# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1954 data_global _publ_contact_author 'Dr. M. J. Mays' _publ_contact_author_email mjm14@cam.ac.uk loop_ _publ_author_name Davies,J.E. Mays,M.J. Raithby,P.R. Shields,G.P. Tompkin,P.K. Woods, A.D. _journal_name_full 'J.Chem.Soc.,Dalton Trans.' _journal_volume '?' _journal_page_first '?' _journal_page_last '?' _journal_year '?' data_15 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C24 H10 As Mo2 O14 P W2' _chemical_formula_weight 1187.79 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'As' 'As' 0.0499 2.0058 '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' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.677(5) _cell_length_b 10.799(5) _cell_length_c 16.916(5) _cell_angle_alpha 90.00 _cell_angle_beta 110.220(10) _cell_angle_gamma 90.00 _cell_volume 3201.6(20) _cell_formula_units_Z 4 _cell_measurement_temperature 290(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 25 _cell_measurement_theta_max 30 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.464 _exptl_crystal_density_method ? _exptl_crystal_F_000 2184 _exptl_absorpt_coefficient_mu 9.066 _exptl_absorpt_correction_type psiscans _exptl_absorpt_correction_T_min 0.765 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 290(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Normal focus rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku AFC7R' _diffrn_measurement_method 'omega/2theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3014 _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_av_sigmaI/netI 0.0742 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3014 _reflns_number_observed 2046 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Rigaku software' _computing_cell_refinement 'Rigaku software' _computing_data_reduction 'TeXsan' _computing_structure_solution 'SIR 92' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL-PLUS' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0181P)^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 'riding atom' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3014 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0786 _refine_ls_R_factor_obs 0.0409 _refine_ls_wR_factor_all 0.0820 _refine_ls_wR_factor_obs 0.0702 _refine_ls_goodness_of_fit_all 0.999 _refine_ls_goodness_of_fit_obs 1.054 _refine_ls_restrained_S_all 0.999 _refine_ls_restrained_S_obs 1.054 _refine_ls_shift/esd_max 0.003 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo1 Mo 0.51902(5) -0.25611(7) 0.66902(5) 0.0353(2) Uani 1 d . . C1 C 0.5157(8) -0.4594(10) 0.6273(8) 0.070(4) Uani 1 d . . H1A H 0.5526(8) -0.5150(10) 0.6587(8) 0.084 Uiso 1 calc R . C2 C 0.5213(8) -0.3824(11) 0.5631(7) 0.068(4) Uani 1 d . . H2A H 0.5628(8) -0.3773(11) 0.5447(7) 0.082 Uiso 1 calc R . C3 C 0.4540(8) -0.3151(12) 0.5316(7) 0.065(3) Uani 1 d . . H3A H 0.4422(8) -0.2580(12) 0.4878(7) 0.078 Uiso 1 calc R . C4 C 0.4071(7) -0.3483(12) 0.5774(8) 0.069(4) Uani 1 d . . H4A H 0.3590(7) -0.3163(12) 0.5702(8) 0.083 Uiso 1 calc R . C5 C 0.4458(7) -0.4382(10) 0.6358(7) 0.063(3) Uani 1 d . . H5A H 0.4276(7) -0.4772(10) 0.6741(7) 0.076 Uiso 1 calc R . C11 C 0.5569(6) -0.1194(10) 0.6159(6) 0.052(3) Uani 1 d . . O11 O 0.5747(5) -0.0412(7) 0.5801(5) 0.077(3) Uani 1 d . . C12 C 0.6264(7) -0.2927(10) 0.7392(7) 0.050(3) Uani 1 d . . O12 O 0.6889(5) -0.3146(8) 0.7782(5) 0.074(3) Uani 1 d . . As1 As 0.43960(7) -0.09677(12) 0.70691(8) 0.0300(3) Uani 0.50 d P . P1 P 0.43960(7) -0.09677(12) 0.70691(8) 0.0300(3) Uani 0.50 d P . W2 W 0.33544(2) 0.06698(4) 0.65179(3) 0.04367(13) Uani 1 d . . C21 C 0.2606(8) -0.0261(12) 0.6909(9) 0.078(4) Uani 1 d . . O21 O 0.2160(6) -0.0744(9) 0.7144(9) 0.136(5) Uani 1 d . . C22 C 0.3704(7) 0.1606(11) 0.7635(8) 0.066(3) Uani 1 d . . O22 O 0.3884(6) 0.2144(10) 0.8239(6) 0.113(4) Uani 1 d . . C23 C 0.4076(6) 0.1726(11) 0.6144(8) 0.065(3) Uani 1 d . . O23 O 0.4443(6) 0.2374(10) 0.5904(7) 0.114(4) Uani 1 d . . C24 C 0.3011(7) -0.0260(13) 0.5405(8) 0.071(4) Uani 1 d . . O24 O 0.2844(6) -0.0774(11) 0.4789(6) 0.114(4) Uani 1 d . . C25 C 0.2552(6) 0.1910(12) 0.6044(8) 0.068(4) Uani 1 d . . O25 O 0.2074(5) 0.2623(10) 0.5778(6) 0.106(4) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0440(5) 0.0315(4) 0.0340(4) -0.0064(4) 0.0182(4) -0.0040(4) C1 0.091(10) 0.037(7) 0.085(9) -0.026(6) 0.036(8) -0.009(6) C2 0.105(11) 0.055(8) 0.064(8) -0.035(7) 0.053(8) -0.034(8) C3 0.085(9) 0.071(9) 0.037(6) -0.017(6) 0.018(6) -0.018(8) C4 0.065(8) 0.072(9) 0.067(8) -0.030(7) 0.018(7) -0.022(7) C5 0.095(9) 0.037(6) 0.070(8) -0.028(6) 0.043(7) -0.035(7) C11 0.072(8) 0.044(6) 0.043(6) -0.015(5) 0.024(6) -0.011(6) O11 0.098(7) 0.061(6) 0.084(6) 0.005(5) 0.048(5) -0.023(5) C12 0.065(8) 0.042(6) 0.050(7) -0.003(5) 0.029(6) 0.004(6) O12 0.057(5) 0.078(6) 0.083(6) -0.003(5) 0.018(5) 0.020(5) As1 0.0298(6) 0.0293(7) 0.0313(7) 0.0021(6) 0.0111(5) 0.0021(6) P1 0.0298(6) 0.0293(7) 0.0313(7) 0.0021(6) 0.0111(5) 0.0021(6) W2 0.0367(2) 0.0481(3) 0.0456(2) 0.0077(2) 0.0135(2) 0.0041(2) C21 0.085(10) 0.062(9) 0.105(11) -0.001(8) 0.057(9) 0.011(7) O21 0.116(9) 0.079(7) 0.275(16) 0.019(9) 0.146(11) -0.007(7) C22 0.062(8) 0.049(7) 0.070(9) 0.006(7) -0.001(7) 0.011(6) O22 0.131(9) 0.105(8) 0.073(7) -0.038(6) -0.004(6) 0.025(7) C23 0.051(7) 0.066(8) 0.079(9) 0.024(7) 0.022(6) -0.002(6) O23 0.112(8) 0.111(8) 0.132(9) 0.030(7) 0.060(7) -0.042(7) C24 0.059(8) 0.088(10) 0.059(8) -0.006(7) 0.011(7) -0.006(7) O24 0.101(8) 0.160(11) 0.068(6) -0.049(7) 0.014(6) -0.037(8) C25 0.045(7) 0.081(9) 0.078(9) 0.044(7) 0.021(6) 0.036(7) O25 0.086(7) 0.142(10) 0.101(8) 0.051(7) 0.045(6) 0.072(7) _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 C11 1.982(11) . ? Mo1 C12 1.986(12) . ? Mo1 C2 2.265(10) . ? Mo1 C1 2.300(10) . ? Mo1 C3 2.309(10) . ? Mo1 C5 2.350(10) . ? Mo1 C4 2.351(11) . ? Mo1 P1 2.496(2) . ? Mo1 As1 2.496(2) . ? Mo1 P1 2.616(2) 2_656 ? Mo1 As1 2.616(2) 2_656 ? Mo1 Mo1 3.059(2) 2_656 ? C1 C5 1.38(2) . ? C1 C2 1.40(2) . ? C2 C3 1.39(2) . ? C3 C4 1.40(2) . ? C4 C5 1.40(2) . ? C11 O11 1.154(12) . ? C12 O12 1.149(12) . ? As1 P1 2.223(3) 2_656 ? As1 As1 2.223(3) 2_656 ? As1 W2 2.5547(15) . ? As1 Mo1 2.616(2) 2_656 ? P1 P1 2.223(3) 2_656 ? P1 As1 2.223(3) 2_656 ? P1 W2 2.5547(15) . ? P1 Mo1 2.616(2) 2_656 ? W2 C25 1.962(10) . ? W2 C21 2.011(13) . ? W2 C23 2.026(11) . ? W2 C24 2.032(13) . ? W2 C22 2.040(14) . ? C21 O21 1.163(14) . ? C22 O22 1.122(14) . ? C23 O23 1.148(13) . ? C24 O24 1.126(13) . ? C25 O25 1.147(12) . ? 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 C11 Mo1 C12 88.5(4) . . ? C11 Mo1 C2 89.0(4) . . ? C12 Mo1 C2 93.5(5) . . ? C11 Mo1 C1 123.2(4) . . ? C12 Mo1 C1 84.7(5) . . ? C2 Mo1 C1 35.7(4) . . ? C11 Mo1 C3 84.0(4) . . ? C12 Mo1 C3 128.2(5) . . ? C2 Mo1 C3 35.4(4) . . ? C1 Mo1 C3 58.6(5) . . ? C11 Mo1 C5 141.7(4) . . ? C12 Mo1 C5 111.2(5) . . ? C2 Mo1 C5 58.4(4) . . ? C1 Mo1 C5 34.6(4) . . ? C3 Mo1 C5 57.9(4) . . ? C11 Mo1 C4 113.1(5) . . ? C12 Mo1 C4 142.6(5) . . ? C2 Mo1 C4 58.6(4) . . ? C1 Mo1 C4 58.0(5) . . ? C3 Mo1 C4 35.0(4) . . ? C5 Mo1 C4 34.5(4) . . ? C11 Mo1 P1 86.5(3) . . ? C12 Mo1 P1 123.4(3) . . ? C2 Mo1 P1 142.6(4) . . ? C1 Mo1 P1 141.4(3) . . ? C3 Mo1 P1 107.2(4) . . ? C5 Mo1 P1 106.8(3) . . ? C4 Mo1 P1 89.4(3) . . ? C11 Mo1 As1 86.5(3) . . ? C12 Mo1 As1 123.4(3) . . ? C2 Mo1 As1 142.6(4) . . ? C1 Mo1 As1 141.4(3) . . ? C3 Mo1 As1 107.2(4) . . ? C5 Mo1 As1 106.8(3) . . ? C4 Mo1 As1 89.4(3) . . ? P1 Mo1 As1 0.00(9) . . ? C11 Mo1 P1 79.7(3) . 2_656 ? C12 Mo1 P1 72.2(3) . 2_656 ? C2 Mo1 P1 161.8(3) . 2_656 ? C1 Mo1 P1 147.5(3) . 2_656 ? C3 Mo1 P1 153.6(4) . 2_656 ? C5 Mo1 P1 136.8(3) . 2_656 ? C4 Mo1 P1 139.2(3) . 2_656 ? P1 Mo1 P1 51.49(6) . 2_656 ? As1 Mo1 P1 51.49(6) . 2_656 ? C11 Mo1 As1 79.7(3) . 2_656 ? C12 Mo1 As1 72.2(3) . 2_656 ? C2 Mo1 As1 161.8(3) . 2_656 ? C1 Mo1 As1 147.5(3) . 2_656 ? C3 Mo1 As1 153.6(4) . 2_656 ? C5 Mo1 As1 136.8(3) . 2_656 ? C4 Mo1 As1 139.2(3) . 2_656 ? P1 Mo1 As1 51.49(6) . 2_656 ? As1 Mo1 As1 51.49(6) . 2_656 ? P1 Mo1 As1 0.00(9) 2_656 2_656 ? C11 Mo1 Mo1 129.5(3) . 2_656 ? C12 Mo1 Mo1 87.9(3) . 2_656 ? C2 Mo1 Mo1 141.5(3) . 2_656 ? C1 Mo1 Mo1 106.6(3) . 2_656 ? C3 Mo1 Mo1 134.2(3) . 2_656 ? C5 Mo1 Mo1 85.3(3) . 2_656 ? C4 Mo1 Mo1 99.3(3) . 2_656 ? P1 Mo1 Mo1 55.06(4) . 2_656 ? As1 Mo1 Mo1 55.06(4) . 2_656 ? P1 Mo1 Mo1 51.47(4) 2_656 2_656 ? As1 Mo1 Mo1 51.47(4) 2_656 2_656 ? C5 C1 C2 108.0(12) . . ? C5 C1 Mo1 74.7(6) . . ? C2 C1 Mo1 70.8(6) . . ? C3 C2 C1 107.9(11) . . ? C3 C2 Mo1 74.1(7) . . ? C1 C2 Mo1 73.5(6) . . ? C2 C3 C4 108.1(12) . . ? C2 C3 Mo1 70.6(6) . . ? C4 C3 Mo1 74.1(6) . . ? C5 C4 C3 107.4(12) . . ? C5 C4 Mo1 72.7(6) . . ? C3 C4 Mo1 70.9(6) . . ? C1 C5 C4 108.6(11) . . ? C1 C5 Mo1 70.8(6) . . ? C4 C5 Mo1 72.8(6) . . ? O11 C11 Mo1 175.3(10) . . ? O12 C12 Mo1 178.4(9) . . ? P1 As1 As1 0.00(11) 2_656 2_656 ? P1 As1 Mo1 67.03(5) 2_656 . ? As1 As1 Mo1 67.03(5) 2_656 . ? P1 As1 W2 135.36(4) 2_656 . ? As1 As1 W2 135.36(4) 2_656 . ? Mo1 As1 W2 145.96(6) . . ? P1 As1 Mo1 61.47(5) 2_656 2_656 ? As1 As1 Mo1 61.47(5) 2_656 2_656 ? Mo1 As1 Mo1 73.47(5) . 2_656 ? W2 As1 Mo1 136.45(6) . 2_656 ? P1 P1 As1 0.00(11) 2_656 2_656 ? P1 P1 Mo1 67.03(5) 2_656 . ? As1 P1 Mo1 67.03(5) 2_656 . ? P1 P1 W2 135.36(4) 2_656 . ? As1 P1 W2 135.36(4) 2_656 . ? Mo1 P1 W2 145.96(6) . . ? P1 P1 Mo1 61.47(5) 2_656 2_656 ? As1 P1 Mo1 61.47(5) 2_656 2_656 ? Mo1 P1 Mo1 73.47(5) . 2_656 ? W2 P1 Mo1 136.45(6) . 2_656 ? C25 W2 C21 87.5(5) . . ? C25 W2 C23 89.1(5) . . ? C21 W2 C23 175.7(5) . . ? C25 W2 C24 90.4(5) . . ? C21 W2 C24 91.4(5) . . ? C23 W2 C24 91.2(5) . . ? C25 W2 C22 89.7(5) . . ? C21 W2 C22 88.8(5) . . ? C23 W2 C22 88.6(5) . . ? C24 W2 C22 179.7(5) . . ? C25 W2 As1 177.5(4) . . ? C21 W2 As1 93.6(4) . . ? C23 W2 As1 89.9(3) . . ? C24 W2 As1 87.3(4) . . ? C22 W2 As1 92.6(3) . . ? C25 W2 P1 177.5(4) . . ? C21 W2 P1 93.6(4) . . ? C23 W2 P1 89.9(3) . . ? C24 W2 P1 87.3(4) . . ? C22 W2 P1 92.6(3) . . ? As1 W2 P1 0.00(10) . . ? O21 C21 W2 176.7(11) . . ? O22 C22 W2 178.2(11) . . ? O23 C23 W2 175.4(11) . . ? O24 C24 W2 177.8(12) . . ? O25 C25 W2 178.4(10) . . ? _refine_diff_density_max 0.776 _refine_diff_density_min -0.837 _refine_diff_density_rms 0.167 data_13 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C19 H10 Mo2 O9 P Sb W' _chemical_formula_weight 910.72 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sb' 'Sb' -0.5866 1.5461 '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 15.974(5) _cell_length_b 16.236(8) _cell_length_c 10.623(2) _cell_angle_alpha 97.85(3) _cell_angle_beta 96.34(2) _cell_angle_gamma 118.86(2) _cell_volume 2340.4(14) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour 'v dark' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.585 _exptl_crystal_density_method ? _exptl_crystal_F_000 1680 _exptl_absorpt_coefficient_mu 7.203 _exptl_absorpt_correction_type psiscan _exptl_absorpt_correction_T_min 0.666 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device AFC7R _diffrn_measurement_method '\w/2\q scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_decay_% -1.5 _diffrn_reflns_number 8554 _diffrn_reflns_av_R_equivalents 0.0301 _diffrn_reflns_av_sigmaI/netI 0.0380 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 24.99 _reflns_number_total 8232 _reflns_number_observed 7556 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Rigaku software' _computing_cell_refinement 'Rigaku software' _computing_data_reduction 'TeXsan' _computing_structure_solution 'SIR 92' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL-PLUS' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0465P)^2^+11.5801P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8232 _refine_ls_number_parameters 595 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0389 _refine_ls_R_factor_obs 0.0350 _refine_ls_wR_factor_all 0.0922 _refine_ls_wR_factor_obs 0.0896 _refine_ls_goodness_of_fit_all 1.092 _refine_ls_goodness_of_fit_obs 1.111 _refine_ls_restrained_S_all 1.092 _refine_ls_restrained_S_obs 1.111 _refine_ls_shift/esd_max 0.204 _refine_ls_shift/esd_mean 0.013 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group W1 W 0.56639(2) 0.35187(2) 0.62594(3) 0.01587(8) Uani 1 d . . Sb1 Sb 0.29970(4) 0.10877(3) 0.70657(5) 0.02017(12) Uani 1 d . . Mo1 Mo 0.23195(4) 0.22430(4) 0.60373(6) 0.01630(14) Uani 1 d . . Mo2 Mo 0.32715(4) 0.26333(4) 0.88783(6) 0.01481(13) Uani 1 d . . P1 P 0.40156(13) 0.27228(13) 0.6889(2) 0.0153(4) Uani 1 d . . C1 C 0.1174(5) 0.1056(6) 0.6351(7) 0.024(2) Uani 1 d . . O1 O 0.0471(4) 0.0430(4) 0.6492(6) 0.0333(14) Uani 1 d . . O2 O 0.2313(5) 0.1035(5) 0.3498(6) 0.045(2) Uani 1 d . . C2 C 0.2328(6) 0.1438(6) 0.4470(8) 0.027(2) Uani 1 d . . O3 O 0.4397(4) 0.4801(4) 0.8695(6) 0.0336(14) Uani 1 d . . C3 C 0.4006(5) 0.4008(6) 0.8752(7) 0.022(2) Uani 1 d . . C4 C 0.4522(6) 0.2766(6) 0.9696(8) 0.026(2) Uani 1 d . . O4 O 0.5222(4) 0.2847(5) 1.0263(6) 0.039(2) Uani 1 d . . C5 C 0.4928(5) 0.2999(6) 0.4367(8) 0.023(2) Uani 1 d . . O5 O 0.4544(5) 0.2728(5) 0.3308(6) 0.0366(14) Uani 1 d . . C6 C 0.5592(5) 0.4726(5) 0.6322(7) 0.0174(15) Uani 1 d . . O6 O 0.5564(4) 0.5426(4) 0.6372(5) 0.0291(13) Uani 1 d . . O7 O 0.7681(4) 0.4524(4) 0.5385(6) 0.0352(14) Uani 1 d . . C7 C 0.6932(6) 0.4134(6) 0.5719(8) 0.027(2) Uani 1 d . . C8 C 0.6456(6) 0.4062(6) 0.8132(8) 0.028(2) Uani 1 d . . O8 O 0.6922(5) 0.4378(5) 0.9124(6) 0.047(2) Uani 1 d . . C9 C 0.5652(6) 0.2241(6) 0.6213(8) 0.024(2) Uani 1 d . . O9 O 0.5625(5) 0.1527(4) 0.6186(7) 0.0380(15) Uani 1 d . . C10 C 0.1310(6) 0.2896(7) 0.6021(9) 0.032(2) Uani 1 d . . H10 H 0.0698(6) 0.2644(7) 0.6372(9) 0.038 Uiso 1 calc R . C11 C 0.1363(6) 0.2601(6) 0.4718(8) 0.032(2) Uani 1 d . . H11 H 0.0801(6) 0.2140(6) 0.3994(8) 0.039 Uiso 1 calc R . C12 C 0.2348(6) 0.3194(6) 0.4610(8) 0.031(2) Uani 1 d . . H12 H 0.2603(6) 0.3209(6) 0.3790(8) 0.037 Uiso 1 calc R . C13 C 0.2872(6) 0.3832(6) 0.5810(8) 0.027(2) Uani 1 d . . H13 H 0.3569(6) 0.4364(6) 0.5999(8) 0.032 Uiso 1 calc R . C14 C 0.2212(6) 0.3646(6) 0.6684(8) 0.027(2) Uani 1 d . . H14A H 0.2368(6) 0.4015(6) 0.7594(8) 0.033 Uiso 1 calc R . C15 C 0.1693(5) 0.2205(6) 0.9277(7) 0.023(2) Uani 1 d . . H15 H 0.1122(5) 0.2087(6) 0.8629(7) 0.027 Uiso 1 calc R . C16 C 0.2396(6) 0.3093(6) 1.0098(7) 0.027(2) Uani 1 d . . H16 H 0.2393(6) 0.3712(6) 1.0155(7) 0.033 Uiso 1 calc R . C17 C 0.3048(6) 0.2945(7) 1.0925(7) 0.032(2) Uani 1 d . . H17 H 0.3563(6) 0.3429(7) 1.1683(7) 0.038 Uiso 1 calc R . C18 C 0.2738(6) 0.1952(6) 1.0607(8) 0.029(2) Uani 1 d . . H18 H 0.3013(6) 0.1619(6) 1.1087(8) 0.035 Uiso 1 calc R . C19 C 0.1908(5) 0.1495(6) 0.9589(7) 0.022(2) Uani 1 d . . H19 H 0.1512(5) 0.0788(6) 0.9201(7) 0.027 Uiso 1 calc R . W1' W 0.86087(2) 0.16449(2) -0.18905(3) 0.01473(8) Uani 1 d . . Sb1' Sb 0.87271(3) 0.13674(3) 0.22752(4) 0.01563(11) Uani 1 d . . Mo1' Mo 0.91887(4) 0.33067(4) 0.22820(6) 0.01484(13) Uani 1 d . . Mo2' Mo 0.71126(4) 0.15759(5) 0.17497(6) 0.01610(14) Uani 1 d . . P1' P 0.84166(13) 0.19558(13) 0.0418(2) 0.0154(4) Uani 1 d . . O1' O 0.9453(4) 0.3166(4) 0.5196(5) 0.0266(12) Uani 1 d . . C1' C 0.9342(5) 0.3167(5) 0.4117(7) 0.019(2) Uani 1 d . . O2' O 1.1205(4) 0.3472(5) 0.2111(6) 0.0342(14) Uani 1 d . . C2' C 1.0459(6) 0.3376(6) 0.2183(7) 0.024(2) Uani 1 d . . C3' C 0.6754(6) 0.1983(6) 0.0183(8) 0.026(2) Uani 1 d . . O3' O 0.6507(5) 0.2178(5) -0.0727(6) 0.041(2) Uani 1 d . . O4' O 0.6239(5) -0.0480(4) 0.0023(6) 0.039(2) Uani 1 d . . C4' C 0.6579(5) 0.0282(6) 0.0634(7) 0.021(2) Uani 1 d . . O5' O 1.0675(4) 0.3558(4) -0.1073(6) 0.0316(13) Uani 1 d . . C5' C 0.9946(6) 0.2841(5) -0.1360(7) 0.021(2) Uani 1 d . . C6' C 0.8145(5) 0.2528(6) -0.2455(7) 0.022(2) Uani 1 d . . O6' O 0.7919(4) 0.3041(5) -0.2791(6) 0.0344(14) Uani 1 d . . C7' C 0.8815(5) 0.1312(5) -0.3651(7) 0.020(2) Uani 1 d . . O7' O 0.8910(4) 0.1058(4) -0.4666(5) 0.0306(13) Uani 1 d . . C8' C 0.7196(6) 0.0516(6) -0.2480(8) 0.029(2) Uani 1 d . . O8' O 0.6418(5) -0.0077(6) -0.2854(7) 0.057(2) Uani 1 d . . C20' C 0.9101(5) 0.0778(6) -0.1300(7) 0.023(2) Uani 1 d . . O20' O 0.9378(4) 0.0289(4) -0.0988(6) 0.0316(13) Uani 1 d . . C10' C 0.9079(6) 0.4652(6) 0.3081(8) 0.029(2) Uani 1 d . . H10' H 0.8949(6) 0.4809(6) 0.3956(8) 0.035 Uiso 1 calc R . C11' C 1.0017(6) 0.4958(5) 0.2780(8) 0.028(2) Uani 1 d . . H11' H 1.0657(6) 0.5383(5) 0.3399(8) 0.033 Uiso 1 calc R . C12' C 0.9888(6) 0.4653(6) 0.1432(8) 0.028(2) Uani 1 d . . H12' H 1.0420(6) 0.4826(6) 0.0926(8) 0.034 Uiso 1 calc R . C13' C 0.8868(7) 0.4178(6) 0.0900(8) 0.031(2) Uani 1 d . . H13' H 0.8561(7) 0.3930(6) -0.0045(8) 0.037 Uiso 1 calc R . C14' C 0.8371(7) 0.4173(6) 0.1921(8) 0.030(2) Uani 1 d . . H14' H 0.7654(7) 0.3918(6) 0.1829(8) 0.036 Uiso 1 calc R . C15' C 0.7078(6) 0.2350(7) 0.3787(8) 0.031(2) Uani 1 d . . H15' H 0.7621(6) 0.2975(7) 0.4337(8) 0.037 Uiso 1 calc R . C16' C 0.6324(6) 0.2239(7) 0.2849(9) 0.035(2) Uani 1 d . . H16' H 0.6229(6) 0.2773(7) 0.2634(9) 0.042 Uiso 1 calc R . C17' C 0.5675(6) 0.1263(8) 0.2362(8) 0.037(2) Uani 1 d . . H17' H 0.5028(6) 0.0978(8) 0.1763(8) 0.045 Uiso 1 calc R . C18' C 0.6033(6) 0.0736(7) 0.3005(8) 0.033(2) Uani 1 d . . H18' H 0.5684(6) 0.0023(7) 0.2935(8) 0.040 Uiso 1 calc R . C19' C 0.6909(6) 0.1427(6) 0.3878(7) 0.026(2) Uani 1 d . . H19' H 0.7306(6) 0.1285(6) 0.4513(7) 0.032 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.01190(15) 0.0179(2) 0.0202(2) 0.00565(11) 0.00581(11) 0.00843(12) Sb1 0.0215(3) 0.0161(2) 0.0229(3) 0.0045(2) 0.0072(2) 0.0089(2) Mo1 0.0111(3) 0.0204(3) 0.0145(3) 0.0044(2) 0.0020(2) 0.0057(3) Mo2 0.0124(3) 0.0190(3) 0.0137(3) 0.0028(2) 0.0031(2) 0.0085(3) P1 0.0114(8) 0.0181(9) 0.0177(9) 0.0052(7) 0.0052(7) 0.0076(7) C1 0.016(4) 0.031(4) 0.018(4) 0.002(3) -0.002(3) 0.008(4) O1 0.017(3) 0.036(3) 0.031(3) 0.010(3) 0.003(2) 0.001(3) O2 0.065(5) 0.039(4) 0.020(3) -0.001(3) 0.013(3) 0.018(3) C2 0.018(4) 0.027(4) 0.028(4) 0.008(3) 0.001(3) 0.005(3) O3 0.037(3) 0.019(3) 0.029(3) 0.001(2) -0.003(3) 0.005(3) C3 0.017(4) 0.026(4) 0.017(4) -0.002(3) 0.000(3) 0.009(3) C4 0.028(5) 0.024(4) 0.024(4) 0.003(3) 0.008(3) 0.011(3) O4 0.020(3) 0.063(4) 0.042(4) 0.015(3) 0.002(3) 0.027(3) C5 0.017(4) 0.024(4) 0.027(4) 0.007(3) 0.006(3) 0.009(3) O5 0.041(4) 0.051(4) 0.023(3) 0.000(3) 0.000(3) 0.031(3) C6 0.018(4) 0.017(4) 0.016(3) 0.005(3) 0.003(3) 0.008(3) O6 0.034(3) 0.022(3) 0.029(3) 0.002(2) -0.002(2) 0.016(3) O7 0.020(3) 0.033(3) 0.057(4) 0.016(3) 0.025(3) 0.011(3) C7 0.029(5) 0.021(4) 0.035(4) 0.007(3) 0.009(4) 0.016(4) C8 0.028(4) 0.028(4) 0.028(4) 0.007(3) 0.004(4) 0.013(4) O8 0.048(4) 0.046(4) 0.031(4) 0.008(3) -0.014(3) 0.018(3) C9 0.022(4) 0.024(4) 0.028(4) 0.009(3) 0.012(3) 0.011(3) O9 0.041(4) 0.030(3) 0.058(4) 0.018(3) 0.022(3) 0.025(3) C10 0.018(4) 0.048(5) 0.039(5) 0.021(4) 0.008(3) 0.022(4) C11 0.018(4) 0.040(5) 0.034(5) 0.010(4) -0.004(3) 0.013(4) C12 0.034(5) 0.036(5) 0.028(4) 0.019(4) 0.007(4) 0.017(4) C13 0.027(4) 0.030(4) 0.030(4) 0.013(3) 0.004(3) 0.018(4) C14 0.027(4) 0.030(4) 0.038(5) 0.014(4) 0.010(4) 0.022(4) C15 0.018(4) 0.034(4) 0.021(4) 0.004(3) 0.012(3) 0.015(3) C16 0.028(4) 0.036(5) 0.022(4) 0.001(3) 0.017(3) 0.019(4) C17 0.029(4) 0.052(6) 0.015(4) 0.002(4) 0.008(3) 0.021(4) C18 0.029(4) 0.043(5) 0.022(4) 0.018(4) 0.013(3) 0.018(4) C19 0.020(4) 0.023(4) 0.025(4) 0.011(3) 0.014(3) 0.008(3) W1' 0.01242(15) 0.0207(2) 0.01302(14) 0.00550(11) 0.00500(11) 0.00893(12) Sb1' 0.0151(2) 0.0180(2) 0.0163(2) 0.0054(2) 0.0032(2) 0.0099(2) Mo1' 0.0156(3) 0.0166(3) 0.0145(3) 0.0059(2) 0.0066(2) 0.0085(2) Mo2' 0.0122(3) 0.0242(3) 0.0156(3) 0.0081(2) 0.0060(2) 0.0106(3) P1' 0.0142(9) 0.0211(9) 0.0145(8) 0.0062(7) 0.0058(7) 0.0105(8) O1' 0.036(3) 0.029(3) 0.017(3) 0.005(2) 0.007(2) 0.019(3) C1' 0.016(4) 0.012(3) 0.027(4) 0.007(3) 0.011(3) 0.004(3) O2' 0.017(3) 0.055(4) 0.035(3) 0.015(3) 0.012(2) 0.019(3) C2' 0.027(5) 0.023(4) 0.020(4) 0.005(3) 0.003(3) 0.012(3) C3' 0.020(4) 0.041(5) 0.032(4) 0.012(4) 0.015(3) 0.023(4) O3' 0.045(4) 0.077(5) 0.031(3) 0.028(3) 0.015(3) 0.046(4) O4' 0.031(3) 0.031(4) 0.037(3) 0.002(3) -0.010(3) 0.005(3) C4' 0.013(4) 0.025(4) 0.019(4) 0.006(3) 0.001(3) 0.005(3) O5' 0.019(3) 0.023(3) 0.047(4) 0.006(3) 0.008(3) 0.007(3) C5' 0.023(4) 0.025(4) 0.023(4) 0.009(3) 0.008(3) 0.016(4) C6' 0.017(4) 0.030(4) 0.021(4) 0.007(3) 0.005(3) 0.012(3) O6' 0.027(3) 0.044(4) 0.042(4) 0.020(3) 0.008(3) 0.023(3) C7' 0.014(4) 0.018(4) 0.022(4) 0.006(3) 0.000(3) 0.003(3) O7' 0.043(4) 0.042(3) 0.013(3) 0.004(2) 0.010(2) 0.026(3) C8' 0.020(4) 0.037(5) 0.027(4) 0.006(4) 0.010(3) 0.011(4) O8' 0.021(4) 0.069(5) 0.057(5) 0.014(4) 0.008(3) 0.004(4) C20' 0.016(4) 0.028(4) 0.015(3) 0.005(3) 0.002(3) 0.005(3) O20' 0.037(3) 0.033(3) 0.042(3) 0.018(3) 0.016(3) 0.026(3) C10' 0.040(5) 0.019(4) 0.038(5) 0.012(3) 0.020(4) 0.019(4) C11' 0.028(4) 0.013(4) 0.041(5) 0.009(3) 0.011(4) 0.008(3) C12' 0.036(5) 0.020(4) 0.029(4) 0.017(3) 0.017(4) 0.009(4) C13' 0.046(5) 0.023(4) 0.029(4) 0.011(3) 0.003(4) 0.021(4) C14' 0.036(5) 0.024(4) 0.042(5) 0.016(4) 0.013(4) 0.022(4) C15' 0.031(5) 0.044(5) 0.026(4) 0.008(4) 0.017(4) 0.023(4) C16' 0.033(5) 0.055(6) 0.039(5) 0.023(4) 0.026(4) 0.032(5) C17' 0.012(4) 0.078(7) 0.024(4) 0.017(4) 0.014(3) 0.021(4) C18' 0.020(4) 0.045(5) 0.037(5) 0.021(4) 0.022(4) 0.012(4) C19' 0.024(4) 0.043(5) 0.021(4) 0.011(3) 0.010(3) 0.022(4) _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 C7 1.973(8) . ? W1 C6 2.011(7) . ? W1 C5 2.048(8) . ? W1 C8 2.056(8) . ? W1 C9 2.059(8) . ? W1 P1 2.528(2) . ? Sb1 P1 2.401(2) . ? Sb1 Mo2 2.762(2) . ? Sb1 Mo1 2.8532(13) . ? Mo1 C2 1.977(9) . ? Mo1 C1 2.020(8) . ? Mo1 C11 2.289(8) . ? Mo1 C12 2.295(8) . ? Mo1 C10 2.318(8) . ? Mo1 C13 2.348(8) . ? Mo1 C14 2.380(8) . ? Mo1 P1 2.448(2) . ? Mo1 Mo2 3.0588(12) . ? Mo2 C4 1.986(9) . ? Mo2 C3 1.991(8) . ? Mo2 C17 2.271(8) . ? Mo2 C18 2.305(7) . ? Mo2 C16 2.310(7) . ? Mo2 C19 2.363(7) . ? Mo2 C15 2.376(7) . ? Mo2 P1 2.524(2) . ? C1 O1 1.137(9) . ? O2 C2 1.136(10) . ? O3 C3 1.143(9) . ? C4 O4 1.148(10) . ? C5 O5 1.134(9) . ? C6 O6 1.154(9) . ? O7 C7 1.175(10) . ? C8 O8 1.112(10) . ? C9 O9 1.135(10) . ? C10 C14 1.379(12) . ? C10 C11 1.426(13) . ? C11 C12 1.423(12) . ? C12 C13 1.402(12) . ? C13 C14 1.432(12) . ? C15 C16 1.407(11) . ? C15 C19 1.420(11) . ? C16 C17 1.419(12) . ? C17 C18 1.415(13) . ? C18 C19 1.411(11) . ? W1' C7' 1.983(8) . ? W1' C5' 2.021(8) . ? W1' C6' 2.032(8) . ? W1' C20' 2.048(8) . ? W1' C8' 2.056(8) . ? W1' P1' 2.518(2) . ? Sb1' P1' 2.410(2) . ? Sb1' Mo2' 2.7665(11) . ? Sb1' Mo1' 2.865(2) . ? Mo1' C2' 1.992(8) . ? Mo1' C1' 1.994(7) . ? Mo1' C12' 2.291(7) . ? Mo1' C11' 2.291(8) . ? Mo1' C10' 2.328(8) . ? Mo1' C13' 2.349(8) . ? Mo1' C14' 2.374(8) . ? Mo1' P1' 2.432(2) . ? Mo1' Mo2' 3.061(2) . ? Mo2' C4' 1.977(8) . ? Mo2' C3' 1.998(8) . ? Mo2' C17' 2.291(7) . ? Mo2' C18' 2.312(7) . ? Mo2' C16' 2.323(8) . ? Mo2' C19' 2.348(7) . ? Mo2' C15' 2.370(8) . ? Mo2' P1' 2.524(2) . ? O1' C1' 1.141(9) . ? O2' C2' 1.138(10) . ? C3' O3' 1.144(10) . ? O4' C4' 1.141(10) . ? O5' C5' 1.149(9) . ? C6' O6' 1.138(9) . ? C7' O7' 1.153(9) . ? C8' O8' 1.123(10) . ? C20' O20' 1.147(10) . ? C10' C14' 1.408(13) . ? C10' C11' 1.424(12) . ? C11' C12' 1.408(12) . ? C12' C13' 1.426(12) . ? C13' C14' 1.412(12) . ? C15' C16' 1.398(13) . ? C15' C19' 1.408(12) . ? C16' C17' 1.387(14) . ? C17' C18' 1.440(13) . ? C18' C19' 1.410(12) . ? 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 C7 W1 C6 90.7(3) . . ? C7 W1 C5 91.3(3) . . ? C6 W1 C5 90.8(3) . . ? C7 W1 C8 86.3(3) . . ? C6 W1 C8 89.4(3) . . ? C5 W1 C8 177.6(3) . . ? C7 W1 C9 92.7(3) . . ? C6 W1 C9 176.5(3) . . ? C5 W1 C9 88.6(3) . . ? C8 W1 C9 91.3(3) . . ? C7 W1 P1 178.4(2) . . ? C6 W1 P1 88.9(2) . . ? C5 W1 P1 87.1(2) . . ? C8 W1 P1 95.3(2) . . ? C9 W1 P1 87.6(2) . . ? P1 Sb1 Mo2 58.03(5) . . ? P1 Sb1 Mo1 54.73(5) . . ? Mo2 Sb1 Mo1 65.99(3) . . ? C2 Mo1 C1 88.8(3) . . ? C2 Mo1 C11 87.6(3) . . ? C1 Mo1 C11 94.0(3) . . ? C2 Mo1 C12 82.2(3) . . ? C1 Mo1 C12 129.3(3) . . ? C11 Mo1 C12 36.2(3) . . ? C2 Mo1 C10 122.5(3) . . ? C1 Mo1 C10 85.8(3) . . ? C11 Mo1 C10 36.1(3) . . ? C12 Mo1 C10 59.3(3) . . ? C2 Mo1 C13 111.6(3) . . ? C1 Mo1 C13 143.9(3) . . ? C11 Mo1 C13 59.2(3) . . ? C12 Mo1 C13 35.1(3) . . ? C10 Mo1 C13 58.2(3) . . ? C2 Mo1 C14 140.6(3) . . ? C1 Mo1 C14 111.6(3) . . ? C11 Mo1 C14 58.8(3) . . ? C12 Mo1 C14 58.7(3) . . ? C10 Mo1 C14 34.1(3) . . ? C13 Mo1 C14 35.3(3) . . ? C2 Mo1 P1 89.4(2) . . ? C1 Mo1 P1 122.6(2) . . ? C11 Mo1 P1 143.2(2) . . ? C12 Mo1 P1 107.2(2) . . ? C10 Mo1 P1 139.3(2) . . ? C13 Mo1 P1 88.3(2) . . ? C14 Mo1 P1 105.2(2) . . ? C2 Mo1 Sb1 76.6(2) . . ? C1 Mo1 Sb1 70.7(2) . . ? C11 Mo1 Sb1 158.0(2) . . ? C12 Mo1 Sb1 150.7(2) . . ? C10 Mo1 Sb1 150.1(2) . . ? C13 Mo1 Sb1 141.2(2) . . ? C14 Mo1 Sb1 141.0(2) . . ? P1 Mo1 Sb1 53.19(5) . . ? C2 Mo1 Mo2 130.4(2) . . ? C1 Mo1 Mo2 87.3(2) . . ? C11 Mo1 Mo2 142.0(2) . . ? C12 Mo1 Mo2 134.7(2) . . ? C10 Mo1 Mo2 106.5(2) . . ? C13 Mo1 Mo2 99.7(2) . . ? C14 Mo1 Mo2 85.4(2) . . ? P1 Mo1 Mo2 53.16(5) . . ? Sb1 Mo1 Mo2 55.57(3) . . ? C4 Mo2 C3 88.7(3) . . ? C4 Mo2 C17 86.6(3) . . ? C3 Mo2 C17 95.4(3) . . ? C4 Mo2 C18 82.9(3) . . ? C3 Mo2 C18 130.9(3) . . ? C17 Mo2 C18 36.0(3) . . ? C4 Mo2 C16 121.0(3) . . ? C3 Mo2 C16 85.5(3) . . ? C17 Mo2 C16 36.1(3) . . ? C18 Mo2 C16 59.3(3) . . ? C4 Mo2 C19 113.2(3) . . ? C3 Mo2 C19 143.5(3) . . ? C17 Mo2 C19 59.2(3) . . ? C18 Mo2 C19 35.2(3) . . ? C16 Mo2 C19 58.4(3) . . ? C4 Mo2 C15 141.0(3) . . ? C3 Mo2 C15 111.0(3) . . ? C17 Mo2 C15 59.2(3) . . ? C18 Mo2 C15 58.6(3) . . ? C16 Mo2 C15 34.9(3) . . ? C19 Mo2 C15 34.9(3) . . ? C4 Mo2 P1 81.9(2) . . ? C3 Mo2 P1 71.7(2) . . ? C17 Mo2 P1 162.8(2) . . ? C18 Mo2 P1 152.4(2) . . ? C16 Mo2 P1 147.7(2) . . ? C19 Mo2 P1 137.4(2) . . ? C15 Mo2 P1 135.4(2) . . ? C4 Mo2 Sb1 87.9(2) . . ? C3 Mo2 Sb1 125.3(2) . . ? C17 Mo2 Sb1 138.8(2) . . ? C18 Mo2 Sb1 102.8(2) . . ? C16 Mo2 Sb1 140.0(2) . . ? C19 Mo2 Sb1 86.0(2) . . ? C15 Mo2 Sb1 105.2(2) . . ? P1 Mo2 Sb1 53.79(5) . . ? C4 Mo2 Mo1 131.8(2) . . ? C3 Mo2 Mo1 85.5(2) . . ? C17 Mo2 Mo1 141.5(2) . . ? C18 Mo2 Mo1 133.9(2) . . ? C16 Mo2 Mo1 106.1(2) . . ? C19 Mo2 Mo1 98.8(2) . . ? C15 Mo2 Mo1 84.5(2) . . ? P1 Mo2 Mo1 50.93(5) . . ? Sb1 Mo2 Mo1 58.44(3) . . ? Sb1 P1 Mo1 72.08(6) . . ? Sb1 P1 Mo2 68.17(6) . . ? Mo1 P1 Mo2 75.91(6) . . ? Sb1 P1 W1 130.01(8) . . ? Mo1 P1 W1 139.46(8) . . ? Mo2 P1 W1 140.08(8) . . ? O1 C1 Mo1 172.7(7) . . ? O2 C2 Mo1 172.8(8) . . ? O3 C3 Mo2 177.1(7) . . ? O4 C4 Mo2 174.5(7) . . ? O5 C5 W1 178.0(7) . . ? O6 C6 W1 179.0(6) . . ? O7 C7 W1 177.7(7) . . ? O8 C8 W1 176.8(8) . . ? O9 C9 W1 178.6(7) . . ? C14 C10 C11 109.7(7) . . ? C14 C10 Mo1 75.4(5) . . ? C11 C10 Mo1 70.9(5) . . ? C12 C11 C10 106.3(7) . . ? C12 C11 Mo1 72.1(5) . . ? C10 C11 Mo1 73.0(5) . . ? C13 C12 C11 108.4(8) . . ? C13 C12 Mo1 74.5(5) . . ? C11 C12 Mo1 71.7(5) . . ? C12 C13 C14 108.0(8) . . ? C12 C13 Mo1 70.4(5) . . ? C14 C13 Mo1 73.6(5) . . ? C10 C14 C13 107.5(8) . . ? C10 C14 Mo1 70.5(5) . . ? C13 C14 Mo1 71.2(5) . . ? C16 C15 C19 107.6(7) . . ? C16 C15 Mo2 70.0(4) . . ? C19 C15 Mo2 72.1(4) . . ? C15 C16 C17 108.7(8) . . ? C15 C16 Mo2 75.1(4) . . ? C17 C16 Mo2 70.5(4) . . ? C18 C17 C16 107.3(7) . . ? C18 C17 Mo2 73.3(4) . . ? C16 C17 Mo2 73.5(4) . . ? C19 C18 C17 108.3(7) . . ? C19 C18 Mo2 74.7(4) . . ? C17 C18 Mo2 70.7(4) . . ? C18 C19 C15 108.1(7) . . ? C18 C19 Mo2 70.2(4) . . ? C15 C19 Mo2 73.0(4) . . ? C7' W1' C5' 92.8(3) . . ? C7' W1' C6' 91.8(3) . . ? C5' W1' C6' 85.6(3) . . ? C7' W1' C20' 88.6(3) . . ? C5' W1' C20' 93.3(3) . . ? C6' W1' C20' 178.9(3) . . ? C7' W1' C8' 87.7(3) . . ? C5' W1' C8' 174.3(3) . . ? C6' W1' C8' 88.7(3) . . ? C20' W1' C8' 92.4(3) . . ? C7' W1' P1' 173.9(2) . . ? C5' W1' P1' 87.4(2) . . ? C6' W1' P1' 94.3(2) . . ? C20' W1' P1' 85.3(2) . . ? C8' W1' P1' 92.7(2) . . ? P1' Sb1' Mo2' 57.87(5) . . ? P1' Sb1' Mo1' 54.08(5) . . ? Mo2' Sb1' Mo1' 65.82(3) . . ? C2' Mo1' C1' 89.9(3) . . ? C2' Mo1' C12' 81.6(3) . . ? C1' Mo1' C12' 130.1(3) . . ? C2' Mo1' C11' 88.0(3) . . ? C1' Mo1' C11' 95.3(3) . . ? C12' Mo1' C11' 35.8(3) . . ? C2' Mo1' C10' 122.7(3) . . ? C1' Mo1' C10' 86.3(3) . . ? C12' Mo1' C10' 59.4(3) . . ? C11' Mo1' C10' 35.9(3) . . ? C2' Mo1' C13' 111.5(3) . . ? C1' Mo1' C13' 144.2(3) . . ? C12' Mo1' C13' 35.8(3) . . ? C11' Mo1' C13' 59.0(3) . . ? C10' Mo1' C13' 58.2(3) . . ? C2' Mo1' C14' 140.7(3) . . ? C1' Mo1' C14' 112.2(3) . . ? C12' Mo1' C14' 59.2(3) . . ? C11' Mo1' C14' 59.0(3) . . ? C10' Mo1' C14' 34.8(3) . . ? C13' Mo1' C14' 34.8(3) . . ? C2' Mo1' P1' 88.8(2) . . ? C1' Mo1' P1' 123.8(2) . . ? C12' Mo1' P1' 105.2(2) . . ? C11' Mo1' P1' 140.8(2) . . ? C10' Mo1' P1' 138.2(2) . . ? C13' Mo1' P1' 86.3(2) . . ? C14' Mo1' P1' 103.3(2) . . ? C2' Mo1' Sb1' 77.7(2) . . ? C1' Mo1' Sb1' 71.6(2) . . ? C12' Mo1' Sb1' 150.0(2) . . ? C11' Mo1' Sb1' 160.3(2) . . ? C10' Mo1' Sb1' 150.5(2) . . ? C13' Mo1' Sb1' 139.1(2) . . ? C14' Mo1' Sb1' 139.1(2) . . ? P1' Mo1' Sb1' 53.36(5) . . ? C2' Mo1' Mo2' 130.9(2) . . ? C1' Mo1' Mo2' 88.6(2) . . ? C12' Mo1' Mo2' 132.8(2) . . ? C11' Mo1' Mo2' 141.0(2) . . ? C10' Mo1' Mo2' 106.2(2) . . ? C13' Mo1' Mo2' 97.2(2) . . ? C14' Mo1' Mo2' 83.6(2) . . ? P1' Mo1' Mo2' 53.22(5) . . ? Sb1' Mo1' Mo2' 55.54(3) . . ? C4' Mo2' C3' 87.7(3) . . ? C4' Mo2' C17' 95.3(3) . . ? C3' Mo2' C17' 90.8(3) . . ? C4' Mo2' C18' 83.7(3) . . ? C3' Mo2' C18' 124.6(3) . . ? C17' Mo2' C18' 36.4(3) . . ? C4' Mo2' C16' 129.9(3) . . ? C3' Mo2' C16' 87.9(3) . . ? C17' Mo2' C16' 35.0(3) . . ? C18' Mo2' C16' 59.1(3) . . ? C4' Mo2' C19' 109.4(3) . . ? C3' Mo2' C19' 145.7(3) . . ? C17' Mo2' C19' 59.0(3) . . ? C18' Mo2' C19' 35.2(3) . . ? C16' Mo2' C19' 58.2(3) . . ? C4' Mo2' C15' 141.6(3) . . ? C3' Mo2' C15' 117.1(3) . . ? C17' Mo2' C15' 58.1(3) . . ? C18' Mo2' C15' 58.4(3) . . ? C16' Mo2' C15' 34.6(3) . . ? C19' Mo2' C15' 34.7(3) . . ? C4' Mo2' P1' 80.7(2) . . ? C3' Mo2' P1' 71.1(2) . . ? C17' Mo2' P1' 161.5(2) . . ? C18' Mo2' P1' 157.4(2) . . ? C16' Mo2' P1' 142.9(2) . . ? C19' Mo2' P1' 139.3(2) . . ? C15' Mo2' P1' 133.2(2) . . ? C4' Mo2' Sb1' 81.4(2) . . ? C3' Mo2' Sb1' 124.9(2) . . ? C17' Mo2' Sb1' 143.7(2) . . ? C18' Mo2' Sb1' 107.6(2) . . ? C16' Mo2' Sb1' 138.2(2) . . ? C19' Mo2' Sb1' 87.8(2) . . ? C15' Mo2' Sb1' 103.6(2) . . ? P1' Mo2' Sb1' 53.96(5) . . ? C4' Mo2' Mo1' 128.6(2) . . ? C3' Mo2' Mo1' 90.3(2) . . ? C17' Mo2' Mo1' 136.1(3) . . ? C18' Mo2' Mo1' 135.7(2) . . ? C16' Mo2' Mo1' 101.2(2) . . ? C19' Mo2' Mo1' 100.5(2) . . ? C15' Mo2' Mo1' 82.7(2) . . ? P1' Mo2' Mo1' 50.52(5) . . ? Sb1' Mo2' Mo1' 58.64(4) . . ? Sb1' P1' Mo1' 72.56(6) . . ? Sb1' P1' W1' 131.97(8) . . ? Mo1' P1' W1' 136.89(8) . . ? Sb1' P1' Mo2' 68.17(5) . . ? Mo1' P1' Mo2' 76.26(6) . . ? W1' P1' Mo2' 140.94(8) . . ? O1' C1' Mo1' 174.3(6) . . ? O2' C2' Mo1' 175.7(7) . . ? O3' C3' Mo2' 176.8(8) . . ? O4' C4' Mo2' 176.9(7) . . ? O5' C5' W1' 175.2(6) . . ? O6' C6' W1' 177.2(7) . . ? O7' C7' W1' 175.6(6) . . ? O8' C8' W1' 176.2(8) . . ? O20' C20' W1' 178.9(6) . . ? C14' C10' C11' 108.6(7) . . ? C14' C10' Mo1' 74.4(5) . . ? C11' C10' Mo1' 70.7(4) . . ? C12' C11' C10' 107.9(8) . . ? C12' C11' Mo1' 72.1(4) . . ? C10' C11' Mo1' 73.4(4) . . ? C11' C12' C13' 107.4(7) . . ? C11' C12' Mo1' 72.1(4) . . ? C13' C12' Mo1' 74.4(4) . . ? C14' C13' C12' 108.6(7) . . ? C14' C13' Mo1' 73.6(4) . . ? C12' C13' Mo1' 69.9(4) . . ? C10' C14' C13' 107.4(8) . . ? C10' C14' Mo1' 70.8(4) . . ? C13' C14' Mo1' 71.6(5) . . ? C16' C15' C19' 108.2(8) . . ? C16' C15' Mo2' 70.9(5) . . ? C19' C15' Mo2' 71.8(5) . . ? C17' C16' C15' 108.9(8) . . ? C17' C16' Mo2' 71.2(5) . . ? C15' C16' Mo2' 74.5(5) . . ? C16' C17' C18' 108.0(8) . . ? C16' C17' Mo2' 73.8(4) . . ? C18' C17' Mo2' 72.6(4) . . ? C19' C18' C17' 106.6(8) . . ? C19' C18' Mo2' 73.8(4) . . ? C17' C18' Mo2' 71.0(4) . . ? C15' C19' C18' 108.3(8) . . ? C15' C19' Mo2' 73.5(4) . . ? C18' C19' Mo2' 71.0(4) . . ? _refine_diff_density_max 1.907 _refine_diff_density_min -2.340 _refine_diff_density_rms 0.219 data_12 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C19 H10 As O9 P W3' _chemical_formula_weight 1039.71 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'As' 'As' 0.0499 2.0058 '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 monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.306(3) _cell_length_b 8.103(2) _cell_length_c 32.374(2) _cell_angle_alpha 90.00 _cell_angle_beta 107.987(7) _cell_angle_gamma 90.00 _cell_volume 4817.1(14) _cell_formula_units_Z 8 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15 _cell_measurement_theta_max 20 _exptl_crystal_description rod _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.867 _exptl_crystal_density_method ? _exptl_crystal_F_000 3728 _exptl_absorpt_coefficient_mu 15.768 _exptl_absorpt_correction_type psiscan _exptl_absorpt_correction_T_min 0.756 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal focus rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku AFC7r' _diffrn_measurement_method \w _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2 _diffrn_reflns_number 4392 _diffrn_reflns_av_R_equivalents 0.1009 _diffrn_reflns_av_sigmaI/netI 0.1149 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3961 _reflns_number_observed 2585 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Rigaku software' _computing_cell_refinement 'Rigaku software' _computing_data_reduction 'TeXsan' _computing_structure_solution 'SIR 92' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL-PLUS' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 9 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 refU _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3952 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1051 _refine_ls_R_factor_obs 0.0440 _refine_ls_wR_factor_all 0.1730 _refine_ls_wR_factor_obs 0.1150 _refine_ls_goodness_of_fit_all 0.829 _refine_ls_goodness_of_fit_obs 0.799 _refine_ls_restrained_S_all 0.955 _refine_ls_restrained_S_obs 0.799 _refine_ls_shift/esd_max 0.007 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group W1 W 0.64679(4) 0.13609(10) 0.18979(2) 0.0348(2) Uani 1 d . . W2 W 0.55249(4) 0.28676(10) 0.10513(2) 0.0334(2) Uani 1 d . . W3 W 0.78097(4) 0.19212(11) 0.08903(2) 0.0390(2) Uani 1 d . . As1 As 0.66380(11) 0.4339(2) 0.16543(6) 0.0371(5) Uani 1 d . . P1 P 0.6824(2) 0.2302(5) 0.12435(13) 0.0260(10) Uani 1 d . . O11 O 0.4877(9) 0.5297(24) 0.1596(6) 0.084(6) Uani 1 d . . O12 O 0.5735(10) 0.5985(21) 0.0532(5) 0.074(5) Uani 1 d . . O13 O 0.6508(13) -0.1819(21) 0.1358(5) 0.090(7) Uani 1 d . . O14 O 0.8163(10) 0.0990(23) 0.2254(6) 0.078(5) Uani 1 d . . O15 O 0.8281(11) -0.1451(26) 0.1381(7) 0.096(7) Uani 1 d . . O16 O 0.6652(11) 0.0002(29) 0.0138(5) 0.095(7) Uani 1 d . . O17 O 0.7332(12) 0.5394(24) 0.0452(7) 0.097(7) Uani 1 d . . O18 O 0.8978(10) 0.3813(28) 0.1655(6) 0.096(7) Uani 1 d . . O19 O 0.9002(9) 0.1663(21) 0.0407(6) 0.076(6) Uani 1 d . . C1 C 0.5908(13) 0.2589(31) 0.2373(7) 0.057(6) Uani 1 d . . H1 H 0.5831(13) 0.3720(31) 0.2381(7) 0.069 Uiso 1 calc R . C2 C 0.5420(13) 0.1384(44) 0.2116(8) 0.078(9) Uani 1 d . . H2 H 0.4967(13) 0.1618(44) 0.1917(8) 0.093 Uiso 1 calc R . C3 C 0.5713(14) -0.0160(34) 0.2203(8) 0.062(7) Uani 1 d . . H3 H 0.5504(14) -0.1145(34) 0.2078(8) 0.074 Uiso 1 calc R . C4 C 0.6398(15) 0.0036(34) 0.2524(7) 0.072(8) Uani 1 d . . H4 H 0.6708(15) -0.0824(34) 0.2654(7) 0.087 Uiso 1 calc R . C5 C 0.6539(13) 0.1684(33) 0.2615(6) 0.058(7) Uani 1 d . . H5 H 0.6967(13) 0.2128(33) 0.2800(6) 0.069 Uiso 1 calc R . C6 C 0.5039(14) 0.1795(28) 0.0361(5) 0.059(7) Uani 1 d . . H6 H 0.5210(14) 0.2147(28) 0.0137(5) 0.071 Uiso 1 calc R . C7 C 0.4459(14) 0.2548(28) 0.0492(7) 0.059(7) Uani 1 d . . H7 H 0.4183(14) 0.3470(28) 0.0372(7) 0.071 Uiso 1 calc R . C8 C 0.4407(12) 0.1597(31) 0.0832(9) 0.066(7) Uani 1 d . . H8 H 0.4076(12) 0.1823(31) 0.0981(9) 0.080 Uiso 1 calc R . C9 C 0.4894(11) 0.0248(27) 0.0938(6) 0.046(5) Uani 1 d . . H9 H 0.4947(11) -0.0559(27) 0.1150(6) 0.055 Uiso 1 calc R . C10 C 0.5288(12) 0.0470(24) 0.0627(6) 0.044(5) Uani 1 d . . H10 H 0.5666(12) -0.0210(24) 0.0610(6) 0.053 Uiso 1 calc R . C11 C 0.5133(11) 0.4411(32) 0.1398(7) 0.056(6) Uani 1 d . . C12 C 0.5697(11) 0.4874(27) 0.0719(7) 0.052(6) Uani 1 d . . C13 C 0.6472(12) -0.0660(24) 0.1547(6) 0.045(5) Uani 1 d . . C14 C 0.7521(13) 0.1170(23) 0.2119(7) 0.047(5) Uani 1 d . . C15 C 0.8108(14) -0.0282(30) 0.1193(7) 0.059(7) Uani 1 d . . C16 C 0.7058(13) 0.0660(31) 0.0394(7) 0.058(6) Uani 1 d . . C17 C 0.7476(15) 0.4165(30) 0.0596(8) 0.062(7) Uani 1 d . . C18 C 0.8547(14) 0.3105(39) 0.1391(8) 0.075(8) Uani 1 d . . C19 C 0.8573(12) 0.1714(32) 0.0597(7) 0.061(7) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.0409(5) 0.0342(4) 0.0279(4) 0.0028(3) 0.0088(3) -0.0025(4) W2 0.0315(4) 0.0343(4) 0.0299(4) -0.0035(3) 0.0028(3) 0.0025(4) W3 0.0362(5) 0.0485(5) 0.0337(4) -0.0008(4) 0.0129(4) 0.0010(4) As1 0.0412(12) 0.0283(10) 0.0349(10) -0.0031(8) 0.0014(9) -0.0021(9) P1 0.028(2) 0.024(2) 0.025(2) 0.006(2) 0.008(2) 0.005(2) O11 0.065(11) 0.107(15) 0.084(12) -0.049(12) 0.027(10) 0.030(11) O12 0.087(13) 0.055(11) 0.070(11) 0.032(9) 0.010(10) -0.009(10) O13 0.152(20) 0.046(11) 0.062(11) -0.012(9) 0.018(12) 0.003(12) O14 0.063(12) 0.084(14) 0.083(12) 0.023(10) 0.016(10) 0.031(11) O15 0.098(15) 0.093(15) 0.108(15) 0.062(13) 0.047(13) 0.045(13) O16 0.079(13) 0.138(19) 0.060(11) -0.021(12) 0.010(10) -0.044(14) O17 0.120(18) 0.058(12) 0.119(16) 0.035(12) 0.048(14) 0.019(12) O18 0.069(13) 0.142(19) 0.078(12) -0.051(13) 0.023(10) -0.054(13) O19 0.056(10) 0.074(12) 0.126(15) 0.004(11) 0.069(11) 0.015(9) C1 0.057(14) 0.072(16) 0.057(14) -0.010(13) 0.039(12) -0.011(14) C2 0.046(15) 0.144(29) 0.050(14) -0.007(17) 0.024(12) -0.021(18) C3 0.066(17) 0.057(16) 0.067(15) 0.002(13) 0.027(14) -0.028(14) C4 0.073(18) 0.074(19) 0.061(15) 0.029(14) 0.008(14) -0.001(16) C5 0.055(15) 0.094(20) 0.018(9) 0.010(11) 0.003(9) -0.002(14) C6 0.094(19) 0.065(15) 0.005(8) -0.002(9) -0.003(10) 0.012(14) C7 0.082(18) 0.034(12) 0.045(12) 0.007(10) -0.005(12) 0.001(12) C8 0.031(12) 0.064(16) 0.098(19) -0.040(15) 0.012(13) -0.006(12) C9 0.051(13) 0.059(14) 0.032(10) -0.011(10) 0.019(9) -0.019(12) C10 0.051(13) 0.038(11) 0.031(10) -0.021(9) -0.003(9) -0.006(10) C11 0.031(12) 0.078(17) 0.044(12) 0.005(12) -0.009(10) 0.018(12) C12 0.038(12) 0.041(13) 0.051(12) 0.004(11) -0.026(10) 0.007(11) C13 0.060(14) 0.022(10) 0.043(11) 0.015(9) 0.000(10) 0.008(10) C14 0.067(16) 0.022(10) 0.048(12) -0.004(9) 0.012(11) 0.007(11) C15 0.090(19) 0.059(15) 0.050(13) 0.002(12) 0.051(13) 0.022(14) C16 0.054(14) 0.075(17) 0.037(11) -0.015(12) 0.006(11) -0.027(13) C17 0.097(21) 0.048(15) 0.058(14) 0.006(12) 0.049(14) 0.019(14) C18 0.062(17) 0.113(24) 0.059(15) -0.025(16) 0.034(14) -0.002(17) C19 0.040(13) 0.087(19) 0.041(12) -0.003(12) -0.010(10) 0.003(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 C14 1.94(2) . ? W1 C13 1.99(2) . ? W1 C5 2.30(2) . ? W1 C4 2.33(2) . ? W1 C2 2.34(2) . ? W1 C3 2.35(2) . ? W1 C1 2.36(2) . ? W1 P1 2.537(4) . ? W1 As1 2.591(2) . ? W1 W2 3.0388(11) . ? W2 C11 1.98(2) . ? W2 C12 2.03(2) . ? W2 C8 2.30(2) . ? W2 C7 2.30(2) . ? W2 C6 2.31(2) . ? W2 C10 2.34(2) . ? W2 C9 2.42(2) . ? W2 P1 2.433(4) . ? W2 As1 2.694(2) . ? W3 C19 1.99(3) . ? W3 C15 2.03(2) . ? W3 C18 2.04(3) . ? W3 C17 2.06(2) . ? W3 C16 2.07(2) . ? W3 P1 2.524(4) . ? As1 P1 2.217(5) . ? O11 C11 1.17(3) . ? O12 C12 1.10(2) . ? O13 C13 1.14(2) . ? O14 C14 1.19(3) . ? O15 C15 1.12(3) . ? O16 C16 1.09(2) . ? O17 C17 1.10(3) . ? O18 C18 1.15(3) . ? O19 C19 1.17(3) . ? C1 C5 1.43(3) . ? C1 C2 1.43(3) . ? C1 H1 0.93 . ? C2 C3 1.37(4) . ? C2 H2 0.93 . ? C3 C4 1.42(3) . ? C3 H3 0.93 . ? C4 C5 1.38(3) . ? C4 H4 0.93 . ? C5 H5 0.93 . ? C6 C10 1.37(3) . ? C6 C7 1.45(3) . ? C6 H6 0.93 . ? C7 C8 1.37(3) . ? C7 H7 0.93 . ? C8 C9 1.41(3) . ? C8 H8 0.93 . ? C9 C10 1.45(3) . ? C9 H9 0.93 . ? C10 H10 0.93 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C14 W1 C13 87.5(8) . . ? C14 W1 C5 84.7(8) . . ? C13 W1 C5 131.2(8) . . ? C14 W1 C4 88.8(9) . . ? C13 W1 C4 97.3(9) . . ? C5 W1 C4 34.6(8) . . ? C14 W1 C2 142.6(9) . . ? C13 W1 C2 109.5(10) . . ? C5 W1 C2 58.8(8) . . ? C4 W1 C2 56.9(9) . . ? C14 W1 C3 121.2(9) . . ? C13 W1 C3 85.5(9) . . ? C5 W1 C3 59.0(8) . . ? C4 W1 C3 35.2(8) . . ? C2 W1 C3 33.9(9) . . ? C14 W1 C1 115.7(8) . . ? C13 W1 C1 143.3(9) . . ? C5 W1 C1 35.8(8) . . ? C4 W1 C1 57.8(9) . . ? C2 W1 C1 35.5(8) . . ? C3 W1 C1 58.5(9) . . ? C14 W1 P1 79.0(6) . . ? C13 W1 P1 73.8(6) . . ? C5 W1 P1 149.5(7) . . ? C4 W1 P1 165.1(7) . . ? C2 W1 P1 137.0(7) . . ? C3 W1 P1 150.8(6) . . ? C1 W1 P1 135.6(6) . . ? C14 W1 As1 88.3(6) . . ? C13 W1 As1 124.6(6) . . ? C5 W1 As1 103.2(7) . . ? C4 W1 As1 137.7(7) . . ? C2 W1 As1 106.7(9) . . ? C3 W1 As1 140.4(7) . . ? C1 W1 As1 86.1(6) . . ? P1 W1 As1 51.22(11) . . ? C14 W1 W2 129.2(6) . . ? C13 W1 W2 85.6(5) . . ? C5 W1 W2 134.2(6) . . ? C4 W1 W2 142.1(7) . . ? C2 W1 W2 86.3(7) . . ? C3 W1 W2 108.3(6) . . ? C1 W1 W2 98.7(6) . . ? P1 W1 W2 50.77(10) . . ? As1 W1 W2 56.51(5) . . ? C11 W2 C12 87.0(9) . . ? C11 W2 C8 88.3(9) . . ? C12 W2 C8 119.1(9) . . ? C11 W2 C7 96.4(9) . . ? C12 W2 C7 85.8(8) . . ? C8 W2 C7 34.7(8) . . ? C11 W2 C6 132.4(8) . . ? C12 W2 C6 82.7(8) . . ? C8 W2 C6 58.0(9) . . ? C7 W2 C6 36.7(8) . . ? C11 W2 C10 144.7(9) . . ? C12 W2 C10 112.8(8) . . ? C8 W2 C10 56.7(8) . . ? C7 W2 C10 58.6(8) . . ? C6 W2 C10 34.2(7) . . ? C11 W2 C9 112.2(9) . . ? C12 W2 C9 141.2(7) . . ? C8 W2 C9 34.8(8) . . ? C7 W2 C9 59.7(7) . . ? C6 W2 C9 59.2(7) . . ? C10 W2 C9 35.4(7) . . ? C11 W2 P1 121.2(6) . . ? C12 W2 P1 87.8(6) . . ? C8 W2 P1 142.2(6) . . ? C7 W2 P1 141.4(7) . . ? C6 W2 P1 104.8(7) . . ? C10 W2 P1 89.6(5) . . ? C9 W2 P1 107.7(5) . . ? C11 W2 As1 70.7(6) . . ? C12 W2 As1 78.8(5) . . ? C8 W2 As1 152.3(7) . . ? C7 W2 As1 160.2(6) . . ? C6 W2 As1 149.6(7) . . ? C10 W2 As1 139.5(5) . . ? C9 W2 As1 138.6(5) . . ? P1 W2 As1 50.93(11) . . ? C11 W2 W1 88.3(6) . . ? C12 W2 W1 130.4(5) . . ? C8 W2 W1 110.1(7) . . ? C7 W2 W1 143.8(6) . . ? C6 W2 W1 132.3(6) . . ? C10 W2 W1 98.6(5) . . ? C9 W2 W1 85.3(5) . . ? P1 W2 W1 53.88(10) . . ? As1 W2 W1 53.32(5) . . ? C19 W3 C15 90.8(9) . . ? C19 W3 C18 88.9(9) . . ? C15 W3 C18 90.4(11) . . ? C19 W3 C17 91.4(10) . . ? C15 W3 C17 177.8(9) . . ? C18 W3 C17 89.7(11) . . ? C19 W3 C16 91.9(9) . . ? C15 W3 C16 88.1(10) . . ? C18 W3 C16 178.3(11) . . ? C17 W3 C16 91.8(10) . . ? C19 W3 P1 177.4(7) . . ? C15 W3 P1 91.7(6) . . ? C18 W3 P1 91.2(7) . . ? C17 W3 P1 86.0(6) . . ? C16 W3 P1 88.0(6) . . ? P1 As1 W1 63.15(12) . . ? P1 As1 W2 58.43(12) . . ? W1 As1 W2 70.17(5) . . ? As1 P1 W2 70.64(14) . . ? As1 P1 W3 130.3(2) . . ? W2 P1 W3 140.3(2) . . ? As1 P1 W1 65.63(12) . . ? W2 P1 W1 75.35(13) . . ? W3 P1 W1 141.1(2) . . ? C5 C1 C2 105.4(23) . . ? C5 C1 W1 69.9(12) . . ? C2 C1 W1 71.6(13) . . ? C5 C1 H1 127.3(14) . . ? C2 C1 H1 127.3(17) . . ? W1 C1 H1 122.9(6) . . ? C3 C2 C1 110.3(24) . . ? C3 C2 W1 73.4(14) . . ? C1 C2 W1 72.8(12) . . ? C3 C2 H2 124.8(15) . . ? C1 C2 H2 124.8(17) . . ? W1 C2 H2 120.6(6) . . ? C2 C3 C4 106.4(23) . . ? C2 C3 W1 72.7(14) . . ? C4 C3 W1 71.8(13) . . ? C2 C3 H3 126.8(15) . . ? C4 C3 H3 126.8(16) . . ? W1 C3 H3 120.6(6) . . ? C5 C4 C3 110.1(23) . . ? C5 C4 W1 71.3(12) . . ? C3 C4 W1 73.0(13) . . ? C5 C4 H4 124.9(14) . . ? C3 C4 H4 124.9(16) . . ? W1 C4 H4 122.4(7) . . ? C4 C5 C1 107.5(22) . . ? C4 C5 W1 74.1(13) . . ? C1 C5 W1 74.3(11) . . ? C4 C5 H5 126.3(15) . . ? C1 C5 H5 126.3(14) . . ? W1 C5 H5 117.3(6) . . ? C10 C6 C7 107.3(20) . . ? C10 C6 W2 74.1(10) . . ? C7 C6 W2 71.2(11) . . ? C10 C6 H6 126.3(14) . . ? C7 C6 H6 126.3(12) . . ? W2 C6 H6 120.2(6) . . ? C8 C7 C6 104.6(20) . . ? C8 C7 W2 72.6(13) . . ? C6 C7 W2 72.1(12) . . ? C8 C7 H7 127.7(15) . . ? C6 C7 H7 127.7(12) . . ? W2 C7 H7 119.7(6) . . ? C7 C8 C9 115.0(22) . . ? C7 C8 W2 72.7(14) . . ? C9 C8 W2 77.3(12) . . ? C7 C8 H8 122.5(15) . . ? C9 C8 H8 122.5(14) . . ? W2 C8 H8 118.8(6) . . ? C8 C9 C10 100.8(19) . . ? C8 C9 W2 67.9(12) . . ? C10 C9 W2 69.4(10) . . ? C8 C9 H9 129.6(14) . . ? C10 C9 H9 129.6(12) . . ? W2 C9 H9 124.8(5) . . ? C6 C10 C9 112.2(20) . . ? C6 C10 W2 71.7(11) . . ? C9 C10 W2 75.2(11) . . ? C6 C10 H10 123.9(14) . . ? C9 C10 H10 123.9(12) . . ? W2 C10 H10 120.7(5) . . ? O11 C11 W2 177.6(20) . . ? O12 C12 W2 174.5(21) . . ? O13 C13 W1 176.8(21) . . ? O14 C14 W1 177.5(18) . . ? O15 C15 W3 176.0(21) . . ? O16 C16 W3 178.4(22) . . ? O17 C17 W3 176.3(25) . . ? O18 C18 W3 176.0(23) . . ? O19 C19 W3 176.0(21) . . ? 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 C14 W1 W2 C11 -121.1(10) . . . . ? C13 W1 W2 C11 155.7(10) . . . . ? C5 W1 W2 C11 7.7(11) . . . . ? C4 W1 W2 C11 59.4(14) . . . . ? C2 W1 W2 C11 45.8(11) . . . . ? C3 W1 W2 C11 72.0(10) . . . . ? C1 W1 W2 C11 12.4(9) . . . . ? P1 W1 W2 C11 -131.6(7) . . . . ? As1 W1 W2 C11 -67.0(7) . . . . ? C14 W1 W2 C12 -36.5(11) . . . . ? C13 W1 W2 C12 -119.6(11) . . . . ? C5 W1 W2 C12 92.4(13) . . . . ? C4 W1 W2 C12 144.1(15) . . . . ? C2 W1 W2 C12 130.5(12) . . . . ? C3 W1 W2 C12 156.6(11) . . . . ? C1 W1 W2 C12 97.1(10) . . . . ? P1 W1 W2 C12 -46.9(9) . . . . ? As1 W1 W2 C12 17.7(9) . . . . ? C14 W1 W2 C8 151.2(9) . . . . ? C13 W1 W2 C8 68.1(9) . . . . ? C5 W1 W2 C8 -79.9(11) . . . . ? C4 W1 W2 C8 -28.2(13) . . . . ? C2 W1 W2 C8 -41.8(10) . . . . ? C3 W1 W2 C8 -15.6(9) . . . . ? C1 W1 W2 C8 -75.2(8) . . . . ? P1 W1 W2 C8 140.8(6) . . . . ? As1 W1 W2 C8 -154.6(6) . . . . ? C14 W1 W2 C7 140.3(13) . . . . ? C13 W1 W2 C7 57.2(13) . . . . ? C5 W1 W2 C7 -90.8(15) . . . . ? C4 W1 W2 C7 -39.1(16) . . . . ? C2 W1 W2 C7 -52.7(14) . . . . ? C3 W1 W2 C7 -26.5(13) . . . . ? C1 W1 W2 C7 -86.1(13) . . . . ? P1 W1 W2 C7 129.9(11) . . . . ? As1 W1 W2 C7 -165.5(11) . . . . ? C14 W1 W2 C6 86.7(12) . . . . ? C13 W1 W2 C6 3.6(11) . . . . ? C5 W1 W2 C6 -144.4(13) . . . . ? C4 W1 W2 C6 -92.7(15) . . . . ? C2 W1 W2 C6 -106.3(12) . . . . ? C3 W1 W2 C6 -80.1(11) . . . . ? C1 W1 W2 C6 -139.7(11) . . . . ? P1 W1 W2 C6 76.3(9) . . . . ? As1 W1 W2 C6 140.9(9) . . . . ? C14 W1 W2 C10 93.6(9) . . . . ? C13 W1 W2 C10 10.5(8) . . . . ? C5 W1 W2 C10 -137.6(11) . . . . ? C4 W1 W2 C10 -85.8(13) . . . . ? C2 W1 W2 C10 -99.5(10) . . . . ? C3 W1 W2 C10 -73.3(9) . . . . ? C1 W1 W2 C10 -132.8(8) . . . . ? P1 W1 W2 C10 83.2(6) . . . . ? As1 W1 W2 C10 147.7(6) . . . . ? C14 W1 W2 C9 126.4(9) . . . . ? C13 W1 W2 C9 43.3(8) . . . . ? C5 W1 W2 C9 -104.7(10) . . . . ? C4 W1 W2 C9 -53.0(12) . . . . ? C2 W1 W2 C9 -66.6(10) . . . . ? C3 W1 W2 C9 -40.4(9) . . . . ? C1 W1 W2 C9 -100.0(7) . . . . ? P1 W1 W2 C9 116.0(5) . . . . ? As1 W1 W2 C9 -179.4(5) . . . . ? C14 W1 W2 P1 10.4(7) . . . . ? C13 W1 W2 P1 -72.7(7) . . . . ? C5 W1 W2 P1 139.3(9) . . . . ? C4 W1 W2 P1 -169.0(12) . . . . ? C2 W1 W2 P1 177.4(8) . . . . ? C3 W1 W2 P1 -156.4(7) . . . . ? C1 W1 W2 P1 144.0(6) . . . . ? P1 W1 W2 P1 0.0 . . . . ? As1 W1 W2 P1 64.57(14) . . . . ? C14 W1 W2 As1 -54.1(7) . . . . ? C13 W1 W2 As1 -137.3(7) . . . . ? C5 W1 W2 As1 74.7(9) . . . . ? C4 W1 W2 As1 126.4(12) . . . . ? C2 W1 W2 As1 112.8(8) . . . . ? C3 W1 W2 As1 139.0(7) . . . . ? C1 W1 W2 As1 79.4(6) . . . . ? P1 W1 W2 As1 -64.57(14) . . . . ? As1 W1 W2 As1 0.0 . . . . ? C14 W1 As1 P1 77.2(6) . . . . ? C13 W1 As1 P1 -8.5(8) . . . . ? C5 W1 As1 P1 161.4(6) . . . . ? C4 W1 As1 P1 163.5(10) . . . . ? C2 W1 As1 P1 -137.6(6) . . . . ? C3 W1 As1 P1 -141.7(9) . . . . ? C1 W1 As1 P1 -166.9(6) . . . . ? P1 W1 As1 P1 0.0 . . . . ? W2 W1 As1 P1 -63.82(13) . . . . ? C14 W1 As1 W2 141.1(6) . . . . ? C13 W1 As1 W2 55.3(8) . . . . ? C5 W1 As1 W2 -134.8(6) . . . . ? C4 W1 As1 W2 -132.7(10) . . . . ? C2 W1 As1 W2 -73.8(6) . . . . ? C3 W1 As1 W2 -77.9(9) . . . . ? C1 W1 As1 W2 -103.1(6) . . . . ? P1 W1 As1 W2 63.82(13) . . . . ? W2 W1 As1 W2 0.0 . . . . ? C11 W2 As1 P1 172.8(7) . . . . ? C12 W2 As1 P1 -96.4(7) . . . . ? C8 W2 As1 P1 130.0(14) . . . . ? C7 W2 As1 P1 -135.8(20) . . . . ? C6 W2 As1 P1 -42.8(11) . . . . ? C10 W2 As1 P1 15.7(8) . . . . ? C9 W2 As1 P1 70.9(7) . . . . ? P1 W2 As1 P1 0.0 . . . . ? W1 W2 As1 P1 70.00(13) . . . . ? C11 W2 As1 W1 102.8(7) . . . . ? C12 W2 As1 W1 -166.4(7) . . . . ? C8 W2 As1 W1 60.0(14) . . . . ? C7 W2 As1 W1 154.2(20) . . . . ? C6 W2 As1 W1 -112.8(11) . . . . ? C10 W2 As1 W1 -54.3(8) . . . . ? C9 W2 As1 W1 0.9(7) . . . . ? P1 W2 As1 W1 -70.00(13) . . . . ? W1 W2 As1 W1 0.0 . . . . ? W1 As1 P1 W2 82.23(9) . . . . ? W2 As1 P1 W2 0.0 . . . . ? W1 As1 P1 W3 -137.4(3) . . . . ? W2 As1 P1 W3 140.4(3) . . . . ? W1 As1 P1 W1 0.0 . . . . ? W2 As1 P1 W1 -82.23(9) . . . . ? C11 W2 P1 As1 -7.9(8) . . . . ? C12 W2 P1 As1 77.3(6) . . . . ? C8 W2 P1 As1 -144.5(12) . . . . ? C7 W2 P1 As1 157.7(9) . . . . ? C6 W2 P1 As1 159.1(6) . . . . ? C10 W2 P1 As1 -169.9(5) . . . . ? C9 W2 P1 As1 -139.0(5) . . . . ? As1 W2 P1 As1 0.0 . . . . ? W1 W2 P1 As1 -68.89(10) . . . . ? C11 W2 P1 W3 -138.4(8) . . . . ? C12 W2 P1 W3 -53.2(7) . . . . ? C8 W2 P1 W3 84.9(12) . . . . ? C7 W2 P1 W3 27.2(10) . . . . ? C6 W2 P1 W3 28.6(7) . . . . ? C10 W2 P1 W3 59.6(6) . . . . ? C9 W2 P1 W3 90.5(5) . . . . ? As1 W2 P1 W3 -130.5(3) . . . . ? W1 W2 P1 W3 160.6(4) . . . . ? C11 W2 P1 W1 61.0(8) . . . . ? C12 W2 P1 W1 146.2(6) . . . . ? C8 W2 P1 W1 -75.6(12) . . . . ? C7 W2 P1 W1 -133.4(9) . . . . ? C6 W2 P1 W1 -132.0(6) . . . . ? C10 W2 P1 W1 -101.0(5) . . . . ? C9 W2 P1 W1 -70.1(5) . . . . ? As1 W2 P1 W1 68.89(10) . . . . ? W1 W2 P1 W1 0.0 . . . . ? C19 W3 P1 As1 -60.2(141) . . . . ? C15 W3 P1 As1 123.4(8) . . . . ? C18 W3 P1 As1 33.0(9) . . . . ? C17 W3 P1 As1 -56.6(8) . . . . ? C16 W3 P1 As1 -148.5(7) . . . . ? C19 W3 P1 W2 49.7(141) . . . . ? C15 W3 P1 W2 -126.7(8) . . . . ? C18 W3 P1 W2 142.9(9) . . . . ? C17 W3 P1 W2 53.3(8) . . . . ? C16 W3 P1 W2 -38.6(7) . . . . ? C19 W3 P1 W1 -161.1(140) . . . . ? C15 W3 P1 W1 22.5(8) . . . . ? C18 W3 P1 W1 -67.9(9) . . . . ? C17 W3 P1 W1 -157.5(8) . . . . ? C16 W3 P1 W1 110.6(7) . . . . ? C14 W1 P1 As1 -96.7(6) . . . . ? C13 W1 P1 As1 172.7(6) . . . . ? C5 W1 P1 As1 -37.8(12) . . . . ? C4 W1 P1 As1 -132.0(26) . . . . ? C2 W1 P1 As1 71.2(12) . . . . ? C3 W1 P1 As1 126.1(15) . . . . ? C1 W1 P1 As1 18.9(8) . . . . ? As1 W1 P1 As1 0.0 . . . . ? W2 W1 P1 As1 75.07(11) . . . . ? C14 W1 P1 W2 -171.8(6) . . . . ? C13 W1 P1 W2 97.7(6) . . . . ? C5 W1 P1 W2 -112.9(12) . . . . ? C4 W1 P1 W2 152.9(26) . . . . ? C2 W1 P1 W2 -3.8(12) . . . . ? C3 W1 P1 W2 51.0(15) . . . . ? C1 W1 P1 W2 -56.2(8) . . . . ? As1 W1 P1 W2 -75.07(11) . . . . ? W2 W1 P1 W2 0.0 . . . . ? C14 W1 P1 W3 28.0(6) . . . . ? C13 W1 P1 W3 -62.6(7) . . . . ? C5 W1 P1 W3 86.9(12) . . . . ? C4 W1 P1 W3 -7.3(27) . . . . ? C2 W1 P1 W3 -164.1(12) . . . . ? C3 W1 P1 W3 -109.2(15) . . . . ? C1 W1 P1 W3 143.6(8) . . . . ? As1 W1 P1 W3 124.7(3) . . . . ? W2 W1 P1 W3 -160.2(4) . . . . ? C14 W1 C1 C5 -32.8(17) . . . . ? C13 W1 C1 C5 91.5(18) . . . . ? C5 W1 C1 C5 0.000(11) . . . . ? C4 W1 C1 C5 37.9(14) . . . . ? C2 W1 C1 C5 114.8(22) . . . . ? C3 W1 C1 C5 79.6(15) . . . . ? P1 W1 C1 C5 -133.6(13) . . . . ? As1 W1 C1 C5 -119.0(14) . . . . ? W2 W1 C1 C5 -174.2(13) . . . . ? C14 W1 C1 C2 -147.6(17) . . . . ? C13 W1 C1 C2 -23.3(23) . . . . ? C5 W1 C1 C2 -114.8(22) . . . . ? C4 W1 C1 C2 -76.9(17) . . . . ? C2 W1 C1 C2 0.000(3) . . . . ? C3 W1 C1 C2 -35.2(15) . . . . ? P1 W1 C1 C2 111.6(16) . . . . ? As1 W1 C1 C2 126.2(17) . . . . ? W2 W1 C1 C2 71.0(16) . . . . ? C5 C1 C2 C3 2.2(25) . . . . ? W1 C1 C2 C3 64.3(18) . . . . ? C5 C1 C2 W1 -62.1(14) . . . . ? W1 C1 C2 W1 0.000(2) . . . . ? C14 W1 C2 C3 -65.4(23) . . . . ? C13 W1 C2 C3 47.3(17) . . . . ? C5 W1 C2 C3 -79.8(16) . . . . ? C4 W1 C2 C3 -38.7(15) . . . . ? C3 W1 C2 C3 0.000(7) . . . . ? C1 W1 C2 C3 -118.2(23) . . . . ? P1 W1 C2 C3 134.3(13) . . . . ? As1 W1 C2 C3 -175.3(14) . . . . ? W2 W1 C2 C3 131.3(15) . . . . ? C14 W1 C2 C1 52.7(26) . . . . ? C13 W1 C2 C1 165.5(15) . . . . ? C5 W1 C2 C1 38.4(14) . . . . ? C4 W1 C2 C1 79.4(16) . . . . ? C3 W1 C2 C1 118.2(23) . . . . ? C1 W1 C2 C1 0.000(3) . . . . ? P1 W1 C2 C1 -107.6(14) . . . . ? As1 W1 C2 C1 -57.2(16) . . . . ? W2 W1 C2 C1 -110.5(16) . . . . ? C1 C2 C3 C4 0.4(27) . . . . ? W1 C2 C3 C4 64.4(17) . . . . ? C1 C2 C3 W1 -64.0(16) . . . . ? W1 C2 C3 W1 0.000(3) . . . . ? C14 W1 C3 C2 139.7(15) . . . . ? C13 W1 C3 C2 -136.0(16) . . . . ? C5 W1 C3 C2 79.1(16) . . . . ? C4 W1 C3 C2 114.5(23) . . . . ? C2 W1 C3 C2 0.000(8) . . . . ? C1 W1 C3 C2 36.9(15) . . . . ? P1 W1 C3 C2 -91.5(19) . . . . ? As1 W1 C3 C2 7.1(20) . . . . ? W2 W1 C3 C2 -52.1(16) . . . . ? C14 W1 C3 C4 25.3(20) . . . . ? C13 W1 C3 C4 109.6(17) . . . . ? C5 W1 C3 C4 -35.4(16) . . . . ? C4 W1 C3 C4 0.000(5) . . . . ? C2 W1 C3 C4 -114.5(23) . . . . ? C1 W1 C3 C4 -77.5(17) . . . . ? P1 W1 C3 C4 154.1(14) . . . . ? As1 W1 C3 C4 -107.4(17) . . . . ? W2 W1 C3 C4 -166.6(15) . . . . ? C2 C3 C4 C5 -3.0(29) . . . . ? W1 C3 C4 C5 62.0(18) . . . . ? C2 C3 C4 W1 -65.0(17) . . . . ? W1 C3 C4 W1 0.000(1) . . . . ? C14 W1 C4 C5 82.5(16) . . . . ? C13 W1 C4 C5 169.8(16) . . . . ? C5 W1 C4 C5 0.000(9) . . . . ? C2 W1 C4 C5 -81.7(18) . . . . ? C3 W1 C4 C5 -119.0(24) . . . . ? C1 W1 C4 C5 -39.2(15) . . . . ? P1 W1 C4 C5 117.0(26) . . . . ? As1 W1 C4 C5 -3.6(21) . . . . ? W2 W1 C4 C5 -98.0(16) . . . . ? C14 W1 C4 C3 -158.6(17) . . . . ? C13 W1 C4 C3 -71.3(18) . . . . ? C5 W1 C4 C3 119.0(24) . . . . ? C2 W1 C4 C3 37.3(15) . . . . ? C3 W1 C4 C3 0.000(4) . . . . ? C1 W1 C4 C3 79.7(17) . . . . ? P1 W1 C4 C3 -124.0(24) . . . . ? As1 W1 C4 C3 115.4(16) . . . . ? W2 W1 C4 C3 21.0(23) . . . . ? C3 C4 C5 C1 4.4(27) . . . . ? W1 C4 C5 C1 67.4(14) . . . . ? C3 C4 C5 W1 -63.0(18) . . . . ? W1 C4 C5 W1 0.000(3) . . . . ? C2 C1 C5 C4 -4.0(24) . . . . ? W1 C1 C5 C4 -67.3(16) . . . . ? C2 C1 C5 W1 63.3(14) . . . . ? W1 C1 C5 W1 0.000(5) . . . . ? C14 W1 C5 C4 -95.5(16) . . . . ? C13 W1 C5 C4 -13.6(21) . . . . ? C4 W1 C5 C4 0.000(6) . . . . ? C2 W1 C5 C4 75.8(18) . . . . ? C3 W1 C5 C4 36.0(16) . . . . ? C1 W1 C5 C4 113.8(22) . . . . ? P1 W1 C5 C4 -153.1(13) . . . . ? As1 W1 C5 C4 177.5(14) . . . . ? W2 W1 C5 C4 121.8(15) . . . . ? C14 W1 C5 C1 150.6(15) . . . . ? C13 W1 C5 C1 -127.4(15) . . . . ? C4 W1 C5 C1 -113.8(22) . . . . ? C2 W1 C5 C1 -38.0(15) . . . . ? C3 W1 C5 C1 -77.8(15) . . . . ? C1 W1 C5 C1 0.000(10) . . . . ? P1 W1 C5 C1 93.1(16) . . . . ? As1 W1 C5 C1 63.7(14) . . . . ? W2 W1 C5 C1 8.0(18) . . . . ? C11 W2 C6 C10 -128.6(15) . . . . ? C12 W2 C6 C10 152.2(16) . . . . ? C8 W2 C6 C10 -76.7(16) . . . . ? C7 W2 C6 C10 -115.1(21) . . . . ? C10 W2 C6 C10 0.000(1) . . . . ? C9 W2 C6 C10 -35.7(13) . . . . ? P1 W2 C6 C10 66.4(15) . . . . ? As1 W2 C6 C10 99.4(16) . . . . ? W1 W2 C6 C10 12.1(19) . . . . ? C11 W2 C6 C7 -13.6(19) . . . . ? C12 W2 C6 C7 -92.8(14) . . . . ? C8 W2 C6 C7 38.4(13) . . . . ? C7 W2 C6 C7 0.000(1) . . . . ? C10 W2 C6 C7 115.1(21) . . . . ? C9 W2 C6 C7 79.4(14) . . . . ? P1 W2 C6 C7 -178.5(12) . . . . ? As1 W2 C6 C7 -145.5(11) . . . . ? W1 W2 C6 C7 127.2(12) . . . . ? C10 C6 C7 C8 0.0(24) . . . . ? W2 C6 C7 C8 -65.8(15) . . . . ? C10 C6 C7 W2 65.9(14) . . . . ? W2 C6 C7 W2 0.000(2) . . . . ? C11 W2 C7 C8 -77.7(16) . . . . ? C12 W2 C7 C8 -164.3(16) . . . . ? C8 W2 C7 C8 0.000(1) . . . . ? C6 W2 C7 C8 112.3(20) . . . . ? C10 W2 C7 C8 75.7(14) . . . . ? C9 W2 C7 C8 34.2(13) . . . . ? P1 W2 C7 C8 114.6(15) . . . . ? As1 W2 C7 C8 -125.6(17) . . . . ? W1 W2 C7 C8 18.1(21) . . . . ? C11 W2 C7 C6 170.0(14) . . . . ? C12 W2 C7 C6 83.4(14) . . . . ? C8 W2 C7 C6 -112.3(20) . . . . ? C6 W2 C7 C6 0.000(1) . . . . ? C10 W2 C7 C6 -36.6(12) . . . . ? C9 W2 C7 C6 -78.1(13) . . . . ? P1 W2 C7 C6 2.3(18) . . . . ? As1 W2 C7 C6 122.1(18) . . . . ? W1 W2 C7 C6 -94.2(16) . . . . ? C6 C7 C8 C9 -1.0(26) . . . . ? W2 C7 C8 C9 -66.5(16) . . . . ? C6 C7 C8 W2 65.5(15) . . . . ? W2 C7 C8 W2 0.0 . . . . ? C11 W2 C8 C7 103.7(16) . . . . ? C12 W2 C8 C7 18.0(18) . . . . ? C7 W2 C8 C7 0.0 . . . . ? C6 W2 C8 C7 -40.7(14) . . . . ? C10 W2 C8 C7 -81.5(15) . . . . ? C9 W2 C8 C7 -121.6(20) . . . . ? P1 W2 C8 C7 -112.3(16) . . . . ? As1 W2 C8 C7 143.6(13) . . . . ? W1 W2 C8 C7 -168.7(13) . . . . ? C11 W2 C8 C9 -134.7(14) . . . . ? C12 W2 C8 C9 139.6(13) . . . . ? C7 W2 C8 C9 121.6(20) . . . . ? C6 W2 C8 C9 80.9(13) . . . . ? C10 W2 C8 C9 40.1(11) . . . . ? C9 W2 C8 C9 0.0 . . . . ? P1 W2 C8 C9 9.3(21) . . . . ? As1 W2 C8 C9 -94.8(15) . . . . ? W1 W2 C8 C9 -47.1(14) . . . . ? C7 C8 C9 C10 1.4(23) . . . . ? W2 C8 C9 C10 -62.4(12) . . . . ? C7 C8 C9 W2 63.8(17) . . . . ? W2 C8 C9 W2 0.0 . . . . ? C11 W2 C9 C8 50.1(15) . . . . ? C12 W2 C9 C8 -64.6(19) . . . . ? C8 W2 C9 C8 0.0 . . . . ? C7 W2 C9 C8 -34.2(14) . . . . ? C6 W2 C9 C8 -77.1(15) . . . . ? C10 W2 C9 C8 -111.6(18) . . . . ? P1 W2 C9 C8 -174.0(13) . . . . ? As1 W2 C9 C8 135.6(13) . . . . ? W1 W2 C9 C8 136.3(14) . . . . ? C11 W2 C9 C10 161.7(12) . . . . ? C12 W2 C9 C10 47.0(18) . . . . ? C8 W2 C9 C10 111.6(18) . . . . ? C7 W2 C9 C10 77.3(13) . . . . ? C6 W2 C9 C10 34.5(12) . . . . ? C10 W2 C9 C10 0.0 . . . . ? P1 W2 C9 C10 -62.5(12) . . . . ? As1 W2 C9 C10 -112.8(11) . . . . ? W1 W2 C9 C10 -112.1(11) . . . . ? C7 C6 C10 C9 0.9(23) . . . . ? W2 C6 C10 C9 64.8(14) . . . . ? C7 C6 C10 W2 -63.9(14) . . . . ? W2 C6 C10 W2 0.000(2) . . . . ? C8 C9 C10 C6 -1.3(21) . . . . ? W2 C9 C10 C6 -62.7(14) . . . . ? C8 C9 C10 W2 61.3(13) . . . . ? W2 C9 C10 W2 0.0 . . . . ? C11 W2 C10 C6 89.7(19) . . . . ? C12 W2 C10 C6 -30.2(17) . . . . ? C8 W2 C10 C6 80.7(17) . . . . ? C7 W2 C10 C6 39.3(15) . . . . ? C6 W2 C10 C6 0.000(2) . . . . ? C9 W2 C10 C6 120.0(20) . . . . ? P1 W2 C10 C6 -117.6(15) . . . . ? As1 W2 C10 C6 -129.8(13) . . . . ? W1 W2 C10 C6 -171.0(14) . . . . ? C11 W2 C10 C9 -30.3(19) . . . . ? C12 W2 C10 C9 -150.2(12) . . . . ? C8 W2 C10 C9 -39.4(13) . . . . ? C7 W2 C10 C9 -80.7(14) . . . . ? C6 W2 C10 C9 -120.0(20) . . . . ? C9 W2 C10 C9 0.0 . . . . ? P1 W2 C10 C9 122.4(11) . . . . ? As1 W2 C10 C9 110.2(12) . . . . ? W1 W2 C10 C9 69.0(12) . . . . ? C12 W2 C11 O11 114.9(478) . . . . ? C8 W2 C11 O11 -4.4(478) . . . . ? C7 W2 C11 O11 29.5(479) . . . . ? C6 W2 C11 O11 37.6(483) . . . . ? C10 W2 C11 O11 -11.9(485) . . . . ? C9 W2 C11 O11 -30.3(479) . . . . ? P1 W2 C11 O11 -159.5(474) . . . . ? As1 W2 C11 O11 -166.0(480) . . . . ? W1 W2 C11 O11 -114.5(478) . . . . ? C11 W2 C12 O12 -56.3(209) . . . . ? C8 W2 C12 O12 30.1(211) . . . . ? C7 W2 C12 O12 40.3(208) . . . . ? C6 W2 C12 O12 77.0(208) . . . . ? C10 W2 C12 O12 93.6(209) . . . . ? C9 W2 C12 O12 66.2(213) . . . . ? P1 W2 C12 O12 -177.8(1000) . . . . ? As1 W2 C12 O12 -127.2(209) . . . . ? W1 W2 C12 O12 -141.6(205) . . . . ? C14 W1 C13 O13 8.5(346) . . . . ? C5 W1 C13 O13 -72.2(349) . . . . ? C4 W1 C13 O13 -79.9(346) . . . . ? C2 W1 C13 O13 -137.4(345) . . . . ? C3 W1 C13 O13 -113.1(346) . . . . ? C1 W1 C13 O13 -123.2(344) . . . . ? P1 W1 C13 O13 87.8(346) . . . . ? As1 W1 C13 O13 94.7(344) . . . . ? W2 W1 C13 O13 138.1(346) . . . . ? C13 W1 C14 O14 -38.8(426) . . . . ? C5 W1 C14 O14 93.0(426) . . . . ? C4 W1 C14 O14 58.6(426) . . . . ? C2 W1 C14 O14 80.8(427) . . . . ? C3 W1 C14 O14 44.4(428) . . . . ? C1 W1 C14 O14 111.6(425) . . . . ? P1 W1 C14 O14 -112.8(426) . . . . ? As1 W1 C14 O14 -163.6(426) . . . . ? W2 W1 C14 O14 -121.0(424) . . . . ? C19 W3 C15 O15 119.9(334) . . . . ? C18 W3 C15 O15 31.0(334) . . . . ? C17 W3 C15 O15 -60.1(508) . . . . ? C16 W3 C15 O15 -148.2(334) . . . . ? P1 W3 C15 O15 -60.2(334) . . . . ? C19 W3 C16 O16 179.6(1000) . . . . ? C15 W3 C16 O16 88.8(899) . . . . ? C18 W3 C16 O16 62.5(1000) . . . . ? C17 W3 C16 O16 -88.9(899) . . . . ? P1 W3 C16 O16 -3.0(899) . . . . ? C19 W3 C17 O17 -70.6(334) . . . . ? C15 W3 C17 O17 109.4(416) . . . . ? C18 W3 C17 O17 18.3(334) . . . . ? C16 W3 C17 O17 -162.5(334) . . . . ? P1 W3 C17 O17 109.6(334) . . . . ? C19 W3 C18 O18 36.2(377) . . . . ? C15 W3 C18 O18 127.0(377) . . . . ? C17 W3 C18 O18 -55.2(377) . . . . ? C16 W3 C18 O18 153.3(328) . . . . ? P1 W3 C18 O18 -141.2(377) . . . . ? C15 W3 C19 O19 163.4(298) . . . . ? C18 W3 C19 O19 -106.2(298) . . . . ? C17 W3 C19 O19 -16.6(298) . . . . ? C16 W3 C19 O19 75.3(298) . . . . ? P1 W3 C19 O19 -13.0(424) . . . . ? _refine_diff_density_max 1.057 _refine_diff_density_min -1.226 _refine_diff_density_rms 0.267 data_17 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C19 H10 O9 P2 W3' _chemical_formula_weight 995.76 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.255(3) _cell_length_b 8.095(4) _cell_length_c 31.957(4) _cell_angle_alpha 90.00 _cell_angle_beta 106.510(10) _cell_angle_gamma 90.00 _cell_volume 4775.7(25) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'irregular block' _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.770 _exptl_crystal_density_method ? _exptl_crystal_F_000 3584 _exptl_absorpt_coefficient_mu 14.597 _exptl_absorpt_correction_type 'empirical (10 psi scans) ' _exptl_absorpt_correction_T_min 0.334 _exptl_absorpt_correction_T_max 1.000 _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 AFC5R _diffrn_measurement_method 'omega scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1% _diffrn_reflns_number 4356 _diffrn_reflns_av_R_equivalents 0.0500 _diffrn_reflns_av_sigmaI/netI 0.1084 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4223 _reflns_number_observed 2666 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 11 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0319P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4212 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1189 _refine_ls_R_factor_obs 0.0444 _refine_ls_wR_factor_all 0.2240 _refine_ls_wR_factor_obs 0.0891 _refine_ls_goodness_of_fit_all 1.028 _refine_ls_goodness_of_fit_obs 1.095 _refine_ls_restrained_S_all 2.141 _refine_ls_restrained_S_obs 1.095 _refine_ls_shift/esd_max 0.185 _refine_ls_shift/esd_mean 0.008 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group W1 W 1.30189(3) 0.53559(8) 0.10554(2) 0.0321(2) Uani 1 d . . W2 W 1.29124(3) 0.38932(8) 0.19058(2) 0.0330(2) Uani 1 d . . W3 W 1.05756(3) 0.44667(9) 0.08990(2) 0.0384(2) Uani 1 d . . P1 P 1.2512(2) 0.6723(5) 0.16401(14) 0.0352(10) Uani 1 d . . P2 P 1.1912(2) 0.4831(5) 0.12539(14) 0.0327(10) Uani 1 d . . O1 O 1.0161(7) 0.6314(24) 0.1674(5) 0.104(6) Uani 1 d . . C1 C 1.0324(10) 0.5667(26) 0.1394(6) 0.061(6) Uani 1 d . . O2 O 1.0576(8) 0.1060(21) 0.1387(6) 0.102(6) Uani 1 d . . C2 C 1.0584(9) 0.2267(25) 0.1215(6) 0.052(5) Uani 1 d . . C3 C 0.9525(10) 0.4271(23) 0.0594(6) 0.055(5) Uani 1 d . . O3 O 0.8911(6) 0.4146(17) 0.0414(5) 0.074(4) Uani 1 d . . O4 O 1.0987(8) 0.2497(22) 0.0147(5) 0.090(5) Uani 1 d . . C4 C 1.0806(9) 0.3262(29) 0.0402(6) 0.062(6) Uani 1 d . . O5 O 1.0617(8) 0.7966(21) 0.0449(6) 0.098(6) Uani 1 d . . C5 C 1.0611(10) 0.6704(27) 0.0612(7) 0.064(6) Uani 1 d . . C6 C 1.3775(10) 0.6927(25) 0.1417(6) 0.052(5) Uani 1 d . . O6 O 1.4191(8) 0.7807(20) 0.1585(5) 0.093(6) Uani 1 d . . C7 C 1.2525(9) 0.7341(21) 0.0724(5) 0.041(4) Uani 1 d . . O7 O 1.2275(7) 0.8482(17) 0.0533(4) 0.073(4) Uani 1 d . . O8 O 1.2360(8) 0.0664(15) 0.1376(5) 0.076(5) Uani 1 d . . C8 C 1.2555(10) 0.1882(23) 0.1559(6) 0.050(5) Uani 1 d . . C9 C 1.2045(9) 0.3685(22) 0.2129(6) 0.050(5) Uani 1 d . . O9 O 1.1570(7) 0.3581(18) 0.2270(5) 0.073(4) Uani 1 d . . C10 C 1.3524(11) 0.4989(21) 0.0484(6) 0.051(5) Uani 1 d . . H10A H 1.3692(11) 0.5871(21) 0.0327(6) 0.061 Uiso 1 calc R . C11 C 1.3956(10) 0.4097(24) 0.0840(7) 0.058(6) Uani 1 d . . H11A H 1.4475(10) 0.4264(24) 0.0977(7) 0.070 Uiso 1 calc R . C12 C 1.3526(10) 0.2787(24) 0.0940(6) 0.051(5) Uani 1 d . . H12A H 1.3695(10) 0.1911(24) 0.1157(6) 0.061 Uiso 1 calc R . C13 C 1.2830(9) 0.2914(21) 0.0638(5) 0.043(4) Uani 1 d . . H13A H 1.2431(9) 0.2135(21) 0.0614(5) 0.051 Uiso 1 calc R . C14 C 1.2814(9) 0.4272(21) 0.0362(5) 0.048(5) Uani 1 d . . H14A H 1.2415(9) 0.4567(21) 0.0106(5) 0.057 Uiso 1 calc R . C15 C 1.4190(9) 0.3925(28) 0.2131(6) 0.060(6) Uani 1 d . . H15A H 1.4500(9) 0.4105(28) 0.1940(6) 0.072 Uiso 1 calc R . C16 C 1.3959(9) 0.5160(27) 0.2373(5) 0.058(5) Uani 1 d . . H16A H 1.4082(9) 0.6337(27) 0.2381(5) 0.069 Uiso 1 calc R . C17 C 1.3563(11) 0.4358(24) 0.2627(7) 0.062(6) Uani 1 d . . H17A H 1.3375(11) 0.4887(24) 0.2848(7) 0.075 Uiso 1 calc R . C18 C 1.3552(11) 0.2691(26) 0.2542(6) 0.065(6) Uani 1 d . . H18A H 1.3367(11) 0.1837(26) 0.2700(6) 0.078 Uiso 1 calc R . C19 C 1.3956(11) 0.2391(26) 0.2236(7) 0.067(6) Uani 1 d . . H19A H 1.4088(11) 0.1309(26) 0.2144(7) 0.081 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.0342(3) 0.0366(4) 0.0281(4) -0.0036(3) 0.0134(3) -0.0041(3) W2 0.0369(4) 0.0348(4) 0.0263(4) 0.0028(3) 0.0070(3) 0.0042(3) W3 0.0289(3) 0.0508(4) 0.0338(4) -0.0001(3) 0.0063(3) -0.0012(3) P1 0.046(2) 0.029(2) 0.034(3) -0.003(2) 0.018(2) -0.002(2) P2 0.026(2) 0.038(2) 0.034(2) 0.005(2) 0.007(2) 0.001(2) O1 0.057(9) 0.173(18) 0.078(12) -0.050(12) 0.014(8) 0.017(10) C1 0.051(12) 0.078(16) 0.047(13) -0.011(11) 0.005(10) -0.016(11) O2 0.084(11) 0.080(12) 0.124(16) 0.043(12) 0.001(10) 0.002(10) C2 0.032(10) 0.064(13) 0.054(13) 0.001(11) 0.000(9) -0.010(9) C3 0.057(12) 0.060(13) 0.048(12) -0.005(10) 0.014(10) -0.016(10) O3 0.037(7) 0.087(11) 0.083(11) 0.007(9) -0.005(7) -0.009(7) O4 0.081(11) 0.131(15) 0.058(11) -0.012(10) 0.019(8) 0.015(10) C4 0.038(10) 0.107(18) 0.042(12) -0.022(12) 0.012(9) -0.012(11) O5 0.077(11) 0.089(12) 0.122(15) 0.048(12) 0.017(10) -0.004(9) C5 0.046(11) 0.074(15) 0.069(15) 0.033(13) 0.011(10) -0.005(11) C6 0.055(11) 0.077(14) 0.039(11) 0.005(11) 0.037(10) -0.015(11) O6 0.085(11) 0.127(14) 0.075(11) -0.049(10) 0.036(9) -0.086(10) C7 0.065(12) 0.037(10) 0.023(9) 0.001(8) 0.016(8) -0.006(9) O7 0.095(11) 0.063(10) 0.064(10) 0.029(8) 0.024(8) 0.021(8) O8 0.119(12) 0.027(7) 0.083(11) -0.008(8) 0.029(9) -0.004(8) C8 0.072(13) 0.036(11) 0.053(13) 0.024(10) 0.035(10) 0.004(10) C9 0.050(11) 0.043(11) 0.054(12) 0.026(10) 0.008(9) -0.005(9) O9 0.060(9) 0.099(12) 0.069(10) 0.016(9) 0.035(8) -0.005(8) C10 0.086(14) 0.036(10) 0.051(12) 0.008(9) 0.052(11) 0.017(10) C11 0.047(11) 0.060(13) 0.074(15) -0.034(12) 0.025(10) -0.001(10) C12 0.057(11) 0.063(13) 0.035(11) -0.004(10) 0.015(9) 0.008(10) C13 0.065(12) 0.046(10) 0.023(9) 0.005(8) 0.023(9) 0.008(9) C14 0.056(11) 0.054(12) 0.035(10) -0.010(9) 0.015(9) 0.009(9) C15 0.033(10) 0.082(15) 0.050(12) -0.011(12) -0.013(9) 0.009(10) C16 0.049(11) 0.081(15) 0.029(11) -0.007(11) -0.012(8) 0.006(11) C17 0.076(14) 0.059(14) 0.054(13) -0.006(11) 0.022(11) 0.019(11) C18 0.088(16) 0.073(15) 0.032(12) 0.033(11) 0.016(11) 0.015(12) C19 0.080(15) 0.052(13) 0.055(14) 0.011(11) -0.006(12) 0.023(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 C7 2.01(2) . ? W1 C6 2.03(2) . ? W1 C14 2.31(2) . ? W1 C10 2.32(2) . ? W1 C11 2.34(2) . ? W1 C13 2.35(2) . ? W1 C12 2.37(2) . ? W1 P2 2.427(4) . ? W1 P1 2.590(4) . ? W1 W2 3.0242(10) . ? W2 C8 1.98(2) . ? W2 C9 2.00(2) . ? W2 C18 2.28(2) . ? W2 C17 2.32(2) . ? W2 C19 2.33(2) . ? W2 C15 2.36(2) . ? W2 C16 2.37(2) . ? W2 P1 2.488(4) . ? W2 P2 2.519(4) . ? W3 C3 1.99(2) . ? W3 C4 2.02(2) . ? W3 C1 2.03(2) . ? W3 C5 2.04(2) . ? W3 C2 2.05(2) . ? W3 P2 2.517(4) . ? P1 P2 2.096(6) . ? O1 C1 1.15(2) . ? O2 C2 1.12(2) . ? C3 O3 1.16(2) . ? O4 C4 1.15(2) . ? O5 C5 1.15(2) . ? C6 O6 1.09(2) . ? C7 O7 1.14(2) . ? O8 C8 1.15(2) . ? C9 O9 1.13(2) . ? C10 C11 1.40(2) . ? C10 C14 1.43(2) . ? C11 C12 1.44(2) . ? C12 C13 1.41(2) . ? C13 C14 1.40(2) . ? C15 C19 1.39(3) . ? C15 C16 1.41(2) . ? C16 C17 1.42(3) . ? C17 C18 1.38(3) . ? C18 C19 1.43(3) . ? 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 C7 W1 C6 87.4(7) . . ? C7 W1 C14 82.6(6) . . ? C6 W1 C14 133.1(6) . . ? C7 W1 C10 85.9(6) . . ? C6 W1 C10 97.8(7) . . ? C14 W1 C10 36.1(6) . . ? C7 W1 C11 118.8(7) . . ? C6 W1 C11 87.2(7) . . ? C14 W1 C11 59.2(6) . . ? C10 W1 C11 35.1(6) . . ? C7 W1 C13 113.5(6) . . ? C6 W1 C13 145.0(7) . . ? C14 W1 C13 35.0(5) . . ? C10 W1 C13 58.6(6) . . ? C11 W1 C13 58.4(6) . . ? C7 W1 C12 140.7(6) . . ? C6 W1 C12 112.2(7) . . ? C14 W1 C12 58.9(6) . . ? C10 W1 C12 58.8(6) . . ? C11 W1 C12 35.5(6) . . ? C13 W1 C12 34.8(5) . . ? C7 W1 P2 87.7(5) . . ? C6 W1 P2 120.1(5) . . ? C14 W1 P2 105.1(5) . . ? C10 W1 P2 141.2(5) . . ? C11 W1 P2 143.9(5) . . ? C13 W1 P2 89.7(4) . . ? C12 W1 P2 108.5(5) . . ? C7 W1 P1 79.6(5) . . ? C6 W1 P1 71.2(5) . . ? C14 W1 P1 149.0(4) . . ? C10 W1 P1 162.1(4) . . ? C11 W1 P1 151.5(5) . . ? C13 W1 P1 137.6(4) . . ? C12 W1 P1 138.0(5) . . ? P2 W1 P1 49.25(14) . . ? C7 W1 W2 130.1(5) . . ? C6 W1 W2 87.4(5) . . ? C14 W1 W2 132.6(4) . . ? C10 W1 W2 143.9(4) . . ? C11 W1 W2 110.4(5) . . ? C13 W1 W2 98.1(4) . . ? C12 W1 W2 86.1(4) . . ? P2 W1 W2 53.69(10) . . ? P1 W1 W2 51.92(10) . . ? C8 W2 C9 86.4(7) . . ? C8 W2 C18 99.3(8) . . ? C9 W2 C18 86.5(7) . . ? C8 W2 C17 133.9(7) . . ? C9 W2 C17 85.9(7) . . ? C18 W2 C17 34.8(6) . . ? C8 W2 C19 86.7(7) . . ? C9 W2 C19 119.6(7) . . ? C18 W2 C19 36.2(7) . . ? C17 W2 C19 58.8(7) . . ? C8 W2 C15 110.3(7) . . ? C9 W2 C15 142.7(7) . . ? C18 W2 C15 58.6(7) . . ? C17 W2 C15 58.2(7) . . ? C19 W2 C15 34.6(6) . . ? C8 W2 C16 143.7(7) . . ? C9 W2 C16 117.2(7) . . ? C18 W2 C16 58.4(7) . . ? C17 W2 C16 35.2(6) . . ? C19 W2 C16 58.1(7) . . ? C15 W2 C16 34.7(6) . . ? C8 W2 P1 122.8(5) . . ? C9 W2 P1 89.4(5) . . ? C18 W2 P1 137.3(6) . . ? C17 W2 P1 102.6(5) . . ? C19 W2 P1 141.2(6) . . ? C15 W2 P1 106.8(6) . . ? C16 W2 P1 86.7(5) . . ? C8 W2 P2 73.9(5) . . ? C9 W2 P2 78.5(5) . . ? C18 W2 P2 163.8(5) . . ? C17 W2 P2 147.5(5) . . ? C19 W2 P2 153.0(6) . . ? C15 W2 P2 137.3(5) . . ? C16 W2 P2 134.7(5) . . ? P1 W2 P2 49.48(14) . . ? C8 W2 W1 85.4(5) . . ? C9 W2 W1 129.1(5) . . ? C18 W2 W1 144.4(5) . . ? C17 W2 W1 132.4(5) . . ? C19 W2 W1 110.0(6) . . ? C15 W2 W1 86.5(5) . . ? C16 W2 W1 97.7(5) . . ? P1 W2 W1 55.01(10) . . ? P2 W2 W1 50.95(9) . . ? C3 W3 C4 89.7(7) . . ? C3 W3 C1 89.2(7) . . ? C4 W3 C1 178.9(7) . . ? C3 W3 C5 90.5(7) . . ? C4 W3 C5 91.9(9) . . ? C1 W3 C5 88.3(9) . . ? C3 W3 C2 92.1(7) . . ? C4 W3 C2 89.7(9) . . ? C1 W3 C2 90.1(8) . . ? C5 W3 C2 176.9(8) . . ? C3 W3 P2 176.8(5) . . ? C4 W3 P2 89.2(5) . . ? C1 W3 P2 91.8(5) . . ? C5 W3 P2 86.5(5) . . ? C2 W3 P2 90.9(5) . . ? P2 P1 W2 66.0(2) . . ? P2 P1 W1 61.33(15) . . ? W2 P1 W1 73.06(12) . . ? P1 P2 W1 69.4(2) . . ? P1 P2 W3 132.2(2) . . ? W1 P2 W3 139.8(2) . . ? P1 P2 W2 64.5(2) . . ? W1 P2 W2 75.35(10) . . ? W3 P2 W2 141.3(2) . . ? O1 C1 W3 177.6(17) . . ? O2 C2 W3 178.8(17) . . ? O3 C3 W3 179.5(19) . . ? O4 C4 W3 173.5(19) . . ? O5 C5 W3 178.7(18) . . ? O6 C6 W1 175.0(15) . . ? O7 C7 W1 176.9(16) . . ? O8 C8 W2 176.5(15) . . ? O9 C9 W2 177.5(17) . . ? C11 C10 C14 108.2(16) . . ? C11 C10 W1 73.3(10) . . ? C14 C10 W1 71.7(9) . . ? C10 C11 C12 108.3(16) . . ? C10 C11 W1 71.6(9) . . ? C12 C11 W1 73.4(10) . . ? C13 C12 C11 106.8(17) . . ? C13 C12 W1 72.0(10) . . ? C11 C12 W1 71.1(10) . . ? C14 C13 C12 109.5(17) . . ? C14 C13 W1 70.8(10) . . ? C12 C13 W1 73.2(10) . . ? C13 C14 C10 107.2(16) . . ? C13 C14 W1 74.2(10) . . ? C10 C14 W1 72.2(9) . . ? C19 C15 C16 109.0(20) . . ? C19 C15 W2 71.5(11) . . ? C16 C15 W2 73.2(10) . . ? C15 C16 C17 107.0(19) . . ? C15 C16 W2 72.1(10) . . ? C17 C16 W2 70.4(11) . . ? C18 C17 C16 108.5(18) . . ? C18 C17 W2 70.8(11) . . ? C16 C17 W2 74.4(11) . . ? C17 C18 C19 108.6(19) . . ? C17 C18 W2 74.4(11) . . ? C19 C18 W2 73.9(10) . . ? C15 C19 C18 106.8(19) . . ? C15 C19 W2 73.9(10) . . ? C18 C19 W2 69.8(10) . . ? _refine_diff_density_max 1.192 _refine_diff_density_min -1.417 _refine_diff_density_rms 0.283