# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1466 data_IC5570 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C20 H16 O6 S2 W2' _chemical_formula_weight 784.15 _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' 'S' 'S' 0.1246 0.1234 '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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.1165(2) _cell_length_b 46.4397(12) _cell_length_c 7.5328(2) _cell_angle_alpha 90.00 _cell_angle_beta 116.457(1) _cell_angle_gamma 90.00 _cell_volume 2228.77(10) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 5612 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 2.337 _exptl_crystal_density_method ? _exptl_crystal_F_000 1456 _exptl_absorpt_coefficient_mu 10.535 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.2728 _exptl_absorpt_correction_T_max 0.4910 _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART CCD' _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11302 _diffrn_reflns_av_R_equivalents 0.0336 _diffrn_reflns_av_sigmaI/netI 0.0341 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -55 _diffrn_reflns_limit_k_max 55 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 0.88 _diffrn_reflns_theta_max 25.03 _reflns_number_total 3925 _reflns_number_observed 3703 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SAINT' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _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^)+(0.0388P)^2^+42.4687P] 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 SHELXL _refine_ls_extinction_coef 0.0015(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3925 _refine_ls_number_parameters 291 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0633 _refine_ls_R_factor_obs 0.0586 _refine_ls_wR_factor_all 0.1389 _refine_ls_wR_factor_obs 0.1367 _refine_ls_goodness_of_fit_all 1.392 _refine_ls_goodness_of_fit_obs 1.413 _refine_ls_restrained_S_all 1.392 _refine_ls_restrained_S_obs 1.413 _refine_ls_shift/esd_max -0.423 _refine_ls_shift/esd_mean 0.033 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 0.76350(10) 0.684878(12) 0.57130(9) 0.0317(2) Uani 1 d . . W2 W 0.67988(9) 0.564895(12) 0.09837(9) 0.0301(2) Uani 1 d . . S1 S 0.7844(6) 0.59379(8) 0.4063(5) 0.0328(8) Uani 1 d . . C1 C 0.8245(29) 0.7263(3) 0.6109(27) 0.046(4) Uani 1 d . . C2 C 1.0348(32) 0.6848(4) 0.8148(29) 0.056(5) Uani 1 d . . C3 C 0.8144(30) 0.6973(3) 0.3417(27) 0.049(4) Uani 1 d . . C4 C 0.4793(26) 0.5987(3) 0.0080(25) 0.038(3) Uani 1 d . . C5 C 0.6042(27) 0.5402(3) 0.2691(25) 0.041(4) Uani 1 d . . C6 C 0.4056(30) 0.5472(3) -0.0881(26) 0.044(4) Uani 1 d . . C7 C 0.9562(24) 0.6469(3) 0.5382(24) 0.041(4) Uani 1 d . . H7A H 1.0853(24) 0.6544(3) 0.5426(24) 0.049 Uiso 1 calc R . H7B H 0.9940(24) 0.6341(3) 0.6508(24) 0.049 Uiso 1 calc R . C8 C 0.8467(23) 0.6298(3) 0.3533(24) 0.035(3) Uani 1 d . . C9 C 0.3984(27) 0.6893(4) 0.4238(28) 0.050(4) Uani 1 d . . H9A H 0.3125(27) 0.7020(4) 0.3139(28) 0.059 Uiso 1 calc R . C10 C 0.4507(24) 0.6604(3) 0.4092(23) 0.039(4) Uani 1 d . . H10A H 0.4073(24) 0.6498(3) 0.2849(23) 0.046 Uiso 1 calc R . C11 C 0.5519(26) 0.6482(3) 0.6013(27) 0.044(4) Uani 1 d . . H11A H 0.5916(26) 0.6280(3) 0.6321(27) 0.052 Uiso 1 calc R . C12 C 0.5678(27) 0.6697(4) 0.7379(24) 0.045(4) Uani 1 d . . H12A H 0.6236(27) 0.6670(4) 0.8814(24) 0.055 Uiso 1 calc R . C13 C 0.4732(29) 0.6950(3) 0.6339(27) 0.046(4) Uani 1 d . . C14 C 0.4395(36) 0.7231(4) 0.7166(38) 0.072(6) Uani 1 d . . H14A H 0.3709(36) 0.7366(4) 0.6103(38) 0.107 Uiso 1 calc R . H14B H 0.5727(36) 0.7308(4) 0.8089(38) 0.107 Uiso 1 calc R . H14C H 0.3536(36) 0.7198(4) 0.7832(38) 0.107 Uiso 1 calc R . C15 C 0.9947(27) 0.5403(3) 0.1703(27) 0.044(4) Uani 1 d . . H15A H 1.0627(27) 0.5263(3) 0.2778(27) 0.052 Uiso 1 calc R . C16 C 0.8446(28) 0.5336(4) -0.0256(29) 0.050(4) Uani 1 d . . H16A H 0.7960(28) 0.5142(4) -0.0780(29) 0.061 Uiso 1 calc R . C17 C 0.7996(29) 0.5597(5) -0.1397(22) 0.053(5) Uani 1 d . . H17A H 0.7148(29) 0.5614(5) -0.2835(22) 0.064 Uiso 1 calc R . C18 C 0.9253(26) 0.5819(4) -0.0098(26) 0.044(4) Uani 1 d . . H18A H 0.9342(26) 0.6017(4) -0.0494(26) 0.053 Uiso 1 calc R . C19 C 1.0496(26) 0.5701(4) 0.1782(29) 0.047(4) Uani 1 d . . C20 C 1.2200(28) 0.5849(5) 0.3513(34) 0.066(6) Uani 1 d . . H20A H 1.2249(28) 0.6048(5) 0.3201(34) 0.099 Uiso 1 calc R . H20B H 1.3523(28) 0.5760(5) 0.3803(34) 0.099 Uiso 1 calc R . H20C H 1.1924(28) 0.5834(5) 0.4645(34) 0.099 Uiso 1 calc R . O1 O 0.8650(30) 0.7505(3) 0.6428(28) 0.088(5) Uani 1 d . . O2 O 1.1898(26) 0.6843(4) 0.9525(23) 0.096(6) Uani 1 d . . O3 O 0.8421(26) 0.7046(3) 0.2115(21) 0.068(4) Uani 1 d . . O4 O 0.3583(21) 0.6165(3) -0.0474(22) 0.068(4) Uani 1 d . . O7 O 0.8082(20) 0.6377(2) 0.1887(17) 0.048(3) Uani 1 d . . S2 S 0.1981(22) 0.5360(3) -0.2340(21) 0.058(4) Uani 0.67(4) d P 1 O5 O 0.5496(76) 0.5239(8) 0.3526(68) 0.072(13) Uani 0.67(4) d P 1 S2' S 0.5707(44) 0.5177(6) 0.4106(39) 0.041(6) Uani 0.33(4) d P 2 O6 O 0.2605(132) 0.5287(18) -0.1806(151) 0.099(40) Uani 0.33(4) d P 2 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 0.0423(4) 0.0246(3) 0.0259(3) -0.0017(2) 0.0132(3) -0.0014(2) W2 0.0368(4) 0.0274(3) 0.0314(3) -0.0005(2) 0.0200(3) 0.0001(2) S1 0.044(2) 0.030(2) 0.029(2) -0.0003(15) 0.021(2) -0.001(2) C1 0.066(11) 0.031(9) 0.052(10) -0.001(7) 0.034(9) 0.004(8) C2 0.065(12) 0.053(11) 0.050(12) -0.016(9) 0.026(11) -0.007(9) C3 0.075(12) 0.019(7) 0.051(11) -0.006(7) 0.027(10) -0.014(7) C4 0.047(9) 0.024(7) 0.043(9) 0.001(6) 0.020(8) 0.002(7) C5 0.058(10) 0.032(8) 0.043(9) -0.008(7) 0.032(8) -0.003(7) C6 0.069(11) 0.032(8) 0.045(10) -0.009(7) 0.039(9) -0.001(8) C7 0.033(8) 0.041(9) 0.037(9) -0.004(7) 0.005(7) -0.005(7) C8 0.041(8) 0.016(6) 0.043(9) -0.007(6) 0.014(7) -0.002(6) C9 0.042(9) 0.056(11) 0.049(10) 0.004(8) 0.019(8) 0.005(8) C10 0.043(9) 0.039(8) 0.034(8) -0.013(7) 0.016(7) -0.012(7) C11 0.052(10) 0.027(8) 0.062(11) 0.004(7) 0.034(9) -0.005(7) C12 0.057(10) 0.043(9) 0.027(8) -0.003(7) 0.011(8) -0.006(8) C13 0.068(11) 0.033(8) 0.051(10) -0.004(7) 0.040(9) 0.004(8) C14 0.080(15) 0.048(11) 0.106(18) -0.021(12) 0.058(15) -0.006(10) C15 0.054(10) 0.030(8) 0.057(11) -0.003(7) 0.034(9) -0.001(7) C16 0.051(10) 0.038(9) 0.071(13) -0.017(9) 0.035(10) -0.004(8) C17 0.060(11) 0.091(15) 0.014(7) -0.007(8) 0.023(8) 0.000(10) C18 0.049(10) 0.043(9) 0.050(10) 0.002(8) 0.031(9) -0.006(8) C19 0.044(9) 0.048(10) 0.074(12) -0.016(9) 0.049(9) -0.010(7) C20 0.039(10) 0.066(13) 0.097(17) -0.026(12) 0.034(11) -0.005(9) O1 0.124(14) 0.037(8) 0.118(14) -0.012(8) 0.068(12) -0.010(8) O2 0.078(11) 0.114(14) 0.044(9) -0.020(9) -0.020(8) -0.025(10) O3 0.119(12) 0.042(7) 0.057(8) 0.013(6) 0.052(9) -0.016(7) O4 0.055(8) 0.056(8) 0.073(9) 0.012(7) 0.011(7) 0.016(7) O7 0.072(8) 0.036(6) 0.042(7) 0.005(5) 0.031(6) 0.001(5) S2 0.053(7) 0.052(7) 0.069(7) -0.007(5) 0.028(6) -0.007(5) O5 0.117(27) 0.047(19) 0.086(27) 0.024(15) 0.075(23) -0.007(16) S2' 0.065(10) 0.027(10) 0.042(12) 0.005(8) 0.035(9) -0.006(7) O6 0.063(48) 0.068(44) 0.110(69) -0.012(37) -0.011(42) 0.037(35) _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 C1 1.97(2) . ? W1 C2 1.98(2) . ? W1 C3 2.00(2) . ? W1 C10 2.305(15) . ? W1 C7 2.32(2) . ? W1 C9 2.34(2) . ? W1 C11 2.349(15) . ? W1 C13 2.36(2) . ? W1 C12 2.36(2) . ? W2 C5 1.97(2) . ? W2 C6 2.00(2) . ? W2 C4 2.03(2) . ? W2 C16 2.31(2) . ? W2 C17 2.315(15) . ? W2 C15 2.35(2) . ? W2 C18 2.37(2) . ? W2 C19 2.44(2) . ? W2 S1 2.489(4) . ? S1 C8 1.820(14) . ? C1 O1 1.16(2) . ? C2 O2 1.13(2) . ? C3 O3 1.13(2) . ? C4 O4 1.13(2) . ? C5 O5 1.16(4) . ? C5 S2' 1.58(3) . ? C6 O6 1.29(9) . ? C6 S2 1.49(2) . ? C7 C8 1.49(2) . ? C8 O7 1.20(2) . ? C9 C10 1.41(2) . ? C9 C13 1.45(2) . ? C10 C11 1.42(2) . ? C11 C12 1.40(2) . ? C12 C13 1.41(2) . ? C13 C14 1.51(2) . ? C15 C19 1.43(2) . ? C15 C16 1.42(3) . ? C16 C17 1.44(3) . ? C17 C18 1.43(2) . ? C18 C19 1.40(3) . ? C19 C20 1.49(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 C1 W1 C2 78.7(8) . . ? C1 W1 C3 74.7(7) . . ? C2 W1 C3 108.8(8) . . ? C1 W1 C10 131.2(7) . . ? C2 W1 C10 143.2(7) . . ? C3 W1 C10 100.8(6) . . ? C1 W1 C7 131.4(7) . . ? C2 W1 C7 73.7(7) . . ? C3 W1 C7 77.5(7) . . ? C10 W1 C7 92.6(5) . . ? C1 W1 C9 96.4(7) . . ? C2 W1 C9 149.1(7) . . ? C3 W1 C9 98.9(7) . . ? C10 W1 C9 35.3(6) . . ? C7 W1 C9 127.0(6) . . ? C1 W1 C11 143.4(6) . . ? C2 W1 C11 108.1(7) . . ? C3 W1 C11 131.5(6) . . ? C10 W1 C11 35.4(6) . . ? C7 W1 C11 83.9(6) . . ? C9 W1 C11 58.9(6) . . ? C1 W1 C13 85.9(6) . . ? C2 W1 C13 113.2(7) . . ? C3 W1 C13 128.7(7) . . ? C10 W1 C13 58.6(6) . . ? C7 W1 C13 141.8(6) . . ? C9 W1 C13 36.0(6) . . ? C11 W1 C13 58.0(6) . . ? C1 W1 C12 110.8(6) . . ? C2 W1 C12 94.0(7) . . ? C3 W1 C12 157.2(7) . . ? C10 W1 C12 58.3(6) . . ? C7 W1 C12 110.4(6) . . ? C9 W1 C12 58.9(6) . . ? C11 W1 C12 34.6(6) . . ? C13 W1 C12 34.7(6) . . ? C5 W2 C6 75.8(7) . . ? C5 W2 C4 108.3(7) . . ? C6 W2 C4 76.2(6) . . ? C5 W2 C16 103.5(7) . . ? C6 W2 C16 88.3(6) . . ? C4 W2 C16 139.5(7) . . ? C5 W2 C17 138.4(7) . . ? C6 W2 C17 89.7(6) . . ? C4 W2 C17 105.5(7) . . ? C16 W2 C17 36.2(7) . . ? C5 W2 C15 94.4(6) . . ? C6 W2 C15 119.6(6) . . ? C4 W2 C15 155.5(6) . . ? C16 W2 C15 35.4(6) . . ? C17 W2 C15 59.1(6) . . ? C5 W2 C18 151.3(7) . . ? C6 W2 C18 122.2(6) . . ? C4 W2 C18 98.2(6) . . ? C16 W2 C18 59.1(6) . . ? C17 W2 C18 35.5(6) . . ? C15 W2 C18 57.9(6) . . ? C5 W2 C19 118.5(7) . . ? C6 W2 C19 145.3(6) . . ? C4 W2 C19 121.8(6) . . ? C16 W2 C19 58.4(6) . . ? C17 W2 C19 58.1(6) . . ? C15 W2 C19 34.8(5) . . ? C18 W2 C19 33.9(6) . . ? C5 W2 S1 76.1(5) . . ? C6 W2 S1 131.8(4) . . ? C4 W2 S1 76.6(5) . . ? C16 W2 S1 136.2(5) . . ? C17 W2 S1 135.8(5) . . ? C15 W2 S1 100.9(4) . . ? C18 W2 S1 100.4(4) . . ? C19 W2 S1 82.8(4) . . ? C8 S1 W2 107.0(5) . . ? O1 C1 W1 177.1(17) . . ? O2 C2 W1 179.0(18) . . ? O3 C3 W1 179.4(13) . . ? O4 C4 W2 176.1(15) . . ? O5 C5 W2 173.0(26) . . ? S2' C5 W2 172.1(15) . . ? O6 C6 W2 161.9(40) . . ? S2 C6 W2 176.2(13) . . ? C8 C7 W1 114.8(10) . . ? O7 C8 C7 126.1(14) . . ? O7 C8 S1 122.6(11) . . ? C7 C8 S1 111.2(12) . . ? C10 C9 C13 106.2(15) . . ? C10 C9 W1 71.2(9) . . ? C13 C9 W1 73.0(10) . . ? C9 C10 C11 109.5(14) . . ? C9 C10 W1 73.6(9) . . ? C11 C10 W1 74.0(9) . . ? C12 C11 C10 107.7(14) . . ? C12 C11 W1 73.1(10) . . ? C10 C11 W1 70.6(9) . . ? C11 C12 C13 108.9(15) . . ? C11 C12 W1 72.3(10) . . ? C13 C12 W1 72.8(10) . . ? C12 C13 C9 107.8(15) . . ? C12 C13 C14 128.1(18) . . ? C9 C13 C14 124.0(18) . . ? C12 C13 W1 72.6(10) . . ? C9 C13 W1 71.0(9) . . ? C14 C13 W1 124.6(13) . . ? C19 C15 C16 108.7(16) . . ? C19 C15 W2 75.8(9) . . ? C16 C15 W2 70.7(10) . . ? C15 C16 C17 107.4(15) . . ? C15 C16 W2 73.9(9) . . ? C17 C16 W2 72.1(9) . . ? C18 C17 C16 107.1(15) . . ? C18 C17 W2 74.2(9) . . ? C16 C17 W2 71.7(9) . . ? C17 C18 C19 109.4(15) . . ? C17 C18 W2 70.3(9) . . ? C19 C18 W2 75.7(9) . . ? C15 C19 C18 107.3(16) . . ? C15 C19 C20 125.5(19) . . ? C18 C19 C20 127.1(17) . . ? C15 C19 W2 69.5(9) . . ? C18 C19 W2 70.4(9) . . ? C20 C19 W2 129.0(11) . . ? _refine_diff_density_max 1.741 _refine_diff_density_min -2.275 _refine_diff_density_rms 0.189 data_IC4915 #======================================================================= # 5. CHEMICAL DATA _chemical_name_systematic ; ? #Insert the chemical name here. ; _chemical_name_common ? _chemical_formula_moiety 'C17 H12 O5 S W2 ' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C17 H12 O5 S W2 ' _chemical_formula_weight 696.03 _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 ? 0.002 0.002 'International Tables Vol. IV Table 2.2B' H ? 0.000 0.000 'International Tables Vol. IV Table 2.2B' O ? 0.008 0.006 'International Tables Vol. IV Table 2.2B' S ? 0.110 0.124 'International Tables Vol. IV Table 2.2B' W ? -1.421 6.872 'International Tables Vol. IV Table 2.2B' #======================================================================= # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z 1/2-x,1/2+y,1/2-z 1/2+x,1/2-y,1/2+z _cell_length_a 9.7547(20) _cell_length_b 15.936(4) _cell_length_c 12.226(4) _cell_angle_alpha 90.0 _cell_angle_beta 111.811(23) _cell_angle_gamma 90.0 _cell_volume 1764.5(8) _cell_formula_units_Z 4 _cell_measurement_temperature 298 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8.44 _cell_measurement_theta_max 13.56 _cell_special_details ; ? #Insert any comments here. ; _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.620 _exptl_crystal_density_method ? _exptl_crystal_F_000 1263.97 _exptl_absorpt_coefficient_mu 13.45 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5694 _exptl_absorpt_correction_T_max 0.9973 #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ; ? #Insert any special details here. ; _diffrn_ambient_temperature 298 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Molybdenum K\a' _diffrn_radiation_source 'xray tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius CAD-4 ' _diffrn_measurement_method 'Theta/2theta scan b/P/b ' _diffrn_standards_number 3 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0.0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 0 0 0 0 0 0 0 0 _diffrn_reflns_number 3100 _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 24.93 _diffrn_reflns_reduction_process ? _reflns_number_total 3100 _reflns_number_observed 2105 _reflns_observed_criterion 'Inet > 2.0\s(Inet)' _computing_data_collection 'NONIUS CAD4' _computing_cell_refinement 'NONIUS CAD4' _computing_data_reduction 'NRCVAX DATRD2' _computing_structure_solution 'NRCVAX SOLVER' _computing_structure_refinement 'NRCVAX LSTSQ' _computing_molecular_graphics 'NRCVAX ORTEP' _computing_publication_material 'NRCVAX TABLES' #======================================================================= # 8. REFINEMENT DATA _refine_special_details ; ? #Insert any special details here. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type atomblock _refine_ls_weighting_scheme 1/(\s^2^(F)+0.0001F^2^) _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method Larson _refine_ls_extinction_coef 6131(369) _refine_ls_number_reflns 2105 _refine_ls_number_parameters 227 _refine_ls_number_restraints ? _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.093 _refine_ls_R_factor_obs 0.057 _refine_ls_wR_factor_all 0.059 _refine_ls_wR_factor_obs 0.056 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.85 _refine_ls_restrained_S_all ? _refine_ls_restrained_S_obs ? _refine_ls_shift/esd_max 0.011 _refine_ls_shift/esd_mean ? _refine_diff_density_max 2.62 _refine_diff_density_min -4.19 #======================================================================= # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _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_calc_flag _atom_site_refinement_flags _atom_site_type_symbol W1 0.17974(10) 0.84536(6) 0.37300(8) 0.0260(5) Uani ? . W W2 0.31151(10) 0.86953(6) 0.06132(7) 0.0242(5) Uani ? . W S 0.1710(6) 0.9126(4) 0.1830(5) 0.032(4) Uani ? . S C1 0.2423(22) 0.7339(17) 0.4431(18) 0.036(15) Uani ? . C C2 0.399(3) 0.8483(21) 0.3943(23) 0.061(21) Uani ? . C C3 0.0663(24) 0.7649(15) 0.2468(18) 0.031(13) Uani ? . C C4 0.3204(24) 0.7567(16) 0.1177(18) 0.038(14) Uani ? . C C5 0.528(3) 0.850(3) 0.1479(25) 0.12(3) Uani ? . C C6 0.339(3) 0.9610(14) 0.1883(18) 0.037(15) Uani ? . C C7 0.398(3) 1.0252(19) 0.2566(24) 0.065(22) Uani ? . C C8 0.205(3) 0.9616(21) 0.501(3) 0.073(22) Uani ? . C C9 0.085(3) 0.9765(17) 0.3949(21) 0.050(18) Uani ? . C C10 -0.018(3) 0.9205(19) 0.3821(23) 0.056(19) Uani ? . C C11 0.028(3) 0.8637(18) 0.470(3) 0.075(24) Uani ? . C C12 0.170(3) 0.8881(18) 0.5483(21) 0.061(21) Uani ? . C C13 0.175(3) 0.8365(19) -0.1374(20) 0.067(20) Uani ? . C C14 0.309(3) 0.8521(21) -0.1222(22) 0.066(21) Uani ? . C C15 0.332(3) 0.9362(23) -0.0962(24) 0.082(24) Uani ? . C C16 0.205(4) 0.9685(19) -0.0852(22) 0.079(23) Uani ? . C C17 0.114(3) 0.9098(21) -0.1127(19) 0.062(21) Uani ? . C O1 0.2825(24) 0.6684(12) 0.4824(16) 0.083(16) Uani ? . O O2 0.5201(17) 0.8478(14) 0.4175(16) 0.069(14) Uani ? . O O3 0.0006(19) 0.7197(12) 0.1770(14) 0.057(12) Uani ? . O O4 0.3236(18) 0.6890(12) 0.1566(15) 0.057(12) Uani ? . O O5 0.6474(17) 0.8470(17) 0.2011(16) 0.092(18) Uani ? . O H7a 0.397 1.023 0.335 0.0725 Uiso ? . H H7b 0.489 1.035 0.245 0.0725 Uiso ? . H H8 0.293 0.998 0.529 0.0801 Uiso ? . H H9 0.078 1.022 0.340 0.0625 Uiso ? . H H10 -0.114 0.921 0.317 0.0597 Uiso ? . H H11 -0.028 0.816 0.480 0.0878 Uiso ? . H H12 0.233 0.863 0.622 0.0706 Uiso ? . H H13 0.124 0.783 -0.160 0.0665 Uiso ? . H H14 0.383 0.813 -0.127 0.0731 Uiso ? . H H15 0.423 0.967 -0.090 0.0834 Uiso ? . H H16 0.195 1.027 -0.064 0.0739 Uiso ? . H H17 0.015 0.916 -0.115 0.0705 Uiso ? . H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol W1 0.0243(4) 0.0334(6) 0.0212(4) 0.0030(5) 0.0094(4) 0.0004(4) W W2 0.0230(4) 0.0294(5) 0.0206(4) 0.0001(4) 0.0084(4) 0.0015(4) W S 0.031(3) 0.041(4) 0.025(3) 0.008(3) 0.010(3) 0.007(3) S C1 0.023(12) 0.060(19) 0.029(13) 0.000(12) 0.012(10) -0.012(12) C C2 0.045(16) 0.09(3) 0.057(17) 0.016(17) 0.027(14) 0.018(18) C C3 0.037(13) 0.032(15) 0.025(12) 0.019(12) 0.012(10) 0.017(11) C C4 0.032(13) 0.047(17) 0.025(12) 0.014(13) 0.000(10) 0.009(12) C C5 0.047(18) 0.26(5) 0.061(20) 0.08(3) 0.039(16) 0.08(3) C C6 0.054(16) 0.024(14) 0.017(11) -0.015(12) -0.004(11) 0.003(10) C C7 0.090(24) 0.053(21) 0.062(19) -0.018(18) 0.038(18) 0.000(16) C C8 0.058(19) 0.08(3) 0.069(20) 0.012(19) 0.013(16) -0.028(19) C C9 0.077(20) 0.046(18) 0.046(15) 0.032(16) 0.046(15) 0.020(14) C C10 0.024(13) 0.067(23) 0.070(19) 0.002(14) 0.010(13) -0.021(17) C C11 0.061(19) 0.040(20) 0.14(3) -0.003(16) 0.062(20) 0.025(20) C C12 0.104(24) 0.055(20) 0.032(15) 0.037(18) 0.036(16) 0.012(13) C C13 0.078(20) 0.066(22) 0.024(14) 0.014(18) -0.020(14) -0.018(15) C C14 0.048(17) 0.11(3) 0.044(16) 0.049(18) 0.023(14) 0.036(18) C C15 0.074(21) 0.12(3) 0.046(17) -0.067(22) 0.011(16) 0.003(19) C C16 0.11(3) 0.056(21) 0.034(16) 0.015(20) -0.016(17) -0.017(15) C C17 0.038(15) 0.13(3) 0.019(12) 0.031(17) 0.009(12) 0.043(16) C O1 0.113(18) 0.046(14) 0.056(13) 0.011(13) -0.010(12) 0.008(11) O O2 0.025(9) 0.100(18) 0.078(14) 0.013(11) 0.013(9) 0.016(13) O O3 0.061(12) 0.057(14) 0.038(10) -0.013(10) 0.003(9) -0.013(10) O O4 0.053(11) 0.050(13) 0.059(12) 0.008(10) 0.009(10) 0.017(10) O O5 0.014(8) 0.19(3) 0.067(13) 0.025(13) 0.005(9) 0.031(16) O #======================================================================= # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 S 2.530(6) ? ? ? W1 C1 1.97(3) ? ? ? W1 C2 2.061(25) ? ? ? W1 C3 1.995(23) ? ? ? W1 C8 2.38(3) ? ? ? W1 C9 2.34(3) ? ? ? W1 C10 2.309(25) ? ? ? W1 C11 2.23(3) ? ? ? W1 C12 2.285(24) ? ? ? W2 S 2.466(6) ? ? ? W2 C4 1.915(24) ? ? ? W2 C5 2.01(3) ? ? ? W2 C6 2.072(23) ? ? ? W2 C13 2.356(22) ? ? ? W2 C14 2.25(3) ? ? ? W2 C15 2.27(3) ? ? ? W2 C16 2.32(3) ? ? ? W2 C17 2.367(21) ? ? ? S C6 1.793(24) ? ? ? C1 O1 1.15(3) ? ? ? C2 O2 1.10(3) ? ? ? C3 O3 1.12(3) ? ? ? C4 O4 1.17(3) ? ? ? C5 O5 1.10(3) ? ? ? C6 C7 1.31(4) ? ? ? C8 C9 1.40(4) ? ? ? C8 C12 1.41(5) ? ? ? C9 C10 1.31(4) ? ? ? C10 C11 1.35(4) ? ? ? C11 C12 1.42(4) ? ? ? C13 C14 1.28(4) ? ? ? C13 C17 1.39(4) ? ? ? C14 C15 1.38(5) ? ? ? C15 C16 1.39(5) ? ? ? C16 C17 1.25(5) ? ? ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S W1 C1 132.9(6) ? ? ? ? S W1 C2 77.6(7) ? ? ? ? S W1 C3 75.1(6) ? ? ? ? S W1 C8 103.5(8) ? ? ? ? S W1 C9 81.2(6) ? ? ? ? S W1 C10 94.7(7) ? ? ? ? S W1 C11 128.9(8) ? ? ? ? S W1 C12 137.4(7) ? ? ? ? C1 W1 C2 80.0(11) ? ? ? ? C1 W1 C3 75.5(9) ? ? ? ? C1 W1 C8 118.6(10) ? ? ? ? C1 W1 C9 145.9(8) ? ? ? ? C1 W1 C10 125.2(10) ? ? ? ? C1 W1 C11 92.7(10) ? ? ? ? C1 W1 C12 88.6(9) ? ? ? ? C2 W1 C3 111.4(11) ? ? ? ? C2 W1 C8 93.0(11) ? ? ? ? C2 W1 C9 113.6(11) ? ? ? ? C2 W1 C10 146.2(11) ? ? ? ? C2 W1 C11 142.5(11) ? ? ? ? C2 W1 C12 106.2(11) ? ? ? ? C3 W1 C8 154.3(9) ? ? ? ? C3 W1 C9 122.2(9) ? ? ? ? C3 W1 C10 97.9(9) ? ? ? ? C3 W1 C11 102.0(10) ? ? ? ? C3 W1 C12 135.4(10) ? ? ? ? C8 W1 C9 34.6(10) ? ? ? ? C8 W1 C10 56.5(9) ? ? ? ? C8 W1 C11 58.4(11) ? ? ? ? C8 W1 C12 35.0(11) ? ? ? ? C9 W1 C10 32.8(10) ? ? ? ? C9 W1 C11 56.9(9) ? ? ? ? C9 W1 C12 58.0(9) ? ? ? ? C10 W1 C11 34.4(11) ? ? ? ? C10 W1 C12 58.2(9) ? ? ? ? C11 W1 C12 36.5(12) ? ? ? ? S W2 C4 90.3(7) ? ? ? ? S W2 C5 116.0(9) ? ? ? ? S W2 C6 45.5(7) ? ? ? ? S W2 C13 117.1(8) ? ? ? ? S W2 C14 146.5(6) ? ? ? ? S W2 C15 128.7(10) ? ? ? ? S W2 C16 95.0(8) ? ? ? ? S W2 C17 91.0(6) ? ? ? ? C4 W2 C5 76.5(14) ? ? ? ? C4 W2 C6 114.5(9) ? ? ? ? C4 W2 C13 95.4(10) ? ? ? ? C4 W2 C14 103.0(11) ? ? ? ? C4 W2 C15 137.5(12) ? ? ? ? C4 W2 C16 149.6(10) ? ? ? ? C4 W2 C17 119.4(10) ? ? ? ? C5 W2 C6 84.0(14) ? ? ? ? C5 W2 C13 126.2(12) ? ? ? ? C5 W2 C14 97.1(10) ? ? ? ? C5 W2 C15 96.5(12) ? ? ? ? C5 W2 C16 126.4(14) ? ? ? ? C5 W2 C17 149.6(10) ? ? ? ? C6 W2 C13 142.7(9) ? ? ? ? C6 W2 C14 141.5(11) ? ? ? ? C6 W2 C15 106.1(11) ? ? ? ? C6 W2 C16 89.8(9) ? ? ? ? C6 W2 C17 108.6(10) ? ? ? ? C13 W2 C14 32.2(11) ? ? ? ? C13 W2 C15 54.9(11) ? ? ? ? C13 W2 C16 55.8(10) ? ? ? ? C13 W2 C17 34.3(10) ? ? ? ? C14 W2 C15 35.4(12) ? ? ? ? C14 W2 C16 58.6(10) ? ? ? ? C14 W2 C17 55.6(9) ? ? ? ? C15 W2 C16 35.2(13) ? ? ? ? C15 W2 C17 53.8(10) ? ? ? ? C16 W2 C17 30.9(11) ? ? ? ? W1 S W2 126.82(25) ? ? ? ? W1 S C6 115.5(7) ? ? ? ? W2 S C6 55.6(8) ? ? ? ? W1 C1 O1 177.7(20) ? ? ? ? W1 C2 O2 172.8(23) ? ? ? ? W1 C3 O3 178.6(20) ? ? ? ? W2 C4 O4 176.7(20) ? ? ? ? W2 C5 O5 172(4) ? ? ? ? W2 C6 S 78.9(8) ? ? ? ? W2 C6 C7 158.4(21) ? ? ? ? S C6 C7 122.6(21) ? ? ? ? W1 C8 C9 71.3(16) ? ? ? ? W1 C8 C12 69.0(16) ? ? ? ? C9 C8 C12 106(3) ? ? ? ? W1 C9 C8 74.1(16) ? ? ? ? W1 C9 C10 72.4(16) ? ? ? ? C8 C9 C10 109.5(25) ? ? ? ? W1 C10 C9 74.9(15) ? ? ? ? W1 C10 C11 69.7(16) ? ? ? ? C9 C10 C11 110.4(23) ? ? ? ? W1 C11 C10 75.9(17) ? ? ? ? W1 C11 C12 73.7(15) ? ? ? ? C10 C11 C12 107.9(24) ? ? ? ? W1 C12 C8 76.0(15) ? ? ? ? W1 C12 C11 69.8(16) ? ? ? ? C8 C12 C11 105.9(23) ? ? ? ? W2 C13 C14 69.5(15) ? ? ? ? W2 C13 C17 73.3(13) ? ? ? ? C14 C13 C17 107(3) ? ? ? ? W2 C14 C13 78.4(16) ? ? ? ? W2 C14 C15 73.1(16) ? ? ? ? C13 C14 C15 106(3) ? ? ? ? W2 C15 C14 71.5(16) ? ? ? ? W2 C15 C16 74.4(17) ? ? ? ? C14 C15 C16 108.2(24) ? ? ? ? W2 C16 C15 70.5(17) ? ? ? ? W2 C16 C17 76.5(18) ? ? ? ? C15 C16 C17 105(3) ? ? ? ? W2 C17 C13 72.4(13) ? ? ? ? W2 C17 C16 72.6(16) ? ? ? ? C13 C17 C16 111(3) ? ? ? ? data_IC3807 #======================================================================= # 5. CHEMICAL DATA _chemical_name_systematic ; ? #Insert the chemical name here. ; _chemical_name_common ? _chemical_formula_moiety 'C20 H16 O6 W2 ' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C20 H16 O6 W2 ' _chemical_formula_weight 720.04 _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 ? 0.002 0.002 'International Tables Vol. IV Table 2.2B' H ? 0.000 0.000 'International Tables Vol. IV Table 2.2B' O ? 0.008 0.006 'International Tables Vol. IV Table 2.2B' W ? -1.421 6.872 'International Tables Vol. IV Table 2.2B' #======================================================================= # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z 1/2+x,1/2+y,z 1/2-x,1/2-y,-z -x,y,1/2-z x,-y,1/2+z 1/2-x,1/2+y,1/2-z 1/2+x,1/2-y,1/2+z _cell_length_a 26.296(5) _cell_length_b 7.0225(22) _cell_length_c 24.226(6) _cell_angle_alpha 90.0 _cell_angle_beta 118.299(20) _cell_angle_gamma 90.0 _cell_volume 3939.0(17) _cell_formula_units_Z 8 _cell_measurement_temperature 298 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 9.50 _cell_measurement_theta_max 13.50 _cell_special_details ; ? #Insert any comments here. ; _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.05 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.428 _exptl_crystal_density_method ? _exptl_crystal_F_000 2639.16 _exptl_absorpt_coefficient_mu 11.96 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3934 _exptl_absorpt_correction_T_max 0.9998 #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ; ? #Insert any special details here. ; _diffrn_ambient_temperature 298 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Molybdenum K\a' _diffrn_radiation_source 'xray tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius CAD-4 ' _diffrn_measurement_method 'Theta/2theta scan b/P/b ' _diffrn_standards_number 3 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0.0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 0 0 0 0 0 0 0 0 _diffrn_reflns_number 3483 _diffrn_reflns_av_R_equivalents 0.035 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 24.94 _diffrn_reflns_reduction_process ? _reflns_number_total 3465 _reflns_number_observed 2549 _reflns_observed_criterion 'Inet > 2.0\s(Inet)' _computing_data_collection 'NONIUS CAD4' _computing_cell_refinement 'NONIUS CAD4' _computing_data_reduction 'NRCVAX DATRD2' _computing_structure_solution 'NRCVAX SOLVER' _computing_structure_refinement 'NRCVAX LSTSQ' _computing_molecular_graphics 'NRCVAX ORTEP' _computing_publication_material 'NRCVAX TABLES' #======================================================================= # 8. REFINEMENT DATA _refine_special_details ; ? #Insert any special details here. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type atomblock _refine_ls_weighting_scheme 1/(\s^2^(F)+0.0001F^2^) _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method Larson _refine_ls_extinction_coef 5251(198) _refine_ls_number_reflns 2549 _refine_ls_number_parameters 254 _refine_ls_number_restraints ? _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.062 _refine_ls_R_factor_obs 0.038 _refine_ls_wR_factor_all 0.039 _refine_ls_wR_factor_obs 0.038 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.14 _refine_ls_restrained_S_all ? _refine_ls_restrained_S_obs ? _refine_ls_shift/esd_max 0.024 _refine_ls_shift/esd_mean ? _refine_diff_density_max 5.70 _refine_diff_density_min -1.37 #======================================================================= # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _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_calc_flag _atom_site_refinement_flags _atom_site_type_symbol W1 0.501947(19) 0.28562(7) 0.130823(24) 0.0317(3) Uani ? . W W2 0.723868(18) 0.25191(7) 0.107392(24) 0.0327(3) Uani ? . W C1 0.5366(5) 0.0950(19) 0.1967(6) 0.045(9) Uani ? . C C2 0.5015(5) 0.0530(18) 0.0862(6) 0.042(9) Uani ? . C C3 0.6912(5) 0.4877(18) 0.1221(7) 0.050(11) Uani ? . C C4 0.7343(6) 0.4443(19) 0.0552(7) 0.052(11) Uani ? . C C5 0.6750(5) 0.1616(18) 0.0237(6) 0.045(8) Uani ? . C C6 0.5511(5) 0.4122(19) 0.0827(6) 0.044(9) Uani ? . C C7 0.5911(5) 0.3572(18) 0.1436(6) 0.041(9) Uani ? . C C8 0.5856(5) 0.4465(19) 0.1929(7) 0.050(10) Uani ? . C C9 0.6343(4) 0.1930(18) 0.1592(6) 0.039(9) Uani ? . C C10 0.6430(5) 0.1163(19) 0.1089(7) 0.053(11) Uani ? . C C11 0.4104(5) 0.2635(19) 0.1194(7) 0.057(10) Uani ? . C C12 0.4402(5) 0.3923(23) 0.1652(6) 0.054(10) Uani ? . C C13 0.4521(5) 0.5539(19) 0.1391(8) 0.062(12) Uani ? . C C14 0.4311(5) 0.5191(22) 0.0758(8) 0.066(11) Uani ? . C C15 0.4057(5) 0.3411(24) 0.0638(7) 0.073(11) Uani ? . C C16 0.7822(6) -0.0136(20) 0.1466(9) 0.081(13) Uani ? . C C17 0.7711(6) 0.045(3) 0.1914(9) 0.092(15) Uani ? . C C18 0.7952(8) 0.217(3) 0.2108(7) 0.113(15) Uani ? . C C19 0.8204(6) 0.2651(23) 0.1731(8) 0.087(13) Uani ? . C C20 0.8123(6) 0.118(3) 0.1348(8) 0.093(15) Uani ? . C O1 0.5545(4) -0.0193(16) 0.2358(5) 0.073(9) Uani ? . O O2 0.4993(4) -0.0845(14) 0.0586(6) 0.080(10) Uani ? . O O3 0.6759(4) 0.6309(13) 0.1314(6) 0.084(11) Uani ? . O O4 0.7403(4) 0.5600(16) 0.0255(6) 0.087(10) Uani ? . O O5 0.6470(4) 0.1043(17) -0.0279(5) 0.077(8) Uani ? . O O6 0.6615(4) 0.1422(16) 0.2137(5) 0.069(8) Uani ? . O H6a 0.525 0.510 0.077 0.0541 Uiso ? . H H6b 0.548 0.343 0.046 0.0541 Uiso ? . H H8a 0.590 0.364 0.229 0.0604 Uiso ? . H H8b 0.580 0.578 0.196 0.0604 Uiso ? . H H10a 0.647 -0.019 0.113 0.0639 Uiso ? . H H10b 0.609 0.142 0.069 0.0639 Uiso ? . H H11 0.395 0.141 0.123 0.0602 Uiso ? . H H12 0.451 0.375 0.209 0.0614 Uiso ? . H H13 0.471 0.669 0.160 0.0634 Uiso ? . H H14 0.432 0.607 0.046 0.0727 Uiso ? . H H15 0.389 0.276 0.022 0.0786 Uiso ? . H H16 0.773 -0.133 0.122 0.0822 Uiso ? . H H17 0.750 -0.039 0.205 0.0868 Uiso ? . H H18 0.792 0.291 0.242 0.0979 Uiso ? . H H19 0.842 0.385 0.177 0.0854 Uiso ? . H H20 0.826 0.129 0.103 0.0901 Uiso ? . H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol W1 0.02442(23) 0.0342(3) 0.0362(3) 0.00294(21) 0.01397(21) 0.0018(3) W W2 0.02663(23) 0.02853(24) 0.0416(3) 0.00191(21) 0.01510(21) -0.0019(3) W C1 0.031(7) 0.056(9) 0.050(10) 0.004(6) 0.021(7) 0.004(8) C C2 0.041(7) 0.047(8) 0.043(9) -0.007(6) 0.026(7) -0.005(7) C C3 0.057(9) 0.035(8) 0.082(12) -0.006(6) 0.053(9) 0.002(8) C C4 0.061(9) 0.044(8) 0.060(11) 0.011(7) 0.036(8) 0.018(8) C C5 0.037(7) 0.040(8) 0.046(9) 0.002(6) 0.011(6) -0.007(7) C C6 0.040(7) 0.054(9) 0.045(9) 0.018(6) 0.025(7) 0.021(7) C C7 0.031(7) 0.044(8) 0.054(9) -0.008(6) 0.025(6) 0.002(7) C C8 0.034(7) 0.045(8) 0.079(12) -0.008(6) 0.033(8) -0.012(8) C C9 0.030(6) 0.040(7) 0.051(9) 0.001(5) 0.024(6) 0.005(7) C C10 0.036(7) 0.037(8) 0.087(13) 0.004(6) 0.030(8) 0.013(8) C C11 0.027(6) 0.048(8) 0.094(12) 0.005(6) 0.028(7) 0.022(9) C C12 0.034(7) 0.093(12) 0.039(9) 0.012(7) 0.020(7) -0.010(9) C C13 0.035(7) 0.039(8) 0.115(15) 0.013(6) 0.038(9) -0.001(9) C C14 0.036(8) 0.073(11) 0.087(14) 0.031(7) 0.028(8) 0.036(10) C C15 0.016(6) 0.098(13) 0.072(12) 0.016(7) -0.007(7) 0.002(10) C C16 0.045(9) 0.038(9) 0.116(17) 0.013(7) 0.002(9) -0.008(10) C C17 0.054(10) 0.129(16) 0.105(16) 0.040(10) 0.047(10) 0.072(14) C C18 0.117(14) 0.129(17) 0.029(9) 0.078(13) -0.019(9) -0.019(11) C C19 0.051(9) 0.068(11) 0.096(14) -0.016(8) -0.003(9) 0.027(11) C C20 0.043(9) 0.166(19) 0.063(12) 0.049(11) 0.020(8) 0.026(13) C O1 0.058(6) 0.093(9) 0.080(9) 0.026(6) 0.041(6) 0.043(7) O O2 0.090(8) 0.048(6) 0.104(10) -0.013(6) 0.048(7) -0.035(7) O O3 0.092(8) 0.036(6) 0.151(13) 0.006(5) 0.078(8) -0.008(7) O O4 0.092(8) 0.077(8) 0.111(11) 0.009(7) 0.064(8) 0.033(8) O O5 0.051(6) 0.095(9) 0.071(8) 0.009(6) 0.016(6) -0.019(7) O O6 0.045(6) 0.102(9) 0.067(8) 0.028(6) 0.032(5) 0.036(7) O #======================================================================= # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 C1 1.946(13) ? ? ? W1 C2 1.955(13) ? ? ? W1 C6 2.291(13) ? ? ? W1 C7 2.270(10) ? ? ? W1 C8 2.289(12) ? ? ? W1 C11 2.295(11) ? ? ? W1 C12 2.275(12) ? ? ? W1 C13 2.358(12) ? ? ? W1 C14 2.363(12) ? ? ? W1 C15 2.301(11) ? ? ? W2 C3 1.974(13) ? ? ? W2 C4 1.957(14) ? ? ? W2 C5 1.921(13) ? ? ? W2 C10 2.346(12) ? ? ? W2 C16 2.314(13) ? ? ? W2 C17 2.323(16) ? ? ? W2 C18 2.323(14) ? ? ? W2 C19 2.271(13) ? ? ? W2 C20 2.296(13) ? ? ? C1 O1 1.158(17) ? ? ? C2 O2 1.161(16) ? ? ? C3 O3 1.145(16) ? ? ? C4 O4 1.145(17) ? ? ? C5 O5 1.182(17) ? ? ? C6 C7 1.401(18) ? ? ? C7 C8 1.417(20) ? ? ? C7 C9 1.536(17) ? ? ? C9 C10 1.446(20) ? ? ? C9 O6 1.220(16) ? ? ? C11 C12 1.357(21) ? ? ? C11 C15 1.402(23) ? ? ? C12 C13 1.405(22) ? ? ? C13 C14 1.382(25) ? ? ? C14 C15 1.382(23) ? ? ? C16 C17 1.32(3) ? ? ? C16 C20 1.33(3) ? ? ? C17 C18 1.34(3) ? ? ? C18 C19 1.40(3) ? ? ? C19 C20 1.34(3) ? ? ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 W1 C2 75.9(6) ? ? ? ? C1 W1 C6 121.8(4) ? ? ? ? C1 W1 C7 89.4(5) ? ? ? ? C1 W1 C8 82.6(5) ? ? ? ? C1 W1 C11 96.2(5) ? ? ? ? C1 W1 C12 93.7(5) ? ? ? ? C1 W1 C13 122.9(6) ? ? ? ? C1 W1 C14 151.3(5) ? ? ? ? C1 W1 C15 128.7(5) ? ? ? ? C2 W1 C6 84.3(5) ? ? ? ? C2 W1 C7 89.8(5) ? ? ? ? C2 W1 C8 121.9(5) ? ? ? ? C2 W1 C11 98.3(5) ? ? ? ? C2 W1 C12 131.2(5) ? ? ? ? C2 W1 C13 148.9(5) ? ? ? ? C2 W1 C14 118.1(6) ? ? ? ? C2 W1 C15 92.0(5) ? ? ? ? C6 W1 C7 35.8(5) ? ? ? ? C6 W1 C8 63.0(5) ? ? ? ? C6 W1 C11 141.0(5) ? ? ? ? C6 W1 C12 137.0(5) ? ? ? ? C6 W1 C13 101.8(5) ? ? ? ? C6 W1 C14 85.9(5) ? ? ? ? C6 W1 C15 105.8(5) ? ? ? ? C7 W1 C8 36.2(5) ? ? ? ? C7 W1 C11 171.1(5) ? ? ? ? C7 W1 C12 138.4(5) ? ? ? ? C7 W1 C13 113.1(5) ? ? ? ? C7 W1 C14 114.2(5) ? ? ? ? C7 W1 C15 141.1(6) ? ? ? ? C8 W1 C11 137.6(5) ? ? ? ? C8 W1 C12 103.1(5) ? ? ? ? C8 W1 C13 87.1(5) ? ? ? ? C8 W1 C14 106.5(5) ? ? ? ? C8 W1 C15 140.6(5) ? ? ? ? C11 W1 C12 34.5(5) ? ? ? ? C11 W1 C13 58.0(5) ? ? ? ? C11 W1 C14 58.5(5) ? ? ? ? C11 W1 C15 35.5(6) ? ? ? ? C12 W1 C13 35.2(6) ? ? ? ? C12 W1 C14 57.9(5) ? ? ? ? C12 W1 C15 57.7(5) ? ? ? ? C13 W1 C14 34.1(6) ? ? ? ? C13 W1 C15 56.9(6) ? ? ? ? C14 W1 C15 34.4(6) ? ? ? ? C3 W2 C4 75.1(6) ? ? ? ? C3 W2 C5 109.7(6) ? ? ? ? C3 W2 C10 82.1(5) ? ? ? ? C3 W2 C16 149.6(7) ? ? ? ? C3 W2 C17 117.6(7) ? ? ? ? C3 W2 C18 95.3(6) ? ? ? ? C3 W2 C19 106.1(6) ? ? ? ? C3 W2 C20 139.5(7) ? ? ? ? C4 W2 C5 76.9(6) ? ? ? ? C4 W2 C10 134.1(5) ? ? ? ? C4 W2 C16 123.6(6) ? ? ? ? C4 W2 C17 144.8(5) ? ? ? ? C4 W2 C18 118.7(7) ? ? ? ? C4 W2 C19 88.4(6) ? ? ? ? C4 W2 C20 92.2(6) ? ? ? ? C5 W2 C10 74.1(6) ? ? ? ? C5 W2 C16 98.6(6) ? ? ? ? C5 W2 C17 122.0(7) ? ? ? ? C5 W2 C18 153.8(6) ? ? ? ? C5 W2 C19 136.0(6) ? ? ? ? C5 W2 C20 104.4(6) ? ? ? ? C10 W2 C16 95.5(5) ? ? ? ? C10 W2 C17 81.1(5) ? ? ? ? C10 W2 C18 102.4(7) ? ? ? ? C10 W2 C19 136.6(6) ? ? ? ? C10 W2 C20 129.0(6) ? ? ? ? C16 W2 C17 33.0(7) ? ? ? ? C16 W2 C18 55.5(6) ? ? ? ? C16 W2 C19 56.0(5) ? ? ? ? C16 W2 C20 33.5(7) ? ? ? ? C17 W2 C18 33.6(7) ? ? ? ? C17 W2 C19 57.0(6) ? ? ? ? C17 W2 C20 56.1(6) ? ? ? ? C18 W2 C19 35.5(8) ? ? ? ? C18 W2 C20 57.0(6) ? ? ? ? C19 W2 C20 34.1(7) ? ? ? ? W1 C1 O1 176.5(10) ? ? ? ? W1 C2 O2 177.8(10) ? ? ? ? W2 C3 O3 175.0(10) ? ? ? ? W2 C4 O4 178.5(14) ? ? ? ? W2 C5 O5 177.3(11) ? ? ? ? W1 C6 C7 71.3(7) ? ? ? ? W1 C7 C6 72.9(7) ? ? ? ? W1 C7 C8 72.6(6) ? ? ? ? W1 C7 C9 117.6(8) ? ? ? ? C6 C7 C8 116.2(11) ? ? ? ? C6 C7 C9 124.4(12) ? ? ? ? C8 C7 C9 119.0(12) ? ? ? ? W1 C8 C7 71.2(7) ? ? ? ? C7 C9 C10 117.8(11) ? ? ? ? C7 C9 O6 118.2(12) ? ? ? ? C10 C9 O6 123.9(11) ? ? ? ? W2 C10 C9 111.6(8) ? ? ? ? W1 C11 C12 71.9(7) ? ? ? ? W1 C11 C15 72.5(7) ? ? ? ? C12 C11 C15 106.3(13) ? ? ? ? W1 C12 C11 73.5(8) ? ? ? ? W1 C12 C13 75.6(7) ? ? ? ? C11 C12 C13 109.6(13) ? ? ? ? W1 C13 C12 69.2(7) ? ? ? ? W1 C13 C14 73.2(8) ? ? ? ? C12 C13 C14 107.4(13) ? ? ? ? W1 C14 C13 72.8(7) ? ? ? ? W1 C14 C15 70.4(7) ? ? ? ? C13 C14 C15 107.0(14) ? ? ? ? W1 C15 C11 72.0(7) ? ? ? ? W1 C15 C14 75.2(7) ? ? ? ? C11 C15 C14 109.6(14) ? ? ? ? W2 C16 C17 73.9(9) ? ? ? ? W2 C16 C20 72.5(9) ? ? ? ? C17 C16 C20 110.3(16) ? ? ? ? W2 C17 C16 73.1(10) ? ? ? ? W2 C17 C18 73.2(9) ? ? ? ? C16 C17 C18 108.5(16) ? ? ? ? W2 C18 C17 73.2(9) ? ? ? ? W2 C18 C19 70.3(8) ? ? ? ? C17 C18 C19 106.2(15) ? ? ? ? W2 C19 C18 74.3(8) ? ? ? ? W2 C19 C20 74.0(8) ? ? ? ? C18 C19 C20 107.2(15) ? ? ? ? W2 C20 C16 74.0(8) ? ? ? ? W2 C20 C19 72.0(9) ? ? ? ? C16 C20 C19 107.7(16) ? ? ? ?