Supplementary Material (ESI) for Journal of Materials Chemistry This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 1145 _publ_requested_journal 'Journal of Materials Chemistry' loop_ _publ_author_name 'Almeida, M.' 'Clemente-Leon, Miguel' 'Coronado, Eugenio' 'Gimenez-Saiz, Carlos' 'Gomez-Garcia, Carlos J.' 'Lopes, Elsa B.' _publ_contact_author_name 'Prof Eugenio Coronado' _publ_contact_author_address ; Prof Eugenio Coronado Instituto de Ciencia Molecular University de Valencia Dr Moliner 50, E-46100 Burjasot SPAIN ; _publ_contact_author_email 'EUGENIO.CORONADO@UV.ES' data_(per)5[Mo6O19]_(1) _database_code_CSD 161773 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H30 Mo3 O9.50' _chemical_formula_weight 1070.56 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' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.983(5) _cell_length_b 12.8986(19) _cell_length_c 13.627(7) _cell_angle_alpha 83.21(2) _cell_angle_beta 81.05(4) _cell_angle_gamma 82.20(2) _cell_volume 1880.0(13) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 4.26 _cell_measurement_theta_max 11.40 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.891 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1064 _exptl_absorpt_coefficient_mu 1.053 _exptl_absorpt_correction_type 'Psi scan' _exptl_absorpt_correction_T_min 0.519 _exptl_absorpt_correction_T_max 0.593 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD-4' _diffrn_measurement_method 'Omega/2Theta scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 400 _diffrn_standards_interval_time '60 min' _diffrn_standards_decay_% 1 _diffrn_reflns_number 6915 _diffrn_reflns_av_R_equivalents 0.0250 _diffrn_reflns_av_sigmaI/netI 0.0828 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 24.98 _reflns_number_total 6595 _reflns_number_gt 3980 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD-4 Software (Enraf-Nonius, 1988)' _computing_cell_refinement 'CAD-4 Software (Enraf-Nonius, 1988)' _computing_data_reduction 'CAD-4 Software (Enraf-Nonius, 1988)' _computing_structure_solution 'SIR97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0456P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6595 _refine_ls_number_parameters 566 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1140 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_ref 0.0935 _refine_ls_wR_factor_gt 0.0779 _refine_ls_goodness_of_fit_ref 0.984 _refine_ls_restrained_S_all 0.984 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.28452(4) 0.02547(3) 0.02126(4) 0.04048(14) Uani 1 1 d . . . Mo2 Mo 0.50067(4) 0.11870(4) 0.11509(4) 0.04635(15) Uani 1 1 d . . . Mo3 Mo 0.50552(4) 0.13554(4) 0.87206(4) 0.04664(15) Uani 1 1 d . . . O1 O 0.3231(3) -0.0749(3) 0.9276(3) 0.0430(9) Uani 1 1 d . . . O2 O 0.3301(3) 0.1317(3) 0.9131(3) 0.0498(10) Uani 1 1 d . . . O3 O 0.1283(3) 0.0457(3) 0.0382(3) 0.0507(10) Uani 1 1 d . . . O4 O 0.4995(3) -0.0113(3) 0.1957(3) 0.0512(10) Uani 1 1 d . . . O5 O 0.6789(3) 0.0842(3) 0.8763(3) 0.0433(9) Uani 1 1 d . . . O6 O 0.3292(3) 0.1203(3) 0.1087(3) 0.0470(9) Uani 1 1 d . . . O7 O 0.5093(3) 0.2054(3) 0.9865(3) 0.0503(10) Uani 1 1 d . . . O8 O 0.5050(4) 0.2065(3) 0.1947(3) 0.0690(13) Uani 1 1 d . . . O9 O 0.5118(4) 0.2319(3) 0.7790(3) 0.0707(13) Uani 1 1 d . . . O10 O 0.5000 0.0000 0.0000 0.0341(11) Uani 1 2 d S . . C1 C -0.1035(4) 0.4495(4) 0.8944(4) 0.0366(12) Uani 1 1 d . . . C2 C -0.1259(5) 0.5611(4) 0.8827(4) 0.0391(12) Uani 1 1 d . . . C3 C -0.2499(5) 0.6084(4) 0.8929(4) 0.0459(13) Uani 1 1 d . . . H3 H -0.2658 0.6814 0.8858 0.055 Uiso 1 1 calc R . . C4 C -0.3480(5) 0.5501(5) 0.9130(4) 0.0515(15) Uani 1 1 d . . . H4 H -0.4288 0.5838 0.9203 0.062 Uiso 1 1 calc R . . C5 C -0.3276(5) 0.4428(5) 0.9225(4) 0.0488(14) Uani 1 1 d . . . H5 H -0.3949 0.4042 0.9339 0.059 Uiso 1 1 calc R . . C6 C -0.2065(5) 0.3901(4) 0.9151(4) 0.0419(13) Uani 1 1 d . . . C7 C -0.1844(5) 0.2800(4) 0.9284(4) 0.0506(14) Uani 1 1 d . . . H7 H -0.2513 0.2408 0.9417 0.061 Uiso 1 1 calc R . . C8 C -0.0660(5) 0.2293(4) 0.9220(5) 0.0550(16) Uani 1 1 d . . . H8 H -0.0528 0.1563 0.9315 0.066 Uiso 1 1 calc R . . C9 C 0.0335(5) 0.2866(4) 0.9014(4) 0.0498(14) Uani 1 1 d . . . H9 H 0.1133 0.2508 0.8970 0.060 Uiso 1 1 calc R . . C10 C 0.0195(4) 0.3960(4) 0.8869(4) 0.0358(11) Uani 1 1 d . . . C11 C 0.1245(4) 0.4563(4) 0.8668(4) 0.0379(12) Uani 1 1 d . . . C12 C 0.2473(4) 0.4086(4) 0.8583(4) 0.0454(13) Uani 1 1 d . . . H12 H 0.2629 0.3357 0.8668 0.054 Uiso 1 1 calc R . . C13 C 0.3466(5) 0.4677(5) 0.8375(4) 0.0532(15) Uani 1 1 d . . . H13 H 0.4275 0.4342 0.8323 0.064 Uiso 1 1 calc R . . C14 C 0.3256(5) 0.5753(4) 0.8248(4) 0.0484(14) Uani 1 1 d . . . H14 H 0.3926 0.6143 0.8113 0.058 Uiso 1 1 calc R . . C15 C 0.2055(5) 0.6270(4) 0.8317(4) 0.0430(13) Uani 1 1 d . . . C16 C 0.1828(6) 0.7377(5) 0.8194(4) 0.0553(16) Uani 1 1 d . . . H16 H 0.2495 0.7770 0.8060 0.066 Uiso 1 1 calc R . . C17 C 0.0635(6) 0.7888(5) 0.8270(5) 0.0608(17) Uani 1 1 d . . . H17 H 0.0500 0.8618 0.8181 0.073 Uiso 1 1 calc R . . C18 C -0.0351(5) 0.7310(4) 0.8477(4) 0.0510(14) Uani 1 1 d . . . H18 H -0.1150 0.7666 0.8530 0.061 Uiso 1 1 calc R . . C19 C -0.0210(5) 0.6216(4) 0.8613(4) 0.0384(12) Uani 1 1 d . . . C20 C 0.1015(4) 0.5689(4) 0.8531(4) 0.0348(11) Uani 1 1 d . . . C21 C 0.1696(5) 0.5067(4) 0.6062(4) 0.0453(13) Uani 1 1 d . . . C22 C 0.1117(5) 0.6133(4) 0.6000(4) 0.0472(14) Uani 1 1 d . . . C23 C 0.1877(6) 0.6940(5) 0.5824(5) 0.0599(16) Uani 1 1 d . . . H23 H 0.1514 0.7635 0.5769 0.072 Uiso 1 1 calc R . . C24 C 0.3159(6) 0.6731(5) 0.5731(5) 0.0665(18) Uani 1 1 d . . . H24 H 0.3645 0.7282 0.5611 0.080 Uiso 1 1 calc R . . C25 C 0.3707(6) 0.5723(6) 0.5813(5) 0.0629(17) Uani 1 1 d . . . H25 H 0.4567 0.5594 0.5765 0.075 Uiso 1 1 calc R . . C26 C 0.3009(5) 0.4869(5) 0.5968(4) 0.0515(14) Uani 1 1 d . . . C27 C 0.3585(6) 0.3815(5) 0.6065(5) 0.0635(17) Uani 1 1 d . . . H27 H 0.4444 0.3676 0.6024 0.076 Uiso 1 1 calc R . . C28 C 0.2876(6) 0.3015(5) 0.6217(5) 0.0681(18) Uani 1 1 d . . . H28 H 0.3261 0.2326 0.6277 0.082 Uiso 1 1 calc R . . C29 C 0.1605(6) 0.3188(5) 0.6285(5) 0.0612(16) Uani 1 1 d . . . H29 H 0.1153 0.2616 0.6372 0.073 Uiso 1 1 calc R . . C30 C 0.0979(5) 0.4202(4) 0.6227(4) 0.0462(13) Uani 1 1 d . . . C31 C -0.0374(5) 0.4407(5) 0.6343(4) 0.0467(13) Uani 1 1 d . . . C32 C -0.1125(6) 0.3605(5) 0.6498(4) 0.0599(16) Uani 1 1 d . . . H32 H -0.0756 0.2912 0.6496 0.072 Uiso 1 1 calc R . . C33 C -0.2423(6) 0.3807(6) 0.6657(5) 0.0674(18) Uani 1 1 d . . . H33 H -0.2903 0.3252 0.6768 0.081 Uiso 1 1 calc R . . C34 C -0.2977(6) 0.4808(6) 0.6650(5) 0.0673(19) Uani 1 1 d . . . H34 H -0.3838 0.4934 0.6764 0.081 Uiso 1 1 calc R . . C35 C -0.2277(6) 0.5661(6) 0.6473(4) 0.0602(16) Uani 1 1 d . . . C36 C -0.2851(6) 0.6701(7) 0.6477(5) 0.072(2) Uani 1 1 d . . . H36 H -0.3712 0.6833 0.6597 0.087 Uiso 1 1 calc R . . C37 C -0.2151(7) 0.7525(6) 0.6303(6) 0.078(2) Uani 1 1 d . . . H37 H -0.2539 0.8213 0.6295 0.094 Uiso 1 1 calc R . . C38 C -0.0863(6) 0.7332(5) 0.6140(5) 0.0683(18) Uani 1 1 d . . . H38 H -0.0406 0.7902 0.6019 0.082 Uiso 1 1 calc R . . C39 C -0.0239(5) 0.6337(5) 0.6152(4) 0.0493(14) Uani 1 1 d . . . C40 C -0.0963(5) 0.5465(5) 0.6318(4) 0.0498(14) Uani 1 1 d . . . C41 C 0.1134(5) -0.0043(4) 0.5418(5) 0.0527(15) Uani 1 1 d . . . C42 C -0.0026(5) 0.0275(4) 0.6013(5) 0.0512(15) Uani 1 1 d . . . C43 C -0.0025(6) 0.0545(5) 0.6958(5) 0.0611(16) Uani 1 1 d . . . H43 H -0.0774 0.0769 0.7336 0.073 Uiso 1 1 calc R . . C44 C 0.1078(8) 0.0492(5) 0.7362(5) 0.0699(19) Uani 1 1 d . . . H44 H 0.1056 0.0668 0.8007 0.084 Uiso 1 1 calc R . . C45 C 0.2181(7) 0.0183(5) 0.6817(5) 0.0659(18) Uani 1 1 d . . . H45 H 0.2908 0.0150 0.7097 0.079 Uiso 1 1 calc R . . C46 C 0.2252(6) -0.0086(5) 0.5843(5) 0.0571(16) Uani 1 1 d . . . C47 C 0.3388(6) -0.0389(6) 0.5264(6) 0.076(2) Uani 1 1 d . . . H47 H 0.4121 -0.0421 0.5534 0.092 Uiso 1 1 calc R . . C48 C 0.3440(6) -0.0634(6) 0.4324(6) 0.082(2) Uani 1 1 d . . . H48 H 0.4205 -0.0829 0.3952 0.099 Uiso 1 1 calc R . . C49 C 0.2344(6) -0.0598(5) 0.3900(5) 0.0703(19) Uani 1 1 d . . . H49 H 0.2395 -0.0771 0.3250 0.084 Uiso 1 1 calc R . . C50 C 0.1191(6) -0.0309(5) 0.4430(5) 0.0560(15) 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 Mo1 0.0238(2) 0.0329(3) 0.0645(3) -0.0068(2) -0.0058(2) -0.00119(17) Mo2 0.0338(2) 0.0410(3) 0.0677(4) -0.0217(2) -0.0060(2) -0.0037(2) Mo3 0.0355(3) 0.0367(3) 0.0647(4) 0.0089(2) -0.0083(2) -0.0041(2) O1 0.0321(18) 0.039(2) 0.060(2) -0.0141(18) -0.0064(17) -0.0066(15) O2 0.0320(19) 0.040(2) 0.074(3) 0.0080(19) -0.0107(18) -0.0005(16) O3 0.0272(19) 0.043(2) 0.083(3) -0.010(2) -0.0082(18) -0.0019(16) O4 0.047(2) 0.060(3) 0.049(2) -0.005(2) -0.0084(18) -0.0127(19) O5 0.0315(18) 0.037(2) 0.059(2) 0.0009(17) -0.0003(17) -0.0071(15) O6 0.0298(18) 0.039(2) 0.074(3) -0.0200(19) -0.0027(17) -0.0009(15) O7 0.0350(19) 0.0285(19) 0.087(3) -0.0070(19) -0.0036(19) -0.0059(15) O8 0.045(2) 0.073(3) 0.096(3) -0.047(3) 0.001(2) -0.010(2) O9 0.048(2) 0.067(3) 0.091(3) 0.027(3) -0.011(2) -0.011(2) O10 0.028(2) 0.023(2) 0.053(3) -0.007(2) -0.008(2) -0.0021(19) C1 0.038(3) 0.040(3) 0.034(3) -0.006(2) -0.005(2) -0.009(2) C2 0.039(3) 0.043(3) 0.036(3) -0.004(2) -0.003(2) -0.010(2) C3 0.041(3) 0.040(3) 0.053(4) -0.010(3) 0.003(3) -0.001(2) C4 0.032(3) 0.059(4) 0.061(4) -0.010(3) 0.000(3) -0.001(3) C5 0.036(3) 0.061(4) 0.052(4) -0.002(3) -0.006(3) -0.018(3) C6 0.038(3) 0.046(3) 0.043(3) -0.002(3) -0.005(2) -0.011(2) C7 0.045(3) 0.049(3) 0.063(4) 0.001(3) -0.012(3) -0.024(3) C8 0.054(4) 0.031(3) 0.081(5) 0.001(3) -0.015(3) -0.006(3) C9 0.040(3) 0.039(3) 0.070(4) 0.004(3) -0.015(3) -0.003(2) C10 0.035(3) 0.036(3) 0.038(3) -0.003(2) -0.009(2) -0.007(2) C11 0.035(3) 0.047(3) 0.033(3) -0.003(2) -0.006(2) -0.006(2) C12 0.032(3) 0.047(3) 0.057(4) 0.000(3) -0.010(2) -0.002(2) C13 0.035(3) 0.066(4) 0.059(4) -0.010(3) -0.011(3) -0.003(3) C14 0.039(3) 0.053(4) 0.057(4) -0.006(3) -0.009(3) -0.016(3) C15 0.049(3) 0.043(3) 0.041(3) -0.006(3) -0.009(3) -0.016(3) C16 0.056(4) 0.051(4) 0.063(4) -0.009(3) 0.001(3) -0.025(3) C17 0.058(4) 0.033(3) 0.092(5) -0.011(3) 0.000(3) -0.016(3) C18 0.049(3) 0.040(3) 0.063(4) -0.016(3) 0.002(3) -0.003(3) C19 0.042(3) 0.036(3) 0.038(3) -0.009(2) -0.003(2) -0.005(2) C20 0.037(3) 0.037(3) 0.031(3) -0.004(2) -0.007(2) -0.005(2) C21 0.056(3) 0.048(3) 0.032(3) 0.000(2) -0.008(3) -0.010(3) C22 0.063(4) 0.044(3) 0.036(3) -0.004(3) -0.010(3) -0.009(3) C23 0.079(5) 0.047(4) 0.056(4) 0.001(3) -0.020(3) -0.011(3) C24 0.069(4) 0.061(4) 0.074(5) -0.001(4) -0.011(4) -0.027(4) C25 0.049(4) 0.082(5) 0.058(4) -0.001(4) -0.008(3) -0.013(3) C26 0.057(4) 0.054(4) 0.043(4) 0.000(3) -0.011(3) -0.010(3) C27 0.058(4) 0.070(5) 0.060(4) -0.002(4) -0.013(3) 0.003(3) C28 0.068(4) 0.053(4) 0.079(5) -0.005(4) -0.010(4) 0.003(3) C29 0.075(4) 0.046(4) 0.064(4) -0.003(3) -0.013(3) -0.010(3) C30 0.058(3) 0.045(3) 0.035(3) -0.005(3) -0.007(3) -0.006(3) C31 0.055(3) 0.054(4) 0.032(3) -0.002(3) -0.008(3) -0.009(3) C32 0.076(4) 0.058(4) 0.046(4) -0.002(3) -0.005(3) -0.018(3) C33 0.060(4) 0.088(5) 0.059(4) -0.002(4) -0.003(3) -0.034(4) C34 0.053(4) 0.101(6) 0.048(4) -0.015(4) -0.004(3) -0.008(4) C35 0.059(4) 0.076(5) 0.045(4) -0.011(3) -0.006(3) -0.004(4) C36 0.051(4) 0.101(6) 0.061(4) -0.019(4) -0.005(3) 0.013(4) C37 0.073(5) 0.072(5) 0.085(5) -0.019(4) -0.016(4) 0.018(4) C38 0.074(5) 0.059(4) 0.071(5) -0.007(4) -0.016(4) 0.000(3) C39 0.058(4) 0.049(4) 0.040(3) -0.004(3) -0.010(3) -0.001(3) C40 0.055(3) 0.062(4) 0.031(3) -0.005(3) -0.009(3) -0.001(3) C41 0.057(4) 0.035(3) 0.064(4) 0.011(3) -0.008(3) -0.013(3) C42 0.060(4) 0.038(3) 0.056(4) 0.004(3) -0.007(3) -0.015(3) C43 0.073(4) 0.045(4) 0.065(4) 0.000(3) -0.009(4) -0.011(3) C44 0.098(6) 0.057(4) 0.057(4) -0.002(3) -0.013(4) -0.020(4) C45 0.079(5) 0.055(4) 0.069(5) 0.020(3) -0.030(4) -0.029(4) C46 0.063(4) 0.049(4) 0.062(4) 0.012(3) -0.020(3) -0.020(3) C47 0.050(4) 0.086(5) 0.089(6) 0.014(4) -0.011(4) -0.015(4) C48 0.050(4) 0.097(6) 0.090(6) 0.010(5) 0.003(4) -0.009(4) C49 0.069(5) 0.074(5) 0.062(4) 0.001(4) 0.003(4) -0.010(4) C50 0.060(4) 0.040(3) 0.067(4) -0.004(3) -0.004(3) -0.009(3) _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 Mo1 O3 1.684(3) . ? Mo1 O1 1.886(3) 1_554 ? Mo1 O5 1.914(4) 2_656 ? Mo1 O2 1.945(4) 1_554 ? Mo1 O6 1.961(4) . ? Mo1 O10 2.3218(12) . ? Mo2 O8 1.668(4) . ? Mo2 O4 1.893(4) . ? Mo2 O6 1.896(3) . ? Mo2 O1 1.958(3) 2_656 ? Mo2 O7 1.961(4) 1_554 ? Mo2 O10 2.3191(9) . ? Mo3 O9 1.668(4) . ? Mo3 O7 1.900(4) . ? Mo3 O2 1.926(4) . ? Mo3 O5 1.937(3) . ? Mo3 O4 1.953(4) 2_656 ? Mo3 O10 2.3184(9) 1_556 ? O1 Mo1 1.886(3) 1_556 ? O1 Mo2 1.958(3) 2_656 ? O2 Mo1 1.945(4) 1_556 ? O4 Mo3 1.953(4) 2_656 ? O5 Mo1 1.914(4) 2_656 ? O7 Mo2 1.961(4) 1_556 ? O10 Mo3 2.3184(9) 2_656 ? O10 Mo3 2.3184(9) 1_554 ? O10 Mo2 2.3190(9) 2_655 ? O10 Mo1 2.3219(12) 2_655 ? C1 C2 1.422(7) . ? C1 C6 1.425(7) . ? C1 C10 1.425(7) . ? C2 C3 1.408(7) . ? C2 C19 1.451(7) . ? C3 C4 1.372(7) . ? C4 C5 1.365(8) . ? C5 C6 1.404(7) . ? C6 C7 1.404(7) . ? C7 C8 1.368(7) . ? C8 C9 1.377(7) . ? C9 C10 1.393(7) . ? C10 C11 1.451(7) . ? C11 C12 1.398(7) . ? C11 C20 1.434(7) . ? C12 C13 1.389(7) . ? C13 C14 1.371(8) . ? C14 C15 1.389(7) . ? C15 C16 1.410(8) . ? C15 C20 1.425(7) . ? C16 C17 1.378(8) . ? C17 C18 1.372(8) . ? C18 C19 1.392(7) . ? C19 C20 1.417(7) . ? C21 C26 1.418(8) . ? C21 C30 1.428(8) . ? C21 C22 1.434(8) . ? C22 C23 1.397(8) . ? C22 C39 1.463(8) . ? C23 C24 1.386(9) . ? C24 C25 1.356(9) . ? C25 C26 1.403(8) . ? C26 C27 1.420(8) . ? C27 C28 1.355(9) . ? C28 C29 1.374(8) . ? C29 C30 1.393(8) . ? C30 C31 1.461(8) . ? C31 C32 1.386(8) . ? C31 C40 1.427(8) . ? C32 C33 1.401(8) . ? C33 C34 1.350(9) . ? C34 C35 1.404(9) . ? C35 C36 1.403(9) . ? C35 C40 1.418(8) . ? C36 C37 1.371(10) . ? C37 C38 1.390(9) . ? C38 C39 1.371(8) . ? C39 C40 1.440(8) . ? C41 C50 1.418(9) . ? C41 C46 1.429(8) . ? C41 C42 1.437(8) . ? C42 C43 1.373(8) . ? C42 C50 1.492(8) 2_556 ? C43 C44 1.397(9) . ? C44 C45 1.355(9) . ? C45 C46 1.400(9) . ? C46 C47 1.402(9) . ? C47 C48 1.346(10) . ? C48 C49 1.407(9) . ? C49 C50 1.384(8) . ? C50 C42 1.492(8) 2_556 ? 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 O3 Mo1 O1 103.87(16) . 1_554 ? O3 Mo1 O5 103.38(17) . 2_656 ? O1 Mo1 O5 88.69(16) 1_554 2_656 ? O3 Mo1 O2 103.05(17) . 1_554 ? O1 Mo1 O2 87.94(16) 1_554 1_554 ? O5 Mo1 O2 153.39(14) 2_656 1_554 ? O3 Mo1 O6 103.06(16) . . ? O1 Mo1 O6 153.06(14) 1_554 . ? O5 Mo1 O6 85.63(15) 2_656 . ? O2 Mo1 O6 85.51(16) 1_554 . ? O3 Mo1 O10 178.91(13) . . ? O1 Mo1 O10 77.21(10) 1_554 . ? O5 Mo1 O10 76.62(10) 2_656 . ? O2 Mo1 O10 76.89(10) 1_554 . ? O6 Mo1 O10 75.85(10) . . ? O8 Mo2 O4 104.4(2) . . ? O8 Mo2 O6 104.23(17) . . ? O4 Mo2 O6 89.66(16) . . ? O8 Mo2 O1 102.61(17) . 2_656 ? O4 Mo2 O1 86.64(15) . 2_656 ? O6 Mo2 O1 152.99(15) . 2_656 ? O8 Mo2 O7 102.3(2) . 1_554 ? O4 Mo2 O7 153.18(15) . 1_554 ? O6 Mo2 O7 86.81(16) . 1_554 ? O1 Mo2 O7 84.58(15) 2_656 1_554 ? O8 Mo2 O10 177.79(16) . . ? O4 Mo2 O10 77.32(12) . . ? O6 Mo2 O10 77.10(11) . . ? O1 Mo2 O10 75.98(10) 2_656 . ? O7 Mo2 O10 75.98(11) 1_554 . ? O9 Mo3 O7 103.5(2) . . ? O9 Mo3 O2 103.53(17) . . ? O7 Mo3 O2 88.47(16) . . ? O9 Mo3 O5 102.84(17) . . ? O7 Mo3 O5 87.69(15) . . ? O2 Mo3 O5 153.53(15) . . ? O9 Mo3 O4 103.2(2) . 2_656 ? O7 Mo3 O4 153.35(16) . 2_656 ? O2 Mo3 O4 86.03(15) . 2_656 ? O5 Mo3 O4 85.76(15) . 2_656 ? O9 Mo3 O10 178.98(16) . 1_556 ? O7 Mo3 O10 77.11(11) . 1_556 ? O2 Mo3 O10 77.31(11) . 1_556 ? O5 Mo3 O10 76.30(11) . 1_556 ? O4 Mo3 O10 76.24(11) 2_656 1_556 ? Mo1 O1 Mo2 116.95(17) 1_556 2_656 ? Mo3 O2 Mo1 115.84(17) . 1_556 ? Mo2 O4 Mo3 116.64(19) . 2_656 ? Mo1 O5 Mo3 116.91(17) 2_656 . ? Mo2 O6 Mo1 116.84(17) . . ? Mo3 O7 Mo2 116.65(17) . 1_556 ? Mo3 O10 Mo3 180.0 2_656 1_554 ? Mo3 O10 Mo2 90.23(4) 2_656 2_655 ? Mo3 O10 Mo2 89.77(4) 1_554 2_655 ? Mo3 O10 Mo2 89.77(4) 2_656 . ? Mo3 O10 Mo2 90.23(4) 1_554 . ? Mo2 O10 Mo2 179.999(1) 2_655 . ? Mo3 O10 Mo1 90.04(4) 2_656 . ? Mo3 O10 Mo1 89.96(4) 1_554 . ? Mo2 O10 Mo1 89.84(4) 2_655 . ? Mo2 O10 Mo1 90.16(3) . . ? Mo3 O10 Mo1 89.96(4) 2_656 2_655 ? Mo3 O10 Mo1 90.04(4) 1_554 2_655 ? Mo2 O10 Mo1 90.16(4) 2_655 2_655 ? Mo2 O10 Mo1 89.84(3) . 2_655 ? Mo1 O10 Mo1 180.0 . 2_655 ? C2 C1 C6 119.1(5) . . ? C2 C1 C10 121.4(4) . . ? C6 C1 C10 119.5(5) . . ? C3 C2 C1 118.2(5) . . ? C3 C2 C19 122.7(5) . . ? C1 C2 C19 119.1(4) . . ? C4 C3 C2 122.0(5) . . ? C5 C4 C3 120.4(5) . . ? C4 C5 C6 120.9(5) . . ? C5 C6 C7 121.4(5) . . ? C5 C6 C1 119.5(5) . . ? C7 C6 C1 119.1(5) . . ? C8 C7 C6 121.0(5) . . ? C7 C8 C9 119.9(5) . . ? C8 C9 C10 122.6(5) . . ? C9 C10 C1 117.8(4) . . ? C9 C10 C11 122.5(4) . . ? C1 C10 C11 119.6(4) . . ? C12 C11 C20 118.8(5) . . ? C12 C11 C10 122.4(5) . . ? C20 C11 C10 118.8(4) . . ? C13 C12 C11 121.5(5) . . ? C14 C13 C12 120.1(5) . . ? C13 C14 C15 120.9(5) . . ? C14 C15 C16 121.4(5) . . ? C14 C15 C20 120.5(5) . . ? C16 C15 C20 118.1(5) . . ? C17 C16 C15 121.3(5) . . ? C18 C17 C16 119.5(5) . . ? C17 C18 C19 123.0(5) . . ? C18 C19 C20 117.7(5) . . ? C18 C19 C2 122.6(5) . . ? C20 C19 C2 119.8(5) . . ? C19 C20 C15 120.5(5) . . ? C19 C20 C11 121.3(4) . . ? C15 C20 C11 118.2(4) . . ? C26 C21 C30 119.5(5) . . ? C26 C21 C22 119.1(5) . . ? C30 C21 C22 121.4(5) . . ? C23 C22 C21 118.3(5) . . ? C23 C22 C39 122.6(5) . . ? C21 C22 C39 119.1(5) . . ? C24 C23 C22 121.7(6) . . ? C25 C24 C23 120.0(6) . . ? C24 C25 C26 121.7(6) . . ? C25 C26 C21 119.1(6) . . ? C25 C26 C27 121.5(6) . . ? C21 C26 C27 119.4(6) . . ? C28 C27 C26 119.5(6) . . ? C27 C28 C29 122.0(6) . . ? C28 C29 C30 121.4(6) . . ? C29 C30 C21 118.2(5) . . ? C29 C30 C31 122.4(5) . . ? C21 C30 C31 119.4(5) . . ? C32 C31 C40 117.9(6) . . ? C32 C31 C30 122.3(5) . . ? C40 C31 C30 119.7(5) . . ? C31 C32 C33 122.0(6) . . ? C34 C33 C32 119.9(6) . . ? C33 C34 C35 121.3(6) . . ? C36 C35 C34 121.4(7) . . ? C36 C35 C40 119.5(6) . . ? C34 C35 C40 119.2(6) . . ? C37 C36 C35 120.5(6) . . ? C36 C37 C38 120.0(7) . . ? C39 C38 C37 122.7(7) . . ? C38 C39 C40 117.8(6) . . ? C38 C39 C22 122.7(6) . . ? C40 C39 C22 119.5(5) . . ? C35 C40 C31 119.7(6) . . ? C35 C40 C39 119.5(6) . . ? C31 C40 C39 120.9(5) . . ? C50 C41 C46 119.8(6) . . ? C50 C41 C42 121.8(5) . . ? C46 C41 C42 118.4(6) . . ? C43 C42 C41 119.3(6) . . ? C43 C42 C50 122.5(6) . 2_556 ? C41 C42 C50 118.2(5) . 2_556 ? C42 C43 C44 121.4(7) . . ? C45 C44 C43 120.2(7) . . ? C44 C45 C46 121.5(6) . . ? C45 C46 C47 122.1(6) . . ? C45 C46 C41 119.1(6) . . ? C47 C46 C41 118.7(6) . . ? C48 C47 C46 121.3(7) . . ? C47 C48 C49 120.4(7) . . ? C50 C49 C48 121.4(7) . . ? C49 C50 C41 118.4(6) . . ? C49 C50 C42 121.6(6) . 2_556 ? C41 C50 C42 120.0(5) . 2_556 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.535 _refine_diff_density_min -0.376 _refine_diff_density_rms 0.097 #===END data_(per)5[VW5O19] (3) _database_code_CSD 161774 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H30 O9.50 V0.50 W2.50' _chemical_formula_weight 1267.83 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' 'V' 'V' 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9272(9) _cell_length_b 12.7077(11) _cell_length_c 13.5723(12) _cell_angle_alpha 82.1386(19) _cell_angle_beta 83.3466(18) _cell_angle_gamma 81.4233(18) _cell_volume 1837.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.292 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1205 _exptl_absorpt_coefficient_mu 8.001 _exptl_absorpt_correction_type 'multi-scan (SADABS; Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.3269 _exptl_absorpt_correction_T_max 0.3799 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD area detector diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21636 _diffrn_reflns_av_R_equivalents 0.0553 _diffrn_reflns_av_sigmaI/netI 0.1203 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 30.59 _reflns_number_total 10746 _reflns_number_gt 6201 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0786P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00100(16) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 10746 _refine_ls_number_parameters 567 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1128 _refine_ls_R_factor_gt 0.0562 _refine_ls_wR_factor_ref 0.1432 _refine_ls_wR_factor_gt 0.1272 _refine_ls_goodness_of_fit_ref 0.906 _refine_ls_restrained_S_all 0.906 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.99425(4) -0.13323(3) -0.09819(3) 0.02274(12) Uani 0.83 1 d P . . V1 V 0.99425(4) -0.13323(3) -0.09819(3) 0.02274(12) Uani 0.17 1 d P . . W2 W 0.78598(4) 0.02934(3) 0.01862(4) 0.02806(13) Uani 0.83 1 d P . . V2 V 0.78598(4) 0.02934(3) 0.01862(4) 0.02806(13) Uani 0.17 1 d P . . W3 W 0.99799(4) -0.12417(3) 0.14120(3) 0.02516(12) Uani 0.83 1 d P . . V3 V 0.99799(4) -0.12417(3) 0.14120(3) 0.02516(12) Uani 0.17 1 d P . . O1 O 1.1700(5) -0.1326(5) -0.0922(5) 0.0282(15) Uani 1 1 d . . . O2 O 0.9934(6) -0.2092(5) 0.0348(5) 0.0297(15) Uani 1 1 d . . . O3 O 0.9891(7) -0.2319(6) -0.1679(6) 0.0441(19) Uani 1 1 d . . . O4 O 1.1721(6) -0.1237(5) 0.0997(5) 0.0279(15) Uani 1 1 d . . . O5 O 1.0012(6) 0.0064(5) 0.1929(5) 0.0291(15) Uani 1 1 d . . . O6 O 0.8211(5) -0.0839(5) -0.0646(5) 0.0250(14) Uani 1 1 d . . . O7 O 0.8243(5) -0.0745(5) 0.1281(5) 0.0256(14) Uani 1 1 d . . . O8 O 0.6296(6) 0.0498(5) 0.0325(5) 0.0349(17) Uani 1 1 d . . . O9 O 0.9949(7) -0.2160(6) 0.2435(6) 0.0428(19) Uani 1 1 d . . . O10 O 1.0000 0.0000 0.0000 0.0197(18) Uani 1 2 d S . . C1 C 0.4004(8) 0.4362(7) -0.1069(7) 0.0234(19) Uani 1 1 d . . . C2 C 1.3787(8) -0.4523(7) -0.1084(7) 0.0237(19) Uani 1 1 d . . . C3 C 1.2545(8) -0.4019(8) -0.0923(7) 0.029(2) Uani 1 1 d . . . H3 H 1.2392 -0.3277 -0.0937 0.058(7) Uiso 1 1 calc R . . C4 C 0.8435(9) -0.5398(8) 0.0746(8) 0.035(2) Uani 1 1 d . . . H4 H 0.9240 -0.5746 0.0630 0.058(7) Uiso 1 1 calc R . . C5 C 0.8235(9) -0.4299(8) 0.0738(8) 0.033(2) Uani 1 1 d . . . H5 H 0.8909 -0.3915 0.0629 0.058(7) Uiso 1 1 calc R . . C6 C 0.7024(8) -0.3750(8) 0.0893(7) 0.027(2) Uani 1 1 d . . . C7 C 0.6832(8) -0.2636(7) 0.0842(7) 0.029(2) Uani 1 1 d . . . H7 H 0.7501 -0.2246 0.0707 0.058(7) Uiso 1 1 calc R . . C8 C 0.4369(10) 0.2119(8) -0.0994(8) 0.033(2) Uani 1 1 d . . . H8 H 0.4495 0.1378 -0.0986 0.058(7) Uiso 1 1 calc R . . C9 C 0.5373(9) 0.2662(7) -0.1157(7) 0.029(2) Uani 1 1 d . . . H9 H 0.6169 0.2285 -0.1236 0.058(7) Uiso 1 1 calc R . . C10 C 0.5220(8) 0.3794(7) -0.1207(7) 0.0220(18) Uani 1 1 d . . . C11 C 0.6244(8) -0.5578(7) -0.1375(7) 0.0232(19) Uani 1 1 d . . . C12 C 0.7487(8) -0.6103(8) -0.1501(7) 0.029(2) Uani 1 1 d . . . H12 H 0.7636 -0.6847 -0.1460 0.058(7) Uiso 1 1 calc R . . C13 C 0.8484(9) -0.5511(8) -0.1686(8) 0.036(2) Uani 1 1 d . . . H13 H 0.9290 -0.5861 -0.1785 0.058(7) Uiso 1 1 calc R . . C14 C 0.8286(8) -0.4424(8) -0.1724(8) 0.032(2) Uani 1 1 d . . . H14 H 0.8960 -0.4039 -0.1838 0.058(7) Uiso 1 1 calc R . . C15 C 0.7072(8) -0.3874(7) -0.1592(7) 0.027(2) Uani 1 1 d . . . C16 C 0.6866(9) -0.2754(8) -0.1615(8) 0.035(2) Uani 1 1 d . . . H16 H 0.7533 -0.2362 -0.1738 0.058(7) Uiso 1 1 calc R . . C17 C 0.5664(10) -0.2237(8) -0.1453(8) 0.040(3) Uani 1 1 d . . . H17 H 0.5536 -0.1496 -0.1458 0.058(7) Uiso 1 1 calc R . . C18 C 1.4672(9) -0.2781(8) -0.1286(7) 0.031(2) Uani 1 1 d . . . H18 H 1.3877 -0.2409 -0.1182 0.058(7) Uiso 1 1 calc R . . C19 C 1.4826(8) -0.3909(7) -0.1270(7) 0.025(2) Uani 1 1 d . . . C20 C 0.6037(8) -0.4481(7) -0.1415(6) 0.0205(18) Uani 1 1 d . . . C21 C 0.6483(12) -0.4959(9) -0.3965(8) 0.043(3) Uani 1 1 d . . . C22 C 0.5863(13) -0.3906(10) -0.3948(8) 0.048(3) Uani 1 1 d . . . C23 C 0.6578(16) -0.3080(10) -0.4074(9) 0.060(4) Uani 1 1 d . . . H23 H 0.6183 -0.2382 -0.4047 0.058(7) Uiso 1 1 calc R . . C24 C 0.7841(17) -0.3249(14) -0.4236(11) 0.078(5) Uani 1 1 d . . . H24 H 0.8295 -0.2674 -0.4341 0.058(7) Uiso 1 1 calc R . . C25 C 0.8434(16) -0.4280(13) -0.4244(10) 0.072(4) Uani 1 1 d . . . H25 H 0.9297 -0.4403 -0.4353 0.058(7) Uiso 1 1 calc R . . C26 C 0.7749(13) -0.5147(10) -0.4088(9) 0.051(3) Uani 1 1 d . . . C27 C 0.8373(14) -0.6203(12) -0.4076(9) 0.065(4) Uani 1 1 d . . . H27 H 0.9237 -0.6326 -0.4155 0.058(7) Uiso 1 1 calc R . . C28 C 0.7698(14) 0.2953(11) -0.3945(10) 0.061(4) Uani 1 1 d . . . H28 H 0.8106 0.2256 -0.3936 0.058(7) Uiso 1 1 calc R . . C29 C 0.6417(13) 0.3133(10) -0.3829(9) 0.050(3) Uani 1 1 d . . . H29 H 0.5974 0.2551 -0.3750 0.058(7) Uiso 1 1 calc R . . C30 C 0.5776(11) 0.4157(9) -0.3827(8) 0.041(3) Uani 1 1 d . . . C31 C 0.4426(12) 0.4342(9) -0.3664(8) 0.043(3) Uani 1 1 d . . . C32 C 0.3682(12) 0.3532(10) -0.3539(9) 0.050(3) Uani 1 1 d . . . H32 H 0.4069 0.2836 -0.3589 0.058(7) Uiso 1 1 calc R . . C33 C 0.2428(14) 0.3688(13) -0.3349(11) 0.068(4) Uani 1 1 d . . . H33 H 0.1966 0.3118 -0.3262 0.058(7) Uiso 1 1 calc R . . C34 C 1.1873(15) -0.5293(14) -0.3291(10) 0.075(5) Uani 1 1 d . . . H34 H 1.1011 -0.5179 -0.3167 0.058(7) Uiso 1 1 calc R . . C35 C 1.2512(15) -0.4394(12) -0.3405(10) 0.063(4) Uani 1 1 d . . . C36 C 1.1908(16) -0.3363(15) -0.3348(10) 0.078(5) Uani 1 1 d . . . H36 H 1.1047 -0.3247 -0.3216 0.058(7) Uiso 1 1 calc R . . C37 C 1.257(2) -0.2526(13) -0.3482(12) 0.085(5) Uani 1 1 d . . . H37 H 1.2156 -0.1833 -0.3448 0.058(7) Uiso 1 1 calc R . . C38 C 1.3803(17) -0.2690(10) -0.3664(10) 0.067(4) Uani 1 1 d . . . H38 H 1.4232 -0.2101 -0.3732 0.058(7) Uiso 1 1 calc R . . C39 C 1.4487(15) -0.3696(10) -0.3756(8) 0.055(4) Uani 1 1 d . . . C40 C 1.3808(13) -0.4579(10) -0.3618(8) 0.048(3) Uani 1 1 d . . . C41 C 0.6142(10) -0.0047(8) -0.4587(8) 0.036(2) Uani 1 1 d . . . C42 C 0.4983(10) -0.0191(8) 0.3971(8) 0.036(2) Uani 1 1 d . . . C43 C 0.5055(11) 0.0360(9) -0.3012(8) 0.043(3) Uani 1 1 d . . . H43 H 0.4312 0.0527 -0.2621 0.058(7) Uiso 1 1 calc R . . C44 C 0.6184(12) 0.0290(9) -0.2591(9) 0.048(3) Uani 1 1 d . . . H44 H 0.6181 0.0408 -0.1929 0.058(7) Uiso 1 1 calc R . . C45 C 0.7255(12) 0.0057(9) -0.3135(10) 0.053(3) Uani 1 1 d . . . H45 H 0.7992 0.0021 -0.2844 0.058(7) Uiso 1 1 calc R . . C46 C 0.7317(12) -0.0143(10) -0.4156(9) 0.048(3) Uani 1 1 d . . . C47 C 0.8415(12) -0.0424(11) -0.4742(11) 0.059(4) Uani 1 1 d . . . H47 H 0.9162 -0.0506 -0.4455 0.058(7) Uiso 1 1 calc R . . C48 C 0.8450(13) -0.0583(13) 0.4306(12) 0.072(4) Uani 1 1 d . . . H48 H 0.9208 -0.0731 0.3929 0.058(7) Uiso 1 1 calc R . . C49 C 0.7322(12) -0.0523(12) 0.3872(10) 0.061(4) Uani 1 1 d . . . H49 H 0.7346 -0.0665 0.3216 0.058(7) Uiso 1 1 calc R . . C50 C 0.6139(10) -0.0249(9) 0.4425(8) 0.037(2) 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 W1 0.01128(18) 0.0196(2) 0.0389(3) -0.01153(18) -0.00139(17) -0.00070(14) V1 0.01128(18) 0.0196(2) 0.0389(3) -0.01153(18) -0.00139(17) -0.00070(14) W2 0.01112(19) 0.0248(2) 0.0476(3) -0.00601(19) -0.00271(18) 0.00103(16) V2 0.01112(19) 0.0248(2) 0.0476(3) -0.00601(19) -0.00271(18) 0.00103(16) W3 0.01369(19) 0.0228(2) 0.0368(3) 0.00193(18) -0.00318(17) -0.00027(15) V3 0.01369(19) 0.0228(2) 0.0368(3) 0.00193(18) -0.00318(17) -0.00027(15) O1 0.013(3) 0.023(3) 0.050(4) -0.010(3) -0.004(3) 0.000(2) O2 0.020(3) 0.016(3) 0.051(4) -0.001(3) -0.005(3) -0.001(2) O3 0.026(4) 0.043(4) 0.068(6) -0.027(4) 0.004(4) -0.009(3) O4 0.016(3) 0.023(3) 0.043(4) 0.002(3) -0.005(3) 0.001(2) O5 0.025(3) 0.032(4) 0.030(4) -0.003(3) -0.002(3) -0.003(3) O6 0.012(3) 0.023(3) 0.040(4) -0.006(3) 0.000(3) -0.002(2) O7 0.008(3) 0.026(3) 0.041(4) -0.002(3) 0.001(3) 0.000(2) O8 0.015(3) 0.031(4) 0.060(5) -0.009(3) -0.003(3) -0.003(3) O9 0.025(4) 0.045(4) 0.055(5) 0.005(4) -0.002(3) -0.005(3) O10 0.018(4) 0.019(4) 0.022(5) -0.004(3) -0.003(3) 0.001(3) C1 0.014(4) 0.027(5) 0.029(5) -0.007(4) -0.008(4) 0.004(3) C2 0.016(4) 0.028(5) 0.029(5) -0.009(4) -0.005(4) 0.000(4) C3 0.013(4) 0.030(5) 0.040(6) -0.002(4) -0.001(4) 0.005(4) C4 0.011(4) 0.043(6) 0.050(7) -0.013(5) 0.005(4) 0.003(4) C5 0.017(4) 0.032(5) 0.050(7) 0.003(5) -0.003(4) -0.006(4) C6 0.017(4) 0.036(5) 0.030(5) -0.005(4) -0.002(4) -0.006(4) C7 0.019(4) 0.033(5) 0.035(6) -0.002(4) -0.006(4) -0.007(4) C8 0.039(6) 0.022(5) 0.039(6) -0.001(4) -0.007(5) -0.003(4) C9 0.028(5) 0.024(5) 0.035(6) 0.001(4) -0.008(4) 0.000(4) C10 0.013(4) 0.026(4) 0.025(5) -0.003(4) -0.004(3) 0.005(3) C11 0.012(4) 0.033(5) 0.023(5) -0.001(4) -0.002(3) -0.002(3) C12 0.013(4) 0.031(5) 0.042(6) -0.005(4) -0.004(4) 0.001(4) C13 0.015(4) 0.041(6) 0.052(7) -0.002(5) -0.001(4) -0.005(4) C14 0.015(4) 0.036(5) 0.046(6) -0.005(5) 0.001(4) -0.009(4) C15 0.016(4) 0.033(5) 0.032(5) -0.006(4) 0.004(4) -0.007(4) C16 0.024(5) 0.036(6) 0.047(7) -0.007(5) 0.001(5) -0.009(4) C17 0.041(6) 0.020(5) 0.059(8) -0.011(5) 0.003(5) -0.009(4) C18 0.022(5) 0.034(5) 0.039(6) -0.013(4) -0.001(4) -0.003(4) C19 0.017(4) 0.030(5) 0.026(5) -0.001(4) 0.001(4) -0.001(4) C20 0.015(4) 0.025(4) 0.021(5) -0.002(4) -0.003(3) -0.003(3) C21 0.061(8) 0.041(6) 0.028(6) -0.001(5) -0.010(5) -0.009(6) C22 0.070(9) 0.045(7) 0.032(6) 0.002(5) -0.011(6) -0.019(6) C23 0.094(12) 0.045(7) 0.043(8) -0.002(6) -0.011(8) -0.014(7) C24 0.094(13) 0.074(11) 0.075(11) 0.000(8) 0.000(9) -0.060(10) C25 0.071(11) 0.092(12) 0.055(9) 0.001(8) -0.008(8) -0.031(9) C26 0.060(8) 0.057(8) 0.038(7) 0.009(6) -0.012(6) -0.023(7) C27 0.056(9) 0.087(11) 0.045(8) 0.000(7) -0.003(7) 0.004(8) C28 0.059(9) 0.052(8) 0.069(10) -0.006(7) -0.012(7) 0.008(7) C29 0.063(9) 0.045(7) 0.043(7) -0.004(5) -0.007(6) -0.012(6) C30 0.051(7) 0.048(7) 0.024(6) -0.002(5) -0.006(5) -0.008(6) C31 0.055(8) 0.044(6) 0.027(6) -0.005(5) -0.004(5) 0.003(6) C32 0.052(8) 0.054(7) 0.042(7) -0.001(6) -0.001(6) -0.012(6) C33 0.054(9) 0.081(11) 0.071(10) -0.005(8) 0.011(7) -0.030(8) C34 0.057(9) 0.108(14) 0.045(9) 0.000(8) 0.017(7) 0.008(9) C35 0.076(11) 0.066(9) 0.039(8) -0.011(7) 0.007(7) 0.007(8) C36 0.066(11) 0.111(14) 0.048(9) -0.021(9) -0.003(7) 0.027(10) C37 0.111(16) 0.054(10) 0.080(12) -0.013(8) -0.009(11) 0.025(10) C38 0.105(14) 0.039(7) 0.054(9) -0.013(6) -0.014(8) 0.013(8) C39 0.094(11) 0.040(7) 0.027(6) 0.003(5) -0.011(7) 0.000(7) C40 0.065(9) 0.056(8) 0.018(6) -0.005(5) 0.004(5) 0.000(6) C41 0.033(6) 0.042(6) 0.034(6) -0.006(5) 0.002(5) -0.015(5) C42 0.038(6) 0.028(5) 0.041(7) 0.001(5) -0.004(5) -0.010(4) C43 0.042(7) 0.052(7) 0.036(7) -0.004(5) -0.005(5) -0.007(5) C44 0.048(7) 0.050(7) 0.046(8) -0.011(6) -0.010(6) -0.004(6) C45 0.053(8) 0.042(7) 0.072(9) 0.005(6) -0.035(7) -0.018(6) C46 0.048(7) 0.054(7) 0.045(7) 0.000(6) -0.019(6) -0.012(6) C47 0.033(7) 0.084(10) 0.061(9) 0.001(7) -0.012(6) -0.019(6) C48 0.032(7) 0.110(13) 0.079(11) -0.015(9) -0.005(7) -0.021(8) C49 0.037(7) 0.094(11) 0.051(8) -0.017(7) 0.013(6) -0.010(7) C50 0.033(6) 0.043(6) 0.034(6) -0.005(5) 0.003(5) -0.003(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 W1 O3 1.683(7) . ? W1 O5 1.922(6) 2_755 ? W1 O6 1.925(6) . ? W1 O2 1.926(7) . ? W1 O1 1.933(6) . ? W1 O10 2.3053(4) . ? W2 O8 1.683(6) . ? W2 O7 1.889(6) . ? W2 O1 1.900(6) 2_755 ? W2 O6 1.916(6) . ? W2 O4 1.922(6) 2_755 ? W2 O10 2.3023(4) . ? W3 O9 1.688(7) . ? W3 O5 1.894(6) . ? W3 O4 1.921(6) . ? W3 O2 1.928(7) . ? W3 O7 1.929(6) . ? W3 O10 2.3100(5) . ? O1 V2 1.900(6) 2_755 ? O1 W2 1.900(6) 2_755 ? O4 V2 1.922(6) 2_755 ? O4 W2 1.922(6) 2_755 ? O5 V1 1.922(6) 2_755 ? O5 W1 1.922(6) 2_755 ? O10 V2 2.3023(4) 2_755 ? O10 W2 2.3023(4) 2_755 ? O10 V1 2.3053(4) 2_755 ? O10 W1 2.3053(4) 2_755 ? O10 V3 2.3100(5) 2_755 ? O10 W3 2.3100(5) 2_755 ? C1 C2 1.400(12) 1_465 ? C1 C10 1.420(11) . ? C1 C6 1.440(12) 2_655 ? C2 C1 1.400(12) 1_645 ? C2 C3 1.418(12) . ? C2 C19 1.451(12) . ? C3 C4 1.372(13) 2_745 ? C4 C3 1.372(13) 2_745 ? C4 C5 1.380(13) . ? C5 C6 1.408(13) . ? C6 C7 1.392(13) . ? C6 C1 1.440(12) 2_655 ? C7 C8 1.384(13) 2_655 ? C8 C9 1.363(13) . ? C8 C7 1.384(13) 2_655 ? C9 C10 1.415(12) . ? C10 C11 1.448(12) 1_565 ? C11 C20 1.374(12) . ? C11 C12 1.424(12) . ? C11 C10 1.448(12) 1_545 ? C12 C13 1.395(13) . ? C13 C14 1.361(14) . ? C14 C15 1.408(12) . ? C15 C16 1.403(13) . ? C15 C20 1.442(12) . ? C16 C17 1.386(14) . ? C17 C18 1.353(14) 1_455 ? C18 C17 1.353(14) 1_655 ? C18 C19 1.415(13) . ? C19 C20 1.418(12) 1_655 ? C20 C19 1.418(12) 1_455 ? C21 C26 1.363(17) . ? C21 C22 1.409(16) . ? C21 C30 1.436(16) 1_545 ? C22 C23 1.380(17) . ? C22 C39 1.487(19) 1_455 ? C23 C24 1.36(2) . ? C24 C25 1.37(2) . ? C25 C26 1.402(18) . ? C26 C27 1.411(19) . ? C27 C28 1.370(19) 1_545 ? C28 C27 1.370(19) 1_565 ? C28 C29 1.378(18) . ? C29 C30 1.384(16) . ? C30 C21 1.436(16) 1_565 ? C30 C31 1.454(16) . ? C31 C32 1.385(17) . ? C31 C40 1.441(16) 1_465 ? C32 C33 1.355(18) . ? C33 C34 1.35(2) 1_465 ? C34 C33 1.35(2) 1_645 ? C34 C35 1.41(2) . ? C35 C36 1.38(2) . ? C35 C40 1.403(19) . ? C36 C37 1.35(2) . ? C37 C38 1.34(2) . ? C38 C39 1.395(17) . ? C39 C40 1.416(18) . ? C39 C22 1.487(19) 1_655 ? C40 C31 1.441(16) 1_645 ? C41 C50 1.400(14) 1_554 ? C41 C42 1.422(14) 2_655 ? C41 C46 1.454(15) . ? C42 C43 1.354(14) 2_655 ? C42 C41 1.421(14) 2_655 ? C42 C50 1.457(14) . ? C43 C42 1.354(14) 2_655 ? C43 C44 1.406(16) . ? C44 C45 1.326(17) . ? C45 C46 1.435(17) . ? C46 C47 1.388(18) . ? C47 C48 1.331(18) 1_554 ? C48 C47 1.331(18) 1_556 ? C48 C49 1.414(18) . ? C49 C50 1.438(15) . ? C50 C41 1.400(14) 1_556 ? 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 O3 W1 O5 104.6(3) . 2_755 ? O3 W1 O6 102.8(3) . . ? O5 W1 O6 87.6(3) 2_755 . ? O3 W1 O2 102.2(3) . . ? O5 W1 O2 153.2(3) 2_755 . ? O6 W1 O2 86.8(3) . . ? O3 W1 O1 103.9(3) . . ? O5 W1 O1 87.0(3) 2_755 . ? O6 W1 O1 153.3(3) . . ? O2 W1 O1 86.3(3) . . ? O3 W1 O10 178.9(3) . . ? O5 W1 O10 76.41(19) 2_755 . ? O6 W1 O10 76.86(18) . . ? O2 W1 O10 76.83(18) . . ? O1 W1 O10 76.43(18) . . ? O8 W2 O7 102.6(3) . . ? O8 W2 O1 103.2(3) . 2_755 ? O7 W2 O1 87.5(3) . 2_755 ? O8 W2 O6 102.6(3) . . ? O7 W2 O6 87.8(3) . . ? O1 W2 O6 154.2(2) 2_755 . ? O8 W2 O4 103.6(3) . 2_755 ? O7 W2 O4 153.9(2) . 2_755 ? O1 W2 O4 86.8(3) 2_755 2_755 ? O6 W2 O4 86.3(3) . 2_755 ? O8 W2 O10 179.6(2) . . ? O7 W2 O10 77.09(17) . . ? O1 W2 O10 77.12(18) 2_755 . ? O6 W2 O10 77.09(17) . . ? O4 W2 O10 76.76(18) 2_755 . ? O9 W3 O5 104.0(3) . . ? O9 W3 O4 104.0(3) . . ? O5 W3 O4 87.2(3) . . ? O9 W3 O2 102.5(3) . . ? O5 W3 O2 153.5(3) . . ? O4 W3 O2 87.3(3) . . ? O9 W3 O7 103.3(3) . . ? O5 W3 O7 86.0(3) . . ? O4 W3 O7 152.7(3) . . ? O2 W3 O7 87.0(3) . . ? O9 W3 O10 179.0(3) . . ? O5 W3 O10 76.79(19) . . ? O4 W3 O10 76.58(18) . . ? O2 W3 O10 76.68(18) . . ? O7 W3 O10 76.16(19) . . ? V2 O1 W2 0.00(3) 2_755 2_755 ? V2 O1 W1 116.4(3) 2_755 . ? W2 O1 W1 116.4(3) 2_755 . ? W1 O2 W3 116.2(3) . . ? W3 O4 V2 116.4(3) . 2_755 ? W3 O4 W2 116.4(3) . 2_755 ? V2 O4 W2 0.00(4) 2_755 2_755 ? W3 O5 V1 117.1(3) . 2_755 ? W3 O5 W1 117.1(3) . 2_755 ? V1 O5 W1 0.00(4) 2_755 2_755 ? W2 O6 W1 116.0(3) . . ? W2 O7 W3 117.0(3) . . ? V2 O10 W2 0.00(3) 2_755 2_755 ? V2 O10 W2 180.0 2_755 . ? W2 O10 W2 180.0 2_755 . ? V2 O10 V1 90.016(15) 2_755 2_755 ? W2 O10 V1 90.016(15) 2_755 2_755 ? W2 O10 V1 89.986(15) . 2_755 ? V2 O10 W1 90.016(15) 2_755 2_755 ? W2 O10 W1 90.016(15) 2_755 2_755 ? W2 O10 W1 89.986(15) . 2_755 ? V1 O10 W1 0.00(3) 2_755 2_755 ? V2 O10 W1 89.984(15) 2_755 . ? W2 O10 W1 89.984(15) 2_755 . ? W2 O10 W1 90.014(15) . . ? V1 O10 W1 180.0 2_755 . ? W1 O10 W1 180.0 2_755 . ? V2 O10 V3 89.787(16) 2_755 2_755 ? W2 O10 V3 89.787(16) 2_755 2_755 ? W2 O10 V3 90.213(16) . 2_755 ? V1 O10 V3 90.297(17) 2_755 2_755 ? W1 O10 V3 90.297(17) 2_755 2_755 ? W1 O10 V3 89.703(17) . 2_755 ? V2 O10 W3 89.787(16) 2_755 2_755 ? W2 O10 W3 89.787(16) 2_755 2_755 ? W2 O10 W3 90.213(16) . 2_755 ? V1 O10 W3 90.297(17) 2_755 2_755 ? W1 O10 W3 90.297(17) 2_755 2_755 ? W1 O10 W3 89.703(17) . 2_755 ? V3 O10 W3 0.00(2) 2_755 2_755 ? V2 O10 W3 90.214(16) 2_755 . ? W2 O10 W3 90.214(16) 2_755 . ? W2 O10 W3 89.787(16) . . ? V1 O10 W3 89.702(17) 2_755 . ? W1 O10 W3 89.702(17) 2_755 . ? W1 O10 W3 90.298(18) . . ? V3 O10 W3 180.0 2_755 . ? W3 O10 W3 180.0 2_755 . ? C2 C1 C10 122.3(8) 1_465 . ? C2 C1 C6 120.0(8) 1_465 2_655 ? C10 C1 C6 117.8(8) . 2_655 ? C1 C2 C3 118.7(8) 1_645 . ? C1 C2 C19 119.7(8) 1_645 . ? C3 C2 C19 121.5(8) . . ? C4 C3 C2 121.4(9) 2_745 . ? C3 C4 C5 120.5(9) 2_745 . ? C4 C5 C6 120.9(9) . . ? C7 C6 C5 120.3(8) . . ? C7 C6 C1 121.2(8) . 2_655 ? C5 C6 C1 118.5(9) . 2_655 ? C8 C7 C6 118.9(9) 2_655 . ? C9 C8 C7 122.0(9) . 2_655 ? C8 C9 C10 120.8(9) . . ? C9 C10 C1 119.2(8) . . ? C9 C10 C11 123.8(8) . 1_565 ? C1 C10 C11 117.0(8) . 1_565 ? C20 C11 C12 119.2(8) . . ? C20 C11 C10 121.1(8) . 1_545 ? C12 C11 C10 119.7(8) . 1_545 ? C13 C12 C11 120.6(9) . . ? C14 C13 C12 120.5(9) . . ? C13 C14 C15 120.8(9) . . ? C16 C15 C14 120.9(8) . . ? C16 C15 C20 120.2(8) . . ? C14 C15 C20 118.9(8) . . ? C17 C16 C15 119.7(9) . . ? C18 C17 C16 121.7(9) 1_455 . ? C17 C18 C19 120.9(9) 1_655 . ? C18 C19 C20 119.7(8) . 1_655 ? C18 C19 C2 122.6(8) . . ? C20 C19 C2 117.6(8) 1_655 . ? C11 C20 C19 122.2(8) . 1_455 ? C11 C20 C15 120.0(8) . . ? C19 C20 C15 117.8(8) 1_455 . ? C26 C21 C22 120.5(11) . . ? C26 C21 C30 119.8(11) . 1_545 ? C22 C21 C30 119.7(12) . 1_545 ? C23 C22 C21 117.9(13) . . ? C23 C22 C39 121.1(13) . 1_455 ? C21 C22 C39 121.0(11) . 1_455 ? C24 C23 C22 122.4(14) . . ? C23 C24 C25 119.2(14) . . ? C24 C25 C26 120.4(16) . . ? C21 C26 C25 119.5(13) . . ? C21 C26 C27 120.6(12) . . ? C25 C26 C27 119.8(14) . . ? C28 C27 C26 119.6(14) 1_545 . ? C27 C28 C29 120.4(13) 1_565 . ? C28 C29 C30 121.5(12) . . ? C29 C30 C21 118.1(12) . 1_565 ? C29 C30 C31 121.5(11) . . ? C21 C30 C31 120.4(11) 1_565 . ? C32 C31 C40 117.1(12) . 1_465 ? C32 C31 C30 123.7(11) . . ? C40 C31 C30 119.2(11) 1_465 . ? C33 C32 C31 124.3(13) . . ? C34 C33 C32 117.3(14) 1_465 . ? C33 C34 C35 124.4(15) 1_645 . ? C36 C35 C40 120.5(15) . . ? C36 C35 C34 122.6(16) . . ? C40 C35 C34 116.9(13) . . ? C37 C36 C35 120.2(16) . . ? C38 C37 C36 120.1(15) . . ? C37 C38 C39 123.7(16) . . ? C38 C39 C40 116.7(15) . . ? C38 C39 C22 124.9(14) . 1_655 ? C40 C39 C22 118.4(11) . 1_655 ? C35 C40 C39 118.8(12) . . ? C35 C40 C31 119.9(12) . 1_645 ? C39 C40 C31 121.3(13) . 1_645 ? C50 C41 C42 121.6(10) 1_554 2_655 ? C50 C41 C46 119.5(10) 1_554 . ? C42 C41 C46 118.8(10) 2_655 . ? C43 C42 C41 120.0(10) 2_655 2_655 ? C43 C42 C50 123.0(10) 2_655 . ? C41 C42 C50 117.0(9) 2_655 . ? C42 C43 C44 121.9(11) 2_655 . ? C45 C44 C43 120.1(12) . . ? C44 C45 C46 122.4(11) . . ? C47 C46 C45 124.3(11) . . ? C47 C46 C41 118.9(11) . . ? C45 C46 C41 116.8(11) . . ? C48 C47 C46 123.1(12) 1_554 . ? C47 C48 C49 119.3(13) 1_556 . ? C48 C49 C50 121.5(12) . . ? C41 C50 C49 117.6(11) 1_556 . ? C41 C50 C42 121.4(9) 1_556 . ? C49 C50 C42 121.0(10) . . ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 30.59 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 3.166 _refine_diff_density_min -4.407 _refine_diff_density_rms 0.322