# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 186/2321 4-CH3OC6H4CS2AsPh2 data_General _audit_creation_date 'Thu Feb 24 10:47:12 2000' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #------------------------------------------------------------------------------ # SUBMISSION DETAILS _publ_contact_author_name ' ENTER NAME' _publ_contact_author_address ; ENTER ADDRESS ; _publ_contact_author_email ' ENTER EMAIL ADDRESS ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? #------------------------------------------------------------------------------ # TITLE AND AUTHOR LIST _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_footnote _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS FOOTNOTES ; ; FIRST AUTHORS ADDRESS ; _publ_section_synopsis ; ENTER SYNOPSIS ; #------------------------------------------------------------------------------ # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1999). teXsan. Single Crystal Structure Analysis Software. Version 1.10. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #------------------------------------------------------------------------------ data_4-CH3OC6H4CS2AsPh2 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C20 H17 As O S2 ' _chemical_formula_moiety 'C20 H17 As O S2 ' _chemical_formula_weight 412.40 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 10.464(2) _cell_length_b 11.022(3) _cell_length_c 8.916(2) _cell_angle_alpha 96.09(2) _cell_angle_beta 92.36(2) _cell_angle_gamma 63.01(1) _cell_volume 911.2(4) _cell_formula_units_Z 2 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 10.0 _cell_measurement_theta_max 12.4 _cell_measurement_temperature 193.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.430 _exptl_crystal_size_mid 0.370 _exptl_crystal_size_min 0.270 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.503 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 2.098 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.852 _exptl_absorpt_correction_T_max 0.999 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 4424 _diffrn_reflns_av_R_equivalents 0.037 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 1.0029 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.0029 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.33 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 4194 _reflns_number_gt 3432 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0346 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3432 _refine_ls_number_parameters 218 _refine_ls_goodness_of_fit_ref 1.689 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00010|Fo|^2^]' _refine_ls_shift/su_max 7.6370 _refine_diff_density_max 0.61 _refine_diff_density_min -0.38 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'As' 'As' 0.050 2.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group As(1) As 0.14863(3) 0.05094(3) 0.45208(3) 0.02895(8) Uani 1.00 d . . . S(11) S 0.26306(8) -0.26696(7) 0.45225(9) 0.0408(2) Uani 1.00 d . . . S(12) S 0.36464(7) -0.08171(7) 0.33948(8) 0.0320(2) Uani 1.00 d . . . O(11) O 0.8093(2) -0.6731(2) -0.0110(2) 0.0439(6) Uani 1.00 d . . . C(11) C 0.3757(3) -0.2445(3) 0.3469(3) 0.0296(7) Uani 1.00 d . . . C(12) C 0.4915(3) -0.3564(3) 0.2564(3) 0.0284(7) Uani 1.00 d . . . C(13) C 0.5164(3) -0.4915(3) 0.2623(3) 0.0385(8) Uani 1.00 d . . . C(14) C 0.6203(3) -0.5990(3) 0.1764(3) 0.0389(8) Uani 1.00 d . . . C(15) C 0.7043(3) -0.5744(3) 0.0793(3) 0.0330(7) Uani 1.00 d . . . C(16) C 0.6843(3) -0.4411(3) 0.0733(3) 0.0371(8) Uani 1.00 d . . . C(17) C 0.5803(3) -0.3341(3) 0.1598(3) 0.0339(7) Uani 1.00 d . . . C(18) C 0.8297(3) -0.8104(3) -0.0100(4) 0.0481(9) Uani 1.00 d . . . C(21) C 0.1542(3) 0.2186(2) 0.4045(3) 0.0278(7) Uani 1.00 d . . . C(22) C 0.2611(3) 0.2536(3) 0.4558(4) 0.0411(9) Uani 1.00 d . . . C(23) C 0.2609(4) 0.3724(3) 0.4167(4) 0.0477(10) Uani 1.00 d . . . C(24) C 0.1531(4) 0.4568(3) 0.3275(3) 0.0437(9) Uani 1.00 d . . . C(25) C 0.0443(4) 0.4252(3) 0.2798(4) 0.0469(9) Uani 1.00 d . . . C(26) C 0.0448(3) 0.3059(3) 0.3184(3) 0.0370(8) Uani 1.00 d . . . C(31) C 0.2108(3) 0.0591(3) 0.6623(3) 0.0295(7) Uani 1.00 d . . . C(32) C 0.1180(3) 0.1703(3) 0.7575(3) 0.0421(8) Uani 1.00 d . . . C(33) C 0.1517(4) 0.1849(3) 0.9080(3) 0.0478(10) Uani 1.00 d . . . C(34) C 0.2763(4) 0.0890(4) 0.9650(3) 0.0461(10) Uani 1.00 d . . . C(35) C 0.3687(3) -0.0223(3) 0.8714(4) 0.0457(9) Uani 1.00 d . . . C(36) C 0.3361(3) -0.0375(3) 0.7192(3) 0.0370(8) Uani 1.00 d . . . H(11) H 0.4424 -0.4992 0.3303 0.0550 Uiso 1.00 calc . . . H(12) H 0.6451 -0.6998 0.1933 0.0550 Uiso 1.00 calc . . . H(13) H 0.7450 -0.4255 0.0005 0.0550 Uiso 1.00 calc . . . H(14) H 0.5698 -0.2364 0.1388 0.0550 Uiso 1.00 calc . . . H(15) H 0.9036 -0.8717 -0.0813 0.0563 Uiso 1.00 calc . . . H(16) H 0.7438 -0.8175 -0.0372 0.0563 Uiso 1.00 calc . . . H(17) H 0.8586 -0.8428 0.0874 0.0563 Uiso 1.00 calc . . . H(21) H 0.3391 0.1959 0.5179 0.0550 Uiso 1.00 calc . . . H(22) H 0.3460 0.3945 0.4627 0.0550 Uiso 1.00 calc . . . H(23) H 0.1495 0.5483 0.3012 0.0550 Uiso 1.00 calc . . . H(24) H -0.0330 0.4796 0.2090 0.0550 Uiso 1.00 calc . . . H(25) H -0.0318 0.2778 0.2742 0.0550 Uiso 1.00 calc . . . H(31) H 0.0236 0.2316 0.7083 0.0550 Uiso 1.00 calc . . . H(32) H 0.0726 0.2713 0.9734 0.0550 Uiso 1.00 calc . . . H(33) H 0.3027 0.1024 1.0728 0.0550 Uiso 1.00 calc . . . H(34) H 0.4692 -0.1086 0.9026 0.0550 Uiso 1.00 calc . . . H(35) H 0.4100 -0.1174 0.6553 0.0550 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 As(1) 0.0286(2) 0.0293(2) 0.0313(2) -0.0147(1) -0.0005(1) 0.0054(1) S(11) 0.0474(5) 0.0360(4) 0.0452(4) -0.0236(4) 0.0125(4) 0.0022(3) S(12) 0.0363(4) 0.0263(3) 0.0362(4) -0.0159(3) 0.0073(3) 0.0031(3) O(11) 0.040(1) 0.033(1) 0.055(1) -0.0139(9) 0.013(1) -0.0059(9) C(11) 0.035(1) 0.031(1) 0.027(1) -0.019(1) -0.002(1) 0.006(1) C(12) 0.032(1) 0.030(1) 0.027(1) -0.017(1) -0.001(1) 0.005(1) C(13) 0.046(2) 0.032(1) 0.041(2) -0.020(1) 0.009(1) 0.003(1) C(14) 0.045(2) 0.028(1) 0.044(2) -0.016(1) 0.005(1) 0.003(1) C(15) 0.030(1) 0.033(1) 0.033(1) -0.012(1) -0.003(1) 0.001(1) C(16) 0.036(2) 0.036(1) 0.041(2) -0.017(1) 0.006(1) 0.006(1) C(17) 0.035(2) 0.031(1) 0.037(2) -0.016(1) 0.003(1) 0.008(1) C(18) 0.048(2) 0.034(2) 0.057(2) -0.016(1) 0.005(2) -0.008(1) C(21) 0.031(1) 0.026(1) 0.025(1) -0.012(1) 0.002(1) 0.003(1) C(22) 0.038(2) 0.040(2) 0.052(2) -0.021(1) -0.013(1) 0.018(1) C(23) 0.052(2) 0.048(2) 0.057(2) -0.032(2) -0.010(2) 0.018(2) C(24) 0.058(2) 0.031(1) 0.045(2) -0.021(1) 0.000(2) 0.010(1) C(25) 0.055(2) 0.037(2) 0.046(2) -0.016(2) -0.014(2) 0.016(1) C(26) 0.039(2) 0.034(1) 0.036(2) -0.015(1) -0.009(1) 0.005(1) C(31) 0.031(1) 0.033(1) 0.029(1) -0.018(1) 0.001(1) 0.008(1) C(32) 0.038(2) 0.046(2) 0.038(2) -0.014(1) 0.004(1) 0.005(1) C(33) 0.052(2) 0.059(2) 0.036(2) -0.029(2) 0.011(1) -0.005(1) C(34) 0.059(2) 0.068(2) 0.030(2) -0.045(2) -0.004(1) 0.010(2) C(35) 0.048(2) 0.051(2) 0.046(2) -0.027(2) -0.014(2) 0.020(2) C(36) 0.034(2) 0.037(2) 0.040(2) -0.015(1) -0.003(1) 0.009(1) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SHELXS86 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag As(1) S(11) 3.1470(8) . . yes As(1) S(12) 2.2651(8) . . yes As(1) C(21) 1.966(3) . . yes As(1) C(31) 1.965(3) . . yes S(11) C(11) 1.655(3) . . yes S(12) C(11) 1.753(3) . . yes O(11) C(15) 1.357(3) . . yes O(11) C(18) 1.431(4) . . yes C(11) C(12) 1.467(4) . . yes C(12) C(13) 1.397(4) . . yes C(12) C(17) 1.408(4) . . yes C(13) C(14) 1.372(4) . . yes C(13) H(11) 1.041 . . no C(14) C(15) 1.387(4) . . yes C(14) H(12) 1.046 . . no C(15) C(16) 1.393(4) . . yes C(16) C(17) 1.372(4) . . yes C(16) H(13) 1.006 . . no C(17) H(14) 1.067 . . no C(18) H(15) 0.967 . . no C(18) H(16) 0.956 . . no C(18) H(17) 0.958 . . no C(21) C(22) 1.387(4) . . yes C(21) C(26) 1.382(4) . . yes C(22) C(23) 1.389(4) . . yes C(22) H(21) 0.971 . . no C(23) C(24) 1.379(4) . . yes C(23) H(22) 1.079 . . no C(24) C(25) 1.374(4) . . yes C(24) H(23) 1.044 . . no C(25) C(26) 1.391(4) . . yes C(25) H(24) 1.005 . . no C(26) H(25) 1.033 . . no C(31) C(32) 1.390(4) . . yes C(31) C(36) 1.379(4) . . yes C(32) C(33) 1.385(4) . . yes C(32) H(31) 1.023 . . no C(33) C(34) 1.373(5) . . yes C(33) H(32) 1.067 . . no C(34) C(35) 1.381(5) . . yes C(34) H(33) 1.003 . . no C(35) C(36) 1.398(4) . . yes C(35) H(34) 1.101 . . no C(36) H(35) 1.005 . . no #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S(11) As(1) S(12) 64.08(2) . 1_555 1_555 yes S(11) As(1) C(21) 155.55(8) . 1_555 1_555 yes S(11) As(1) C(31) 89.20(8) . 1_555 1_555 yes S(12) As(1) C(21) 91.47(8) . 1_555 1_555 yes S(12) As(1) C(31) 99.44(8) . 1_555 1_555 yes C(21) As(1) C(31) 96.0(1) . 1_555 1_555 yes As(1) S(11) C(11) 73.27(9) . 1_555 1_555 yes As(1) S(12) C(11) 100.44(9) . 1_555 1_555 yes C(15) O(11) C(18) 117.4(2) . 1_555 1_555 yes S(11) C(11) S(12) 121.0(2) . 1_555 1_555 yes S(11) C(11) C(12) 123.6(2) . 1_555 1_555 yes S(12) C(11) C(12) 115.4(2) . 1_555 1_555 yes C(11) C(12) C(13) 120.1(2) . 1_555 1_555 yes C(11) C(12) C(17) 122.7(2) . 1_555 1_555 yes C(13) C(12) C(17) 117.2(2) . 1_555 1_555 yes C(12) C(13) C(14) 122.3(3) . 1_555 1_555 yes C(12) C(13) H(11) 112.8 . 1_555 1_555 no C(14) C(13) H(11) 124.7 . 1_555 1_555 no C(13) C(14) C(15) 119.6(3) . 1_555 1_555 yes C(13) C(14) H(12) 120.4 . 1_555 1_555 no C(15) C(14) H(12) 119.6 . 1_555 1_555 no O(11) C(15) C(14) 124.3(3) . 1_555 1_555 yes O(11) C(15) C(16) 116.2(2) . 1_555 1_555 yes C(14) C(15) C(16) 119.5(3) . 1_555 1_555 yes C(15) C(16) C(17) 120.6(3) . 1_555 1_555 yes C(15) C(16) H(13) 118.1 . 1_555 1_555 no C(17) C(16) H(13) 121.3 . 1_555 1_555 no C(12) C(17) C(16) 120.8(2) . 1_555 1_555 yes C(12) C(17) H(14) 125.4 . 1_555 1_555 no C(16) C(17) H(14) 113.6 . 1_555 1_555 no O(11) C(18) H(15) 110.7 . 1_555 1_555 no O(11) C(18) H(16) 111.3 . 1_555 1_555 no O(11) C(18) H(17) 111.5 . 1_555 1_555 no H(15) C(18) H(16) 107.5 . 1_555 1_555 no H(15) C(18) H(17) 107.4 . 1_555 1_555 no H(16) C(18) H(17) 108.2 . 1_555 1_555 no As(1) C(21) C(22) 122.9(2) . 1_555 1_555 yes As(1) C(21) C(26) 118.1(2) . 1_555 1_555 yes C(22) C(21) C(26) 119.0(2) . 1_555 1_555 yes C(21) C(22) C(23) 120.4(3) . 1_555 1_555 yes C(21) C(22) H(21) 121.7 . 1_555 1_555 no C(23) C(22) H(21) 117.9 . 1_555 1_555 no C(22) C(23) C(24) 119.8(3) . 1_555 1_555 yes C(22) C(23) H(22) 116.5 . 1_555 1_555 no C(24) C(23) H(22) 123.7 . 1_555 1_555 no C(23) C(24) C(25) 120.2(3) . 1_555 1_555 yes C(23) C(24) H(23) 120.5 . 1_555 1_555 no C(25) C(24) H(23) 119.2 . 1_555 1_555 no C(24) C(25) C(26) 119.9(3) . 1_555 1_555 yes C(24) C(25) H(24) 123.3 . 1_555 1_555 no C(26) C(25) H(24) 116.5 . 1_555 1_555 no C(21) C(26) C(25) 120.5(3) . 1_555 1_555 yes C(21) C(26) H(25) 119.5 . 1_555 1_555 no C(25) C(26) H(25) 119.7 . 1_555 1_555 no As(1) C(31) C(32) 115.9(2) . 1_555 1_555 yes As(1) C(31) C(36) 124.6(2) . 1_555 1_555 yes C(32) C(31) C(36) 119.5(3) . 1_555 1_555 yes C(31) C(32) C(33) 120.3(3) . 1_555 1_555 yes C(31) C(32) H(31) 114.1 . 1_555 1_555 no C(33) C(32) H(31) 125.4 . 1_555 1_555 no C(32) C(33) C(34) 120.3(3) . 1_555 1_555 yes C(32) C(33) H(32) 115.1 . 1_555 1_555 no C(34) C(33) H(32) 124.5 . 1_555 1_555 no C(33) C(34) C(35) 119.8(3) . 1_555 1_555 yes C(33) C(34) H(33) 120.0 . 1_555 1_555 no C(35) C(34) H(33) 120.1 . 1_555 1_555 no C(34) C(35) C(36) 120.3(3) . 1_555 1_555 yes C(34) C(35) H(34) 127.5 . 1_555 1_555 no C(36) C(35) H(34) 112.1 . 1_555 1_555 no C(31) C(36) C(35) 119.8(3) . 1_555 1_555 yes C(31) C(36) H(35) 123.4 . 1_555 1_555 no C(35) C(36) H(35) 116.7 . 1_555 1_555 no #------------------------------------------------------------------------------ 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 As(1) S(11) C(11) S(12) 9.2(1) 1_555 1_555 1_555 1_555 yes As(1) S(11) C(11) C(12) -171.9(2) 1_555 1_555 1_555 1_555 yes As(1) S(12) C(11) S(11) -12.4(2) 1_555 1_555 1_555 1_555 yes As(1) S(12) C(11) C(12) 168.5(2) 1_555 1_555 1_555 1_555 yes As(1) C(21) C(22) C(23) 179.0(2) 1_555 1_555 1_555 1_555 yes As(1) C(21) C(26) C(25) -179.2(2) 1_555 1_555 1_555 1_555 yes As(1) C(31) C(32) C(33) 179.6(2) 1_555 1_555 1_555 1_555 yes As(1) C(31) C(36) C(35) -179.1(2) 1_555 1_555 1_555 1_555 yes S(11) As(1) S(12) C(11) 6.20(9) 1_555 1_555 1_555 1_555 yes S(11) As(1) C(21) C(22) -61.6(3) 1_555 1_555 1_555 1_555 yes S(11) As(1) C(21) C(26) 119.6(2) 1_555 1_555 1_555 1_555 yes S(11) As(1) C(31) C(32) -139.7(2) 1_555 1_555 1_555 1_555 yes S(11) As(1) C(31) C(36) 39.3(2) 1_555 1_555 1_555 1_555 yes S(11) C(11) C(12) C(13) -3.5(4) 1_555 1_555 1_555 1_555 yes S(11) C(11) C(12) C(17) 175.7(2) 1_555 1_555 1_555 1_555 yes S(12) As(1) S(11) C(11) -6.74(10) 1_555 1_555 1_555 1_555 yes S(12) As(1) C(21) C(22) -60.0(2) 1_555 1_555 1_555 1_555 yes S(12) As(1) C(21) C(26) 121.2(2) 1_555 1_555 1_555 1_555 yes S(12) As(1) C(31) C(32) 156.7(2) 1_555 1_555 1_555 1_555 yes S(12) As(1) C(31) C(36) -24.3(2) 1_555 1_555 1_555 1_555 yes S(12) C(11) C(12) C(13) 175.5(2) 1_555 1_555 1_555 1_555 yes S(12) C(11) C(12) C(17) -5.3(3) 1_555 1_555 1_555 1_555 yes O(11) C(15) C(14) C(13) -179.6(3) 1_555 1_555 1_555 1_555 yes O(11) C(15) C(16) C(17) 179.7(3) 1_555 1_555 1_555 1_555 yes C(11) S(11) As(1) C(21) -4.9(2) 1_555 1_555 1_555 1_555 yes C(11) S(11) As(1) C(31) -107.6(1) 1_555 1_555 1_555 1_555 yes C(11) S(12) As(1) C(21) -173.1(1) 1_555 1_555 1_555 1_555 yes C(11) S(12) As(1) C(31) 90.7(1) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(14) 178.0(3) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(17) C(16) -177.8(3) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(14) C(15) -0.2(5) 1_555 1_555 1_555 1_555 yes C(12) C(17) C(16) C(15) -0.1(4) 1_555 1_555 1_555 1_555 yes C(13) C(12) C(17) C(16) 1.4(4) 1_555 1_555 1_555 1_555 yes C(13) C(14) C(15) C(16) 1.6(4) 1_555 1_555 1_555 1_555 yes C(14) C(13) C(12) C(17) -1.3(4) 1_555 1_555 1_555 1_555 yes C(14) C(15) O(11) C(18) 2.8(4) 1_555 1_555 1_555 1_555 yes C(14) C(15) C(16) C(17) -1.5(4) 1_555 1_555 1_555 1_555 yes C(16) C(15) O(11) C(18) -178.4(3) 1_555 1_555 1_555 1_555 yes C(21) As(1) C(31) C(32) 64.2(2) 1_555 1_555 1_555 1_555 yes C(21) As(1) C(31) C(36) -116.8(2) 1_555 1_555 1_555 1_555 yes C(21) C(22) C(23) C(24) 0.6(5) 1_555 1_555 1_555 1_555 yes C(21) C(26) C(25) C(24) 0.0(5) 1_555 1_555 1_555 1_555 yes C(22) C(21) As(1) C(31) 39.7(3) 1_555 1_555 1_555 1_555 yes C(22) C(21) C(26) C(25) 1.9(4) 1_555 1_555 1_555 1_555 yes C(22) C(23) C(24) C(25) 1.4(5) 1_555 1_555 1_555 1_555 yes C(23) C(22) C(21) C(26) -2.2(5) 1_555 1_555 1_555 1_555 yes C(23) C(24) C(25) C(26) -1.7(5) 1_555 1_555 1_555 1_555 yes C(26) C(21) As(1) C(31) -139.1(2) 1_555 1_555 1_555 1_555 yes C(31) C(32) C(33) C(34) -0.6(5) 1_555 1_555 1_555 1_555 yes C(31) C(36) C(35) C(34) -0.2(5) 1_555 1_555 1_555 1_555 yes C(32) C(31) C(36) C(35) -0.1(4) 1_555 1_555 1_555 1_555 yes C(32) C(33) C(34) C(35) 0.2(5) 1_555 1_555 1_555 1_555 yes C(33) C(32) C(31) C(36) 0.6(4) 1_555 1_555 1_555 1_555 yes C(33) C(34) C(35) C(36) 0.2(5) 1_555 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ #===END (4-CH3C6H4CS2)2AsPh data_General _audit_creation_date 'Thu Feb 24 14:02:20 2000' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #------------------------------------------------------------------------------ # SUBMISSION DETAILS _publ_contact_author_name ' ENTER NAME' _publ_contact_author_address ; ENTER ADDRESS ; _publ_contact_author_email ' ENTER EMAIL ADDRESS ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? #------------------------------------------------------------------------------ # TITLE AND AUTHOR LIST _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_footnote _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS FOOTNOTES ; ; FIRST AUTHORS ADDRESS ; _publ_section_synopsis ; ENTER SYNOPSIS ; #------------------------------------------------------------------------------ # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1999). teXsan. Single Crystal Structure Analysis Software. Version 1.10. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #------------------------------------------------------------------------------ data_[4-CH3C6H4CS2]2AsPh #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C22 H19 As S4 ' _chemical_formula_moiety 'C22 H19 As S4 ' _chemical_formula_weight 486.55 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,-y,1/2+z 1/2+x,1/2-y,-z -x,1/2+y,1/2-z _cell_length_a 16.458(3) _cell_length_b 22.083(4) _cell_length_c 5.947(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2161.3(9) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.1 _cell_measurement_theta_max 12.4 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'reddish' _exptl_crystal_size_max 0.290 _exptl_crystal_size_mid 0.140 _exptl_crystal_size_min 0.030 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.495 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.964 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.789 _exptl_absorpt_correction_T_max 0.988 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 2867 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 0.9986 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.9986 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 7 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 1.20 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 2867 _reflns_number_gt 1243 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0537 _refine_ls_wR_factor_ref 0.0568 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 1243 _refine_ls_number_parameters 246 _refine_ls_goodness_of_fit_ref 1.211 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00040|Fo|^2^]' _refine_ls_shift/su_max 1.6008 _refine_diff_density_max 0.50 _refine_diff_density_min -0.45 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack -0.01(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'As' 'As' 0.050 2.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group As(1) As 0.46454(8) 0.23621(6) 1.0128(3) 0.0509(4) Uani 1.00 d . . . S(11) S 0.4695(2) 0.1207(2) 0.7614(6) 0.066(1) Uani 1.00 d . . . S(12) S 0.4135(2) 0.1555(2) 1.2118(6) 0.055(1) Uani 1.00 d . . . S(21) S 0.4996(2) 0.3671(2) 0.9755(7) 0.066(1) Uani 1.00 d . . . S(22) S 0.4315(2) 0.2905(1) 1.3330(6) 0.058(1) Uani 1.00 d . . . C(11) C 0.4245(7) 0.1018(5) 0.997(2) 0.048(3) Uani 1.00 d . . . C(12) C 0.3904(7) 0.0417(6) 1.046(2) 0.047(3) Uani 1.00 d . . . C(13) C 0.3996(7) -0.0055(6) 0.890(2) 0.057(4) Uani 1.00 d . . . C(14) C 0.3668(8) -0.0601(6) 0.930(3) 0.066(5) Uani 1.00 d . . . C(15) C 0.3258(8) -0.0747(6) 1.130(3) 0.055(4) Uani 1.00 d . . . C(16) C 0.3184(8) -0.0274(6) 1.288(2) 0.058(4) Uani 1.00 d . . . C(17) C 0.3517(7) 0.0285(6) 1.246(2) 0.056(4) Uani 1.00 d . . . C(18) C 0.2899(8) -0.1358(6) 1.176(3) 0.081(6) Uani 1.00 d . . . C(21) C 0.4486(6) 0.3612(5) 1.213(2) 0.046(3) Uani 1.00 d . . . C(22) C 0.4157(7) 0.4138(6) 1.337(2) 0.043(3) Uani 1.00 d . . . C(23) C 0.4243(8) 0.4724(6) 1.252(2) 0.059(4) Uani 1.00 d . . . C(24) C 0.3936(8) 0.5211(6) 1.363(3) 0.066(5) Uani 1.00 d . . . C(25) C 0.3515(8) 0.5154(6) 1.567(3) 0.064(4) Uani 1.00 d . . . C(26) C 0.3427(8) 0.4568(7) 1.647(3) 0.068(5) Uani 1.00 d . . . C(27) C 0.3741(8) 0.4074(6) 1.543(2) 0.057(4) Uani 1.00 d . . . C(28) C 0.3175(9) 0.5683(7) 1.689(3) 0.090(6) Uani 1.00 d . . . C(31) C 0.5814(7) 0.2236(5) 1.071(2) 0.042(3) Uani 1.00 d . . . C(32) C 0.6332(8) 0.2417(6) 0.902(2) 0.051(3) Uani 1.00 d . . . C(33) C 0.7146(8) 0.2342(7) 0.934(3) 0.070(5) Uani 1.00 d . . . C(34) C 0.7469(8) 0.2112(7) 1.125(3) 0.073(5) Uani 1.00 d . . . C(35) C 0.6946(8) 0.1940(6) 1.292(3) 0.058(4) Uani 1.00 d . . . C(36) C 0.6111(8) 0.2002(6) 1.268(2) 0.060(4) Uani 1.00 d . . . H(11) H 0.4290 0.0006 0.7473 0.0639 Uiso 1.00 calc . . . H(12) H 0.3807 -0.0987 0.8334 0.0886 Uiso 1.00 calc . . . H(13) H 0.2892 -0.0349 1.4266 0.0640 Uiso 1.00 calc . . . H(14) H 0.3478 0.0612 1.3568 0.0641 Uiso 1.00 calc . . . H(15) H 0.3122 -0.1543 1.3065 0.0837 Uiso 1.00 calc . . . H(16) H 0.3015 -0.1637 1.0497 0.0837 Uiso 1.00 calc . . . H(17) H 0.2321 -0.1348 1.1898 0.0837 Uiso 1.00 calc . . . H(21) H 0.4525 0.4787 1.1070 0.0698 Uiso 1.00 calc . . . H(22) H 0.4013 0.5620 1.2968 0.0779 Uiso 1.00 calc . . . H(23) H 0.3113 0.4504 1.7892 0.0850 Uiso 1.00 calc . . . H(24) H 0.3668 0.3669 1.6082 0.0670 Uiso 1.00 calc . . . H(25) H 0.3594 0.5978 1.7334 0.1094 Uiso 1.00 calc . . . H(26) H 0.2925 0.5560 1.8320 0.1094 Uiso 1.00 calc . . . H(27) H 0.2775 0.5900 1.6076 0.1094 Uiso 1.00 calc . . . H(31) H 0.6127 0.2606 0.7669 0.0622 Uiso 1.00 calc . . . H(32) H 0.7524 0.2435 0.8117 0.0798 Uiso 1.00 calc . . . H(33) H 0.8047 0.2093 1.1441 0.0821 Uiso 1.00 calc . . . H(34) H 0.7188 0.1774 1.4289 0.0732 Uiso 1.00 calc . . . H(35) H 0.5741 0.1880 1.3897 0.0688 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 As(1) 0.0431(7) 0.0577(8) 0.0519(8) -0.0015(7) -0.0028(9) 0.0101(8) S(11) 0.076(3) 0.076(2) 0.045(2) -0.011(2) 0.009(2) 0.008(2) S(12) 0.059(2) 0.053(2) 0.052(2) -0.010(2) 0.007(2) -0.001(2) S(21) 0.066(2) 0.067(2) 0.064(3) 0.004(2) 0.017(2) 0.015(2) S(22) 0.063(2) 0.051(2) 0.059(2) 0.002(2) 0.012(2) 0.006(2) C(11) 0.039(6) 0.060(6) 0.046(5) -0.004(5) -0.003(6) -0.001(4) C(12) 0.037(7) 0.056(6) 0.048(7) 0.006(5) -0.018(6) 0.005(5) C(13) 0.053(9) 0.065(7) 0.053(9) -0.003(7) 0.013(7) -0.006(6) C(14) 0.060(10) 0.056(7) 0.08(1) 0.005(7) 0.012(8) -0.018(8) C(15) 0.037(8) 0.049(7) 0.079(9) 0.018(6) -0.009(7) 0.000(6) C(16) 0.068(9) 0.056(7) 0.051(9) -0.005(7) 0.011(8) 0.017(6) C(17) 0.049(8) 0.056(7) 0.062(8) -0.009(6) 0.010(7) -0.002(8) C(18) 0.09(1) 0.057(9) 0.10(1) -0.013(8) -0.01(1) 0.017(10) C(21) 0.024(6) 0.051(4) 0.062(6) 0.002(5) -0.013(5) 0.009(5) C(22) 0.020(6) 0.054(6) 0.055(7) -0.003(6) -0.009(6) 0.010(5) C(23) 0.058(8) 0.059(6) 0.060(10) -0.010(8) 0.011(8) 0.019(7) C(24) 0.051(9) 0.050(8) 0.10(1) -0.005(7) 0.003(8) 0.014(8) C(25) 0.041(8) 0.060(6) 0.09(1) -0.003(7) -0.008(7) -0.013(7) C(26) 0.064(10) 0.065(7) 0.07(1) 0.004(8) 0.012(9) -0.003(7) C(27) 0.058(9) 0.067(8) 0.047(9) -0.007(7) -0.001(6) -0.001(7) C(28) 0.10(1) 0.08(1) 0.10(1) 0.017(9) 0.02(1) -0.036(10) C(31) 0.039(2) 0.031(7) 0.057(7) -0.007(5) 0.013(4) -0.007(5) C(32) 0.052(6) 0.066(9) 0.036(6) -0.002(7) 0.002(5) 0.013(7) C(33) 0.050(6) 0.08(1) 0.08(1) -0.003(9) 0.007(8) -0.014(9) C(34) 0.034(8) 0.09(1) 0.09(1) -0.014(8) -0.005(7) -0.001(10) C(35) 0.056(6) 0.044(8) 0.07(1) 0.008(7) -0.008(7) 0.014(8) C(36) 0.054(6) 0.067(9) 0.059(8) 0.016(7) 0.011(7) 0.009(8) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SAPI91 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag As(1) S(11) 2.958(4) . . yes As(1) S(12) 2.299(4) . . yes As(1) S(21) 2.956(4) . . yes As(1) S(22) 2.315(4) . . yes As(1) C(31) 1.97(1) . . yes S(11) C(11) 1.64(1) . . yes S(12) C(11) 1.75(1) . . yes S(21) C(21) 1.65(1) . . yes S(22) C(21) 1.74(1) . . yes C(11) C(12) 1.47(2) . . yes C(12) C(13) 1.40(2) . . yes C(12) C(17) 1.38(2) . . yes C(13) C(14) 1.34(2) . . yes C(13) H(11) 0.986 . . no C(14) C(15) 1.40(2) . . yes C(14) H(12) 1.052 . . no C(15) C(16) 1.41(2) . . yes C(15) C(18) 1.50(2) . . yes C(16) C(17) 1.37(2) . . yes C(16) H(13) 0.969 . . no C(17) H(14) 0.977 . . no C(18) H(15) 0.950 . . no C(18) H(16) 0.992 . . no C(18) H(17) 0.955 . . no C(21) C(22) 1.48(2) . . yes C(22) C(23) 1.40(2) . . yes C(22) C(27) 1.41(2) . . yes C(23) C(24) 1.36(2) . . yes C(23) H(21) 0.991 . . no C(24) C(25) 1.40(2) . . yes C(24) H(22) 0.993 . . no C(25) C(26) 1.39(2) . . yes C(25) C(28) 1.48(2) . . yes C(26) C(27) 1.36(2) . . yes C(26) H(23) 1.001 . . no C(27) H(24) 0.982 . . no C(28) H(25) 0.986 . . no C(28) H(26) 0.985 . . no C(28) H(27) 0.947 . . no C(31) C(32) 1.38(2) . . yes C(31) C(36) 1.37(2) . . yes C(32) C(33) 1.36(2) . . yes C(32) H(31) 0.968 . . no C(33) C(34) 1.36(2) . . yes C(33) H(32) 0.979 . . no C(34) C(35) 1.37(2) . . yes C(34) H(33) 0.959 . . no C(35) C(36) 1.39(2) . . yes C(35) H(34) 0.979 . . no C(36) H(35) 0.982 . . no #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S(11) As(1) S(12) 66.5(1) . 1_555 1_555 yes S(11) As(1) S(21) 143.1(1) . 1_555 1_555 yes S(11) As(1) S(22) 150.3(1) . 1_555 1_555 yes S(11) As(1) C(31) 86.6(4) . 1_555 1_555 yes S(12) As(1) S(21) 150.3(1) . 1_555 1_555 yes S(12) As(1) S(22) 83.8(1) . 1_555 1_555 yes S(12) As(1) C(31) 99.0(4) . 1_555 1_555 yes S(21) As(1) S(22) 66.5(1) . 1_555 1_555 yes S(21) As(1) C(31) 87.8(3) . 1_555 1_555 yes S(22) As(1) C(31) 99.1(4) . 1_555 1_555 yes As(1) S(11) C(11) 77.0(5) . 1_555 1_555 yes As(1) S(12) C(11) 96.4(5) . 1_555 1_555 yes As(1) S(21) C(21) 76.1(5) . 1_555 1_555 yes As(1) S(22) C(21) 95.1(5) . 1_555 1_555 yes S(11) C(11) S(12) 119.8(7) . 1_555 1_555 yes S(11) C(11) C(12) 124(1) . 1_555 1_555 yes S(12) C(11) C(12) 115(1) . 1_555 1_555 yes C(11) C(12) C(13) 120(1) . 1_555 1_555 yes C(11) C(12) C(17) 122(1) . 1_555 1_555 yes C(13) C(12) C(17) 117(1) . 1_555 1_555 yes C(12) C(13) C(14) 120(1) . 1_555 1_555 yes C(12) C(13) H(11) 121.4 . 1_555 1_555 no C(14) C(13) H(11) 118.1 . 1_555 1_555 no C(13) C(14) C(15) 123(1) . 1_555 1_555 yes C(13) C(14) H(12) 122.9 . 1_555 1_555 no C(15) C(14) H(12) 112.3 . 1_555 1_555 no C(14) C(15) C(16) 115(1) . 1_555 1_555 yes C(14) C(15) C(18) 123(1) . 1_555 1_555 yes C(16) C(15) C(18) 120(1) . 1_555 1_555 yes C(15) C(16) C(17) 120(1) . 1_555 1_555 yes C(15) C(16) H(13) 118.9 . 1_555 1_555 no C(17) C(16) H(13) 120.3 . 1_555 1_555 no C(12) C(17) C(16) 121(1) . 1_555 1_555 yes C(12) C(17) H(14) 117.1 . 1_555 1_555 no C(16) C(17) H(14) 121.1 . 1_555 1_555 no C(15) C(18) H(15) 112.7 . 1_555 1_555 no C(15) C(18) H(16) 110.1 . 1_555 1_555 no C(15) C(18) H(17) 112.8 . 1_555 1_555 no H(15) C(18) H(16) 106.0 . 1_555 1_555 no H(15) C(18) H(17) 109.1 . 1_555 1_555 no H(16) C(18) H(17) 105.7 . 1_555 1_555 no S(21) C(21) S(22) 120.3(8) . 1_555 1_555 yes S(21) C(21) C(22) 123.6(10) . 1_555 1_555 yes S(22) C(21) C(22) 116(1) . 1_555 1_555 yes C(21) C(22) C(23) 120(1) . 1_555 1_555 yes C(21) C(22) C(27) 122(1) . 1_555 1_555 yes C(23) C(22) C(27) 117(1) . 1_555 1_555 yes C(22) C(23) C(24) 121(1) . 1_555 1_555 yes C(22) C(23) H(21) 119.7 . 1_555 1_555 no C(24) C(23) H(21) 118.9 . 1_555 1_555 no C(23) C(24) C(25) 122(1) . 1_555 1_555 yes C(23) C(24) H(22) 118.8 . 1_555 1_555 no C(25) C(24) H(22) 119.0 . 1_555 1_555 no C(24) C(25) C(26) 115(1) . 1_555 1_555 yes C(24) C(25) C(28) 122(1) . 1_555 1_555 yes C(26) C(25) C(28) 121(1) . 1_555 1_555 yes C(25) C(26) C(27) 123(1) . 1_555 1_555 yes C(25) C(26) H(23) 118.4 . 1_555 1_555 no C(27) C(26) H(23) 117.9 . 1_555 1_555 no C(22) C(27) C(26) 120(1) . 1_555 1_555 yes C(22) C(27) H(24) 119.5 . 1_555 1_555 no C(26) C(27) H(24) 120.5 . 1_555 1_555 no C(25) C(28) H(25) 112.8 . 1_555 1_555 no C(25) C(28) H(26) 111.4 . 1_555 1_555 no C(25) C(28) H(27) 114.4 . 1_555 1_555 no H(25) C(28) H(26) 103.9 . 1_555 1_555 no H(25) C(28) H(27) 106.8 . 1_555 1_555 no H(26) C(28) H(27) 106.9 . 1_555 1_555 no As(1) C(31) C(32) 115(1) . 1_555 1_555 yes As(1) C(31) C(36) 123(1) . 1_555 1_555 yes C(32) C(31) C(36) 120(1) . 1_555 1_555 yes C(31) C(32) C(33) 118(1) . 1_555 1_555 yes C(31) C(32) H(31) 121.1 . 1_555 1_555 no C(33) C(32) H(31) 120.7 . 1_555 1_555 no C(32) C(33) C(34) 123(1) . 1_555 1_555 yes C(32) C(33) H(32) 119.7 . 1_555 1_555 no C(34) C(33) H(32) 117.0 . 1_555 1_555 no C(33) C(34) C(35) 117(1) . 1_555 1_555 yes C(33) C(34) H(33) 120.1 . 1_555 1_555 no C(35) C(34) H(33) 122.0 . 1_555 1_555 no C(34) C(35) C(36) 121(1) . 1_555 1_555 yes C(34) C(35) H(34) 116.8 . 1_555 1_555 no C(36) C(35) H(34) 121.5 . 1_555 1_555 no C(31) C(36) C(35) 118(1) . 1_555 1_555 yes C(31) C(36) H(35) 120.7 . 1_555 1_555 no C(35) C(36) H(35) 120.8 . 1_555 1_555 no #------------------------------------------------------------------------------ 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 As(1) S(11) C(11) S(12) -4.1(7) 1_555 1_555 1_555 1_555 yes As(1) S(11) C(11) C(12) 175(1) 1_555 1_555 1_555 1_555 yes As(1) S(12) C(11) S(11) 5.1(8) 1_555 1_555 1_555 1_555 yes As(1) S(12) C(11) C(12) -174.1(9) 1_555 1_555 1_555 1_555 yes As(1) S(21) C(21) S(22) 12.4(6) 1_555 1_555 1_555 1_555 yes As(1) S(21) C(21) C(22) -168(1) 1_555 1_555 1_555 1_555 yes As(1) S(22) C(21) S(21) -15.4(7) 1_555 1_555 1_555 1_555 yes As(1) S(22) C(21) C(22) 165.2(8) 1_555 1_555 1_555 1_555 yes As(1) C(31) C(32) C(33) 179(1) 1_555 1_555 1_555 1_555 yes As(1) C(31) C(36) C(35) -179(1) 1_555 1_555 1_555 1_555 yes S(11) As(1) S(12) C(11) -2.7(4) 1_555 1_555 1_555 1_555 yes S(11) As(1) S(21) C(21) 169.1(4) 1_555 1_555 1_555 1_555 yes S(11) As(1) S(22) C(21) -169.3(4) 1_555 1_555 1_555 1_555 yes S(11) As(1) C(31) C(32) 82(1) 1_555 1_555 1_555 1_555 yes S(11) As(1) C(31) C(36) -98(1) 1_555 1_555 1_555 1_555 yes S(11) C(11) C(12) C(13) 4(1) 1_555 1_555 1_555 1_555 yes S(11) C(11) C(12) C(17) -178(1) 1_555 1_555 1_555 1_555 yes S(12) As(1) S(11) C(11) 2.9(5) 1_555 1_555 1_555 1_555 yes S(12) As(1) S(21) C(21) -5.3(5) 1_555 1_555 1_555 1_555 yes S(12) As(1) S(22) C(21) -170.3(4) 1_555 1_555 1_555 1_555 yes S(12) As(1) C(31) C(32) 148.5(10) 1_555 1_555 1_555 1_555 yes S(12) As(1) C(31) C(36) -33(1) 1_555 1_555 1_555 1_555 yes S(12) C(11) C(12) C(13) -176(1) 1_555 1_555 1_555 1_555 yes S(12) C(11) C(12) C(17) 0(1) 1_555 1_555 1_555 1_555 yes S(21) As(1) S(11) C(11) -174.0(5) 1_555 1_555 1_555 1_555 yes S(21) As(1) S(12) C(11) 173.6(5) 1_555 1_555 1_555 1_555 yes S(21) As(1) S(22) C(21) 8.0(4) 1_555 1_555 1_555 1_555 yes S(21) As(1) C(31) C(32) -60(1) 1_555 1_555 1_555 1_555 yes S(21) As(1) C(31) C(36) 117(1) 1_555 1_555 1_555 1_555 yes S(21) C(21) C(22) C(23) 2(1) 1_555 1_555 1_555 1_555 yes S(21) C(21) C(22) C(27) -178.3(10) 1_555 1_555 1_555 1_555 yes S(22) As(1) S(11) C(11) 1.9(6) 1_555 1_555 1_555 1_555 yes S(22) As(1) S(12) C(11) 176.8(5) 1_555 1_555 1_555 1_555 yes S(22) As(1) S(21) C(21) -8.7(4) 1_555 1_555 1_555 1_555 yes S(22) As(1) C(31) C(32) -126(1) 1_555 1_555 1_555 1_555 yes S(22) As(1) C(31) C(36) 51(1) 1_555 1_555 1_555 1_555 yes S(22) C(21) C(22) C(23) -178(1) 1_555 1_555 1_555 1_555 yes S(22) C(21) C(22) C(27) 1(1) 1_555 1_555 1_555 1_555 yes C(11) S(11) As(1) C(31) 104.2(6) 1_555 1_555 1_555 1_555 yes C(11) S(12) As(1) C(31) -85.0(6) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(14) -178(1) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(17) C(16) 178(1) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(14) C(15) -3(2) 1_555 1_555 1_555 1_555 yes C(12) C(17) C(16) C(15) 3(2) 1_555 1_555 1_555 1_555 yes C(13) C(12) C(17) C(16) -4(2) 1_555 1_555 1_555 1_555 yes C(13) C(14) C(15) C(16) 2(2) 1_555 1_555 1_555 1_555 yes C(13) C(14) C(15) C(18) -179(1) 1_555 1_555 1_555 1_555 yes C(14) C(13) C(12) C(17) 4(2) 1_555 1_555 1_555 1_555 yes C(14) C(15) C(16) C(17) -1(2) 1_555 1_555 1_555 1_555 yes C(17) C(16) C(15) C(18) 179(1) 1_555 1_555 1_555 1_555 yes C(21) S(21) As(1) C(31) -109.6(6) 1_555 1_555 1_555 1_555 yes C(21) S(22) As(1) C(31) 91.6(5) 1_555 1_555 1_555 1_555 yes C(21) C(22) C(23) C(24) 179(1) 1_555 1_555 1_555 1_555 yes C(21) C(22) C(27) C(26) -177(1) 1_555 1_555 1_555 1_555 yes C(22) C(23) C(24) C(25) 0(2) 1_555 1_555 1_555 1_555 yes C(22) C(27) C(26) C(25) -2(2) 1_555 1_555 1_555 1_555 yes C(23) C(22) C(27) C(26) 1(2) 1_555 1_555 1_555 1_555 yes C(23) C(24) C(25) C(26) 0(2) 1_555 1_555 1_555 1_555 yes C(23) C(24) C(25) C(28) -179(1) 1_555 1_555 1_555 1_555 yes C(24) C(23) C(22) C(27) 0(2) 1_555 1_555 1_555 1_555 yes C(24) C(25) C(26) C(27) 1(2) 1_555 1_555 1_555 1_555 yes C(27) C(26) C(25) C(28) -178(1) 1_555 1_555 1_555 1_555 yes C(31) C(32) C(33) C(34) -1(2) 1_555 1_555 1_555 1_555 yes C(31) C(36) C(35) C(34) 0(2) 1_555 1_555 1_555 1_555 yes C(32) C(31) C(36) C(35) -1(2) 1_555 1_555 1_555 1_555 yes C(32) C(33) C(34) C(35) 1(2) 1_555 1_555 1_555 1_555 yes C(33) C(32) C(31) C(36) 1(2) 1_555 1_555 1_555 1_555 yes C(33) C(34) C(35) C(36) 0(2) 1_555 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ #===END (4-CH3C6H4CS2)3As data_General _audit_creation_date 'Thu Feb 24 13:39:08 2000' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #------------------------------------------------------------------------------ # SUBMISSION DETAILS _publ_contact_author_name ' ENTER NAME' _publ_contact_author_address ; ENTER ADDRESS ; _publ_contact_author_email ' ENTER EMAIL ADDRESS ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? #------------------------------------------------------------------------------ # TITLE AND AUTHOR LIST _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_footnote _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS FOOTNOTES ; ; FIRST AUTHORS ADDRESS ; _publ_section_synopsis ; ENTER SYNOPSIS ; #------------------------------------------------------------------------------ # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1999). teXsan. Single Crystal Structure Analysis Software. Version 1.10. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #------------------------------------------------------------------------------ data_[4-CH3C6H4CS2]3As #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C24 H21 As S6 ' _chemical_formula_moiety 'C24 H21 As S6 ' _chemical_formula_weight 576.71 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'P -3 ' _symmetry_Int_Tables_number 147 loop_ _symmetry_equiv_pos_as_xyz x,y,z -y,x-y,z -x+y,-x,z -x,-y,-z y,-x+y,-z x-y,x,-z _cell_length_a 18.846(1) _cell_length_b 18.846(1) _cell_length_c 4.855(1) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 1493.4(3) _cell_formula_units_Z 2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.0 _cell_measurement_theta_max 12.4 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.340 _exptl_crystal_size_mid 0.140 _exptl_crystal_size_min 0.140 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.282 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.567 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.824 _exptl_absorpt_correction_T_max 0.995 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 2674 _diffrn_reflns_av_R_equivalents 0.045 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9978 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.9978 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 6 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.65 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 1.4 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 2290 _reflns_number_gt 886 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0710 _refine_ls_wR_factor_ref 0.1017 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 985 _refine_ls_number_parameters 95 _refine_ls_goodness_of_fit_ref 1.887 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00063|Fo|^2^]' _refine_ls_shift/su_max 3.4680 _refine_diff_density_max 0.74 _refine_diff_density_min -0.56 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'As' 'As' 0.050 2.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group As(1) As 0.6667 0.3333 0.2672(5) 0.0472(4) Uani 1.00 d SP . . S(11) S 0.5783(2) 0.1555(2) 0.3956(7) 0.064(1) Uani 1.00 d . . . S(12) S 0.7014(2) 0.2565(2) -0.0162(7) 0.054(1) Uani 1.00 d . . . C(11) C 0.6426(7) 0.1630(7) 0.144(2) 0.046(4) Uani 1.00 d . . . C(12) C 0.6487(8) 0.0945(7) 0.034(2) 0.046(4) Uani 1.00 d . . . C(13) C 0.7020(8) 0.1054(8) -0.170(3) 0.059(5) Uani 1.00 d . . . C(14) C 0.7061(10) 0.0381(10) -0.270(3) 0.081(6) Uani 1.00 d . . . C(15) C 0.653(1) -0.0419(9) -0.178(3) 0.072(5) Uani 1.00 d . . . C(16) C 0.5972(10) -0.0529(8) 0.029(3) 0.075(6) Uani 1.00 d . . . C(17) C 0.5964(8) 0.0143(9) 0.128(3) 0.068(5) Uani 1.00 d . . . C(18) C 0.655(1) -0.1126(9) -0.305(4) 0.107(7) Uani 1.00 d . . . H(11) H 0.7350 0.1601 -0.2471 0.0677 Uiso 1.00 calc . . . H(12) H 0.7475 0.0480 -0.4082 0.1013 Uiso 1.00 calc . . . H(13) H 0.5573 -0.1086 0.1139 0.0899 Uiso 1.00 calc . . . H(14) H 0.5562 0.0086 0.2718 0.0848 Uiso 1.00 calc . . . H(15) H 0.6130 -0.1656 -0.2368 0.1220 Uiso 1.00 calc . . . H(16) H 0.7072 -0.1095 -0.2621 0.1220 Uiso 1.00 calc . . . H(17) H 0.6505 -0.1128 -0.4993 0.1220 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 As(1) 0.046(1) 0.0463 0.049(2) 0.0231 0.0000 0.0000 S(11) 0.072(3) 0.061(2) 0.056(2) 0.030(2) 0.011(2) 0.009(2) S(12) 0.053(2) 0.045(2) 0.063(2) 0.023(2) 0.006(2) 0.000(2) C(11) 0.044(7) 0.041(7) 0.048(8) 0.017(6) -0.002(6) 0.009(6) C(12) 0.053(8) 0.036(7) 0.045(8) 0.020(6) -0.010(6) 0.003(6) C(13) 0.065(9) 0.044(8) 0.07(1) 0.029(7) 0.015(8) 0.006(7) C(14) 0.08(1) 0.08(1) 0.08(1) 0.036(10) 0.012(9) 0.006(9) C(15) 0.09(1) 0.045(9) 0.09(1) 0.041(9) -0.01(1) -0.009(8) C(16) 0.09(1) 0.046(9) 0.10(1) 0.038(9) 0.010(10) 0.002(9) C(17) 0.061(10) 0.07(1) 0.07(1) 0.032(8) -0.004(8) 0.002(8) C(18) 0.15(2) 0.06(1) 0.11(2) 0.06(1) 0.01(1) -0.01(1) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution MITHRIL90 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag As(1) S(11) 2.969(4) . . yes As(1) S(11) 2.969(4) . 2_655 yes As(1) S(11) 2.969(4) . 3_665 yes As(1) S(12) 2.316(4) . . yes As(1) S(12) 2.316(4) . 2_655 yes As(1) S(12) 2.316(4) . 3_665 yes S(11) C(11) 1.68(1) . . yes S(12) C(11) 1.73(1) . . yes C(11) C(12) 1.45(2) . . yes C(12) C(13) 1.35(2) . . yes C(12) C(17) 1.41(2) . . yes C(13) C(14) 1.40(2) . . yes C(13) H(11) 0.975 . . no C(14) C(15) 1.40(2) . . yes C(14) H(12) 0.974 . . no C(15) C(16) 1.40(2) . . yes C(15) C(18) 1.49(2) . . yes C(16) C(17) 1.36(2) . . yes C(16) H(13) 1.023 . . no C(17) H(14) 0.997 . . no C(18) H(15) 0.971 . . no C(18) H(16) 0.977 . . no C(18) H(17) 0.947 . . no #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S(11) As(1) S(11) 115.71(6) . 1_555 2_655 yes S(11) As(1) S(11) 115.71(6) . 1_555 3_665 yes S(11) As(1) S(12) 66.0(1) . 1_555 1_555 yes S(11) As(1) S(12) 153.2(1) . 1_555 2_655 yes S(11) As(1) S(12) 83.6(1) . 1_555 3_665 yes S(11) As(1) S(11) 115.71(6) . 2_655 3_665 yes S(11) As(1) S(12) 83.6(1) . 2_655 1_555 yes S(11) As(1) S(12) 66.0(1) . 2_655 2_655 yes S(11) As(1) S(12) 153.2(1) . 2_655 3_665 yes S(11) As(1) S(12) 153.2(1) . 3_665 1_555 yes S(11) As(1) S(12) 83.6(1) . 3_665 2_655 yes S(11) As(1) S(12) 66.0(1) . 3_665 3_665 yes S(12) As(1) S(12) 88.3(1) . 1_555 2_655 yes S(12) As(1) S(12) 88.3(1) . 1_555 3_665 yes S(12) As(1) S(12) 88.3(1) . 2_655 3_665 yes As(1) S(11) C(11) 77.1(4) . 1_555 1_555 yes As(1) S(12) C(11) 97.6(4) . 1_555 1_555 yes S(11) C(11) S(12) 118.8(7) . 1_555 1_555 yes S(11) C(11) C(12) 124.5(9) . 1_555 1_555 yes S(12) C(11) C(12) 116.4(9) . 1_555 1_555 yes C(11) C(12) C(13) 121(1) . 1_555 1_555 yes C(11) C(12) C(17) 120(1) . 1_555 1_555 yes C(13) C(12) C(17) 117(1) . 1_555 1_555 yes C(12) C(13) C(14) 119(1) . 1_555 1_555 yes C(12) C(13) H(11) 118.4 . 1_555 1_555 no C(14) C(13) H(11) 122.1 . 1_555 1_555 no C(13) C(14) C(15) 122(1) . 1_555 1_555 yes C(13) C(14) H(12) 118.0 . 1_555 1_555 no C(15) C(14) H(12) 119.7 . 1_555 1_555 no C(14) C(15) C(16) 117(1) . 1_555 1_555 yes C(14) C(15) C(18) 120(1) . 1_555 1_555 yes C(16) C(15) C(18) 121(1) . 1_555 1_555 yes C(15) C(16) C(17) 118(1) . 1_555 1_555 yes C(15) C(16) H(13) 123.7 . 1_555 1_555 no C(17) C(16) H(13) 118.0 . 1_555 1_555 no C(12) C(17) C(16) 123(1) . 1_555 1_555 yes C(12) C(17) H(14) 115.5 . 1_555 1_555 no C(16) C(17) H(14) 120.5 . 1_555 1_555 no C(15) C(18) H(15) 114.0 . 1_555 1_555 no C(15) C(18) H(16) 109.3 . 1_555 1_555 no C(15) C(18) H(17) 112.0 . 1_555 1_555 no H(15) C(18) H(16) 105.6 . 1_555 1_555 no H(15) C(18) H(17) 108.0 . 1_555 1_555 no H(16) C(18) H(17) 107.5 . 1_555 1_555 no #------------------------------------------------------------------------------ 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 As(1) S(11) C(11) S(12) -5.4(6) 1_555 1_555 1_555 1_555 yes As(1) S(11) C(11) C(12) 179(1) 1_555 1_555 1_555 1_555 yes As(1) S(11) C(11) S(12) -5.4(6) 1_555 2_655 2_655 2_655 yes As(1) S(11) C(11) C(12) 179(1) 1_555 2_655 2_655 2_655 yes As(1) S(11) C(11) S(12) -5.4(6) 1_555 3_665 3_665 3_665 yes As(1) S(11) C(11) C(12) 179(1) 1_555 3_665 3_665 3_665 yes As(1) S(12) C(11) S(11) 6.8(7) 1_555 1_555 1_555 1_555 yes As(1) S(12) C(11) C(12) -177.7(8) 1_555 1_555 1_555 1_555 yes As(1) S(12) C(11) S(11) 6.8(7) 1_555 2_655 2_655 2_655 yes As(1) S(12) C(11) C(12) -177.7(8) 1_555 2_655 2_655 2_655 yes As(1) S(12) C(11) S(11) 6.8(7) 1_555 3_665 3_665 3_665 yes As(1) S(12) C(11) C(12) -177.7(8) 1_555 3_665 3_665 3_665 yes S(11) As(1) S(11) C(11) 154.3(4) 1_555 1_555 2_655 2_655 yes S(11) As(1) S(11) C(11) -65.7(5) 1_555 1_555 3_665 3_665 yes S(11) As(1) S(12) C(11) -3.7(4) 1_555 1_555 1_555 1_555 yes S(11) As(1) S(12) C(11) -103.6(5) 1_555 1_555 2_655 2_655 yes S(11) As(1) S(12) C(11) 118.2(4) 1_555 1_555 3_665 3_665 yes S(11) C(11) C(12) C(13) 179(1) 1_555 1_555 1_555 1_555 yes S(11) C(11) C(12) C(17) 2(1) 1_555 1_555 1_555 1_555 yes S(12) As(1) S(11) C(11) 3.8(4) 1_555 1_555 1_555 1_555 yes S(12) As(1) S(11) C(11) 94.9(4) 1_555 1_555 2_655 2_655 yes S(12) As(1) S(11) C(11) 21.6(5) 1_555 1_555 3_665 3_665 yes S(12) As(1) S(12) C(11) -87.4(4) 1_555 1_555 2_655 2_655 yes S(12) As(1) S(12) C(11) -175.7(4) 1_555 1_555 3_665 3_665 yes S(12) C(11) C(12) C(13) 4(1) 1_555 1_555 1_555 1_555 yes S(12) C(11) C(12) C(17) -172.4(10) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(14) 179(1) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(17) C(16) 178(1) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(14) C(15) 3(2) 1_555 1_555 1_555 1_555 yes C(12) C(17) C(16) C(15) 0(2) 1_555 1_555 1_555 1_555 yes C(13) C(12) C(17) C(16) 1(2) 1_555 1_555 1_555 1_555 yes C(13) C(14) C(15) C(16) -2(2) 1_555 1_555 1_555 1_555 yes C(13) C(14) C(15) C(18) 175(1) 1_555 1_555 1_555 1_555 yes C(14) C(13) C(12) C(17) -2(2) 1_555 1_555 1_555 1_555 yes C(14) C(15) C(16) C(17) 0(2) 1_555 1_555 1_555 1_555 yes C(17) C(16) C(15) C(18) -176(1) 1_555 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ #===END 4-ClC6H4COSAsPh2 data_General _audit_creation_date 'Thu Feb 24 15:10:46 2000' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #------------------------------------------------------------------------------ # SUBMISSION DETAILS _publ_contact_author_name ' ENTER NAME' _publ_contact_author_address ; ENTER ADDRESS ; _publ_contact_author_email ' ENTER EMAIL ADDRESS ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? #------------------------------------------------------------------------------ # TITLE AND AUTHOR LIST _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_footnote _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS FOOTNOTES ; ; FIRST AUTHORS ADDRESS ; _publ_section_synopsis ; ENTER SYNOPSIS ; #------------------------------------------------------------------------------ # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1999). teXsan. Single Crystal Structure Analysis Software. Version 1.10. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. Zachariasen, W. H. (1967). Acta Cryst. 23, 558-564. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #------------------------------------------------------------------------------ data_4-ClC6H4COSAsPh2 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C19 H14 As Cl O S ' _chemical_formula_moiety 'C19 H14 As Cl O S ' _chemical_formula_weight 400.75 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z x,1/2-y,1/2+z _cell_length_a 5.870(3) _cell_length_b 8.373(3) _cell_length_c 35.147(2) _cell_angle_alpha 90 _cell_angle_beta 90.44(2) _cell_angle_gamma 90 _cell_volume 1727.3(7) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.0 _cell_measurement_theta_max 11.1 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.340 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.140 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.541 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 2.244 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.854 _exptl_absorpt_correction_T_max 0.999 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 4352 _diffrn_reflns_av_R_equivalents 0.017 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 0.9995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.9995 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 45 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 4.72 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 3972 _reflns_number_gt 2587 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.0397 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 2587 _refine_ls_number_parameters 209 _refine_ls_goodness_of_fit_ref 1.353 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00016|Fo|^2^]' _refine_ls_shift/su_max 0.0008 _refine_diff_density_max 0.41 _refine_diff_density_min -0.34 _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.0090(8) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'As' 'As' 0.050 2.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Cl' 'Cl' 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group As(1) As 0.02794(7) 0.52674(4) 0.34584(1) 0.0450(1) Uani 1.00 d . . . Cl(11) Cl 0.7532(2) 0.1122(2) 0.54650(3) 0.0785(4) Uani 1.00 d . . . S(11) S 0.3504(2) 0.4627(1) 0.37848(3) 0.0485(3) Uani 1.00 d . . . O(11) O 0.0219(5) 0.4817(3) 0.42886(8) 0.0633(9) Uani 1.00 d . . . C(11) C 0.2152(7) 0.4371(4) 0.4236(1) 0.045(1) Uani 1.00 d . . . C(12) C 0.3545(6) 0.3565(4) 0.45344(10) 0.042(1) Uani 1.00 d . . . C(13) C 0.2675(7) 0.3472(5) 0.4904(1) 0.053(1) Uani 1.00 d . . . C(14) C 0.3906(8) 0.2719(5) 0.5187(1) 0.059(1) Uani 1.00 d . . . C(15) C 0.5983(7) 0.2048(4) 0.5107(1) 0.052(1) Uani 1.00 d . . . C(16) C 0.6875(7) 0.2114(5) 0.4745(1) 0.054(1) Uani 1.00 d . . . C(17) C 0.5664(6) 0.2899(4) 0.44611(10) 0.047(1) Uani 1.00 d . . . C(21) C 0.1711(6) 0.5402(4) 0.29577(10) 0.046(1) Uani 1.00 d . . . C(22) C 0.3616(8) 0.4536(5) 0.2854(1) 0.071(1) Uani 1.00 d . . . C(23) C 0.4350(9) 0.4571(6) 0.2476(1) 0.085(2) Uani 1.00 d . . . C(24) C 0.3208(9) 0.5436(6) 0.2211(1) 0.073(2) Uani 1.00 d . . . C(25) C 0.1327(9) 0.6278(6) 0.2312(1) 0.077(2) Uani 1.00 d . . . C(26) C 0.0577(7) 0.6284(5) 0.2683(1) 0.064(1) Uani 1.00 d . . . C(31) C 0.0095(6) 0.7547(4) 0.35710(9) 0.0390(9) Uani 1.00 d . . . C(32) C 0.1811(6) 0.8627(4) 0.3484(1) 0.045(1) Uani 1.00 d . . . C(33) C 0.1528(7) 1.0224(4) 0.3584(1) 0.051(1) Uani 1.00 d . . . C(34) C -0.0414(7) 1.0732(4) 0.3766(1) 0.051(1) Uani 1.00 d . . . C(35) C -0.2099(7) 0.9664(4) 0.3851(1) 0.051(1) Uani 1.00 d . . . C(36) C -0.1864(6) 0.8051(4) 0.3756(1) 0.045(1) Uani 1.00 d . . . H(11) H 0.0958 0.4045 0.4935 0.0790 Uiso 1.00 calc . . . H(12) H 0.3206 0.2768 0.5459 0.0790 Uiso 1.00 calc . . . H(13) H 0.8391 0.1621 0.4689 0.0625 Uiso 1.00 calc . . . H(14) H 0.6291 0.2832 0.4164 0.0790 Uiso 1.00 calc . . . H(21) H 0.4594 0.3790 0.3064 0.0790 Uiso 1.00 calc . . . H(22) H 0.5698 0.3962 0.2395 0.0932 Uiso 1.00 calc . . . H(23) H 0.3756 0.5476 0.1944 0.0815 Uiso 1.00 calc . . . H(24) H 0.0503 0.6893 0.2107 0.0824 Uiso 1.00 calc . . . H(25) H -0.1106 0.6812 0.2768 0.0790 Uiso 1.00 calc . . . H(31) H 0.3418 0.8241 0.3336 0.0790 Uiso 1.00 calc . . . H(32) H 0.2728 1.1011 0.3528 0.0574 Uiso 1.00 calc . . . H(33) H -0.0773 1.1934 0.3825 0.0790 Uiso 1.00 calc . . . H(34) H -0.3507 1.0023 0.3980 0.0563 Uiso 1.00 calc . . . H(35) H -0.3275 0.7171 0.3804 0.0790 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 As(1) 0.0460(2) 0.0348(2) 0.0541(2) -0.0035(2) 0.0019(2) -0.0007(2) Cl(11) 0.0873(9) 0.0888(9) 0.0592(7) -0.0068(7) -0.0220(6) 0.0142(6) S(11) 0.0469(5) 0.0489(5) 0.0499(5) 0.0005(5) 0.0073(4) 0.0099(4) O(11) 0.050(2) 0.070(2) 0.070(2) 0.012(1) 0.017(1) 0.012(1) C(11) 0.052(2) 0.032(2) 0.053(2) -0.003(2) 0.010(2) 0.000(2) C(12) 0.049(2) 0.035(2) 0.044(2) -0.003(2) 0.006(2) -0.003(1) C(13) 0.056(2) 0.053(2) 0.051(2) 0.002(2) 0.011(2) -0.003(2) C(14) 0.070(3) 0.065(3) 0.041(2) -0.006(2) 0.009(2) -0.002(2) C(15) 0.066(3) 0.043(2) 0.046(2) -0.008(2) -0.011(2) 0.002(2) C(16) 0.050(2) 0.061(3) 0.051(2) 0.003(2) 0.000(2) 0.001(2) C(17) 0.047(2) 0.049(2) 0.044(2) 0.004(2) 0.006(2) -0.005(2) C(21) 0.056(2) 0.039(2) 0.044(2) -0.003(2) -0.001(2) -0.007(2) C(22) 0.079(3) 0.078(3) 0.055(3) 0.027(3) 0.007(2) 0.003(2) C(23) 0.091(4) 0.106(4) 0.058(3) 0.033(3) 0.013(3) -0.007(3) C(24) 0.097(4) 0.075(3) 0.047(2) 0.003(3) 0.005(2) -0.009(2) C(25) 0.102(4) 0.079(3) 0.051(3) 0.014(3) -0.016(3) -0.001(2) C(26) 0.067(3) 0.072(3) 0.053(3) 0.015(2) -0.006(2) -0.007(2) C(31) 0.045(2) 0.034(2) 0.037(2) 0.001(2) -0.004(2) 0.002(1) C(32) 0.045(2) 0.043(2) 0.048(2) -0.006(2) 0.006(2) 0.000(2) C(33) 0.056(2) 0.042(2) 0.057(2) -0.010(2) 0.005(2) 0.004(2) C(34) 0.064(3) 0.036(2) 0.052(2) 0.000(2) 0.001(2) -0.002(2) C(35) 0.053(2) 0.049(2) 0.051(2) 0.007(2) 0.009(2) -0.005(2) C(36) 0.046(2) 0.044(2) 0.045(2) -0.004(2) 0.003(2) -0.001(2) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SHELXS86 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag As(1) S(11) 2.270(1) . . yes As(1) O(11) 2.943(3) . . yes As(1) C(21) 1.959(4) . . yes As(1) C(31) 1.953(3) . . yes Cl(11) C(15) 1.731(4) . . yes S(11) C(11) 1.793(4) . . yes O(11) C(11) 1.210(4) . . yes C(11) C(12) 1.486(5) . . yes C(12) C(13) 1.403(4) . . yes C(12) C(17) 1.389(5) . . yes C(13) C(14) 1.376(5) . . yes C(13) H(11) 1.122 . . no C(14) C(15) 1.373(5) . . yes C(14) H(12) 1.044 . . no C(15) C(16) 1.379(5) . . yes C(16) C(17) 1.386(5) . . yes C(16) H(13) 1.002 . . no C(17) H(14) 1.112 . . no C(21) C(22) 1.385(5) . . yes C(21) C(26) 1.382(5) . . yes C(22) C(23) 1.397(6) . . yes C(22) H(21) 1.122 . . no C(23) C(24) 1.356(6) . . yes C(23) H(22) 0.986 . . no C(24) C(25) 1.360(6) . . yes C(24) H(23) 0.995 . . no C(25) C(26) 1.380(6) . . yes C(25) H(24) 1.006 . . no C(26) H(25) 1.125 . . no C(31) C(32) 1.390(4) . . yes C(31) C(36) 1.390(4) . . yes C(32) C(33) 1.392(5) . . yes C(32) H(31) 1.128 . . no C(33) C(34) 1.380(5) . . yes C(33) H(32) 0.985 . . no C(34) C(35) 1.368(5) . . yes C(34) H(33) 1.048 . . no C(35) C(36) 1.398(5) . . yes C(35) H(34) 0.993 . . no C(36) H(35) 1.122 . . no #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S(11) As(1) O(11) 58.99(6) . 1_555 1_555 yes S(11) As(1) C(21) 96.1(1) . 1_555 1_555 yes S(11) As(1) C(31) 100.1(1) . 1_555 1_555 yes O(11) As(1) C(21) 155.0(1) . 1_555 1_555 yes O(11) As(1) C(31) 85.6(1) . 1_555 1_555 yes C(21) As(1) C(31) 98.7(1) . 1_555 1_555 yes As(1) S(11) C(11) 95.9(1) . 1_555 1_555 yes As(1) O(11) C(11) 82.6(2) . 1_555 1_555 yes S(11) C(11) O(11) 121.3(3) . 1_555 1_555 yes S(11) C(11) C(12) 115.7(3) . 1_555 1_555 yes O(11) C(11) C(12) 123.0(3) . 1_555 1_555 yes C(11) C(12) C(13) 118.5(3) . 1_555 1_555 yes C(11) C(12) C(17) 122.7(3) . 1_555 1_555 yes C(13) C(12) C(17) 118.8(3) . 1_555 1_555 yes C(12) C(13) C(14) 120.1(4) . 1_555 1_555 yes C(12) C(13) H(11) 113.5 . 1_555 1_555 no C(14) C(13) H(11) 126.4 . 1_555 1_555 no C(13) C(14) C(15) 120.1(4) . 1_555 1_555 yes C(13) C(14) H(12) 115.7 . 1_555 1_555 no C(15) C(14) H(12) 124.0 . 1_555 1_555 no Cl(11) C(15) C(14) 119.8(3) . 1_555 1_555 yes Cl(11) C(15) C(16) 119.2(3) . 1_555 1_555 yes C(14) C(15) C(16) 121.1(4) . 1_555 1_555 yes C(15) C(16) C(17) 119.1(4) . 1_555 1_555 yes C(15) C(16) H(13) 120.5 . 1_555 1_555 no C(17) C(16) H(13) 120.4 . 1_555 1_555 no C(12) C(17) C(16) 120.8(3) . 1_555 1_555 yes C(12) C(17) H(14) 119.9 . 1_555 1_555 no C(16) C(17) H(14) 118.8 . 1_555 1_555 no As(1) C(21) C(22) 124.1(3) . 1_555 1_555 yes As(1) C(21) C(26) 116.8(3) . 1_555 1_555 yes C(22) C(21) C(26) 118.7(4) . 1_555 1_555 yes C(21) C(22) C(23) 119.7(4) . 1_555 1_555 yes C(21) C(22) H(21) 121.8 . 1_555 1_555 no C(23) C(22) H(21) 118.5 . 1_555 1_555 no C(22) C(23) C(24) 120.7(4) . 1_555 1_555 yes C(22) C(23) H(22) 121.3 . 1_555 1_555 no C(24) C(23) H(22) 118.0 . 1_555 1_555 no C(23) C(24) C(25) 119.6(4) . 1_555 1_555 yes C(23) C(24) H(23) 120.4 . 1_555 1_555 no C(25) C(24) H(23) 119.9 . 1_555 1_555 no C(24) C(25) C(26) 121.0(4) . 1_555 1_555 yes C(24) C(25) H(24) 117.7 . 1_555 1_555 no C(26) C(25) H(24) 121.3 . 1_555 1_555 no C(21) C(26) C(25) 120.2(4) . 1_555 1_555 yes C(21) C(26) H(25) 116.3 . 1_555 1_555 no C(25) C(26) H(25) 122.6 . 1_555 1_555 no As(1) C(31) C(32) 123.4(3) . 1_555 1_555 yes As(1) C(31) C(36) 116.0(3) . 1_555 1_555 yes C(32) C(31) C(36) 120.6(3) . 1_555 1_555 yes C(31) C(32) C(33) 118.7(3) . 1_555 1_555 yes C(31) C(32) H(31) 121.7 . 1_555 1_555 no C(33) C(32) H(31) 119.6 . 1_555 1_555 no C(32) C(33) C(34) 121.0(3) . 1_555 1_555 yes C(32) C(33) H(32) 120.4 . 1_555 1_555 no C(34) C(33) H(32) 118.7 . 1_555 1_555 no C(33) C(34) C(35) 120.0(3) . 1_555 1_555 yes C(33) C(34) H(33) 123.7 . 1_555 1_555 no C(35) C(34) H(33) 116.0 . 1_555 1_555 no C(34) C(35) C(36) 120.4(3) . 1_555 1_555 yes C(34) C(35) H(34) 120.5 . 1_555 1_555 no C(36) C(35) H(34) 119.1 . 1_555 1_555 no C(31) C(36) C(35) 119.2(3) . 1_555 1_555 yes C(31) C(36) H(35) 119.1 . 1_555 1_555 no C(35) C(36) H(35) 121.5 . 1_555 1_555 no #------------------------------------------------------------------------------ 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 As(1) S(11) C(11) O(11) -12.8(3) 1_555 1_555 1_555 1_555 yes As(1) S(11) C(11) C(12) 166.4(2) 1_555 1_555 1_555 1_555 yes As(1) O(11) C(11) S(11) 9.9(2) 1_555 1_555 1_555 1_555 yes As(1) O(11) C(11) C(12) -169.3(3) 1_555 1_555 1_555 1_555 yes As(1) C(21) C(22) C(23) 172.5(4) 1_555 1_555 1_555 1_555 yes As(1) C(21) C(26) C(25) -172.2(4) 1_555 1_555 1_555 1_555 yes As(1) C(31) C(32) C(33) -178.7(3) 1_555 1_555 1_555 1_555 yes As(1) C(31) C(36) C(35) 179.0(3) 1_555 1_555 1_555 1_555 yes Cl(11) C(15) C(14) C(13) 179.3(3) 1_555 1_555 1_555 1_555 yes Cl(11) C(15) C(16) C(17) -178.0(3) 1_555 1_555 1_555 1_555 yes S(11) As(1) O(11) C(11) -7.8(2) 1_555 1_555 1_555 1_555 yes S(11) As(1) C(21) C(22) 28.8(4) 1_555 1_555 1_555 1_555 yes S(11) As(1) C(21) C(26) -158.6(3) 1_555 1_555 1_555 1_555 yes S(11) As(1) C(31) C(32) 58.1(3) 1_555 1_555 1_555 1_555 yes S(11) As(1) C(31) C(36) -120.4(3) 1_555 1_555 1_555 1_555 yes S(11) C(11) C(12) C(13) 173.7(3) 1_555 1_555 1_555 1_555 yes S(11) C(11) C(12) C(17) -6.5(4) 1_555 1_555 1_555 1_555 yes O(11) As(1) S(11) C(11) 5.2(1) 1_555 1_555 1_555 1_555 yes O(11) As(1) C(21) C(22) 31.8(5) 1_555 1_555 1_555 1_555 yes O(11) As(1) C(21) C(26) -155.6(3) 1_555 1_555 1_555 1_555 yes O(11) As(1) C(31) C(32) 115.5(3) 1_555 1_555 1_555 1_555 yes O(11) As(1) C(31) C(36) -63.0(3) 1_555 1_555 1_555 1_555 yes O(11) C(11) C(12) C(13) -7.2(5) 1_555 1_555 1_555 1_555 yes O(11) C(11) C(12) C(17) 172.6(3) 1_555 1_555 1_555 1_555 yes C(11) S(11) As(1) C(21) -176.3(1) 1_555 1_555 1_555 1_555 yes C(11) S(11) As(1) C(31) 83.8(1) 1_555 1_555 1_555 1_555 yes C(11) O(11) As(1) C(21) -11.2(4) 1_555 1_555 1_555 1_555 yes C(11) O(11) As(1) C(31) -112.3(2) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(14) 179.3(3) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(17) C(16) -178.0(3) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(14) C(15) -0.4(6) 1_555 1_555 1_555 1_555 yes C(12) C(17) C(16) C(15) -2.2(6) 1_555 1_555 1_555 1_555 yes C(13) C(12) C(17) C(16) 1.8(5) 1_555 1_555 1_555 1_555 yes C(13) C(14) C(15) C(16) 0.0(6) 1_555 1_555 1_555 1_555 yes C(14) C(13) C(12) C(17) -0.5(5) 1_555 1_555 1_555 1_555 yes C(14) C(15) C(16) C(17) 1.2(6) 1_555 1_555 1_555 1_555 yes C(21) As(1) C(31) C(32) -39.7(3) 1_555 1_555 1_555 1_555 yes C(21) As(1) C(31) C(36) 141.8(3) 1_555 1_555 1_555 1_555 yes C(21) C(22) C(23) C(24) -0.4(8) 1_555 1_555 1_555 1_555 yes C(21) C(26) C(25) C(24) -1.3(7) 1_555 1_555 1_555 1_555 yes C(22) C(21) As(1) C(31) 130.1(4) 1_555 1_555 1_555 1_555 yes C(22) C(21) C(26) C(25) 0.8(7) 1_555 1_555 1_555 1_555 yes C(22) C(23) C(24) C(25) 0.0(8) 1_555 1_555 1_555 1_555 yes C(23) C(22) C(21) C(26) 0.1(7) 1_555 1_555 1_555 1_555 yes C(23) C(24) C(25) C(26) 0.9(8) 1_555 1_555 1_555 1_555 yes C(26) C(21) As(1) C(31) -57.4(3) 1_555 1_555 1_555 1_555 yes C(31) C(32) C(33) C(34) 0.0(6) 1_555 1_555 1_555 1_555 yes C(31) C(36) C(35) C(34) -0.5(6) 1_555 1_555 1_555 1_555 yes C(32) C(31) C(36) C(35) 0.5(5) 1_555 1_555 1_555 1_555 yes C(32) C(33) C(34) C(35) 0.0(6) 1_555 1_555 1_555 1_555 yes C(33) C(32) C(31) C(36) -0.2(5) 1_555 1_555 1_555 1_555 yes C(33) C(34) C(35) C(36) 0.3(6) 1_555 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag As(1) O(11) 2.943(3) . . ? Cl(11) C(34) 3.537(4) . 3_666 ? Cl(11) C(33) 3.567(4) . 3_666 ? O(11) C(17) 3.181(5) . 1_455 ? O(11) C(16) 3.405(5) . 1_455 ? C(12) C(14) 3.585(5) . 3_666 ? #------------------------------------------------------------------------------ #===END (4-CH3OC6H4COS)2AsPh data_General _audit_creation_date 'Thu Feb 24 14:49:39 2000' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #------------------------------------------------------------------------------ # SUBMISSION DETAILS _publ_contact_author_name ' ENTER NAME' _publ_contact_author_address ; ENTER ADDRESS ; _publ_contact_author_email ' ENTER EMAIL ADDRESS ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? #------------------------------------------------------------------------------ # TITLE AND AUTHOR LIST _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_footnote _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS FOOTNOTES ; ; FIRST AUTHORS ADDRESS ; _publ_section_synopsis ; ENTER SYNOPSIS ; #------------------------------------------------------------------------------ # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1999). teXsan. Single Crystal Structure Analysis Software. Version 1.10. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #------------------------------------------------------------------------------ data_[4-CH3OC6H4COS]2AsPh #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C22 H19 As O4 S2 ' _chemical_formula_moiety 'C22 H19 As O4 S2 ' _chemical_formula_weight 486.43 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 11.304(2) _cell_length_b 12.119(2) _cell_length_c 8.725(1) _cell_angle_alpha 99.71(1) _cell_angle_beta 101.91(1) _cell_angle_gamma 110.14(1) _cell_volume 1060.0(3) _cell_formula_units_Z 2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.0 _cell_measurement_theta_max 11.9 _cell_measurement_temperature 193.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.340 _exptl_crystal_size_mid 0.340 _exptl_crystal_size_min 0.170 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.524 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.826 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.807 _exptl_absorpt_correction_T_max 0.998 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 5114 _diffrn_reflns_av_R_equivalents 0.044 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 1.0002 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.0002 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.75 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 4880 _reflns_number_gt 3055 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.0414 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3055 _refine_ls_number_parameters 262 _refine_ls_goodness_of_fit_ref 1.218 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00022|Fo|^2^]' _refine_ls_shift/su_max 0.0376 _refine_diff_density_max 0.38 _refine_diff_density_min -0.38 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'As' 'As' 0.050 2.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group As(1) As 0.55065(4) 0.68649(4) 0.19008(5) 0.0300(1) Uani 1.00 d . . . S(11) S 0.3478(1) 0.6101(1) 0.0052(1) 0.0359(3) Uani 1.00 d . . . S(21) S 0.5936(1) 0.8643(1) 0.1148(1) 0.0355(3) Uani 1.00 d . . . O(11) O 0.3833(3) 0.4594(3) 0.1730(4) 0.0430(9) Uani 1.00 d . . . O(12) O -0.1884(3) 0.0973(3) -0.2662(4) 0.0503(10) Uani 1.00 d . . . O(21) O 0.7820(3) 0.8780(3) 0.3576(3) 0.0375(9) Uani 1.00 d . . . O(22) O 1.0529(3) 1.4244(3) 0.3177(4) 0.0497(10) Uani 1.00 d . . . C(11) C 0.3047(4) 0.4716(4) 0.0647(5) 0.032(1) Uani 1.00 d . . . C(12) C 0.1741(4) 0.3748(4) -0.0230(5) 0.030(1) Uani 1.00 d . . . C(13) C 0.1517(4) 0.2576(4) -0.0078(5) 0.034(1) Uani 1.00 d . . . C(14) C 0.0331(4) 0.1619(4) -0.0889(5) 0.036(1) Uani 1.00 d . . . C(15) C -0.0668(4) 0.1842(4) -0.1831(5) 0.036(1) Uani 1.00 d . . . C(16) C -0.0465(4) 0.3017(4) -0.1988(6) 0.044(1) Uani 1.00 d . . . C(17) C 0.0739(4) 0.3958(4) -0.1192(5) 0.038(1) Uani 1.00 d . . . C(18) C -0.2152(5) -0.0244(4) -0.2599(6) 0.051(1) Uani 1.00 d . . . C(21) C 0.7500(4) 0.9353(4) 0.2669(5) 0.032(1) Uani 1.00 d . . . C(22) C 0.8291(4) 1.0622(4) 0.2743(5) 0.030(1) Uani 1.00 d . . . C(23) C 0.9457(4) 1.1240(4) 0.4017(5) 0.037(1) Uani 1.00 d . . . C(24) C 1.0242(4) 1.2445(4) 0.4198(5) 0.039(1) Uani 1.00 d . . . C(25) C 0.9851(4) 1.3053(4) 0.3100(5) 0.035(1) Uani 1.00 d . . . C(26) C 0.8711(4) 1.2449(4) 0.1827(5) 0.037(1) Uani 1.00 d . . . C(27) C 0.7948(4) 1.1249(4) 0.1658(5) 0.032(1) Uani 1.00 d . . . C(28) C 1.1734(5) 1.4896(5) 0.4443(7) 0.068(2) Uani 1.00 d . . . C(31) C 0.4972(4) 0.7308(3) 0.3830(4) 0.0261(10) Uani 1.00 d . . . C(32) C 0.4328(4) 0.8090(4) 0.4003(5) 0.032(1) Uani 1.00 d . . . C(33) C 0.3985(4) 0.8344(4) 0.5406(5) 0.038(1) Uani 1.00 d . . . C(34) C 0.4276(4) 0.7824(4) 0.6653(5) 0.039(1) Uani 1.00 d . . . C(35) C 0.4908(4) 0.7036(4) 0.6479(5) 0.037(1) Uani 1.00 d . . . C(36) C 0.5250(4) 0.6770(4) 0.5067(5) 0.031(1) Uani 1.00 d . . . H(11) H 0.2203 0.2429 0.0611 0.0416 Uiso 1.00 calc . . . H(12) H 0.0060 0.0784 -0.0751 0.0562 Uiso 1.00 calc . . . H(13) H -0.1159 0.3091 -0.3026 0.0562 Uiso 1.00 calc . . . H(14) H 0.0862 0.4811 -0.1442 0.0562 Uiso 1.00 calc . . . H(15) H -0.1537 -0.0533 -0.2995 0.0597 Uiso 1.00 calc . . . H(16) H -0.2054 -0.0322 -0.1502 0.0597 Uiso 1.00 calc . . . H(17) H -0.3015 -0.0787 -0.3240 0.0597 Uiso 1.00 calc . . . H(21) H 0.9705 1.0839 0.4936 0.0562 Uiso 1.00 calc . . . H(22) H 1.1152 1.2866 0.5110 0.0562 Uiso 1.00 calc . . . H(23) H 0.8370 1.2917 0.0988 0.0562 Uiso 1.00 calc . . . H(24) H 0.7173 1.0801 0.0681 0.0562 Uiso 1.00 calc . . . H(25) H 1.1699 1.4959 0.5657 0.0562 Uiso 1.00 calc . . . H(26) H 1.2357 1.4451 0.4283 0.0562 Uiso 1.00 calc . . . H(27) H 1.2061 1.5736 0.4291 0.0562 Uiso 1.00 calc . . . H(31) H 0.4084 0.8498 0.3072 0.0562 Uiso 1.00 calc . . . H(32) H 0.3538 0.8897 0.5528 0.0441 Uiso 1.00 calc . . . H(33) H 0.3833 0.7849 0.7625 0.0562 Uiso 1.00 calc . . . H(34) H 0.5027 0.6582 0.7221 0.0562 Uiso 1.00 calc . . . H(35) H 0.5680 0.6206 0.4930 0.0372 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 As(1) 0.0270(2) 0.0287(2) 0.0323(2) 0.0111(2) 0.0071(2) 0.0039(2) S(11) 0.0348(6) 0.0311(6) 0.0328(6) 0.0068(5) 0.0020(5) 0.0079(5) S(21) 0.0308(6) 0.0367(6) 0.0320(6) 0.0067(5) 0.0040(4) 0.0111(5) O(11) 0.039(2) 0.031(2) 0.049(2) 0.012(1) -0.004(1) 0.008(1) O(12) 0.033(2) 0.037(2) 0.064(2) 0.002(2) -0.003(2) 0.014(2) O(21) 0.036(2) 0.034(2) 0.040(2) 0.011(1) 0.004(1) 0.016(1) O(22) 0.040(2) 0.030(2) 0.070(2) 0.006(2) 0.006(2) 0.019(2) C(11) 0.032(2) 0.028(2) 0.035(2) 0.013(2) 0.009(2) 0.004(2) C(12) 0.035(2) 0.024(2) 0.033(2) 0.013(2) 0.010(2) 0.004(2) C(13) 0.029(2) 0.031(2) 0.041(2) 0.012(2) 0.005(2) 0.009(2) C(14) 0.034(2) 0.027(2) 0.047(3) 0.011(2) 0.013(2) 0.010(2) C(15) 0.027(2) 0.032(2) 0.041(2) 0.006(2) 0.005(2) 0.006(2) C(16) 0.035(2) 0.036(3) 0.050(3) 0.006(2) -0.002(2) 0.013(2) C(17) 0.035(2) 0.031(2) 0.046(3) 0.011(2) 0.004(2) 0.016(2) C(18) 0.043(3) 0.037(3) 0.055(3) 0.000(2) 0.009(2) 0.006(2) C(21) 0.028(2) 0.036(2) 0.030(2) 0.010(2) 0.009(2) 0.006(2) C(22) 0.029(2) 0.030(2) 0.031(2) 0.010(2) 0.010(2) 0.007(2) C(23) 0.033(2) 0.037(3) 0.042(3) 0.013(2) 0.007(2) 0.015(2) C(24) 0.030(2) 0.035(3) 0.046(3) 0.006(2) 0.005(2) 0.012(2) C(25) 0.035(2) 0.030(2) 0.044(2) 0.014(2) 0.015(2) 0.011(2) C(26) 0.037(3) 0.041(3) 0.041(2) 0.020(2) 0.012(2) 0.018(2) C(27) 0.027(2) 0.038(3) 0.031(2) 0.012(2) 0.007(2) 0.010(2) C(28) 0.047(3) 0.037(3) 0.095(4) 0.000(3) -0.005(3) 0.022(3) C(31) 0.023(2) 0.023(2) 0.028(2) 0.005(2) 0.005(2) 0.003(2) C(32) 0.031(2) 0.034(2) 0.034(2) 0.016(2) 0.007(2) 0.010(2) C(33) 0.034(2) 0.044(3) 0.041(2) 0.021(2) 0.013(2) 0.009(2) C(34) 0.034(2) 0.052(3) 0.032(2) 0.018(2) 0.009(2) 0.012(2) C(35) 0.034(2) 0.045(3) 0.033(2) 0.014(2) 0.006(2) 0.020(2) C(36) 0.027(2) 0.029(2) 0.035(2) 0.010(2) 0.006(2) 0.011(2) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SHELXS86 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag As(1) S(11) 2.286(1) . . yes As(1) S(21) 2.280(1) . . yes As(1) O(11) 2.708(3) . . yes As(1) O(21) 2.731(3) . . yes As(1) C(31) 1.956(4) . . yes S(11) C(11) 1.776(4) . . yes S(21) C(21) 1.796(4) . . yes O(11) C(11) 1.223(5) . . yes O(12) C(15) 1.363(5) . . yes O(12) C(18) 1.413(6) . . yes O(21) C(21) 1.217(5) . . yes O(22) C(25) 1.363(5) . . yes O(22) C(28) 1.429(6) . . yes C(11) C(12) 1.477(5) . . yes C(12) C(13) 1.389(5) . . yes C(12) C(17) 1.389(5) . . yes C(13) C(14) 1.380(6) . . yes C(13) H(11) 0.966 . . no C(14) C(15) 1.388(6) . . yes C(14) H(12) 0.988 . . no C(15) C(16) 1.397(6) . . yes C(16) C(17) 1.381(6) . . yes C(16) H(13) 1.107 . . no C(17) H(14) 1.061 . . no C(18) H(15) 0.975 . . no C(18) H(16) 0.965 . . no C(18) H(17) 0.952 . . no C(21) C(22) 1.471(6) . . yes C(22) C(23) 1.403(5) . . yes C(22) C(27) 1.385(5) . . yes C(23) C(24) 1.384(6) . . yes C(23) H(21) 1.044 . . no C(24) C(25) 1.394(6) . . yes C(24) H(22) 1.056 . . no C(25) C(26) 1.384(6) . . yes C(26) C(27) 1.376(6) . . yes C(26) H(23) 1.086 . . no C(27) H(24) 0.998 . . no C(28) H(25) 1.060 . . no C(28) H(26) 1.040 . . no C(28) H(27) 0.998 . . no C(31) C(32) 1.387(5) . . yes C(31) C(36) 1.387(5) . . yes C(32) C(33) 1.376(5) . . yes C(32) H(31) 1.057 . . no C(33) C(34) 1.384(6) . . yes C(33) H(32) 0.973 . . no C(34) C(35) 1.383(6) . . yes C(34) H(33) 1.071 . . no C(35) C(36) 1.385(6) . . yes C(35) H(34) 0.935 . . no C(36) H(35) 0.971 . . no #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S(11) As(1) S(21) 88.46(4) . 1_555 1_555 yes S(11) As(1) O(11) 62.28(7) . 1_555 1_555 yes S(11) As(1) O(21) 150.18(7) . 1_555 1_555 yes S(11) As(1) C(31) 97.6(1) . 1_555 1_555 yes S(21) As(1) O(11) 150.59(7) . 1_555 1_555 yes S(21) As(1) O(21) 62.08(6) . 1_555 1_555 yes S(21) As(1) C(31) 98.8(1) . 1_555 1_555 yes O(11) As(1) O(21) 146.57(8) . 1_555 1_555 yes O(11) As(1) C(31) 83.2(1) . 1_555 1_555 yes O(21) As(1) C(31) 83.5(1) . 1_555 1_555 yes As(1) S(11) C(11) 90.9(1) . 1_555 1_555 yes As(1) S(21) C(21) 91.5(1) . 1_555 1_555 yes As(1) O(11) C(11) 87.2(3) . 1_555 1_555 yes C(15) O(12) C(18) 118.6(4) . 1_555 1_555 yes As(1) O(21) C(21) 87.4(2) . 1_555 1_555 yes C(25) O(22) C(28) 117.6(4) . 1_555 1_555 yes S(11) C(11) O(11) 119.7(3) . 1_555 1_555 yes S(11) C(11) C(12) 117.4(3) . 1_555 1_555 yes O(11) C(11) C(12) 122.9(4) . 1_555 1_555 yes C(11) C(12) C(13) 117.9(4) . 1_555 1_555 yes C(11) C(12) C(17) 123.1(4) . 1_555 1_555 yes C(13) C(12) C(17) 119.1(4) . 1_555 1_555 yes C(12) C(13) C(14) 121.2(4) . 1_555 1_555 yes C(12) C(13) H(11) 119.3 . 1_555 1_555 no C(14) C(13) H(11) 119.5 . 1_555 1_555 no C(13) C(14) C(15) 119.3(4) . 1_555 1_555 yes C(13) C(14) H(12) 126.0 . 1_555 1_555 no C(15) C(14) H(12) 114.2 . 1_555 1_555 no O(12) C(15) C(14) 124.4(4) . 1_555 1_555 yes O(12) C(15) C(16) 115.3(4) . 1_555 1_555 yes C(14) C(15) C(16) 120.4(4) . 1_555 1_555 yes C(15) C(16) C(17) 119.5(4) . 1_555 1_555 yes C(15) C(16) H(13) 116.5 . 1_555 1_555 no C(17) C(16) H(13) 121.4 . 1_555 1_555 no C(12) C(17) C(16) 120.7(4) . 1_555 1_555 yes C(12) C(17) H(14) 123.3 . 1_555 1_555 no C(16) C(17) H(14) 115.9 . 1_555 1_555 no O(12) C(18) H(15) 110.9 . 1_555 1_555 no O(12) C(18) H(16) 111.6 . 1_555 1_555 no O(12) C(18) H(17) 112.4 . 1_555 1_555 no H(15) C(18) H(16) 106.2 . 1_555 1_555 no H(15) C(18) H(17) 107.3 . 1_555 1_555 no H(16) C(18) H(17) 108.1 . 1_555 1_555 no S(21) C(21) O(21) 119.1(3) . 1_555 1_555 yes S(21) C(21) C(22) 116.2(3) . 1_555 1_555 yes O(21) C(21) C(22) 124.7(4) . 1_555 1_555 yes C(21) C(22) C(23) 117.6(4) . 1_555 1_555 yes C(21) C(22) C(27) 124.3(4) . 1_555 1_555 yes C(23) C(22) C(27) 118.1(4) . 1_555 1_555 yes C(22) C(23) C(24) 121.3(4) . 1_555 1_555 yes C(22) C(23) H(21) 120.9 . 1_555 1_555 no C(24) C(23) H(21) 117.5 . 1_555 1_555 no C(23) C(24) C(25) 119.0(4) . 1_555 1_555 yes C(23) C(24) H(22) 119.6 . 1_555 1_555 no C(25) C(24) H(22) 121.3 . 1_555 1_555 no O(22) C(25) C(24) 124.2(4) . 1_555 1_555 yes O(22) C(25) C(26) 115.5(4) . 1_555 1_555 yes C(24) C(25) C(26) 120.3(4) . 1_555 1_555 yes C(25) C(26) C(27) 119.9(4) . 1_555 1_555 yes C(25) C(26) H(23) 121.4 . 1_555 1_555 no C(27) C(26) H(23) 118.7 . 1_555 1_555 no C(22) C(27) C(26) 121.5(4) . 1_555 1_555 yes C(22) C(27) H(24) 119.2 . 1_555 1_555 no C(26) C(27) H(24) 119.2 . 1_555 1_555 no O(22) C(28) H(25) 117.8 . 1_555 1_555 no O(22) C(28) H(26) 107.1 . 1_555 1_555 no O(22) C(28) H(27) 104.8 . 1_555 1_555 no H(25) C(28) H(26) 105.8 . 1_555 1_555 no H(25) C(28) H(27) 108.5 . 1_555 1_555 no H(26) C(28) H(27) 113.1 . 1_555 1_555 no As(1) C(31) C(32) 124.2(3) . 1_555 1_555 yes As(1) C(31) C(36) 116.1(3) . 1_555 1_555 yes C(32) C(31) C(36) 119.7(4) . 1_555 1_555 yes C(31) C(32) C(33) 120.1(4) . 1_555 1_555 yes C(31) C(32) H(31) 121.4 . 1_555 1_555 no C(33) C(32) H(31) 118.6 . 1_555 1_555 no C(32) C(33) C(34) 120.5(4) . 1_555 1_555 yes C(32) C(33) H(32) 119.9 . 1_555 1_555 no C(34) C(33) H(32) 119.5 . 1_555 1_555 no C(33) C(34) C(35) 119.6(4) . 1_555 1_555 yes C(33) C(34) H(33) 121.1 . 1_555 1_555 no C(35) C(34) H(33) 117.8 . 1_555 1_555 no C(34) C(35) C(36) 120.2(4) . 1_555 1_555 yes C(34) C(35) H(34) 122.8 . 1_555 1_555 no C(36) C(35) H(34) 116.5 . 1_555 1_555 no C(31) C(36) C(35) 120.0(4) . 1_555 1_555 yes C(31) C(36) H(35) 119.5 . 1_555 1_555 no C(35) C(36) H(35) 120.6 . 1_555 1_555 no #------------------------------------------------------------------------------ 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 As(1) S(11) C(11) O(11) 1.0(3) 1_555 1_555 1_555 1_555 yes As(1) S(11) C(11) C(12) -178.0(3) 1_555 1_555 1_555 1_555 yes As(1) S(21) C(21) O(21) -2.2(3) 1_555 1_555 1_555 1_555 yes As(1) S(21) C(21) C(22) 179.3(3) 1_555 1_555 1_555 1_555 yes As(1) O(11) C(11) S(11) -0.9(3) 1_555 1_555 1_555 1_555 yes As(1) O(11) C(11) C(12) 178.1(4) 1_555 1_555 1_555 1_555 yes As(1) O(21) C(21) S(21) 1.9(3) 1_555 1_555 1_555 1_555 yes As(1) O(21) C(21) C(22) -179.9(4) 1_555 1_555 1_555 1_555 yes As(1) C(31) C(32) C(33) 179.7(3) 1_555 1_555 1_555 1_555 yes As(1) C(31) C(36) C(35) 179.8(3) 1_555 1_555 1_555 1_555 yes S(11) As(1) S(21) C(21) 176.1(1) 1_555 1_555 1_555 1_555 yes S(11) As(1) O(11) C(11) 0.7(2) 1_555 1_555 1_555 1_555 yes S(11) As(1) O(21) C(21) -11.2(3) 1_555 1_555 1_555 1_555 yes S(11) As(1) C(31) C(32) -57.1(3) 1_555 1_555 1_555 1_555 yes S(11) As(1) C(31) C(36) 121.6(3) 1_555 1_555 1_555 1_555 yes S(11) C(11) C(12) C(13) 164.1(3) 1_555 1_555 1_555 1_555 yes S(11) C(11) C(12) C(17) -15.8(5) 1_555 1_555 1_555 1_555 yes S(21) As(1) S(11) C(11) -177.4(1) 1_555 1_555 1_555 1_555 yes S(21) As(1) O(11) C(11) 7.0(3) 1_555 1_555 1_555 1_555 yes S(21) As(1) O(21) C(21) -1.5(2) 1_555 1_555 1_555 1_555 yes S(21) As(1) C(31) C(32) 32.5(3) 1_555 1_555 1_555 1_555 yes S(21) As(1) C(31) C(36) -148.7(3) 1_555 1_555 1_555 1_555 yes S(21) C(21) C(22) C(23) 173.9(3) 1_555 1_555 1_555 1_555 yes S(21) C(21) C(22) C(27) -4.9(5) 1_555 1_555 1_555 1_555 yes O(11) As(1) S(11) C(11) -0.5(1) 1_555 1_555 1_555 1_555 yes O(11) As(1) S(21) C(21) 170.6(2) 1_555 1_555 1_555 1_555 yes O(11) As(1) O(21) C(21) -172.2(2) 1_555 1_555 1_555 1_555 yes O(11) As(1) C(31) C(32) -117.9(3) 1_555 1_555 1_555 1_555 yes O(11) As(1) C(31) C(36) 60.9(3) 1_555 1_555 1_555 1_555 yes O(11) C(11) C(12) C(13) -14.9(6) 1_555 1_555 1_555 1_555 yes O(11) C(11) C(12) C(17) 165.2(4) 1_555 1_555 1_555 1_555 yes O(12) C(15) C(14) C(13) -178.9(4) 1_555 1_555 1_555 1_555 yes O(12) C(15) C(16) C(17) -179.9(4) 1_555 1_555 1_555 1_555 yes O(21) As(1) S(11) C(11) -168.7(2) 1_555 1_555 1_555 1_555 yes O(21) As(1) S(21) C(21) 1.0(1) 1_555 1_555 1_555 1_555 yes O(21) As(1) O(11) C(11) 170.1(2) 1_555 1_555 1_555 1_555 yes O(21) As(1) C(31) C(32) 92.8(3) 1_555 1_555 1_555 1_555 yes O(21) As(1) C(31) C(36) -88.4(3) 1_555 1_555 1_555 1_555 yes O(21) C(21) C(22) C(23) -4.5(6) 1_555 1_555 1_555 1_555 yes O(21) C(21) C(22) C(27) 176.8(4) 1_555 1_555 1_555 1_555 yes O(22) C(25) C(24) C(23) 178.6(4) 1_555 1_555 1_555 1_555 yes O(22) C(25) C(26) C(27) -179.1(4) 1_555 1_555 1_555 1_555 yes C(11) S(11) As(1) C(31) -78.7(2) 1_555 1_555 1_555 1_555 yes C(11) O(11) As(1) C(31) 103.0(3) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(14) -178.6(4) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(17) C(16) 179.9(4) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(14) C(15) -2.1(6) 1_555 1_555 1_555 1_555 yes C(12) C(17) C(16) C(15) -0.5(7) 1_555 1_555 1_555 1_555 yes C(13) C(12) C(17) C(16) 0.0(7) 1_555 1_555 1_555 1_555 yes C(13) C(14) C(15) C(16) 1.6(7) 1_555 1_555 1_555 1_555 yes C(14) C(13) C(12) C(17) 1.3(6) 1_555 1_555 1_555 1_555 yes C(14) C(15) O(12) C(18) -1.3(6) 1_555 1_555 1_555 1_555 yes C(14) C(15) C(16) C(17) -0.3(7) 1_555 1_555 1_555 1_555 yes C(16) C(15) O(12) C(18) 178.2(4) 1_555 1_555 1_555 1_555 yes C(21) S(21) As(1) C(31) 78.7(2) 1_555 1_555 1_555 1_555 yes C(21) O(21) As(1) C(31) -105.1(3) 1_555 1_555 1_555 1_555 yes C(21) C(22) C(23) C(24) -178.4(4) 1_555 1_555 1_555 1_555 yes C(21) C(22) C(27) C(26) 177.8(4) 1_555 1_555 1_555 1_555 yes C(22) C(23) C(24) C(25) 0.8(7) 1_555 1_555 1_555 1_555 yes C(22) C(27) C(26) C(25) 0.3(6) 1_555 1_555 1_555 1_555 yes C(23) C(22) C(27) C(26) -1.0(6) 1_555 1_555 1_555 1_555 yes C(23) C(24) C(25) C(26) -1.5(6) 1_555 1_555 1_555 1_555 yes C(24) C(23) C(22) C(27) 0.4(6) 1_555 1_555 1_555 1_555 yes C(24) C(25) O(22) C(28) 1.7(6) 1_555 1_555 1_555 1_555 yes C(24) C(25) C(26) C(27) 1.0(6) 1_555 1_555 1_555 1_555 yes C(26) C(25) O(22) C(28) -178.2(4) 1_555 1_555 1_555 1_555 yes C(31) C(32) C(33) C(34) -0.1(6) 1_555 1_555 1_555 1_555 yes C(31) C(36) C(35) C(34) 0.8(6) 1_555 1_555 1_555 1_555 yes C(32) C(31) C(36) C(35) -1.3(6) 1_555 1_555 1_555 1_555 yes C(32) C(33) C(34) C(35) -0.5(7) 1_555 1_555 1_555 1_555 yes C(33) C(32) C(31) C(36) 1.0(6) 1_555 1_555 1_555 1_555 yes C(33) C(34) C(35) C(36) 0.2(7) 1_555 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ #===END (4-CH3C6H4COS)3As data_General _audit_creation_date 'Thu Feb 24 14:29:32 2000' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #------------------------------------------------------------------------------ # SUBMISSION DETAILS _publ_contact_author_name ' ENTER NAME' _publ_contact_author_address ; ENTER ADDRESS ; _publ_contact_author_email ' ENTER EMAIL ADDRESS ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? #------------------------------------------------------------------------------ # TITLE AND AUTHOR LIST _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_footnote _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS FOOTNOTES ; ; FIRST AUTHORS ADDRESS ; _publ_section_synopsis ; ENTER SYNOPSIS ; #------------------------------------------------------------------------------ # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1999). teXsan. Single Crystal Structure Analysis Software. Version 1.10. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #------------------------------------------------------------------------------ data_(4-CH3C6H4COS)3As #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C24 H21 As O3 S3 ' _chemical_formula_moiety 'C24 H21 As O3 S3 ' _chemical_formula_weight 528.53 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R 3 c ' _symmetry_Int_Tables_number 161 loop_ _symmetry_equiv_pos_as_xyz x,y,z -y,x-y,z -x+y,-x,z -y,-x,1/2+z x,x-y,1/2+z -x+y,y,1/2+z 2/3+x,1/3+y,1/3+z 2/3-y,1/3+x-y,1/3+z 2/3-x+y,1/3-x,1/3+z 2/3-y,1/3-x,5/6+z 2/3+x,1/3+x-y,5/6+z 2/3-x+y,1/3+y,5/6+z 1/3+x,2/3+y,2/3+z 1/3-y,2/3+x-y,2/3+z 1/3-x+y,2/3-x,2/3+z 1/3-y,2/3-x,+z 1/3+x,2/3+x-y,+z 1/3-x+y,2/3+y,+z _cell_length_a 13.587(1) _cell_length_b 13.587(1) _cell_length_c 27.285(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 4362.0(5) _cell_formula_units_Z 8 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.1 _cell_measurement_theta_max 12.1 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.260 _exptl_crystal_size_mid 0.230 _exptl_crystal_size_min 0.230 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.610 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.872 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 2396 _diffrn_reflns_av_R_equivalents 0.075 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.49 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 35 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 5.79 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 1145 _reflns_number_gt 607 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0667 _refine_ls_wR_factor_ref 0.2306 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 607 _refine_ls_number_parameters 94 _refine_ls_goodness_of_fit_ref 1.278 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0090 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack -0.06(6) _refine_diff_density_max 0.74 _refine_diff_density_min -0.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; 'As' 'As' 0.050 2.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group As(1) As 1.0000 0.0000 0.5340(1) 0.0529(7) Uani 1.00 d SP . . S(11) S 0.9565(3) 0.1125(3) 0.4886(2) 0.062(1) Uani 1.00 d . . . O(11) O 1.1019(9) 0.2329(9) 0.5562(4) 0.076(3) Uani 1.00 d . . . C(11) C 1.042(1) 0.236(1) 0.5257(6) 0.061(4) Uani 1.00 d . . . C(12) C 1.035(1) 0.338(1) 0.5127(5) 0.064(4) Uani 1.00 d . . . C(13) C 1.104(2) 0.438(1) 0.5388(7) 0.083(5) Uani 1.00 d . . . C(14) C 1.096(2) 0.533(2) 0.5289(10) 0.123(10) Uani 1.00 d . . . C(15) C 1.017(2) 0.530(2) 0.4976(8) 0.118(9) Uani 1.00 d . . . C(16) C 0.958(2) 0.436(2) 0.4681(8) 0.121(9) Uani 1.00 d . . . C(17) C 0.961(2) 0.338(2) 0.4774(8) 0.100(7) Uani 1.00 d . . . C(18) C 1.007(4) 0.638(2) 0.490(1) 0.23(2) Uani 1.00 d . . . H(11) H 1.1554 0.4383 0.5636 0.0967 Uiso 1.00 calc . . . H(12) H 1.1545 0.6055 0.5430 0.1567 Uiso 1.00 calc . . . H(13) H 0.9119 0.4378 0.4416 0.1505 Uiso 1.00 calc . . . H(14) H 0.9121 0.2693 0.4598 0.1202 Uiso 1.00 calc . . . H(15) H 1.0511 0.6953 0.5116 0.2840 Uiso 1.00 calc . . . H(16) H 1.0236 0.6639 0.4566 0.2840 Uiso 1.00 calc . . . H(17) H 0.9265 0.6161 0.4951 0.2840 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 As(1) 0.0527(8) 0.0527(8) 0.053(1) 0.0264(4) 0.0000 0.0000 S(11) 0.064(2) 0.057(2) 0.067(2) 0.032(2) -0.019(2) -0.013(2) O(11) 0.069(7) 0.070(7) 0.087(7) 0.033(6) -0.044(6) -0.015(6) C(11) 0.050(8) 0.053(9) 0.073(9) 0.021(7) -0.012(8) -0.009(8) C(12) 0.076(10) 0.038(7) 0.070(9) 0.023(8) -0.025(8) -0.008(7) C(13) 0.10(1) 0.06(1) 0.08(1) 0.034(10) -0.053(10) -0.014(8) C(14) 0.18(3) 0.05(1) 0.13(2) 0.05(1) -0.07(2) -0.03(1) C(15) 0.18(3) 0.10(1) 0.10(2) 0.09(2) -0.07(2) -0.04(1) C(16) 0.19(2) 0.10(1) 0.10(1) 0.10(2) -0.09(2) -0.04(1) C(17) 0.12(2) 0.06(1) 0.12(2) 0.05(1) -0.07(1) -0.03(1) C(18) 0.38(6) 0.11(2) 0.25(3) 0.17(3) -0.18(4) -0.06(2) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SAPI91 _computing_structure_refinement 'SHELXL97' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag As(1) S(11) 2.264(5) . . yes As(1) O(11) 2.81(1) . . yes As(1) S(11*) 2.264(4) . . yes As(1) S(11') 2.264(5) . . yes As(1) O(11') 2.81(2) . . yes As(1) O(11*) 2.81(1) . . yes S(11) C(11) 1.80(1) . . yes O(11) C(11) 1.18(2) . . yes C(11) C(12) 1.48(3) . . yes C(12) C(13) 1.39(2) . . yes C(12) C(17) 1.39(3) . . yes C(13) C(14) 1.38(4) . . yes C(13) H(11) 0.967 . . no C(14) C(15) 1.36(4) . . yes C(14) H(12) 0.984 . . no C(15) C(16) 1.38(3) . . yes C(15) C(18) 1.54(5) . . yes C(16) C(17) 1.38(4) . . yes C(16) H(13) 0.963 . . no C(17) H(14) 0.963 . . no C(18) H(15) 0.927 . . no C(18) H(16) 0.955 . . no C(18) H(17) 0.993 . . no S(11*) C(11*) 1.80(2) . . yes S(11') C(11') 1.80(2) . . yes O(11') C(11') 1.18(2) . . yes C(11*) O(11*) 1.18(2) . . yes C(11*) C(12*) 1.48(2) . . yes C(11') C(12') 1.48(3) . . yes C(12*) C(13*) 1.39(3) . . yes C(12*) C(17*) 1.39(3) . . yes C(12') C(13') 1.39(3) . . yes C(12') C(17') 1.39(2) . . yes C(13*) C(14*) 1.38(2) . . yes C(13*) H(11*) 0.967 . . no C(17*) C(16*) 1.38(3) . . yes C(17*) H(14*) 0.963 . . no C(13') C(14') 1.38(4) . . yes C(13') H(11') 0.967 . . no C(17') C(16') 1.38(4) . . yes C(17') H(14') 0.963 . . no C(14*) C(15*) 1.36(4) . . yes C(14*) H(12*) 0.984 . . no C(16*) C(15*) 1.38(4) . . yes C(16*) H(13*) 0.963 . . no C(14') C(15') 1.36(3) . . yes C(14') H(12') 0.984 . . no C(16') C(15') 1.38(4) . . yes C(16') H(13') 0.963 . . no C(15*) C(18*) 1.54(4) . . yes C(15') C(18') 1.54(6) . . yes C(18*) H(15*) 0.927 . . no C(18*) H(16*) 0.955 . . no C(18*) H(17*) 0.993 . . no C(18') H(15') 0.927 . . no C(18') H(16') 0.955 . . no C(18') H(17') 0.993 . . no #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S(11) As(1) O(11) 60.4(3) . 1_555 1_555 yes S(11) As(1) S(11*) 92.9(2) . 1_555 1_555 yes S(11) As(1) S(11') 92.9(2) . 1_555 1_555 yes S(11) As(1) O(11') 153.3(3) . 1_555 1_555 yes S(11) As(1) O(11*) 87.4(3) . 1_555 1_555 yes O(11) As(1) S(11*) 153.3(3) . 1_555 1_555 yes O(11) As(1) S(11') 87.4(3) . 1_555 1_555 yes O(11) As(1) O(11') 115.5(3) . 1_555 1_555 yes O(11) As(1) O(11*) 115.5(4) . 1_555 1_555 yes S(11*) As(1) S(11') 92.9(2) . 1_555 1_555 yes S(11*) As(1) O(11') 87.4(3) . 1_555 1_555 yes S(11*) As(1) O(11*) 60.4(3) . 1_555 1_555 yes S(11') As(1) O(11') 60.4(3) . 1_555 1_555 yes S(11') As(1) O(11*) 153.3(3) . 1_555 1_555 yes O(11') As(1) O(11*) 115.5(4) . 1_555 1_555 yes As(1) S(11) C(11) 93.4(6) . 1_555 1_555 yes As(1) O(11) C(11) 86.1(9) . 1_555 1_555 yes S(11) C(11) O(11) 119(1) . 1_555 1_555 yes S(11) C(11) C(12) 115(1) . 1_555 1_555 yes O(11) C(11) C(12) 125(1) . 1_555 1_555 yes C(11) C(12) C(13) 117(1) . 1_555 1_555 yes C(11) C(12) C(17) 123(1) . 1_555 1_555 yes C(13) C(12) C(17) 119(1) . 1_555 1_555 yes C(12) C(13) C(14) 118(1) . 1_555 1_555 yes C(12) C(13) H(11) 120.0 . 1_555 1_555 no C(14) C(13) H(11) 121.6 . 1_555 1_555 no C(13) C(14) C(15) 122(1) . 1_555 1_555 yes C(13) C(14) H(12) 117.5 . 1_555 1_555 no C(15) C(14) H(12) 120.0 . 1_555 1_555 no C(14) C(15) C(16) 118(2) . 1_555 1_555 yes C(14) C(15) C(18) 120(2) . 1_555 1_555 yes C(16) C(15) C(18) 120(2) . 1_555 1_555 yes C(15) C(16) C(17) 120(2) . 1_555 1_555 yes C(15) C(16) H(13) 120.1 . 1_555 1_555 no C(17) C(16) H(13) 119.6 . 1_555 1_555 no C(12) C(17) C(16) 119(1) . 1_555 1_555 yes C(12) C(17) H(14) 119.8 . 1_555 1_555 no C(16) C(17) H(14) 120.3 . 1_555 1_555 no C(15) C(18) H(15) 112.6 . 1_555 1_555 no C(15) C(18) H(16) 111.7 . 1_555 1_555 no C(15) C(18) H(17) 107.7 . 1_555 1_555 no H(15) C(18) H(16) 111.0 . 1_555 1_555 no H(15) C(18) H(17) 107.8 . 1_555 1_555 no H(16) C(18) H(17) 105.6 . 1_555 1_555 no As(1) S(11*) C(11*) 93.4(5) . 1_555 1_555 yes As(1) S(11') C(11') 93.4(5) . 1_555 1_555 yes As(1) O(11') C(11') 86(1) . 1_555 1_555 yes S(11*) C(11*) O(11*) 119.6(10) . 1_555 1_555 yes S(11*) C(11*) C(12*) 115(1) . 1_555 1_555 yes O(11*) C(11*) C(12*) 125(1) . 1_555 1_555 yes S(11') C(11') O(11') 119(1) . 1_555 1_555 yes S(11') C(11') C(12') 115(1) . 1_555 1_555 yes O(11') C(11') C(12') 125(1) . 1_555 1_555 yes As(1) O(11*) C(11*) 86.1(9) . 1_555 1_555 yes C(11*) C(12*) C(13*) 117(1) . 1_555 1_555 yes C(11*) C(12*) C(17*) 123(1) . 1_555 1_555 yes C(13*) C(12*) C(17*) 119(1) . 1_555 1_555 yes C(11') C(12') C(13') 117(1) . 1_555 1_555 yes C(11') C(12') C(17') 123(1) . 1_555 1_555 yes C(13') C(12') C(17') 119(2) . 1_555 1_555 yes C(12*) C(13*) C(14*) 118(2) . 1_555 1_555 yes C(12*) C(13*) H(11*) 120.0 . 1_555 1_555 no C(14*) C(13*) H(11*) 121.6 . 1_555 1_555 no C(12*) C(17*) C(16*) 119(2) . 1_555 1_555 yes C(12*) C(17*) H(14*) 119.8 . 1_555 1_555 no C(16*) C(17*) H(14*) 120.3 . 1_555 1_555 no C(12') C(13') C(14') 118(1) . 1_555 1_555 yes C(12') C(13') H(11') 120.0 . 1_555 1_555 no C(14') C(13') H(11') 121.6 . 1_555 1_555 no C(12') C(17') C(16') 119(2) . 1_555 1_555 yes C(12') C(17') H(14') 119.8 . 1_555 1_555 no C(16') C(17') H(14') 120.3 . 1_555 1_555 no C(13*) C(14*) C(15*) 122(2) . 1_555 1_555 yes C(13*) C(14*) H(12*) 117.5 . 1_555 1_555 no C(15*) C(14*) H(12*) 120.0 . 1_555 1_555 no C(17*) C(16*) C(15*) 120(2) . 1_555 1_555 yes C(17*) C(16*) H(13*) 119.6 . 1_555 1_555 no C(15*) C(16*) H(13*) 120.1 . 1_555 1_555 no C(13') C(14') C(15') 122(2) . 1_555 1_555 yes C(13') C(14') H(12') 117.5 . 1_555 1_555 no C(15') C(14') H(12') 120.0 . 1_555 1_555 no C(17') C(16') C(15') 120(2) . 1_555 1_555 yes C(17') C(16') H(13') 119.6 . 1_555 1_555 no C(15') C(16') H(13') 120.1 . 1_555 1_555 no C(14*) C(15*) C(16*) 118(1) . 1_555 1_555 yes C(14*) C(15*) C(18*) 120(2) . 1_555 1_555 yes C(16*) C(15*) C(18*) 120(2) . 1_555 1_555 yes C(14') C(15') C(16') 118(2) . 1_555 1_555 yes C(14') C(15') C(18') 120(2) . 1_555 1_555 yes C(16') C(15') C(18') 120(2) . 1_555 1_555 yes C(15*) C(18*) H(15*) 112.6 . 1_555 1_555 no C(15*) C(18*) H(16*) 111.7 . 1_555 1_555 no C(15*) C(18*) H(17*) 107.7 . 1_555 1_555 no H(15*) C(18*) H(16*) 111.0 . 1_555 1_555 no H(15*) C(18*) H(17*) 107.8 . 1_555 1_555 no H(16*) C(18*) H(17*) 105.6 . 1_555 1_555 no C(15') C(18') H(15') 112.6 . 1_555 1_555 no C(15') C(18') H(16') 111.7 . 1_555 1_555 no C(15') C(18') H(17') 107.7 . 1_555 1_555 no H(15') C(18') H(16') 111.0 . 1_555 1_555 no H(15') C(18') H(17') 107.8 . 1_555 1_555 no H(16') C(18') H(17') 105.6 . 1_555 1_555 no #------------------------------------------------------------------------------ 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 As(1) S(11) C(11) O(11) 8(1) 1_555 1_555 1_555 1_555 yes As(1) S(11) C(11) C(12) -175(1) 1_555 1_555 1_555 1_555 yes As(1) O(11) C(11) S(11) -6(1) 1_555 1_555 1_555 1_555 yes As(1) O(11) C(11) C(12) 177(1) 1_555 1_555 1_555 1_555 yes As(1) S(11*) C(11*) O(11*) 8(1) 1_555 1_555 1_555 1_555 yes As(1) S(11*) C(11*) C(12*) -175(1) 1_555 1_555 1_555 1_555 yes As(1) S(11') C(11') O(11') 8(1) 1_555 1_555 1_555 1_555 yes As(1) S(11') C(11') C(12') -175.2(10) 1_555 1_555 1_555 1_555 yes As(1) O(11') C(11') S(11') -6(1) 1_555 1_555 1_555 1_555 yes As(1) O(11') C(11') C(12') 177(1) 1_555 1_555 1_555 1_555 yes As(1) O(11*) C(11*) S(11*) -6(1) 1_555 1_555 1_555 1_555 yes As(1) O(11*) C(11*) C(12*) 177(1) 1_555 1_555 1_555 1_555 yes S(11) As(1) O(11) C(11) 5.2(9) 1_555 1_555 1_555 1_555 yes S(11) As(1) S(11*) C(11*) -88.8(6) 1_555 1_555 1_555 1_555 yes S(11) As(1) S(11') C(11') 178.2(5) 1_555 1_555 1_555 1_555 yes S(11) As(1) O(11') C(11') 8(1) 1_555 1_555 1_555 1_555 yes S(11) As(1) O(11*) C(11*) 100(1) 1_555 1_555 1_555 1_555 yes S(11) C(11) C(12) C(13) -176(1) 1_555 1_555 1_555 1_555 yes S(11) C(11) C(12) C(17) 5(2) 1_555 1_555 1_555 1_555 yes O(11) As(1) S(11) C(11) -3.4(6) 1_555 1_555 1_555 1_555 yes O(11) As(1) S(11*) C(11*) -91.9(9) 1_555 1_555 1_555 1_555 yes O(11) As(1) S(11') C(11') 118.0(5) 1_555 1_555 1_555 1_555 yes O(11) As(1) O(11') C(11') -65.6(10) 1_555 1_555 1_555 1_555 yes O(11) As(1) O(11*) C(11*) 155(1) 1_555 1_555 1_555 1_555 yes O(11) C(11) C(12) C(13) 0(2) 1_555 1_555 1_555 1_555 yes O(11) C(11) C(12) C(17) -178(1) 1_555 1_555 1_555 1_555 yes C(11) S(11) As(1) S(11*) 178.2(5) 1_555 1_555 1_555 1_555 yes C(11) S(11) As(1) S(11') -88.8(5) 1_555 1_555 1_555 1_555 yes C(11) S(11) As(1) O(11') -91.9(8) 1_555 1_555 1_555 1_555 yes C(11) S(11) As(1) O(11*) 118.0(6) 1_555 1_555 1_555 1_555 yes C(11) O(11) As(1) S(11*) 8(1) 1_555 1_555 1_555 1_555 yes C(11) O(11) As(1) S(11') 100.0(10) 1_555 1_555 1_555 1_555 yes C(11) O(11) As(1) O(11') 155.3(10) 1_555 1_555 1_555 1_555 yes C(11) O(11) As(1) O(11*) -65(1) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(14) -177(1) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(17) C(16) 178(1) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(14) C(15) 5(3) 1_555 1_555 1_555 1_555 yes C(12) C(17) C(16) C(15) -7(3) 1_555 1_555 1_555 1_555 yes C(13) C(12) C(17) C(16) 0(3) 1_555 1_555 1_555 1_555 yes C(13) C(14) C(15) C(16) -12(3) 1_555 1_555 1_555 1_555 yes C(13) C(14) C(15) C(18) 176(2) 1_555 1_555 1_555 1_555 yes C(14) C(13) C(12) C(17) 0(2) 1_555 1_555 1_555 1_555 yes C(14) C(15) C(16) C(17) 13(3) 1_555 1_555 1_555 1_555 yes C(17) C(16) C(15) C(18) -175(2) 1_555 1_555 1_555 1_555 yes S(11*) As(1) S(11') C(11') -88.8(5) 1_555 1_555 1_555 1_555 yes S(11*) As(1) O(11') C(11') 100.0(9) 1_555 1_555 1_555 1_555 yes S(11*) As(1) O(11*) C(11*) 5(1) 1_555 1_555 1_555 1_555 yes S(11*) C(11*) C(12*) C(13*) -176(1) 1_555 1_555 1_555 1_555 yes S(11*) C(11*) C(12*) C(17*) 5(2) 1_555 1_555 1_555 1_555 yes S(11') As(1) S(11*) C(11*) 178.2(6) 1_555 1_555 1_555 1_555 yes S(11') As(1) O(11') C(11') 5.2(8) 1_555 1_555 1_555 1_555 yes S(11') As(1) O(11*) C(11*) 8(1) 1_555 1_555 1_555 1_555 yes S(11') C(11') C(12') C(13') -176(1) 1_555 1_555 1_555 1_555 yes S(11') C(11') C(12') C(17') 5(1) 1_555 1_555 1_555 1_555 yes O(11') As(1) S(11*) C(11*) 118.0(7) 1_555 1_555 1_555 1_555 yes O(11') As(1) S(11') C(11') -3.4(5) 1_555 1_555 1_555 1_555 yes O(11') As(1) O(11*) C(11*) -65(1) 1_555 1_555 1_555 1_555 yes O(11') C(11') C(12') C(13') 0(2) 1_555 1_555 1_555 1_555 yes O(11') C(11') C(12') C(17') -178(1) 1_555 1_555 1_555 1_555 yes C(11*) S(11*) As(1) O(11*) -3.4(7) 1_555 1_555 1_555 1_555 yes C(11*) C(12*) C(13*) C(14*) -177(2) 1_555 1_555 1_555 1_555 yes C(11*) C(12*) C(17*) C(16*) 178(2) 1_555 1_555 1_555 1_555 yes C(11') S(11') As(1) O(11*) -91.9(8) 1_555 1_555 1_555 1_555 yes C(11') O(11') As(1) O(11*) 155.3(9) 1_555 1_555 1_555 1_555 yes C(11') C(12') C(13') C(14') -177(1) 1_555 1_555 1_555 1_555 yes C(11') C(12') C(17') C(16') 178(1) 1_555 1_555 1_555 1_555 yes O(11*) C(11*) C(12*) C(13*) 0(2) 1_555 1_555 1_555 1_555 yes O(11*) C(11*) C(12*) C(17*) -178(2) 1_555 1_555 1_555 1_555 yes C(12*) C(13*) C(14*) C(15*) 5(3) 1_555 1_555 1_555 1_555 yes C(12*) C(17*) C(16*) C(15*) -7(4) 1_555 1_555 1_555 1_555 yes C(12') C(13') C(14') C(15') 5(3) 1_555 1_555 1_555 1_555 yes C(12') C(17') C(16') C(15') -7(2) 1_555 1_555 1_555 1_555 yes C(13*) C(12*) C(17*) C(16*) 0(3) 1_555 1_555 1_555 1_555 yes C(13*) C(14*) C(15*) C(16*) -12(4) 1_555 1_555 1_555 1_555 yes C(13*) C(14*) C(15*) C(18*) 176(2) 1_555 1_555 1_555 1_555 yes C(17*) C(12*) C(13*) C(14*) 0(3) 1_555 1_555 1_555 1_555 yes C(17*) C(16*) C(15*) C(14*) 13(4) 1_555 1_555 1_555 1_555 yes C(17*) C(16*) C(15*) C(18*) -175(3) 1_555 1_555 1_555 1_555 yes C(13') C(12') C(17') C(16') 0(2) 1_555 1_555 1_555 1_555 yes C(13') C(14') C(15') C(16') -12(3) 1_555 1_555 1_555 1_555 yes C(13') C(14') C(15') C(18') 176(2) 1_555 1_555 1_555 1_555 yes C(17') C(12') C(13') C(14') 0(2) 1_555 1_555 1_555 1_555 yes C(17') C(16') C(15') C(14') 13(3) 1_555 1_555 1_555 1_555 yes C(17') C(16') C(15') C(18') -175(2) 1_555 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ #===END Ph2AsS2- +NH2C5H10 data_General _audit_creation_date 'Fri Feb 25 12:29:16 2000' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #------------------------------------------------------------------------------ # SUBMISSION DETAILS _publ_contact_author_name ' ENTER NAME' _publ_contact_author_address ; ENTER ADDRESS ; _publ_contact_author_email ' ENTER EMAIL ADDRESS ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? #------------------------------------------------------------------------------ # TITLE AND AUTHOR LIST _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_footnote _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS FOOTNOTES ; ; FIRST AUTHORS ADDRESS ; _publ_section_synopsis ; ENTER SYNOPSIS ; #------------------------------------------------------------------------------ # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1999). teXsan. Single Crystal Structure Analysis Software. Version 1.10. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. Walker, N. & Stuart. D. (1983). Acta Cryst. A39, 158-166. Zachariasen, W. H. (1967). Acta Cryst. 23, 558-564. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #------------------------------------------------------------------------------ data_Ph2AsS2-_NH2C5H10_tani58 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C17 H22 As N S2 ' _chemical_formula_moiety '?' _chemical_formula_weight 379.41 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 9.8461(8) _cell_length_b 12.9809(9) _cell_length_c 14.2520(8) _cell_angle_alpha 90 _cell_angle_beta 96.757(6) _cell_angle_gamma 90 _cell_volume 1808.9(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.1 _cell_measurement_theta_max 12.0 _cell_measurement_temperature 193.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.340 _exptl_crystal_size_mid 0.230 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.393 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 2.104 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details '(Walker & Stuart, 1983)' _exptl_absorpt_correction_T_min 0.561 _exptl_absorpt_correction_T_max 0.657 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 4381 _diffrn_reflns_av_R_equivalents 0.023 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 0.9998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.9998 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.39 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 4147 _reflns_number_gt 2774 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_ref 0.0389 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 2774 _refine_ls_number_parameters 191 _refine_ls_goodness_of_fit_ref 1.170 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00022|Fo|^2^]' _refine_ls_shift/su_max 0.0275 _refine_diff_density_max 0.35 _refine_diff_density_min -0.34 _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.0000(4) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'As' 'As' 0.050 2.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group As(1) As 0.10969(4) 0.49032(3) 0.78266(3) 0.02455(9) Uani 1.00 d . . . S(1) S 0.14992(10) 0.39100(7) 0.90151(7) 0.0307(3) Uani 1.00 d . . . S(2) S 0.0365(1) 0.63809(7) 0.80974(8) 0.0373(3) Uani 1.00 d . . . N(1) N 0.1604(3) 0.6115(3) 1.0469(2) 0.0384(10) Uani 1.00 d . . . C(1) C 0.2755(4) 0.4992(3) 0.7221(2) 0.0267(9) Uani 1.00 d . . . C(2) C 0.3242(4) 0.5942(3) 0.6958(3) 0.033(1) Uani 1.00 d . . . C(3) C 0.4411(4) 0.5987(3) 0.6502(3) 0.037(1) Uani 1.00 d . . . C(4) C 0.5104(4) 0.5097(3) 0.6324(3) 0.040(1) Uani 1.00 d . . . C(5) C 0.4622(4) 0.4151(3) 0.6586(3) 0.038(1) Uani 1.00 d . . . C(6) C 0.3442(4) 0.4092(3) 0.7031(3) 0.034(1) Uani 1.00 d . . . C(7) C -0.0184(4) 0.4235(3) 0.6881(2) 0.0250(9) Uani 1.00 d . . . C(8) C -0.0765(4) 0.4793(3) 0.6117(3) 0.037(1) Uani 1.00 d . . . C(9) C -0.1667(4) 0.4331(3) 0.5425(3) 0.042(1) Uani 1.00 d . . . C(10) C -0.1993(5) 0.3307(4) 0.5512(3) 0.047(1) Uani 1.00 d . . . C(11) C -0.1431(5) 0.2750(3) 0.6271(4) 0.055(2) Uani 1.00 d . . . C(12) C -0.0503(5) 0.3203(3) 0.6961(3) 0.040(1) Uani 1.00 d . . . C(13) C 0.2068(4) 0.7192(3) 1.0362(3) 0.043(1) Uani 1.00 d . . . C(14) C 0.3490(5) 0.7195(4) 1.0062(3) 0.050(1) Uani 1.00 d . . . C(15) C 0.4478(4) 0.6603(4) 1.0762(3) 0.047(1) Uani 1.00 d . . . C(16) C 0.3968(4) 0.5516(3) 1.0897(3) 0.044(1) Uani 1.00 d . . . C(17) C 0.2530(4) 0.5521(3) 1.1170(3) 0.041(1) Uani 1.00 d . . . H(1) H 0.2738 0.6576 0.7087 0.0384 Uiso 1.00 calc . . . H(2) H 0.4729 0.6653 0.6300 0.0431 Uiso 1.00 calc . . . H(3) H 0.5929 0.5138 0.5996 0.0444 Uiso 1.00 calc . . . H(4) H 0.5135 0.3522 0.6474 0.0456 Uiso 1.00 calc . . . H(5) H 0.3081 0.3417 0.7215 0.0401 Uiso 1.00 calc . . . H(6) H -0.0357 0.5503 0.6013 0.0475 Uiso 1.00 calc . . . H(7) H -0.2191 0.4773 0.4836 0.0475 Uiso 1.00 calc . . . H(8) H -0.2628 0.2973 0.5015 0.0553 Uiso 1.00 calc . . . H(9) H -0.1675 0.2026 0.6335 0.0610 Uiso 1.00 calc . . . H(10) H -0.0072 0.2806 0.7495 0.0455 Uiso 1.00 calc . . . H(11) H 0.1639 0.5801 0.9817 0.0475 Uiso 1.00 calc . . . H(12) H 0.0667 0.6078 1.0637 0.0475 Uiso 1.00 calc . . . H(13) H 0.1426 0.7533 0.9893 0.0508 Uiso 1.00 calc . . . H(14) H 0.2049 0.7539 1.0944 0.0508 Uiso 1.00 calc . . . H(15) H 0.3477 0.6882 0.9446 0.0576 Uiso 1.00 calc . . . H(16) H 0.3803 0.7891 1.0010 0.0576 Uiso 1.00 calc . . . H(17) H 0.5378 0.6576 1.0558 0.0520 Uiso 1.00 calc . . . H(18) H 0.4572 0.6946 1.1367 0.0520 Uiso 1.00 calc . . . H(19) H 0.4579 0.5160 1.1381 0.0507 Uiso 1.00 calc . . . H(20) H 0.3994 0.5131 1.0322 0.0507 Uiso 1.00 calc . . . H(21) H 0.2525 0.5838 1.1780 0.0448 Uiso 1.00 calc . . . H(22) H 0.2192 0.4828 1.1218 0.0448 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 As(1) 0.0250(2) 0.0245(2) 0.0242(2) -0.0011(2) 0.0029(1) -0.0005(2) S(1) 0.0267(5) 0.0366(5) 0.0284(5) 0.0014(4) 0.0019(4) 0.0070(4) S(2) 0.0437(6) 0.0273(5) 0.0416(6) 0.0035(4) 0.0080(5) -0.0055(4) N(1) 0.022(2) 0.058(2) 0.036(2) -0.002(2) 0.005(1) -0.006(2) C(1) 0.027(2) 0.027(2) 0.025(2) -0.001(2) 0.002(1) -0.006(2) C(2) 0.036(2) 0.027(2) 0.035(2) -0.006(2) 0.007(2) -0.004(2) C(3) 0.037(2) 0.040(2) 0.036(2) -0.015(2) 0.012(2) -0.003(2) C(4) 0.034(2) 0.048(2) 0.038(2) -0.006(2) 0.010(2) -0.008(2) C(5) 0.035(2) 0.036(2) 0.045(3) 0.000(2) 0.011(2) -0.004(2) C(6) 0.035(2) 0.030(2) 0.036(2) -0.004(2) 0.008(2) -0.001(2) C(7) 0.022(2) 0.032(2) 0.021(2) 0.000(2) 0.004(1) -0.001(1) C(8) 0.036(2) 0.037(2) 0.037(2) -0.005(2) -0.002(2) 0.003(2) C(9) 0.033(2) 0.052(3) 0.040(2) 0.003(2) -0.004(2) -0.003(2) C(10) 0.039(3) 0.052(3) 0.048(3) -0.003(2) -0.006(2) -0.020(2) C(11) 0.061(3) 0.034(2) 0.066(3) -0.013(2) -0.004(3) -0.012(2) C(12) 0.046(3) 0.034(2) 0.039(2) -0.004(2) -0.005(2) -0.001(2) C(13) 0.037(2) 0.050(3) 0.041(3) 0.007(2) -0.001(2) 0.000(2) C(14) 0.040(3) 0.056(3) 0.053(3) -0.013(2) 0.005(2) -0.003(2) C(15) 0.024(2) 0.058(3) 0.059(3) -0.003(2) 0.001(2) -0.014(2) C(16) 0.029(2) 0.050(3) 0.053(3) 0.005(2) 0.002(2) -0.013(2) C(17) 0.039(3) 0.042(2) 0.041(2) 0.003(2) 0.004(2) -0.001(2) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SHELXS86 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag As(1) S(1) 2.128(1) . . yes As(1) S(2) 2.101(1) . . yes As(1) C(1) 1.938(3) . . yes As(1) C(7) 1.939(4) . . yes N(1) C(13) 1.485(5) . . yes N(1) C(17) 1.486(5) . . yes N(1) H(11) 1.019 . . no N(1) H(12) 0.981 . . no C(1) C(2) 1.390(5) . . yes C(1) C(6) 1.392(5) . . yes C(2) C(3) 1.387(5) . . yes C(2) H(1) 0.989 . . no C(3) C(4) 1.380(5) . . yes C(3) H(2) 0.976 . . no C(4) C(5) 1.384(5) . . yes C(4) H(3) 0.985 . . no C(5) C(6) 1.390(5) . . yes C(5) H(4) 0.983 . . no C(6) H(5) 0.993 . . no C(7) C(8) 1.375(5) . . yes C(7) C(12) 1.383(5) . . yes C(8) C(9) 1.384(5) . . yes C(8) H(6) 1.024 . . no C(9) C(10) 1.376(6) . . yes C(9) H(7) 1.094 . . no C(10) C(11) 1.363(6) . . yes C(10) H(8) 0.989 . . no C(11) C(12) 1.392(6) . . yes C(11) H(9) 0.977 . . no C(12) H(10) 0.975 . . no C(13) C(14) 1.511(6) . . yes C(13) H(13) 0.971 . . no C(13) H(14) 0.946 . . no C(14) C(15) 1.518(6) . . yes C(14) H(15) 0.966 . . no C(14) H(16) 0.961 . . no C(15) C(16) 1.518(6) . . yes C(15) H(17) 0.965 . . no C(15) H(18) 0.966 . . no C(16) C(17) 1.512(6) . . yes C(16) H(19) 0.977 . . no C(16) H(20) 0.962 . . no C(17) H(21) 0.962 . . no C(17) H(22) 0.964 . . no #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S(1) As(1) S(2) 116.27(4) . 1_555 1_555 yes S(1) As(1) C(1) 107.6(1) . 1_555 1_555 yes S(1) As(1) C(7) 109.1(1) . 1_555 1_555 yes S(2) As(1) C(1) 110.7(1) . 1_555 1_555 yes S(2) As(1) C(7) 109.1(1) . 1_555 1_555 yes C(1) As(1) C(7) 103.3(1) . 1_555 1_555 yes C(13) N(1) C(17) 112.7(3) . 1_555 1_555 yes C(13) N(1) H(11) 103.8 . 1_555 1_555 no C(13) N(1) H(12) 112.3 . 1_555 1_555 no C(17) N(1) H(11) 108.8 . 1_555 1_555 no C(17) N(1) H(12) 109.3 . 1_555 1_555 no H(11) N(1) H(12) 109.7 . 1_555 1_555 no As(1) C(1) C(2) 120.6(3) . 1_555 1_555 yes As(1) C(1) C(6) 119.4(3) . 1_555 1_555 yes C(2) C(1) C(6) 120.0(3) . 1_555 1_555 yes C(1) C(2) C(3) 119.7(3) . 1_555 1_555 yes C(1) C(2) H(1) 119.4 . 1_555 1_555 no C(3) C(2) H(1) 120.9 . 1_555 1_555 no C(2) C(3) C(4) 120.4(4) . 1_555 1_555 yes C(2) C(3) H(2) 119.3 . 1_555 1_555 no C(4) C(3) H(2) 120.3 . 1_555 1_555 no C(3) C(4) C(5) 120.0(4) . 1_555 1_555 yes C(3) C(4) H(3) 119.7 . 1_555 1_555 no C(5) C(4) H(3) 120.3 . 1_555 1_555 no C(4) C(5) C(6) 120.2(4) . 1_555 1_555 yes C(4) C(5) H(4) 119.7 . 1_555 1_555 no C(6) C(5) H(4) 120.1 . 1_555 1_555 no C(1) C(6) C(5) 119.6(3) . 1_555 1_555 yes C(1) C(6) H(5) 119.5 . 1_555 1_555 no C(5) C(6) H(5) 120.9 . 1_555 1_555 no As(1) C(7) C(8) 119.3(3) . 1_555 1_555 yes As(1) C(7) C(12) 120.8(3) . 1_555 1_555 yes C(8) C(7) C(12) 119.9(4) . 1_555 1_555 yes C(7) C(8) C(9) 120.5(4) . 1_555 1_555 yes C(7) C(8) H(6) 117.1 . 1_555 1_555 no C(9) C(8) H(6) 121.1 . 1_555 1_555 no C(8) C(9) C(10) 119.4(4) . 1_555 1_555 yes C(8) C(9) H(7) 121.6 . 1_555 1_555 no C(10) C(9) H(7) 118.8 . 1_555 1_555 no C(9) C(10) C(11) 120.5(4) . 1_555 1_555 yes C(9) C(10) H(8) 119.6 . 1_555 1_555 no C(11) C(10) H(8) 119.9 . 1_555 1_555 no C(10) C(11) C(12) 120.5(4) . 1_555 1_555 yes C(10) C(11) H(9) 120.2 . 1_555 1_555 no C(12) C(11) H(9) 119.3 . 1_555 1_555 no C(7) C(12) C(11) 119.2(4) . 1_555 1_555 yes C(7) C(12) H(10) 119.7 . 1_555 1_555 no C(11) C(12) H(10) 121.1 . 1_555 1_555 no N(1) C(13) C(14) 109.7(3) . 1_555 1_555 yes N(1) C(13) H(13) 108.4 . 1_555 1_555 no N(1) C(13) H(14) 108.7 . 1_555 1_555 no C(14) C(13) H(13) 110.7 . 1_555 1_555 no C(14) C(13) H(14) 111.2 . 1_555 1_555 no H(13) C(13) H(14) 108.0 . 1_555 1_555 no C(13) C(14) C(15) 110.9(4) . 1_555 1_555 yes C(13) C(14) H(15) 110.0 . 1_555 1_555 no C(13) C(14) H(16) 109.8 . 1_555 1_555 no C(15) C(14) H(15) 108.9 . 1_555 1_555 no C(15) C(14) H(16) 109.9 . 1_555 1_555 no H(15) C(14) H(16) 107.2 . 1_555 1_555 no C(14) C(15) C(16) 110.9(3) . 1_555 1_555 yes C(14) C(15) H(17) 111.2 . 1_555 1_555 no C(14) C(15) H(18) 109.9 . 1_555 1_555 no C(16) C(15) H(17) 109.5 . 1_555 1_555 no C(16) C(15) H(18) 108.3 . 1_555 1_555 no H(17) C(15) H(18) 106.9 . 1_555 1_555 no C(15) C(16) C(17) 111.3(3) . 1_555 1_555 yes C(15) C(16) H(19) 110.1 . 1_555 1_555 no C(15) C(16) H(20) 109.4 . 1_555 1_555 no C(17) C(16) H(19) 109.8 . 1_555 1_555 no C(17) C(16) H(20) 110.0 . 1_555 1_555 no H(19) C(16) H(20) 106.2 . 1_555 1_555 no N(1) C(17) C(16) 110.3(3) . 1_555 1_555 yes N(1) C(17) H(21) 108.5 . 1_555 1_555 no N(1) C(17) H(22) 110.0 . 1_555 1_555 no C(16) C(17) H(21) 109.8 . 1_555 1_555 no C(16) C(17) H(22) 110.8 . 1_555 1_555 no H(21) C(17) H(22) 107.3 . 1_555 1_555 no #------------------------------------------------------------------------------ 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 As(1) C(1) C(2) C(3) -178.3(3) 1_555 1_555 1_555 1_555 yes As(1) C(1) C(6) C(5) 179.2(3) 1_555 1_555 1_555 1_555 yes As(1) C(7) C(8) C(9) 179.1(3) 1_555 1_555 1_555 1_555 yes As(1) C(7) C(12) C(11) 179.7(3) 1_555 1_555 1_555 1_555 yes S(1) As(1) C(1) C(2) -133.0(3) 1_555 1_555 1_555 1_555 yes S(1) As(1) C(1) C(6) 48.4(3) 1_555 1_555 1_555 1_555 yes S(1) As(1) C(7) C(8) 169.5(3) 1_555 1_555 1_555 1_555 yes S(1) As(1) C(7) C(12) -11.3(3) 1_555 1_555 1_555 1_555 yes S(2) As(1) C(1) C(2) -4.9(3) 1_555 1_555 1_555 1_555 yes S(2) As(1) C(1) C(6) 176.4(3) 1_555 1_555 1_555 1_555 yes S(2) As(1) C(7) C(8) 41.6(3) 1_555 1_555 1_555 1_555 yes S(2) As(1) C(7) C(12) -139.3(3) 1_555 1_555 1_555 1_555 yes N(1) C(13) C(14) C(15) -56.7(5) 1_555 1_555 1_555 1_555 yes N(1) C(17) C(16) C(15) 54.5(5) 1_555 1_555 1_555 1_555 yes C(1) As(1) C(7) C(8) -76.2(3) 1_555 1_555 1_555 1_555 yes C(1) As(1) C(7) C(12) 103.0(3) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(3) C(4) -1.2(6) 1_555 1_555 1_555 1_555 yes C(1) C(6) C(5) C(4) -0.6(6) 1_555 1_555 1_555 1_555 yes C(2) C(1) As(1) C(7) 111.7(3) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(6) C(5) 0.5(6) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(4) C(5) 1.1(6) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(1) C(6) 0.4(6) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(6) -0.2(6) 1_555 1_555 1_555 1_555 yes C(6) C(1) As(1) C(7) -66.9(3) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(9) C(10) 0.8(7) 1_555 1_555 1_555 1_555 yes C(7) C(12) C(11) C(10) 1.7(7) 1_555 1_555 1_555 1_555 yes C(8) C(7) C(12) C(11) -1.1(6) 1_555 1_555 1_555 1_555 yes C(8) C(9) C(10) C(11) -0.3(7) 1_555 1_555 1_555 1_555 yes C(9) C(8) C(7) C(12) -0.1(6) 1_555 1_555 1_555 1_555 yes C(9) C(10) C(11) C(12) -1.0(8) 1_555 1_555 1_555 1_555 yes C(13) N(1) C(17) C(16) -57.5(4) 1_555 1_555 1_555 1_555 yes C(13) C(14) C(15) C(16) 55.3(5) 1_555 1_555 1_555 1_555 yes C(14) C(13) N(1) C(17) 58.5(4) 1_555 1_555 1_555 1_555 yes C(14) C(15) C(16) C(17) -54.2(5) 1_555 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ #===END PhAsS32- (+NH2C5H10)2 data_General _audit_creation_date 'Fri Feb 25 15:07:54 2000' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #------------------------------------------------------------------------------ # SUBMISSION DETAILS _publ_contact_author_name ' ENTER NAME' _publ_contact_author_address ; ENTER ADDRESS ; _publ_contact_author_email ' ENTER EMAIL ADDRESS ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? #------------------------------------------------------------------------------ # TITLE AND AUTHOR LIST _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_footnote _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS FOOTNOTES ; ; FIRST AUTHORS ADDRESS ; _publ_section_synopsis ; ENTER SYNOPSIS ; #------------------------------------------------------------------------------ # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1999). teXsan. Single Crystal Structure Analysis Software. Version 1.10. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. Walker, N. & Stuart. D. (1983). Acta Cryst. A39, 158-166. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #------------------------------------------------------------------------------ data_PhAsS(S-_NH2+C5H10)2 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C16 H29 As N2 S3 ' _chemical_formula_moiety '?' _chemical_formula_weight 420.52 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 10.500(2) _cell_length_b 11.643(3) _cell_length_c 9.012(2) _cell_angle_alpha 94.42(2) _cell_angle_beta 108.82(1) _cell_angle_gamma 73.02(2) _cell_volume 997.2(4) _cell_formula_units_Z 2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.3 _cell_measurement_theta_max 12.3 _cell_measurement_temperature 193.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.290 _exptl_crystal_size_mid 0.110 _exptl_crystal_size_min 0.110 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.400 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 2.018 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details '(Walker & Stuart, 1983)' _exptl_absorpt_correction_T_min 0.457 _exptl_absorpt_correction_T_max 0.801 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 4802 _diffrn_reflns_av_R_equivalents 0.038 _diffrn_reflns_theta_max 27.51 _diffrn_measured_fraction_theta_max 0.9996 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.9996 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.25 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 4575 _reflns_number_gt 2344 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0659 _refine_ls_wR_factor_ref 0.0673 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 2344 _refine_ls_number_parameters 199 _refine_ls_goodness_of_fit_ref 1.613 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00031|Fo|^2^]' _refine_ls_shift/su_max 0.0302 _refine_diff_density_max 0.70 _refine_diff_density_min -0.82 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'As' 'As' 0.050 2.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group As(1) As 0.39615(9) 0.27484(9) 0.6315(1) 0.0355(3) Uani 1.00 d . . . S(1) S 0.3418(2) 0.3735(2) 0.4177(2) 0.0392(6) Uani 1.00 d . . . S(2) S 0.6159(2) 0.2391(2) 0.7603(3) 0.0546(8) Uani 1.00 d . . . S(3) S 0.3236(2) 0.1184(2) 0.5929(3) 0.0568(8) Uani 1.00 d . . . N(1) N 0.6917(6) 0.3505(6) 0.4791(8) 0.038(2) Uani 1.00 d . . . N(2) N 0.3140(7) 0.0532(8) 0.2392(9) 0.063(3) Uani 1.00 d . . . C(1) C 0.2957(7) 0.3795(8) 0.7585(8) 0.034(2) Uani 1.00 d . . . C(2) C 0.3618(8) 0.4097(10) 0.9100(9) 0.052(3) Uani 1.00 d . . . C(3) C 0.2850(10) 0.487(1) 0.995(1) 0.064(3) Uani 1.00 d . . . C(4) C 0.1434(10) 0.5352(10) 0.933(1) 0.059(3) Uani 1.00 d . . . C(5) C 0.0750(8) 0.5062(9) 0.783(1) 0.047(3) Uani 1.00 d . . . C(6) C 0.1504(8) 0.4288(8) 0.6961(9) 0.038(2) Uani 1.00 d . . . C(11) C 0.6490(8) 0.3348(8) 0.308(1) 0.043(3) Uani 1.00 d . . . C(12) C 0.694(1) 0.2045(9) 0.269(1) 0.059(3) Uani 1.00 d . . . C(13) C 0.851(1) 0.1511(10) 0.338(2) 0.084(4) Uani 1.00 d . . . C(14) C 0.894(1) 0.170(1) 0.514(2) 0.080(4) Uani 1.00 d . . . C(15) C 0.8459(9) 0.300(1) 0.554(1) 0.060(3) Uani 1.00 d . . . C(21) C 0.379(1) 0.088(2) 0.132(2) 0.146(7) Uani 1.00 d . . . C(22) C 0.318(1) 0.134(2) 0.014(2) 0.206(9) Uani 1.00 d . . . C(23) C 0.163(1) 0.176(1) -0.050(2) 0.109(5) Uani 1.00 d . . . C(24) C 0.097(1) 0.133(2) 0.053(2) 0.214(10) Uani 1.00 d . . . C(25) C 0.159(1) 0.093(2) 0.179(2) 0.139(6) Uani 1.00 d . . . H(1) H 0.4623 0.3795 0.9544 0.0578 Uiso 1.00 calc . . . H(2) H 0.3334 0.5085 1.1013 0.0701 Uiso 1.00 calc . . . H(3) H 0.0890 0.5905 0.9934 0.0668 Uiso 1.00 calc . . . H(4) H -0.0352 0.5347 0.7339 0.0690 Uiso 1.00 calc . . . H(5) H 0.1020 0.4055 0.5903 0.0444 Uiso 1.00 calc . . . H(6) H 0.6632 0.4353 0.5020 0.0451 Uiso 1.00 calc . . . H(7) H 0.6431 0.3115 0.5232 0.0451 Uiso 1.00 calc . . . H(8) H 0.6931 0.3787 0.2626 0.0502 Uiso 1.00 calc . . . H(9) H 0.5495 0.3675 0.2628 0.0502 Uiso 1.00 calc . . . H(10) H 0.6646 0.1950 0.1580 0.0633 Uiso 1.00 calc . . . H(11) H 0.6476 0.1616 0.3125 0.0633 Uiso 1.00 calc . . . H(12) H 0.8980 0.1923 0.2921 0.0938 Uiso 1.00 calc . . . H(13) H 0.8789 0.0684 0.3154 0.0938 Uiso 1.00 calc . . . H(14) H 0.9919 0.1403 0.5578 0.0921 Uiso 1.00 calc . . . H(15) H 0.8494 0.1260 0.5574 0.0921 Uiso 1.00 calc . . . H(16) H 0.8698 0.3081 0.6673 0.0646 Uiso 1.00 calc . . . H(17) H 0.8950 0.3456 0.5200 0.0646 Uiso 1.00 calc . . . H(18) H 0.3428 -0.0340 0.2487 0.0776 Uiso 1.00 calc . . . H(19) H 0.3485 0.0835 0.3408 0.0776 Uiso 1.00 calc . . . H(20) H 0.4302 0.1421 0.1900 0.1491 Uiso 1.00 calc . . . H(21) H 0.4486 0.0155 0.1172 0.1491 Uiso 1.00 calc . . . H(22) H 0.3579 0.1954 0.0090 0.2017 Uiso 1.00 calc . . . H(23) H 0.3503 0.0702 -0.0590 0.2017 Uiso 1.00 calc . . . H(24) H 0.1353 0.2622 -0.0541 0.1223 Uiso 1.00 calc . . . H(25) H 0.1302 0.1484 -0.1548 0.1223 Uiso 1.00 calc . . . H(26) H 0.0185 0.2001 0.0623 0.2024 Uiso 1.00 calc . . . H(27) H 0.0571 0.0715 -0.0019 0.2024 Uiso 1.00 calc . . . H(28) H 0.1243 0.0298 0.1960 0.1392 Uiso 1.00 calc . . . H(29) H 0.1310 0.1579 0.2516 0.1392 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 As(1) 0.0329(4) 0.0349(6) 0.0406(5) -0.0090(4) 0.0139(4) -0.0014(4) S(1) 0.050(1) 0.042(1) 0.031(1) -0.017(1) 0.0177(10) -0.011(1) S(2) 0.034(1) 0.068(2) 0.062(2) -0.011(1) 0.014(1) 0.008(1) S(3) 0.052(1) 0.037(1) 0.091(2) -0.014(1) 0.031(1) 0.003(1) N(1) 0.037(3) 0.030(4) 0.042(4) -0.001(3) 0.013(3) -0.001(3) N(2) 0.037(4) 0.084(7) 0.063(5) 0.009(4) 0.023(4) 0.038(5) C(1) 0.032(4) 0.047(6) 0.024(4) -0.014(4) 0.008(3) 0.007(4) C(2) 0.035(4) 0.092(8) 0.025(5) -0.018(5) 0.003(4) 0.010(5) C(3) 0.055(6) 0.112(10) 0.029(5) -0.031(6) 0.017(4) -0.020(6) C(4) 0.058(6) 0.084(8) 0.039(5) -0.020(6) 0.024(5) -0.016(5) C(5) 0.038(4) 0.062(7) 0.044(5) -0.011(4) 0.019(4) -0.007(5) C(6) 0.035(4) 0.051(6) 0.027(4) -0.015(4) 0.006(4) -0.007(4) C(11) 0.042(5) 0.043(6) 0.041(5) -0.001(4) 0.018(4) -0.004(4) C(12) 0.086(7) 0.039(6) 0.060(7) -0.024(6) 0.035(6) -0.024(5) C(13) 0.100(9) 0.044(7) 0.10(1) 0.028(6) 0.060(8) 0.008(7) C(14) 0.057(6) 0.055(8) 0.11(1) 0.026(6) 0.024(7) 0.026(7) C(15) 0.036(5) 0.072(8) 0.062(7) -0.014(5) 0.001(5) 0.006(6) C(21) 0.043(6) 0.22(2) 0.17(2) 0.034(9) 0.058(9) 0.14(1) C(22) 0.059(8) 0.40(3) 0.16(2) -0.06(1) -0.013(9) 0.21(2) C(23) 0.088(9) 0.14(1) 0.085(10) -0.024(9) -0.005(7) 0.078(9) C(24) 0.044(7) 0.36(3) 0.22(2) -0.04(1) -0.032(10) 0.24(2) C(25) 0.033(6) 0.26(2) 0.11(1) 0.008(9) 0.031(7) 0.09(1) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SHELXS86 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag As(1) S(1) 2.146(2) . . yes As(1) S(2) 2.151(2) . . yes As(1) S(3) 2.135(3) . . yes As(1) C(1) 1.929(8) . . yes N(1) C(11) 1.48(1) . . yes N(1) C(15) 1.49(1) . . yes N(1) H(6) 0.971 . . no N(1) H(7) 0.958 . . no N(2) C(21) 1.49(1) . . yes N(2) C(25) 1.48(1) . . yes N(2) H(18) 0.973 . . no N(2) H(19) 0.951 . . no C(1) C(2) 1.39(1) . . yes C(1) C(6) 1.400(10) . . yes C(2) C(3) 1.39(1) . . yes C(2) H(1) 0.965 . . no C(3) C(4) 1.37(1) . . yes C(3) H(2) 0.978 . . no C(4) C(5) 1.37(1) . . yes C(4) H(3) 0.988 . . no C(5) C(6) 1.39(1) . . yes C(5) H(4) 1.056 . . no C(6) H(5) 0.984 . . no C(11) C(12) 1.50(1) . . yes C(11) H(8) 0.965 . . no C(11) H(9) 0.959 . . no C(12) C(13) 1.51(1) . . yes C(12) H(10) 0.954 . . no C(12) H(11) 0.969 . . no C(13) C(14) 1.52(2) . . yes C(13) H(12) 0.975 . . no C(13) H(13) 0.948 . . no C(14) C(15) 1.50(1) . . yes C(14) H(14) 0.939 . . no C(14) H(15) 0.961 . . no C(15) H(16) 0.974 . . no C(15) H(17) 0.965 . . no C(21) C(22) 1.13(2) . . yes C(21) H(20) 0.958 . . no C(21) H(21) 0.975 . . no C(22) C(23) 1.48(2) . . yes C(22) H(22) 0.939 . . no C(22) H(23) 1.006 . . no C(23) C(24) 1.51(2) . . yes C(23) H(24) 0.962 . . no C(23) H(25) 0.956 . . no C(24) C(25) 1.17(2) . . yes C(24) H(26) 0.983 . . no C(24) H(27) 0.960 . . no C(25) H(28) 0.954 . . no C(25) H(29) 0.997 . . no #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S(1) As(1) S(2) 111.69(9) . 1_555 1_555 yes S(1) As(1) S(3) 112.0(1) . 1_555 1_555 yes S(1) As(1) C(1) 105.8(2) . 1_555 1_555 yes S(2) As(1) S(3) 113.6(1) . 1_555 1_555 yes S(2) As(1) C(1) 106.7(2) . 1_555 1_555 yes S(3) As(1) C(1) 106.5(2) . 1_555 1_555 yes C(11) N(1) C(15) 112.1(7) . 1_555 1_555 yes C(11) N(1) H(6) 109.4 . 1_555 1_555 no C(11) N(1) H(7) 109.0 . 1_555 1_555 no C(15) N(1) H(6) 109.9 . 1_555 1_555 no C(15) N(1) H(7) 109.3 . 1_555 1_555 no H(6) N(1) H(7) 107.0 . 1_555 1_555 no C(21) N(2) C(25) 112.5(8) . 1_555 1_555 yes C(21) N(2) H(18) 108.4 . 1_555 1_555 no C(21) N(2) H(19) 109.3 . 1_555 1_555 no C(25) N(2) H(18) 107.7 . 1_555 1_555 no C(25) N(2) H(19) 111.3 . 1_555 1_555 no H(18) N(2) H(19) 107.4 . 1_555 1_555 no As(1) C(1) C(2) 122.7(6) . 1_555 1_555 yes As(1) C(1) C(6) 119.2(6) . 1_555 1_555 yes C(2) C(1) C(6) 118.1(7) . 1_555 1_555 yes C(1) C(2) C(3) 120.4(8) . 1_555 1_555 yes C(1) C(2) H(1) 119.7 . 1_555 1_555 no C(3) C(2) H(1) 119.8 . 1_555 1_555 no C(2) C(3) C(4) 120.9(8) . 1_555 1_555 yes C(2) C(3) H(2) 119.4 . 1_555 1_555 no C(4) C(3) H(2) 119.7 . 1_555 1_555 no C(3) C(4) C(5) 119.9(9) . 1_555 1_555 yes C(3) C(4) H(3) 120.7 . 1_555 1_555 no C(5) C(4) H(3) 119.3 . 1_555 1_555 no C(4) C(5) C(6) 119.9(8) . 1_555 1_555 yes C(4) C(5) H(4) 122.5 . 1_555 1_555 no C(6) C(5) H(4) 117.4 . 1_555 1_555 no C(1) C(6) C(5) 120.8(7) . 1_555 1_555 yes C(1) C(6) H(5) 118.7 . 1_555 1_555 no C(5) C(6) H(5) 120.5 . 1_555 1_555 no N(1) C(11) C(12) 110.6(7) . 1_555 1_555 yes N(1) C(11) H(8) 108.9 . 1_555 1_555 no N(1) C(11) H(9) 110.3 . 1_555 1_555 no C(12) C(11) H(8) 108.9 . 1_555 1_555 no C(12) C(11) H(9) 110.7 . 1_555 1_555 no H(8) C(11) H(9) 107.5 . 1_555 1_555 no C(11) C(12) C(13) 111.7(8) . 1_555 1_555 yes C(11) C(12) H(10) 110.1 . 1_555 1_555 no C(11) C(12) H(11) 108.2 . 1_555 1_555 no C(13) C(12) H(10) 110.7 . 1_555 1_555 no C(13) C(12) H(11) 108.5 . 1_555 1_555 no H(10) C(12) H(11) 107.5 . 1_555 1_555 no C(12) C(13) C(14) 109.3(8) . 1_555 1_555 yes C(12) C(13) H(12) 109.0 . 1_555 1_555 no C(12) C(13) H(13) 111.8 . 1_555 1_555 no C(14) C(13) H(12) 108.6 . 1_555 1_555 no C(14) C(13) H(13) 110.6 . 1_555 1_555 no H(12) C(13) H(13) 107.6 . 1_555 1_555 no C(13) C(14) C(15) 112.0(9) . 1_555 1_555 yes C(13) C(14) H(14) 110.2 . 1_555 1_555 no C(13) C(14) H(15) 107.3 . 1_555 1_555 no C(15) C(14) H(14) 110.1 . 1_555 1_555 no C(15) C(14) H(15) 107.6 . 1_555 1_555 no H(14) C(14) H(15) 109.4 . 1_555 1_555 no N(1) C(15) C(14) 111.1(8) . 1_555 1_555 yes N(1) C(15) H(16) 109.9 . 1_555 1_555 no N(1) C(15) H(17) 109.6 . 1_555 1_555 no C(14) C(15) H(16) 109.9 . 1_555 1_555 no C(14) C(15) H(17) 109.9 . 1_555 1_555 no H(16) C(15) H(17) 106.3 . 1_555 1_555 no N(2) C(21) C(22) 124(1) . 1_555 1_555 yes N(2) C(21) H(20) 106.0 . 1_555 1_555 no N(2) C(21) H(21) 106.1 . 1_555 1_555 no C(22) C(21) H(20) 104.8 . 1_555 1_555 no C(22) C(21) H(21) 107.9 . 1_555 1_555 no H(20) C(21) H(21) 106.7 . 1_555 1_555 no C(21) C(22) C(23) 124(1) . 1_555 1_555 yes C(21) C(22) H(22) 105.7 . 1_555 1_555 no C(21) C(22) H(23) 101.7 . 1_555 1_555 no C(23) C(22) H(22) 110.8 . 1_555 1_555 no C(23) C(22) H(23) 106.3 . 1_555 1_555 no H(22) C(22) H(23) 105.8 . 1_555 1_555 no C(22) C(23) C(24) 110(1) . 1_555 1_555 yes C(22) C(23) H(24) 108.0 . 1_555 1_555 no C(22) C(23) H(25) 111.3 . 1_555 1_555 no C(24) C(23) H(24) 109.6 . 1_555 1_555 no C(24) C(23) H(25) 109.5 . 1_555 1_555 no H(24) C(23) H(25) 107.9 . 1_555 1_555 no C(23) C(24) C(25) 123(1) . 1_555 1_555 yes C(23) C(24) H(26) 107.2 . 1_555 1_555 no C(23) C(24) H(27) 108.0 . 1_555 1_555 no C(25) C(24) H(26) 106.0 . 1_555 1_555 no C(25) C(24) H(27) 104.5 . 1_555 1_555 no H(26) C(24) H(27) 106.0 . 1_555 1_555 no N(2) C(25) C(24) 122(1) . 1_555 1_555 yes N(2) C(25) H(28) 108.5 . 1_555 1_555 no N(2) C(25) H(29) 104.9 . 1_555 1_555 no C(24) C(25) H(28) 108.8 . 1_555 1_555 no C(24) C(25) H(29) 105.8 . 1_555 1_555 no H(28) C(25) H(29) 105.3 . 1_555 1_555 no #------------------------------------------------------------------------------ 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 As(1) C(1) C(2) C(3) 178.7(7) 1_555 1_555 1_555 1_555 yes As(1) C(1) C(6) C(5) -178.8(6) 1_555 1_555 1_555 1_555 yes S(1) As(1) C(1) C(2) -125.4(7) 1_555 1_555 1_555 1_555 yes S(1) As(1) C(1) C(6) 53.9(6) 1_555 1_555 1_555 1_555 yes S(2) As(1) C(1) C(2) -6.4(8) 1_555 1_555 1_555 1_555 yes S(2) As(1) C(1) C(6) 172.9(6) 1_555 1_555 1_555 1_555 yes S(3) As(1) C(1) C(2) 115.3(7) 1_555 1_555 1_555 1_555 yes S(3) As(1) C(1) C(6) -65.4(6) 1_555 1_555 1_555 1_555 yes N(1) C(11) C(12) C(13) -57.7(10) 1_555 1_555 1_555 1_555 yes N(1) C(15) C(14) C(13) 54(1) 1_555 1_555 1_555 1_555 yes N(2) C(21) C(22) C(23) 5(4) 1_555 1_555 1_555 1_555 yes N(2) C(25) C(24) C(23) -15(4) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(3) C(4) 0(1) 1_555 1_555 1_555 1_555 yes C(1) C(6) C(5) C(4) 0(1) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(6) C(5) 0(1) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(4) C(5) 0(1) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(1) C(6) 0(1) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(6) 0(1) 1_555 1_555 1_555 1_555 yes C(11) N(1) C(15) C(14) -55(1) 1_555 1_555 1_555 1_555 yes C(11) C(12) C(13) C(14) 55(1) 1_555 1_555 1_555 1_555 yes C(12) C(11) N(1) C(15) 56.8(9) 1_555 1_555 1_555 1_555 yes C(12) C(13) C(14) C(15) -54(1) 1_555 1_555 1_555 1_555 yes C(21) N(2) C(25) C(24) 9(2) 1_555 1_555 1_555 1_555 yes C(21) C(22) C(23) C(24) -8(3) 1_555 1_555 1_555 1_555 yes C(22) C(21) N(2) C(25) -4(3) 1_555 1_555 1_555 1_555 yes C(22) C(23) C(24) C(25) 13(3) 1_555 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ #===END (PhAsS)4 data_General _audit_creation_date 'Mon Jun 26 13:42:39 2000' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #------------------------------------------------------------------------------ # SUBMISSION DETAILS _publ_contact_author_name ' ENTER NAME' _publ_contact_author_address ; ENTER ADDRESS ; _publ_contact_author_email ' ENTER EMAIL ADDRESS ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? #------------------------------------------------------------------------------ # TITLE AND AUTHOR LIST _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_footnote _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS FOOTNOTES ; ; FIRST AUTHORS ADDRESS ; _publ_section_synopsis ; ENTER SYNOPSIS ; #------------------------------------------------------------------------------ # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1999). teXsan. Single Crystal Structure Analysis Software. Version 1.10. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. Zachariasen, W. H. (1967). Acta Cryst. 23, 558-564. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #------------------------------------------------------------------------------ data_(Ph2AsS)4 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C24 H20 As4 S4 ' _chemical_formula_moiety 'C24 H20 As4 S4 ' _chemical_formula_weight 736.35 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 42/n (origin at -1)' _symmetry_Int_Tables_number 86 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2-y,z -y,1/2+x,1/2+z 1/2+y,-x,1/2+z -x,-y,-z 1/2+x,1/2+y,-z y,1/2-x,1/2-z 1/2-y,x,1/2-z _cell_length_a 16.4696(5) _cell_length_b 16.4696(5) _cell_length_c 9.971(1) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2704.6(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.3 _cell_measurement_theta_max 12.5 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.340 _exptl_crystal_size_mid 0.140 _exptl_crystal_size_min 0.140 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.808 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 5.222 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.937 _exptl_absorpt_correction_T_max 0.995 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 3512 _diffrn_reflns_av_R_equivalents 0.054 _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 0.9994 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.9994 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.28 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > -10.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 3105 _reflns_number_gt 1051 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_ref 0.1353 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3105 _refine_ls_number_parameters 146 _refine_ls_goodness_of_fit_ref 0.921 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0015 _refine_diff_density_max 1.52 _refine_diff_density_min -1.46 _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.0021(3) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'As' 'As' 0.050 2.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group As(1) As 0.38346(6) 0.69441(6) 0.22931(10) 0.0408(4) Uani 1.00 d . . . As(2) As 0.19412(6) 0.61729(6) 0.23310(10) 0.0427(4) Uani 1.00 d . . . S(1) S 0.3834(2) 0.8053(2) 0.0991(3) 0.059(1) Uani 1.00 d . . . S(2) S 0.3086(2) 0.6061(2) 0.1109(3) 0.0549(10) Uani 1.00 d . . . C(1) C 0.4900(5) 0.6542(5) 0.1692(9) 0.037(3) Uani 1.00 d . . . C(2) C 0.5542(5) 0.7059(5) 0.1522(9) 0.050(3) Uani 1.00 d . . . C(3) C 0.6300(6) 0.6775(6) 0.121(1) 0.064(3) Uani 1.00 d . . . C(4) C 0.6424(6) 0.5943(7) 0.106(1) 0.066(4) Uani 1.00 d . . . C(5) C 0.5796(6) 0.5407(5) 0.124(1) 0.059(3) Uani 1.00 d . . . C(6) C 0.5034(5) 0.5707(5) 0.1573(9) 0.051(3) Uani 1.00 d . . . C(7) C 0.1503(5) 0.5119(6) 0.177(1) 0.044(4) Uani 1.00 d . . . C(8) C 0.1256(8) 0.4956(6) 0.050(1) 0.092(5) Uani 1.00 d . . . C(9) C 0.0961(10) 0.4210(7) 0.016(1) 0.111(5) Uani 1.00 d . . . C(10) C 0.0918(8) 0.3599(6) 0.110(1) 0.077(5) Uani 1.00 d . . . C(11) C 0.1165(6) 0.3761(5) 0.238(1) 0.064(3) Uani 1.00 d . . . C(12) C 0.1455(5) 0.4530(5) 0.2716(9) 0.050(3) Uani 1.00 d . . . H(1) H 0.5451 0.7652 0.1634 0.0593 Uiso 1.00 calc . . . H(2) H 0.6741 0.7162 0.1056 0.0729 Uiso 1.00 calc . . . H(3) H 0.6970 0.5746 0.0830 0.0852 Uiso 1.00 calc . . . H(4) H 0.5877 0.4810 0.1145 0.0700 Uiso 1.00 calc . . . H(5) H 0.4576 0.5329 0.1716 0.0577 Uiso 1.00 calc . . . H(6) H 0.1284 0.5392 -0.0180 0.1013 Uiso 1.00 calc . . . H(7) H 0.0779 0.4107 -0.0765 0.1180 Uiso 1.00 calc . . . H(8) H 0.0693 0.3071 0.0882 0.0835 Uiso 1.00 calc . . . H(9) H 0.1152 0.3333 0.3055 0.0741 Uiso 1.00 calc . . . H(10) H 0.1615 0.4649 0.3666 0.0596 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 As(1) 0.0408(8) 0.0357(7) 0.0459(7) 0.0008(6) -0.0016(7) 0.0017(6) As(2) 0.0424(8) 0.0347(7) 0.0510(8) -0.0052(6) 0.0011(7) -0.0027(7) S(1) 0.067(2) 0.045(2) 0.065(2) 0.013(2) 0.015(2) 0.012(2) S(2) 0.038(2) 0.049(2) 0.077(2) -0.003(1) 0.004(2) -0.021(2) C(1) 0.036(6) 0.046(7) 0.030(6) -0.005(5) -0.009(5) 0.000(5) C(2) 0.042(5) 0.045(5) 0.063(6) -0.003(4) -0.004(5) -0.001(5) C(3) 0.043(5) 0.082(7) 0.066(7) -0.020(5) 0.000(5) -0.004(6) C(4) 0.042(7) 0.091(9) 0.065(9) 0.013(7) -0.002(6) -0.007(8) C(5) 0.063(7) 0.051(6) 0.063(7) 0.018(5) -0.010(6) 0.002(5) C(6) 0.041(5) 0.048(5) 0.063(6) 0.006(4) -0.011(5) 0.002(5) C(7) 0.038(7) 0.039(7) 0.057(8) -0.009(5) 0.006(6) -0.006(6) C(8) 0.16(1) 0.057(7) 0.057(8) -0.043(8) 0.008(8) 0.003(6) C(9) 0.20(2) 0.078(9) 0.053(7) -0.06(1) -0.027(9) 0.001(7) C(10) 0.13(1) 0.050(8) 0.055(8) -0.046(8) 0.005(9) 0.001(7) C(11) 0.079(8) 0.038(5) 0.075(8) -0.007(5) 0.010(6) 0.023(5) C(12) 0.055(6) 0.037(5) 0.059(6) -0.001(4) -0.012(5) 0.009(5) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SHELXS86 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag As(1) S(1) 2.241(3) . . yes As(1) S(2) 2.243(3) . . yes As(1) C(1) 1.970(9) . . yes As(2) S(1) 2.246(3) . 2_565 yes As(2) S(2) 2.252(3) . . yes As(2) C(7) 1.961(9) . . yes C(1) C(2) 1.37(1) . . yes C(1) C(6) 1.40(1) . . yes C(2) C(3) 1.37(1) . . yes C(2) H(1) 0.993 . . no C(3) C(4) 1.39(1) . . yes C(3) H(2) 0.977 . . no C(4) C(5) 1.37(1) . . yes C(4) H(3) 0.984 . . no C(5) C(6) 1.39(1) . . yes C(5) H(4) 0.997 . . no C(6) H(5) 0.988 . . no C(7) C(8) 1.36(1) . . yes C(7) C(12) 1.35(1) . . yes C(8) C(9) 1.36(1) . . yes C(8) H(6) 0.990 . . no C(9) C(10) 1.38(1) . . yes C(9) H(7) 0.985 . . no C(10) C(11) 1.36(1) . . yes C(10) H(8) 0.970 . . no C(11) C(12) 1.40(1) . . yes C(11) H(9) 0.978 . . no C(12) H(10) 1.003 . . no #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S(1) As(1) S(2) 102.9(1) . 1_555 1_555 yes S(1) As(1) C(1) 95.6(3) . 1_555 1_555 yes S(2) As(1) C(1) 96.4(3) . 1_555 1_555 yes S(1) As(2) S(2) 101.6(1) . 2_565 1_555 yes S(1) As(2) C(7) 97.1(3) . 2_565 1_555 yes S(2) As(2) C(7) 94.7(3) . 1_555 1_555 yes As(1) S(1) As(2) 96.8(1) . 1_555 2_565 yes As(1) S(2) As(2) 97.02(10) . 1_555 1_555 yes As(1) C(1) C(2) 121.1(7) . 1_555 1_555 yes As(1) C(1) C(6) 119.8(7) . 1_555 1_555 yes C(2) C(1) C(6) 118.8(9) . 1_555 1_555 yes C(1) C(2) C(3) 121.3(9) . 1_555 1_555 yes C(1) C(2) H(1) 118.9 . 1_555 1_555 no C(3) C(2) H(1) 119.9 . 1_555 1_555 no C(2) C(3) C(4) 119.6(9) . 1_555 1_555 yes C(2) C(3) H(2) 119.3 . 1_555 1_555 no C(4) C(3) H(2) 121.1 . 1_555 1_555 no C(3) C(4) C(5) 120.6(9) . 1_555 1_555 yes C(3) C(4) H(3) 119.0 . 1_555 1_555 no C(5) C(4) H(3) 120.4 . 1_555 1_555 no C(4) C(5) C(6) 118.9(8) . 1_555 1_555 yes C(4) C(5) H(4) 121.5 . 1_555 1_555 no C(6) C(5) H(4) 119.5 . 1_555 1_555 no C(1) C(6) C(5) 120.8(8) . 1_555 1_555 yes C(1) C(6) H(5) 119.1 . 1_555 1_555 no C(5) C(6) H(5) 120.1 . 1_555 1_555 no As(2) C(7) C(8) 123.5(8) . 1_555 1_555 yes As(2) C(7) C(12) 117.2(7) . 1_555 1_555 yes C(8) C(7) C(12) 119.3(9) . 1_555 1_555 yes C(7) C(8) C(9) 121(1) . 1_555 1_555 yes C(7) C(8) H(6) 118.8 . 1_555 1_555 no C(9) C(8) H(6) 119.9 . 1_555 1_555 no C(8) C(9) C(10) 120(1) . 1_555 1_555 yes C(8) C(9) H(7) 119.8 . 1_555 1_555 no C(10) C(9) H(7) 119.8 . 1_555 1_555 no C(9) C(10) C(11) 118.5(10) . 1_555 1_555 yes C(9) C(10) H(8) 121.5 . 1_555 1_555 no C(11) C(10) H(8) 119.9 . 1_555 1_555 no C(10) C(11) C(12) 120.5(9) . 1_555 1_555 yes C(10) C(11) H(9) 120.0 . 1_555 1_555 no C(12) C(11) H(9) 119.5 . 1_555 1_555 no C(7) C(12) C(11) 120.0(9) . 1_555 1_555 yes C(7) C(12) H(10) 120.1 . 1_555 1_555 no C(11) C(12) H(10) 119.8 . 1_555 1_555 no #------------------------------------------------------------------------------ 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 As(1) S(1) As(2) S(2) -111.5(1) 1_555 1_555 2_565 2_565 yes As(1) S(1) As(2) C(7) 152.2(3) 1_555 1_555 2_565 2_565 yes As(1) S(2) As(2) S(1) 103.9(1) 1_555 1_555 1_555 2_565 yes As(1) S(2) As(2) C(7) -157.9(3) 1_555 1_555 1_555 1_555 yes As(1) C(1) C(2) C(3) 174.8(8) 1_555 1_555 1_555 1_555 yes As(1) C(1) C(6) C(5) -175.7(7) 1_555 1_555 1_555 1_555 yes As(2) S(1) As(1) S(2) 110.7(1) 1_555 2_565 2_565 2_565 yes As(2) S(1) As(1) C(1) -151.4(3) 1_555 2_565 2_565 2_565 yes As(2) S(2) As(1) S(1) -103.1(1) 1_555 1_555 1_555 1_555 yes As(2) S(2) As(1) C(1) 159.6(3) 1_555 1_555 1_555 1_555 yes As(2) C(7) C(8) C(9) 179(1) 1_555 1_555 1_555 1_555 yes As(2) C(7) C(12) C(11) -178.6(7) 1_555 1_555 1_555 1_555 yes S(1) As(1) C(1) C(2) 42.3(8) 1_555 1_555 1_555 1_555 yes S(1) As(1) C(1) C(6) -144.6(7) 1_555 1_555 1_555 1_555 yes S(2) As(1) C(1) C(2) 146.1(8) 1_555 1_555 1_555 1_555 yes S(2) As(1) C(1) C(6) -40.9(7) 1_555 1_555 1_555 1_555 yes S(2) As(2) C(7) C(8) -67(1) 1_555 1_555 1_555 1_555 yes S(2) As(2) C(7) C(12) 111.9(7) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(3) C(4) 0(1) 1_555 1_555 1_555 1_555 yes C(1) C(6) C(5) C(4) 1(1) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(6) C(5) -2(1) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(4) C(5) 0(1) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(1) C(6) 1(1) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(6) 0(1) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(9) C(10) 0(2) 1_555 1_555 1_555 1_555 yes C(7) C(12) C(11) C(10) -1(1) 1_555 1_555 1_555 1_555 yes C(8) C(7) C(12) C(11) 1(1) 1_555 1_555 1_555 1_555 yes C(8) C(9) C(10) C(11) 0(2) 1_555 1_555 1_555 1_555 yes C(9) C(8) C(7) C(12) 0(2) 1_555 1_555 1_555 1_555 yes C(9) C(10) C(11) C(12) 0(2) 1_555 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ #===END