Electronic Supplementary Information for Dalton Transactions This journal is © The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Darren Johnson' _publ_contact_author_address ; Department of Chemistry University of Oregon Eugene OR 97403-1253 UNITED STATES OF AMERICA ; _publ_contact_author_email DWJ@UOREGON.EDU _publ_section_title ; Host-guest interactions in a series of self-assembled As2L2Cl2 macrocycles ; loop_ _publ_author_name 'Darren Johnson' 'Virginia M. Cangelosi' 'Sean A. Fontenot' 'Melanie Pitt' 'Lev N. Zakharov' data_sean5 _database_code_depnum_ccdc_archive 'CCDC 676181' _audit_creation_method SHELXLTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H34 As2 Cl2 S4' _chemical_formula_weight 839.63 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' _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 15.404(7) _cell_length_b 6.395(3) _cell_length_c 19.576(8) _cell_angle_alpha 90.00 _cell_angle_beta 104.071(5) _cell_angle_gamma 90.00 _cell_volume 1870.5(14) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1525 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 21.82 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.491 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 852 _exptl_absorpt_coefficient_mu 2.179 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6822 _exptl_absorpt_correction_T_max 0.9577 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12553 _diffrn_reflns_av_R_equivalents 0.1021 _diffrn_reflns_av_sigmaI/netI 0.0836 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3268 _reflns_number_gt 2060 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0580P)^2^+31.4347P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3268 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1412 _refine_ls_R_factor_gt 0.0897 _refine_ls_wR_factor_ref 0.2356 _refine_ls_wR_factor_gt 0.2091 _refine_ls_goodness_of_fit_ref 1.122 _refine_ls_restrained_S_all 1.122 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group As1 As 0.35864(8) 0.7362(2) 0.10916(6) 0.0360(4) Uani 1 1 d . . . Cl1 Cl 0.3682(3) 1.0864(6) 0.1113(2) 0.0726(12) Uani 1 1 d . . . S1 S 0.45989(19) 0.6446(5) 0.20472(16) 0.0384(8) Uani 1 1 d . . . S2 S 0.4597(2) 0.6690(6) 0.04885(16) 0.0427(8) Uani 1 1 d . . . C1 C 0.3975(7) 0.650(2) 0.2723(6) 0.037(3) Uani 1 1 d . . . H1A H 0.4278 0.5567 0.3112 0.044 Uiso 1 1 calc R . . H1B H 0.4001 0.7936 0.2915 0.044 Uiso 1 1 calc R . . C2 C 0.3008(7) 0.585(2) 0.2491(5) 0.032(3) Uani 1 1 d . . . C3 C 0.2779(8) 0.379(2) 0.2360(7) 0.045(3) Uani 1 1 d . . . H3A H 0.3236 0.2760 0.2429 0.054 Uiso 1 1 calc R . . C4 C 0.1905(8) 0.321(2) 0.2131(7) 0.047(3) Uani 1 1 d . . . H4A H 0.1766 0.1772 0.2048 0.056 Uiso 1 1 calc R . . C5 C 0.1213(8) 0.465(2) 0.2015(6) 0.039(3) Uani 1 1 d . . . C6 C 0.1451(8) 0.669(2) 0.2155(6) 0.041(3) Uani 1 1 d . . . H6A H 0.0996 0.7726 0.2083 0.049 Uiso 1 1 calc R . . C7 C 0.2329(8) 0.728(2) 0.2397(6) 0.039(3) Uani 1 1 d . . . H7A H 0.2467 0.8712 0.2500 0.047 Uiso 1 1 calc R . . C8 C 0.0291(8) 0.386(2) 0.1733(7) 0.048(3) Uani 1 1 d . . . H8A H 0.0224 0.2401 0.1648 0.057 Uiso 1 1 calc R . . C9 C -0.0436(8) 0.498(2) 0.1590(6) 0.045(3) Uani 1 1 d . . . H9A H -0.0373 0.6433 0.1698 0.055 Uiso 1 1 calc R . . C10 C -0.1360(8) 0.420(2) 0.1273(6) 0.041(3) Uani 1 1 d . . . C11 C -0.1534(8) 0.217(2) 0.1032(7) 0.048(3) Uani 1 1 d . . . H11A H -0.1052 0.1218 0.1071 0.058 Uiso 1 1 calc R . . C12 C -0.2388(8) 0.152(2) 0.0738(6) 0.048(3) Uani 1 1 d . . . H12A H -0.2483 0.0124 0.0571 0.057 Uiso 1 1 calc R . . C13 C -0.3128(8) 0.284(2) 0.0675(6) 0.043(3) Uani 1 1 d . . . C14 C -0.2953(8) 0.488(2) 0.0899(6) 0.043(3) Uani 1 1 d . . . H14A H -0.3435 0.5833 0.0854 0.051 Uiso 1 1 calc R . . C15 C -0.2071(8) 0.556(2) 0.1195(6) 0.047(3) Uani 1 1 d . . . H15A H -0.1967 0.6975 0.1342 0.056 Uiso 1 1 calc R . . C16 C -0.4038(8) 0.213(2) 0.0359(6) 0.044(3) Uani 1 1 d . . . H16A H -0.4409 0.2395 0.0697 0.053 Uiso 1 1 calc R . . H16C H -0.4020 0.0593 0.0293 0.053 Uiso 1 1 calc R . . C1S C -0.092(2) -0.008(8) -0.0420(14) 0.129(10) Uani 1 1 d . . . H1S H -0.1502 -0.0061 -0.0719 0.154 Uiso 1 1 calc R . . C2S C -0.035(3) 0.162(6) -0.0328(16) 0.123(11) Uani 1 1 d . . . H2S H -0.0626 0.2854 -0.0550 0.147 Uiso 1 1 calc R . . C3S C 0.053(3) 0.189(5) 0.0019(17) 0.128(10) Uani 1 1 d . . . H3S H 0.0859 0.3137 -0.0003 0.153 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 As1 0.0274(6) 0.0490(8) 0.0306(6) -0.0007(6) 0.0051(4) 0.0011(6) Cl1 0.080(3) 0.048(2) 0.086(3) -0.001(2) 0.014(2) 0.017(2) S1 0.0292(15) 0.052(2) 0.0333(16) 0.0028(14) 0.0062(12) 0.0037(14) S2 0.0319(16) 0.065(2) 0.0312(16) 0.0009(15) 0.0075(13) 0.0056(15) C1 0.032(6) 0.049(8) 0.030(6) -0.009(6) 0.008(5) 0.000(6) C2 0.033(6) 0.043(8) 0.021(5) 0.002(5) 0.009(5) 0.002(5) C3 0.043(7) 0.033(8) 0.058(8) 0.006(6) 0.009(6) 0.012(6) C4 0.046(8) 0.027(7) 0.064(9) 0.000(6) 0.006(7) -0.004(6) C5 0.032(7) 0.040(8) 0.042(7) 0.006(6) 0.003(5) 0.000(6) C6 0.031(6) 0.047(8) 0.042(7) -0.009(6) 0.001(5) 0.012(6) C7 0.043(7) 0.033(7) 0.040(7) -0.007(6) 0.010(5) 0.005(6) C8 0.040(7) 0.047(8) 0.053(8) 0.005(7) 0.004(6) 0.000(7) C9 0.047(8) 0.050(8) 0.044(8) 0.000(7) 0.021(6) -0.004(7) C10 0.035(7) 0.063(9) 0.025(6) -0.003(6) 0.009(5) -0.006(6) C11 0.036(7) 0.059(10) 0.044(7) -0.001(7) -0.001(6) 0.017(7) C12 0.042(8) 0.066(10) 0.032(7) 0.006(6) 0.003(6) 0.007(7) C13 0.041(7) 0.056(9) 0.036(7) 0.012(6) 0.016(5) 0.005(6) C14 0.043(7) 0.044(8) 0.038(7) 0.003(6) 0.005(6) 0.007(6) C15 0.038(7) 0.059(10) 0.040(7) 0.007(6) 0.006(6) 0.005(6) C16 0.050(7) 0.051(9) 0.028(6) 0.009(6) 0.003(5) -0.004(6) C1S 0.15(3) 0.18(3) 0.070(17) -0.04(2) 0.047(17) 0.04(3) C2S 0.18(3) 0.12(3) 0.081(18) 0.027(16) 0.05(2) 0.09(2) C3S 0.20(4) 0.14(3) 0.071(16) -0.017(19) 0.077(19) 0.01(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag As1 S1 2.204(3) . ? As1 S2 2.213(3) . ? As1 Cl1 2.244(4) . ? S1 C1 1.814(11) . ? S2 C16 1.836(11) 3_565 ? C1 C2 1.505(15) . ? C2 C7 1.366(16) . ? C2 C3 1.372(17) . ? C3 C4 1.365(17) . ? C4 C5 1.382(17) . ? C5 C6 1.365(17) . ? C5 C8 1.481(17) . ? C6 C7 1.373(16) . ? C8 C9 1.301(17) . ? C9 C10 1.495(17) . ? C10 C15 1.378(17) . ? C10 C11 1.384(19) . ? C11 C12 1.367(17) . ? C12 C13 1.399(17) . ? C13 C14 1.379(19) . ? C13 C16 1.461(17) . ? C14 C15 1.411(17) . ? C16 S2 1.836(11) 3_565 ? C1S C2S 1.38(4) . ? C1S C3S 1.44(4) 3 ? C2S C3S 1.38(4) . ? C3S C1S 1.44(4) 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 S1 As1 S2 87.52(12) . . ? S1 As1 Cl1 102.69(15) . . ? S2 As1 Cl1 98.77(16) . . ? C1 S1 As1 102.9(4) . . ? C16 S2 As1 99.5(4) 3_565 . ? C2 C1 S1 115.9(8) . . ? C7 C2 C3 117.6(11) . . ? C7 C2 C1 121.8(12) . . ? C3 C2 C1 120.6(11) . . ? C4 C3 C2 120.8(12) . . ? C3 C4 C5 122.2(12) . . ? C6 C5 C4 116.4(11) . . ? C6 C5 C8 125.8(12) . . ? C4 C5 C8 117.8(12) . . ? C5 C6 C7 121.8(12) . . ? C2 C7 C6 121.3(12) . . ? C9 C8 C5 126.1(13) . . ? C8 C9 C10 126.0(14) . . ? C15 C10 C11 118.1(12) . . ? C15 C10 C9 119.1(13) . . ? C11 C10 C9 122.8(12) . . ? C12 C11 C10 121.1(12) . . ? C11 C12 C13 122.2(14) . . ? C14 C13 C12 116.7(12) . . ? C14 C13 C16 121.6(12) . . ? C12 C13 C16 121.6(13) . . ? C13 C14 C15 121.2(13) . . ? C10 C15 C14 120.6(13) . . ? C13 C16 S2 116.4(9) . 3_565 ? C2S C1S C3S 114(3) . 3 ? C3S C2S C1S 133(3) . . ? C2S C3S C1S 113(3) . 3 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.294 _refine_diff_density_min -1.428 _refine_diff_density_rms 0.153 ###end data_g16 _database_code_depnum_ccdc_archive 'CCDC 676182' _audit_creation_method SHELXLTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H20 As Cl S2' _chemical_formula_weight 446.86 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' _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 9.3876(7) _cell_length_b 9.6322(8) _cell_length_c 12.0300(9) _cell_angle_alpha 107.6460(10) _cell_angle_beta 99.3000(10) _cell_angle_gamma 101.4170(10) _cell_volume 987.09(13) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4219 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 26.91 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.503 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 456 _exptl_absorpt_coefficient_mu 2.070 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7070 _exptl_absorpt_correction_T_max 0.7893 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11379 _diffrn_reflns_av_R_equivalents 0.0211 _diffrn_reflns_av_sigmaI/netI 0.0281 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4453 _reflns_number_gt 3914 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0374P)^2^+0.8183P] 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 4453 _refine_ls_number_parameters 318 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0450 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.0910 _refine_ls_wR_factor_gt 0.0876 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.103 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group As1 As 0.73005(3) 0.86935(3) 0.63285(2) 0.03232(10) Uani 1 1 d . . . S1 S 0.63475(10) 0.65435(10) 0.48360(8) 0.0436(2) Uani 0.8690(17) 1 d P A 1 S2 S 0.50023(9) 0.89498(9) 0.62746(8) 0.0391(2) Uani 0.8690(17) 1 d P . 1 Cl1 Cl 0.81573(10) 1.02453(11) 0.53714(9) 0.0495(3) Uani 0.8690(17) 1 d P A 1 C1 C 0.7966(5) 0.5761(5) 0.4665(3) 0.0609(11) Uani 0.8690(17) 1 d P A 1 H1A H 0.7600 0.4655 0.4250 0.073 Uiso 0.8690(17) 1 calc PR A 1 H1B H 0.8498 0.6185 0.4147 0.073 Uiso 0.8690(17) 1 calc PR A 1 C14 C 1.4620(4) 0.8983(3) 1.2975(3) 0.0460(8) Uani 0.8690(17) 1 d P . 1 H14A H 1.5587 0.8718 1.2980 0.055 Uiso 0.8690(17) 1 calc PR A 1 H14B H 1.4090 0.8469 1.3448 0.055 Uiso 0.8690(17) 1 calc PR A 1 S1A S 0.7387(10) 0.7396(10) 0.4514(5) 0.064(3) Uani 0.1310(17) 1 d P A 2 S2A S 0.6921(8) 1.0525(7) 0.5818(5) 0.0506(18) Uani 0.1310(17) 1 d P . 2 Cl1A Cl 0.4638(9) 0.7498(9) 0.6079(9) 0.076(3) Uani 0.1310(17) 1 d P A 2 C1A C 0.7966(5) 0.5761(5) 0.4665(3) 0.0609(11) Uani 0.1310(17) 1 d P A 2 H1AA H 0.7067 0.4970 0.4591 0.073 Uiso 0.1310(17) 1 calc PR A 2 H1AB H 0.8427 0.5356 0.3994 0.073 Uiso 0.1310(17) 1 calc PR A 2 C14A C 1.4620(4) 0.8983(3) 1.2975(3) 0.0460(8) Uani 0.1310(17) 1 d P . 2 H14C H 1.5402 0.9913 1.3114 0.055 Uiso 0.1310(17) 1 calc PR A 2 H14D H 1.5113 0.8222 1.3136 0.055 Uiso 0.1310(17) 1 calc PR A 2 C2 C 0.9057(4) 0.6075(4) 0.5830(3) 0.0424(7) Uani 1 1 d . . . C3 C 0.8767(4) 0.5260(4) 0.6575(3) 0.0413(7) Uani 1 1 d . A . H3 H 0.798(4) 0.460(4) 0.637(3) 0.059(12) Uiso 1 1 d . . . C4 C 0.9717(3) 0.5625(3) 0.7688(3) 0.0349(6) Uani 1 1 d . . . H4 H 0.949(3) 0.511(3) 0.819(3) 0.032(8) Uiso 1 1 d . . . C5 C 1.1011(3) 0.6820(3) 0.8087(2) 0.0299(5) Uani 1 1 d . A . C6 C 1.1334(4) 0.7587(3) 0.7308(3) 0.0368(6) Uani 1 1 d . . . H6 H 1.214(4) 0.835(4) 0.754(3) 0.046(9) Uiso 1 1 d . . . C7 C 1.0360(4) 0.7219(4) 0.6199(3) 0.0454(8) Uani 1 1 d . A . H7 H 1.059(4) 0.776(4) 0.578(3) 0.044(9) Uiso 1 1 d . . . C8 C 1.1960(3) 0.7316(3) 0.9327(2) 0.0285(5) Uani 1 1 d . . . C9 C 1.3498(3) 0.7988(3) 0.9603(3) 0.0343(6) Uani 1 1 d . A . H9 H 1.392(3) 0.804(3) 0.901(3) 0.036(8) Uiso 1 1 d . . . C10 C 1.4344(3) 0.8505(3) 1.0764(3) 0.0385(7) Uani 1 1 d . . . H10 H 1.536(4) 0.890(3) 1.093(3) 0.038(8) Uiso 1 1 d . . . C11 C 1.3703(3) 0.8390(3) 1.1703(3) 0.0354(6) Uani 1 1 d . A . C12 C 1.2174(3) 0.7714(3) 1.1437(3) 0.0353(6) Uani 1 1 d . . . H12 H 1.172(4) 0.765(4) 1.201(3) 0.040(9) Uiso 1 1 d . . . C13 C 1.1317(3) 0.7180(3) 1.0266(2) 0.0312(6) Uani 1 1 d . A . H13 H 1.034(3) 0.681(3) 1.016(2) 0.020(6) Uiso 1 1 d . . . C15 C 1.2354(3) 1.1919(3) 1.0409(3) 0.0393(7) Uani 1 1 d . . . H15 H 1.238(3) 1.151(4) 1.102(3) 0.040(8) Uiso 1 1 d . . . C16 C 1.1503(3) 1.1019(4) 0.9283(3) 0.0421(7) Uani 1 1 d . . . H16 H 1.094(4) 0.996(4) 0.910(3) 0.051(10) Uiso 1 1 d . . . C17 C 1.1426(3) 1.1556(4) 0.8341(3) 0.0440(7) Uani 1 1 d . . . H17 H 1.086(4) 1.095(4) 0.757(3) 0.044(9) Uiso 1 1 d . . . C18 C 1.2182(4) 1.3017(4) 0.8543(3) 0.0449(7) Uani 1 1 d . . . H18 H 1.210(4) 1.336(4) 0.790(3) 0.056(10) Uiso 1 1 d . . . C19 C 1.3035(3) 1.3949(3) 0.9696(3) 0.0384(6) Uani 1 1 d . . . H19 H 1.356(4) 1.497(4) 0.980(3) 0.049(9) Uiso 1 1 d . . . C20 C 1.3147(3) 1.3401(3) 1.0632(3) 0.0366(6) Uani 1 1 d . . . C21 C 1.4124(5) 1.4376(5) 1.1841(3) 0.0522(9) Uani 1 1 d . . . H21C H 1.504(5) 1.435(5) 1.188(4) 0.073(13) Uiso 1 1 d . . . H21B H 1.382(6) 1.398(6) 1.236(5) 0.106(19) Uiso 1 1 d . . . H21A H 1.404(5) 1.535(6) 1.206(4) 0.097(16) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 As1 0.03487(16) 0.03431(17) 0.02623(15) 0.00783(11) 0.00265(11) 0.01358(12) S1 0.0455(5) 0.0345(5) 0.0368(5) -0.0007(4) -0.0042(4) 0.0117(4) S2 0.0269(4) 0.0357(5) 0.0440(5) 0.0021(4) 0.0068(3) 0.0044(3) Cl1 0.0429(5) 0.0572(6) 0.0536(5) 0.0301(5) 0.0127(4) 0.0061(4) C1 0.081(3) 0.074(3) 0.0314(16) 0.0063(16) 0.0059(16) 0.054(2) C14 0.0475(18) 0.0399(17) 0.0444(17) 0.0043(14) -0.0012(14) 0.0235(14) S1A 0.093(6) 0.087(6) 0.027(3) 0.016(3) 0.011(3) 0.062(5) S2A 0.068(4) 0.042(3) 0.033(3) 0.015(3) -0.008(3) 0.008(3) Cl1A 0.059(4) 0.061(5) 0.111(7) 0.037(5) 0.021(4) 0.008(4) C1A 0.081(3) 0.074(3) 0.0314(16) 0.0063(16) 0.0059(16) 0.054(2) C14A 0.0475(18) 0.0399(17) 0.0444(17) 0.0043(14) -0.0012(14) 0.0235(14) C2 0.0559(19) 0.0462(18) 0.0291(14) 0.0061(13) 0.0110(13) 0.0327(15) C3 0.0402(17) 0.0423(17) 0.0363(16) 0.0055(13) 0.0070(13) 0.0143(14) C4 0.0403(15) 0.0334(15) 0.0323(14) 0.0120(12) 0.0099(12) 0.0106(12) C5 0.0361(14) 0.0275(13) 0.0316(13) 0.0091(11) 0.0139(11) 0.0173(11) C6 0.0474(17) 0.0297(15) 0.0388(16) 0.0116(12) 0.0188(13) 0.0160(13) C7 0.077(2) 0.0451(18) 0.0354(16) 0.0232(15) 0.0282(16) 0.0357(17) C8 0.0317(13) 0.0229(12) 0.0336(14) 0.0086(10) 0.0102(11) 0.0127(10) C9 0.0350(15) 0.0293(14) 0.0440(16) 0.0130(12) 0.0178(13) 0.0132(11) C10 0.0308(15) 0.0304(15) 0.0490(18) 0.0064(13) 0.0059(13) 0.0108(12) C11 0.0371(15) 0.0268(13) 0.0389(15) 0.0050(11) 0.0013(12) 0.0168(11) C12 0.0447(16) 0.0354(15) 0.0325(15) 0.0129(12) 0.0146(13) 0.0188(13) C13 0.0300(14) 0.0314(14) 0.0346(14) 0.0107(11) 0.0103(11) 0.0121(11) C15 0.0418(16) 0.0391(16) 0.0453(17) 0.0182(14) 0.0186(13) 0.0169(13) C16 0.0386(16) 0.0340(16) 0.0542(19) 0.0107(14) 0.0172(14) 0.0128(13) C17 0.0324(15) 0.0487(19) 0.0429(18) 0.0042(15) 0.0057(13) 0.0140(13) C18 0.0416(17) 0.057(2) 0.0468(18) 0.0268(16) 0.0136(14) 0.0206(15) C19 0.0328(15) 0.0348(16) 0.0534(18) 0.0187(14) 0.0154(13) 0.0119(12) C20 0.0327(14) 0.0401(16) 0.0388(15) 0.0104(12) 0.0130(12) 0.0147(12) C21 0.046(2) 0.057(2) 0.0433(19) 0.0043(17) 0.0107(16) 0.0119(17) _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 As1 S2A 2.110(6) . ? As1 S1A 2.185(6) . ? As1 S1 2.1922(9) . ? As1 S2 2.2125(9) . ? As1 Cl1 2.2524(9) . ? As1 Cl1A 2.464(8) . ? S1 C1 1.838(3) . ? S2 C14 1.853(3) 2_777 ? C1 C2 1.504(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C14 C11 1.504(4) . ? C14 S2 1.853(3) 2_777 ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? S2A C14A 2.226(8) 2_777 ? C2 C7 1.379(5) . ? C2 C3 1.383(5) . ? C3 C4 1.385(4) . ? C3 H3 0.82(4) . ? C4 C5 1.397(4) . ? C4 H4 0.92(3) . ? C5 C6 1.392(4) . ? C5 C8 1.488(4) . ? C6 C7 1.390(5) . ? C6 H6 0.88(3) . ? C7 H7 0.85(3) . ? C8 C13 1.392(4) . ? C8 C9 1.399(4) . ? C9 C10 1.376(4) . ? C9 H9 0.88(3) . ? C10 C11 1.385(4) . ? C10 H10 0.91(3) . ? C11 C12 1.394(4) . ? C12 C13 1.388(4) . ? C12 H12 0.88(3) . ? C13 H13 0.89(3) . ? C15 C16 1.375(4) . ? C15 C20 1.395(4) . ? C15 H15 0.94(3) . ? C16 C17 1.378(5) . ? C16 H16 0.99(4) . ? C17 C18 1.373(5) . ? C17 H17 0.93(3) . ? C18 C19 1.404(5) . ? C18 H18 0.92(4) . ? C19 C20 1.379(4) . ? C19 H19 0.97(3) . ? C20 C21 1.496(5) . ? C21 H21C 0.86(5) . ? C21 H21B 0.88(6) . ? C21 H21A 0.92(5) . ? 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 S2A As1 S1A 92.4(3) . . ? S2A As1 S1 111.35(17) . . ? S1A As1 S1 35.4(3) . . ? S2A As1 S2 66.3(2) . . ? S1A As1 S2 108.1(2) . . ? S1 As1 S2 88.19(3) . . ? S2A As1 Cl1 37.1(2) . . ? S1A As1 Cl1 69.4(2) . . ? S1 As1 Cl1 101.63(4) . . ? S2 As1 Cl1 101.23(4) . . ? S2A As1 Cl1A 95.4(3) . . ? S1A As1 Cl1A 94.9(3) . . ? S1 As1 Cl1A 64.2(2) . . ? S2 As1 Cl1A 31.9(2) . . ? Cl1 As1 Cl1A 124.7(2) . . ? C1 S1 As1 103.37(13) . . ? C14 S2 As1 101.12(11) 2_777 . ? C2 C1 S1 114.1(2) . . ? C2 C1 H1A 108.7 . . ? S1 C1 H1A 108.7 . . ? C2 C1 H1B 108.7 . . ? S1 C1 H1B 108.7 . . ? H1A C1 H1B 107.6 . . ? C11 C14 S2 114.4(2) . 2_777 ? C11 C14 H14A 108.7 . . ? S2 C14 H14A 108.7 2_777 . ? C11 C14 H14B 108.7 . . ? S2 C14 H14B 108.7 2_777 . ? H14A C14 H14B 107.6 . . ? As1 S2A C14A 93.1(3) . 2_777 ? C7 C2 C3 118.2(3) . . ? C7 C2 C1 120.5(3) . . ? C3 C2 C1 121.2(3) . . ? C2 C3 C4 121.1(3) . . ? C2 C3 H3 119(3) . . ? C4 C3 H3 120(3) . . ? C3 C4 C5 120.9(3) . . ? C3 C4 H4 120.5(19) . . ? C5 C4 H4 118.6(18) . . ? C6 C5 C4 117.6(3) . . ? C6 C5 C8 121.1(3) . . ? C4 C5 C8 121.3(2) . . ? C7 C6 C5 120.8(3) . . ? C7 C6 H6 120(2) . . ? C5 C6 H6 119(2) . . ? C2 C7 C6 121.2(3) . . ? C2 C7 H7 122(2) . . ? C6 C7 H7 117(2) . . ? C13 C8 C9 117.7(3) . . ? C13 C8 C5 120.2(2) . . ? C9 C8 C5 122.0(2) . . ? C10 C9 C8 121.2(3) . . ? C10 C9 H9 121(2) . . ? C8 C9 H9 118(2) . . ? C9 C10 C11 121.2(3) . . ? C9 C10 H10 120.7(19) . . ? C11 C10 H10 118.0(19) . . ? C10 C11 C12 118.1(3) . . ? C10 C11 C14 121.3(3) . . ? C12 C11 C14 120.6(3) . . ? C13 C12 C11 120.9(3) . . ? C13 C12 H12 118(2) . . ? C11 C12 H12 121(2) . . ? C12 C13 C8 120.8(3) . . ? C12 C13 H13 116.9(17) . . ? C8 C13 H13 122.2(17) . . ? C16 C15 C20 121.0(3) . . ? C16 C15 H15 118(2) . . ? C20 C15 H15 121(2) . . ? C15 C16 C17 120.7(3) . . ? C15 C16 H16 123(2) . . ? C17 C16 H16 117(2) . . ? C18 C17 C16 119.3(3) . . ? C18 C17 H17 120(2) . . ? C16 C17 H17 121(2) . . ? C17 C18 C19 120.3(3) . . ? C17 C18 H18 118(2) . . ? C19 C18 H18 122(2) . . ? C20 C19 C18 120.5(3) . . ? C20 C19 H19 122(2) . . ? C18 C19 H19 118(2) . . ? C19 C20 C15 118.2(3) . . ? C19 C20 C21 120.1(3) . . ? C15 C20 C21 121.7(3) . . ? C20 C21 H21C 111(3) . . ? C20 C21 H21B 107(4) . . ? H21C C21 H21B 107(4) . . ? C20 C21 H21A 113(3) . . ? H21C C21 H21A 111(4) . . ? H21B C21 H21A 108(4) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.926 _refine_diff_density_min -0.489 _refine_diff_density_rms 0.069 ###end data_g22 _database_code_depnum_ccdc_archive 'CCDC 676183' _audit_creation_method SHELXLTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H24 As2 Cl2 O4 S4' _chemical_formula_weight 677.37 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' Cl Cl 0.1484 0.1585 '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' _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 8.4805(11) _cell_length_b 9.3290(12) _cell_length_c 9.6719(12) _cell_angle_alpha 117.4210(10) _cell_angle_beta 101.198(2) _cell_angle_gamma 98.034(2) _cell_volume 642.79(14) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3334 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 26.99 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.750 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 340 _exptl_absorpt_coefficient_mu 3.158 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4827 _exptl_absorpt_correction_T_max 0.7430 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5920 _diffrn_reflns_av_R_equivalents 0.0131 _diffrn_reflns_av_sigmaI/netI 0.0193 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 26.99 _reflns_number_total 2713 _reflns_number_gt 2484 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0410P)^2^+0.4548P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2713 _refine_ls_number_parameters 193 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0316 _refine_ls_R_factor_gt 0.0280 _refine_ls_wR_factor_ref 0.0713 _refine_ls_wR_factor_gt 0.0692 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group As1 As 0.16080(3) 0.26118(3) 1.17751(3) 0.02557(9) Uani 1 1 d . . . Cl1 Cl -0.04493(11) 0.38626(11) 1.15588(11) 0.0517(2) Uani 1 1 d . . . S1 S 0.36983(9) 0.41142(8) 1.15372(8) 0.03433(16) Uani 1 1 d . . . S2 S -0.28501(11) -0.40472(10) 0.55809(8) 0.0518(2) Uani 1 1 d . . . O1 O -0.2712(2) 0.0116(2) 0.6084(2) 0.0369(4) Uani 1 1 d . . . O2 O 0.3927(2) 0.0482(3) 0.8293(3) 0.0407(5) Uani 1 1 d . . . C1 C 0.3050(4) 0.3460(3) 0.9355(3) 0.0306(5) Uani 1 1 d . . . C2 C 0.1788(3) 0.1805(3) 0.8255(3) 0.0259(5) Uani 1 1 d . . . C3 C 0.0126(3) 0.1747(3) 0.7723(3) 0.0261(5) Uani 1 1 d . . . C4 C -0.1053(3) 0.0244(3) 0.6647(3) 0.0265(5) Uani 1 1 d . . . C5 C -0.0565(3) -0.1250(3) 0.6053(3) 0.0283(5) Uani 1 1 d . . . C6 C 0.1094(3) -0.1187(3) 0.6603(3) 0.0299(5) Uani 1 1 d . . . C7 C 0.2273(3) 0.0316(3) 0.7709(3) 0.0292(5) Uani 1 1 d . . . C8 C -0.3197(4) 0.1658(4) 0.6703(4) 0.0430(7) Uani 1 1 d . . . C9 C 0.4451(5) -0.1036(5) 0.7831(5) 0.0538(8) Uani 1 1 d . . . C10 C -0.1792(4) -0.2874(3) 0.4803(3) 0.0376(6) Uani 1 1 d . . . H1A H 0.407(4) 0.345(4) 0.909(4) 0.035(8) Uiso 1 1 d . . . H1B H 0.264(4) 0.434(4) 0.931(4) 0.042(8) Uiso 1 1 d . . . H3 H -0.019(4) 0.272(4) 0.808(4) 0.035(8) Uiso 1 1 d . . . H6 H 0.143(4) -0.213(4) 0.628(4) 0.034(7) Uiso 1 1 d . . . H8A H -0.293(4) 0.223(4) 0.788(4) 0.047(9) Uiso 1 1 d . . . H8B H -0.434(5) 0.138(5) 0.628(4) 0.059(11) Uiso 1 1 d . . . H8C H -0.265(4) 0.237(4) 0.640(4) 0.040(8) Uiso 1 1 d . . . H9A H 0.377(5) -0.181(4) 0.811(4) 0.052(10) Uiso 1 1 d . . . H9B H 0.427(4) -0.169(4) 0.662(4) 0.049(9) Uiso 1 1 d . . . H9C H 0.558(5) -0.060(4) 0.845(4) 0.050(9) Uiso 1 1 d . . . H10A H -0.266(5) -0.278(5) 0.413(5) 0.070(12) Uiso 1 1 d . . . H10B H -0.128(5) -0.361(5) 0.416(5) 0.062(11) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 As1 0.02965(15) 0.02064(13) 0.02618(14) 0.01167(10) 0.00936(10) 0.00464(10) Cl1 0.0568(5) 0.0610(5) 0.0660(5) 0.0417(4) 0.0353(4) 0.0382(4) S1 0.0345(4) 0.0325(3) 0.0300(3) 0.0152(3) 0.0073(3) -0.0036(3) S2 0.0609(5) 0.0439(4) 0.0275(3) 0.0143(3) 0.0023(3) -0.0249(4) O1 0.0269(10) 0.0332(10) 0.0415(10) 0.0146(8) 0.0048(8) 0.0040(8) O2 0.0307(10) 0.0437(11) 0.0527(12) 0.0265(10) 0.0124(9) 0.0153(9) C1 0.0323(14) 0.0304(13) 0.0309(13) 0.0194(11) 0.0071(10) 0.0019(11) C2 0.0311(13) 0.0265(11) 0.0246(11) 0.0164(10) 0.0100(9) 0.0047(10) C3 0.0326(13) 0.0228(11) 0.0271(11) 0.0143(10) 0.0124(10) 0.0080(10) C4 0.0264(12) 0.0289(12) 0.0257(11) 0.0153(10) 0.0089(9) 0.0036(10) C5 0.0387(14) 0.0242(11) 0.0234(11) 0.0126(9) 0.0138(10) 0.0037(10) C6 0.0419(15) 0.0259(12) 0.0304(12) 0.0163(10) 0.0188(11) 0.0135(11) C7 0.0331(13) 0.0347(13) 0.0307(12) 0.0215(11) 0.0156(10) 0.0133(11) C8 0.0299(16) 0.0422(16) 0.0514(19) 0.0201(15) 0.0081(13) 0.0116(13) C9 0.045(2) 0.059(2) 0.067(2) 0.0347(19) 0.0180(18) 0.0299(18) C10 0.0533(18) 0.0267(13) 0.0272(13) 0.0106(11) 0.0138(13) 0.0024(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 As1 S2 2.2018(8) 2_557 ? As1 S1 2.2182(7) . ? As1 Cl1 2.2586(8) . ? S1 C1 1.844(3) . ? S2 C10 1.821(3) . ? S2 As1 2.2018(8) 2_557 ? O1 C4 1.373(3) . ? O1 C8 1.437(3) . ? O2 C7 1.364(3) . ? O2 C9 1.440(4) . ? C1 C2 1.498(3) . ? C1 H1A 0.94(3) . ? C1 H1B 0.95(3) . ? C2 C3 1.388(4) . ? C2 C7 1.395(3) . ? C3 C4 1.381(3) . ? C3 H3 0.91(3) . ? C4 C5 1.400(3) . ? C5 C6 1.387(4) . ? C5 C10 1.491(4) . ? C6 C7 1.386(4) . ? C6 H6 0.90(3) . ? C8 H8A 0.97(3) . ? C8 H8B 0.92(4) . ? C8 H8C 0.94(3) . ? C9 H9A 1.02(4) . ? C9 H9B 1.01(3) . ? C9 H9C 0.94(4) . ? C10 H10A 0.92(4) . ? C10 H10B 0.92(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 S2 As1 S1 86.76(3) 2_557 . ? S2 As1 Cl1 101.50(4) 2_557 . ? S1 As1 Cl1 102.73(3) . . ? C1 S1 As1 102.92(9) . . ? C10 S2 As1 103.85(10) . 2_557 ? C4 O1 C8 116.2(2) . . ? C7 O2 C9 117.0(2) . . ? C2 C1 S1 116.08(17) . . ? C2 C1 H1A 111.3(18) . . ? S1 C1 H1A 102.9(18) . . ? C2 C1 H1B 111(2) . . ? S1 C1 H1B 105.0(19) . . ? H1A C1 H1B 110(3) . . ? C3 C2 C7 119.3(2) . . ? C3 C2 C1 119.9(2) . . ? C7 C2 C1 120.7(2) . . ? C4 C3 C2 121.3(2) . . ? C4 C3 H3 119.6(19) . . ? C2 C3 H3 119.1(19) . . ? O1 C4 C3 123.6(2) . . ? O1 C4 C5 116.7(2) . . ? C3 C4 C5 119.7(2) . . ? C6 C5 C4 118.8(2) . . ? C6 C5 C10 120.5(2) . . ? C4 C5 C10 120.7(3) . . ? C5 C6 C7 121.6(2) . . ? C5 C6 H6 120.7(19) . . ? C7 C6 H6 117.7(19) . . ? O2 C7 C6 125.0(2) . . ? O2 C7 C2 115.7(2) . . ? C6 C7 C2 119.3(2) . . ? O1 C8 H8A 111.1(19) . . ? O1 C8 H8B 107(2) . . ? H8A C8 H8B 108(3) . . ? O1 C8 H8C 110.3(19) . . ? H8A C8 H8C 109(3) . . ? H8B C8 H8C 112(3) . . ? O2 C9 H9A 110.8(19) . . ? O2 C9 H9B 110.9(19) . . ? H9A C9 H9B 106(3) . . ? O2 C9 H9C 101(2) . . ? H9A C9 H9C 114(3) . . ? H9B C9 H9C 114(3) . . ? C5 C10 S2 115.99(18) . . ? C5 C10 H10A 114(3) . . ? S2 C10 H10A 103(3) . . ? C5 C10 H10B 111(2) . . ? S2 C10 H10B 103(2) . . ? H10A C10 H10B 109(3) . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 26.99 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 0.661 _refine_diff_density_min -0.399 _refine_diff_density_rms 0.076 ###end ###end data_g24 _database_code_depnum_ccdc_archive 'CCDC 676184' _audit_creation_method SHELXLTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H29 As2 Cl2 O4 S4' _chemical_formula_weight 730.45 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' O O 0.0106 0.0060 '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 13.9458(17) _cell_length_b 9.8297(12) _cell_length_c 21.814(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.784(2) _cell_angle_gamma 90.00 _cell_volume 2990.0(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2964 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 22.19 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.623 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1476 _exptl_absorpt_coefficient_mu 2.722 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6400 _exptl_absorpt_correction_T_max 0.7725 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14607 _diffrn_reflns_av_R_equivalents 0.0309 _diffrn_reflns_av_sigmaI/netI 0.0476 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 27.00 _reflns_number_total 6483 _reflns_number_gt 4716 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0210P)^2^+15.5684P] 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 constr _refine_ls_extinction_coef ? _refine_ls_number_reflns 6483 _refine_ls_number_parameters 371 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0985 _refine_ls_R_factor_gt 0.0713 _refine_ls_wR_factor_ref 0.1440 _refine_ls_wR_factor_gt 0.1340 _refine_ls_goodness_of_fit_ref 1.134 _refine_ls_restrained_S_all 1.141 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group As1 As 0.25623(5) 0.53689(8) 0.04433(3) 0.0478(2) Uani 1 1 d . . . Cl1 Cl 0.14697(17) 0.3695(2) 0.04918(10) 0.0748(6) Uani 1 1 d . . . As2 As 0.1799(4) 0.8465(4) 0.2124(2) 0.0391(11) Uani 0.69(4) 1 d P A 1 Cl2 Cl 0.0674(6) 0.8113(6) 0.2826(3) 0.053(2) Uani 0.69(4) 1 d P A 1 As2A As 0.196(2) 0.861(2) 0.2002(13) 0.073(4) Uani 0.31(4) 1 d P A 2 Cl2A Cl 0.102(4) 0.805(2) 0.2789(9) 0.118(8) Uani 0.31(4) 1 d P A 2 S1 S 0.24741(14) 0.58641(19) -0.05460(7) 0.0514(4) Uani 1 1 d . . . S2 S 0.15529(16) 1.06576(19) 0.18799(8) 0.0610(5) Uani 1 1 d . . . S3 S 0.39013(17) 0.4274(3) 0.02550(10) 0.0917(9) Uani 1 1 d . . . S4 S 0.30473(18) 0.9146(3) 0.26855(12) 0.0886(9) Uani 1 1 d . . . C1 C 0.1275(5) 0.6605(7) -0.0589(3) 0.0464(16) Uani 1 1 d . . . H1A H 0.1185 0.7030 -0.0997 0.056 Uiso 1 1 calc R . . H1B H 0.0798 0.5865 -0.0553 0.056 Uiso 1 1 calc R . . C2 C 0.1080(5) 0.7643(6) -0.0110(3) 0.0407(15) Uani 1 1 d . A . C3 C 0.1407(5) 0.8978(7) -0.0165(3) 0.0417(15) Uani 1 1 d . . . C4 C 0.1244(4) 0.9917(6) 0.0293(3) 0.0388(14) Uani 1 1 d . A . H4A H 0.1481 1.0818 0.0253 0.047 Uiso 1 1 calc R . . C5 C 0.0737(4) 0.9555(6) 0.0813(3) 0.0396(14) Uani 1 1 d . . . C6 C 0.0396(4) 0.8235(6) 0.0868(3) 0.0372(14) Uani 1 1 d . A . C7 C 0.0567(4) 0.7294(6) 0.0406(3) 0.0393(14) Uani 1 1 d . . . H7A H 0.0327 0.6394 0.0446 0.047 Uiso 1 1 calc R A . C8 C 0.0576(5) 1.0568(7) 0.1309(3) 0.0488(16) Uani 1 1 d . A . H8A H -0.0026 1.0336 0.1520 0.059 Uiso 1 1 calc R . . H8B H 0.0491 1.1478 0.1121 0.059 Uiso 1 1 calc R . . C9 C 0.2226(6) 1.0630(8) -0.0772(3) 0.061(2) Uani 1 1 d . . . H9A H 0.2562 1.0707 -0.1161 0.092 Uiso 1 1 calc R . . H9B H 0.2664 1.0868 -0.0433 0.092 Uiso 1 1 calc R . . H9C H 0.1676 1.1251 -0.0773 0.092 Uiso 1 1 calc R . . C10 C -0.0453(6) 0.6581(7) 0.1468(3) 0.0576(19) Uani 1 1 d . A . H10A H -0.0789 0.6510 0.1858 0.086 Uiso 1 1 calc R . . H10B H 0.0086 0.5941 0.1466 0.086 Uiso 1 1 calc R . . H10C H -0.0897 0.6362 0.1130 0.086 Uiso 1 1 calc R . . C11 C 0.4273(7) 0.3698(9) 0.1011(4) 0.078(3) Uani 1 1 d . . . H11A H 0.3941 0.2831 0.1097 0.094 Uiso 1 1 calc R B 1 H11B H 0.4969 0.3504 0.1004 0.094 Uiso 1 1 calc R B 1 C12 C 0.4087(5) 0.4661(7) 0.1532(3) 0.0503(17) Uani 0.734(8) 1 d P A 1 C13 C 0.4742(5) 0.5680(7) 0.1664(3) 0.0501(17) Uani 0.734(8) 1 d P A 1 C14 C 0.4561(5) 0.6609(7) 0.2131(3) 0.0509(17) Uani 0.734(8) 1 d P A 1 H14A H 0.5009 0.7313 0.2216 0.061 Uiso 0.734(8) 1 calc PR A 1 C15 C 0.3744(5) 0.6518(8) 0.2469(3) 0.0506(17) Uani 0.734(8) 1 d P A 1 C16 C 0.3098(5) 0.5504(8) 0.2338(3) 0.0538(19) Uani 0.734(8) 1 d P A 1 C17 C 0.3288(6) 0.4576(7) 0.1876(3) 0.0551(19) Uani 0.734(8) 1 d P A 1 H17A H 0.2845 0.3860 0.1799 0.066 Uiso 0.734(8) 1 calc PR A 1 C19 C 0.6185(8) 0.6960(12) 0.1415(6) 0.068(3) Uani 0.734(8) 1 d P A 1 H19A H 0.6728 0.6911 0.1135 0.102 Uiso 0.734(8) 1 calc PR A 1 H19B H 0.6424 0.6949 0.1840 0.102 Uiso 0.734(8) 1 calc PR A 1 H19C H 0.5828 0.7804 0.1340 0.102 Uiso 0.734(8) 1 calc PR A 1 C20 C 0.1575(8) 0.4347(13) 0.2491(5) 0.071(4) Uani 0.734(8) 1 d P A 1 H20A H 0.1033 0.4383 0.2771 0.106 Uiso 0.734(8) 1 calc PR A 1 H20B H 0.1868 0.3441 0.2508 0.106 Uiso 0.734(8) 1 calc PR A 1 H20C H 0.1347 0.4531 0.2072 0.106 Uiso 0.734(8) 1 calc PR A 1 O3 O 0.5570(4) 0.5824(7) 0.1315(3) 0.057(2) Uani 0.734(8) 1 d P A 1 O4 O 0.2270(5) 0.5348(7) 0.2667(3) 0.059(2) Uani 0.734(8) 1 d P A 1 C12A C 0.4087(5) 0.4661(7) 0.1532(3) 0.0503(17) Uani 0.266(8) 1 d PD A 2 C13A C 0.4742(5) 0.5680(7) 0.1664(3) 0.0501(17) Uani 0.266(8) 1 d PD A 2 H13A H 0.5316 0.5747 0.1437 0.060 Uiso 0.266(8) 1 calc PR A 2 C14A C 0.4561(5) 0.6609(7) 0.2131(3) 0.0509(17) Uani 0.266(8) 1 d P A 2 C15A C 0.3744(5) 0.6518(8) 0.2469(3) 0.0506(17) Uani 0.266(8) 1 d PD A 2 C16A C 0.3098(5) 0.5504(8) 0.2338(3) 0.0538(19) Uani 0.266(8) 1 d PD A 2 H16A H 0.2521 0.5438 0.2563 0.065 Uiso 0.266(8) 1 calc PR A 2 C17A C 0.3288(6) 0.4576(7) 0.1876(3) 0.0551(19) Uani 0.266(8) 1 d P A 2 C19A C 0.601(3) 0.764(4) 0.1786(19) 0.092(12) Uiso 0.266(8) 1 d P A 2 H19D H 0.6450 0.8380 0.1894 0.138 Uiso 0.266(8) 1 calc PR A 2 H19E H 0.5783 0.7750 0.1362 0.138 Uiso 0.266(8) 1 calc PR A 2 H19F H 0.6348 0.6765 0.1826 0.138 Uiso 0.266(8) 1 calc PR A 2 C20A C 0.158(3) 0.406(4) 0.2159(18) 0.080(11) Uiso 0.266(8) 1 d P A 2 H20D H 0.1121 0.3316 0.2112 0.120 Uiso 0.266(8) 1 calc PR A 2 H20E H 0.1302 0.4902 0.1996 0.120 Uiso 0.266(8) 1 calc PR A 2 H20F H 0.1743 0.4182 0.2594 0.120 Uiso 0.266(8) 1 calc PR A 2 O3A O 0.5241(12) 0.7654(18) 0.2174(9) 0.074(7) Uani 0.266(8) 1 d PD A 2 O4A O 0.2500(13) 0.3717(19) 0.1805(10) 0.096(9) Uani 0.266(8) 1 d PD A 2 C18 C 0.3523(6) 0.7536(9) 0.2966(4) 0.075(3) Uani 1 1 d . A . H18A H 0.4118 0.7716 0.3205 0.090 Uiso 1 1 calc R C 1 H18B H 0.3053 0.7127 0.3248 0.090 Uiso 1 1 calc R C 1 O1 O 0.1897(3) 0.9263(5) -0.06943(19) 0.0520(12) Uani 1 1 d . . . O2 O -0.0099(3) 0.7942(4) 0.13932(18) 0.0473(11) Uani 1 1 d . . . C3S C 0.5056(7) 1.0302(9) 0.0609(4) 0.072(2) Uani 1 1 d . . . H3SA H 0.5105 1.0522 0.1032 0.086 Uiso 1 1 calc R . . C2S C 0.4377(5) 0.9395(9) 0.0411(4) 0.065(2) Uani 1 1 d . . . C1S C 0.3708(7) 0.8748(12) 0.0860(5) 0.114(4) Uani 1 1 d . . . H1SA H 0.3272 0.8128 0.0642 0.170 Uiso 1 1 calc R . . H1SB H 0.3336 0.9456 0.1065 0.170 Uiso 1 1 calc R . . H1SC H 0.4082 0.8237 0.1167 0.170 Uiso 1 1 calc R . . C4S C 0.5668(6) 1.0898(8) 0.0201(5) 0.074(3) Uani 1 1 d . . . H4SA H 0.6133 1.1529 0.0347 0.089 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 As1 0.0510(4) 0.0537(4) 0.0384(4) -0.0115(3) -0.0085(3) 0.0091(4) Cl1 0.0958(17) 0.0486(11) 0.0801(14) 0.0101(10) 0.0008(12) -0.0118(11) As2 0.0444(14) 0.0408(18) 0.0318(13) -0.0120(8) -0.0044(9) 0.0023(10) Cl2 0.060(3) 0.065(3) 0.0327(19) 0.0035(14) 0.0013(17) -0.0005(18) As2A 0.081(7) 0.095(6) 0.043(6) -0.030(4) -0.022(5) 0.034(4) Cl2A 0.13(2) 0.168(15) 0.055(6) 0.003(6) 0.011(9) 0.025(12) S1 0.0618(12) 0.0542(10) 0.0383(9) -0.0064(8) 0.0049(8) 0.0015(9) S2 0.0825(15) 0.0494(11) 0.0506(10) -0.0162(8) -0.0119(10) -0.0042(10) S3 0.0690(15) 0.148(2) 0.0578(12) -0.0373(14) -0.0161(11) 0.0512(16) S4 0.0795(16) 0.0827(16) 0.1023(18) -0.0526(14) -0.0450(14) 0.0199(13) C1 0.053(4) 0.053(4) 0.034(3) -0.004(3) -0.005(3) -0.004(3) C2 0.048(4) 0.043(4) 0.031(3) -0.001(3) -0.013(3) 0.002(3) C3 0.045(4) 0.046(4) 0.034(3) 0.005(3) -0.008(3) 0.001(3) C4 0.041(4) 0.028(3) 0.047(3) 0.006(3) -0.011(3) -0.001(3) C5 0.042(4) 0.036(3) 0.041(3) -0.002(3) -0.010(3) 0.006(3) C6 0.040(3) 0.036(3) 0.036(3) 0.005(2) -0.007(3) 0.000(3) C7 0.045(4) 0.036(3) 0.037(3) -0.001(3) -0.014(3) -0.003(3) C8 0.058(4) 0.037(4) 0.051(4) -0.006(3) -0.001(3) 0.006(3) C9 0.066(5) 0.062(5) 0.056(4) 0.014(4) -0.001(4) -0.010(4) C10 0.074(5) 0.047(4) 0.052(4) 0.006(3) 0.012(4) -0.011(4) C11 0.085(6) 0.076(6) 0.072(5) -0.023(5) -0.027(5) 0.035(5) C12 0.053(4) 0.049(4) 0.048(4) -0.003(3) -0.017(3) 0.012(4) C13 0.041(4) 0.061(5) 0.048(4) 0.001(3) -0.008(3) 0.009(3) C14 0.044(4) 0.052(4) 0.056(4) 0.001(3) -0.017(3) 0.000(3) C15 0.049(4) 0.066(5) 0.037(3) -0.007(3) -0.013(3) 0.011(4) C16 0.042(4) 0.081(5) 0.038(3) 0.015(4) -0.004(3) 0.002(4) C17 0.062(5) 0.051(4) 0.052(4) 0.010(3) -0.021(4) -0.014(4) C19 0.047(6) 0.059(7) 0.097(9) 0.018(6) 0.010(6) 0.002(5) C20 0.062(7) 0.098(10) 0.054(7) -0.017(6) 0.018(5) -0.038(7) O3 0.038(4) 0.070(5) 0.064(4) -0.002(4) 0.003(3) 0.007(3) O4 0.057(4) 0.073(5) 0.046(4) -0.010(3) 0.012(3) -0.010(4) C12A 0.053(4) 0.049(4) 0.048(4) -0.003(3) -0.017(3) 0.012(4) C13A 0.041(4) 0.061(5) 0.048(4) 0.001(3) -0.008(3) 0.009(3) C14A 0.044(4) 0.052(4) 0.056(4) 0.001(3) -0.017(3) 0.000(3) C15A 0.049(4) 0.066(5) 0.037(3) -0.007(3) -0.013(3) 0.011(4) C16A 0.042(4) 0.081(5) 0.038(3) 0.015(4) -0.004(3) 0.002(4) C17A 0.062(5) 0.051(4) 0.052(4) 0.010(3) -0.021(4) -0.014(4) O3A 0.071(15) 0.072(15) 0.078(14) -0.016(11) -0.018(12) -0.019(12) O4A 0.084(18) 0.072(16) 0.13(2) 0.002(15) -0.043(16) 0.007(13) C18 0.064(5) 0.103(7) 0.058(5) -0.031(5) -0.026(4) 0.018(5) O1 0.065(3) 0.055(3) 0.037(2) 0.007(2) -0.002(2) -0.008(2) O2 0.062(3) 0.043(3) 0.036(2) -0.0031(19) 0.004(2) -0.004(2) C3S 0.083(6) 0.063(5) 0.069(5) -0.001(4) -0.008(5) 0.012(5) C2S 0.043(4) 0.065(5) 0.086(6) 0.023(5) -0.005(4) 0.008(4) C1S 0.072(7) 0.133(10) 0.136(10) 0.054(8) -0.006(6) -0.007(7) C4S 0.067(6) 0.053(5) 0.103(7) -0.001(5) -0.029(5) -0.009(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 As1 S3 2.199(2) . ? As1 S1 2.2140(18) . ? As1 Cl1 2.246(2) . ? As2 S4 2.218(5) . ? As2 Cl2 2.235(7) . ? As2 S2 2.245(5) . ? As2A S2 2.105(19) . ? As2A S4 2.177(13) . ? As2A Cl2A 2.24(2) . ? S1 C1 1.825(7) . ? S2 C8 1.836(7) . ? S3 C11 1.813(8) . ? S4 C18 1.819(9) . ? C1 C2 1.487(8) . ? C2 C7 1.386(8) . ? C2 C3 1.395(9) . ? C3 O1 1.378(7) . ? C3 C4 1.382(8) . ? C4 C5 1.391(8) . ? C5 C6 1.388(8) . ? C5 C8 1.489(8) . ? C6 O2 1.377(7) . ? C6 C7 1.389(8) . ? C9 O1 1.431(8) . ? C10 O2 1.436(8) . ? C11 C12 1.504(10) . ? C12 C17 1.354(10) . ? C12 C13 1.384(10) . ? C13 C14 1.394(9) . ? C13 O3 1.399(9) . ? C14 C15 1.367(9) . ? C15 C16 1.371(10) . ? C15 C18 1.510(10) . ? C16 O4 1.375(9) . ? C16 C17 1.388(10) . ? C19 O3 1.424(13) . ? C20 O4 1.430(12) . ? C19A O3A 1.38(4) . ? C20A O4A 1.54(4) . ? C3S C2S 1.366(12) . ? C3S C4S 1.373(12) . ? C2S C4S 1.365(12) 3_675 ? C2S C1S 1.504(12) . ? C4S C2S 1.365(12) 3_675 ? 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 S3 As1 S1 87.80(8) . . ? S3 As1 Cl1 103.22(11) . . ? S1 As1 Cl1 100.27(8) . . ? S4 As2 Cl2 102.8(3) . . ? S4 As2 S2 87.58(16) . . ? Cl2 As2 S2 101.8(2) . . ? S2 As2A S4 92.3(7) . . ? S2 As2A Cl2A 99.9(8) . . ? S4 As2A Cl2A 86.7(18) . . ? C1 S1 As1 100.1(2) . . ? C8 S2 As2A 103.7(4) . . ? C8 S2 As2 103.0(3) . . ? As2A S2 As2 9.3(10) . . ? C11 S3 As1 102.4(3) . . ? C18 S4 As2A 105.6(6) . . ? C18 S4 As2 101.7(3) . . ? As2A S4 As2 9.8(10) . . ? C2 C1 S1 114.5(4) . . ? C7 C2 C3 118.4(6) . . ? C7 C2 C1 120.2(6) . . ? C3 C2 C1 121.4(6) . . ? O1 C3 C4 123.9(6) . . ? O1 C3 C2 115.4(6) . . ? C4 C3 C2 120.6(6) . . ? C3 C4 C5 120.6(6) . . ? C6 C5 C4 119.2(6) . . ? C6 C5 C8 120.5(6) . . ? C4 C5 C8 120.3(6) . . ? O2 C6 C5 116.3(5) . . ? O2 C6 C7 123.8(5) . . ? C5 C6 C7 119.9(6) . . ? C2 C7 C6 121.3(6) . . ? C5 C8 S2 114.0(5) . . ? C12 C11 S3 116.2(5) . . ? C17 C12 C13 118.4(7) . . ? C17 C12 C11 122.1(7) . . ? C13 C12 C11 119.5(7) . . ? C12 C13 C14 120.0(7) . . ? C12 C13 O3 120.5(7) . . ? C14 C13 O3 119.5(7) . . ? C15 C14 C13 120.8(7) . . ? C14 C15 C16 119.0(7) . . ? C14 C15 C18 121.5(7) . . ? C16 C15 C18 119.4(7) . . ? C15 C16 O4 121.8(7) . . ? C15 C16 C17 119.8(7) . . ? O4 C16 C17 118.4(7) . . ? C12 C17 C16 121.9(7) . . ? C13 O3 C19 119.7(8) . . ? C16 O4 C20 120.5(7) . . ? C15 C18 S4 114.3(5) . . ? C3 O1 C9 116.9(5) . . ? C6 O2 C10 117.8(5) . . ? C2S C3S C4S 120.5(8) . . ? C4S C2S C3S 117.9(8) 3_675 . ? C4S C2S C1S 121.9(9) 3_675 . ? C3S C2S C1S 120.2(9) . . ? C2S C4S C3S 121.6(8) 3_675 . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.037 _refine_diff_density_min -1.096 _refine_diff_density_rms 0.098 ###end data_gr17 _database_code_depnum_ccdc_archive 'CCDC 676185' _audit_creation_method SHELXLTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23.50 H28 As2 Cl2 O4 S4' _chemical_formula_weight 723.44 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' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 13.8813(13) _cell_length_b 9.8378(9) _cell_length_c 21.764(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.202(2) _cell_angle_gamma 90.00 _cell_volume 2972.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6716 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 27.92 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.617 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1460 _exptl_absorpt_coefficient_mu 2.738 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4745 _exptl_absorpt_correction_T_max 0.6385 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33472 _diffrn_reflns_av_R_equivalents 0.0186 _diffrn_reflns_av_sigmaI/netI 0.0243 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 0.94 _diffrn_reflns_theta_max 27.00 _reflns_number_total 12933 _reflns_number_gt 10744 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0867P)^2^+3.5818P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.302(14) _refine_ls_number_reflns 12933 _refine_ls_number_parameters 643 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0615 _refine_ls_R_factor_gt 0.0516 _refine_ls_wR_factor_ref 0.1550 _refine_ls_wR_factor_gt 0.1469 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group As1 As 0.76106(4) 0.74835(7) -0.70643(3) 0.04700(18) Uani 1 1 d . . . As2 As 0.68300(7) 1.06376(9) -0.54191(4) 0.0502(2) Uani 0.8797(19) 1 d P A 1 Cl2 Cl 0.57343(18) 1.0314(3) -0.46855(9) 0.0725(7) Uani 0.8797(19) 1 d P A 1 S2 S 0.80801(19) 1.1285(3) -0.48514(13) 0.0794(8) Uani 0.8797(19) 1 d P A 1 S3 S 0.6589(2) 1.2826(3) -0.56650(12) 0.0608(7) Uani 0.8797(19) 1 d P A 1 C8 C 0.8501(5) 0.9542(7) -0.4543(3) 0.0545(11) Uani 0.8797(19) 1 d P A 1 H8A H 0.9073 0.9664 -0.4276 0.065 Uiso 0.8797(19) 1 calc PR A 1 H8B H 0.7983 0.9125 -0.4295 0.065 Uiso 0.8797(19) 1 calc PR A 1 C11 C 0.5572(5) 1.2691(8) -0.6218(3) 0.0545(11) Uani 0.8797(19) 1 d P A 1 H11A H 0.4981 1.2434 -0.5992 0.065 Uiso 0.8797(19) 1 calc PR A 1 H11B H 0.5459 1.3591 -0.6408 0.065 Uiso 0.8797(19) 1 calc PR A 1 As2A As 0.7203(5) 1.1035(8) -0.5594(3) 0.0502(2) Uani 0.1203(19) 1 d PD A 2 Cl2A Cl 0.8513(11) 1.2524(17) -0.5555(6) 0.0725(7) Uani 0.1203(19) 1 d PD A 2 S2A S 0.7232(13) 1.0684(18) -0.4627(9) 0.0794(8) Uani 0.1203(19) 1 d P A 2 S3A S 0.6276(17) 1.274(2) -0.5511(10) 0.0608(7) Uani 0.1203(19) 1 d P A 2 C8A C 0.8501(5) 0.9542(7) -0.4543(3) 0.0545(11) Uani 0.1203(19) 1 d P A 2 H8AA H 0.9044 1.0180 -0.4480 0.065 Uiso 0.1203(19) 1 calc PR A 2 H8AB H 0.8451 0.8977 -0.4168 0.065 Uiso 0.1203(19) 1 calc PR A 2 C11A C 0.5572(5) 1.2691(8) -0.6218(3) 0.0545(11) Uani 0.1203(19) 1 d P A 2 H11C H 0.4890 1.2588 -0.6096 0.065 Uiso 0.1203(19) 1 calc PR A 2 H11D H 0.5631 1.3599 -0.6410 0.065 Uiso 0.1203(19) 1 calc PR A 2 Cl1 Cl 0.65085(16) 0.5823(2) -0.69719(10) 0.0740(6) Uani 1 1 d . . . S1 S 0.89435(14) 0.6354(3) -0.72648(9) 0.0776(7) Uani 1 1 d . . . S4 S 0.74999(14) 0.7928(3) -0.80591(8) 0.0587(5) Uani 1 1 d . A . O1 O 1.0590(4) 0.7944(8) -0.6235(3) 0.0667(18) Uani 0.843(5) 1 d P B 1 O2 O 0.7266(5) 0.7505(10) -0.4851(2) 0.0702(18) Uani 0.843(5) 1 d P A 1 C9 C 1.1246(6) 0.9064(10) -0.6118(5) 0.069(3) Uani 0.843(5) 1 d P B 1 C10 C 0.6570(6) 0.6480(14) -0.5023(5) 0.076(3) Uani 0.843(5) 1 d P A 1 O1A O 1.040(2) 0.970(4) -0.5413(15) 0.0667(18) Uani 0.157(5) 1 d PD A 2 O2A O 0.7612(16) 0.577(3) -0.5774(11) 0.0702(18) Uani 0.157(5) 1 d PD A 2 C9A C 1.106(3) 0.976(5) -0.591(2) 0.069(3) Uani 0.157(5) 1 d PD A 2 C10A C 0.671(2) 0.603(6) -0.546(2) 0.076(3) Uani 0.157(5) 1 d PD A 2 O3 O 0.4897(4) 1.0076(5) -0.6110(2) 0.0522(12) Uani 1 1 d . . . O4 O 0.6937(4) 1.1281(7) -0.8198(2) 0.0607(14) Uani 1 1 d . A . C1 C 0.9338(6) 0.5804(11) -0.6497(3) 0.069(2) Uani 1 1 d . . . H1A H 0.9010 0.4939 -0.6396 0.083 Uiso 1 1 calc R . . H1B H 1.0039 0.5619 -0.6509 0.083 Uiso 1 1 calc R . . C2 C 0.9144(5) 0.6811(10) -0.5992(3) 0.0544(18) Uani 1 1 d D A . C3 C 0.9770(4) 0.7857(8) -0.5871(3) 0.0488(16) Uani 1 1 d . . . C4 C 0.9595(5) 0.8765(10) -0.5398(4) 0.060(2) Uani 1 1 d . A . C5 C 0.8739(5) 0.8662(9) -0.5050(3) 0.0518(17) Uani 1 1 d . . . C6 C 0.8110(5) 0.7563(10) -0.5170(3) 0.0570(19) Uani 1 1 d D A . C7 C 0.8306(5) 0.6707(9) -0.5647(3) 0.0562(19) Uani 1 1 d . . . C12 C 0.5750(4) 1.1689(8) -0.6703(3) 0.0454(15) Uani 1 1 d . . . C13 C 0.5399(4) 1.0329(7) -0.6645(3) 0.0428(15) Uani 1 1 d . A . C14 C 0.5574(4) 0.9361(8) -0.7094(3) 0.0438(15) Uani 1 1 d . . . H14A H 0.5333 0.8463 -0.7048 0.053 Uiso 1 1 calc R A . C15 C 0.6102(4) 0.9708(8) -0.7611(3) 0.0428(15) Uani 1 1 d . A . C16 C 0.6442(4) 1.1031(8) -0.7683(3) 0.0441(15) Uani 1 1 d . . . C17 C 0.6274(4) 1.1997(7) -0.7225(3) 0.0433(15) Uani 1 1 d . A . H17A H 0.6525 1.2888 -0.7273 0.052 Uiso 1 1 calc R . . C18 C 0.6282(5) 0.8667(9) -0.8083(3) 0.0508(17) Uani 1 1 d . . . H18A H 0.6176 0.9077 -0.8493 0.061 Uiso 1 1 calc R A . H18B H 0.5806 0.7926 -0.8032 0.061 Uiso 1 1 calc R . . C19 C 0.4563(6) 0.8673(10) -0.6013(4) 0.065(2) Uani 1 1 d . . . H19A H 0.4208 0.8620 -0.5625 0.097 Uiso 1 1 calc R . . H19B H 0.5119 0.8060 -0.5996 0.097 Uiso 1 1 calc R . . H19C H 0.4139 0.8405 -0.6353 0.097 Uiso 1 1 calc R . . C20 C 0.7260(6) 1.2637(12) -0.8286(4) 0.073(3) Uani 1 1 d . . . H20A H 0.7600 1.2703 -0.8679 0.109 Uiso 1 1 calc R A . H20B H 0.7698 1.2889 -0.7951 0.109 Uiso 1 1 calc R . . H20C H 0.6706 1.3253 -0.8289 0.109 Uiso 1 1 calc R . . As3 As 0.75368(4) 1.16817(7) -0.20515(3) 0.04905(19) Uani 1 1 d . . . As4 As 0.68736(9) 0.84175(11) -0.04520(5) 0.0672(4) Uani 0.915(2) 1 d P C 1 Cl4 Cl 0.5818(2) 0.8827(3) 0.03063(10) 0.0892(9) Uani 0.915(2) 1 d P C 1 S6 S 0.8130(2) 0.7704(4) 0.00841(17) 0.1225(16) Uani 0.915(2) 1 d P C 1 S7 S 0.65690(19) 0.6277(3) -0.06734(10) 0.0674(6) Uani 0.915(2) 1 d P C 1 C28 C 0.8594(6) 0.9154(8) 0.0388(3) 0.0693(15) Uani 0.915(2) 1 d P C 1 H28A H 0.8153 0.9469 0.0715 0.083 Uiso 0.915(2) 1 calc PR C 1 H28B H 0.9216 0.8926 0.0586 0.083 Uiso 0.915(2) 1 calc PR C 1 C31 C 0.5547(6) 0.6418(10) -0.1206(4) 0.0693(15) Uani 0.915(2) 1 d P C 1 H31A H 0.5440 0.5526 -0.1407 0.083 Uiso 0.915(2) 1 calc PR C 1 H31B H 0.4960 0.6646 -0.0971 0.083 Uiso 0.915(2) 1 calc PR C 1 As4A As 0.7281(9) 0.8131(15) -0.0622(6) 0.0672(4) Uani 0.085(2) 1 d PD C 2 Cl4A Cl 0.8535(18) 0.670(3) -0.0744(10) 0.0892(9) Uani 0.085(2) 1 d PD C 2 S6A S 0.719(2) 0.881(4) 0.0307(18) 0.1225(16) Uani 0.085(2) 1 d P C 2 S7A S 0.5956(18) 0.676(2) -0.0412(10) 0.0674(6) Uani 0.085(2) 1 d P C 2 C28A C 0.8594(6) 0.9154(8) 0.0388(3) 0.0693(15) Uani 0.085(2) 1 d P C 2 H28C H 0.8767 0.9404 0.0815 0.083 Uiso 0.085(2) 1 calc PR C 2 H28D H 0.8972 0.8346 0.0265 0.083 Uiso 0.085(2) 1 calc PR C 2 C31A C 0.5547(6) 0.6418(10) -0.1206(4) 0.0693(15) Uani 0.085(2) 1 d P C 2 H31C H 0.5870 0.5575 -0.1345 0.083 Uiso 0.085(2) 1 calc PR C 2 H31D H 0.4848 0.6222 -0.1191 0.083 Uiso 0.085(2) 1 calc PR C 2 Cl3 Cl 0.64024(16) 1.3305(2) -0.19935(11) 0.0727(6) Uani 1 1 d . . . S5 S 0.88386(16) 1.2874(4) -0.22350(11) 0.1022(12) Uani 1 1 d . . . S8 S 0.74501(13) 1.1222(2) -0.30452(8) 0.0554(5) Uani 1 1 d . C . O5 O 1.0573(5) 1.1231(11) -0.1224(4) 0.0610(19) Uani 0.619(5) 1 d P D 1 O6 O 0.7297(5) 1.1634(10) 0.0179(4) 0.0596(17) Uani 0.619(5) 1 d P C 1 C29 C 1.1160(9) 1.0038(19) -0.1148(6) 0.075(4) Uani 0.619(5) 1 d P D 1 C30 C 0.6568(12) 1.266(2) 0.0005(7) 0.085(5) Uani 0.619(5) 1 d P C 1 O5A O 1.0245(8) 0.9314(15) -0.0360(6) 0.0610(19) Uani 0.381(5) 1 d P C 2 O6A O 0.7432(8) 1.3174(12) -0.0590(6) 0.0596(17) Uani 0.381(5) 1 d PD C 2 C29A C 1.1178(14) 0.954(3) -0.0775(9) 0.075(4) Uani 0.381(5) 1 d P C 2 C30A C 0.650(2) 1.281(3) -0.0294(11) 0.085(5) Uani 0.381(5) 1 d P C 2 O7 O 0.4842(3) 0.9055(5) -0.1108(2) 0.0513(12) Uani 1 1 d . . . O8 O 0.6897(4) 0.7827(6) -0.3210(2) 0.0595(14) Uani 1 1 d . C . C21 C 0.9247(7) 1.3358(11) -0.1470(4) 0.097(4) Uani 1 1 d . . . H21A H 0.9949 1.3530 -0.1487 0.117 Uiso 1 1 calc R . . H21B H 0.8931 1.4226 -0.1358 0.117 Uiso 1 1 calc R . . C22 C 0.9062(5) 1.2360(8) -0.0972(4) 0.0592(19) Uani 1 1 d D C . C23 C 0.9734(5) 1.1331(11) -0.0868(3) 0.062(2) Uani 1 1 d . . . C24 C 0.9564(5) 1.0331(8) -0.0414(3) 0.0521(17) Uani 1 1 d . C . C25 C 0.8771(5) 1.0385(12) -0.0069(3) 0.064(2) Uani 1 1 d . . . C26 C 0.8100(6) 1.1374(11) -0.0169(4) 0.070(3) Uani 1 1 d D C . C27 C 0.8274(5) 1.2444(12) -0.0623(4) 0.065(2) Uani 1 1 d . . . C32 C 0.5702(4) 0.7487(8) -0.1697(3) 0.0419(14) Uani 1 1 d . . . C33 C 0.5350(4) 0.8778(8) -0.1629(3) 0.0429(15) Uani 1 1 d . C . C34 C 0.5513(4) 0.9718(7) -0.2088(3) 0.0418(14) Uani 1 1 d . . . H34A H 0.5251 1.0606 -0.2048 0.050 Uiso 1 1 calc R C . C35 C 0.6044(4) 0.9405(8) -0.2606(3) 0.0444(15) Uani 1 1 d . C . C36 C 0.6397(5) 0.8086(8) -0.2671(3) 0.0459(15) Uani 1 1 d . . . C37 C 0.6224(4) 0.7133(7) -0.2215(3) 0.0477(17) Uani 1 1 d . C . H37A H 0.6465 0.6234 -0.2258 0.057 Uiso 1 1 calc R . . C38 C 0.6249(5) 1.0472(9) -0.3088(3) 0.0529(18) Uani 1 1 d . . . H38A H 0.5767 1.1208 -0.3048 0.064 Uiso 1 1 calc R C . H38B H 0.6164 1.0058 -0.3499 0.064 Uiso 1 1 calc R . . C39 C 0.4490(6) 1.0374(8) -0.1022(4) 0.060(2) Uani 1 1 d . . . H39A H 0.4149 1.0423 -0.0629 0.091 Uiso 1 1 calc R . . H39B H 0.4046 1.0605 -0.1357 0.091 Uiso 1 1 calc R . . H39C H 0.5029 1.1018 -0.1019 0.091 Uiso 1 1 calc R . . C40 C 0.7289(6) 0.6494(9) -0.3302(4) 0.066(2) Uani 1 1 d . . . H40A H 0.7621 0.6460 -0.3698 0.099 Uiso 1 1 calc R C . H40B H 0.6767 0.5824 -0.3299 0.099 Uiso 1 1 calc R . . H40C H 0.7747 0.6287 -0.2971 0.099 Uiso 1 1 calc R . . C1S C 0.9597(12) 1.7797(19) -0.2937(5) 0.145(13) Uiso 0.50 1 d PG . . C2S C 1.0239(15) 1.710(2) -0.3312(5) 0.146(10) Uiso 0.50 1 d PG . . C3S C 1.0856(12) 1.614(2) -0.3060(7) 0.177(7) Uiso 0.50 1 d PG . . C4S C 1.0832(11) 1.5868(17) -0.2433(8) 0.131(9) Uiso 0.50 1 d PG . . C5S C 1.0190(10) 1.6564(15) -0.2058(5) 0.084(5) Uiso 0.50 1 d PG . . C6S C 0.9573(7) 1.7528(12) -0.2310(4) 0.093(6) Uiso 0.50 1 d PGD . . C7S C 0.8907(10) 1.8290(16) -0.1945(6) 0.078(4) Uiso 0.50 1 d PGD . . C1SA C 0.9696(9) 1.7639(14) -0.2780(4) 0.082(5) Uiso 0.50 1 d PG . . C2SA C 0.9085(9) 1.8184(14) -0.2339(6) 0.080(4) Uiso 0.50 1 d PG . . C3SA C 0.9170(9) 1.7781(15) -0.1729(5) 0.113(7) Uiso 0.50 1 d PG . . C4SA C 0.9865(10) 1.6834(16) -0.1560(4) 0.090(5) Uiso 0.50 1 d PG . . C5SA C 1.0475(9) 1.6289(14) -0.2001(5) 0.098(7) Uiso 0.50 1 d PG . . C6SA C 1.0391(8) 1.6692(13) -0.2611(5) 0.083(5) Uiso 0.50 1 d PGD . . C7SA C 1.0819(13) 1.624(2) -0.3135(6) 0.177(7) Uiso 0.50 1 d PGD . . 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 As1 0.0482(3) 0.0504(4) 0.0424(4) -0.0049(3) -0.0084(3) -0.0019(3) As2 0.0545(5) 0.0504(5) 0.0455(5) -0.0149(4) -0.0096(4) 0.0032(4) Cl2 0.0917(15) 0.0841(19) 0.0416(10) 0.0011(12) -0.0042(10) 0.0057(14) S2 0.0747(14) 0.0669(15) 0.0964(18) -0.0383(15) -0.0356(13) 0.0100(12) S3 0.0810(19) 0.0503(13) 0.0510(15) -0.0120(12) -0.0109(11) -0.0101(13) C8 0.070(3) 0.041(2) 0.053(3) 0.002(2) -0.008(2) -0.005(2) C11 0.070(3) 0.041(2) 0.053(3) 0.002(2) -0.008(2) -0.005(2) As2A 0.0545(5) 0.0504(5) 0.0455(5) -0.0149(4) -0.0096(4) 0.0032(4) Cl2A 0.0917(15) 0.0841(19) 0.0416(10) 0.0011(12) -0.0042(10) 0.0057(14) S2A 0.0747(14) 0.0669(15) 0.0964(18) -0.0383(15) -0.0356(13) 0.0100(12) S3A 0.0810(19) 0.0503(13) 0.0510(15) -0.0120(12) -0.0109(11) -0.0101(13) C8A 0.070(3) 0.041(2) 0.053(3) 0.002(2) -0.008(2) -0.005(2) C11A 0.070(3) 0.041(2) 0.053(3) 0.002(2) -0.008(2) -0.005(2) Cl1 0.0780(12) 0.0582(13) 0.0857(14) 0.0110(11) -0.0084(10) -0.0200(10) S1 0.0583(10) 0.123(2) 0.0511(10) -0.0132(13) -0.0101(8) 0.0254(12) S4 0.0664(11) 0.0671(14) 0.0427(9) 0.0050(10) 0.0045(8) 0.0014(9) O1 0.048(3) 0.070(5) 0.082(4) 0.000(4) 0.001(3) -0.003(3) O2 0.080(4) 0.092(5) 0.039(3) -0.008(3) 0.013(3) -0.016(4) C9 0.043(4) 0.040(5) 0.125(8) 0.007(5) 0.028(4) 0.001(4) C10 0.054(4) 0.100(9) 0.073(6) 0.005(6) 0.013(4) -0.034(5) O1A 0.048(3) 0.070(5) 0.082(4) 0.000(4) 0.001(3) -0.003(3) O2A 0.080(4) 0.092(5) 0.039(3) -0.008(3) 0.013(3) -0.016(4) C9A 0.043(4) 0.040(5) 0.125(8) 0.007(5) 0.028(4) 0.001(4) C10A 0.054(4) 0.100(9) 0.073(6) 0.005(6) 0.013(4) -0.034(5) O3 0.065(3) 0.045(3) 0.046(3) 0.005(2) 0.002(2) 0.001(2) O4 0.073(3) 0.063(4) 0.045(3) 0.013(3) -0.002(2) -0.018(3) C1 0.081(5) 0.070(6) 0.057(4) -0.002(4) -0.010(4) -0.003(4) C2 0.051(3) 0.065(5) 0.047(4) -0.010(4) -0.019(3) 0.010(4) C3 0.044(3) 0.049(4) 0.053(4) 0.007(3) -0.012(3) 0.001(3) C4 0.042(3) 0.061(5) 0.078(5) 0.007(5) -0.016(3) 0.004(3) C5 0.058(4) 0.055(4) 0.041(3) 0.000(3) -0.021(3) 0.001(3) C6 0.046(3) 0.080(5) 0.045(4) 0.016(4) -0.009(3) -0.009(4) C7 0.072(4) 0.050(4) 0.046(4) 0.013(4) -0.031(3) -0.017(4) C12 0.048(3) 0.036(3) 0.052(4) 0.001(3) -0.015(3) -0.004(3) C13 0.048(3) 0.039(4) 0.042(3) 0.007(3) -0.008(3) -0.005(3) C14 0.047(3) 0.035(3) 0.050(4) 0.000(3) -0.009(3) -0.004(3) C15 0.043(3) 0.050(4) 0.035(3) -0.006(3) -0.013(2) -0.001(3) C16 0.043(3) 0.050(4) 0.039(3) 0.012(3) -0.012(3) -0.005(3) C17 0.047(3) 0.039(4) 0.043(4) -0.004(3) -0.009(3) -0.007(3) C18 0.054(4) 0.055(5) 0.043(4) 0.002(4) -0.006(3) -0.005(3) C19 0.078(5) 0.061(5) 0.057(4) 0.008(4) 0.009(4) -0.012(4) C20 0.075(5) 0.094(8) 0.049(4) 0.011(5) -0.001(4) -0.023(5) As3 0.0493(4) 0.0544(5) 0.0434(4) 0.0135(3) -0.0111(3) -0.0073(3) As4 0.0689(7) 0.0740(7) 0.0586(6) 0.0332(6) -0.0254(5) -0.0228(6) Cl4 0.143(2) 0.0833(19) 0.0417(11) -0.0084(13) -0.0087(12) -0.0045(18) S6 0.0995(19) 0.121(3) 0.147(3) 0.093(3) -0.077(2) -0.0431(19) S7 0.0894(16) 0.0585(14) 0.0543(12) 0.0177(12) -0.0121(11) 0.0093(12) C28 0.083(3) 0.066(3) 0.059(3) 0.021(3) -0.022(3) -0.018(3) C31 0.083(3) 0.066(3) 0.059(3) 0.021(3) -0.022(3) -0.018(3) As4A 0.0689(7) 0.0740(7) 0.0586(6) 0.0332(6) -0.0254(5) -0.0228(6) Cl4A 0.143(2) 0.0833(19) 0.0417(11) -0.0084(13) -0.0087(12) -0.0045(18) S6A 0.0995(19) 0.121(3) 0.147(3) 0.093(3) -0.077(2) -0.0431(19) S7A 0.0894(16) 0.0585(14) 0.0543(12) 0.0177(12) -0.0121(11) 0.0093(12) C28A 0.083(3) 0.066(3) 0.059(3) 0.021(3) -0.022(3) -0.018(3) C31A 0.083(3) 0.066(3) 0.059(3) 0.021(3) -0.022(3) -0.018(3) Cl3 0.0811(13) 0.0483(11) 0.0887(15) -0.0179(11) 0.0056(11) 0.0030(10) S5 0.0657(12) 0.157(3) 0.0837(15) 0.0618(19) -0.0294(11) -0.0533(16) S8 0.0614(10) 0.0599(12) 0.0450(9) 0.0094(10) 0.0040(8) -0.0040(9) O5 0.049(3) 0.065(5) 0.070(4) 0.017(4) 0.000(3) 0.006(3) O6 0.055(3) 0.055(4) 0.069(4) 0.015(4) -0.002(3) 0.011(3) C29 0.059(5) 0.104(11) 0.061(7) 0.001(7) -0.010(6) 0.033(7) C30 0.088(7) 0.110(11) 0.059(9) 0.041(9) 0.028(8) 0.051(8) O5A 0.049(3) 0.065(5) 0.070(4) 0.017(4) 0.000(3) 0.006(3) O6A 0.055(3) 0.055(4) 0.069(4) 0.015(4) -0.002(3) 0.011(3) C29A 0.059(5) 0.104(11) 0.061(7) 0.001(7) -0.010(6) 0.033(7) C30A 0.088(7) 0.110(11) 0.059(9) 0.041(9) 0.028(8) 0.051(8) O7 0.063(3) 0.040(3) 0.050(3) 0.009(2) 0.002(2) 0.005(2) O8 0.070(3) 0.066(4) 0.043(3) -0.007(3) -0.005(2) 0.009(3) C21 0.108(7) 0.071(6) 0.112(7) 0.037(6) -0.074(6) -0.045(5) C22 0.067(4) 0.039(4) 0.070(5) -0.008(4) -0.030(4) 0.000(4) C23 0.048(4) 0.086(6) 0.051(4) 0.008(4) -0.011(3) -0.015(4) C24 0.060(4) 0.053(4) 0.043(3) 0.005(3) -0.022(3) 0.007(3) C25 0.056(4) 0.099(7) 0.038(4) 0.005(4) -0.016(3) -0.022(5) C26 0.059(4) 0.104(8) 0.048(4) -0.028(5) -0.010(3) -0.011(5) C27 0.054(4) 0.076(6) 0.065(5) -0.013(5) -0.017(3) 0.008(4) C32 0.047(3) 0.040(4) 0.038(3) 0.001(3) -0.009(2) -0.007(3) C33 0.043(3) 0.042(4) 0.043(3) 0.000(3) -0.011(3) -0.009(3) C34 0.048(3) 0.038(3) 0.039(3) -0.004(3) -0.017(3) 0.004(3) C35 0.046(3) 0.047(4) 0.040(3) -0.004(3) -0.018(3) 0.000(3) C36 0.051(3) 0.044(4) 0.042(3) -0.001(3) -0.011(3) -0.005(3) C37 0.049(3) 0.037(4) 0.057(4) -0.018(3) -0.016(3) 0.001(3) C38 0.062(4) 0.058(5) 0.038(3) 0.011(4) -0.015(3) 0.002(4) C39 0.085(5) 0.037(4) 0.060(4) -0.002(4) 0.021(4) -0.001(4) C40 0.073(5) 0.056(5) 0.068(5) -0.030(4) -0.011(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 As1 S1 2.203(2) . ? As1 S4 2.214(2) . ? As1 Cl1 2.248(2) . ? As2 S2 2.220(3) . ? As2 Cl2 2.232(3) . ? As2 S3 2.244(3) . ? S2 C8 1.931(7) . ? S3 C11 1.856(7) . ? C8 C5 1.442(10) . ? C11 C12 1.466(10) . ? As2A S3A 2.13(3) . ? As2A S2A 2.13(2) . ? As2A Cl2A 2.336(14) . ? S1 C1 1.838(8) . ? S4 C18 1.840(7) . ? O1 C3 1.392(8) . ? O1 C9 1.451(12) . ? O2 C6 1.367(9) . ? O2 C10 1.445(13) . ? O1A C9A 1.43(2) . ? O1A C4 1.44(3) . ? O2A C7 1.364(18) . ? O2A C10A 1.449(19) . ? O3 C13 1.383(8) . ? O3 C19 1.472(10) . ? O4 C16 1.340(7) . ? O4 C20 1.421(12) . ? C1 C2 1.505(11) . ? C2 C3 1.372(11) . ? C2 C7 1.390(10) . ? C3 C4 1.385(11) . ? C4 C5 1.414(10) . ? C5 C6 1.413(11) . ? C6 C7 1.365(12) . ? C12 C17 1.385(9) . ? C12 C13 1.429(10) . ? C13 C14 1.387(10) . ? C14 C15 1.387(9) . ? C15 C16 1.394(11) . ? C15 C18 1.471(10) . ? C16 C17 1.397(10) . ? As3 S5 2.192(2) . ? As3 S8 2.212(2) . ? As3 Cl3 2.247(2) . ? As4 S7 2.201(3) . ? As4 S6 2.209(3) . ? As4 Cl4 2.248(3) . ? S6 C28 1.698(9) . ? S7 C31 1.835(8) . ? C28 C25 1.586(12) . ? C31 C32 1.515(10) . ? As4A S6A 2.13(5) . ? As4A Cl4A 2.254(18) . ? As4A S7A 2.32(3) . ? S5 C21 1.821(9) . ? S8 C38 1.825(7) . ? O5 C23 1.405(10) . ? O5 C29 1.439(18) . ? O6 C26 1.374(11) . ? O6 C30 1.477(17) . ? O5A C24 1.381(15) . ? O5A C29A 1.60(2) . ? O6A C27 1.373(13) . ? O6A C30A 1.50(3) . ? O7 C33 1.364(8) . ? O7 C39 1.399(9) . ? O8 C36 1.389(8) . ? O8 C40 1.434(10) . ? C21 C22 1.485(12) . ? C22 C27 1.337(10) . ? C22 C23 1.394(12) . ? C23 C24 1.415(11) . ? C24 C25 1.337(10) . ? C25 C26 1.364(14) . ? C26 C27 1.464(14) . ? C32 C33 1.369(11) . ? C32 C37 1.387(9) . ? C33 C34 1.381(10) . ? C34 C35 1.384(9) . ? C35 C36 1.394(11) . ? C35 C38 1.511(10) . ? C36 C37 1.387(10) . ? C1S C2S 1.3900 . ? C1S C6S 1.3900 . ? C1S C2SA 1.533(15) . ? C1S C6SA 1.701(16) . ? C2S C7SA 1.23(2) . ? C2S C3S 1.3900 . ? C2S C1SA 1.481(14) . ? C2S C6SA 1.591(16) . ? C3S C6SA 1.293(13) . ? C3S C4S 1.3900 . ? C4S C6SA 1.086(16) . ? C4S C5SA 1.141(18) . ? C4S C7SA 1.57(2) . ? C4S C5S 1.3900 . ? C5S C6SA 1.242(15) . ? C5S C4SA 1.205(16) . ? C5S C6S 1.3900 . ? C5S C1SA 2.012(13) . ? C6S C2SA 0.937(12) . ? C6S C1SA 1.043(12) . ? C6S C3SA 1.407(12) . ? C6S C7S 1.4333 . ? C6S C6SA 1.549(12) . ? C6S C4SA 1.814(12) . ? C6S C5SA 1.872(12) . ? C7S C3SA 0.777(18) . ? C7S C2SA 0.900(16) . ? C7S C4SA 2.125(17) . ? C1SA C2SA 1.3900 . ? C1SA C6SA 1.3900 . ? C2SA C3SA 1.3900 . ? C3SA C4SA 1.3900 . ? C4SA C5SA 1.3900 . ? C5SA C6SA 1.3900 . ? C6SA C7SA 1.3613 . ? 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 S1 As1 S4 87.79(8) . . ? S1 As1 Cl1 102.93(11) . . ? S4 As1 Cl1 100.74(9) . . ? S2 As2 Cl2 100.14(11) . . ? S2 As2 S3 88.47(11) . . ? Cl2 As2 S3 101.88(11) . . ? C8 S2 As2 100.0(2) . . ? C11 S3 As2 101.4(3) . . ? C5 C8 S2 109.7(5) . . ? C12 C11 S3 112.7(5) . . ? S3A As2A S2A 93.0(8) . . ? S3A As2A Cl2A 88.4(8) . . ? S2A As2A Cl2A 93.1(6) . . ? C1 S1 As1 102.5(3) . . ? C18 S4 As1 99.5(2) . . ? C3 O1 C9 117.5(7) . . ? C6 O2 C10 118.1(7) . . ? C9A O1A C4 123(3) . . ? C7 O2A C10A 113(2) . . ? C13 O3 C19 116.7(6) . . ? C16 O4 C20 116.6(6) . . ? C2 C1 S1 114.6(7) . . ? C3 C2 C7 118.8(7) . . ? C3 C2 C1 121.3(7) . . ? C7 C2 C1 119.9(7) . . ? C4 C3 C2 120.9(6) . . ? C4 C3 O1 121.9(7) . . ? C2 C3 O1 117.1(7) . . ? C3 C4 O1A 104.9(14) . . ? C3 C4 C5 120.1(7) . . ? O1A C4 C5 135.0(15) . . ? C6 C5 C4 118.4(7) . . ? C6 C5 C8 117.3(7) . . ? C4 C5 C8 124.2(7) . . ? C7 C6 O2 122.3(7) . . ? C7 C6 C5 119.2(6) . . ? O2 C6 C5 117.9(8) . . ? C6 C7 O2A 115.5(10) . . ? C6 C7 C2 122.3(7) . . ? O2A C7 C2 122.1(11) . . ? C17 C12 C13 117.2(7) . . ? C17 C12 C11 122.3(6) . . ? C13 C12 C11 120.6(6) . . ? C14 C13 O3 124.1(6) . . ? C14 C13 C12 121.4(6) . . ? O3 C13 C12 114.5(6) . . ? C15 C14 C13 119.8(6) . . ? C14 C15 C16 120.0(7) . . ? C14 C15 C18 119.1(7) . . ? C16 C15 C18 120.9(6) . . ? O4 C16 C17 124.0(7) . . ? O4 C16 C15 116.1(7) . . ? C17 C16 C15 119.9(6) . . ? C16 C17 C12 121.8(6) . . ? C15 C18 S4 114.5(5) . . ? S5 As3 S8 88.47(9) . . ? S5 As3 Cl3 102.02(12) . . ? S8 As3 Cl3 99.47(9) . . ? S7 As4 S6 87.83(14) . . ? S7 As4 Cl4 101.94(12) . . ? S6 As4 Cl4 100.64(14) . . ? C28 S6 As4 103.7(3) . . ? C31 S7 As4 102.3(3) . . ? C25 C28 S6 117.2(5) . . ? C32 C31 S7 112.8(5) . . ? S6A As4A Cl4A 110.8(11) . . ? S6A As4A S7A 86.8(11) . . ? Cl4A As4A S7A 105.9(12) . . ? C21 S5 As3 103.1(3) . . ? C38 S8 As3 100.3(2) . . ? C23 O5 C29 117.7(9) . . ? C26 O6 C30 122.9(9) . . ? C24 O5A C29A 114.0(12) . . ? C27 O6A C30A 129.5(13) . . ? C33 O7 C39 118.7(6) . . ? C36 O8 C40 118.5(6) . . ? C22 C21 S5 116.1(6) . . ? C27 C22 C23 120.0(8) . . ? C27 C22 C21 121.2(9) . . ? C23 C22 C21 118.8(8) . . ? O5 C23 C22 121.1(8) . . ? O5 C23 C24 118.5(8) . . ? C22 C23 C24 120.4(7) . . ? C25 C24 O5A 123.1(9) . . ? C25 C24 C23 120.3(8) . . ? O5A C24 C23 116.6(8) . . ? C24 C25 C26 120.1(8) . . ? C24 C25 C28 116.8(9) . . ? C26 C25 C28 122.5(7) . . ? C25 C26 O6 126.8(9) . . ? C25 C26 C27 120.4(7) . . ? O6 C26 C27 112.0(8) . . ? C22 C27 O6A 139.4(10) . . ? C22 C27 C26 118.5(8) . . ? O6A C27 C26 101.5(7) . . ? C33 C32 C37 120.6(7) . . ? C33 C32 C31 121.1(7) . . ? C37 C32 C31 118.3(7) . . ? O7 C33 C32 117.5(6) . . ? O7 C33 C34 123.6(7) . . ? C32 C33 C34 118.9(6) . . ? C35 C34 C33 122.0(7) . . ? C36 C35 C34 118.5(7) . . ? C36 C35 C38 120.6(6) . . ? C34 C35 C38 120.8(7) . . ? C37 C36 C35 119.7(6) . . ? C37 C36 O8 124.6(7) . . ? C35 C36 O8 115.7(7) . . ? C32 C37 C36 120.2(7) . . ? C35 C38 S8 114.8(4) . . ? C2S C1S C6S 120.0 . . ? C2S C1S C2SA 157.0(5) . . ? C6S C1S C2SA 37.0(5) . . ? C2S C1S C6SA 61.0(5) . . ? C6S C1S C6SA 59.1(5) . . ? C2SA C1S C6SA 96.1(6) . . ? C7SA C2S C3S 5.2(8) . . ? C7SA C2S C1S 125.2(7) . . ? C3S C2S C1S 120.0 . . ? C7SA C2S C1SA 109.6(11) . . ? C3S C2S C1SA 104.5(5) . . ? C1S C2S C1SA 15.6(5) . . ? C7SA C2S C6SA 56.0(8) . . ? C3S C2S C6SA 50.9(5) . . ? C1S C2S C6SA 69.2(5) . . ? C1SA C2S C6SA 53.7(4) . . ? C6SA C3S C2S 72.6(7) . . ? C6SA C3S C4S 47.6(7) . . ? C2S C3S C4S 120.0 . . ? C6SA C4S C5SA 77.2(8) . . ? C6SA C4S C7SA 58.3(10) . . ? C5SA C4S C7SA 135.4(12) . . ? C6SA C4S C3S 61.5(7) . . ? C5SA C4S C3S 138.7(7) . . ? C7SA C4S C3S 3.3(7) . . ? C6SA C4S C5S 58.7(7) . . ? C5SA C4S C5S 19.6(7) . . ? C7SA C4S C5S 116.8(6) . . ? C3S C4S C5S 120.0 . . ? C6SA C5S C4SA 159.2(13) . . ? C6SA C5S C4S 48.3(7) . . ? C4SA C5S C4S 151.5(8) . . ? C6SA C5S C6S 71.9(6) . . ? C4SA C5S C6S 88.4(8) . . ? C4S C5S C6S 120.0 . . ? C6SA C5S C1SA 42.9(4) . . ? C4SA C5S C1SA 117.3(8) . . ? C4S C5S C1SA 91.0(4) . . ? C6S C5S C1SA 29.0(4) . . ? C2SA C6S C1SA 89.0(10) . . ? C2SA C6S C5S 160.2(10) . . ? C1SA C6S C5S 110.8(8) . . ? C2SA C6S C1S 79.8(10) . . ? C1SA C6S C1S 9.4(9) . . ? C5S C6S C1S 120.0 . . ? C2SA C6S C3SA 69.5(7) . . ? C1SA C6S C3SA 158.4(12) . . ? C5S C6S C3SA 90.7(7) . . ? C1S C6S C3SA 149.3(7) . . ? C2SA C6S C7S 37.8(10) . . ? C1SA C6S C7S 126.7(8) . . ? C5S C6S C7S 122.4 . . ? C1S C6S C7S 117.6 . . ? C3SA C6S C7S 31.7(7) . . ? C2SA C6S C6SA 150.2(12) . . ? C1SA C6S C6SA 61.2(6) . . ? C5S C6S C6SA 49.6(6) . . ? C1S C6S C6SA 70.5(6) . . ? C3SA C6S C6SA 140.2(9) . . ? C7S C6S C6SA 170.9(7) . . ? C2SA C6S C4SA 118.6(10) . . ? C1SA C6S C4SA 152.2(10) . . ? C5S C6S C4SA 41.6(6) . . ? C1S C6S C4SA 161.5(6) . . ? C3SA C6S C4SA 49.1(4) . . ? C7S C6S C4SA 80.8(6) . . ? C6SA C6S C4SA 91.1(6) . . ? C2SA C6S C5SA 162.8(11) . . ? C1SA C6S C5SA 108.0(9) . . ? C5S C6S C5SA 4.1(8) . . ? C1S C6S C5SA 117.3(6) . . ? C3SA C6S C5SA 93.4(6) . . ? C7S C6S C5SA 125.0(6) . . ? C6SA C6S C5SA 46.8(3) . . ? C4SA C6S C5SA 44.3(3) . . ? C3SA C7S C2SA 111.7(14) . . ? C3SA C7S C6S 72.3(9) . . ? C2SA C7S C6S 39.6(8) . . ? C3SA C7S C4SA 15.1(7) . . ? C2SA C7S C4SA 97.1(10) . . ? C6S C7S C4SA 57.5(4) . . ? C6S C1SA C2SA 42.4(7) . . ? C6S C1SA C6SA 77.7(7) . . ? C2SA C1SA C6SA 120.0 . . ? C6S C1SA C2S 144.5(13) . . ? C2SA C1SA C2S 172.1(10) . . ? C6SA C1SA C2S 67.2(9) . . ? C6S C1SA C5S 40.2(5) . . ? C2SA C1SA C5S 82.6(4) . . ? C6SA C1SA C5S 37.5(4) . . ? C2S C1SA C5S 104.4(8) . . ? C6S C2SA C7S 102.6(14) . . ? C6S C2SA C1SA 48.6(8) . . ? C7S C2SA C1SA 150.9(10) . . ? C6S C2SA C3SA 71.4(7) . . ? C7S C2SA C3SA 31.3(10) . . ? C1SA C2SA C3SA 120.0 . . ? C6S C2SA C1S 63.2(8) . . ? C7S C2SA C1S 165.5(13) . . ? C1SA C2SA C1S 14.7(6) . . ? C3SA C2SA C1S 134.6(6) . . ? C7S C3SA C4SA 156.5(10) . . ? C7S C3SA C2SA 37.0(10) . . ? C4SA C3SA C2SA 120.0 . . ? C7S C3SA C6S 76.0(10) . . ? C4SA C3SA C6S 80.9(5) . . ? C2SA C3SA C6S 39.1(5) . . ? C5S C4SA C5SA 20.4(6) . . ? C5S C4SA C3SA 99.9(6) . . ? C5SA C4SA C3SA 120.0 . . ? C5S C4SA C6S 50.0(4) . . ? C5SA C4SA C6S 70.0(4) . . ? C3SA C4SA C6S 50.0(4) . . ? C5S C4SA C7S 91.7(7) . . ? C5SA C4SA C7S 111.7(4) . . ? C3SA C4SA C7S 8.4(4) . . ? C6S C4SA C7S 41.7(3) . . ? C4S C5SA C4SA 167.3(12) . . ? C4S C5SA C6SA 49.6(9) . . ? C4SA C5SA C6SA 120.0 . . ? C4S C5SA C6S 103.4(10) . . ? C4SA C5SA C6S 65.7(4) . . ? C6SA C5SA C6S 54.3(4) . . ? C4S C6SA C5S 73.0(10) . . ? C4S C6SA C7SA 79.0(11) . . ? C5S C6SA C7SA 151.4(6) . . ? C4S C6SA C3S 70.9(7) . . ? C5S C6SA C3S 143.4(14) . . ? C7SA C6SA C3S 8.1(11) . . ? C4S C6SA C5SA 53.2(11) . . ? C5S C6SA C5SA 20.7(6) . . ? C7SA C6SA C5SA 132.2 . . ? C3S C6SA C5SA 124.1(11) . . ? C4S C6SA C1SA 169.9(14) . . ? C5S C6SA C1SA 99.6(6) . . ? C7SA C6SA C1SA 107.5 . . ? C3S C6SA C1SA 115.5(11) . . ? C5SA C6SA C1SA 120.0 . . ? C4S C6SA C6S 131.2(13) . . ? C5S C6SA C6S 58.5(5) . . ? C7SA C6SA C6S 148.1(5) . . ? C3S C6SA C6S 155.8(14) . . ? C5SA C6SA C6S 78.9(5) . . ? C1SA C6SA C6S 41.1(5) . . ? C4S C6SA C2S 127.2(10) . . ? C5S C6SA C2S 157.6(11) . . ? C7SA C6SA C2S 48.4(8) . . ? C3S C6SA C2S 56.5(6) . . ? C5SA C6SA C2S 176.7(15) . . ? C1SA C6SA C2S 59.1(7) . . ? C6S C6SA C2S 100.1(9) . . ? C4S C6SA C1S 171.5(19) . . ? C5S C6SA C1S 108.7(8) . . ? C7SA C6SA C1S 98.2(5) . . ? C3S C6SA C1S 106.2(10) . . ? C5SA C6SA C1S 129.3(5) . . ? C1SA C6SA C1S 9.3(5) . . ? C6S C6SA C1S 50.4(4) . . ? C2S C6SA C1S 49.8(5) . . ? C6SA C7SA C2S 75.6(6) . . ? C6SA C7SA C4S 42.7(5) . . ? C2S C7SA C4S 118.1(9) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.155 _refine_diff_density_min -0.772 _refine_diff_density_rms 0.095