# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Darren Johnson' _publ_contact_author_email DWJ@UOREGON.EDU _publ_section_title ; Three's Company: Co-crystallization of a Self-Assembled S4 Metallacyclophane with Two Diastereomeric Metallacycle Intermediates ; loop_ _publ_author_name 'Darren Johnson' 'Virginia M Cangelosi' 'Timothy G. Carter' 'Nathan R. Lindquist' 'Lev N. Zakharov' # Attachment 'nath1_AS4L2_revised.cif' data_nath1 _database_code_depnum_ccdc_archive 'CCDC 743840' #TrackingRef 'nath1_AS4L2_revised.cif' _audit_creation_method SHELXLTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H24 As4 Cl12 S8' _chemical_formula_weight 1293.99 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 17.9104(11) _cell_length_b 25.7564(16) _cell_length_c 18.9947(12) _cell_angle_alpha 90.00 _cell_angle_beta 93.0860(10) _cell_angle_gamma 90.00 _cell_volume 8749.7(9) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7355 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 27.33 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.965 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5056 _exptl_absorpt_coefficient_mu 4.166 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3491 _exptl_absorpt_correction_T_max 0.6348 _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 Bruker Apex' _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 97922 _diffrn_reflns_av_R_equivalents 0.0341 _diffrn_reflns_av_sigmaI/netI 0.0272 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 27.00 _reflns_number_total 19054 _reflns_number_gt 15435 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _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^)+(0.0717P)^2^+14.3914P] 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 19054 _refine_ls_number_parameters 757 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0579 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.1554 _refine_ls_wR_factor_gt 0.1486 _refine_ls_goodness_of_fit_ref 1.286 _refine_ls_restrained_S_all 1.286 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.500 0.000 448 162 2 0.000 0.000 0.500 448 161 3 0.500 0.500 0.500 369 161 4 0.500 0.000 1.000 369 161 _platon_squeeze_details ; In the crystal structure there are four solvent molecules, C2H2Cl4. Two of them are highly disordered and were treated by SQUEEZE [Van der Sluis,P. & Spek, A.L. (1990) Acta Cryst., Sect.A,A46,194-201.]. Corrections of the X-ray data by SQUEEZE (645 electron/cell); the required values (656 electron/cell) for eight solvent molecules in the full unit cell. ; 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 0.16273(3) 0.650674(19) 0.55249(3) 0.02529(12) Uani 1 1 d . . . As2 As 0.09130(3) 0.75752(2) 0.67079(3) 0.03033(13) Uani 1 1 d . . . As3 As -0.10497(3) 0.70886(2) 0.62410(3) 0.02811(12) Uani 1 1 d . . . As4 As -0.03479(3) 0.625109(19) 0.48465(3) 0.02453(12) Uani 1 1 d . . . Cl1 Cl 0.27639(7) 0.63992(6) 0.60617(8) 0.0393(3) Uani 1 1 d . . . Cl2 Cl 0.06176(10) 0.83155(7) 0.72318(10) 0.0576(4) Uani 1 1 d . . . Cl3 Cl -0.21413(7) 0.66808(6) 0.63258(7) 0.0383(3) Uani 1 1 d . . . Cl4 Cl -0.00895(8) 0.59749(5) 0.37747(7) 0.0385(3) Uani 1 1 d . . . S1 S 0.19163(7) 0.66969(5) 0.44339(7) 0.0289(3) Uani 1 1 d . . . S2 S 0.14125(7) 0.56810(5) 0.52230(7) 0.0272(3) Uani 1 1 d . . . S3 S 0.19274(7) 0.78480(6) 0.61822(7) 0.0319(3) Uani 1 1 d . . . S4 S 0.16350(8) 0.71938(6) 0.75401(7) 0.0358(3) Uani 1 1 d . . . S5 S -0.14252(8) 0.78994(6) 0.60314(8) 0.0359(3) Uani 1 1 d . . . S6 S -0.08463(8) 0.72771(6) 0.73817(7) 0.0362(3) Uani 1 1 d . . . S7 S -0.14067(7) 0.66658(5) 0.45278(7) 0.0272(3) Uani 1 1 d . . . S8 S -0.10119(7) 0.55993(5) 0.52545(6) 0.0276(3) Uani 1 1 d . . . C1 C 0.1757(3) 0.7400(2) 0.4422(3) 0.0277(10) Uani 1 1 d . . . H1A H 0.2114 0.7563 0.4770 0.033 Uiso 1 1 calc R . . H1B H 0.1869 0.7534 0.3950 0.033 Uiso 1 1 calc R . . C2 C 0.1455(3) 0.8241(2) 0.5478(3) 0.0310(11) Uani 1 1 d . . . H2A H 0.1242 0.8555 0.5691 0.037 Uiso 1 1 calc R . . H2B H 0.1830 0.8356 0.5147 0.037 Uiso 1 1 calc R . . C3 C -0.1283(3) 0.7969(2) 0.5078(3) 0.0300(11) Uani 1 1 d . . . H3A H -0.1651 0.7747 0.4812 0.036 Uiso 1 1 calc R . . H3B H -0.1385 0.8334 0.4938 0.036 Uiso 1 1 calc R . . C4 C -0.0998(3) 0.7155(2) 0.3968(3) 0.0266(10) Uani 1 1 d . . . H4A H -0.0794 0.6982 0.3554 0.032 Uiso 1 1 calc R . . H4B H -0.1393 0.7399 0.3795 0.032 Uiso 1 1 calc R . . C5 C 0.0978(3) 0.75639(19) 0.4580(3) 0.0251(10) Uani 1 1 d . . . C6 C 0.0844(3) 0.79542(18) 0.5074(3) 0.0245(10) Uani 1 1 d . . . C7 C 0.0103(3) 0.8075(2) 0.5218(3) 0.0306(11) Uani 1 1 d . . . H7A H 0.0013 0.8333 0.5560 0.037 Uiso 1 1 calc R . . C8 C -0.0509(3) 0.7826(2) 0.4871(3) 0.0270(10) Uani 1 1 d . . . C9 C -0.0377(3) 0.74562(19) 0.4361(3) 0.0259(10) Uani 1 1 d . . . C10 C 0.0362(3) 0.73305(19) 0.4224(3) 0.0256(10) Uani 1 1 d . . . H10A H 0.0448 0.7076 0.3875 0.031 Uiso 1 1 calc R . . C11 C 0.1347(3) 0.5416(2) 0.6112(3) 0.0301(11) Uani 1 1 d . . . H11A H 0.1199 0.5047 0.6077 0.036 Uiso 1 1 calc R . . H11B H 0.1846 0.5433 0.6362 0.036 Uiso 1 1 calc R . . C12 C 0.0945(3) 0.6768(2) 0.7930(3) 0.0299(11) Uani 1 1 d . . . H12C H 0.1191 0.6584 0.8337 0.036 Uiso 1 1 calc R . . H12D H 0.0542 0.6985 0.8110 0.036 Uiso 1 1 calc R . . C13 C -0.0736(3) 0.6617(2) 0.7722(3) 0.0357(12) Uani 1 1 d . . . H13A H -0.0568 0.6633 0.8227 0.043 Uiso 1 1 calc R . . H13B H -0.1227 0.6440 0.7687 0.043 Uiso 1 1 calc R . . C14 C -0.0329(3) 0.52878(19) 0.5884(3) 0.0289(11) Uani 1 1 d . . . H14C H -0.0584 0.5005 0.6130 0.035 Uiso 1 1 calc R . . H14D H 0.0071 0.5129 0.5617 0.035 Uiso 1 1 calc R . . C15 C 0.0796(3) 0.57015(19) 0.6536(3) 0.0265(10) Uani 1 1 d . . . C16 C 0.1067(3) 0.6059(2) 0.7047(3) 0.0292(11) Uani 1 1 d . . . H16A H 0.1592 0.6090 0.7136 0.035 Uiso 1 1 calc R . . C17 C 0.0600(3) 0.6370(2) 0.7426(2) 0.0278(10) Uani 1 1 d . . . C18 C -0.0176(3) 0.6299(2) 0.7327(3) 0.0306(11) Uani 1 1 d . . . C19 C -0.0448(3) 0.5939(2) 0.6843(2) 0.0274(10) Uani 1 1 d . . . H19A H -0.0973 0.5884 0.6790 0.033 Uiso 1 1 calc R . . C20 C 0.0023(3) 0.56494(19) 0.6426(3) 0.0277(10) Uani 1 1 d . . . As1' As 0.46115(3) 0.74556(2) 0.31756(3) 0.02818(12) Uani 1 1 d . . . As2' As 0.65253(3) 0.80050(2) 0.36945(3) 0.02713(12) Uani 1 1 d . . . As3' As 0.57230(3) 0.877894(19) 0.50882(3) 0.02384(12) Uani 1 1 d . . . As4' As 0.38148(3) 0.845133(19) 0.43631(3) 0.02373(12) Uani 1 1 d . . . Cl1' Cl 0.49941(9) 0.67256(6) 0.26659(8) 0.0445(3) Uani 1 1 d . . . Cl2' Cl 0.75946(7) 0.84526(6) 0.36556(7) 0.0380(3) Uani 1 1 d . . . Cl3' Cl 0.53658(7) 0.90395(5) 0.61466(6) 0.0322(3) Uani 1 1 d . . . Cl4' Cl 0.26886(7) 0.85193(6) 0.37918(7) 0.0387(3) Uani 1 1 d . . . S1' S 0.38955(8) 0.78123(5) 0.23157(7) 0.0328(3) Uani 1 1 d . . . S2' S 0.35980(7) 0.71460(6) 0.36637(7) 0.0315(3) Uani 1 1 d . . . S3' S 0.63693(7) 0.78255(5) 0.25463(7) 0.0318(3) Uani 1 1 d . . . S4' S 0.69418(7) 0.72020(6) 0.38854(7) 0.0334(3) Uani 1 1 d . . . S5' S 0.63407(7) 0.94654(5) 0.47236(6) 0.0271(3) Uani 1 1 d . . . S6' S 0.68024(7) 0.84086(5) 0.54600(7) 0.0283(3) Uani 1 1 d . . . S7' S 0.39241(7) 0.92810(5) 0.46843(6) 0.0259(2) Uani 1 1 d . . . S8' S 0.35045(7) 0.82434(5) 0.54411(7) 0.0269(3) Uani 1 1 d . . . C1' C 0.4552(3) 0.8272(2) 0.1958(3) 0.0294(11) Uani 1 1 d . . . H1'A H 0.4978 0.8076 0.1779 0.035 Uiso 1 1 calc R . . H1'B H 0.4300 0.8454 0.1553 0.035 Uiso 1 1 calc R . . C2' C 0.6213(3) 0.8492(2) 0.2216(3) 0.0309(11) Uani 1 1 d . . . H2'A H 0.6688 0.8689 0.2271 0.037 Uiso 1 1 calc R . . H2'B H 0.6065 0.8478 0.1707 0.037 Uiso 1 1 calc R . . C3' C 0.5645(3) 0.97611(18) 0.4091(3) 0.0258(10) Uani 1 1 d . . . H3'A H 0.5220 0.9891 0.4353 0.031 Uiso 1 1 calc R . . H3'B H 0.5876 1.0063 0.3866 0.031 Uiso 1 1 calc R . . C4' C 0.3989(3) 0.95676(19) 0.3804(3) 0.0263(10) Uani 1 1 d . . . H4'A H 0.3498 0.9536 0.3542 0.032 Uiso 1 1 calc R . . H4'B H 0.4106 0.9942 0.3854 0.032 Uiso 1 1 calc R . . C5' C 0.4853(3) 0.86712(19) 0.2477(2) 0.0253(10) Uani 1 1 d . . . C6' C 0.5625(3) 0.87716(19) 0.2593(2) 0.0250(10) Uani 1 1 d . . . C7' C 0.5848(3) 0.91328(19) 0.3111(2) 0.0264(10) Uani 1 1 d . . . H7'A H 0.6367 0.9204 0.3184 0.032 Uiso 1 1 calc R . . C8' C 0.5352(3) 0.93951(18) 0.3526(2) 0.0229(9) Uani 1 1 d . . . C9' C 0.4573(3) 0.93132(18) 0.3389(2) 0.0226(9) Uani 1 1 d . . . C10' C 0.4346(3) 0.8953(2) 0.2864(2) 0.0263(10) Uani 1 1 d . . . H10B H 0.3826 0.8899 0.2768 0.032 Uiso 1 1 calc R . . C11' C 0.4079(3) 0.6742(2) 0.4359(3) 0.0300(11) Uani 1 1 d . . . H11C H 0.3703 0.6607 0.4675 0.036 Uiso 1 1 calc R . . H11D H 0.4315 0.6441 0.4135 0.036 Uiso 1 1 calc R . . C12' C 0.6787(3) 0.7110(2) 0.4825(3) 0.0331(12) Uani 1 1 d . . . H12A H 0.6920 0.6749 0.4956 0.040 Uiso 1 1 calc R . . H12B H 0.7128 0.7343 0.5103 0.040 Uiso 1 1 calc R . . C13' C 0.6408(3) 0.7880(2) 0.5974(3) 0.0277(10) Uani 1 1 d . . . H13C H 0.6817 0.7647 0.6146 0.033 Uiso 1 1 calc R . . H13D H 0.6177 0.8030 0.6391 0.033 Uiso 1 1 calc R . . C14' C 0.3700(3) 0.75433(19) 0.5438(3) 0.0253(10) Uani 1 1 d . . . H14A H 0.3584 0.7398 0.5902 0.030 Uiso 1 1 calc R . . H14B H 0.3360 0.7376 0.5077 0.030 Uiso 1 1 calc R . . C15' C 0.4663(3) 0.70352(19) 0.4788(3) 0.0259(10) Uani 1 1 d . . . C16' C 0.5414(3) 0.6946(2) 0.4670(3) 0.0296(11) Uani 1 1 d . . . H16B H 0.5535 0.6690 0.4333 0.036 Uiso 1 1 calc R . . C17' C 0.5994(3) 0.7214(2) 0.5023(3) 0.0271(10) Uani 1 1 d . . . C18' C 0.5821(3) 0.75629(18) 0.5548(2) 0.0227(9) Uani 1 1 d . . . C19' C 0.5077(3) 0.76512(19) 0.5684(2) 0.0232(9) Uani 1 1 d . . . H19B H 0.4963 0.7885 0.6050 0.028 Uiso 1 1 calc R . . C20' C 0.4488(3) 0.74027(19) 0.5293(2) 0.0245(10) Uani 1 1 d . . . Cl1S Cl 0.66540(15) 0.42461(12) 0.77668(15) 0.0967(8) Uani 1 1 d . . . Cl2S Cl 0.76159(15) 0.44556(10) 0.90134(12) 0.0822(7) Uani 1 1 d . . . Cl3S Cl 0.77921(15) 0.52618(9) 0.77295(16) 0.0892(7) Uani 1 1 d . . . Cl4S Cl 0.81565(18) 0.43692(13) 0.68477(14) 0.1080(10) Uani 1 1 d . . . C1S C 0.7583(5) 0.4264(4) 0.8088(5) 0.075(2) Uani 1 1 d . . . H1SA H 0.7784 0.3903 0.8065 0.090 Uiso 1 1 calc R . . C2S C 0.8095(5) 0.4604(4) 0.7731(5) 0.081(3) Uani 1 1 d . . . H2SA H 0.8601 0.4583 0.7979 0.097 Uiso 1 1 calc R . . Cl6S Cl 0.2298(3) 0.3640(2) 0.75692(17) 0.1607(19) Uani 1 1 d . . . Cl5S Cl 0.2442(3) 0.48520(17) 0.76032(19) 0.1481(16) Uani 1 1 d . . . Cl7S Cl 0.4073(3) 0.46611(16) 0.7149(2) 0.1602(18) Uani 1 1 d . . . Cl8S Cl 0.29065(18) 0.42194(11) 0.61929(13) 0.0999(8) Uani 1 1 d . . . C3S C 0.2864(9) 0.4206(5) 0.7597(7) 0.133(5) Uani 1 1 d . . . H3SA H 0.3189 0.4180 0.8040 0.160 Uiso 1 1 calc R . . C4S C 0.3349(7) 0.4184(4) 0.7039(6) 0.097(3) Uani 1 1 d . . . H4SA H 0.3601 0.3838 0.7071 0.116 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 0.0238(2) 0.0265(3) 0.0256(3) 0.00021(19) 0.00219(19) -0.00182(19) As2 0.0293(3) 0.0367(3) 0.0251(3) -0.0030(2) 0.0026(2) -0.0027(2) As3 0.0223(2) 0.0398(3) 0.0225(2) -0.0020(2) 0.00384(19) 0.0042(2) As4 0.0224(2) 0.0263(3) 0.0249(2) 0.00182(19) 0.00102(19) 0.00122(19) Cl1 0.0293(6) 0.0447(8) 0.0426(8) 0.0038(6) -0.0095(6) -0.0077(6) Cl2 0.0633(11) 0.0471(9) 0.0648(11) -0.0171(8) 0.0243(9) 0.0010(8) Cl3 0.0260(6) 0.0557(9) 0.0335(7) 0.0028(6) 0.0041(5) -0.0026(6) Cl4 0.0501(8) 0.0373(7) 0.0295(6) 0.0017(5) 0.0137(6) 0.0076(6) S1 0.0255(6) 0.0338(7) 0.0281(6) 0.0003(5) 0.0069(5) -0.0001(5) S2 0.0268(6) 0.0275(6) 0.0274(6) -0.0020(5) 0.0033(5) -0.0012(5) S3 0.0250(6) 0.0417(7) 0.0290(6) -0.0004(5) 0.0001(5) -0.0031(5) S4 0.0353(7) 0.0463(8) 0.0251(6) -0.0032(6) -0.0059(5) -0.0096(6) S5 0.0297(7) 0.0407(8) 0.0378(7) -0.0039(6) 0.0069(6) 0.0087(6) S6 0.0357(7) 0.0475(8) 0.0256(6) -0.0095(6) 0.0046(5) 0.0042(6) S7 0.0194(5) 0.0319(6) 0.0303(6) 0.0055(5) 0.0003(5) 0.0000(5) S8 0.0261(6) 0.0298(6) 0.0268(6) 0.0005(5) -0.0008(5) -0.0035(5) C1 0.022(2) 0.032(3) 0.029(3) 0.005(2) 0.0021(19) 0.000(2) C2 0.027(3) 0.034(3) 0.032(3) 0.003(2) -0.001(2) -0.005(2) C3 0.022(2) 0.036(3) 0.031(3) 0.003(2) 0.002(2) 0.006(2) C4 0.024(2) 0.032(3) 0.023(2) 0.006(2) -0.0029(19) -0.001(2) C5 0.021(2) 0.027(2) 0.027(2) 0.0105(19) 0.0020(19) -0.0003(18) C6 0.023(2) 0.024(2) 0.026(2) 0.0043(19) 0.0000(19) -0.0013(18) C7 0.031(3) 0.030(3) 0.030(3) -0.001(2) -0.001(2) 0.002(2) C8 0.021(2) 0.033(3) 0.026(2) 0.005(2) -0.0012(19) 0.007(2) C9 0.024(2) 0.026(2) 0.028(2) 0.0093(19) -0.0010(19) 0.0000(19) C10 0.025(2) 0.028(2) 0.024(2) 0.0048(19) 0.0022(19) -0.0002(19) C11 0.031(3) 0.033(3) 0.026(2) 0.002(2) -0.003(2) 0.000(2) C12 0.028(3) 0.040(3) 0.022(2) 0.000(2) -0.004(2) -0.006(2) C13 0.031(3) 0.056(4) 0.020(2) -0.006(2) 0.006(2) -0.001(2) C14 0.036(3) 0.023(2) 0.027(3) 0.000(2) 0.001(2) -0.002(2) C15 0.031(3) 0.023(2) 0.025(2) 0.0042(19) 0.002(2) 0.001(2) C16 0.030(3) 0.033(3) 0.024(2) 0.004(2) -0.002(2) -0.004(2) C17 0.028(2) 0.038(3) 0.017(2) -0.001(2) 0.0011(19) -0.001(2) C18 0.032(3) 0.040(3) 0.021(2) 0.004(2) 0.005(2) -0.002(2) C19 0.028(2) 0.033(3) 0.022(2) 0.003(2) 0.0049(19) 0.000(2) C20 0.033(3) 0.023(2) 0.026(2) 0.0044(19) 0.001(2) -0.003(2) As1' 0.0285(3) 0.0334(3) 0.0227(2) -0.0033(2) 0.0021(2) -0.0021(2) As2' 0.0204(2) 0.0379(3) 0.0233(2) 0.0024(2) 0.00354(19) 0.0045(2) As3' 0.0237(2) 0.0240(2) 0.0235(2) 0.00191(19) -0.00198(19) -0.00065(18) As4' 0.0224(2) 0.0242(2) 0.0248(2) -0.00053(19) 0.00264(19) -0.00282(18) Cl1' 0.0508(8) 0.0399(8) 0.0442(8) -0.0094(6) 0.0148(7) 0.0031(6) Cl2' 0.0253(6) 0.0520(8) 0.0367(7) 0.0073(6) 0.0030(5) -0.0034(6) Cl3' 0.0380(7) 0.0323(6) 0.0267(6) 0.0025(5) 0.0052(5) 0.0009(5) Cl4' 0.0300(6) 0.0456(8) 0.0394(7) 0.0042(6) -0.0078(5) -0.0112(6) S1' 0.0333(7) 0.0386(7) 0.0257(6) -0.0027(5) -0.0053(5) -0.0054(6) S2' 0.0251(6) 0.0414(7) 0.0277(6) -0.0008(5) -0.0006(5) -0.0049(5) S3' 0.0316(7) 0.0386(7) 0.0257(6) -0.0024(5) 0.0056(5) 0.0048(5) S4' 0.0270(6) 0.0407(7) 0.0330(7) 0.0043(6) 0.0065(5) 0.0088(5) S5' 0.0280(6) 0.0280(6) 0.0251(6) 0.0015(5) -0.0020(5) -0.0059(5) S6' 0.0206(6) 0.0338(7) 0.0303(6) 0.0073(5) -0.0006(5) -0.0026(5) S7' 0.0294(6) 0.0252(6) 0.0233(6) -0.0032(5) 0.0041(5) -0.0023(5) S8' 0.0237(6) 0.0306(6) 0.0270(6) 0.0004(5) 0.0061(5) -0.0002(5) C1' 0.030(3) 0.032(3) 0.026(2) -0.003(2) 0.004(2) -0.001(2) C2' 0.028(3) 0.046(3) 0.019(2) 0.000(2) 0.007(2) 0.001(2) C3' 0.030(2) 0.022(2) 0.026(2) 0.0031(19) -0.002(2) -0.0024(19) C4' 0.028(2) 0.026(2) 0.025(2) 0.0000(19) -0.0009(19) 0.005(2) C5' 0.028(2) 0.030(3) 0.018(2) 0.0013(19) 0.0013(18) -0.002(2) C6' 0.027(2) 0.029(3) 0.019(2) 0.0020(18) 0.0010(19) 0.0033(19) C7' 0.028(2) 0.031(3) 0.020(2) 0.0041(19) 0.0008(19) -0.006(2) C8' 0.025(2) 0.022(2) 0.021(2) 0.0024(18) 0.0008(18) -0.0010(18) C9' 0.025(2) 0.024(2) 0.019(2) 0.0033(18) 0.0020(18) 0.0002(18) C10' 0.021(2) 0.035(3) 0.022(2) 0.002(2) -0.0017(18) 0.003(2) C11' 0.030(3) 0.027(3) 0.033(3) 0.002(2) 0.001(2) -0.002(2) C12' 0.025(3) 0.042(3) 0.032(3) 0.010(2) -0.001(2) 0.009(2) C13' 0.022(2) 0.033(3) 0.028(2) 0.010(2) -0.0041(19) -0.002(2) C14' 0.022(2) 0.028(2) 0.026(2) 0.0066(19) 0.0028(19) -0.0033(19) C15' 0.023(2) 0.027(2) 0.027(2) 0.0071(19) -0.0007(19) -0.0009(19) C16' 0.030(3) 0.030(3) 0.029(3) 0.004(2) 0.002(2) 0.003(2) C17' 0.020(2) 0.030(3) 0.031(3) 0.008(2) 0.0005(19) 0.0011(19) C18' 0.019(2) 0.027(2) 0.022(2) 0.0072(18) -0.0016(18) 0.0016(18) C19' 0.023(2) 0.029(2) 0.018(2) 0.0057(18) 0.0024(18) -0.0024(19) C20' 0.020(2) 0.030(3) 0.024(2) 0.0098(19) 0.0041(18) -0.0023(19) Cl1S 0.0767(15) 0.120(2) 0.0931(18) -0.0031(15) 0.0042(13) -0.0189(15) Cl2S 0.1018(17) 0.0815(15) 0.0640(12) 0.0101(11) 0.0123(12) 0.0292(13) Cl3S 0.0928(17) 0.0631(13) 0.1147(19) 0.0057(13) 0.0328(14) 0.0096(12) Cl4S 0.118(2) 0.132(2) 0.0767(16) -0.0132(16) 0.0303(15) 0.0415(19) C1S 0.072(5) 0.070(5) 0.084(6) 0.014(5) 0.013(5) 0.022(4) C2S 0.073(6) 0.079(6) 0.091(7) 0.004(5) 0.010(5) 0.014(5) Cl6S 0.183(4) 0.213(5) 0.087(2) 0.013(2) 0.012(2) -0.088(4) Cl5S 0.202(4) 0.129(3) 0.109(3) -0.014(2) -0.036(3) 0.056(3) Cl7S 0.188(4) 0.135(3) 0.150(3) 0.023(3) -0.056(3) -0.070(3) Cl8S 0.133(2) 0.1000(19) 0.0653(14) -0.0176(13) -0.0101(14) -0.0195(17) C3S 0.170(14) 0.121(11) 0.105(10) 0.013(8) -0.023(10) 0.056(10) C4S 0.115(9) 0.081(7) 0.094(8) -0.013(6) -0.005(7) -0.015(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 As1 S1 2.2176(13) . ? As1 S2 2.2308(13) . ? As1 Cl1 2.2443(14) . ? As2 S4 2.2172(15) . ? As2 Cl2 2.2277(17) . ? As2 S3 2.2331(14) . ? As3 S5 2.2234(15) . ? As3 S6 2.2312(14) . ? As3 Cl3 2.2328(14) . ? As4 S8 2.2208(13) . ? As4 Cl4 2.2286(14) . ? As4 S7 2.2316(13) . ? S1 C1 1.832(5) . ? S2 C11 1.831(5) . ? S3 C2 1.846(5) . ? S4 C12 1.837(5) . ? S5 C3 1.851(5) . ? S6 C13 1.826(6) . ? S7 C4 1.827(5) . ? S8 C14 1.847(5) . ? C1 C5 1.504(7) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C6 1.498(7) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C8 1.507(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C9 1.520(7) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C10 1.398(7) . ? C5 C6 1.404(7) . ? C6 C7 1.404(7) . ? C7 C8 1.403(7) . ? C7 H7A 0.9500 . ? C8 C9 1.387(7) . ? C9 C10 1.400(7) . ? C10 H10A 0.9500 . ? C11 C15 1.499(7) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C17 1.512(7) . ? C12 H12C 0.9900 . ? C12 H12D 0.9900 . ? C13 C18 1.524(7) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C20 1.502(7) . ? C14 H14C 0.9900 . ? C14 H14D 0.9900 . ? C15 C20 1.396(7) . ? C15 C16 1.405(7) . ? C16 C17 1.387(7) . ? C16 H16A 0.9500 . ? C17 C18 1.404(7) . ? C18 C19 1.375(7) . ? C19 C20 1.403(7) . ? C19 H19A 0.9500 . ? As1' S1' 2.2205(14) . ? As1' S2' 2.2297(14) . ? As1' Cl1' 2.2391(15) . ? As2' S4' 2.2218(15) . ? As2' S3' 2.2322(14) . ? As2' Cl2' 2.2401(14) . ? As3' S5' 2.2163(13) . ? As3' S6' 2.2358(13) . ? As3' Cl3' 2.2451(13) . ? As4' S8' 2.2160(13) . ? As4' S7' 2.2280(13) . ? As4' Cl4' 2.2452(14) . ? S1' C1' 1.826(5) . ? S2' C11' 1.856(5) . ? S3' C2' 1.843(6) . ? S4' C12' 1.835(5) . ? S5' C3' 1.848(5) . ? S6' C13' 1.838(5) . ? S7' C4' 1.837(5) . ? S8' C14' 1.837(5) . ? C1' C5' 1.503(7) . ? C1' H1'A 0.9900 . ? C1' H1'B 0.9900 . ? C2' C6' 1.491(7) . ? C2' H2'A 0.9900 . ? C2' H2'B 0.9900 . ? C3' C8' 1.503(7) . ? C3' H3'A 0.9900 . ? C3' H3'B 0.9900 . ? C4' C9' 1.495(7) . ? C4' H4'A 0.9900 . ? C4' H4'B 0.9900 . ? C5' C10' 1.402(7) . ? C5' C6' 1.412(7) . ? C6' C7' 1.397(7) . ? C7' C8' 1.395(7) . ? C7' H7'A 0.9500 . ? C8' C9' 1.421(7) . ? C9' C10' 1.405(7) . ? C10' H10B 0.9500 . ? C11' C15' 1.496(7) . ? C11' H11C 0.9900 . ? C11' H11D 0.9900 . ? C12' C17' 1.512(7) . ? C12' H12A 0.9900 . ? C12' H12B 0.9900 . ? C13' C18' 1.529(7) . ? C13' H13C 0.9900 . ? C13' H13D 0.9900 . ? C14' C20' 1.497(7) . ? C14' H14A 0.9900 . ? C14' H14B 0.9900 . ? C15' C16' 1.395(7) . ? C15' C20' 1.396(7) . ? C16' C17' 1.390(7) . ? C16' H16B 0.9500 . ? C17' C18' 1.389(7) . ? C18' C19' 1.388(6) . ? C19' C20' 1.410(7) . ? C19' H19B 0.9500 . ? Cl1S C1S 1.741(9) . ? Cl2S C1S 1.824(10) . ? Cl3S C2S 1.778(9) . ? Cl4S C2S 1.793(10) . ? C1S C2S 1.462(13) . ? C1S H1SA 1.0000 . ? C2S H2SA 1.0000 . ? Cl6S C3S 1.774(17) . ? Cl5S C3S 1.829(13) . ? Cl7S C4S 1.789(11) . ? Cl8S C4S 1.755(11) . ? C3S C4S 1.407(17) . ? C3S H3SA 1.0000 . ? C4S H4SA 1.0000 . ? 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 90.92(5) . . ? S1 As1 Cl1 101.55(5) . . ? S2 As1 Cl1 97.98(5) . . ? S4 As2 Cl2 101.79(7) . . ? S4 As2 S3 90.05(5) . . ? Cl2 As2 S3 98.57(6) . . ? S5 As3 S6 90.08(6) . . ? S5 As3 Cl3 101.37(6) . . ? S6 As3 Cl3 97.48(6) . . ? S8 As4 Cl4 102.65(5) . . ? S8 As4 S7 89.62(5) . . ? Cl4 As4 S7 96.90(5) . . ? C1 S1 As1 100.73(17) . . ? C11 S2 As1 97.84(18) . . ? C2 S3 As2 98.32(17) . . ? C12 S4 As2 99.96(17) . . ? C3 S5 As3 102.13(18) . . ? C13 S6 As3 98.63(17) . . ? C4 S7 As4 97.25(16) . . ? C14 S8 As4 101.90(17) . . ? C5 C1 S1 114.9(3) . . ? C5 C1 H1A 108.5 . . ? S1 C1 H1A 108.5 . . ? C5 C1 H1B 108.5 . . ? S1 C1 H1B 108.5 . . ? H1A C1 H1B 107.5 . . ? C6 C2 S3 113.2(4) . . ? C6 C2 H2A 108.9 . . ? S3 C2 H2A 108.9 . . ? C6 C2 H2B 108.9 . . ? S3 C2 H2B 108.9 . . ? H2A C2 H2B 107.8 . . ? C8 C3 S5 114.1(3) . . ? C8 C3 H3A 108.7 . . ? S5 C3 H3A 108.7 . . ? C8 C3 H3B 108.7 . . ? S5 C3 H3B 108.7 . . ? H3A C3 H3B 107.6 . . ? C9 C4 S7 111.8(3) . . ? C9 C4 H4A 109.3 . . ? S7 C4 H4A 109.3 . . ? C9 C4 H4B 109.3 . . ? S7 C4 H4B 109.3 . . ? H4A C4 H4B 107.9 . . ? C10 C5 C6 118.2(4) . . ? C10 C5 C1 119.9(5) . . ? C6 C5 C1 121.9(4) . . ? C5 C6 C7 119.1(4) . . ? C5 C6 C2 123.3(4) . . ? C7 C6 C2 117.6(5) . . ? C8 C7 C6 122.0(5) . . ? C8 C7 H7A 119.0 . . ? C6 C7 H7A 119.0 . . ? C9 C8 C7 118.9(5) . . ? C9 C8 C3 123.0(5) . . ? C7 C8 C3 118.1(5) . . ? C8 C9 C10 119.2(5) . . ? C8 C9 C4 123.1(4) . . ? C10 C9 C4 117.7(5) . . ? C5 C10 C9 122.6(5) . . ? C5 C10 H10A 118.7 . . ? C9 C10 H10A 118.7 . . ? C15 C11 S2 112.9(4) . . ? C15 C11 H11A 109.0 . . ? S2 C11 H11A 109.0 . . ? C15 C11 H11B 109.0 . . ? S2 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? C17 C12 S4 114.3(4) . . ? C17 C12 H12C 108.7 . . ? S4 C12 H12C 108.7 . . ? C17 C12 H12D 108.7 . . ? S4 C12 H12D 108.7 . . ? H12C C12 H12D 107.6 . . ? C18 C13 S6 112.8(4) . . ? C18 C13 H13A 109.0 . . ? S6 C13 H13A 109.0 . . ? C18 C13 H13B 109.0 . . ? S6 C13 H13B 109.0 . . ? H13A C13 H13B 107.8 . . ? C20 C14 S8 114.4(4) . . ? C20 C14 H14C 108.7 . . ? S8 C14 H14C 108.7 . . ? C20 C14 H14D 108.7 . . ? S8 C14 H14D 108.7 . . ? H14C C14 H14D 107.6 . . ? C20 C15 C16 118.0(5) . . ? C20 C15 C11 123.3(5) . . ? C16 C15 C11 118.6(5) . . ? C17 C16 C15 122.8(5) . . ? C17 C16 H16A 118.6 . . ? C15 C16 H16A 118.6 . . ? C16 C17 C18 118.4(5) . . ? C16 C17 C12 118.8(5) . . ? C18 C17 C12 122.8(5) . . ? C19 C18 C17 119.3(5) . . ? C19 C18 C13 118.2(5) . . ? C17 C18 C13 122.5(5) . . ? C18 C19 C20 122.2(5) . . ? C18 C19 H19A 118.9 . . ? C20 C19 H19A 118.9 . . ? C15 C20 C19 119.1(5) . . ? C15 C20 C14 122.6(5) . . ? C19 C20 C14 118.3(5) . . ? S1' As1' S2' 90.18(5) . . ? S1' As1' Cl1' 101.97(6) . . ? S2' As1' Cl1' 98.88(6) . . ? S4' As2' S3' 89.43(5) . . ? S4' As2' Cl2' 101.79(6) . . ? S3' As2' Cl2' 97.85(5) . . ? S5' As3' S6' 90.07(5) . . ? S5' As3' Cl3' 102.27(5) . . ? S6' As3' Cl3' 97.35(5) . . ? S8' As4' S7' 90.09(5) . . ? S8' As4' Cl4' 101.66(5) . . ? S7' As4' Cl4' 96.95(5) . . ? C1' S1' As1' 100.59(18) . . ? C11' S2' As1' 98.03(17) . . ? C2' S3' As2' 98.53(17) . . ? C12' S4' As2' 102.22(18) . . ? C3' S5' As3' 101.62(16) . . ? C13' S6' As3' 97.64(16) . . ? C4' S7' As4' 98.34(16) . . ? C14' S8' As4' 100.21(16) . . ? C5' C1' S1' 114.5(3) . . ? C5' C1' H1'A 108.6 . . ? S1' C1' H1'A 108.6 . . ? C5' C1' H1'B 108.6 . . ? S1' C1' H1'B 108.6 . . ? H1'A C1' H1'B 107.6 . . ? C6' C2' S3' 112.6(3) . . ? C6' C2' H2'A 109.1 . . ? S3' C2' H2'A 109.1 . . ? C6' C2' H2'B 109.1 . . ? S3' C2' H2'B 109.1 . . ? H2'A C2' H2'B 107.8 . . ? C8' C3' S5' 113.8(3) . . ? C8' C3' H3'A 108.8 . . ? S5' C3' H3'A 108.8 . . ? C8' C3' H3'B 108.8 . . ? S5' C3' H3'B 108.8 . . ? H3'A C3' H3'B 107.7 . . ? C9' C4' S7' 112.6(3) . . ? C9' C4' H4'A 109.1 . . ? S7' C4' H4'A 109.1 . . ? C9' C4' H4'B 109.1 . . ? S7' C4' H4'B 109.1 . . ? H4'A C4' H4'B 107.8 . . ? C10' C5' C6' 118.7(4) . . ? C10' C5' C1' 118.6(4) . . ? C6' C5' C1' 122.7(4) . . ? C7' C6' C5' 118.2(4) . . ? C7' C6' C2' 118.5(5) . . ? C5' C6' C2' 123.3(4) . . ? C8' C7' C6' 123.6(5) . . ? C8' C7' H7'A 118.2 . . ? C6' C7' H7'A 118.2 . . ? C7' C8' C9' 118.3(4) . . ? C7' C8' C3' 119.9(4) . . ? C9' C8' C3' 121.7(4) . . ? C10' C9' C8' 118.2(4) . . ? C10' C9' C4' 118.6(4) . . ? C8' C9' C4' 123.1(4) . . ? C5' C10' C9' 122.8(4) . . ? C5' C10' H10B 118.6 . . ? C9' C10' H10B 118.6 . . ? C15' C11' S2' 112.9(3) . . ? C15' C11' H11C 109.0 . . ? S2' C11' H11C 109.0 . . ? C15' C11' H11D 109.0 . . ? S2' C11' H11D 109.0 . . ? H11C C11' H11D 107.8 . . ? C17' C12' S4' 114.3(4) . . ? C17' C12' H12A 108.7 . . ? S4' C12' H12A 108.7 . . ? C17' C12' H12B 108.7 . . ? S4' C12' H12B 108.7 . . ? H12A C12' H12B 107.6 . . ? C18' C13' S6' 112.8(3) . . ? C18' C13' H13C 109.0 . . ? S6' C13' H13C 109.0 . . ? C18' C13' H13D 109.0 . . ? S6' C13' H13D 109.0 . . ? H13C C13' H13D 107.8 . . ? C20' C14' S8' 114.8(3) . . ? C20' C14' H14A 108.6 . . ? S8' C14' H14A 108.6 . . ? C20' C14' H14B 108.6 . . ? S8' C14' H14B 108.6 . . ? H14A C14' H14B 107.5 . . ? C16' C15' C20' 118.5(5) . . ? C16' C15' C11' 118.8(5) . . ? C20' C15' C11' 122.7(4) . . ? C17' C16' C15' 122.9(5) . . ? C17' C16' H16B 118.6 . . ? C15' C16' H16B 118.6 . . ? C16' C17' C18' 118.5(4) . . ? C16' C17' C12' 118.6(5) . . ? C18' C17' C12' 122.9(5) . . ? C19' C18' C17' 119.6(4) . . ? C19' C18' C13' 116.9(4) . . ? C17' C18' C13' 123.5(4) . . ? C18' C19' C20' 121.7(5) . . ? C18' C19' H19B 119.2 . . ? C20' C19' H19B 119.2 . . ? C15' C20' C19' 118.7(4) . . ? C15' C20' C14' 122.6(4) . . ? C19' C20' C14' 118.6(4) . . ? C2S C1S Cl1S 117.7(7) . . ? C2S C1S Cl2S 107.2(7) . . ? Cl1S C1S Cl2S 109.0(5) . . ? C2S C1S H1SA 107.5 . . ? Cl1S C1S H1SA 107.5 . . ? Cl2S C1S H1SA 107.5 . . ? C1S C2S Cl3S 111.9(7) . . ? C1S C2S Cl4S 107.6(7) . . ? Cl3S C2S Cl4S 110.7(5) . . ? C1S C2S H2SA 108.8 . . ? Cl3S C2S H2SA 108.8 . . ? Cl4S C2S H2SA 108.8 . . ? C4S C3S Cl6S 108.7(10) . . ? C4S C3S Cl5S 108.2(10) . . ? Cl6S C3S Cl5S 120.8(9) . . ? C4S C3S H3SA 106.1 . . ? Cl6S C3S H3SA 106.1 . . ? Cl5S C3S H3SA 106.1 . . ? C3S C4S Cl8S 114.9(10) . . ? C3S C4S Cl7S 111.0(10) . . ? Cl8S C4S Cl7S 111.1(7) . . ? C3S C4S H4SA 106.4 . . ? Cl8S C4S H4SA 106.4 . . ? Cl7S C4S H4SA 106.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S2 As1 S1 C1 158.01(17) . . . . ? Cl1 As1 S1 C1 -103.65(17) . . . . ? S1 As1 S2 C11 168.83(17) . . . . ? Cl1 As1 S2 C11 67.03(18) . . . . ? S4 As2 S3 C2 -175.41(18) . . . . ? Cl2 As2 S3 C2 -73.48(19) . . . . ? Cl2 As2 S4 C12 96.86(19) . . . . ? S3 As2 S4 C12 -164.38(18) . . . . ? S6 As3 S5 C3 157.76(18) . . . . ? Cl3 As3 S5 C3 -104.60(18) . . . . ? S5 As3 S6 C13 167.10(18) . . . . ? Cl3 As3 S6 C13 65.63(19) . . . . ? S8 As4 S7 C4 -166.38(17) . . . . ? Cl4 As4 S7 C4 -63.68(17) . . . . ? Cl4 As4 S8 C14 104.87(17) . . . . ? S7 As4 S8 C14 -158.14(17) . . . . ? As1 S1 C1 C5 -58.2(4) . . . . ? As2 S3 C2 C6 -51.0(4) . . . . ? As3 S5 C3 C8 -52.5(4) . . . . ? As4 S7 C4 C9 -55.3(4) . . . . ? S1 C1 C5 C10 -49.6(6) . . . . ? S1 C1 C5 C6 131.3(4) . . . . ? C10 C5 C6 C7 3.4(7) . . . . ? C1 C5 C6 C7 -177.5(4) . . . . ? C10 C5 C6 C2 -178.7(4) . . . . ? C1 C5 C6 C2 0.4(7) . . . . ? S3 C2 C6 C5 -73.8(6) . . . . ? S3 C2 C6 C7 104.1(5) . . . . ? C5 C6 C7 C8 -1.5(8) . . . . ? C2 C6 C7 C8 -179.6(5) . . . . ? C6 C7 C8 C9 -1.3(8) . . . . ? C6 C7 C8 C3 178.1(5) . . . . ? S5 C3 C8 C9 124.3(5) . . . . ? S5 C3 C8 C7 -55.0(6) . . . . ? C7 C8 C9 C10 2.1(7) . . . . ? C3 C8 C9 C10 -177.2(5) . . . . ? C7 C8 C9 C4 178.5(4) . . . . ? C3 C8 C9 C4 -0.8(7) . . . . ? S7 C4 C9 C8 -73.2(5) . . . . ? S7 C4 C9 C10 103.3(5) . . . . ? C6 C5 C10 C9 -2.6(7) . . . . ? C1 C5 C10 C9 178.3(4) . . . . ? C8 C9 C10 C5 -0.2(7) . . . . ? C4 C9 C10 C5 -176.7(4) . . . . ? As1 S2 C11 C15 53.0(4) . . . . ? As2 S4 C12 C17 61.7(4) . . . . ? As3 S6 C13 C18 50.8(4) . . . . ? As4 S8 C14 C20 53.7(4) . . . . ? S2 C11 C15 C20 74.6(6) . . . . ? S2 C11 C15 C16 -102.1(5) . . . . ? C20 C15 C16 C17 -2.0(7) . . . . ? C11 C15 C16 C17 174.9(5) . . . . ? C15 C16 C17 C18 4.3(8) . . . . ? C15 C16 C17 C12 -176.1(5) . . . . ? S4 C12 C17 C16 51.3(6) . . . . ? S4 C12 C17 C18 -129.1(5) . . . . ? C16 C17 C18 C19 -2.3(7) . . . . ? C12 C17 C18 C19 178.1(5) . . . . ? C16 C17 C18 C13 179.5(5) . . . . ? C12 C17 C18 C13 -0.1(8) . . . . ? S6 C13 C18 C19 -102.8(5) . . . . ? S6 C13 C18 C17 75.5(6) . . . . ? C17 C18 C19 C20 -2.0(8) . . . . ? C13 C18 C19 C20 176.3(5) . . . . ? C16 C15 C20 C19 -2.3(7) . . . . ? C11 C15 C20 C19 -179.1(5) . . . . ? C16 C15 C20 C14 178.7(4) . . . . ? C11 C15 C20 C14 1.9(7) . . . . ? C18 C19 C20 C15 4.4(7) . . . . ? C18 C19 C20 C14 -176.6(5) . . . . ? S8 C14 C20 C15 -125.8(5) . . . . ? S8 C14 C20 C19 55.2(6) . . . . ? S2' As1' S1' C1' 163.24(17) . . . . ? Cl1' As1' S1' C1' -97.64(18) . . . . ? S1' As1' S2' C11' 172.71(17) . . . . ? Cl1' As1' S2' C11' 70.56(18) . . . . ? S4' As2' S3' C2' -167.96(17) . . . . ? Cl2' As2' S3' C2' -66.14(18) . . . . ? S3' As2' S4' C12' -158.22(19) . . . . ? Cl2' As2' S4' C12' 103.88(19) . . . . ? S6' As3' S5' C3' 160.32(17) . . . . ? Cl3' As3' S5' C3' -102.14(17) . . . . ? S5' As3' S6' C13' 167.87(18) . . . . ? Cl3' As3' S6' C13' 65.49(18) . . . . ? S8' As4' S7' C4' -168.38(16) . . . . ? Cl4' As4' S7' C4' -66.62(17) . . . . ? S7' As4' S8' C14' -160.56(16) . . . . ? Cl4' As4' S8' C14' 102.33(16) . . . . ? As1' S1' C1' C5' -59.9(4) . . . . ? As2' S3' C2' C6' -51.2(4) . . . . ? As3' S5' C3' C8' -54.6(4) . . . . ? As4' S7' C4' C9' -51.6(4) . . . . ? S1' C1' C5' C10' -50.7(6) . . . . ? S1' C1' C5' C6' 129.0(4) . . . . ? C10' C5' C6' C7' 2.7(7) . . . . ? C1' C5' C6' C7' -177.0(4) . . . . ? C10' C5' C6' C2' 179.4(5) . . . . ? C1' C5' C6' C2' -0.3(7) . . . . ? S3' C2' C6' C7' 101.7(5) . . . . ? S3' C2' C6' C5' -75.0(5) . . . . ? C5' C6' C7' C8' 0.8(7) . . . . ? C2' C6' C7' C8' -176.1(5) . . . . ? C6' C7' C8' C9' -3.7(7) . . . . ? C6' C7' C8' C3' 177.5(4) . . . . ? S5' C3' C8' C7' -54.4(5) . . . . ? S5' C3' C8' C9' 126.9(4) . . . . ? C7' C8' C9' C10' 3.0(7) . . . . ? C3' C8' C9' C10' -178.2(4) . . . . ? C7' C8' C9' C4' 179.2(4) . . . . ? C3' C8' C9' C4' -2.0(7) . . . . ? S7' C4' C9' C10' 101.8(5) . . . . ? S7' C4' C9' C8' -74.4(5) . . . . ? C6' C5' C10' C9' -3.4(7) . . . . ? C1' C5' C10' C9' 176.4(5) . . . . ? C8' C9' C10' C5' 0.5(7) . . . . ? C4' C9' C10' C5' -175.9(4) . . . . ? As1' S2' C11' C15' 51.4(4) . . . . ? As2' S4' C12' C17' 54.0(4) . . . . ? As3' S6' C13' C18' 53.1(4) . . . . ? As4' S8' C14' C20' 58.1(4) . . . . ? S2' C11' C15' C16' -104.7(5) . . . . ? S2' C11' C15' C20' 74.0(5) . . . . ? C20' C15' C16' C17' -1.4(7) . . . . ? C11' C15' C16' C17' 177.4(5) . . . . ? C15' C16' C17' C18' 4.2(7) . . . . ? C15' C16' C17' C12' -176.5(5) . . . . ? S4' C12' C17' C16' 55.4(6) . . . . ? S4' C12' C17' C18' -125.3(5) . . . . ? C16' C17' C18' C19' -2.9(7) . . . . ? C12' C17' C18' C19' 177.8(4) . . . . ? C16' C17' C18' C13' 179.9(4) . . . . ? C12' C17' C18' C13' 0.6(7) . . . . ? S6' C13' C18' C19' -104.3(4) . . . . ? S6' C13' C18' C17' 73.0(5) . . . . ? C17' C18' C19' C20' -1.2(7) . . . . ? C13' C18' C19' C20' 176.2(4) . . . . ? C16' C15' C20' C19' -2.7(7) . . . . ? C11' C15' C20' C19' 178.6(4) . . . . ? C16' C15' C20' C14' 177.4(4) . . . . ? C11' C15' C20' C14' -1.3(7) . . . . ? C18' C19' C20' C15' 4.1(7) . . . . ? C18' C19' C20' C14' -176.0(4) . . . . ? S8' C14' C20' C15' -130.0(4) . . . . ? S8' C14' C20' C19' 50.1(5) . . . . ? Cl1S C1S C2S Cl3S 58.1(9) . . . . ? Cl2S C1S C2S Cl3S -65.2(8) . . . . ? Cl1S C1S C2S Cl4S -63.8(8) . . . . ? Cl2S C1S C2S Cl4S 172.9(4) . . . . ? Cl6S C3S C4S Cl8S 66.0(10) . . . . ? Cl5S C3S C4S Cl8S -66.8(12) . . . . ? Cl6S C3S C4S Cl7S -166.9(6) . . . . ? Cl5S C3S C4S Cl7S 60.3(11) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.710 _refine_diff_density_min -1.576 _refine_diff_density_rms 0.138 # Attachment 'nathr3_AS4L2_As2Ls.cif' data_nathr3 _database_code_depnum_ccdc_archive 'CCDC 743841' #TrackingRef 'nathr3_AS4L2_As2Ls.cif' _audit_creation_method SHELXLTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H39 As7 Cl11 S14' _chemical_formula_weight 1846.91 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 14.3168(10) _cell_length_b 14.5379(10) _cell_length_c 16.8865(11) _cell_angle_alpha 80.5640(10) _cell_angle_beta 80.5110(10) _cell_angle_gamma 61.5270(10) _cell_volume 3032.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5310 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 27.00 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.023 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1806 _exptl_absorpt_coefficient_mu 4.808 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4782 _exptl_absorpt_correction_T_max 0.6997 _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 Bruker Apex' _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 34380 _diffrn_reflns_av_R_equivalents 0.0280 _diffrn_reflns_av_sigmaI/netI 0.0353 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 27.00 _reflns_number_total 13158 _reflns_number_gt 11084 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _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^)+(0.0360P)^2^+2.0878P] 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 13158 _refine_ls_number_parameters 649 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0406 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0766 _refine_ls_wR_factor_gt 0.0721 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.029 _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 0.36874(3) 0.86049(3) 0.12823(2) 0.02209(8) Uani 1 1 d . . . As2 As 0.08464(3) 1.08720(3) 0.115772(19) 0.02150(8) Uani 1 1 d . . . As3 As 0.07423(3) 1.12570(3) 0.328787(19) 0.02166(8) Uani 1 1 d . . . As4 As 0.33876(3) 0.87667(3) 0.34991(2) 0.02336(8) Uani 1 1 d . . . As5 As 0.25217(3) 0.33588(3) 0.71399(2) 0.02965(9) Uani 1 1 d . . . As6 As 0.62118(3) -0.34449(3) 0.72202(2) 0.03770(10) Uani 1 1 d . . . As7 As 0.62640(3) 0.56934(3) 0.00007(2) 0.02450(8) Uani 1 1 d . . . Cl1 Cl 0.42161(8) 0.87017(7) -0.00399(5) 0.0375(2) Uani 1 1 d . . . Cl2 Cl -0.09253(7) 1.17257(7) 0.10795(5) 0.03058(18) Uani 1 1 d . . . Cl3 Cl 0.07487(7) 1.18945(7) 0.44074(5) 0.03323(19) Uani 1 1 d . . . Cl4 Cl 0.46256(7) 0.71337(7) 0.38246(6) 0.0413(2) Uani 1 1 d . . . Cl5 Cl 0.08227(8) 0.43560(7) 0.69059(6) 0.0427(2) Uani 1 1 d . . . Cl6 Cl 0.55951(10) -0.45928(7) 0.72788(7) 0.0549(3) Uani 1 1 d . . . Cl7 Cl 0.64601(8) 0.40942(7) 0.04361(5) 0.0349(2) Uani 1 1 d . . . S1 S 0.40897(7) 0.69187(6) 0.15262(5) 0.02648(18) Uani 1 1 d . . . S2 S 0.51917(6) 0.82887(6) 0.17463(6) 0.02674(18) Uani 1 1 d . . . S3 S 0.12926(6) 0.95813(6) 0.03907(5) 0.02274(17) Uani 1 1 d . . . S4 S 0.13973(7) 1.17086(7) 0.01224(5) 0.02742(18) Uani 1 1 d . . . S5 S -0.08009(6) 1.11954(6) 0.35265(5) 0.02510(17) Uani 1 1 d . . . S6 S 0.00085(6) 1.27786(6) 0.25154(5) 0.02505(17) Uani 1 1 d . . . S7 S 0.22001(7) 0.88926(7) 0.45707(5) 0.02555(18) Uani 1 1 d . . . S8 S 0.39399(7) 0.96952(7) 0.40331(5) 0.02808(18) Uani 1 1 d . . . S9 S 0.22465(6) 0.23589(6) 0.82098(5) 0.02479(17) Uani 1 1 d . . . S10 S 0.30694(7) 0.24126(7) 0.60954(5) 0.02924(19) Uani 1 1 d . . . S11 S 0.55435(8) -0.24680(7) 0.60945(5) 0.0383(2) Uani 1 1 d . . . S12 S 0.51454(7) -0.25517(7) 0.82391(5) 0.0314(2) Uani 1 1 d . . . S13 S 0.75612(6) 0.52673(6) -0.10296(5) 0.02449(17) Uani 1 1 d . . . S14 S 0.69892(6) 0.59147(6) 0.09819(5) 0.02559(18) Uani 1 1 d . . . C1 C 0.2755(3) 0.7052(2) 0.1492(2) 0.0240(7) Uani 1 1 d . . . H1A H 0.2531 0.7346 0.0944 0.029 Uiso 1 1 calc R . . H1B H 0.2791 0.6346 0.1596 0.029 Uiso 1 1 calc R . . C2 C 0.0634(3) 0.8868(3) 0.10371(19) 0.0226(7) Uani 1 1 d . . . H2A H -0.0150 0.9309 0.1051 0.027 Uiso 1 1 calc R . . H2B H 0.0821 0.8217 0.0798 0.027 Uiso 1 1 calc R . . C3 C -0.0317(2) 0.9791(2) 0.38689(19) 0.0227(7) Uani 1 1 d . . . H3A H 0.0018 0.9637 0.4375 0.027 Uiso 1 1 calc R . . H3B H -0.0938 0.9648 0.3996 0.027 Uiso 1 1 calc R . . C4 C 0.1784(3) 0.7960(3) 0.43289(18) 0.0229(7) Uani 1 1 d . . . H4A H 0.2386 0.7240 0.4380 0.028 Uiso 1 1 calc R . . H4B H 0.1185 0.7977 0.4724 0.028 Uiso 1 1 calc R . . C5 C 0.1925(2) 0.7751(2) 0.20979(18) 0.0197(6) Uani 1 1 d . . . C6 C 0.0941(2) 0.8584(2) 0.18869(18) 0.0198(6) Uani 1 1 d . . . C7 C 0.0243(2) 0.9210(2) 0.24760(18) 0.0196(6) Uani 1 1 d . . . H7A H -0.0423 0.9769 0.2331 0.023 Uiso 1 1 calc R . . C8 C 0.0475(2) 0.9055(2) 0.32739(18) 0.0190(6) Uani 1 1 d . . . C9 C 0.1442(2) 0.8204(2) 0.34931(18) 0.0202(6) Uani 1 1 d . . . C10 C 0.2137(2) 0.7566(2) 0.29025(18) 0.0199(6) Uani 1 1 d . . . H10A H 0.2784 0.6981 0.3054 0.024 Uiso 1 1 calc R . . C11 C 0.5164(2) 0.9566(2) 0.1400(2) 0.0248(7) Uani 1 1 d . . . H11A H 0.5762 0.9586 0.1605 0.030 Uiso 1 1 calc R . . H11B H 0.5272 0.9640 0.0803 0.030 Uiso 1 1 calc R . . C12 C 0.1706(3) 1.2536(2) 0.06405(19) 0.0224(7) Uani 1 1 d . . . H12A H 0.2041 1.2894 0.0236 0.027 Uiso 1 1 calc R . . H12B H 0.1029 1.3085 0.0881 0.027 Uiso 1 1 calc R . . C13 C 0.1130(2) 1.3102(2) 0.2370(2) 0.0226(7) Uani 1 1 d . . . H13A H 0.0968 1.3723 0.1968 0.027 Uiso 1 1 calc R . . H13B H 0.1202 1.3292 0.2886 0.027 Uiso 1 1 calc R . . C14 C 0.4586(2) 1.0111(3) 0.3121(2) 0.0243(7) Uani 1 1 d . . . H14A H 0.4878 1.0548 0.3270 0.029 Uiso 1 1 calc R . . H14B H 0.5194 0.9479 0.2903 0.029 Uiso 1 1 calc R . . C15 C 0.4133(2) 1.0477(2) 0.16742(19) 0.0205(6) Uani 1 1 d . . . C16 C 0.3420(2) 1.1092(2) 0.11011(19) 0.0203(6) Uani 1 1 d . . . H16A H 0.3612 1.0923 0.0558 0.024 Uiso 1 1 calc R . . C17 C 0.2439(2) 1.1941(2) 0.12947(18) 0.0186(6) Uani 1 1 d . . . C18 C 0.2172(2) 1.2210(2) 0.20899(19) 0.0192(6) Uani 1 1 d . . . C19 C 0.2888(2) 1.1595(2) 0.26628(18) 0.0199(6) Uani 1 1 d . . . H19A H 0.2708 1.1775 0.3203 0.024 Uiso 1 1 calc R . . C20 C 0.3856(2) 1.0727(2) 0.24681(19) 0.0196(6) Uani 1 1 d . . . C21 C 0.1523(2) 0.1753(3) 0.7894(2) 0.0254(7) Uani 1 1 d . . . H21A H 0.1126 0.1568 0.8377 0.030 Uiso 1 1 calc R . . H21B H 0.0992 0.2276 0.7532 0.030 Uiso 1 1 calc R . . C22 C 0.2138(3) 0.1876(3) 0.6105(2) 0.0261(7) Uani 1 1 d . . . H22A H 0.1414 0.2389 0.6310 0.031 Uiso 1 1 calc R . . H22B H 0.2109 0.1771 0.5547 0.031 Uiso 1 1 calc R . . C23 C 0.4102(3) -0.2044(3) 0.6258(2) 0.0348(9) Uani 1 1 d . . . H23A H 0.3825 -0.1900 0.5728 0.042 Uiso 1 1 calc R . . H23B H 0.3985 -0.2628 0.6564 0.042 Uiso 1 1 calc R . . C24 C 0.3764(3) -0.2152(3) 0.8077(2) 0.0315(8) Uani 1 1 d . . . H24A H 0.3744 -0.2710 0.7824 0.038 Uiso 1 1 calc R . . H24B H 0.3328 -0.2076 0.8605 0.038 Uiso 1 1 calc R . . C25 C 0.2225(2) 0.0780(3) 0.7466(2) 0.0229(7) Uani 1 1 d . . . C26 C 0.2465(2) 0.0842(2) 0.66275(19) 0.0223(7) Uani 1 1 d . . . C27 C 0.3067(3) -0.0095(3) 0.6267(2) 0.0255(7) Uani 1 1 d . . . H27A H 0.3207 -0.0058 0.5696 0.031 Uiso 1 1 calc R . . C28 C 0.3473(3) -0.1081(3) 0.6706(2) 0.0268(7) Uani 1 1 d . . . C29 C 0.3281(3) -0.1129(3) 0.7546(2) 0.0262(7) Uani 1 1 d . . . C30 C 0.2649(3) -0.0200(3) 0.7911(2) 0.0264(7) Uani 1 1 d . . . H30A H 0.2503 -0.0238 0.8482 0.032 Uiso 1 1 calc R . . C31 C 0.8787(2) 0.4200(2) -0.0634(2) 0.0238(7) Uani 1 1 d . . . H31A H 0.8594 0.3745 -0.0210 0.029 Uiso 1 1 calc R . . H31B H 0.9243 0.3766 -0.1074 0.029 Uiso 1 1 calc R . . C32 C 0.8299(2) 0.4759(2) 0.10722(19) 0.0240(7) Uani 1 1 d . . . H32A H 0.8481 0.4642 0.1633 0.029 Uiso 1 1 calc R . . H32B H 0.8258 0.4133 0.0961 0.029 Uiso 1 1 calc R . . C33 C 0.9411(2) 0.4596(2) -0.02866(19) 0.0199(6) Uani 1 1 d . . . C34 C 0.9174(2) 0.4873(2) 0.05043(19) 0.0205(6) Uani 1 1 d . . . C35 C 0.9767(2) 0.5272(2) 0.07728(19) 0.0204(6) Uani 1 1 d . . . H35A H 0.9604 0.5461 0.1310 0.025 Uiso 1 1 calc R . . Cl1S Cl 0.13938(13) 0.58223(11) 0.39227(9) 0.0788(4) Uani 1 1 d . . . Cl2S Cl 0.12817(11) 0.38717(9) 0.44465(7) 0.0593(3) Uani 1 1 d . . . C1S C 0.1577(5) 0.4825(4) 0.4698(3) 0.0623(14) Uani 1 1 d . . . H1SA H 0.1113 0.5134 0.5187 0.075 Uiso 1 1 calc R . . H1SB H 0.2328 0.4483 0.4826 0.075 Uiso 1 1 calc R . . Cl3S Cl 0.6057(2) 0.49788(18) 0.51801(16) 0.0591(6) Uani 0.50 1 d PD A 1 Cl4S Cl 0.7306(4) 0.3997(3) 0.3735(2) 0.0979(12) Uani 0.50 1 d PD A 1 C2S C 0.6093(8) 0.4373(7) 0.4350(5) 0.058(3) Uani 0.50 1 d PD A 1 H2SA H 0.5990 0.3744 0.4546 0.070 Uiso 0.50 1 calc PR A 1 H2SB H 0.5498 0.4866 0.4027 0.070 Uiso 0.50 1 calc PR A 1 Cl3A Cl 0.6931(5) 0.4631(4) 0.4287(4) 0.165(3) Uani 0.50 1 d PD B 2 Cl4A Cl 0.7171(3) 0.3759(4) 0.2770(3) 0.1187(15) Uani 0.50 1 d PD B 2 C2SA C 0.6411(12) 0.4633(11) 0.3411(10) 0.137(8) Uani 0.50 1 d PD B 2 H2SC H 0.5760 0.4547 0.3584 0.164 Uiso 0.50 1 calc PR B 2 H2SD H 0.6183 0.5339 0.3111 0.164 Uiso 0.50 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 As1 0.02351(17) 0.02133(16) 0.02166(17) -0.00387(13) 0.00207(13) -0.01135(14) As2 0.02797(17) 0.02257(17) 0.01675(16) 0.00108(13) -0.00616(13) -0.01363(14) As3 0.02245(16) 0.02248(17) 0.01994(17) -0.00078(13) -0.00019(13) -0.01128(14) As4 0.02305(17) 0.02672(18) 0.01981(17) 0.00128(14) -0.00214(13) -0.01220(14) As5 0.0372(2) 0.02490(18) 0.02841(19) -0.00068(15) -0.00592(16) -0.01538(16) As6 0.0447(2) 0.0288(2) 0.0260(2) -0.00073(16) -0.00504(17) -0.00615(17) As7 0.02032(16) 0.02563(18) 0.02514(18) 0.00090(14) -0.00453(13) -0.00904(14) Cl1 0.0540(6) 0.0429(5) 0.0223(4) -0.0052(4) 0.0085(4) -0.0308(5) Cl2 0.0278(4) 0.0304(4) 0.0335(5) -0.0049(4) -0.0072(3) -0.0116(4) Cl3 0.0455(5) 0.0421(5) 0.0233(4) -0.0042(4) -0.0025(4) -0.0292(4) Cl4 0.0329(5) 0.0264(4) 0.0551(6) 0.0058(4) -0.0036(4) -0.0095(4) Cl5 0.0416(5) 0.0310(5) 0.0333(5) -0.0026(4) -0.0095(4) 0.0027(4) Cl6 0.0840(8) 0.0234(5) 0.0510(7) 0.0008(4) -0.0167(6) -0.0180(5) Cl7 0.0455(5) 0.0352(5) 0.0329(5) 0.0015(4) -0.0024(4) -0.0275(4) S1 0.0256(4) 0.0206(4) 0.0313(5) -0.0054(3) 0.0050(3) -0.0107(3) S2 0.0205(4) 0.0179(4) 0.0384(5) -0.0015(3) -0.0023(3) -0.0066(3) S3 0.0299(4) 0.0254(4) 0.0160(4) -0.0006(3) -0.0044(3) -0.0150(4) S4 0.0409(5) 0.0303(4) 0.0167(4) 0.0034(3) -0.0061(3) -0.0219(4) S5 0.0212(4) 0.0239(4) 0.0294(4) -0.0048(3) 0.0019(3) -0.0104(3) S6 0.0199(4) 0.0236(4) 0.0275(4) 0.0010(3) -0.0021(3) -0.0079(3) S7 0.0271(4) 0.0359(5) 0.0169(4) -0.0026(3) -0.0015(3) -0.0173(4) S8 0.0313(4) 0.0343(5) 0.0214(4) 0.0015(4) -0.0060(3) -0.0176(4) S9 0.0259(4) 0.0249(4) 0.0230(4) -0.0025(3) -0.0053(3) -0.0104(3) S10 0.0327(5) 0.0269(4) 0.0257(4) -0.0003(4) -0.0003(4) -0.0134(4) S11 0.0514(6) 0.0282(5) 0.0211(4) -0.0026(4) -0.0024(4) -0.0073(4) S12 0.0398(5) 0.0291(4) 0.0209(4) 0.0009(4) -0.0060(4) -0.0124(4) S13 0.0245(4) 0.0283(4) 0.0214(4) 0.0013(3) -0.0058(3) -0.0128(4) S14 0.0199(4) 0.0250(4) 0.0278(4) -0.0087(3) 0.0002(3) -0.0061(3) C1 0.0288(17) 0.0209(16) 0.0237(17) -0.0030(13) -0.0025(14) -0.0125(14) C2 0.0278(17) 0.0248(16) 0.0202(16) 0.0005(13) -0.0045(13) -0.0162(14) C3 0.0240(16) 0.0266(17) 0.0186(16) -0.0003(13) 0.0002(13) -0.0138(14) C4 0.0257(16) 0.0265(17) 0.0180(16) 0.0021(13) -0.0030(13) -0.0143(14) C5 0.0243(16) 0.0181(15) 0.0205(16) -0.0001(12) -0.0008(13) -0.0138(13) C6 0.0244(16) 0.0206(15) 0.0195(16) 0.0012(12) -0.0047(13) -0.0147(13) C7 0.0196(15) 0.0199(15) 0.0201(16) 0.0036(12) -0.0042(12) -0.0108(13) C8 0.0212(15) 0.0200(15) 0.0203(16) 0.0001(12) -0.0009(12) -0.0141(13) C9 0.0231(16) 0.0233(16) 0.0161(15) 0.0026(13) -0.0020(12) -0.0135(13) C10 0.0199(15) 0.0190(15) 0.0222(16) 0.0047(13) -0.0053(12) -0.0112(13) C11 0.0180(15) 0.0218(16) 0.0321(19) -0.0014(14) 0.0016(13) -0.0089(13) C12 0.0288(17) 0.0181(15) 0.0208(16) 0.0011(13) -0.0039(13) -0.0116(14) C13 0.0236(16) 0.0189(15) 0.0237(17) -0.0014(13) -0.0009(13) -0.0093(13) C14 0.0216(16) 0.0240(17) 0.0285(18) 0.0031(14) -0.0066(13) -0.0120(14) C15 0.0189(15) 0.0172(15) 0.0269(17) -0.0016(13) 0.0026(13) -0.0111(13) C16 0.0218(15) 0.0202(15) 0.0200(16) -0.0014(13) 0.0027(12) -0.0122(13) C17 0.0209(15) 0.0151(14) 0.0217(16) 0.0009(12) -0.0014(12) -0.0110(12) C18 0.0199(15) 0.0153(14) 0.0236(16) -0.0006(12) 0.0005(12) -0.0104(13) C19 0.0238(16) 0.0221(16) 0.0162(15) -0.0022(12) -0.0008(12) -0.0129(13) C20 0.0189(15) 0.0177(15) 0.0253(17) 0.0018(13) -0.0032(13) -0.0120(13) C21 0.0212(16) 0.0309(18) 0.0258(17) -0.0030(14) -0.0026(13) -0.0133(14) C22 0.0291(17) 0.0257(17) 0.0240(17) -0.0020(14) -0.0097(14) -0.0109(14) C23 0.054(2) 0.0242(18) 0.0275(19) -0.0026(15) -0.0158(17) -0.0159(17) C24 0.039(2) 0.0292(19) 0.0286(19) 0.0050(15) -0.0046(16) -0.0190(16) C25 0.0209(15) 0.0269(17) 0.0261(17) -0.0035(14) -0.0044(13) -0.0142(14) C26 0.0216(15) 0.0251(17) 0.0231(17) -0.0021(13) -0.0053(13) -0.0123(14) C27 0.0320(18) 0.0296(18) 0.0184(16) -0.0019(14) -0.0097(14) -0.0151(15) C28 0.0317(18) 0.0238(17) 0.0293(18) -0.0017(14) -0.0095(15) -0.0148(15) C29 0.0283(17) 0.0268(17) 0.0297(18) 0.0005(14) -0.0060(14) -0.0178(15) C30 0.0282(17) 0.0313(18) 0.0250(18) -0.0013(14) -0.0046(14) -0.0178(15) C31 0.0234(16) 0.0185(16) 0.0250(17) -0.0033(13) -0.0036(13) -0.0055(13) C32 0.0233(16) 0.0217(16) 0.0220(17) 0.0003(13) -0.0041(13) -0.0066(14) C33 0.0178(14) 0.0144(14) 0.0225(16) -0.0015(12) -0.0059(12) -0.0022(12) C34 0.0165(14) 0.0157(15) 0.0237(16) -0.0001(12) -0.0052(12) -0.0024(12) C35 0.0189(15) 0.0174(15) 0.0182(15) -0.0046(12) -0.0017(12) -0.0021(12) Cl1S 0.1151(12) 0.0686(9) 0.0756(9) 0.0204(7) -0.0196(8) -0.0663(9) Cl2S 0.0934(9) 0.0498(6) 0.0548(7) 0.0119(5) -0.0326(7) -0.0467(7) C1S 0.099(4) 0.063(3) 0.053(3) 0.006(2) -0.020(3) -0.060(3) Cl3S 0.0744(16) 0.0469(13) 0.0634(15) 0.0001(11) -0.0322(13) -0.0278(12) Cl4S 0.122(3) 0.0542(18) 0.094(3) -0.0061(17) 0.002(2) -0.026(2) C2S 0.082(7) 0.049(6) 0.054(6) 0.008(5) -0.023(5) -0.038(5) Cl3A 0.196(5) 0.116(4) 0.236(7) 0.090(4) -0.158(5) -0.104(4) Cl4A 0.072(2) 0.152(4) 0.133(3) 0.045(3) -0.014(2) -0.070(2) C2SA 0.110(12) 0.061(9) 0.27(3) -0.023(12) -0.079(15) -0.042(9) _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 2.2163(9) . ? As1 S2 2.2265(9) . ? As1 Cl1 2.2404(9) . ? As2 S4 2.2182(9) . ? As2 S3 2.2333(9) . ? As2 Cl2 2.2466(9) . ? As3 S5 2.2214(9) . ? As3 S6 2.2336(9) . ? As3 Cl3 2.2409(9) . ? As4 S8 2.2163(9) . ? As4 Cl4 2.2273(9) . ? As4 S7 2.2351(9) . ? As5 S10 2.2200(9) . ? As5 Cl5 2.2229(10) . ? As5 S9 2.2323(9) . ? As6 Cl6 2.2126(12) . ? As6 S12 2.2256(10) . ? As6 S11 2.2283(10) . ? As7 Cl7 2.2157(9) . ? As7 S14 2.2332(9) . ? As7 S13 2.2473(9) . ? S1 C1 1.837(3) . ? S2 C11 1.837(3) . ? S3 C2 1.838(3) . ? S4 C12 1.841(3) . ? S5 C3 1.838(3) . ? S6 C13 1.848(3) . ? S7 C4 1.841(3) . ? S8 C14 1.830(3) . ? S9 C21 1.827(3) . ? S10 C22 1.835(3) . ? S11 C23 1.835(4) . ? S12 C24 1.832(4) . ? S13 C31 1.839(3) . ? S14 C32 1.836(3) . ? C1 C5 1.509(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C6 1.505(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C8 1.504(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C9 1.502(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C10 1.396(4) . ? C5 C6 1.406(4) . ? C6 C7 1.385(4) . ? C7 C8 1.397(4) . ? C7 H7A 0.9500 . ? C8 C9 1.404(4) . ? C9 C10 1.393(4) . ? C10 H10A 0.9500 . ? C11 C15 1.504(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C17 1.508(4) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C18 1.501(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C20 1.509(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C20 1.390(4) . ? C15 C16 1.396(4) . ? C16 C17 1.389(4) . ? C16 H16A 0.9500 . ? C17 C18 1.401(4) . ? C18 C19 1.399(4) . ? C19 C20 1.393(4) . ? C19 H19A 0.9500 . ? C21 C25 1.508(4) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C26 1.513(4) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C28 1.504(5) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C29 1.509(5) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C30 1.393(5) . ? C25 C26 1.400(4) . ? C26 C27 1.395(4) . ? C27 C28 1.395(5) . ? C27 H27A 0.9500 . ? C28 C29 1.397(5) . ? C29 C30 1.394(5) . ? C30 H30A 0.9500 . ? C31 C33 1.499(4) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C34 1.505(4) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C35 1.393(4) 2_765 ? C33 C34 1.399(4) . ? C34 C35 1.395(4) . ? C35 C33 1.393(4) 2_765 ? C35 H35A 0.9500 . ? Cl1S C1S 1.735(5) . ? Cl2S C1S 1.759(4) . ? C1S H1SA 0.9900 . ? C1S H1SB 0.9900 . ? Cl3S C2S 1.755(9) . ? Cl4S C2S 1.754(10) . ? C2S H2SA 0.9900 . ? C2S H2SB 0.9900 . ? Cl3A C2SA 1.762(13) . ? Cl4A C2SA 1.647(13) . ? C2SA H2SC 0.9900 . ? C2SA H2SD 0.9900 . ? 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 90.91(3) . . ? S1 As1 Cl1 100.77(3) . . ? S2 As1 Cl1 98.23(4) . . ? S4 As2 S3 89.10(3) . . ? S4 As2 Cl2 100.78(3) . . ? S3 As2 Cl2 99.47(3) . . ? S5 As3 S6 91.36(3) . . ? S5 As3 Cl3 101.27(3) . . ? S6 As3 Cl3 98.29(4) . . ? S8 As4 Cl4 101.17(4) . . ? S8 As4 S7 90.93(3) . . ? Cl4 As4 S7 97.94(4) . . ? S10 As5 Cl5 98.64(4) . . ? S10 As5 S9 106.65(3) . . ? Cl5 As5 S9 97.23(4) . . ? Cl6 As6 S12 98.24(4) . . ? Cl6 As6 S11 98.70(4) . . ? S12 As6 S11 106.26(4) . . ? Cl7 As7 S14 98.55(3) . . ? Cl7 As7 S13 98.38(3) . . ? S14 As7 S13 104.14(3) . . ? C1 S1 As1 98.30(10) . . ? C11 S2 As1 98.25(11) . . ? C2 S3 As2 99.22(11) . . ? C12 S4 As2 101.40(10) . . ? C3 S5 As3 99.83(10) . . ? C13 S6 As3 98.90(10) . . ? C4 S7 As4 98.30(10) . . ? C14 S8 As4 99.48(11) . . ? C21 S9 As5 107.13(11) . . ? C22 S10 As5 107.02(11) . . ? C23 S11 As6 105.91(12) . . ? C24 S12 As6 108.13(12) . . ? C31 S13 As7 107.47(11) . . ? C32 S14 As7 107.11(11) . . ? C5 C1 S1 113.0(2) . . ? C5 C1 H1A 109.0 . . ? S1 C1 H1A 109.0 . . ? C5 C1 H1B 109.0 . . ? S1 C1 H1B 109.0 . . ? H1A C1 H1B 107.8 . . ? C6 C2 S3 113.1(2) . . ? C6 C2 H2A 109.0 . . ? S3 C2 H2A 109.0 . . ? C6 C2 H2B 109.0 . . ? S3 C2 H2B 109.0 . . ? H2A C2 H2B 107.8 . . ? C8 C3 S5 114.9(2) . . ? C8 C3 H3A 108.6 . . ? S5 C3 H3A 108.6 . . ? C8 C3 H3B 108.6 . . ? S5 C3 H3B 108.6 . . ? H3A C3 H3B 107.5 . . ? C9 C4 S7 112.6(2) . . ? C9 C4 H4A 109.1 . . ? S7 C4 H4A 109.1 . . ? C9 C4 H4B 109.1 . . ? S7 C4 H4B 109.1 . . ? H4A C4 H4B 107.8 . . ? C10 C5 C6 118.2(3) . . ? C10 C5 C1 119.0(3) . . ? C6 C5 C1 122.7(3) . . ? C7 C6 C5 118.8(3) . . ? C7 C6 C2 118.1(3) . . ? C5 C6 C2 122.9(3) . . ? C6 C7 C8 122.9(3) . . ? C6 C7 H7A 118.5 . . ? C8 C7 H7A 118.5 . . ? C7 C8 C9 118.4(3) . . ? C7 C8 C3 119.4(3) . . ? C9 C8 C3 122.2(3) . . ? C10 C9 C8 118.6(3) . . ? C10 C9 C4 118.0(3) . . ? C8 C9 C4 123.4(3) . . ? C9 C10 C5 122.9(3) . . ? C9 C10 H10A 118.6 . . ? C5 C10 H10A 118.6 . . ? C15 C11 S2 112.8(2) . . ? C15 C11 H11A 109.0 . . ? S2 C11 H11A 109.0 . . ? C15 C11 H11B 109.0 . . ? S2 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? C17 C12 S4 114.1(2) . . ? C17 C12 H12A 108.7 . . ? S4 C12 H12A 108.7 . . ? C17 C12 H12B 108.7 . . ? S4 C12 H12B 108.7 . . ? H12A C12 H12B 107.6 . . ? C18 C13 S6 112.7(2) . . ? C18 C13 H13A 109.0 . . ? S6 C13 H13A 109.0 . . ? C18 C13 H13B 109.0 . . ? S6 C13 H13B 109.0 . . ? H13A C13 H13B 107.8 . . ? C20 C14 S8 114.1(2) . . ? C20 C14 H14A 108.7 . . ? S8 C14 H14A 108.7 . . ? C20 C14 H14B 108.7 . . ? S8 C14 H14B 108.7 . . ? H14A C14 H14B 107.6 . . ? C20 C15 C16 118.9(3) . . ? C20 C15 C11 123.2(3) . . ? C16 C15 C11 117.9(3) . . ? C17 C16 C15 122.5(3) . . ? C17 C16 H16A 118.8 . . ? C15 C16 H16A 118.8 . . ? C16 C17 C18 118.7(3) . . ? C16 C17 C12 118.7(3) . . ? C18 C17 C12 122.6(3) . . ? C19 C18 C17 118.7(3) . . ? C19 C18 C13 117.9(3) . . ? C17 C18 C13 123.3(3) . . ? C20 C19 C18 122.2(3) . . ? C20 C19 H19A 118.9 . . ? C18 C19 H19A 118.9 . . ? C15 C20 C19 119.0(3) . . ? C15 C20 C14 122.2(3) . . ? C19 C20 C14 118.8(3) . . ? C25 C21 S9 114.2(2) . . ? C25 C21 H21A 108.7 . . ? S9 C21 H21A 108.7 . . ? C25 C21 H21B 108.7 . . ? S9 C21 H21B 108.7 . . ? H21A C21 H21B 107.6 . . ? C26 C22 S10 111.9(2) . . ? C26 C22 H22A 109.2 . . ? S10 C22 H22A 109.2 . . ? C26 C22 H22B 109.2 . . ? S10 C22 H22B 109.2 . . ? H22A C22 H22B 107.9 . . ? C28 C23 S11 114.2(2) . . ? C28 C23 H23A 108.7 . . ? S11 C23 H23A 108.7 . . ? C28 C23 H23B 108.7 . . ? S11 C23 H23B 108.7 . . ? H23A C23 H23B 107.6 . . ? C29 C24 S12 112.4(2) . . ? C29 C24 H24A 109.1 . . ? S12 C24 H24A 109.1 . . ? C29 C24 H24B 109.1 . . ? S12 C24 H24B 109.1 . . ? H24A C24 H24B 107.9 . . ? C30 C25 C26 119.1(3) . . ? C30 C25 C21 119.6(3) . . ? C26 C25 C21 121.3(3) . . ? C27 C26 C25 118.2(3) . . ? C27 C26 C22 119.0(3) . . ? C25 C26 C22 122.8(3) . . ? C28 C27 C26 123.0(3) . . ? C28 C27 H27A 118.5 . . ? C26 C27 H27A 118.5 . . ? C27 C28 C29 118.2(3) . . ? C27 C28 C23 118.8(3) . . ? C29 C28 C23 123.0(3) . . ? C30 C29 C28 119.2(3) . . ? C30 C29 C24 118.7(3) . . ? C28 C29 C24 122.1(3) . . ? C25 C30 C29 122.2(3) . . ? C25 C30 H30A 118.9 . . ? C29 C30 H30A 118.9 . . ? C33 C31 S13 112.8(2) . . ? C33 C31 H31A 109.0 . . ? S13 C31 H31A 109.0 . . ? C33 C31 H31B 109.0 . . ? S13 C31 H31B 109.0 . . ? H31A C31 H31B 107.8 . . ? C34 C32 S14 112.9(2) . . ? C34 C32 H32A 109.0 . . ? S14 C32 H32A 109.0 . . ? C34 C32 H32B 109.0 . . ? S14 C32 H32B 109.0 . . ? H32A C32 H32B 107.8 . . ? C35 C33 C34 118.6(3) 2_765 . ? C35 C33 C31 119.2(3) 2_765 . ? C34 C33 C31 122.2(3) . . ? C35 C34 C33 118.7(3) . . ? C35 C34 C32 119.0(3) . . ? C33 C34 C32 122.3(3) . . ? C33 C35 C34 122.7(3) 2_765 . ? C33 C35 H35A 118.6 2_765 . ? C34 C35 H35A 118.6 . . ? Cl1S C1S Cl2S 112.2(3) . . ? Cl1S C1S H1SA 109.2 . . ? Cl2S C1S H1SA 109.2 . . ? Cl1S C1S H1SB 109.2 . . ? Cl2S C1S H1SB 109.2 . . ? H1SA C1S H1SB 107.9 . . ? Cl4S C2S Cl3S 111.9(5) . . ? Cl4S C2S H2SA 109.2 . . ? Cl3S C2S H2SA 109.2 . . ? Cl4S C2S H2SB 109.2 . . ? Cl3S C2S H2SB 109.2 . . ? H2SA C2S H2SB 107.9 . . ? Cl4A C2SA Cl3A 119.2(9) . . ? Cl4A C2SA H2SC 107.5 . . ? Cl3A C2SA H2SC 107.5 . . ? Cl4A C2SA H2SD 107.5 . . ? Cl3A C2SA H2SD 107.5 . . ? H2SC C2SA H2SD 107.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S2 As1 S1 C1 162.62(11) . . . . ? Cl1 As1 S1 C1 -98.82(11) . . . . ? S1 As1 S2 C11 168.58(11) . . . . ? Cl1 As1 S2 C11 67.56(11) . . . . ? S4 As2 S3 C2 -167.71(11) . . . . ? Cl2 As2 S3 C2 -66.93(11) . . . . ? S3 As2 S4 C12 -155.86(11) . . . . ? Cl2 As2 S4 C12 104.66(11) . . . . ? S6 As3 S5 C3 161.34(11) . . . . ? Cl3 As3 S5 C3 -99.92(11) . . . . ? S5 As3 S6 C13 171.35(11) . . . . ? Cl3 As3 S6 C13 69.76(11) . . . . ? S8 As4 S7 C4 -170.84(11) . . . . ? Cl4 As4 S7 C4 -69.42(11) . . . . ? Cl4 As4 S8 C14 101.10(11) . . . . ? S7 As4 S8 C14 -160.62(11) . . . . ? S10 As5 S9 C21 -44.74(11) . . . . ? Cl5 As5 S9 C21 56.57(11) . . . . ? Cl5 As5 S10 C22 -51.45(11) . . . . ? S9 As5 S10 C22 48.83(11) . . . . ? Cl6 As6 S11 C23 54.70(12) . . . . ? S12 As6 S11 C23 -46.58(12) . . . . ? Cl6 As6 S12 C24 -51.93(12) . . . . ? S11 As6 S12 C24 49.69(12) . . . . ? Cl7 As7 S13 C31 -51.04(11) . . . . ? S14 As7 S13 C31 50.03(11) . . . . ? Cl7 As7 S14 C32 51.52(11) . . . . ? S13 As7 S14 C32 -49.43(12) . . . . ? As1 S1 C1 C5 -58.3(2) . . . . ? As2 S3 C2 C6 -53.1(2) . . . . ? As3 S5 C3 C8 -57.9(2) . . . . ? As4 S7 C4 C9 -52.6(2) . . . . ? S1 C1 C5 C10 -50.6(3) . . . . ? S1 C1 C5 C6 129.5(3) . . . . ? C10 C5 C6 C7 2.4(4) . . . . ? C1 C5 C6 C7 -177.6(3) . . . . ? C10 C5 C6 C2 178.9(3) . . . . ? C1 C5 C6 C2 -1.2(4) . . . . ? S3 C2 C6 C7 100.0(3) . . . . ? S3 C2 C6 C5 -76.4(3) . . . . ? C5 C6 C7 C8 0.4(4) . . . . ? C2 C6 C7 C8 -176.2(3) . . . . ? C6 C7 C8 C9 -2.3(4) . . . . ? C6 C7 C8 C3 178.2(3) . . . . ? S5 C3 C8 C7 -49.7(3) . . . . ? S5 C3 C8 C9 130.9(3) . . . . ? C7 C8 C9 C10 1.4(4) . . . . ? C3 C8 C9 C10 -179.2(3) . . . . ? C7 C8 C9 C4 179.6(3) . . . . ? C3 C8 C9 C4 -1.0(5) . . . . ? S7 C4 C9 C10 105.0(3) . . . . ? S7 C4 C9 C8 -73.2(3) . . . . ? C8 C9 C10 C5 1.5(4) . . . . ? C4 C9 C10 C5 -176.8(3) . . . . ? C6 C5 C10 C9 -3.5(4) . . . . ? C1 C5 C10 C9 176.6(3) . . . . ? As1 S2 C11 C15 53.5(2) . . . . ? As2 S4 C12 C17 52.2(2) . . . . ? As3 S6 C13 C18 50.8(2) . . . . ? As4 S8 C14 C20 58.3(2) . . . . ? S2 C11 C15 C20 72.6(3) . . . . ? S2 C11 C15 C16 -106.8(3) . . . . ? C20 C15 C16 C17 -0.4(4) . . . . ? C11 C15 C16 C17 179.0(3) . . . . ? C15 C16 C17 C18 2.1(4) . . . . ? C15 C16 C17 C12 -178.0(3) . . . . ? S4 C12 C17 C16 55.2(3) . . . . ? S4 C12 C17 C18 -124.9(3) . . . . ? C16 C17 C18 C19 -1.9(4) . . . . ? C12 C17 C18 C19 178.2(3) . . . . ? C16 C17 C18 C13 -179.2(3) . . . . ? C12 C17 C18 C13 0.9(4) . . . . ? S6 C13 C18 C19 -100.7(3) . . . . ? S6 C13 C18 C17 76.6(3) . . . . ? C17 C18 C19 C20 0.1(4) . . . . ? C13 C18 C19 C20 177.6(3) . . . . ? C16 C15 C20 C19 -1.4(4) . . . . ? C11 C15 C20 C19 179.2(3) . . . . ? C16 C15 C20 C14 -179.3(3) . . . . ? C11 C15 C20 C14 1.4(4) . . . . ? C18 C19 C20 C15 1.5(4) . . . . ? C18 C19 C20 C14 179.5(3) . . . . ? S8 C14 C20 C15 -130.1(3) . . . . ? S8 C14 C20 C19 52.0(3) . . . . ? As5 S9 C21 C25 82.5(2) . . . . ? As5 S10 C22 C26 -87.3(2) . . . . ? As6 S11 C23 C28 83.9(3) . . . . ? As6 S12 C24 C29 -86.0(3) . . . . ? S9 C21 C25 C30 89.8(3) . . . . ? S9 C21 C25 C26 -89.8(3) . . . . ? C30 C25 C26 C27 4.1(4) . . . . ? C21 C25 C26 C27 -176.2(3) . . . . ? C30 C25 C26 C22 -173.4(3) . . . . ? C21 C25 C26 C22 6.2(5) . . . . ? S10 C22 C26 C27 -95.4(3) . . . . ? S10 C22 C26 C25 82.1(3) . . . . ? C25 C26 C27 C28 -2.6(5) . . . . ? C22 C26 C27 C28 175.0(3) . . . . ? C26 C27 C28 C29 -1.1(5) . . . . ? C26 C27 C28 C23 179.4(3) . . . . ? S11 C23 C28 C27 90.2(3) . . . . ? S11 C23 C28 C29 -89.3(4) . . . . ? C27 C28 C29 C30 3.3(5) . . . . ? C23 C28 C29 C30 -177.2(3) . . . . ? C27 C28 C29 C24 -174.8(3) . . . . ? C23 C28 C29 C24 4.7(5) . . . . ? S12 C24 C29 C30 -97.0(3) . . . . ? S12 C24 C29 C28 81.1(4) . . . . ? C26 C25 C30 C29 -2.0(5) . . . . ? C21 C25 C30 C29 178.4(3) . . . . ? C28 C29 C30 C25 -1.8(5) . . . . ? C24 C29 C30 C25 176.3(3) . . . . ? As7 S13 C31 C33 -86.8(2) . . . . ? As7 S14 C32 C34 86.6(2) . . . . ? S13 C31 C33 C35 -94.0(3) . . . 2_765 ? S13 C31 C33 C34 83.7(3) . . . . ? C35 C33 C34 C35 0.1(5) 2_765 . . . ? C31 C33 C34 C35 -177.6(3) . . . . ? C35 C33 C34 C32 179.9(3) 2_765 . . . ? C31 C33 C34 C32 2.1(4) . . . . ? S14 C32 C34 C35 92.6(3) . . . . ? S14 C32 C34 C33 -87.1(3) . . . . ? C33 C34 C35 C33 -0.2(5) . . . 2_765 ? C32 C34 C35 C33 -179.9(3) . . . 2_765 ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.166 _refine_diff_density_min -1.107 _refine_diff_density_rms 0.094