1 K1 167.00(14) 2_454 2_444 ? O11 K1 K1 45.69(15) 2_444 2_444 ? C17 K1 K1 64.21(15) . 2_444 ? O2 K1 K1 113.78(19) . 2_454 ? O6 K1 K1 44.63(12) . 2_454 ? O10 K1 K1 101.50(13) . 2_454 ? O6 K1 K1 157.17(15) 2_444 2_454 ? O7 K1 K1 80.28(13) . 2_454 ? O11 K1 K1 50.52(18) . 2_454 ? O7 K1 K1 45.55(11) 2_454 2_454 ? O11 K1 K1 120.02(18) 2_444 2_454 ? C17 K1 K1 61.64(15) . 2_454 ? K1 K1 K1 125.59(9) 2_444 2_454 ? O2 K1 K2 50.08(18) . 1_565 ? O6 K1 K2 75.95(13) . 1_565 ? O10 K1 K2 107.34(13) . 1_565 ? O6 K1 K2 137.97(13) 2_444 1_565 ? O7 K1 K2 121.15(13) . 1_565 ? O11 K1 K2 111.81(19) . 1_565 ? O7 K1 K2 41.13(12) 2_454 1_565 ? O11 K1 K2 85.15(15) 2_444 1_565 ? C17 K1 K2 98.57(15) . 1_565 ? K1 K1 K2 129.88(8) 2_444 1_565 ? K1 K1 K2 64.76(5) 2_454 1_565 ? O13 K2 O7 164.3(5) . 2_444 ? O13 K2 O3 92.3(5) . . ? O7 K2 O3 103.36(19) 2_444 . ? O13 K2 O12 72.6(6) . . ? O7 K2 O12 92.8(3) 2_444 . ? O3 K2 O12 151.5(5) . . ? O13 K2 O1 95.8(4) . . ? O7 K2 O1 87.73(19) 2_444 . ? O3 K2 O1 79.0(2) . . ? O12 K2 O1 125.6(5) . . ? O13 K2 O14 51.5(6) . . ? O7 K2 O14 113.9(4) 2_444 . ? O3 K2 O14 138.6(4) . . ? O12 K2 O14 45.7(5) . . ? O1 K2 O14 85.0(4) . . ? O13 K2 O13 54.1(6) . 3_545 ? O7 K2 O13 124.7(3) 2_444 3_545 ? O3 K2 O13 88.9(5) . 3_545 ? O12 K2 O13 62.7(6) . 3_545 ? O1 K2 O13 147.4(3) . 3_545 ? O14 K2 O13 84.5(6) . 3_545 ? O13 K2 O2 116.5(4) . 1_545 ? O7 K2 O2 70.27(17) 2_444 1_545 ? O3 K2 O2 67.52(18) . 1_545 ? O12 K2 O2 97.1(4) . 1_545 ? O1 K2 O2 133.2(2) . 1_545 ? O14 K2 O2 141.4(4) . 1_545 ? O13 K2 O2 65.4(4) 3_545 1_545 ? O13 K2 O11 102.5(5) . 2_444 ? O7 K2 O11 66.90(18) 2_444 2_444 ? O3 K2 O11 133.8(2) . 2_444 ? O12 K2 O11 74.1(5) . 2_444 ? O1 K2 O11 56.4(2) . 2_444 ? O14 K2 O11 55.0(4) . 2_444 ? O13 K2 O11 134.9(5) 3_545 2_444 ? O2 K2 O11 135.6(2) 1_545 2_444 ? O13 K2 K1 131.3(4) . 1_545 ? O7 K2 K1 44.00(12) 2_444 1_545 ? O3 K2 K1 105.22(15) . 1_545 ? O12 K2 K1 70.7(3) . 1_545 ? O1 K2 K1 131.62(16) . 1_545 ? O14 K2 K1 113.8(4) . 1_545 ? O13 K2 K1 80.7(3) 3_545 1_545 ? O2 K2 K1 40.93(12) 1_545 1_545 ? O11 K2 K1 97.16(15) 2_444 1_545 ? O13 K2 K1 124.7(5) . 2_444 ? O7 K2 K1 39.77(12) 2_444 2_444 ? O3 K2 K1 142.61(15) . 2_444 ? O12 K2 K1 59.4(4) . 2_444 ? O1 K2 K1 91.02(16) . 2_444 ? O14 K2 K1 74.8(3) . 2_444 ? O13 K2 K1 115.7(4) 3_545 2_444 ? O2 K2 K1 96.27(14) 1_545 2_444 ? O11 K2 K1 41.30(14) 2_444 2_444 ? K1 K2 K1 56.10(4) 1_545 2_444 ? O13 K2 K2 28.6(4) . 3_545 ? O7 K2 K2 148.04(17) 2_444 3_545 ? O3 K2 K2 90.59(15) . 3_545 ? O12 K2 K2 64.5(4) . 3_545 ? O1 K2 K2 123.47(17) . 3_545 ? O14 K2 K2 67.1(4) . 3_545 ? O13 K2 K2 25.5(3) 3_545 3_545 ? O2 K2 K2 89.54(14) 1_545 3_545 ? O11 K2 K2 122.14(16) 2_444 3_545 ? K1 K2 K2 104.82(9) 1_545 3_545 ? K1 K2 K2 123.96(9) 2_444 3_545 ? C8 Cr1 C10 87.8(4) . . ? C8 Cr1 C9 89.6(4) . . ? C10 Cr1 C9 87.1(4) . . ? C8 Cr1 C3 119.4(3) . . ? C10 Cr1 C3 152.8(3) . . ? C9 Cr1 C3 91.3(3) . . ? C8 Cr1 C2 92.2(4) . . ? C10 Cr1 C2 156.5(3) . . ? C9 Cr1 C2 116.5(3) . . ? C3 Cr1 C2 36.2(3) . . ? C8 Cr1 C6 114.8(4) . . ? C10 Cr1 C6 91.7(3) . . ? C9 Cr1 C6 155.5(4) . . ? C3 Cr1 C6 78.8(3) . . ? C2 Cr1 C6 67.0(3) . . ? C8 Cr1 C1 89.3(4) . . ? C10 Cr1 C1 119.1(3) . . ? C9 Cr1 C1 153.8(3) . . ? C3 Cr1 C1 66.7(3) . . ? C2 Cr1 C1 37.4(3) . . ? C6 Cr1 C1 37.4(3) . . ? C8 Cr1 C4 157.0(4) . . ? C10 Cr1 C4 115.2(3) . . ? C9 Cr1 C4 91.5(4) . . ? C3 Cr1 C4 37.7(3) . . ? C2 Cr1 C4 66.9(3) . . ? C6 Cr1 C4 67.0(3) . . ? C1 Cr1 C4 79.7(3) . . ? C8 Cr1 C5 152.0(4) . . ? C10 Cr1 C5 90.5(3) . . ? C9 Cr1 C5 118.3(4) . . ? C3 Cr1 C5 66.5(3) . . ? C2 Cr1 C5 78.5(3) . . ? C6 Cr1 C5 37.2(3) . . ? C1 Cr1 C5 67.2(3) . . ? C4 Cr1 C5 36.6(3) . . ? C18 Cr2 C19 89.1(3) . . ? C18 Cr2 C20 87.3(3) . . ? C19 Cr2 C20 89.7(3) . . ? C18 Cr2 C14 155.0(3) . . ? C19 Cr2 C14 90.7(3) . . ? C20 Cr2 C14 117.7(3) . . ? C18 Cr2 C13 153.4(3) . . ? C19 Cr2 C13 117.5(3) . . ? C20 Cr2 C13 91.0(3) . . ? C14 Cr2 C13 37.1(3) . . ? C18 Cr2 C16 91.0(3) . . ? C19 Cr2 C16 116.3(3) . . ? C20 Cr2 C16 153.9(3) . . ? C14 Cr2 C16 66.8(3) . . ? C13 Cr2 C16 79.0(3) . . ? C18 Cr2 C12 116.1(3) . . ? C19 Cr2 C12 154.8(3) . . ? C20 Cr2 C12 90.9(3) . . ? C14 Cr2 C12 66.9(3) . . ? C13 Cr2 C12 37.3(3) . . ? C16 Cr2 C12 66.5(3) . . ? C18 Cr2 C11 90.3(3) . 2_454 ? C19 Cr2 C11 153.6(3) . 2_454 ? C20 Cr2 C11 116.6(3) . 2_454 ? C14 Cr2 C11 79.0(3) . 2_454 ? C13 Cr2 C11 66.8(3) . 2_454 ? C16 Cr2 C11 37.3(3) . 2_454 ? C12 Cr2 C11 36.6(3) . 2_454 ? C18 Cr2 C15 117.6(3) . . ? C19 Cr2 C15 90.7(3) . . ? C20 Cr2 C15 155.0(3) . . ? C14 Cr2 C15 37.4(3) . . ? C13 Cr2 C15 66.8(3) . . ? C16 Cr2 C15 36.5(3) . . ? C12 Cr2 C15 78.4(3) . . ? C11 Cr2 C15 66.4(3) 2_454 . ? 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(11) . . . . ? C7 C1 C2 C3 -175.1(7) . . . . ? Cr1 C1 C2 C3 -53.8(6) . . . . ? C6 C1 C2 Cr1 54.9(6) . . . . ? C7 C1 C2 Cr1 -121.4(7) . . . . ? C1 C2 C3 C4 -1.4(11) . . . . ? Cr1 C2 C3 C4 -55.4(7) . . . . ? C1 C2 C3 Cr1 53.9(6) . . . . ? C2 C3 C4 C5 0.1(11) . . . . ? Cr1 C3 C4 C5 -55.3(7) . . . . ? C2 C3 C4 Cr1 55.4(7) . . . . ? C3 C4 C5 C6 1.6(12) . . . . ? Cr1 C4 C5 C6 -52.7(7) . . . . ? C3 C4 C5 Cr1 54.3(6) . . . . ? C4 C5 C6 C1 -1.9(12) . . . . ? Cr1 C5 C6 C1 -54.9(7) . . . . ? C4 C5 C6 Cr1 53.0(7) . . . . ? C2 C1 C6 C5 0.6(11) . . . . ? C7 C1 C6 C5 176.7(7) . . . . ? Cr1 C1 C6 C5 55.3(7) . . . . ? C2 C1 C6 Cr1 -54.7(6) . . . . ? C7 C1 C6 Cr1 121.4(7) . . . . ? C2 C1 C7 O2 9.6(12) . . . . ? C6 C1 C7 O2 -166.5(8) . . . . ? Cr1 C1 C7 O2 -77.7(9) . . . . ? C2 C1 C7 O1 -171.8(7) . . . . ? C6 C1 C7 O1 12.1(11) . . . . ? Cr1 C1 C7 O1 100.9(9) . . . . ? C11 C12 C13 C14 1.0(11) 2_454 . . . ? Cr2 C12 C13 C14 55.0(6) . . . . ? C11 C12 C13 Cr2 -54.0(6) 2_454 . . . ? C12 C13 C14 C15 0.4(11) . . . . ? Cr2 C13 C14 C15 55.7(6) . . . . ? C12 C13 C14 Cr2 -55.2(6) . . . . ? C13 C14 C15 C16 -2.1(11) . . . . ? Cr2 C14 C15 C16 53.3(6) . . . . ? C13 C14 C15 Cr2 -55.4(6) . . . . ? C14 C15 C16 C11 2.4(11) . . . 2_454 ? Cr2 C15 C16 C11 55.3(6) . . . 2_454 ? C14 C15 C16 Cr2 -52.9(6) . . . . ? C12 C11 C17 O7 -170.3(7) 2_444 . . . ? C16 C11 C17 O7 8.2(10) 2_444 . . . ? Cr2 C11 C17 O7 -80.4(8) 2_444 . . . ? C12 C11 C17 O6 10.3(10) 2_444 . . . ? C16 C11 C17 O6 -171.2(7) 2_444 . . . ? Cr2 C11 C17 O6 100.2(8) 2_444 . . . ? C12 C11 C17 K1 -19(11) 2_444 . . . ? C16 C11 C17 K1 160(10) 2_444 . . . ? Cr2 C11 C17 K1 71(10) 2_444 . . . ? O2 C7 O1 K2 -100.6(12) . . . . ? C1 C7 O1 K2 80.9(10) . . . . ? O1 C7 O2 K1 62.6(13) . . . . ? C1 C7 O2 K1 -118.9(8) . . . . ? O1 C7 O2 K2 -70.3(11) . . . 1_565 ? C1 C7 O2 K2 108.2(7) . . . 1_565 ? O7 C17 O6 K1 2.2(9) . . . . ? C11 C17 O6 K1 -178.4(6) . . . . ? O7 C17 O6 K1 -94.8(9) . . . 2_454 ? C11 C17 O6 K1 84.5(8) . . . 2_454 ? K1 C17 O6 K1 -97.0(5) . . . 2_454 ? O6 C17 O7 K2 105.3(8) . . . 2_454 ? C11 C17 O7 K2 -74.1(8) . . . 2_454 ? K1 C17 O7 K2 107.4(5) . . . 2_454 ? O6 C17 O7 K1 -2.1(8) . . . . ? C11 C17 O7 K1 178.5(6) . . . . ? O6 C17 O7 K1 -91.1(9) . . . 2_444 ? C11 C17 O7 K1 89.6(8) . . . 2_444 ? K1 C17 O7 K1 -88.9(5) . . . 2_444 ? Cr2 C18 O10 K1 87(27) . . . . ? C7 O2 K1 O6 -106.1(9) . . . . ? K2 O2 K1 O6 37.1(2) 1_565 . . . ? C7 O2 K1 O10 102.4(9) . . . . ? K2 O2 K1 O10 -114.39(17) 1_565 . . . ? C7 O2 K1 O6 26.5(9) . . . 2_444 ? K2 O2 K1 O6 169.79(18) 1_565 . . 2_444 ? C7 O2 K1 O7 -51.2(10) . . . . ? K2 O2 K1 O7 92.1(3) 1_565 . . . ? C7 O2 K1 O11 151.2(8) . . . . ? K2 O2 K1 O11 -65.5(4) 1_565 . . . ? C7 O2 K1 O7 179.4(9) . . . 2_454 ? K2 O2 K1 O7 -37.35(16) 1_565 . . 2_454 ? C7 O2 K1 O11 -41.3(8) . . . 2_444 ? K2 O2 K1 O11 102.0(2) 1_565 . . 2_444 ? C7 O2 K1 C17 -83.3(9) . . . . ? K2 O2 K1 C17 60.0(3) 1_565 . . . ? C7 O2 K1 K1 -14.0(9) . . . 2_444 ? K2 O2 K1 K1 129.21(13) 1_565 . . 2_444 ? C7 O2 K1 K1 -155.8(8) . . . 2_454 ? K2 O2 K1 K1 -12.6(2) 1_565 . . 2_454 ? C7 O2 K1 K2 -143.3(9) . . . 1_565 ? C17 O6 K1 O2 134.4(5) . . . . ? K1 O6 K1 O2 -96.7(2) 2_454 . . . ? C17 O6 K1 O10 -96.8(5) . . . . ? K1 O6 K1 O10 32.1(3) 2_454 . . . ? C17 O6 K1 O6 22.3(5) . . . 2_444 ? K1 O6 K1 O6 151.2(2) 2_454 . . 2_444 ? C17 O6 K1 O7 -1.1(4) . . . . ? K1 O6 K1 O7 127.9(3) 2_454 . . . ? C17 O6 K1 O11 -78.7(5) . . . . ? K1 O6 K1 O11 50.2(2) 2_454 . . . ? C17 O6 K1 O7 -156.0(5) . . . 2_454 ? K1 O6 K1 O7 -27.05(16) 2_454 . . 2_454 ? C17 O6 K1 O11 75.3(5) . . . 2_444 ? K1 O6 K1 O11 -155.7(2) 2_454 . . 2_444 ? K1 O6 K1 C17 129.0(5) 2_454 . . . ? C17 O6 K1 K1 29.4(4) . . . 2_444 ? K1 O6 K1 K1 158.38(16) 2_454 . . 2_444 ? C17 O6 K1 K1 -129.0(5) . . . 2_454 ? C17 O6 K1 K2 162.9(5) . . . 1_565 ? K1 O6 K1 K2 -68.15(12) 2_454 . . 1_565 ? C18 O10 K1 O2 53.8(7) . . . . ? C18 O10 K1 O6 -82.6(8) . . . . ? C18 O10 K1 O6 143.1(7) . . . 2_444 ? C18 O10 K1 O7 -146.4(7) . . . . ? C18 O10 K1 O11 -100.9(7) . . . . ? C18 O10 K1 O7 -21.4(7) . . . 2_454 ? C18 O10 K1 O11 109.0(7) . . . 2_444 ? C18 O10 K1 C17 -119.8(7) . . . . ? C18 O10 K1 K1 160.6(6) . . . 2_444 ? C18 O10 K1 K1 -60.1(7) . . . 2_454 ? C18 O10 K1 K2 6.8(7) . . . 1_565 ? C17 O7 K1 O2 -80.8(6) . . . . ? K2 O7 K1 O2 148.3(3) 2_454 . . . ? K1 O7 K1 O2 53.7(4) 2_444 . . . ? C17 O7 K1 O6 1.1(4) . . . . ? K2 O7 K1 O6 -129.9(3) 2_454 . . . ? K1 O7 K1 O6 135.5(3) 2_444 . . . ? C17 O7 K1 O10 132.6(4) . . . . ? K2 O7 K1 O10 1.6(3) 2_454 . . . ? K1 O7 K1 O10 -93.0(2) 2_444 . . . ? C17 O7 K1 O6 -160.4(5) . . . 2_444 ? K2 O7 K1 O6 68.60(19) 2_454 . . 2_444 ? K1 O7 K1 O6 -26.02(15) 2_444 . . 2_444 ? C17 O7 K1 O11 86.7(5) . . . . ? K2 O7 K1 O11 -44.3(2) 2_454 . . . ? K1 O7 K1 O11 -138.9(2) 2_444 . . . ? C17 O7 K1 O7 32.3(4) . . . 2_454 ? K2 O7 K1 O7 -98.61(17) 2_454 . . 2_454 ? K1 O7 K1 O7 166.8(2) 2_444 . . 2_454 ? C17 O7 K1 O11 -90.4(5) . . . 2_444 ? K2 O7 K1 O11 138.7(2) 2_454 . . 2_444 ? K1 O7 K1 O11 44.04(19) 2_444 . . 2_444 ? K2 O7 K1 C17 -131.0(5) 2_454 . . . ? K1 O7 K1 C17 134.4(5) 2_444 . . . ? C17 O7 K1 K1 -134.4(5) . . . 2_444 ? K2 O7 K1 K1 94.63(19) 2_454 . . 2_444 ? C17 O7 K1 K1 35.3(4) . . . 2_454 ? K2 O7 K1 K1 -95.63(17) 2_454 . . 2_454 ? K1 O7 K1 K1 169.74(15) 2_444 . . 2_454 ? C17 O7 K1 K2 -17.2(5) . . . 1_565 ? K2 O7 K1 K2 -148.12(14) 2_454 . . 1_565 ? K1 O7 K1 K2 117.26(13) 2_444 . . 1_565 ? K1 O11 K1 O2 71.1(4) 2_454 . . . ? K2 O11 K1 O2 -158.9(3) 2_454 . . . ? K1 O11 K1 O6 -44.40(16) 2_454 . . . ? K2 O11 K1 O6 85.6(2) 2_454 . . . ? K1 O11 K1 O10 124.0(2) 2_454 . . . ? K2 O11 K1 O10 -106.0(2) 2_454 . . . ? K1 O11 K1 O6 -169.06(17) 2_454 . . 2_444 ? K2 O11 K1 O6 -39.1(2) 2_454 . . 2_444 ? K1 O11 K1 O7 -94.10(19) 2_454 . . . ? K2 O11 K1 O7 35.87(16) 2_454 . . . ? K1 O11 K1 O7 43.10(16) 2_454 . . 2_454 ? K2 O11 K1 O7 173.1(2) 2_454 . . 2_454 ? K1 O11 K1 O11 -89.5(5) 2_454 . . 2_444 ? K2 O11 K1 O11 40.5(4) 2_454 . . 2_444 ? K1 O11 K1 C17 -69.1(2) 2_454 . . . ? K2 O11 K1 C17 60.9(2) 2_454 . . . ? K1 O11 K1 K1 -123.56(15) 2_454 . . 2_444 ? K2 O11 K1 K1 6.4(2) 2_454 . . 2_444 ? K2 O11 K1 K1 130.0(3) 2_454 . . 2_454 ? K1 O11 K1 K2 22.4(2) 2_454 . . 1_565 ? K2 O11 K1 K2 152.37(11) 2_454 . . 1_565 ? O7 C17 K1 O2 123.0(5) . . . . ? O6 C17 K1 O2 -59.0(6) . . . . ? C11 C17 K1 O2 -29(10) . . . . ? O7 C17 K1 O6 -178.0(8) . . . . ? C11 C17 K1 O6 30(10) . . . . ? O7 C17 K1 O10 -65.6(6) . . . . ? O6 C17 K1 O10 112.4(5) . . . . ? C11 C17 K1 O10 142(10) . . . . ? O7 C17 K1 O6 20.1(5) . . . 2_444 ? O6 C17 K1 O6 -161.8(4) . . . 2_444 ? C11 C17 K1 O6 -132(10) . . . 2_444 ? O6 C17 K1 O7 178.0(8) . . . . ? C11 C17 K1 O7 -152(10) . . . . ? O7 C17 K1 O11 -84.6(5) . . . . ? O6 C17 K1 O11 93.4(5) . . . . ? C11 C17 K1 O11 123(10) . . . . ? O7 C17 K1 O7 -153.3(4) . . . 2_454 ? O6 C17 K1 O7 24.7(5) . . . 2_454 ? C11 C17 K1 O7 54(10) . . . 2_454 ? O7 C17 K1 O11 82.7(5) . . . 2_444 ? O6 C17 K1 O11 -99.3(5) . . . 2_444 ? C11 C17 K1 O11 -70(10) . . . 2_444 ? O7 C17 K1 K1 34.9(4) . . . 2_444 ? O6 C17 K1 K1 -147.1(5) . . . 2_444 ? C11 C17 K1 K1 -118(10) . . . 2_444 ? O7 C17 K1 K1 -139.6(5) . . . 2_454 ? O6 C17 K1 K1 38.4(4) . . . 2_454 ? C11 C17 K1 K1 68(10) . . . 2_454 ? O7 C17 K1 K2 165.2(4) . . . 1_565 ? O6 C17 K1 K2 -16.8(5) . . . 1_565 ? C11 C17 K1 K2 13(10) . . . 1_565 ? C22 O13 K2 O7 142.5(14) . . . 2_444 ? K2 O13 K2 O7 -91.4(18) 3_545 . . 2_444 ? C22 O13 K2 O3 -39.2(14) . . . . ? K2 O13 K2 O3 86.9(9) 3_545 . . . ? C22 O13 K2 O12 165.4(15) . . . . ? K2 O13 K2 O12 -68.4(10) 3_545 . . . ? C22 O13 K2 O1 39.9(14) . . . . ? K2 O13 K2 O1 166.1(9) 3_545 . . . ? C22 O13 K2 O14 118.8(15) . . . . ? K2 O13 K2 O14 -115.0(12) 3_545 . . . ? C22 O13 K2 O13 -126.1(18) . . . 3_545 ? K2 O13 K2 O13 0.0 3_545 . . 3_545 ? C22 O13 K2 O2 -105.2(13) . . . 1_545 ? K2 O13 K2 O2 21.0(12) 3_545 . . 1_545 ? C22 O13 K2 O11 96.7(13) . . . 2_444 ? K2 O13 K2 O11 -137.1(9) 3_545 . . 2_444 ? C22 O13 K2 K1 -151.9(12) . . . 1_545 ? K2 O13 K2 K1 -25.8(14) 3_545 . . 1_545 ? C22 O13 K2 K1 135.2(12) . . . 2_444 ? K2 O13 K2 K1 -98.6(9) 3_545 . . 2_444 ? C22 O13 K2 K2 -126.1(18) . . . 3_545 ? C8 O3 K2 O13 -114.3(10) 1_545 . . . ? C8 O3 K2 O7 65.2(9) 1_545 . . 2_444 ? C8 O3 K2 O12 -57.8(13) 1_545 . . . ? C8 O3 K2 O1 150.2(9) 1_545 . . . ? C8 O3 K2 O14 -140.6(10) 1_545 . . . ? C8 O3 K2 O13 -60.3(10) 1_545 . . 3_545 ? C8 O3 K2 O2 3.5(9) 1_545 . . 1_545 ? C8 O3 K2 O11 135.9(9) 1_545 . . 2_444 ? C8 O3 K2 K1 19.8(9) 1_545 . . 1_545 ? C8 O3 K2 K1 73.2(10) 1_545 . . 2_444 ? C8 O3 K2 K2 -85.8(9) 1_545 . . 3_545 ? C21 O12 K2 O13 71.5(19) . . . . ? C21 O12 K2 O7 -114.5(19) . . . 2_444 ? C21 O12 K2 O3 11(2) . . . . ? C21 O12 K2 O1 156.2(18) . . . . ? C21 O12 K2 O14 124(2) . . . . ? C21 O12 K2 O13 13.5(18) . . . 3_545 ? C21 O12 K2 O2 -44.1(19) . . . 1_545 ? C21 O12 K2 O11 -180(2) . . . 2_444 ? C21 O12 K2 K1 -75.8(19) . . . 1_545 ? C21 O12 K2 K1 -137(2) . . . 2_444 ? C21 O12 K2 K2 42.0(18) . . . 3_545 ? C7 O1 K2 O13 -176.2(10) . . . . ? C7 O1 K2 O7 19.1(9) . . . 2_444 ? C7 O1 K2 O3 -85.0(9) . . . . ? C7 O1 K2 O12 111.0(10) . . . . ? C7 O1 K2 O14 133.4(10) . . . . ? C7 O1 K2 O13 -155.0(12) . . . 3_545 ? C7 O1 K2 O2 -40.9(10) . . . 1_545 ? C7 O1 K2 O11 82.7(9) . . . 2_444 ? C7 O1 K2 K1 15.6(10) . . . 1_545 ? C7 O1 K2 K1 58.7(9) . . . 2_444 ? C7 O1 K2 K2 -168.3(8) . . . 3_545 ? C23 O14 K2 O13 -142(2) . . . . ? C23 O14 K2 O7 45(2) . . . 2_444 ? C23 O14 K2 O3 -108(2) . . . . ? C23 O14 K2 O12 114(2) . . . . ? C23 O14 K2 O1 -41(2) . . . . ? C23 O14 K2 O13 170(2) . . . 3_545 ? C23 O14 K2 O2 133(2) . . . 1_545 ? C23 O14 K2 O11 11(2) . . . 2_444 ? C23 O14 K2 K1 93(2) . . . 1_545 ? C23 O14 K2 K1 52(2) . . . 2_444 ? C23 O14 K2 K2 -170(2) . . . 3_545 ? O3 C8 Cr1 C10 126(18) 1_565 . . . ? O3 C8 Cr1 C9 -147(18) 1_565 . . . ? O3 C8 Cr1 C3 -55(18) 1_565 . . . ? O3 C8 Cr1 C2 -30(18) 1_565 . . . ? O3 C8 Cr1 C6 36(18) 1_565 . . . ? O3 C8 Cr1 C1 7(18) 1_565 . . . ? O3 C8 Cr1 C4 -54(19) 1_565 . . . ? O3 C8 Cr1 C5 39(19) 1_565 . . . ? O4 C10 Cr1 C8 25(53) . . . . ? O4 C10 Cr1 C9 -65(53) . . . . ? O4 C10 Cr1 C3 -152(53) . . . . ? O4 C10 Cr1 C2 115(53) . . . . ? O4 C10 Cr1 C6 140(53) . . . . ? O4 C10 Cr1 C1 113(53) . . . . ? O4 C10 Cr1 C4 -155(53) . . . . ? O4 C10 Cr1 C5 177(100) . . . . ? O5 C9 Cr1 C8 164(51) . . . . ? O5 C9 Cr1 C10 -108(51) . . . . ? O5 C9 Cr1 C3 45(51) . . . . ? O5 C9 Cr1 C2 72(51) . . . . ? O5 C9 Cr1 C6 -21(51) . . . . ? O5 C9 Cr1 C1 76(51) . . . . ? O5 C9 Cr1 C4 7(51) . . . . ? O5 C9 Cr1 C5 -19(51) . . . . ? C2 C3 Cr1 C8 46.2(6) . . . . ? C4 C3 Cr1 C8 179.0(5) . . . . ? C2 C3 Cr1 C10 -137.6(7) . . . . ? C4 C3 Cr1 C10 -4.8(10) . . . . ? C2 C3 Cr1 C9 136.4(5) . . . . ? C4 C3 Cr1 C9 -90.8(6) . . . . ? C4 C3 Cr1 C2 132.8(7) . . . . ? C2 C3 Cr1 C6 -66.2(5) . . . . ? C4 C3 Cr1 C6 66.7(5) . . . . ? C2 C3 Cr1 C1 -29.0(4) . . . . ? C4 C3 Cr1 C1 103.9(6) . . . . ? C2 C3 Cr1 C4 -132.8(7) . . . . ? C2 C3 Cr1 C5 -103.1(5) . . . . ? C4 C3 Cr1 C5 29.7(5) . . . . ? C3 C2 Cr1 C8 -141.0(5) . . . . ? C1 C2 Cr1 C8 86.0(5) . . . . ? C3 C2 Cr1 C10 129.5(8) . . . . ? C1 C2 Cr1 C10 -3.5(10) . . . . ? C3 C2 Cr1 C9 -50.4(6) . . . . ? C1 C2 Cr1 C9 176.6(5) . . . . ? C1 C2 Cr1 C3 -133.0(7) . . . . ? C3 C2 Cr1 C6 102.9(5) . . . . ? C1 C2 Cr1 C6 -30.1(5) . . . . ? C3 C2 Cr1 C1 133.0(7) . . . . ? C3 C2 Cr1 C4 29.2(5) . . . . ? C1 C2 Cr1 C4 -103.8(5) . . . . ? C3 C2 Cr1 C5 65.7(5) . . . . ? C1 C2 Cr1 C5 -67.3(5) . . . . ? C5 C6 Cr1 C8 177.0(5) . . . . ? C1 C6 Cr1 C8 -51.3(6) . . . . ? C5 C6 Cr1 C10 88.7(5) . . . . ? C1 C6 Cr1 C10 -139.6(5) . . . . ? C5 C6 Cr1 C9 2.0(10) . . . . ? C1 C6 Cr1 C9 133.8(8) . . . . ? C5 C6 Cr1 C3 -65.7(5) . . . . ? C1 C6 Cr1 C3 66.1(5) . . . . ? C5 C6 Cr1 C2 -101.6(5) . . . . ? C1 C6 Cr1 C2 30.1(5) . . . . ? C5 C6 Cr1 C1 -131.7(7) . . . . ? C5 C6 Cr1 C4 -28.1(5) . . . . ? C1 C6 Cr1 C4 103.6(6) . . . . ? C1 C6 Cr1 C5 131.7(7) . . . . ? C2 C1 Cr1 C8 -94.5(5) . . . . ? C6 C1 Cr1 C8 134.9(6) . . . . ? C7 C1 Cr1 C8 19.0(7) . . . . ? C2 C1 Cr1 C10 178.4(5) . . . . ? C6 C1 Cr1 C10 47.9(6) . . . . ? C7 C1 Cr1 C10 -68.0(8) . . . . ? C2 C1 Cr1 C9 -6.8(10) . . . . ? C6 C1 Cr1 C9 -137.4(8) . . . . ? C7 C1 Cr1 C9 106.7(10) . . . . ? C2 C1 Cr1 C3 28.1(5) . . . . ? C6 C1 Cr1 C3 -102.4(6) . . . . ? C7 C1 Cr1 C3 141.7(8) . . . . ? C6 C1 Cr1 C2 -130.5(7) . . . . ? C7 C1 Cr1 C2 113.6(9) . . . . ? C2 C1 Cr1 C6 130.5(7) . . . . ? C7 C1 Cr1 C6 -115.9(9) . . . . ? C2 C1 Cr1 C4 65.2(5) . . . . ? C6 C1 Cr1 C4 -65.4(5) . . . . ? C7 C1 Cr1 C4 178.7(8) . . . . ? C2 C1 Cr1 C5 101.2(5) . . . . ? C6 C1 Cr1 C5 -29.3(5) . . . . ? C7 C1 Cr1 C5 -145.2(8) . . . . ? C5 C4 Cr1 C8 128.1(9) . . . . ? C3 C4 Cr1 C8 -2.3(12) . . . . ? C5 C4 Cr1 C10 -52.0(6) . . . . ? C3 C4 Cr1 C10 177.6(5) . . . . ? C5 C4 Cr1 C9 -139.4(6) . . . . ? C3 C4 Cr1 C9 90.2(6) . . . . ? C5 C4 Cr1 C3 130.4(8) . . . . ? C5 C4 Cr1 C2 102.3(6) . . . . ? C3 C4 Cr1 C2 -28.1(5) . . . . ? C5 C4 Cr1 C6 28.5(5) . . . . ? C3 C4 Cr1 C6 -101.9(6) . . . . ? C5 C4 Cr1 C1 65.4(5) . . . . ? C3 C4 Cr1 C1 -65.0(5) . . . . ? C3 C4 Cr1 C5 -130.4(8) . . . . ? C4 C5 Cr1 C8 -139.2(8) . . . . ? C6 C5 Cr1 C8 -5.8(10) . . . . ? C4 C5 Cr1 C10 134.5(6) . . . . ? C6 C5 Cr1 C10 -92.1(5) . . . . ? C4 C5 Cr1 C9 47.6(6) . . . . ? C6 C5 Cr1 C9 -179.0(5) . . . . ? C4 C5 Cr1 C3 -30.5(5) . . . . ? C6 C5 Cr1 C3 102.9(5) . . . . ? C4 C5 Cr1 C2 -66.5(5) . . . . ? C6 C5 Cr1 C2 66.9(5) . . . . ? C4 C5 Cr1 C6 -133.4(8) . . . . ? C4 C5 Cr1 C1 -103.9(6) . . . . ? C6 C5 Cr1 C1 29.5(5) . . . . ? C6 C5 Cr1 C4 133.4(8) . . . . ? O10 C18 Cr2 C19 143(27) . . . . ? O10 C18 Cr2 C20 53(27) . . . . ? O10 C18 Cr2 C14 -128(27) . . . . ? O10 C18 Cr2 C13 -34(27) . . . . ? O10 C18 Cr2 C16 -101(27) . . . . ? O10 C18 Cr2 C12 -37(27) . . . . ? O10 C18 Cr2 C11 -64(27) . . . 2_454 ? O10 C18 Cr2 C15 -127(27) . . . . ? O9 C19 Cr2 C18 -169(100) . . . . ? O9 C19 Cr2 C20 -82(58) . . . . ? O9 C19 Cr2 C14 36(58) . . . . ? O9 C19 Cr2 C13 9(58) . . . . ? O9 C19 Cr2 C16 100(58) . . . . ? O9 C19 Cr2 C12 10(58) . . . . ? O9 C19 Cr2 C11 102(58) . . . 2_454 ? O9 C19 Cr2 C15 73(58) . . . . ? O8 C20 Cr2 C18 46(28) . . . . ? O8 C20 Cr2 C19 -43(28) . . . . ? O8 C20 Cr2 C14 -134(27) . . . . ? O8 C20 Cr2 C13 -161(28) . . . . ? O8 C20 Cr2 C16 133(27) . . . . ? O8 C20 Cr2 C12 162(28) . . . . ? O8 C20 Cr2 C11 135(27) . . . 2_454 ? O8 C20 Cr2 C15 -134(27) . . . . ? C13 C14 Cr2 C18 132.1(8) . . . . ? C15 C14 Cr2 C18 1.0(9) . . . . ? C13 C14 Cr2 C19 -138.6(5) . . . . ? C15 C14 Cr2 C19 90.3(5) . . . . ? C13 C14 Cr2 C20 -48.6(6) . . . . ? C15 C14 Cr2 C20 -179.7(5) . . . . ? C15 C14 Cr2 C13 -131.1(7) . . . . ? C13 C14 Cr2 C16 102.9(5) . . . . ? C15 C14 Cr2 C16 -28.2(4) . . . . ? C13 C14 Cr2 C12 29.6(5) . . . . ? C15 C14 Cr2 C12 -101.5(5) . . . . ? C13 C14 Cr2 C11 65.8(5) . . . 2_454 ? C15 C14 Cr2 C11 -65.2(5) . . . 2_454 ? C13 C14 Cr2 C15 131.1(7) . . . . ? C14 C13 Cr2 C18 -135.6(7) . . . . ? C12 C13 Cr2 C18 -4.2(9) . . . . ? C14 C13 Cr2 C19 48.2(6) . . . . ? C12 C13 Cr2 C19 179.6(5) . . . . ? C14 C13 Cr2 C20 138.3(5) . . . . ? C12 C13 Cr2 C20 -90.2(5) . . . . ? C12 C13 Cr2 C14 131.4(7) . . . . ? C14 C13 Cr2 C16 -65.9(5) . . . . ? C12 C13 Cr2 C16 65.5(5) . . . . ? C14 C13 Cr2 C12 -131.4(7) . . . . ? C14 C13 Cr2 C11 -103.0(5) . . . 2_454 ? C12 C13 Cr2 C11 28.5(4) . . . 2_454 ? C14 C13 Cr2 C15 -29.9(5) . . . . ? C12 C13 Cr2 C15 101.6(5) . . . . ? C15 C16 Cr2 C18 -139.2(5) . . . . ? C11 C16 Cr2 C18 89.2(5) 2_454 . . . ? C15 C16 Cr2 C19 -49.7(5) . . . . ? C11 C16 Cr2 C19 178.7(4) 2_454 . . . ? C15 C16 Cr2 C20 134.8(7) . . . . ? C11 C16 Cr2 C20 3.3(10) 2_454 . . . ? C15 C16 Cr2 C14 28.9(4) . . . . ? C11 C16 Cr2 C14 -102.7(5) 2_454 . . . ? C15 C16 Cr2 C13 65.7(4) . . . . ? C11 C16 Cr2 C13 -65.9(5) 2_454 . . . ? C15 C16 Cr2 C12 102.6(5) . . . . ? C11 C16 Cr2 C12 -29.0(4) 2_454 . . . ? C15 C16 Cr2 C11 131.6(7) . . . 2_454 ? C11 C16 Cr2 C15 -131.6(7) 2_454 . . . ? C11 C12 Cr2 C18 -49.4(6) 2_454 . . . ? C13 C12 Cr2 C18 177.9(5) . . . . ? C11 C12 Cr2 C19 131.8(7) 2_454 . . . ? C13 C12 Cr2 C19 -0.8(10) . . . . ? C11 C12 Cr2 C20 -136.9(5) 2_454 . . . ? C13 C12 Cr2 C20 90.4(5) . . . . ? C11 C12 Cr2 C14 103.2(5) 2_454 . . . ? C13 C12 Cr2 C14 -29.4(5) . . . . ? C11 C12 Cr2 C13 132.7(7) 2_454 . . . ? C11 C12 Cr2 C16 29.5(5) 2_454 . . . ? C13 C12 Cr2 C16 -103.1(5) . . . . ? C13 C12 Cr2 C11 -132.7(7) . . . 2_454 ? C11 C12 Cr2 C15 65.8(5) 2_454 . . . ? C13 C12 Cr2 C15 -66.8(5) . . . . ? C16 C15 Cr2 C18 47.5(5) . . . . ? C14 C15 Cr2 C18 -179.5(5) . . . . ? C16 C15 Cr2 C19 136.9(5) . . . . ? C14 C15 Cr2 C19 -90.2(5) . . . . ? C16 C15 Cr2 C20 -132.4(7) . . . . ? C14 C15 Cr2 C20 0.6(10) . . . . ? C16 C15 Cr2 C14 -133.0(7) . . . . ? C16 C15 Cr2 C13 -103.4(5) . . . . ? C14 C15 Cr2 C13 29.6(4) . . . . ? C14 C15 Cr2 C16 133.0(7) . . . . ? C16 C15 Cr2 C12 -66.0(4) . . . . ? C14 C15 Cr2 C12 66.9(5) . . . . ? C16 C15 Cr2 C11 -29.7(4) . . . 2_454 ? C14 C15 Cr2 C11 103.3(5) . . . 2_454 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.049 _refine_diff_density_min -0.746 _refine_diff_density_rms 0.109 #============================================================================== data_5 _database_code_depnum_ccdc_archive 'CCDC 778879' #TrackingRef '- deposit.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C11 H16 Cr Na2 O13' _chemical_formula_sum 'C11 H16 Cr Na2 O13' _chemical_formula_weight 454.22 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 6.1130(5) _cell_length_b 22.6678(19) _cell_length_c 12.6748(11) _cell_angle_alpha 90.00 _cell_angle_beta 96.384(7) _cell_angle_gamma 90.00 _cell_volume 1745.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 17989 _cell_measurement_theta_min 1.80 _cell_measurement_theta_max 29.67 _exptl_crystal_description 'fragment from plate' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.729 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 928 _exptl_absorpt_coefficient_mu 0.773 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.6982 _exptl_absorpt_correction_T_max 0.9587 _exptl_absorpt_process_details 'STOE X-RED & X-SHAPE' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 IPDS 2' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17690 _diffrn_reflns_av_R_equivalents 0.0559 _diffrn_reflns_av_sigmaI/netI 0.0347 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 29.18 _reflns_number_total 4694 _reflns_number_gt 4044 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA, PLATON (A.L.Spek, 2005)' _computing_data_reduction 'STOE X-RED, PLATON (A.L.Spek, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e/3' _computing_publication_material 'X-STEP32, Microsoft Word' _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^)+(0.0455P)^2^+0.3603P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4694 _refine_ls_number_parameters 292 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0392 _refine_ls_R_factor_gt 0.0321 _refine_ls_wR_factor_ref 0.0818 _refine_ls_wR_factor_gt 0.0786 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0769(2) 0.22439(6) 0.70304(11) 0.0218(3) Uani 1 1 d . . . C2 C -0.0673(2) 0.27151(6) 0.67251(12) 0.0226(3) Uani 1 1 d . . . H2 H -0.2180 0.2635 0.6504 0.027 Uiso 1 1 calc R . . C3 C 0.0091(2) 0.33063(6) 0.67434(11) 0.0227(3) Uani 1 1 d . . . H3 H -0.0904 0.3620 0.6552 0.027 Uiso 1 1 calc R . . C4 C 0.2338(2) 0.34243(6) 0.70472(11) 0.0216(3) Uani 1 1 d . . . C5 C 0.3779(2) 0.29520(6) 0.73806(11) 0.0221(3) Uani 1 1 d . . . H5 H 0.5280 0.3032 0.7616 0.027 Uiso 1 1 calc R . . C6 C 0.3014(2) 0.23694(6) 0.73655(11) 0.0225(3) Uani 1 1 d . . . H6 H 0.4001 0.2057 0.7580 0.027 Uiso 1 1 calc R . . C7 C -0.0094(2) 0.16159(6) 0.69908(12) 0.0238(3) Uani 1 1 d . . . C8 C 0.3259(2) 0.40470(6) 0.69940(11) 0.0233(3) Uani 1 1 d . . . C9 C 0.3799(3) 0.32570(7) 0.50358(12) 0.0257(3) Uani 1 1 d . . . C10 C 0.3318(3) 0.21021(7) 0.51792(12) 0.0280(3) Uani 1 1 d . . . C11 C -0.0115(3) 0.27364(8) 0.46384(12) 0.0297(3) Uani 1 1 d . . . O1 O 0.11637(19) 0.12272(5) 0.74406(10) 0.0309(2) Uani 1 1 d . . . O2 O -0.19823(19) 0.15288(5) 0.65326(10) 0.0323(2) Uani 1 1 d . . . O3 O 0.20127(19) 0.44359(5) 0.65362(10) 0.0291(2) Uani 1 1 d . . . O4 O 0.52009(19) 0.41230(5) 0.73995(9) 0.0296(2) Uani 1 1 d . . . O5 O 0.4844(2) 0.35848(6) 0.46081(11) 0.0387(3) Uani 1 1 d . . . O6 O 0.3990(3) 0.16884(6) 0.48041(11) 0.0452(3) Uani 1 1 d . . . O7 O -0.1568(2) 0.27037(8) 0.39845(11) 0.0489(4) Uani 1 1 d . . . O8 O 0.9675(2) 0.50633(6) 0.80657(10) 0.0293(2) Uani 1 1 d . . . O9 O 0.8380(3) 0.39544(7) 0.94699(15) 0.0454(3) Uani 1 1 d . . . O10 O 0.7142(2) 0.53598(6) 1.03842(11) 0.0329(3) Uani 1 1 d . . . O11 O 0.4777(2) 0.56911(5) 0.77664(10) 0.0290(2) Uani 1 1 d . . . O12 O 0.0017(2) 0.56986(6) 0.56943(11) 0.0314(2) Uani 1 1 d . . . O13 O 0.3193(2) 0.51907(6) 0.41554(10) 0.0305(2) Uani 1 1 d . . . Na1 Na 0.62551(11) 0.48158(3) 0.87916(5) 0.02979(14) Uani 1 1 d . . . Na2 Na 0.36097(10) 0.53755(3) 0.59929(5) 0.02771(14) Uani 1 1 d . . . Cr1 Cr 0.20894(4) 0.275886(9) 0.576484(18) 0.01920(7) Uani 1 1 d . . . H8A H 0.963(4) 0.5405(12) 0.789(2) 0.049(7) Uiso 1 1 d . . . H8B H 1.034(5) 0.4907(12) 0.762(2) 0.055(7) Uiso 1 1 d . . . H9A H 0.813(4) 0.3820(12) 1.003(2) 0.051(7) Uiso 1 1 d . . . H9B H 0.790(7) 0.372(2) 0.905(4) 0.116(16) Uiso 1 1 d . . . H10A H 0.812(5) 0.5225(13) 1.076(2) 0.055(8) Uiso 1 1 d . . . H10B H 0.750(5) 0.5652(15) 1.032(3) 0.070(10) Uiso 1 1 d . . . H11A H 0.592(4) 0.5887(12) 0.773(2) 0.051(7) Uiso 1 1 d . . . H11B H 0.393(4) 0.5908(11) 0.7975(19) 0.041(6) Uiso 1 1 d . . . H12A H -0.048(4) 0.5928(10) 0.6079(19) 0.036(6) Uiso 1 1 d . . . H12B H -0.027(5) 0.5741(13) 0.510(2) 0.059(8) Uiso 1 1 d . . . H13A H 0.214(4) 0.5013(11) 0.4046(18) 0.039(6) Uiso 1 1 d . . . H13B H 0.334(4) 0.5373(11) 0.370(2) 0.037(6) Uiso 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 C1 0.0239(6) 0.0206(6) 0.0216(6) 0.0006(5) 0.0055(5) -0.0019(5) C2 0.0204(6) 0.0234(6) 0.0250(6) -0.0012(5) 0.0064(5) -0.0012(5) C3 0.0227(6) 0.0208(6) 0.0255(6) -0.0007(5) 0.0060(5) 0.0024(5) C4 0.0249(7) 0.0196(6) 0.0209(6) -0.0019(5) 0.0051(5) -0.0004(5) C5 0.0231(6) 0.0210(6) 0.0221(6) -0.0010(5) 0.0021(5) -0.0006(5) C6 0.0257(7) 0.0202(6) 0.0218(6) 0.0015(5) 0.0026(5) 0.0009(5) C7 0.0279(7) 0.0207(6) 0.0239(6) 0.0005(5) 0.0072(5) -0.0024(5) C8 0.0277(7) 0.0201(6) 0.0231(6) -0.0018(5) 0.0062(5) -0.0001(5) C9 0.0280(7) 0.0240(6) 0.0257(7) -0.0016(5) 0.0057(5) -0.0011(5) C10 0.0329(8) 0.0264(7) 0.0250(7) -0.0004(5) 0.0050(6) 0.0033(6) C11 0.0274(7) 0.0389(8) 0.0236(7) -0.0011(6) 0.0062(6) 0.0010(6) O1 0.0317(6) 0.0214(5) 0.0401(6) 0.0052(4) 0.0060(5) -0.0005(4) O2 0.0307(6) 0.0274(5) 0.0378(6) 0.0015(5) -0.0010(5) -0.0082(4) O3 0.0316(6) 0.0199(5) 0.0361(6) 0.0011(4) 0.0048(4) 0.0015(4) O4 0.0308(6) 0.0247(5) 0.0325(6) -0.0009(4) 0.0000(4) -0.0063(4) O5 0.0426(7) 0.0362(6) 0.0398(7) 0.0042(5) 0.0158(5) -0.0087(5) O6 0.0568(9) 0.0364(7) 0.0428(7) -0.0107(6) 0.0068(6) 0.0160(6) O7 0.0320(6) 0.0850(11) 0.0288(6) -0.0064(7) -0.0010(5) 0.0019(7) O8 0.0298(6) 0.0259(5) 0.0325(6) 0.0014(5) 0.0045(5) 0.0028(4) O9 0.0480(8) 0.0425(8) 0.0451(8) 0.0106(7) 0.0030(6) -0.0075(6) O10 0.0326(6) 0.0328(6) 0.0322(6) 0.0009(5) -0.0009(5) -0.0036(5) O11 0.0265(5) 0.0262(5) 0.0346(6) -0.0035(4) 0.0047(4) 0.0021(5) O12 0.0314(6) 0.0313(6) 0.0318(6) 0.0007(5) 0.0050(5) 0.0061(5) O13 0.0262(6) 0.0386(7) 0.0268(6) 0.0012(5) 0.0031(4) -0.0036(5) Na1 0.0278(3) 0.0349(3) 0.0264(3) -0.0021(2) 0.0017(2) -0.0015(2) Na2 0.0262(3) 0.0296(3) 0.0275(3) -0.0013(2) 0.0034(2) 0.0021(2) Cr1 0.01993(11) 0.01772(11) 0.02029(11) 0.00009(8) 0.00377(8) 0.00022(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 C1 C2 1.411(2) . ? C1 C6 1.420(2) . ? C1 C7 1.5169(19) . ? C1 Cr1 2.2080(14) . ? C2 C3 1.4185(19) . ? C2 Cr1 2.1910(14) . ? C3 C4 1.410(2) . ? C3 Cr1 2.2154(14) . ? C4 C5 1.421(2) . ? C4 C8 1.5239(19) . ? C4 Cr1 2.2103(14) . ? C5 C6 1.4006(19) . ? C5 Cr1 2.2322(15) . ? C6 Cr1 2.2270(14) . ? C7 O2 1.2490(19) . ? C7 O1 1.2627(19) . ? C8 O4 1.2520(19) . ? C8 O3 1.2633(18) . ? C9 O5 1.1541(19) . ? C9 Cr1 1.8534(15) . ? C10 O6 1.148(2) . ? C10 Cr1 1.8589(16) . ? C11 O7 1.148(2) . ? C11 Cr1 1.8518(17) . ? O3 Na2 2.4724(13) . ? O4 Na1 2.3963(13) . ? O5 Na2 2.6809(14) 3_666 ? O8 Na1 2.4413(14) . ? O9 Na1 2.4476(17) . ? O10 Na1 2.3761(15) . ? O10 Na1 2.4585(15) 3_667 ? O11 Na2 2.3911(14) . ? O11 Na1 2.4860(14) . ? O12 Na2 2.3062(14) . ? O13 Na2 2.3522(14) . ? O13 Na2 2.3634(14) 3_666 ? Na1 O10 2.4585(15) 3_667 ? Na1 Na1 3.6717(13) 3_667 ? Na1 Na2 3.9410(10) . ? Na2 O13 2.3633(14) 3_666 ? Na2 O5 2.6809(14) 3_666 ? Na2 Na2 3.6159(13) 3_666 ? 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 C1 C6 118.95(13) . . ? C2 C1 C7 119.80(13) . . ? C6 C1 C7 121.25(13) . . ? C2 C1 Cr1 70.63(8) . . ? C6 C1 Cr1 72.06(8) . . ? C7 C1 Cr1 128.75(10) . . ? C1 C2 C3 121.06(13) . . ? C1 C2 Cr1 71.94(8) . . ? C3 C2 Cr1 72.16(8) . . ? C4 C3 C2 119.51(13) . . ? C4 C3 Cr1 71.22(8) . . ? C2 C3 Cr1 70.29(8) . . ? C3 C4 C5 119.43(13) . . ? C3 C4 C8 121.12(13) . . ? C5 C4 C8 119.42(13) . . ? C3 C4 Cr1 71.61(8) . . ? C5 C4 Cr1 72.19(8) . . ? C8 C4 Cr1 126.52(9) . . ? C6 C5 C4 120.75(13) . . ? C6 C5 Cr1 71.49(8) . . ? C4 C5 Cr1 70.52(8) . . ? C5 C6 C1 120.23(13) . . ? C5 C6 Cr1 71.89(8) . . ? C1 C6 Cr1 70.60(8) . . ? O2 C7 O1 125.76(14) . . ? O2 C7 C1 117.62(13) . . ? O1 C7 C1 116.62(13) . . ? O4 C8 O3 126.04(14) . . ? O4 C8 C4 116.57(13) . . ? O3 C8 C4 117.39(13) . . ? O5 C9 Cr1 177.32(14) . . ? O6 C10 Cr1 177.16(16) . . ? O7 C11 Cr1 175.41(16) . . ? C8 O3 Na2 119.51(10) . . ? C8 O4 Na1 123.88(10) . . ? C9 O5 Na2 158.54(12) . 3_666 ? Na1 O10 Na1 98.82(5) . 3_667 ? Na2 O11 Na1 107.80(5) . . ? Na2 O13 Na2 100.14(5) . 3_666 ? O10 Na1 O4 169.40(6) . . ? O10 Na1 O8 94.41(5) . . ? O4 Na1 O8 92.56(5) . . ? O10 Na1 O9 93.07(6) . . ? O4 Na1 O9 79.89(6) . . ? O8 Na1 O9 82.67(5) . . ? O10 Na1 O10 81.18(5) . 3_667 ? O4 Na1 O10 92.07(5) . 3_667 ? O8 Na1 O10 175.23(5) . 3_667 ? O9 Na1 O10 99.31(6) . 3_667 ? O10 Na1 O11 93.73(5) . . ? O4 Na1 O11 94.93(5) . . ? O8 Na1 O11 84.05(5) . . ? O9 Na1 O11 165.50(6) . . ? O10 Na1 O11 94.38(5) 3_667 . ? O10 Na1 Na1 41.43(4) . 3_667 ? O4 Na1 Na1 131.32(4) . 3_667 ? O8 Na1 Na1 135.81(4) . 3_667 ? O9 Na1 Na1 98.22(5) . 3_667 ? O10 Na1 Na1 39.75(3) 3_667 3_667 ? O11 Na1 Na1 95.35(4) . 3_667 ? O10 Na1 Na2 129.02(4) . . ? O4 Na1 Na2 59.90(3) . . ? O8 Na1 Na2 82.51(4) . . ? O9 Na1 Na2 136.19(5) . . ? O10 Na1 Na2 98.81(4) 3_667 . ? O11 Na1 Na2 35.29(3) . . ? Na1 Na1 Na2 120.66(3) 3_667 . ? O12 Na2 O13 84.13(5) . . ? O12 Na2 O13 160.12(6) . 3_666 ? O13 Na2 O13 79.86(5) . 3_666 ? O12 Na2 O11 103.80(5) . . ? O13 Na2 O11 166.48(6) . . ? O13 Na2 O11 94.26(5) 3_666 . ? O12 Na2 O3 85.46(5) . . ? O13 Na2 O3 96.87(5) . . ? O13 Na2 O3 84.84(5) 3_666 . ? O11 Na2 O3 94.69(5) . . ? O12 Na2 O5 91.93(5) . 3_666 ? O13 Na2 O5 82.99(5) . 3_666 ? O13 Na2 O5 97.70(5) 3_666 3_666 ? O11 Na2 O5 85.78(5) . 3_666 ? O3 Na2 O5 177.39(5) . 3_666 ? O12 Na2 Na2 123.24(5) . 3_666 ? O13 Na2 Na2 40.05(3) . 3_666 ? O13 Na2 Na2 39.82(3) 3_666 3_666 ? O11 Na2 Na2 132.92(4) . 3_666 ? O3 Na2 Na2 91.09(4) . 3_666 ? O5 Na2 Na2 90.47(4) 3_666 3_666 ? O12 Na2 Na1 122.54(4) . . ? O13 Na2 Na1 145.32(4) . . ? O13 Na2 Na1 68.69(4) 3_666 . ? O11 Na2 Na1 36.91(3) . . ? O3 Na2 Na1 66.87(3) . . ? O5 Na2 Na1 114.61(4) 3_666 . ? Na2 Na2 Na1 107.30(3) 3_666 . ? C11 Cr1 C9 91.98(7) . . ? C11 Cr1 C10 87.81(7) . . ? C9 Cr1 C10 90.79(7) . . ? C11 Cr1 C2 83.53(6) . . ? C9 Cr1 C2 144.75(6) . . ? C10 Cr1 C2 123.79(6) . . ? C11 Cr1 C1 104.60(6) . . ? C9 Cr1 C1 162.98(6) . . ? C10 Cr1 C1 93.63(6) . . ? C2 Cr1 C1 37.42(5) . . ? C11 Cr1 C4 124.78(6) . . ? C9 Cr1 C4 87.39(6) . . ? C10 Cr1 C4 147.40(6) . . ? C2 Cr1 C4 67.46(5) . . ? C1 Cr1 C4 80.06(5) . . ? C11 Cr1 C3 92.73(6) . . ? C9 Cr1 C3 108.33(6) . . ? C10 Cr1 C3 160.84(6) . . ? C2 Cr1 C3 37.55(5) . . ? C1 Cr1 C3 67.69(5) . . ? C4 Cr1 C3 37.17(5) . . ? C11 Cr1 C6 141.32(6) . . ? C9 Cr1 C6 126.56(6) . . ? C10 Cr1 C6 88.48(6) . . ? C2 Cr1 C6 67.00(5) . . ? C1 Cr1 C6 37.34(5) . . ? C4 Cr1 C6 67.10(5) . . ? C3 Cr1 C6 79.16(5) . . ? C11 Cr1 C5 159.33(6) . . ? C9 Cr1 C5 96.25(6) . . ? C10 Cr1 C5 110.93(6) . . ? C2 Cr1 C5 78.81(5) . . ? C1 Cr1 C5 66.83(5) . . ? C4 Cr1 C5 37.29(5) . . ? C3 Cr1 C5 66.69(5) . . ? C6 Cr1 C5 36.61(5) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 29.18 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.373 _refine_diff_density_min -0.642 _refine_diff_density_rms 0.064 #============================================================================== data_6 _database_code_depnum_ccdc_archive 'CCDC 778880' #TrackingRef '- deposit.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H12 Cr K2 O10' _chemical_formula_sum 'C12 H12 Cr K2 O10' _chemical_formula_weight 446.42 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall -P2yn _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.765(2) _cell_length_b 7.1637(14) _cell_length_c 22.055(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.24(3) _cell_angle_gamma 90.00 _cell_volume 1690.7(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4287 _cell_measurement_theta_min 1.86 _cell_measurement_theta_max 28.82 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.754 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 1.219 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8196 _exptl_absorpt_correction_T_max 0.9879 _exptl_absorpt_process_details 'STOE X-RED & X-SHAPE' _exptl_special_details ; 'crystal had a low quality' ; _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 IPDS 2' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10098 _diffrn_reflns_av_R_equivalents 0.1619 _diffrn_reflns_av_sigmaI/netI 0.1404 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3312 _reflns_number_gt 1993 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA, PLATON (A.L.Spek, 2005)' _computing_data_reduction 'STOE X-RED, PLATON (A.L.Spek, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e/3' _computing_publication_material 'X-STEP32, Microsoft Word' _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^)+(0.1067P)^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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.006(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3312 _refine_ls_number_parameters 227 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1492 _refine_ls_R_factor_gt 0.0898 _refine_ls_wR_factor_ref 0.2304 _refine_ls_wR_factor_gt 0.1984 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5994(8) 0.3505(11) -0.0514(4) 0.0315(18) Uani 1 1 d . . . C2 C 0.6910(8) 0.4799(11) -0.0248(4) 0.0295(17) Uani 1 1 d . . . H2 H 0.7318 0.5627 -0.0498 0.035 Uiso 1 1 calc R . . C3 C 0.7200(8) 0.4822(11) 0.0402(4) 0.0309(18) Uani 1 1 d . . . H3 H 0.7788 0.5703 0.0582 0.037 Uiso 1 1 calc R . . C4 C 0.6640(7) 0.3583(11) 0.0778(4) 0.0276(16) Uani 1 1 d . . . C5 C 0.5705(8) 0.2317(11) 0.0501(4) 0.0321(18) Uani 1 1 d . . . H5 H 0.5292 0.1489 0.0749 0.039 Uiso 1 1 calc R . . C6 C 0.5404(8) 0.2300(11) -0.0127(4) 0.0277(16) Uani 1 1 d . . . H6 H 0.4784 0.1455 -0.0301 0.033 Uiso 1 1 calc R . . C7 C 0.5689(7) 0.3351(13) -0.1203(4) 0.0330(18) Uani 1 1 d . . . C8 C 0.7007(8) 0.3488(11) 0.1461(4) 0.0304(17) Uani 1 1 d . . . C9 C 0.7536(9) 0.0214(13) -0.0543(4) 0.038(2) Uani 1 1 d . . . C10 C 0.9128(8) 0.2382(11) 0.0047(4) 0.0326(18) Uani 1 1 d . . . C11 C 0.7917(10) 0.0086(13) 0.0626(5) 0.043(2) Uani 1 1 d . . . C12 C 0.5691(13) -0.052(2) -0.3605(6) 0.072(4) Uani 1 1 d . . . H12A H 0.5339 0.0260 -0.3945 0.108 Uiso 1 1 calc R . . H12B H 0.5472 -0.1831 -0.3691 0.108 Uiso 1 1 calc R . . H12C H 0.6603 -0.0389 -0.3553 0.108 Uiso 1 1 calc R . . O1 O 0.5126(6) 0.1880(9) -0.1400(3) 0.0392(14) Uani 1 1 d . . . O2 O 0.6009(6) 0.4685(9) -0.1531(3) 0.0418(15) Uani 1 1 d . . . O3 O 0.6579(6) 0.2149(8) 0.1751(3) 0.0348(13) Uani 1 1 d . . . O4 O 0.7715(6) 0.4764(8) 0.1702(3) 0.0356(14) Uani 1 1 d . . . O5 O 0.7585(7) -0.0880(11) -0.0930(3) 0.056(2) Uani 1 1 d . . . O6 O 1.0185(6) 0.2657(10) 0.0027(4) 0.0480(17) Uani 1 1 d . . . O7 O 0.8222(9) -0.1057(11) 0.0994(3) 0.063(2) Uani 1 1 d . . . O8 O 0.9479(8) 0.0237(15) 0.2345(4) 0.073(3) Uani 1 1 d . . . O9 O 0.7162(9) 0.2209(16) -0.2433(5) 0.084(3) Uani 1 1 d . . . O10 O 0.5197(8) 0.0048(14) -0.3059(3) 0.065(2) Uani 1 1 d . . . K1 K 0.77976(18) 0.3341(3) 0.29086(8) 0.0355(5) Uani 1 1 d . . . K2 K 0.5876(2) -0.1678(3) -0.19541(9) 0.0416(5) Uani 1 1 d . . . Cr1 Cr 0.74542(12) 0.19246(17) 0.00703(6) 0.0271(4) 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 C1 0.035(4) 0.027(4) 0.031(4) 0.002(3) -0.005(3) 0.006(3) C2 0.040(5) 0.023(4) 0.026(4) 0.004(3) 0.007(3) 0.004(3) C3 0.037(4) 0.023(4) 0.032(4) -0.008(3) 0.003(3) 0.004(3) C4 0.034(4) 0.022(4) 0.026(4) -0.004(3) -0.001(3) 0.003(3) C5 0.035(4) 0.022(4) 0.038(5) -0.001(3) -0.004(3) 0.006(3) C6 0.032(4) 0.024(4) 0.026(4) 0.003(3) 0.000(3) -0.002(3) C7 0.028(4) 0.037(5) 0.033(4) -0.004(4) 0.002(3) 0.000(3) C8 0.034(4) 0.026(4) 0.031(4) 0.004(3) 0.002(3) 0.005(3) C9 0.044(5) 0.028(4) 0.040(5) -0.001(4) -0.001(4) 0.004(4) C10 0.044(5) 0.027(4) 0.026(4) 0.001(3) 0.001(4) 0.008(3) C11 0.058(6) 0.029(5) 0.041(5) -0.003(4) 0.007(4) 0.012(4) C12 0.060(7) 0.105(11) 0.051(7) 0.004(7) 0.004(6) 0.013(7) O1 0.051(4) 0.033(3) 0.031(3) -0.006(3) -0.007(3) -0.003(3) O2 0.057(4) 0.036(3) 0.031(3) 0.004(3) -0.001(3) -0.008(3) O3 0.047(3) 0.028(3) 0.027(3) -0.001(3) -0.002(2) -0.003(3) O4 0.044(3) 0.030(3) 0.032(3) -0.005(3) -0.001(3) -0.007(3) O5 0.072(5) 0.045(4) 0.047(4) -0.020(4) -0.015(4) 0.022(4) O6 0.029(3) 0.046(4) 0.069(5) -0.003(3) 0.006(3) -0.001(3) O7 0.106(7) 0.041(4) 0.044(4) 0.017(4) 0.013(4) 0.028(4) O8 0.064(5) 0.100(7) 0.053(5) 0.014(5) -0.008(4) -0.033(5) O9 0.072(6) 0.107(8) 0.076(6) -0.029(6) 0.027(5) -0.023(6) O10 0.055(5) 0.099(7) 0.040(4) -0.004(4) 0.002(3) -0.001(4) K1 0.0475(11) 0.0280(9) 0.0295(9) 0.0012(8) -0.0028(7) -0.0009(8) K2 0.0462(11) 0.0415(11) 0.0370(10) 0.0022(9) 0.0040(8) -0.0004(9) Cr1 0.0351(7) 0.0204(6) 0.0250(6) 0.0006(6) 0.0000(5) 0.0017(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 C1 C6 1.412(12) . ? C1 C2 1.431(12) . ? C1 C7 1.525(11) . ? C1 Cr1 2.230(8) . ? C2 C3 1.435(12) . ? C2 Cr1 2.233(8) . ? C3 C4 1.395(12) . ? C3 Cr1 2.228(8) . ? C4 C5 1.441(11) . ? C4 C8 1.516(11) . ? C4 Cr1 2.217(8) . ? C5 C6 1.388(12) . ? C5 Cr1 2.217(9) . ? C6 Cr1 2.219(8) . ? C7 O2 1.268(11) . ? C7 O1 1.268(10) . ? C8 O3 1.267(10) . ? C8 O4 1.269(10) . ? C8 K1 3.215(8) . ? C9 O5 1.164(11) . ? C9 Cr1 1.834(9) . ? C10 O6 1.161(11) . ? C10 Cr1 1.837(9) . ? C11 O7 1.174(12) . ? C11 Cr1 1.832(10) . ? C12 O10 1.427(15) . ? O1 K1 2.793(6) 4_565 ? O1 K2 2.976(7) . ? O2 K2 2.767(7) 1_565 ? O3 K2 2.748(7) 3_655 ? O3 K1 2.871(6) . ? O3 K1 2.889(6) 2_645 ? O4 K1 2.777(6) 2_655 ? O4 K1 2.843(6) . ? O5 K2 2.812(7) . ? O7 K1 2.797(8) 2_645 ? O8 K1 2.805(8) 2_645 ? O8 K1 3.203(11) . ? O8 K2 3.263(11) 4_656 ? O9 K2 2.747(9) 2_654 ? O9 K2 3.332(11) . ? O10 K2 2.760(8) . ? K1 O4 2.777(6) 2_645 ? K1 O1 2.793(6) 4_666 ? K1 O7 2.797(8) 2_655 ? K1 O8 2.805(8) 2_655 ? K1 O3 2.889(6) 2_655 ? K1 K1 4.0297(18) 2_645 ? K1 K1 4.0297(18) 2_655 ? K1 K2 4.070(3) 4_666 ? K2 O9 2.747(9) 2_644 ? K2 O3 2.748(7) 3_655 ? K2 O2 2.767(7) 1_545 ? K2 O8 3.263(11) 4 ? K2 K1 4.070(3) 4_565 ? K2 K1 4.436(3) 3_655 ? 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 C6 C1 C2 119.0(7) . . ? C6 C1 C7 119.7(7) . . ? C2 C1 C7 121.3(7) . . ? C6 C1 Cr1 71.1(4) . . ? C2 C1 Cr1 71.4(4) . . ? C7 C1 Cr1 127.0(6) . . ? C1 C2 C3 118.8(7) . . ? C1 C2 Cr1 71.2(4) . . ? C3 C2 Cr1 71.0(5) . . ? C4 C3 C2 121.7(8) . . ? C4 C3 Cr1 71.3(5) . . ? C2 C3 Cr1 71.4(5) . . ? C3 C4 C5 118.4(7) . . ? C3 C4 C8 122.4(7) . . ? C5 C4 C8 119.2(7) . . ? C3 C4 Cr1 72.1(5) . . ? C5 C4 Cr1 71.0(5) . . ? C8 C4 Cr1 126.5(5) . . ? C6 C5 C4 120.4(8) . . ? C6 C5 Cr1 71.9(5) . . ? C4 C5 Cr1 71.0(5) . . ? C5 C6 C1 121.7(8) . . ? C5 C6 Cr1 71.7(5) . . ? C1 C6 Cr1 71.9(5) . . ? O2 C7 O1 125.5(8) . . ? O2 C7 C1 118.1(8) . . ? O1 C7 C1 116.4(8) . . ? O3 C8 O4 124.7(8) . . ? O3 C8 C4 117.7(7) . . ? O4 C8 C4 117.6(7) . . ? O3 C8 K1 63.0(4) . . ? O4 C8 K1 61.7(4) . . ? C4 C8 K1 179.3(6) . . ? O5 C9 Cr1 179.6(10) . . ? O6 C10 Cr1 179.1(8) . . ? O7 C11 Cr1 178.2(9) . . ? C7 O1 K1 126.9(5) . 4_565 ? C7 O1 K2 135.3(5) . . ? K1 O1 K2 89.69(17) 4_565 . ? C7 O2 K2 153.5(6) . 1_565 ? C8 O3 K2 125.8(5) . 3_655 ? C8 O3 K1 93.9(5) . . ? K2 O3 K1 104.2(2) 3_655 . ? C8 O3 K1 139.4(5) . 2_645 ? K2 O3 K1 92.41(19) 3_655 2_645 ? K1 O3 K1 88.78(16) . 2_645 ? C8 O4 K1 131.6(5) . 2_655 ? C8 O4 K1 95.1(5) . . ? K1 O4 K1 91.62(18) 2_655 . ? C9 O5 K2 130.4(6) . . ? C11 O7 K1 126.8(7) . 2_645 ? K1 O8 K1 84.0(3) 2_645 . ? K1 O8 K2 93.6(3) 2_645 4_656 ? K1 O8 K2 127.5(3) . 4_656 ? K2 O9 K2 140.1(4) 2_654 . ? C12 O10 K2 121.9(8) . . ? O4 K1 O1 88.58(19) 2_645 4_666 ? O4 K1 O7 76.4(2) 2_645 2_655 ? O1 K1 O7 87.1(2) 4_666 2_655 ? O4 K1 O8 108.0(3) 2_645 2_655 ? O1 K1 O8 148.1(2) 4_666 2_655 ? O7 K1 O8 71.4(3) 2_655 2_655 ? O4 K1 O4 129.32(18) 2_645 . ? O1 K1 O4 117.81(19) 4_666 . ? O7 K1 O4 141.2(2) 2_655 . ? O8 K1 O4 72.7(2) 2_655 . ? O4 K1 O3 85.06(18) 2_645 . ? O1 K1 O3 139.9(2) 4_666 . ? O7 K1 O3 129.1(2) 2_655 . ? O8 K1 O3 70.2(2) 2_655 . ? O4 K1 O3 46.29(17) . . ? O4 K1 O3 147.05(18) 2_645 2_655 ? O1 K1 O3 75.06(18) 4_666 2_655 ? O7 K1 O3 74.42(19) 2_655 2_655 ? O8 K1 O3 76.6(3) 2_655 2_655 ? O4 K1 O3 83.55(17) . 2_655 ? O3 K1 O3 125.65(18) . 2_655 ? O4 K1 O8 67.6(2) 2_645 . ? O1 K1 O8 70.2(2) 4_666 . ? O7 K1 O8 137.3(3) 2_655 . ? O8 K1 O8 141.03(15) 2_655 . ? O4 K1 O8 81.2(2) . . ? O3 K1 O8 70.8(2) . . ? O3 K1 O8 129.1(2) 2_655 . ? O4 K1 C8 107.3(2) 2_645 . ? O1 K1 C8 132.0(2) 4_666 . ? O7 K1 C8 140.1(3) 2_655 . ? O8 K1 C8 69.8(2) 2_655 . ? O4 K1 C8 23.14(19) . . ? O3 K1 C8 23.15(19) . . ? O3 K1 C8 104.84(19) 2_655 . ? O8 K1 C8 74.7(2) . . ? O4 K1 K1 44.85(13) 2_645 2_645 ? O1 K1 K1 106.46(15) 4_666 2_645 ? O7 K1 K1 117.76(16) 2_655 2_645 ? O8 K1 K1 104.4(2) 2_655 2_645 ? O4 K1 K1 84.99(14) . 2_645 ? O3 K1 K1 45.79(13) . 2_645 ? O3 K1 K1 167.62(15) 2_655 2_645 ? O8 K1 K1 43.80(15) . 2_645 ? C8 K1 K1 64.72(15) . 2_645 ? O4 K1 K1 158.65(15) 2_645 2_655 ? O1 K1 K1 112.60(15) 4_666 2_655 ? O7 K1 K1 101.04(18) 2_655 2_655 ? O8 K1 K1 52.2(2) 2_655 2_655 ? O4 K1 K1 43.54(13) . 2_655 ? O3 K1 K1 80.30(14) . 2_655 ? O3 K1 K1 45.43(12) 2_655 2_655 ? O8 K1 K1 120.83(17) . 2_655 ? C8 K1 K1 60.96(15) . 2_655 ? K1 K1 K1 125.46(9) 2_645 2_655 ? O4 K1 K2 134.93(14) 2_645 4_666 ? O1 K1 K2 46.98(14) 4_666 4_666 ? O7 K1 K2 103.76(17) 2_655 4_666 ? O8 K1 K2 114.7(2) 2_655 4_666 ? O4 K1 K2 78.55(13) . 4_666 ? O3 K1 K2 122.04(14) . 4_666 ? O3 K1 K2 42.42(13) 2_655 4_666 ? O8 K1 K2 86.95(16) . 4_666 ? C8 K1 K2 100.38(16) . 4_666 ? K1 K1 K2 130.08(9) 2_645 4_666 ? K1 K1 K2 66.41(6) 2_655 4_666 ? O9 K2 O3 148.1(3) 2_644 3_655 ? O9 K2 O10 80.8(3) 2_644 . ? O3 K2 O10 91.8(2) 3_655 . ? O9 K2 O2 83.0(3) 2_644 1_545 ? O3 K2 O2 81.1(2) 3_655 1_545 ? O10 K2 O2 136.0(2) . 1_545 ? O9 K2 O5 89.0(3) 2_644 . ? O3 K2 O5 116.8(2) 3_655 . ? O10 K2 O5 134.9(3) . . ? O2 K2 O5 85.1(2) 1_545 . ? O9 K2 O1 135.1(3) 2_644 . ? O3 K2 O1 74.32(18) 3_655 . ? O10 K2 O1 85.5(2) . . ? O2 K2 O1 132.43(19) 1_545 . ? O5 K2 O1 71.29(18) . . ? O9 K2 O8 83.1(3) 2_644 4 ? O3 K2 O8 65.2(2) 3_655 4 ? O10 K2 O8 82.4(3) . 4 ? O2 K2 O8 55.1(2) 1_545 4 ? O5 K2 O8 140.1(2) . 4 ? O1 K2 O8 137.1(2) . 4 ? O9 K2 O9 73.65(15) 2_644 . ? O3 K2 O9 126.5(2) 3_655 . ? O10 K2 O9 54.9(3) . . ? O2 K2 O9 152.4(2) 1_545 . ? O5 K2 O9 80.0(3) . . ? O1 K2 O9 63.6(2) . . ? O8 K2 O9 133.5(2) 4 . ? O9 K2 K1 142.9(2) 2_644 4_565 ? O3 K2 K1 45.17(13) 3_655 4_565 ? O10 K2 K1 62.35(18) . 4_565 ? O2 K2 K1 126.18(16) 1_545 4_565 ? O5 K2 K1 113.37(16) . 4_565 ? O1 K2 K1 43.32(12) . 4_565 ? O8 K2 K1 95.41(16) 4 4_565 ? O9 K2 K1 81.29(19) . 4_565 ? O9 K2 K1 112.5(3) 2_644 3_655 ? O3 K2 K1 38.85(13) 3_655 3_655 ? O10 K2 K1 64.17(19) . 3_655 ? O2 K2 K1 85.31(15) 1_545 3_655 ? O5 K2 K1 155.14(19) . 3_655 ? O1 K2 K1 99.05(13) . 3_655 ? O8 K2 K1 39.12(15) 4 3_655 ? O9 K2 K1 117.0(2) . 3_655 ? K1 K2 K1 56.35(4) 4_565 3_655 ? C11 Cr1 C9 89.0(4) . . ? C11 Cr1 C10 87.2(4) . . ? C9 Cr1 C10 88.5(4) . . ? C11 Cr1 C5 89.2(4) . . ? C9 Cr1 C5 120.8(4) . . ? C10 Cr1 C5 150.5(3) . . ? C11 Cr1 C4 90.8(4) . . ? C9 Cr1 C4 158.7(4) . . ? C10 Cr1 C4 112.8(3) . . ? C5 Cr1 C4 37.9(3) . . ? C11 Cr1 C6 114.3(4) . . ? C9 Cr1 C6 93.6(4) . . ? C10 Cr1 C6 158.5(3) . . ? C5 Cr1 C6 36.4(3) . . ? C4 Cr1 C6 67.2(3) . . ? C11 Cr1 C3 118.9(4) . . ? C9 Cr1 C3 151.9(4) . . ? C10 Cr1 C3 89.9(3) . . ? C5 Cr1 C3 66.5(3) . . ? C4 Cr1 C3 36.6(3) . . ? C6 Cr1 C3 78.3(3) . . ? C11 Cr1 C1 151.1(4) . . ? C9 Cr1 C1 90.1(4) . . ? C10 Cr1 C1 121.7(3) . . ? C5 Cr1 C1 66.7(3) . . ? C4 Cr1 C1 80.0(3) . . ? C6 Cr1 C1 37.0(3) . . ? C3 Cr1 C1 67.2(3) . . ? C11 Cr1 C2 156.4(4) . . ? C9 Cr1 C2 114.6(4) . . ? C10 Cr1 C2 93.0(3) . . ? C5 Cr1 C2 79.1(3) . . ? C4 Cr1 C2 67.5(3) . . ? C6 Cr1 C2 66.7(3) . . ? C3 Cr1 C2 37.5(3) . . ? C1 Cr1 C2 37.4(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.155 _refine_diff_density_min -0.546 _refine_diff_density_rms 0.153 #==============================================================================