# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1663 data_mm9636 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C10 H5 As2 Co Mo O5' _chemical_formula_weight 509.85 _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' 'Co' 'Co' 0.3494 0.9721 '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' _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 8.899(2) _cell_length_b 14.465(2) _cell_length_c 11.046(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.440(10) _cell_angle_gamma 90.00 _cell_volume 1421.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.382 _exptl_crystal_density_method ? _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 6.678 _exptl_absorpt_correction_type Psi-scans _exptl_absorpt_correction_T_min 0.806 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 AFC5R _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 3466 _diffrn_reflns_av_R_equivalents 0.0365 _diffrn_reflns_av_sigmaI/netI 0.0798 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3263 _reflns_number_observed 2118 _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 8 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^)+(0.0514P)^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 3255 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1101 _refine_ls_R_factor_obs 0.0409 _refine_ls_wR_factor_all 0.1831 _refine_ls_wR_factor_obs 0.0959 _refine_ls_goodness_of_fit_all 1.025 _refine_ls_goodness_of_fit_obs 1.081 _refine_ls_restrained_S_all 1.640 _refine_ls_restrained_S_obs 1.081 _refine_ls_shift/esd_max 0.000 _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 0.24903(6) 0.41055(4) 0.22110(4) 0.02744(14) Uani 1 d . . As2 As 0.00318(9) 0.37582(6) 0.09198(7) 0.0460(2) Uani 1 d . . As1 As 0.16484(9) 0.25419(5) 0.13000(7) 0.0471(2) Uani 1 d . . Co1 Co -0.00192(10) 0.30381(7) 0.28699(8) 0.0401(3) Uani 1 d . . O2 O -0.2581(7) 0.1851(5) 0.2232(7) 0.084(2) Uani 1 d . . C4 C 0.1248(8) 0.5254(5) 0.2277(7) 0.044(2) Uani 1 d . . C5 C 0.3025(8) 0.4449(5) 0.0525(7) 0.046(2) Uani 1 d . . C2 C -0.1585(9) 0.2322(6) 0.2470(7) 0.054(2) Uani 1 d . . O5 O 0.3399(7) 0.4638(5) -0.0419(5) 0.070(2) Uani 1 d . . C3 C 0.0957(10) 0.2355(6) 0.3985(8) 0.061(2) Uani 1 d . . C8 C 0.3794(8) 0.4797(5) 0.3846(6) 0.044(2) Uani 1 d . . H8 H 0.3464(8) 0.5332(5) 0.4315(6) 0.052 Uiso 1 calc R . O4 O 0.0637(7) 0.5940(4) 0.2338(6) 0.069(2) Uani 1 d . . C9 C 0.3595(9) 0.3859(6) 0.4147(6) 0.051(2) Uani 1 d . . H9 H 0.3067(9) 0.3631(6) 0.4856(6) 0.061 Uiso 1 calc R . O3 O 0.1507(8) 0.1905(5) 0.4716(6) 0.092(2) Uani 1 d . . C6 C 0.5041(8) 0.3907(6) 0.2482(7) 0.051(2) Uani 1 d . . H6 H 0.5750(8) 0.3721(6) 0.1862(7) 0.061 Uiso 1 calc R . C1 C -0.0828(10) 0.3985(6) 0.3661(8) 0.061(2) Uani 1 d . . C7 C 0.4691(8) 0.4818(5) 0.2821(7) 0.046(2) Uani 1 d . . H7 H 0.5105(8) 0.5378(5) 0.2457(7) 0.055 Uiso 1 calc R . O1 O -0.1372(9) 0.4578(6) 0.4164(8) 0.112(3) Uani 1 d . . C10 C 0.4344(9) 0.3314(5) 0.3331(7) 0.052(2) Uani 1 d . . H10 H 0.4459(9) 0.2641(5) 0.3377(7) 0.062 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 Mo1 0.0280(3) 0.0280(3) 0.0262(3) 0.0010(2) -0.0019(2) 0.0005(2) As2 0.0428(4) 0.0530(5) 0.0414(4) 0.0078(4) -0.0163(3) -0.0070(4) As1 0.0522(5) 0.0372(4) 0.0518(5) -0.0131(3) 0.0006(4) -0.0032(4) Co1 0.0349(5) 0.0436(6) 0.0417(5) 0.0048(4) -0.0009(4) -0.0068(4) O2 0.052(4) 0.085(5) 0.116(6) 0.000(4) -0.015(4) -0.029(4) C4 0.044(4) 0.037(4) 0.050(4) 0.002(3) 0.001(3) 0.004(3) C5 0.041(4) 0.053(5) 0.045(4) 0.002(4) 0.006(3) -0.005(3) C2 0.045(4) 0.059(5) 0.059(5) 0.005(4) 0.001(4) -0.006(4) O5 0.075(4) 0.100(5) 0.036(3) 0.017(3) 0.012(3) -0.015(4) C3 0.051(5) 0.065(6) 0.067(6) 0.017(5) -0.005(4) -0.023(4) C8 0.051(4) 0.048(4) 0.031(3) -0.012(3) -0.009(3) -0.001(4) O4 0.068(4) 0.040(3) 0.100(5) 0.000(3) 0.003(4) 0.015(3) C9 0.054(5) 0.066(5) 0.033(4) 0.011(4) -0.013(3) -0.016(4) O3 0.081(5) 0.106(6) 0.089(5) 0.055(5) -0.024(4) -0.014(4) C6 0.026(3) 0.072(6) 0.053(4) -0.015(4) -0.007(3) 0.014(4) C1 0.065(6) 0.063(6) 0.057(5) -0.005(4) 0.022(4) -0.001(5) C7 0.034(4) 0.051(5) 0.050(4) 0.000(3) -0.010(3) -0.017(3) O1 0.111(6) 0.096(6) 0.132(7) -0.045(5) 0.063(6) -0.005(5) C10 0.053(5) 0.040(4) 0.061(5) -0.001(4) -0.027(4) 0.008(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 Mo1 C5 1.997(7) . ? Mo1 C4 1.998(7) . ? Mo1 C7 2.299(6) . ? Mo1 C6 2.300(7) . ? Mo1 C10 2.337(7) . ? Mo1 C8 2.346(6) . ? Mo1 C9 2.359(7) . ? Mo1 As1 2.5791(9) . ? Mo1 As2 2.6299(10) . ? Mo1 Co1 2.8254(11) . ? As2 As1 2.3046(12) . ? As2 Co1 2.3942(12) . ? As1 Co1 2.4195(13) . ? Co1 C2 1.783(8) . ? Co1 C1 1.786(9) . ? Co1 C3 1.787(9) . ? O2 C2 1.143(9) . ? C4 O4 1.134(8) . ? C5 O5 1.135(8) . ? C3 O3 1.139(10) . ? C8 C7 1.402(10) . ? C8 C9 1.410(10) . ? C9 C10 1.381(11) . ? C6 C7 1.407(11) . ? C6 C10 1.425(11) . ? C1 O1 1.137(10) . ? 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 C5 Mo1 C4 88.4(3) . . ? C5 Mo1 C7 86.6(3) . . ? C4 Mo1 C7 94.9(3) . . ? C5 Mo1 C6 84.0(3) . . ? C4 Mo1 C6 130.1(3) . . ? C7 Mo1 C6 35.6(3) . . ? C5 Mo1 C10 115.7(3) . . ? C4 Mo1 C10 140.5(3) . . ? C7 Mo1 C10 58.7(3) . . ? C6 Mo1 C10 35.8(3) . . ? C5 Mo1 C8 119.1(3) . . ? C4 Mo1 C8 83.2(3) . . ? C7 Mo1 C8 35.1(2) . . ? C6 Mo1 C8 59.1(3) . . ? C10 Mo1 C8 58.2(3) . . ? C5 Mo1 C9 141.2(3) . . ? C4 Mo1 C9 108.1(3) . . ? C7 Mo1 C9 58.0(3) . . ? C6 Mo1 C9 58.4(3) . . ? C10 Mo1 C9 34.2(3) . . ? C8 Mo1 C9 34.9(3) . . ? C5 Mo1 As1 85.9(2) . . ? C4 Mo1 As1 126.0(2) . . ? C7 Mo1 As1 138.1(2) . . ? C6 Mo1 As1 102.5(2) . . ? C10 Mo1 As1 88.3(2) . . ? C8 Mo1 As1 143.9(2) . . ? C9 Mo1 As1 109.4(2) . . ? C5 Mo1 As2 75.9(2) . . ? C4 Mo1 As2 74.0(2) . . ? C7 Mo1 As2 159.3(2) . . ? C6 Mo1 As2 148.4(2) . . ? C10 Mo1 As2 139.5(2) . . ? C8 Mo1 As2 152.6(2) . . ? C9 Mo1 As2 141.7(2) . . ? As1 Mo1 As2 52.51(3) . . ? C5 Mo1 Co1 125.8(2) . . ? C4 Mo1 Co1 90.2(2) . . ? C7 Mo1 Co1 147.4(2) . . ? C6 Mo1 Co1 133.0(2) . . ? C10 Mo1 Co1 98.5(2) . . ? C8 Mo1 Co1 114.4(2) . . ? C9 Mo1 Co1 89.9(2) . . ? As1 Mo1 Co1 52.95(3) . . ? As2 Mo1 Co1 51.91(3) . . ? As1 As2 Co1 61.95(4) . . ? As1 As2 Mo1 62.61(3) . . ? Co1 As2 Mo1 68.25(3) . . ? As2 As1 Co1 60.85(4) . . ? As2 As1 Mo1 64.88(3) . . ? Co1 As1 Mo1 68.75(3) . . ? C2 Co1 C1 104.1(4) . . ? C2 Co1 C3 102.3(4) . . ? C1 Co1 C3 106.4(4) . . ? C2 Co1 As2 93.6(3) . . ? C1 Co1 As2 97.1(3) . . ? C3 Co1 As2 147.2(3) . . ? C2 Co1 As1 98.0(3) . . ? C1 Co1 As1 147.2(3) . . ? C3 Co1 As1 91.9(3) . . ? As2 Co1 As1 57.21(4) . . ? C2 Co1 Mo1 150.6(3) . . ? C1 Co1 Mo1 92.2(3) . . ? C3 Co1 Mo1 96.1(3) . . ? As2 Co1 Mo1 59.83(3) . . ? As1 Co1 Mo1 58.30(3) . . ? O4 C4 Mo1 174.9(7) . . ? O5 C5 Mo1 176.8(7) . . ? O2 C2 Co1 178.6(8) . . ? O3 C3 Co1 176.4(8) . . ? C7 C8 C9 106.8(7) . . ? C7 C8 Mo1 70.6(4) . . ? C9 C8 Mo1 73.0(4) . . ? C10 C9 C8 109.3(7) . . ? C10 C9 Mo1 72.0(4) . . ? C8 C9 Mo1 72.1(4) . . ? C7 C6 C10 106.6(7) . . ? C7 C6 Mo1 72.1(4) . . ? C10 C6 Mo1 73.5(4) . . ? O1 C1 Co1 178.5(9) . . ? C8 C7 C6 109.3(7) . . ? C8 C7 Mo1 74.3(4) . . ? C6 C7 Mo1 72.2(4) . . ? C9 C10 C6 108.1(7) . . ? C9 C10 Mo1 73.7(4) . . ? C6 C10 Mo1 70.7(4) . . ? _refine_diff_density_max 0.660 _refine_diff_density_min -0.939 _refine_diff_density_rms 0.173 data_mm9506 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C10 H5 As2 Co O5 W' _chemical_formula_weight 597.76 _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' 'Co' 'Co' 0.3494 0.9721 '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 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 8.899(2) _cell_length_b 14.471(3) _cell_length_c 11.046(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.42(3) _cell_angle_gamma 90.00 _cell_volume 1422.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.792 _exptl_crystal_density_method ? _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 13.876 _exptl_absorpt_correction_type Psi-scans _exptl_absorpt_correction_T_min 0.300 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 AFC5R _diffrn_measurement_method 'omega/2theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_decay_% -0.9% _diffrn_reflns_number 3443 _diffrn_reflns_av_R_equivalents 0.0478 _diffrn_reflns_av_sigmaI/netI 0.0706 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.63 _diffrn_reflns_theta_max 27.46 _reflns_number_total 3243 _reflns_number_observed 2355 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'teXsan' _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 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^)+(0.1000P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3243 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0810 _refine_ls_R_factor_obs 0.0428 _refine_ls_wR_factor_all 0.1347 _refine_ls_wR_factor_obs 0.1122 _refine_ls_goodness_of_fit_all 0.900 _refine_ls_goodness_of_fit_obs 0.887 _refine_ls_restrained_S_all 0.900 _refine_ls_restrained_S_obs 0.887 _refine_ls_shift/esd_max 0.000 _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 W1 W 0.24904(4) 0.40986(3) 0.22008(3) 0.02677(15) Uani 1 d . . As2 As 0.00266(14) 0.37622(10) 0.09085(11) 0.0449(3) Uani 1 d . . As1 As 0.1645(2) 0.25327(8) 0.12948(12) 0.0451(3) Uani 1 d . . Co1 Co -0.0020(2) 0.30426(11) 0.28706(14) 0.0383(4) Uani 1 d . . O2 O -0.2586(11) 0.1861(9) 0.2231(11) 0.081(4) Uani 1 d . . C4 C 0.1249(14) 0.5237(8) 0.2257(11) 0.041(3) Uani 1 d . . C5 C 0.3028(13) 0.4438(9) 0.0520(10) 0.043(3) Uani 1 d . . C2 C -0.1577(15) 0.2331(9) 0.2481(13) 0.053(3) Uani 1 d . . O5 O 0.3409(11) 0.4652(9) -0.0424(9) 0.069(3) Uani 1 d . . C3 C 0.0928(16) 0.2349(10) 0.3987(14) 0.062(4) Uani 1 d . . C8 C 0.3782(13) 0.4779(8) 0.3853(10) 0.040(3) Uani 1 d . . H8A H 0.3432(13) 0.5309(8) 0.4322(10) 0.048 Uiso 1 calc R . O4 O 0.0620(13) 0.5939(6) 0.2335(12) 0.074(3) Uani 1 d . . C9 C 0.3584(13) 0.3851(9) 0.4155(10) 0.041(3) Uani 1 d . . H9A H 0.3055(13) 0.3622(9) 0.4863(10) 0.049 Uiso 1 calc R . O3 O 0.1487(13) 0.1925(9) 0.4724(12) 0.098(4) Uani 1 d . . C6 C 0.5052(13) 0.3913(10) 0.2492(11) 0.046(3) Uani 1 d . . H6A H 0.5765(13) 0.3730(10) 0.1874(11) 0.055 Uiso 1 calc R . C1 C -0.0834(16) 0.4002(10) 0.3657(14) 0.058(4) Uani 1 d . . C7 C 0.4688(13) 0.4827(9) 0.2816(11) 0.044(3) Uani 1 d . . H7A H 0.5104(13) 0.5391(9) 0.2464(11) 0.052 Uiso 1 calc R . O1 O -0.1393(15) 0.4592(11) 0.4128(14) 0.108(5) Uani 1 d . . C10 C 0.4339(16) 0.3308(8) 0.3326(14) 0.058(4) Uani 1 d . . H10A H 0.4461(16) 0.2635(8) 0.3366(14) 0.070 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 0.0278(2) 0.0262(2) 0.0263(2) 0.0011(2) 0.00124(14) 0.0004(2) As2 0.0408(7) 0.0526(7) 0.0407(6) 0.0079(6) -0.0136(5) -0.0059(6) As1 0.0499(7) 0.0352(6) 0.0501(7) -0.0114(5) 0.0035(6) -0.0029(5) Co1 0.0339(8) 0.0413(8) 0.0397(8) 0.0054(7) 0.0029(6) -0.0066(6) O2 0.055(7) 0.076(7) 0.111(10) 0.003(7) -0.007(6) -0.024(5) C4 0.048(7) 0.036(6) 0.040(6) 0.005(5) 0.002(5) 0.001(5) C5 0.043(6) 0.055(7) 0.031(5) 0.013(5) 0.004(5) -0.002(6) C2 0.039(7) 0.053(7) 0.067(9) 0.005(7) 0.004(6) -0.005(6) O5 0.063(6) 0.101(8) 0.043(5) 0.019(5) 0.012(5) -0.020(6) C3 0.051(8) 0.066(9) 0.068(9) 0.019(8) -0.004(7) -0.029(7) C8 0.040(6) 0.040(6) 0.040(6) -0.011(5) -0.001(5) 0.006(5) O4 0.077(8) 0.044(5) 0.101(9) -0.002(5) -0.007(7) 0.022(5) C9 0.042(6) 0.053(7) 0.028(5) 0.015(5) 0.001(5) -0.011(5) O3 0.078(8) 0.114(10) 0.102(9) 0.067(8) -0.019(7) -0.016(8) C6 0.030(6) 0.065(8) 0.043(6) -0.014(6) 0.006(5) 0.016(5) C1 0.050(8) 0.063(9) 0.064(8) -0.022(7) 0.027(7) -0.017(7) C7 0.031(6) 0.056(7) 0.043(6) -0.003(6) -0.003(5) -0.015(5) O1 0.089(10) 0.101(10) 0.135(13) -0.042(10) 0.049(9) -0.002(8) C10 0.060(8) 0.034(6) 0.078(10) 0.012(7) -0.036(8) -0.002(6) _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 C4 1.985(12) . ? W1 C5 1.990(11) . ? W1 C7 2.309(10) . ? W1 C6 2.310(11) . ? W1 C10 2.336(11) . ? W1 C8 2.349(11) . ? W1 C9 2.373(10) . ? W1 As1 2.5816(13) . ? W1 As2 2.6319(14) . ? W1 Co1 2.821(2) . ? As2 As1 2.322(2) . ? As2 Co1 2.406(2) . ? As1 Co1 2.429(2) . ? Co1 C2 1.771(13) . ? Co1 C3 1.786(15) . ? Co1 C1 1.799(14) . ? O2 C2 1.154(15) . ? C4 O4 1.164(14) . ? C5 O5 1.147(14) . ? C3 O3 1.13(2) . ? C8 C9 1.40(2) . ? C8 C7 1.42(2) . ? C9 C10 1.39(2) . ? C6 C7 1.41(2) . ? C6 C10 1.43(2) . ? C1 O1 1.12(2) . ? 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 C4 W1 C5 88.4(5) . . ? C4 W1 C7 94.6(5) . . ? C5 W1 C7 86.6(5) . . ? C4 W1 C6 129.8(5) . . ? C5 W1 C6 84.2(5) . . ? C7 W1 C6 35.5(4) . . ? C4 W1 C10 140.8(5) . . ? C5 W1 C10 115.8(6) . . ? C7 W1 C10 59.1(5) . . ? C6 W1 C10 35.9(5) . . ? C4 W1 C8 83.7(4) . . ? C5 W1 C8 119.8(5) . . ? C7 W1 C8 35.5(4) . . ? C6 W1 C8 58.5(4) . . ? C10 W1 C8 57.8(4) . . ? C4 W1 C9 108.2(5) . . ? C5 W1 C9 141.6(4) . . ? C7 W1 C9 58.4(4) . . ? C6 W1 C9 58.3(4) . . ? C10 W1 C9 34.4(5) . . ? C8 W1 C9 34.4(4) . . ? C4 W1 As1 125.7(3) . . ? C5 W1 As1 86.0(4) . . ? C7 W1 As1 138.7(3) . . ? C6 W1 As1 103.2(3) . . ? C10 W1 As1 88.3(3) . . ? C8 W1 As1 143.3(3) . . ? C9 W1 As1 109.2(3) . . ? C4 W1 As2 73.4(3) . . ? C5 W1 As2 75.9(3) . . ? C7 W1 As2 158.8(3) . . ? C6 W1 As2 149.3(3) . . ? C10 W1 As2 139.8(3) . . ? C8 W1 As2 152.1(3) . . ? C9 W1 As2 141.5(3) . . ? As1 W1 As2 52.88(4) . . ? C4 W1 Co1 89.8(4) . . ? C5 W1 Co1 126.1(4) . . ? C7 W1 Co1 147.2(3) . . ? C6 W1 Co1 133.3(4) . . ? C10 W1 Co1 98.4(4) . . ? C8 W1 Co1 113.5(3) . . ? C9 W1 Co1 89.4(3) . . ? As1 W1 Co1 53.21(5) . . ? As2 W1 Co1 52.22(4) . . ? As1 As2 Co1 61.80(6) . . ? As1 As2 W1 62.45(4) . . ? Co1 As2 W1 67.93(5) . . ? As2 As1 Co1 60.80(6) . . ? As2 As1 W1 64.67(5) . . ? Co1 As1 W1 68.45(5) . . ? C2 Co1 C3 101.2(6) . . ? C2 Co1 C1 104.2(6) . . ? C3 Co1 C1 106.8(8) . . ? C2 Co1 As2 93.7(5) . . ? C3 Co1 As2 147.9(5) . . ? C1 Co1 As2 96.7(5) . . ? C2 Co1 As1 97.9(5) . . ? C3 Co1 As1 92.2(5) . . ? C1 Co1 As1 147.2(5) . . ? As2 Co1 As1 57.41(6) . . ? C2 Co1 W1 150.6(5) . . ? C3 Co1 W1 97.0(4) . . ? C1 Co1 W1 92.2(4) . . ? As2 Co1 W1 59.84(5) . . ? As1 Co1 W1 58.34(5) . . ? O4 C4 W1 174.5(11) . . ? O5 C5 W1 176.4(11) . . ? O2 C2 Co1 179.5(12) . . ? O3 C3 Co1 177.2(16) . . ? C9 C8 C7 108.5(11) . . ? C9 C8 W1 73.7(6) . . ? C7 C8 W1 70.7(6) . . ? C10 C9 C8 108.7(10) . . ? C10 C9 W1 71.4(6) . . ? C8 C9 W1 71.9(6) . . ? C7 C6 C10 107.6(11) . . ? C7 C6 W1 72.2(6) . . ? C10 C6 W1 73.1(7) . . ? O1 C1 Co1 177.3(15) . . ? C6 C7 C8 107.3(11) . . ? C6 C7 W1 72.3(6) . . ? C8 C7 W1 73.8(6) . . ? C9 C10 C6 107.9(10) . . ? C9 C10 W1 74.3(7) . . ? C6 C10 W1 71.1(6) . . ? _refine_diff_density_max 1.412 _refine_diff_density_min -2.019 _refine_diff_density_rms 0.280 data_m2072 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H20 As2 Co O4 P W' _chemical_formula_weight 832.02 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' 'Co' 'Co' 0.3494 0.9721 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.7720(10) _cell_length_b 20.831(2) _cell_length_c 10.493(2) _cell_angle_alpha 90.430(10) _cell_angle_beta 103.480(10) _cell_angle_gamma 90.820(10) _cell_volume 2714.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _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 2.036 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1584 _exptl_absorpt_coefficient_mu 7.355 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_correction_T_min 0.890 _exptl_absorpt_correction_T_max 0.996 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC5R' _diffrn_measurement_method theta/2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5576 _diffrn_reflns_av_R_equivalents 0.0726 _diffrn_reflns_av_sigmaI/netI 0.1096 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 20.00 _reflns_number_total 5032 _reflns_number_gt 3344 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0441P)^2^+123.9303P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5032 _refine_ls_number_parameters 339 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.1131 _refine_ls_R_factor_gt 0.0539 _refine_ls_wR_factor_ref 0.1715 _refine_ls_wR_factor_gt 0.1457 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.722 _refine_ls_shift/su_mean 0.087 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W -0.00299(8) 0.27230(5) 0.22346(11) 0.0329(4) Uani 1 1 d D . . W2 W 0.44405(9) 0.24326(5) 0.63559(11) 0.0373(4) Uani 1 1 d D . . Co1 Co -0.1580(3) 0.19042(15) 0.2839(3) 0.0342(9) Uani 1 1 d D . . Co2 Co 0.3604(3) 0.32452(16) 0.8041(3) 0.0317(9) Uani 1 1 d D . . P1 P -0.2347(5) 0.0986(3) 0.3186(6) 0.0309(17) Uani 1 1 d D . . P2 P 0.2651(5) 0.4090(3) 0.8348(6) 0.0299(17) Uani 1 1 d D . . As11 As 0.0126(2) 0.21084(15) 0.4398(3) 0.0515(9) Uani 1 1 d D . . As12 As 0.0071(2) 0.14647(14) 0.2582(3) 0.0562(9) Uani 1 1 d D . . As21 As 0.2717(2) 0.31017(13) 0.5772(3) 0.0399(8) Uani 1 1 d D . . As22 As 0.4303(2) 0.36946(13) 0.6325(3) 0.0399(8) Uani 1 1 d D . . O11 O -0.2489(19) 0.2728(12) 0.449(2) 0.095(8) Uiso 1 1 d . . . C11 C -0.207(2) 0.2385(14) 0.389(3) 0.062(9) Uiso 1 1 d D . . O12 O -0.2804(18) 0.2020(11) 0.014(2) 0.088(7) Uiso 1 1 d . . . C12 C -0.231(2) 0.1964(13) 0.126(2) 0.049(8) Uiso 1 1 d D . . C13 C 0.1486(17) 0.2555(12) 0.236(2) 0.040(7) Uiso 1 1 d D . . O13 O 0.2394(16) 0.2466(9) 0.2385(19) 0.061(6) Uiso 1 1 d . . . O14 O -0.0397(17) 0.2122(11) -0.059(2) 0.077(7) Uiso 1 1 d . . . C14 C -0.027(2) 0.2337(13) 0.049(2) 0.053(8) Uiso 1 1 d D . . O21 O 0.2502(16) 0.2237(11) 0.913(2) 0.070(6) Uiso 1 1 d . . . C21 C 0.294(2) 0.2655(15) 0.866(3) 0.055(8) Uiso 1 1 d . . . O22 O 0.5549(17) 0.3463(10) 1.007(2) 0.071(6) Uiso 1 1 d . . . C22 C 0.4761(19) 0.3373(14) 0.924(2) 0.056(8) Uiso 1 1 d D . . C23 C 0.476(2) 0.2697(13) 0.470(2) 0.044(7) Uiso 1 1 d D . . O23 O 0.4922(15) 0.2813(9) 0.3679(19) 0.058(5) Uiso 1 1 d . . . C24 C 0.5873(19) 0.2758(14) 0.720(3) 0.054(8) Uiso 1 1 d D . . O24 O 0.6754(17) 0.2919(10) 0.770(2) 0.073(6) Uiso 1 1 d . . . C111 C -0.244(2) 0.0774(13) 0.485(3) 0.042(7) Uiso 1 1 d D . . C112 C -0.193(2) 0.1181(15) 0.589(3) 0.062(9) Uiso 1 1 d . . . H111 H -0.1538 0.1537 0.5731 0.074 Uiso 1 1 calc R . . C113 C -0.203(3) 0.105(2) 0.717(4) 0.100(13) Uiso 1 1 d . . . H113 H -0.1761 0.1336 0.7858 0.119 Uiso 1 1 calc R . . C114 C -0.257(3) 0.0444(16) 0.738(3) 0.076(10) Uiso 1 1 d . . . H114 H -0.2527 0.0296 0.8224 0.091 Uiso 1 1 calc R . . C115 C -0.314(2) 0.0103(14) 0.632(3) 0.056(8) Uiso 1 1 d . . . H115 H -0.3592 -0.0235 0.6436 0.067 Uiso 1 1 calc R . . C116 C -0.304(2) 0.0257(15) 0.508(3) 0.060(9) Uiso 1 1 d . . . H116 H -0.3402 0.0004 0.4374 0.072 Uiso 1 1 calc R . . C121 C -0.3773(17) 0.0950(10) 0.238(2) 0.021(6) Uiso 1 1 d . . . C122 C -0.436(2) 0.1511(13) 0.223(2) 0.042(7) Uiso 1 1 d . . . H122 H -0.4015 0.1903 0.2495 0.050 Uiso 1 1 calc R . . C123 C -0.545(2) 0.1486(14) 0.168(3) 0.046(8) Uiso 1 1 d . . . H123 H -0.5854 0.1856 0.1671 0.055 Uiso 1 1 calc R . . C124 C -0.596(3) 0.0939(15) 0.115(3) 0.064(9) Uiso 1 1 d . . . H124 H -0.6690 0.0937 0.0747 0.076 Uiso 1 1 calc R . . C125 C -0.539(2) 0.0396(15) 0.123(3) 0.061(9) Uiso 1 1 d . . . H125 H -0.5727 0.0012 0.0894 0.073 Uiso 1 1 calc R . . C126 C -0.431(2) 0.0414(14) 0.180(3) 0.049(8) Uiso 1 1 d . . . H126 H -0.3926 0.0039 0.1802 0.059 Uiso 1 1 calc R . . C131 C -0.182(2) 0.0288(13) 0.254(3) 0.045(7) Uiso 1 1 d D . . C132 C -0.183(2) 0.0248(16) 0.126(3) 0.067(9) Uiso 1 1 d . . . H132 H -0.2170 0.0568 0.0702 0.081 Uiso 1 1 calc R . . C133 C -0.134(2) -0.0283(15) 0.070(3) 0.065(9) Uiso 1 1 d . . . H133 H -0.1318 -0.0294 -0.0182 0.078 Uiso 1 1 calc R . . C134 C -0.091(3) -0.0751(19) 0.151(4) 0.087(11) Uiso 1 1 d . . . H134 H -0.0649 -0.1111 0.1168 0.104 Uiso 1 1 calc R . . C135 C -0.085(3) -0.072(2) 0.286(4) 0.105(13) Uiso 1 1 d . . . H135 H -0.0499 -0.1040 0.3403 0.127 Uiso 1 1 calc R . . C136 C -0.131(2) -0.0207(14) 0.342(3) 0.059(9) Uiso 1 1 d . . . H136 H -0.1284 -0.0189 0.4310 0.071 Uiso 1 1 calc R . . C141 C -0.031(2) 0.3653(13) 0.337(3) 0.048(8) Uiso 1 1 d . . . H141 H -0.0303 0.3670 0.4303 0.058 Uiso 1 1 calc R . . C142 C 0.060(2) 0.3762(13) 0.284(3) 0.045(7) Uiso 1 1 d . . . H142 H 0.1328 0.3888 0.3334 0.054 Uiso 1 1 calc R . . C143 C 0.021(2) 0.3737(14) 0.143(3) 0.054(8) Uiso 1 1 d . . . H143 H 0.0621 0.3845 0.0779 0.064 Uiso 1 1 calc R . . C144 C -0.092(2) 0.3630(13) 0.120(3) 0.052(8) Uiso 1 1 d . . . H144 H -0.1430 0.3630 0.0341 0.062 Uiso 1 1 calc R . . C145 C -0.121(2) 0.3564(13) 0.241(3) 0.051(8) Uiso 1 1 d . . . H145 H -0.1941 0.3512 0.2534 0.062 Uiso 1 1 calc R . . C211 C 0.2729(18) 0.4763(11) 0.729(2) 0.030(6) Uiso 1 1 d D . . C212 C 0.364(2) 0.5156(13) 0.749(3) 0.045(7) Uiso 1 1 d . . . H212 H 0.4210 0.5102 0.8218 0.053 Uiso 1 1 calc R . . C213 C 0.370(2) 0.5632(14) 0.658(3) 0.051(8) Uiso 1 1 d . . . H213 H 0.4295 0.5906 0.6720 0.061 Uiso 1 1 calc R . . C214 C 0.289(2) 0.5704(13) 0.549(3) 0.047(8) Uiso 1 1 d . . . H214 H 0.2964 0.6015 0.4881 0.056 Uiso 1 1 calc R . . C215 C 0.200(2) 0.5349(13) 0.526(3) 0.053(8) Uiso 1 1 d . . . H215 H 0.1446 0.5411 0.4525 0.064 Uiso 1 1 calc R . . C216 C 0.193(2) 0.4873(12) 0.618(2) 0.040(7) Uiso 1 1 d . . . H216 H 0.1304 0.4618 0.6034 0.048 Uiso 1 1 calc R . . C221 C 0.2995(18) 0.4398(12) 1.005(2) 0.031(6) Uiso 1 1 d . . . C222 C 0.311(2) 0.5066(13) 1.034(3) 0.046(7) Uiso 1 1 d . . . H222 H 0.3018 0.5369 0.9674 0.056 Uiso 1 1 calc R . . C223 C 0.339(2) 0.5254(14) 1.169(3) 0.052(8) Uiso 1 1 d . . . H223 H 0.3521 0.5684 1.1918 0.062 Uiso 1 1 calc R . . C224 C 0.346(2) 0.4812(13) 1.263(3) 0.048(8) Uiso 1 1 d . . . H224 H 0.3617 0.4943 1.3506 0.058 Uiso 1 1 calc R . . C225 C 0.331(2) 0.4164(14) 1.232(3) 0.055(8) Uiso 1 1 d . . . H225 H 0.3340 0.3863 1.2980 0.066 Uiso 1 1 calc R . . C226 C 0.3100(19) 0.3971(12) 1.102(2) 0.036(7) Uiso 1 1 d . . . H226 H 0.3033 0.3535 1.0812 0.044 Uiso 1 1 calc R . . C231 C 0.1185(18) 0.4004(11) 0.810(2) 0.027(6) Uiso 1 1 d . . . C232 C 0.060(2) 0.4500(13) 0.843(2) 0.042(7) Uiso 1 1 d . . . H232 H 0.0946 0.4880 0.8773 0.050 Uiso 1 1 calc R . . C233 C -0.050(2) 0.4443(13) 0.827(3) 0.046(7) Uiso 1 1 d . . . H233 H -0.0897 0.4783 0.8491 0.055 Uiso 1 1 calc R . . C234 C -0.102(2) 0.3861(13) 0.777(2) 0.043(7) Uiso 1 1 d . . . H234 H -0.1765 0.3815 0.7677 0.052 Uiso 1 1 calc R . . C235 C -0.047(2) 0.3381(13) 0.744(2) 0.043(7) Uiso 1 1 d . . . H235 H -0.0826 0.3002 0.7102 0.052 Uiso 1 1 calc R . . C236 C 0.064(2) 0.3444(13) 0.761(2) 0.044(7) Uiso 1 1 d . . . H236 H 0.1019 0.3103 0.7378 0.053 Uiso 1 1 calc R . . C241 C 0.505(3) 0.1447(18) 0.730(4) 0.091(12) Uiso 1 1 d . . . H241 H 0.5701 0.1387 0.7989 0.110 Uiso 1 1 calc R . . C242 C 0.499(3) 0.1420(16) 0.596(3) 0.074(10) Uiso 1 1 d . . . H242 H 0.5578 0.1317 0.5543 0.089 Uiso 1 1 calc R . . C243 C 0.389(3) 0.1489(17) 0.531(4) 0.082(11) Uiso 1 1 d . . . H243 H 0.3563 0.1420 0.4372 0.098 Uiso 1 1 calc R . . C244 C 0.337(3) 0.1531(16) 0.635(3) 0.076(10) Uiso 1 1 d . . . H244 H 0.2585 0.1543 0.6231 0.092 Uiso 1 1 calc R . . C245 C 0.404(3) 0.1515(16) 0.749(4) 0.076(10) Uiso 1 1 d . . . H245 H 0.3842 0.1517 0.8339 0.091 Uiso 1 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 0.0335(7) 0.0296(7) 0.0380(7) 0.0010(5) 0.0131(5) -0.0016(5) W2 0.0402(7) 0.0278(7) 0.0473(8) -0.0021(6) 0.0170(6) 0.0030(5) Co1 0.032(2) 0.024(2) 0.048(2) 0.0027(17) 0.0106(18) -0.0043(16) Co2 0.031(2) 0.034(2) 0.029(2) -0.0015(16) 0.0060(16) 0.0036(16) P1 0.030(4) 0.035(4) 0.026(4) 0.003(3) 0.004(3) -0.002(3) P2 0.033(4) 0.026(4) 0.031(4) 0.003(3) 0.007(3) 0.000(3) As11 0.0378(18) 0.060(2) 0.052(2) 0.0221(16) 0.0023(15) -0.0114(15) As12 0.0424(19) 0.0353(19) 0.096(3) 0.0054(17) 0.0264(18) 0.0029(15) As21 0.0402(17) 0.0454(19) 0.0322(17) -0.0064(14) 0.0048(14) 0.0066(14) As22 0.0543(19) 0.0283(17) 0.0420(18) 0.0012(14) 0.0210(15) 0.0006(14) _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 C13 1.95(2) . ? W1 C14 1.95(2) . ? W1 C143 2.32(3) . ? W1 C141 2.34(3) . ? W1 C142 2.33(3) . ? W1 C144 2.36(3) . ? W1 C145 2.36(3) . ? W1 As11 2.583(3) . ? W1 As12 2.650(3) . ? W1 Co1 2.781(3) . ? W2 C24 1.95(2) . ? W2 C23 1.95(2) . ? W2 C243 2.27(4) . ? W2 C242 2.30(3) . ? W2 C244 2.31(3) . ? W2 C241 2.35(4) . ? W2 C245 2.37(3) . ? W2 As21 2.576(3) . ? W2 As22 2.637(3) . ? W2 Co2 2.832(3) . ? Co1 C12 1.71(2) . ? Co1 C11 1.71(2) . ? Co1 P1 2.208(7) . ? Co1 As12 2.383(4) . ? Co1 As11 2.431(4) . ? Co2 C21 1.70(3) . ? Co2 C22 1.72(2) . ? Co2 P2 2.219(7) . ? Co2 As22 2.380(4) . ? Co2 As21 2.400(4) . ? P1 C131 1.81(3) . ? P1 C121 1.82(2) . ? P1 C111 1.84(3) . ? P2 C211 1.81(2) . ? P2 C231 1.83(2) . ? P2 C221 1.84(2) . ? As11 As12 2.309(5) . ? As21 As22 2.310(4) . ? O11 C11 1.17(3) . ? O12 C12 1.20(3) . ? C13 O13 1.17(2) . ? O14 C14 1.19(3) . ? O21 C21 1.20(3) . ? O22 C22 1.18(3) . ? C23 O23 1.17(2) . ? C24 O24 1.17(3) . ? C111 C116 1.37(4) . ? C111 C112 1.40(4) . ? C112 C113 1.40(4) . ? C113 C114 1.47(5) . ? C114 C115 1.37(4) . ? C115 C116 1.37(4) . ? C121 C122 1.39(3) . ? C121 C126 1.36(3) . ? C122 C123 1.38(3) . ? C123 C124 1.35(4) . ? C124 C125 1.35(4) . ? C125 C126 1.37(4) . ? C131 C132 1.35(4) . ? C131 C136 1.44(4) . ? C132 C133 1.47(4) . ? C133 C134 1.33(4) . ? C134 C135 1.40(5) . ? C135 C136 1.41(4) . ? C141 C145 1.34(3) . ? C141 C142 1.42(3) . ? C142 C143 1.45(4) . ? C143 C144 1.43(4) . ? C144 C145 1.40(4) . ? C211 C216 1.38(3) . ? C211 C212 1.39(3) . ? C212 C213 1.39(4) . ? C213 C214 1.36(3) . ? C214 C215 1.32(3) . ? C215 C216 1.41(4) . ? C221 C226 1.34(3) . ? C221 C222 1.42(3) . ? C222 C223 1.43(4) . ? C223 C224 1.34(3) . ? C224 C225 1.39(4) . ? C225 C226 1.39(3) . ? C231 C232 1.38(3) . ? C231 C236 1.38(3) . ? C232 C233 1.38(3) . ? C233 C234 1.41(4) . ? C234 C235 1.32(3) . ? C235 C236 1.39(3) . ? C241 C245 1.36(4) . ? C241 C242 1.39(4) . ? C242 C243 1.42(4) . ? C243 C244 1.42(4) . ? C244 C245 1.30(4) . ? 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 C13 W1 C14 85.5(11) . . ? C13 W1 C143 89.2(10) . . ? C14 W1 C143 91.8(11) . . ? C13 W1 C141 113.3(10) . . ? C14 W1 C141 143.1(11) . . ? C143 W1 C141 58.7(10) . . ? C13 W1 C142 83.4(10) . . ? C14 W1 C142 126.7(11) . . ? C143 W1 C142 36.3(9) . . ? C141 W1 C142 35.3(9) . . ? C13 W1 C144 123.7(10) . . ? C14 W1 C144 86.6(11) . . ? C143 W1 C144 35.5(9) . . ? C141 W1 C144 56.5(10) . . ? C142 W1 C144 58.5(10) . . ? C13 W1 C145 141.6(10) . . ? C14 W1 C145 114.2(11) . . ? C143 W1 C145 59.0(10) . . ? C141 W1 C145 33.2(9) . . ? C142 W1 C145 58.2(9) . . ? C144 W1 C145 34.6(9) . . ? C13 W1 As11 88.4(8) . . ? C14 W1 As11 125.9(8) . . ? C143 W1 As11 141.9(7) . . ? C141 W1 As11 87.7(7) . . ? C142 W1 As11 105.8(6) . . ? C144 W1 As11 137.9(7) . . ? C145 W1 As11 103.3(7) . . ? C13 W1 As12 77.4(8) . . ? C14 W1 As12 73.9(8) . . ? C143 W1 As12 161.0(7) . . ? C141 W1 As12 139.2(7) . . ? C142 W1 As12 150.7(7) . . ? C144 W1 As12 150.5(7) . . ? C145 W1 As12 138.2(7) . . ? As11 W1 As12 52.35(11) . . ? C13 W1 Co1 128.1(8) . . ? C14 W1 Co1 90.3(8) . . ? C143 W1 Co1 142.6(7) . . ? C141 W1 Co1 100.5(7) . . ? C142 W1 Co1 135.6(6) . . ? C144 W1 Co1 107.5(7) . . ? C145 W1 Co1 86.3(7) . . ? As11 W1 Co1 53.73(10) . . ? As12 W1 Co1 51.97(9) . . ? C24 W2 C23 86.6(11) . . ? C24 W2 C243 131.0(12) . . ? C23 W2 C243 85.3(12) . . ? C24 W2 C242 95.4(12) . . ? C23 W2 C242 88.1(12) . . ? C243 W2 C242 36.2(11) . . ? C24 W2 C244 139.6(12) . . ? C23 W2 C244 118.3(11) . . ? C243 W2 C244 36.0(11) . . ? C242 W2 C244 57.5(12) . . ? C24 W2 C241 85.3(13) . . ? C23 W2 C241 120.6(12) . . ? C243 W2 C241 58.7(13) . . ? C242 W2 C241 34.9(11) . . ? C244 W2 C241 55.1(13) . . ? C24 W2 C245 109.3(12) . . ? C23 W2 C245 142.2(12) . . ? C243 W2 C245 58.2(12) . . ? C242 W2 C245 57.3(12) . . ? C244 W2 C245 32.1(10) . . ? C241 W2 C245 33.5(11) . . ? C24 W2 As21 125.8(8) . . ? C23 W2 As21 88.4(8) . . ? C243 W2 As21 102.2(9) . . ? C242 W2 As21 138.4(8) . . ? C244 W2 As21 88.5(9) . . ? C241 W2 As21 140.3(9) . . ? C245 W2 As21 107.0(8) . . ? C24 W2 As22 74.2(9) . . ? C23 W2 As22 74.4(8) . . ? C243 W2 As22 147.1(9) . . ? C242 W2 As22 159.9(9) . . ? C244 W2 As22 140.0(9) . . ? C241 W2 As22 154.2(9) . . ? C245 W2 As22 142.1(9) . . ? As21 W2 As22 52.58(9) . . ? C24 W2 Co2 88.3(8) . . ? C23 W2 Co2 124.8(8) . . ? C243 W2 Co2 134.4(9) . . ? C242 W2 Co2 147.1(9) . . ? C244 W2 Co2 100.0(8) . . ? C241 W2 Co2 113.6(9) . . ? C245 W2 Co2 90.7(9) . . ? As21 W2 Co2 52.43(9) . . ? As22 W2 Co2 51.44(9) . . ? C12 Co1 C11 112.0(14) . . ? C12 Co1 P1 94.2(9) . . ? C11 Co1 P1 99.0(11) . . ? C12 Co1 As12 102.9(9) . . ? C11 Co1 As12 140.3(10) . . ? P1 Co1 As12 96.7(2) . . ? C12 Co1 As11 147.1(9) . . ? C11 Co1 As11 83.0(10) . . ? P1 Co1 As11 112.7(2) . . ? As12 Co1 As11 57.32(13) . . ? C12 Co1 W1 88.9(9) . . ? C11 Co1 W1 100.2(10) . . ? P1 Co1 W1 157.7(2) . . ? As12 Co1 W1 61.17(11) . . ? As11 Co1 W1 58.96(10) . . ? C21 Co2 C22 103.9(14) . . ? C21 Co2 P2 100.3(10) . . ? C22 Co2 P2 101.0(10) . . ? C21 Co2 As22 151.7(10) . . ? C22 Co2 As22 95.1(10) . . ? P2 Co2 As22 96.3(2) . . ? C21 Co2 As21 97.9(10) . . ? C22 Co2 As21 150.1(10) . . ? P2 Co2 As21 94.8(2) . . ? As22 Co2 As21 57.79(12) . . ? C21 Co2 W2 96.0(10) . . ? C22 Co2 W2 98.8(10) . . ? P2 Co2 W2 150.4(2) . . ? As22 Co2 W2 60.05(10) . . ? As21 Co2 W2 58.29(10) . . ? C131 P1 C121 103.3(11) . . ? C131 P1 C111 105.6(12) . . ? C121 P1 C111 99.0(11) . . ? C131 P1 Co1 114.5(9) . . ? C121 P1 Co1 112.2(8) . . ? C111 P1 Co1 119.9(9) . . ? C211 P2 C231 100.3(11) . . ? C211 P2 C221 107.3(11) . . ? C231 P2 C221 99.8(11) . . ? C211 P2 Co2 114.9(8) . . ? C231 P2 Co2 119.3(8) . . ? C221 P2 Co2 113.3(8) . . ? As12 As11 Co1 60.29(13) . . ? As12 As11 W1 65.31(11) . . ? Co1 As11 W1 67.30(11) . . ? As11 As12 Co1 62.39(13) . . ? As11 As12 W1 62.34(11) . . ? Co1 As12 W1 66.86(11) . . ? As22 As21 Co2 60.66(12) . . ? As22 As21 W2 65.07(10) . . ? Co2 As21 W2 69.28(10) . . ? As21 As22 Co2 61.55(12) . . ? As21 As22 W2 62.35(10) . . ? Co2 As22 W2 68.52(11) . . ? O11 C11 Co1 173(3) . . ? O12 C12 Co1 178(3) . . ? O13 C13 W1 177(2) . . ? O14 C14 W1 177(3) . . ? O21 C21 Co2 178(3) . . ? O22 C22 Co2 179(3) . . ? O23 C23 W2 175(2) . . ? O24 C24 W2 176(3) . . ? C116 C111 C112 120(3) . . ? C116 C111 P1 121(2) . . ? C112 C111 P1 118(2) . . ? C111 C112 C113 120(3) . . ? C112 C113 C114 117(4) . . ? C115 C114 C113 119(3) . . ? C114 C115 C116 120(3) . . ? C111 C116 C115 122(3) . . ? C122 C121 C126 116(2) . . ? C122 C121 P1 119.1(18) . . ? C126 C121 P1 124.9(19) . . ? C121 C122 C123 120(2) . . ? C124 C123 C122 122(3) . . ? C125 C124 C123 119(3) . . ? C124 C125 C126 120(3) . . ? C121 C126 C125 124(3) . . ? C132 C131 C136 120(3) . . ? C132 C131 P1 120(2) . . ? C136 C131 P1 120(2) . . ? C131 C132 C133 122(3) . . ? C134 C133 C132 117(3) . . ? C133 C134 C135 122(4) . . ? C134 C135 C136 121(4) . . ? C135 C136 C131 117(3) . . ? C145 C141 C142 111(3) . . ? C145 C141 W1 74.1(17) . . ? C142 C141 W1 71.9(15) . . ? C141 C142 C143 106(2) . . ? C141 C142 W1 72.8(15) . . ? C143 C142 W1 71.5(16) . . ? C144 C143 C142 106(2) . . ? C144 C143 W1 73.6(16) . . ? C142 C143 W1 72.2(16) . . ? C145 C144 C143 109(3) . . ? C145 C144 W1 72.6(16) . . ? C143 C144 W1 70.8(16) . . ? C141 C145 C144 108(3) . . ? C141 C145 W1 72.7(17) . . ? C144 C145 W1 72.7(16) . . ? C216 C211 C212 117(2) . . ? C216 C211 P2 121.5(19) . . ? C212 C211 P2 121.2(19) . . ? C213 C212 C211 119(3) . . ? C214 C213 C212 121(3) . . ? C215 C214 C213 122(3) . . ? C214 C215 C216 117(3) . . ? C211 C216 C215 123(3) . . ? C226 C221 C222 120(2) . . ? C226 C221 P2 117.9(19) . . ? C222 C221 P2 121.8(19) . . ? C221 C222 C223 117(2) . . ? C224 C223 C222 120(3) . . ? C223 C224 C225 121(3) . . ? C226 C225 C224 119(3) . . ? C221 C226 C225 122(3) . . ? C232 C231 C236 118(2) . . ? C232 C231 P2 120.1(19) . . ? C236 C231 P2 122.2(18) . . ? C233 C232 C231 121(2) . . ? C232 C233 C234 119(3) . . ? C235 C234 C233 121(3) . . ? C234 C235 C236 120(3) . . ? C235 C236 C231 122(2) . . ? C245 C241 C242 109(4) . . ? C245 C241 W2 74(2) . . ? C242 C241 W2 71(2) . . ? C241 C242 C243 107(3) . . ? C241 C242 W2 75(2) . . ? C243 C242 W2 71(2) . . ? C244 C243 C242 103(3) . . ? C244 C243 W2 74(2) . . ? C242 C243 W2 73(2) . . ? C245 C244 C243 113(3) . . ? C245 C244 W2 77(2) . . ? C243 C244 W2 70(2) . . ? C241 C245 C244 108(4) . . ? C241 C245 W2 72(2) . . ? C244 C245 W2 71(2) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 20.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.250 _refine_diff_density_min -1.054 _refine_diff_density_rms 0.252 data_ff104 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H5 As2 Co Cr2 Mo O15' _chemical_formula_weight 893.95 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' 'As' 'As' 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cr' 'Cr' 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 0.6857 '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 8.913(4) _cell_length_b 19.628(6) _cell_length_c 16.694(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.77(3) _cell_angle_gamma 90.00 _cell_volume 2878.4(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.063 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1712 _exptl_absorpt_coefficient_mu 4.075 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7707 _exptl_absorpt_correction_T_max 0.3527 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens p4' _diffrn_measurement_method theta/2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.2 _diffrn_reflns_number 4100 _diffrn_reflns_av_R_equivalents 0.1017 _diffrn_reflns_av_sigmaI/netI 0.2041 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 21.00 _reflns_number_total 3071 _reflns_number_gt 1486 _reflns_threshold_expression >2sigma(I) _computing_data_collection XSCANS _computing_cell_refinement XSCANS _computing_data_reduction XSCANS _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0542P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3071 _refine_ls_number_parameters 358 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1815 _refine_ls_R_factor_gt 0.0746 _refine_ls_wR_factor_ref 0.1560 _refine_ls_wR_factor_gt 0.1284 _refine_ls_goodness_of_fit_ref 0.921 _refine_ls_restrained_S_all 0.919 _refine_ls_shift/su_max 1.721 _refine_ls_shift/su_mean 0.206 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo -0.3201(2) 0.29780(9) 0.32565(12) 0.0465(6) Uani 1 1 d . . . As1 As -0.3728(2) 0.42572(11) 0.31245(14) 0.0441(7) Uani 1 1 d . . . As2 As -0.2433(3) 0.37945(11) 0.21621(13) 0.0431(7) Uani 1 1 d . . . Co1 Co -0.1023(3) 0.40707(14) 0.34461(18) 0.0466(9) Uani 1 1 d . . . Cr1 Cr -0.5380(4) 0.52739(16) 0.3035(2) 0.0439(10) Uani 1 1 d . . . Cr2 Cr -0.2376(4) 0.38208(18) 0.0689(2) 0.0503(11) Uani 1 1 d . . . C1 C 0.058(3) 0.3577(14) 0.3357(18) 0.092(10) Uani 1 1 d . . . C2 C -0.055(2) 0.4897(13) 0.3167(13) 0.059(7) Uani 1 1 d . . . C3 C -0.090(3) 0.4162(13) 0.4481(18) 0.083(9) Uani 1 1 d . . . C4 C -0.189(3) 0.2441(12) 0.2716(18) 0.080(9) Uani 1 1 d . . . C5 C -0.486(3) 0.2849(14) 0.2339(18) 0.109(11) Uani 1 1 d . . . C6 C -0.501(2) 0.2513(14) 0.3901(13) 0.106(10) Uani 1 1 d G . . C7 C -0.395(3) 0.1967(9) 0.3766(12) 0.126(11) Uani 1 1 d GU . . C8 C -0.246(2) 0.2124(10) 0.4251(13) 0.081(8) Uani 1 1 d G . . C9 C -0.259(3) 0.2767(11) 0.4686(10) 0.085(9) Uani 1 1 d GU . . C10 C -0.417(3) 0.3008(10) 0.4469(13) 0.088(9) Uani 1 1 d GU . . C11 C -0.664(3) 0.6016(12) 0.2979(14) 0.064(7) Uani 1 1 d . . . C12 C -0.622(3) 0.4960(13) 0.3935(14) 0.062(7) Uani 1 1 d . . . C13 C -0.381(3) 0.5755(13) 0.3720(15) 0.079(9) Uani 1 1 d . . . C14 C -0.453(3) 0.5559(11) 0.2134(15) 0.057(7) Uani 1 1 d . . . C15 C -0.694(3) 0.4818(12) 0.2311(15) 0.054(7) Uani 1 1 d . . . C21 C -0.235(2) 0.3863(11) -0.0387(14) 0.058(7) Uani 1 1 d . . . C22 C -0.442(3) 0.4174(12) 0.0572(13) 0.055(7) Uani 1 1 d . . . C23 C -0.158(3) 0.4738(13) 0.0763(16) 0.069(8) Uani 1 1 d . . . C24 C -0.039(3) 0.3439(12) 0.0885(15) 0.079(9) Uani 1 1 d . . . C25 C -0.314(3) 0.2954(12) 0.0532(12) 0.057(7) Uani 1 1 d . . . O1 O 0.164(2) 0.3227(10) 0.3362(14) 0.127(8) Uani 1 1 d . . . O2 O -0.027(2) 0.5416(8) 0.2917(11) 0.090(6) Uani 1 1 d . . . O3 O -0.083(2) 0.4234(9) 0.5230(11) 0.106(7) Uani 1 1 d . . . O4 O -0.108(2) 0.2158(9) 0.2318(12) 0.097(6) Uani 1 1 d . . . O5 O -0.599(7) 0.285(3) 0.192(4) 0.085(19) Uiso 0.61(15) 1 d P . . O5X O -0.564(7) 0.268(3) 0.160(5) 0.05(3) Uiso 0.39(15) 1 d P . . O11 O -0.738(2) 0.6498(8) 0.2974(12) 0.102(7) Uani 1 1 d . . . O12 O -0.670(2) 0.4734(11) 0.4468(10) 0.115(8) Uani 1 1 d . . . O13 O -0.293(2) 0.6064(10) 0.4134(12) 0.111(8) Uani 1 1 d . . . O14 O -0.4039(19) 0.5768(8) 0.1575(10) 0.076(5) Uani 1 1 d . . . O15 O -0.788(2) 0.4527(9) 0.1891(12) 0.096(7) Uani 1 1 d . . . O21 O -0.232(2) 0.3878(10) -0.1104(10) 0.100(7) Uani 1 1 d . . . O22 O -0.5656(19) 0.4360(9) 0.0422(11) 0.083(6) Uani 1 1 d . . . O23 O -0.108(2) 0.5273(9) 0.0802(12) 0.101(7) Uani 1 1 d . . . O24 O 0.069(4) 0.3116(18) 0.1056(18) 0.076(6) Uiso 0.63(4) 1 d P . . O24X O 0.112(7) 0.339(3) 0.088(3) 0.076(6) Uiso 0.37(4) 1 d P . . O25 O -0.358(4) 0.2417(15) 0.028(2) 0.076(6) Uiso 0.63(4) 1 d P . . O25X O -0.395(6) 0.239(3) 0.070(4) 0.076(6) Uiso 0.37(4) 1 d P . . 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 0.0465(13) 0.0400(11) 0.0539(15) 0.0154(11) 0.0112(11) 0.0057(11) As1 0.0377(15) 0.0406(14) 0.0540(18) 0.0073(12) 0.0076(13) 0.0064(13) As2 0.0467(15) 0.0406(13) 0.0401(15) 0.0011(12) 0.0021(13) -0.0019(13) Co1 0.043(2) 0.054(2) 0.042(2) -0.0033(16) 0.0026(17) 0.0016(17) Cr1 0.045(2) 0.045(2) 0.044(2) 0.0050(19) 0.013(2) 0.006(2) Cr2 0.059(3) 0.055(2) 0.035(2) -0.0047(19) 0.002(2) 0.013(2) C1 0.044(18) 0.08(2) 0.13(3) 0.025(19) -0.043(19) 0.022(17) C2 0.026(15) 0.11(2) 0.034(16) 0.002(15) -0.024(12) 0.003(16) C3 0.09(2) 0.075(19) 0.08(2) -0.028(19) 0.00(2) -0.043(17) C4 0.059(19) 0.07(2) 0.12(3) -0.030(17) 0.033(18) 0.019(15) C5 0.08(2) 0.12(2) 0.10(3) 0.07(2) -0.03(2) -0.02(2) C6 0.056(19) 0.14(2) 0.11(3) 0.09(2) -0.006(18) -0.04(2) C7 0.11(3) 0.060(18) 0.20(3) 0.102(19) 0.00(3) -0.02(2) C8 0.12(2) 0.044(17) 0.08(2) 0.043(15) 0.020(18) -0.007(17) C9 0.12(2) 0.085(19) 0.043(17) 0.057(15) 0.004(17) -0.005(18) C10 0.11(2) 0.072(19) 0.09(2) 0.071(17) 0.042(19) 0.04(2) C11 0.073(19) 0.063(18) 0.058(18) 0.009(14) 0.014(15) 0.024(15) C12 0.057(18) 0.11(2) 0.024(15) 0.023(15) 0.020(14) 0.019(16) C13 0.13(3) 0.067(19) 0.04(2) -0.013(15) 0.019(18) -0.006(19) C14 0.065(18) 0.054(16) 0.044(18) 0.010(14) -0.014(15) 0.004(14) C15 0.047(17) 0.065(17) 0.057(18) 0.001(14) 0.028(14) -0.002(14) C21 0.051(16) 0.079(17) 0.033(15) 0.008(15) -0.028(14) 0.009(14) C22 0.079(19) 0.059(16) 0.023(16) 0.015(12) 0.000(15) -0.011(17) C23 0.08(2) 0.059(18) 0.07(2) -0.001(17) 0.024(17) 0.003(17) C24 0.07(2) 0.070(18) 0.09(2) -0.011(15) -0.015(17) 0.041(17) C25 0.097(19) 0.063(15) 0.021(14) 0.005(13) 0.036(14) 0.006(16) O1 0.095(17) 0.129(19) 0.15(2) 0.006(15) 0.007(16) 0.053(15) O2 0.108(15) 0.067(12) 0.105(16) 0.041(11) 0.048(12) -0.026(11) O3 0.131(18) 0.114(15) 0.064(14) -0.024(13) -0.005(14) -0.009(14) O4 0.104(16) 0.076(14) 0.117(18) 0.015(12) 0.033(13) 0.028(12) O11 0.110(16) 0.041(11) 0.161(19) 0.004(12) 0.040(14) 0.027(11) O12 0.108(16) 0.20(2) 0.043(12) 0.027(13) 0.024(12) -0.023(15) O13 0.138(19) 0.096(16) 0.081(16) -0.015(12) -0.034(14) -0.020(14) O14 0.098(14) 0.079(12) 0.059(13) 0.011(10) 0.038(11) 0.013(11) O15 0.076(15) 0.099(15) 0.103(17) -0.017(12) -0.011(12) -0.020(12) O21 0.113(16) 0.151(18) 0.040(12) 0.005(13) 0.023(12) 0.036(14) O22 0.057(12) 0.105(15) 0.087(15) 0.008(11) 0.010(12) 0.004(12) O23 0.092(16) 0.084(14) 0.133(19) -0.005(14) 0.044(14) -0.021(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 Mo1 C4 1.91(3) . ? Mo1 C5 1.95(3) . ? Mo1 C6 2.278(18) . ? Mo1 C7 2.304(15) . ? Mo1 C10 2.334(17) . ? Mo1 C8 2.374(15) . ? Mo1 C9 2.392(17) . ? Mo1 As1 2.557(3) . ? Mo1 As2 2.608(3) . ? Mo1 Co1 2.874(4) . ? As1 As2 2.317(3) . ? As1 Co1 2.408(4) . ? As1 Cr1 2.469(4) . ? As2 Co1 2.357(4) . ? As2 Cr2 2.469(4) . ? Co1 C3 1.72(3) . ? Co1 C2 1.76(3) . ? Co1 C1 1.75(3) . ? Cr1 C11 1.83(2) . ? Cr1 C13 1.90(3) . ? Cr1 C12 1.89(2) . ? Cr1 C15 1.90(3) . ? Cr1 C14 1.88(3) . ? Cr2 C25 1.83(2) . ? Cr2 C21 1.80(2) . ? Cr2 C24 1.90(2) . ? Cr2 C22 1.93(3) . ? Cr2 C23 1.93(3) . ? C1 O1 1.16(3) . ? C2 O2 1.14(2) . ? C3 O3 1.25(3) . ? C4 O4 1.20(2) . ? C5 O5 1.13(4) . ? C5 O5X 1.35(7) . ? C6 C7 1.471(11) . ? C6 C10 1.471(11) . ? C7 C8 1.471(11) . ? C8 C9 1.471(11) . ? C9 C10 1.471(11) . ? C11 O11 1.15(2) . ? C12 O12 1.14(2) . ? C13 O13 1.13(2) . ? C14 O14 1.17(2) . ? C15 O15 1.15(2) . ? C21 O21 1.20(2) . ? C22 O22 1.15(2) . ? C23 O23 1.14(2) . ? C24 O24 1.15(3) . ? C24 O24X 1.35(6) . ? C25 O25 1.18(3) . ? C25 O25X 1.38(6) . ? 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 C4 Mo1 C5 89.9(13) . . ? C4 Mo1 C6 122.8(11) . . ? C5 Mo1 C6 79.4(10) . . ? C4 Mo1 C7 86.5(10) . . ? C5 Mo1 C7 87.1(9) . . ? C6 Mo1 C7 37.4(3) . . ? C4 Mo1 C10 140.4(10) . . ? C5 Mo1 C10 110.0(12) . . ? C6 Mo1 C10 37.2(3) . . ? C7 Mo1 C10 61.8(5) . . ? C4 Mo1 C8 79.7(10) . . ? C5 Mo1 C8 122.7(10) . . ? C6 Mo1 C8 61.5(5) . . ? C7 Mo1 C8 36.6(3) . . ? C10 Mo1 C8 60.7(4) . . ? C4 Mo1 C9 108.8(11) . . ? C5 Mo1 C9 140.6(9) . . ? C6 Mo1 C9 61.2(4) . . ? C7 Mo1 C9 60.9(5) . . ? C10 Mo1 C9 36.3(3) . . ? C8 Mo1 C9 36.0(3) . . ? C4 Mo1 As1 128.3(8) . . ? C5 Mo1 As1 87.5(8) . . ? C6 Mo1 As1 107.4(7) . . ? C7 Mo1 As1 144.8(7) . . ? C10 Mo1 As1 87.7(4) . . ? C8 Mo1 As1 141.2(6) . . ? C9 Mo1 As1 105.2(6) . . ? C4 Mo1 As2 75.7(8) . . ? C5 Mo1 As2 77.5(8) . . ? C6 Mo1 As2 150.3(5) . . ? C7 Mo1 As2 156.3(5) . . ? C10 Mo1 As2 140.6(5) . . ? C8 Mo1 As2 148.1(5) . . ? C9 Mo1 As2 139.7(4) . . ? As1 Mo1 As2 53.30(8) . . ? C4 Mo1 Co1 90.4(8) . . ? C5 Mo1 Co1 126.1(7) . . ? C6 Mo1 Co1 140.1(8) . . ? C7 Mo1 Co1 146.7(6) . . ? C10 Mo1 Co1 103.2(7) . . ? C8 Mo1 Co1 110.3(6) . . ? C9 Mo1 Co1 89.1(4) . . ? As1 Mo1 Co1 52.24(9) . . ? As2 Mo1 Co1 50.64(8) . . ? As2 As1 Co1 59.80(11) . . ? As2 As1 Cr1 129.57(14) . . ? Co1 As1 Cr1 134.46(14) . . ? As2 As1 Mo1 64.47(9) . . ? Co1 As1 Mo1 70.68(10) . . ? Cr1 As1 Mo1 153.87(13) . . ? As1 As2 Co1 62.03(11) . . ? As1 As2 Cr2 141.21(14) . . ? Co1 As2 Cr2 143.43(16) . . ? As1 As2 Mo1 62.23(9) . . ? Co1 As2 Mo1 70.56(10) . . ? Cr2 As2 Mo1 139.72(14) . . ? C3 Co1 C2 101.1(11) . . ? C3 Co1 C1 103.2(13) . . ? C2 Co1 C1 104.5(12) . . ? C3 Co1 As2 150.5(9) . . ? C2 Co1 As2 95.0(7) . . ? C1 Co1 As2 96.5(9) . . ? C3 Co1 As1 95.7(9) . . ? C2 Co1 As1 94.5(7) . . ? C1 Co1 As1 149.9(9) . . ? As2 Co1 As1 58.17(11) . . ? C3 Co1 Mo1 96.6(8) . . ? C2 Co1 Mo1 148.0(7) . . ? C1 Co1 Mo1 97.1(9) . . ? As2 Co1 Mo1 58.80(9) . . ? As1 Co1 Mo1 57.08(9) . . ? C11 Cr1 C13 91.0(11) . . ? C11 Cr1 C12 88.7(10) . . ? C13 Cr1 C12 91.9(11) . . ? C11 Cr1 C15 88.0(10) . . ? C13 Cr1 C15 177.5(11) . . ? C12 Cr1 C15 90.3(10) . . ? C11 Cr1 C14 92.9(10) . . ? C13 Cr1 C14 88.8(11) . . ? C12 Cr1 C14 178.2(10) . . ? C15 Cr1 C14 89.0(9) . . ? C11 Cr1 As1 178.6(8) . . ? C13 Cr1 As1 89.8(8) . . ? C12 Cr1 As1 90.1(7) . . ? C15 Cr1 As1 91.3(7) . . ? C14 Cr1 As1 88.3(7) . . ? C25 Cr2 C21 88.2(10) . . ? C25 Cr2 C24 88.4(10) . . ? C21 Cr2 C24 91.1(10) . . ? C25 Cr2 C22 89.8(10) . . ? C21 Cr2 C22 93.2(10) . . ? C24 Cr2 C22 175.3(11) . . ? C25 Cr2 C23 175.5(10) . . ? C21 Cr2 C23 87.3(11) . . ? C24 Cr2 C23 92.1(11) . . ? C22 Cr2 C23 90.0(10) . . ? C25 Cr2 As2 93.1(6) . . ? C21 Cr2 As2 178.5(7) . . ? C24 Cr2 As2 89.8(8) . . ? C22 Cr2 As2 86.0(7) . . ? C23 Cr2 As2 91.4(8) . . ? O1 C1 Co1 174(3) . . ? O2 C2 Co1 174(2) . . ? O3 C3 Co1 179(3) . . ? O4 C4 Mo1 173(3) . . ? O5 C5 O5X 33(3) . . ? O5 C5 Mo1 165(5) . . ? O5X C5 Mo1 162(4) . . ? C7 C6 C10 108.0 . . ? C7 C6 Mo1 72.2(6) . . ? C10 C6 Mo1 73.5(6) . . ? C8 C7 C6 108.0 . . ? C8 C7 Mo1 74.3(6) . . ? C6 C7 Mo1 70.3(6) . . ? C7 C8 C9 108.0 . . ? C7 C8 Mo1 69.1(6) . . ? C9 C8 Mo1 72.7(6) . . ? C10 C9 C8 108.0 . . ? C10 C9 Mo1 69.7(6) . . ? C8 C9 Mo1 71.3(6) . . ? C9 C10 C6 108.0 . . ? C9 C10 Mo1 74.0(6) . . ? C6 C10 Mo1 69.4(6) . . ? O11 C11 Cr1 177(2) . . ? O12 C12 Cr1 176(2) . . ? O13 C13 Cr1 177(3) . . ? O14 C14 Cr1 176(2) . . ? O15 C15 Cr1 178(2) . . ? O21 C21 Cr2 179(2) . . ? O22 C22 Cr2 173(2) . . ? O23 C23 Cr2 178(3) . . ? O24 C24 O24X 33(2) . . ? O24 C24 Cr2 168(3) . . ? O24X C24 Cr2 158(4) . . ? O25 C25 O25X 36(2) . . ? O25 C25 Cr2 167(3) . . ? O25X C25 Cr2 156(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 21.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.833 _refine_diff_density_min -0.658 _refine_diff_density_rms 0.158 data_my112 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H15 As Mo O6 W2' _chemical_formula_weight 901.89 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' '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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.042(2) _cell_length_b 7.5130(15) _cell_length_c 20.877(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.762(9) _cell_angle_gamma 90.00 _cell_volume 2201.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour black _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.721 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1648 _exptl_absorpt_coefficient_mu 12.512 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2223 _exptl_absorpt_correction_T_max 0.6866 _exptl_absorpt_process_details ? _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_type 'Siemens P4' _diffrn_measurement_method theta/2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.1 _diffrn_reflns_number 5104 _diffrn_reflns_av_R_equivalents 0.0363 _diffrn_reflns_av_sigmaI/netI 0.0652 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3875 _reflns_number_gt 2783 _reflns_threshold_expression >2sigma(I) _computing_data_collection XSCANS _computing_cell_refinement XSCANS _computing_data_reduction XSCANS _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0878P)^2^+76.5706P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3875 _refine_ls_number_parameters 124 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0949 _refine_ls_R_factor_gt 0.0625 _refine_ls_wR_factor_ref 0.1803 _refine_ls_wR_factor_gt 0.1595 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.646 _refine_ls_shift/su_mean 0.025 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1X W 0.17540(6) 0.20598(12) 0.18327(4) 0.0227(3) Uani 0.685(4) 1 d P A 1 Mo1Y Mo 0.17540(6) 0.20598(12) 0.18327(4) 0.0227(3) Uani 0.32 1 d P A 2 W2 W 0.38905(6) 0.25017(11) 0.15002(4) 0.0258(3) Uani 1 1 d . . . Mo1X Mo 0.23689(10) 0.20341(19) 0.04076(6) 0.0314(4) Uani 0.685(4) 1 d P A 2 W1Y W 0.23689(10) 0.20341(19) 0.04076(6) 0.0314(4) Uani 0.32 1 d P A 1 As As 0.25373(12) 0.4572(2) 0.12119(8) 0.0153(4) Uani 1 1 d . A . C1 C 0.0649(14) 0.314(3) 0.1351(9) 0.029(4) Uiso 1 1 d . . . O3 O 0.3882(9) -0.1587(18) 0.1798(6) 0.028(3) Uiso 1 1 d . . . C2 C 0.1771(12) 0.422(2) 0.2363(8) 0.018(4) Uiso 1 1 d . . . O2 O 0.1728(10) 0.5358(19) 0.2741(6) 0.032(3) Uiso 1 1 d . A . C3 C 0.3826(12) -0.011(2) 0.1682(8) 0.016(4) Uiso 1 1 d . A . O1 O -0.0015(13) 0.370(2) 0.1099(8) 0.053(4) Uiso 1 1 d . A . C4 C 0.3719(12) 0.300(2) 0.2432(8) 0.016(4) Uiso 1 1 d . A . O4 O 0.3718(9) 0.3268(18) 0.2963(6) 0.027(3) Uiso 1 1 d . . . O5 O 0.3921(10) -0.087(2) 0.0313(7) 0.038(4) Uiso 1 1 d . A . C5 C 0.3389(13) 0.025(2) 0.0417(9) 0.023(4) Uiso 1 1 d . . . O6 O 0.1074(11) -0.130(2) 0.0554(7) 0.043(4) Uiso 1 1 d . A . C6 C 0.1558(14) -0.006(3) 0.0583(9) 0.028(4) Uiso 1 1 d . . . C01 C 0.1626(11) 0.434(2) -0.0229(8) 0.041(5) Uiso 1 1 d G . . C02 C 0.2589(12) 0.439(2) -0.0352(9) 0.044(6) Uiso 1 1 d G A . C03 C 0.2834(11) 0.277(2) -0.0616(9) 0.056(7) Uiso 1 1 d G A . C04 C 0.2022(12) 0.172(2) -0.0657(9) 0.044(6) Uiso 1 1 d G A . C05 C 0.1276(11) 0.270(2) -0.0418(8) 0.042(6) Uiso 1 1 d G A . C10 C 0.0705(9) -0.0300(19) 0.1938(6) 0.026(4) Uiso 1 1 d G . . C11 C 0.1635(9) -0.1040(18) 0.1975(6) 0.022(4) Uiso 1 1 d G A . C12 C 0.2105(9) -0.0365(19) 0.2535(6) 0.024(4) Uiso 1 1 d G A . C13 C 0.1466(9) 0.0791(19) 0.2845(6) 0.030(5) Uiso 1 1 d G A . C14 C 0.0601(9) 0.0831(19) 0.2476(6) 0.027(4) Uiso 1 1 d G A . C20 C 0.4945(10) 0.3263(17) 0.0675(6) 0.029(4) Uiso 1 1 d G A . C21 C 0.5378(10) 0.1947(16) 0.1075(6) 0.024(4) Uiso 1 1 d G A . C22 C 0.5510(10) 0.2683(17) 0.1697(6) 0.024(4) Uiso 1 1 d G A . C23 C 0.5159(10) 0.4454(17) 0.1682(6) 0.029(5) Uiso 1 1 d G A . C24 C 0.4810(10) 0.4813(17) 0.1050(6) 0.021(4) Uiso 1 1 d G A . 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 W1X 0.0214(5) 0.0217(5) 0.0251(5) 0.0003(4) 0.0020(4) 0.0021(4) Mo1Y 0.0214(5) 0.0217(5) 0.0251(5) 0.0003(4) 0.0020(4) 0.0021(4) W2 0.0258(4) 0.0257(4) 0.0261(4) -0.0009(3) 0.0015(3) -0.0003(3) Mo1X 0.0327(7) 0.0382(8) 0.0230(6) 0.0001(6) -0.0037(5) 0.0020(6) W1Y 0.0327(7) 0.0382(8) 0.0230(6) 0.0001(6) -0.0037(5) 0.0020(6) As 0.0188(9) 0.0088(8) 0.0186(9) 0.0037(7) 0.0023(7) 0.0029(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 W1X C2 1.964(17) . ? W1X C1 2.00(2) . ? W1X C10 2.320(14) . ? W1X C14 2.326(14) . ? W1X C11 2.354(14) . ? W1X C13 2.364(14) . ? W1X C12 2.381(14) . ? W1X As 2.5574(19) . ? W1X W2 3.1180(13) . ? W1X W1Y 3.1236(16) . ? Mo1Y C2 1.964(17) . ? Mo1Y C1 2.00(2) . ? Mo1Y C10 2.320(14) . ? Mo1Y C14 2.326(14) . ? Mo1Y C11 2.354(14) . ? Mo1Y C13 2.364(14) . ? Mo1Y C12 2.381(14) . ? Mo1Y As 2.5574(19) . ? Mo1Y W2 3.1180(13) . ? Mo1Y Mo1X 3.1236(16) . ? W2 C3 1.999(17) . ? W2 C4 2.003(16) . ? W2 C22 2.302(14) . ? W2 C23 2.329(14) . ? W2 C21 2.332(14) . ? W2 C24 2.375(14) . ? W2 C20 2.376(14) . ? W2 As 2.5145(19) . ? W2 W1Y 3.0973(16) . ? W2 Mo1X 3.0973(16) . ? Mo1X C5 1.959(19) . ? Mo1X C6 1.98(2) . ? Mo1X C04 2.273(18) . ? Mo1X C03 2.320(19) . ? Mo1X C05 2.326(17) . ? Mo1X C02 2.401(18) . ? Mo1X C01 2.405(17) . ? Mo1X As 2.547(2) . ? W1Y C5 1.959(19) . ? W1Y C6 1.98(2) . ? W1Y C04 2.273(18) . ? W1Y C03 2.320(19) . ? W1Y C05 2.326(17) . ? W1Y C02 2.401(18) . ? W1Y C01 2.405(17) . ? W1Y As 2.547(2) . ? C1 O1 1.14(2) . ? O3 C3 1.14(2) . ? C2 O2 1.17(2) . ? C4 O4 1.13(2) . ? O5 C5 1.15(2) . ? O6 C6 1.16(2) . ? C01 C05 1.384(12) . ? C01 C02 1.384(12) . ? C02 C03 1.384(12) . ? C03 C04 1.384(12) . ? C04 C05 1.384(12) . ? C10 C11 1.419(10) . ? C10 C14 1.419(10) . ? C11 C12 1.419(10) . ? C12 C13 1.419(10) . ? C13 C14 1.419(10) . ? C20 C21 1.419(10) . ? C20 C24 1.419(10) . ? C21 C22 1.419(10) . ? C22 C23 1.419(10) . ? C23 C24 1.419(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 W1X C1 86.7(8) . . ? C2 W1X C10 125.1(6) . . ? C1 W1X C10 82.7(7) . . ? C2 W1X C14 90.0(6) . . ? C1 W1X C14 84.8(7) . . ? C10 W1X C14 35.6(3) . . ? C2 W1X C11 138.2(6) . . ? C1 W1X C11 114.2(7) . . ? C10 W1X C11 35.3(3) . . ? C14 W1X C11 58.8(4) . . ? C2 W1X C13 80.2(6) . . ? C1 W1X C13 117.6(6) . . ? C10 W1X C13 58.7(4) . . ? C14 W1X C13 35.2(3) . . ? C11 W1X C13 58.2(4) . . ? C2 W1X C12 106.7(6) . . ? C1 W1X C12 140.0(7) . . ? C10 W1X C12 58.5(4) . . ? C14 W1X C12 58.4(4) . . ? C11 W1X C12 34.9(2) . . ? C13 W1X C12 34.8(3) . . ? C2 W1X As 71.2(5) . . ? C1 W1X As 77.5(6) . . ? C10 W1X As 153.7(3) . . ? C14 W1X As 154.6(3) . . ? C11 W1X As 145.8(3) . . ? C13 W1X As 147.0(3) . . ? C12 W1X As 142.4(3) . . ? C2 W1X W2 92.4(5) . . ? C1 W1X W2 125.6(6) . . ? C10 W1X W2 136.1(3) . . ? C14 W1X W2 149.6(3) . . ? C11 W1X W2 101.9(3) . . ? C13 W1X W2 115.7(3) . . ? C12 W1X W2 92.1(3) . . ? As W1X W2 51.45(4) . . ? C2 W1X W1Y 122.9(5) . . ? C1 W1X W1Y 75.9(6) . . ? C10 W1X W1Y 106.3(3) . . ? C14 W1X W1Y 139.9(3) . . ? C11 W1X W1Y 97.9(3) . . ? C13 W1X W1Y 155.3(3) . . ? C12 W1X W1Y 121.6(3) . . ? As W1X W1Y 52.12(5) . . ? W2 W1X W1Y 59.50(3) . . ? C2 Mo1Y C1 86.7(8) . . ? C2 Mo1Y C10 125.1(6) . . ? C1 Mo1Y C10 82.7(7) . . ? C2 Mo1Y C14 90.0(6) . . ? C1 Mo1Y C14 84.8(7) . . ? C10 Mo1Y C14 35.6(3) . . ? C2 Mo1Y C11 138.2(6) . . ? C1 Mo1Y C11 114.2(7) . . ? C10 Mo1Y C11 35.3(3) . . ? C14 Mo1Y C11 58.8(4) . . ? C2 Mo1Y C13 80.2(6) . . ? C1 Mo1Y C13 117.6(6) . . ? C10 Mo1Y C13 58.7(4) . . ? C14 Mo1Y C13 35.2(3) . . ? C11 Mo1Y C13 58.2(4) . . ? C2 Mo1Y C12 106.7(6) . . ? C1 Mo1Y C12 140.0(7) . . ? C10 Mo1Y C12 58.5(4) . . ? C14 Mo1Y C12 58.4(4) . . ? C11 Mo1Y C12 34.9(2) . . ? C13 Mo1Y C12 34.8(3) . . ? C2 Mo1Y As 71.2(5) . . ? C1 Mo1Y As 77.5(6) . . ? C10 Mo1Y As 153.7(3) . . ? C14 Mo1Y As 154.6(3) . . ? C11 Mo1Y As 145.8(3) . . ? C13 Mo1Y As 147.0(3) . . ? C12 Mo1Y As 142.4(3) . . ? C2 Mo1Y W2 92.4(5) . . ? C1 Mo1Y W2 125.6(6) . . ? C10 Mo1Y W2 136.1(3) . . ? C14 Mo1Y W2 149.6(3) . . ? C11 Mo1Y W2 101.9(3) . . ? C13 Mo1Y W2 115.7(3) . . ? C12 Mo1Y W2 92.1(3) . . ? As Mo1Y W2 51.45(4) . . ? C2 Mo1Y Mo1X 122.9(5) . . ? C1 Mo1Y Mo1X 75.9(6) . . ? C10 Mo1Y Mo1X 106.3(3) . . ? C14 Mo1Y Mo1X 139.9(3) . . ? C11 Mo1Y Mo1X 97.9(3) . . ? C13 Mo1Y Mo1X 155.3(3) . . ? C12 Mo1Y Mo1X 121.6(3) . . ? As Mo1Y Mo1X 52.12(5) . . ? W2 Mo1Y Mo1X 59.50(3) . . ? C3 W2 C4 89.6(7) . . ? C3 W2 C22 94.3(6) . . ? C4 W2 C22 87.9(6) . . ? C3 W2 C23 128.7(6) . . ? C4 W2 C23 80.7(6) . . ? C22 W2 C23 35.7(3) . . ? C3 W2 C21 86.8(6) . . ? C4 W2 C21 122.6(6) . . ? C22 W2 C21 35.7(3) . . ? C23 W2 C21 59.0(4) . . ? C3 W2 C24 145.1(6) . . ? C4 W2 C24 109.3(6) . . ? C22 W2 C24 58.8(4) . . ? C23 W2 C24 35.1(2) . . ? C21 W2 C24 58.4(4) . . ? C3 W2 C20 114.0(6) . . ? C4 W2 C20 139.1(6) . . ? C22 W2 C20 58.8(4) . . ? C23 W2 C20 58.4(4) . . ? C21 W2 C20 35.1(3) . . ? C24 W2 C20 34.8(2) . . ? C3 W2 As 127.8(5) . . ? C4 W2 As 90.2(5) . . ? C22 W2 As 137.8(3) . . ? C23 W2 As 102.6(3) . . ? C21 W2 As 134.3(3) . . ? C24 W2 As 82.5(3) . . ? C20 W2 As 99.2(3) . . ? C3 W2 W1Y 89.7(5) . . ? C4 W2 W1Y 129.5(5) . . ? C22 W2 W1Y 142.5(3) . . ? C23 W2 W1Y 134.3(3) . . ? C21 W2 W1Y 107.7(3) . . ? C24 W2 W1Y 99.3(3) . . ? C20 W2 W1Y 85.6(3) . . ? As W2 W1Y 52.75(5) . . ? C3 W2 Mo1X 89.7(5) . . ? C4 W2 Mo1X 129.5(5) . . ? C22 W2 Mo1X 142.5(3) . . ? C23 W2 Mo1X 134.3(3) . . ? C21 W2 Mo1X 107.7(3) . . ? C24 W2 Mo1X 99.3(3) . . ? C20 W2 Mo1X 85.6(3) . . ? As W2 Mo1X 52.75(5) . . ? W1Y W2 Mo1X 0.00(7) . . ? C3 W2 W1X 78.7(5) . . ? C4 W2 W1X 70.0(5) . . ? C22 W2 W1X 156.7(3) . . ? C23 W2 W1X 140.1(3) . . ? C21 W2 W1X 160.9(3) . . ? C24 W2 W1X 134.8(3) . . ? C20 W2 W1X 144.3(3) . . ? As W2 W1X 52.69(5) . . ? W1Y W2 W1X 60.34(3) . . ? Mo1X W2 W1X 60.34(3) . . ? C3 W2 Mo1Y 78.7(5) . . ? C4 W2 Mo1Y 70.0(5) . . ? C22 W2 Mo1Y 156.7(3) . . ? C23 W2 Mo1Y 140.1(3) . . ? C21 W2 Mo1Y 160.9(3) . . ? C24 W2 Mo1Y 134.8(3) . . ? C20 W2 Mo1Y 144.3(3) . . ? As W2 Mo1Y 52.69(5) . . ? W1Y W2 Mo1Y 60.34(3) . . ? Mo1X W2 Mo1Y 60.34(3) . . ? W1X W2 Mo1Y 0.00(5) . . ? C5 Mo1X C6 83.2(8) . . ? C5 Mo1X C04 94.3(7) . . ? C6 Mo1X C04 89.6(7) . . ? C5 Mo1X C03 86.9(7) . . ? C6 Mo1X C03 122.6(7) . . ? C04 Mo1X C03 35.1(3) . . ? C5 Mo1X C05 128.3(7) . . ? C6 Mo1X C05 86.4(7) . . ? C04 Mo1X C05 35.0(3) . . ? C03 Mo1X C05 57.6(5) . . ? C5 Mo1X C02 113.6(7) . . ? C6 Mo1X C02 142.4(7) . . ? C04 Mo1X C02 57.2(5) . . ? C03 Mo1X C02 34.0(3) . . ? C05 Mo1X C02 56.5(5) . . ? C5 Mo1X C01 143.4(6) . . ? C6 Mo1X C01 115.7(7) . . ? C04 Mo1X C01 57.1(5) . . ? C03 Mo1X C01 56.6(5) . . ? C05 Mo1X C01 34.0(3) . . ? C02 Mo1X C01 33.5(3) . . ? C5 Mo1X As 116.8(5) .. . ? C6 Mo1X As 120.9(6) . . ? C04 Mo1X As 137.3(4) . . ? C03 Mo1X As 114.0(4) . . ? C05 Mo1X As 112.0(4) . . ? C02 Mo1X As 82.7(4) . . ? C01 Mo1X As 81.6(4) . . ? C5 Mo1X W2 65.3(5) . . ? C6 Mo1X W2 109.9(6) . . ? C04 Mo1X W2 148.7(4) . . ? C03 Mo1X W2 116.4(4) . . ? C05 Mo1X W2 161.1(4) . . ? C02 Mo1X W2 107.6(4) . . ? C01 Mo1X W2 127.1(4) . . ? As Mo1X W2 51.80(5) . . ? C5 Mo1X Mo1Y 102.6(5) . . ? C6 Mo1X Mo1Y 69.6(6) . . ? C04 Mo1X Mo1Y 151.0(4) . . ? C03 Mo1X Mo1Y 165.9(4) . . ? C05 Mo1X Mo1Y 120.6(4) . . ? C02 Mo1X Mo1Y 132.0(4) . . ? C01 Mo1X Mo1Y 113.2(4) . . ? As Mo1X Mo1Y 52.42(5) . . ? W2 Mo1X Mo1Y 60.16(3) . . ? C5 W1Y C6 83.2(8) . . ? C5 W1Y C04 94.3(7) . . ? C6 W1Y C04 89.6(7) . . ? C5 W1Y C03 86.9(7) . . ? C6 W1Y C03 122.6(7) . . ? C04 W1Y C03 35.1(3) . . ? C5 W1Y C05 128.3(7) . . ? C6 W1Y C05 86.4(7) . . ? C04 W1Y C05 35.0(3) . . ? C03 W1Y C05 57.6(5) . . ? C5 W1Y C02 113.6(7) . . ? C6 W1Y C02 142.4(7) . . ? C04 W1Y C02 57.2(5) . . ? C03 W1Y C02 34.0(3) . . ? C05 W1Y C02 56.5(5) . . ? C5 W1Y C01 143.4(6) . . ? C6 W1Y C01 115.7(7) . . ? C04 W1Y C01 57.1(5) . . ? C03 W1Y C01 56.6(5) . . ? C05 W1Y C01 34.0(3) . . ? C02 W1Y C01 33.5(3) . . ? C5 W1Y As 116.8(5) . . ? C6 W1Y As 120.9(6) . . ? C04 W1Y As 137.3(4) . . ? C03 W1Y As 114.0(4) . . ? C05 W1Y As 112.0(4) . . ? C02 W1Y As 82.7(4) . . ? C01 W1Y As 81.6(4) . . ? C5 W1Y W2 65.3(5) . . ? C6 W1Y W2 109.9(6) . . ? C04 W1Y W2 148.7(4) . . ? C03 W1Y W2 116.4(4) . . ? C05 W1Y W2 161.1(4) . . ? C02 W1Y W2 107.6(4) . . ? C01 W1Y W2 127.1(4) . . ? As W1Y W2 51.80(5) . . ? C5 W1Y W1X 102.6(5) . . ? C6 W1Y W1X 69.6(6) . . ? C04 W1Y W1X 151.0(4) . . ? C03 W1Y W1X 165.9(4) . . ? C05 W1Y W1X 120.6(4) . . ? C02 W1Y W1X 132.0(4) . . ? C01 W1Y W1X 113.2(4) . . ? As W1Y W1X 52.42(5) . . ? W2 W1Y W1X 60.16(3) . . ? W2 As W1Y 75.45(6) . . ? W2 As Mo1X 75.45(6) . . ? W1Y As Mo1X 0.00(9) . . ? W2 As Mo1Y 75.86(5) . . ? W1Y As Mo1Y 75.46(6) . . ? Mo1X As Mo1Y 75.46(6) . . ? W2 As W1X 75.86(5) . . ? W1Y As W1X 75.46(6) . . ? Mo1X As W1X 75.46(6) . . ? Mo1Y As W1X 0.00(6) . . ? O1 C1 W1X 175.9(19) . . ? O1 C1 Mo1Y 175.9(19) . . ? W1X C1 Mo1Y 0.00(7) . . ? O2 C2 W1X 170.7(15) . . ? O2 C2 Mo1Y 170.7(15) . . ? W1X C2 Mo1Y 0.00(5) . . ? O3 C3 W2 173.3(15) . . ? O4 C4 W2 173.2(15) . . ? O5 C5 Mo1X 167.5(16) . . ? O5 C5 W1Y 167.5(16) . . ? Mo1X C5 W1Y 0.00(9) . . ? O6 C6 Mo1X 166.3(17) . . ? O6 C6 W1Y 166.3(17) . . ? Mo1X C6 W1Y 0.00(11) . . ? C05 C01 C02 108.0 . . ? C05 C01 Mo1X 69.9(7) . . ? C02 C01 Mo1X 73.1(7) . . ? C05 C01 W1Y 69.9(7) . . ? C02 C01 W1Y 73.1(7) . . ? Mo1X C01 W1Y 0.00(7) . . ? C01 C02 C03 108.0 . . ? C01 C02 W1Y 73.4(7) . . ? C03 C02 W1Y 69.8(7) . . ? C01 C02 Mo1X 73.4(7) . . ? C03 C02 Mo1X 69.8(7) . . ? W1Y C02 Mo1X 0.00(9) . . ? C04 C03 C02 108.0 . . ? C04 C03 Mo1X 70.6(7) . . ? C02 C03 Mo1X 76.2(7) . . ? C04 C03 W1Y 70.6(7) . . ? C02 C03 W1Y 76..2(7) . . ? Mo1X C03 W1Y 0.00(10) . . ? C05 C04 C03 108.0 . . ? C05 C04 Mo1X 74.6(7) . . ? C03 C04 Mo1X 74.4(7) . . ? C05 C04 W1Y 74.6(7) . . ? C03 C04 W1Y 74.4(7) . . ? Mo1X C04 W1Y 0.000(15) . . ? C04 C05 C01 108.0 . . ? C04 C05 Mo1X 70.4(7) . . ? C01 C05 Mo1X 76.1(7) . . ? C04 C05 W1Y 70.4(7) . . ? C01 C05 W1Y 76.1(7) . . ? Mo1X C05 W1Y 0.00(9) . . ? C11 C10 C14 108.0 . . ? C11 C10 Mo1Y 73.6(5) . . ? C14 C10 Mo1Y 72.5(5) . . ? C11 C10 W1X 73.6(5) . . ? C14 C10 W1X 72.5(5) . . ? Mo1Y C10 W1X 0.00(6) . . ? C12 C11 C10 108.0 . . ? C12 C11 W1X 73.6(5) . . ? C10 C11 W1X 71.0(5) . . ? C12 C11 Mo1Y 73.6(5) . . ? C10 C11 Mo1Y 71.0(5) . . ? W1X C11 Mo1Y 0.00(4) . . ? C11 C12 C13 108.0 . . ? C11 C12 Mo1Y 71.5(5) . . ? C13 C12 Mo1Y 71.9(5) . . ? C11 C12 W1X 71.5(5) . . ? C13 C12 W1X 71.9(5) . . ? Mo1Y C12 W1X 0.00(6) . . ? C14 C13 C12 108.0 . . ? C14 C13 W1X 70.9(5) . . ? C12 C13 W1X 73.3(5) . . ? C14 C13 Mo1Y 70.9(5) . . ? C12 C13 Mo1Y 73.3(5) . . ? W1X C13 Mo1Y 0.00(2) . . ? C13 C14 C10 108.0 . . ? C13 C14 W1X 73.9(5) . . ? C10 C14 W1X 72.0(5) . . ? C13 C14 Mo1Y 73.9(5) . . ? C10 C14 Mo1Y 72.0(5) . . ? W1X C14 Mo1Y 0.00(5) . . ? C21 C20 C24 108.0 . . ? C21 C20 W2 70.8(5) . . ? C24 C20 W2 72.6(5) . . ? C20 C21 C22 108.0 . . ? C20 C21 W2 74.2(5) . . ? C22 C21 W2 71.0(5) . . ? C23 C22 C21 108.0 . . ? C23 C22 W2 73.2(5) . . ? C21 C22 W2 73.3(5) . . ? C22 C23 C24 108.0 . . ? C22 C23 W2 71.1(5) . . ? C24 C23 W2 74.2(5) . . ? C20 C24 C23 108.0 . . ? C20 C24 W2 72.7(5) . . ? C23 C24 W2 70.7(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 3.227 _refine_diff_density_min -2.832 _refine_diff_density_rms 0.404