#------------------------------------------------------------------------------ #$Date: 2024-11-21 01:10:52 +0200 (Thu, 21 Nov 2024) $ #$Revision: 296021 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/32/1573230.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1573230 loop_ _publ_author_name 'Sumida, Akifumi' 'Saeki, Akinori' 'Matsuo, Kyohei' 'Naka, Kensuke' 'Imoto, Hiroaki' _publ_section_title ; Dithienoarsinines: Stable and Planer \p-Extended Arsabenzenes ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC06590E _journal_year 2024 _chemical_formula_moiety 'C17 H9 As S2' _chemical_formula_sum 'C17 H9 As S2' _chemical_formula_weight 352.28 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2024-04-30 _audit_creation_method ; Olex2 1.5-ac5-024 (compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498) ; _audit_update_record ; 2024-09-20 deposited with the CCDC. 2024-11-18 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 99.317(7) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.5703(9) _cell_length_b 3.9421(3) _cell_length_c 23.8017(18) _cell_measurement_reflns_used 1704 _cell_measurement_temperature 100.00 _cell_measurement_theta_max 30.4370 _cell_measurement_theta_min 2.9060 _cell_volume 1349.08(17) _computing_cell_refinement 'CrysAlisPro 1.171.42.91a (Rigaku OD, 2023)' _computing_data_collection 'CrysAlisPro 1.171.42.91a (Rigaku OD, 2023)' _computing_data_reduction 'CrysAlisPro 1.171.42.91a (Rigaku OD, 2023)' _computing_molecular_graphics 'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 100.00 _diffrn_detector 'CCD plate' _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w 15.00 42.00 0.15 15.00 -- 30.00 54.00 -90.00 180 2 \w -66.00 -39.00 0.15 15.00 -- 30.00 54.00 0.00 180 3 \w -65.00 110.05 0.15 15.00 -- 30.00 54.00 30.00 1167 ; _diffrn_measurement_device 'two-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Mini (JP)' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0325814000 _diffrn_orient_matrix_UB_12 -0.0891523000 _diffrn_orient_matrix_UB_13 -0.0200149000 _diffrn_orient_matrix_UB_21 -0.0302175000 _diffrn_orient_matrix_UB_22 -0.0139382000 _diffrn_orient_matrix_UB_23 0.0204526000 _diffrn_orient_matrix_UB_31 -0.0214097000 _diffrn_orient_matrix_UB_32 0.1556868000 _diffrn_orient_matrix_UB_33 -0.0096449000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0343 _diffrn_reflns_av_unetI/netI 0.0558 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 4939 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.372 _diffrn_reflns_theta_min 3.074 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Rigaku (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 2.812 _exptl_absorpt_correction_T_max 0.976 _exptl_absorpt_correction_T_min 0.864 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro 1.171.42.91a (Rigaku Oxford Diffraction, 2023) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour orange _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.734 _exptl_crystal_description needle _exptl_crystal_F_000 704 _exptl_crystal_size_max 0.468 _exptl_crystal_size_mid 0.058 _exptl_crystal_size_min 0.038 _refine_diff_density_max 1.418 _refine_diff_density_min -2.132 _refine_diff_density_rms 0.174 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 181 _refine_ls_number_reflns 2741 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.053 _refine_ls_R_factor_all 0.0685 _refine_ls_R_factor_gt 0.0503 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0839P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1254 _refine_ls_wR_factor_ref 0.1369 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2141 _reflns_number_total 2741 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL 3d-needle_a.res in P2(1)/c 3d-needle.res created by SHELXL-2018/3 at 10:32:08 on 29-Apr-2024 REM Old TITL 3d-needle in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.114, Rweak 0.001, Alpha 0.026 REM 0.321 for 422 systematic absences, Orientation as input REM Formula found by SHELXT: C17 S2 As CELL 0.71073 14.5703 3.9421 23.8017 90 99.317 90 ZERR 4 0.0009 0.0003 0.0018 0 0.007 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H As S UNIT 68 36 4 8 L.S. 10 PLAN 5 SIZE 0.038 0.058 0.468 TEMP -173.15 BOND list 4 fmap 2 53 acta OMIT 2 0 0 REM REM REM WGHT 0.083900 FVAR 0.36846 AS1 3 0.329220 0.446721 0.466282 11.00000 0.00732 0.02758 = 0.01977 -0.00001 -0.00040 0.00130 S2 4 0.043421 0.867620 0.421050 11.00000 0.00893 0.02907 = 0.02578 0.00145 -0.00139 0.00273 S1 4 0.208900 0.323083 0.625288 11.00000 0.01433 0.03142 = 0.01912 -0.00043 0.00087 0.00038 C1 1 0.299695 0.358776 0.537896 11.00000 0.00905 0.01814 = 0.01937 -0.00181 -0.00282 -0.00328 C3 1 0.136939 0.592187 0.520135 11.00000 0.01240 0.02376 = 0.02480 -0.00218 0.00203 -0.00259 AFIX 43 H3 2 0.082206 0.637265 0.535786 11.00000 -1.20000 AFIX 0 C4 1 0.139865 0.678507 0.463866 11.00000 0.01047 0.02021 = 0.02472 -0.00081 -0.00280 0.00044 C14 1 0.070575 1.050314 0.310961 11.00000 0.01498 0.02433 = 0.02739 0.00125 -0.00759 -0.00178 AFIX 43 H14 2 0.009398 1.140615 0.302994 11.00000 -1.20000 AFIX 0 C2 1 0.212718 0.440910 0.553985 11.00000 0.01189 0.02239 = 0.01698 -0.00191 -0.00145 -0.00200 C11 1 0.452701 0.082110 0.583770 11.00000 0.01229 0.02569 = 0.02642 -0.00412 -0.00313 -0.00433 AFIX 43 H11 2 0.480330 0.102710 0.550413 11.00000 -1.20000 AFIX 0 C10 1 0.502100 -0.065130 0.632502 11.00000 0.01204 0.02978 = 0.03218 -0.00272 -0.00685 0.00178 AFIX 43 H10 2 0.563279 -0.148090 0.632365 11.00000 -1.20000 AFIX 0 C5 1 0.215862 0.635931 0.434319 11.00000 0.01660 0.01806 = 0.01799 -0.00363 -0.00092 -0.00011 C12 1 0.194654 0.767107 0.376509 11.00000 0.01445 0.01975 = 0.02136 -0.00047 -0.00256 -0.00077 C13 1 0.103947 0.904260 0.363938 11.00000 0.01351 0.02120 = 0.02457 -0.00032 0.00012 -0.00104 C6 1 0.362445 0.199630 0.583928 11.00000 0.01360 0.02261 = 0.01890 -0.00238 -0.00286 -0.00267 C9 1 0.461661 -0.091094 0.681765 11.00000 0.02155 0.02842 = 0.02370 0.00126 -0.00848 -0.00012 AFIX 43 H9 2 0.496294 -0.190050 0.714976 11.00000 -1.20000 AFIX 0 C7 1 0.323001 0.168268 0.633869 11.00000 0.01349 0.02405 = 0.02245 -0.00375 -0.00020 -0.00311 C8 1 0.372747 0.023555 0.683234 11.00000 0.01978 0.02992 = 0.01873 -0.00006 -0.00158 -0.00465 AFIX 43 H8 2 0.345925 0.004775 0.716919 11.00000 -1.20000 AFIX 0 C15 1 0.128403 1.059998 0.270740 11.00000 0.02806 0.02378 = 0.02185 0.00330 -0.00584 -0.00367 AFIX 43 H15 2 0.106937 1.159466 0.234650 11.00000 -1.20000 AFIX 0 C17 1 0.251880 0.782867 0.334494 11.00000 0.01597 0.02431 = 0.02577 -0.00158 0.00113 0.00059 AFIX 43 H17 2 0.313417 0.695586 0.342097 11.00000 -1.20000 AFIX 0 C16 1 0.218859 0.924978 0.282167 11.00000 0.02326 0.02573 = 0.02445 0.00019 0.00303 -0.00123 AFIX 43 H16 2 0.257494 0.931708 0.253637 11.00000 -1.20000 AFIX 0 HKLF 4 REM 3d-needle_a.res in P2(1)/c REM wR2 = 0.1369, GooF = S = 1.053, Restrained GooF = 1.053 for all data REM R1 = 0.0503 for 2141 Fo > 4sig(Fo) and 0.0685 for all 2741 data REM 181 parameters refined using 0 restraints END WGHT 0.0839 0.0000 REM Highest difference peak 1.418, deepest hole -2.132, 1-sigma level 0.174 Q1 1 0.3270 0.3844 0.4998 11.00000 0.05 1.42 Q2 1 0.3238 0.1954 0.4586 11.00000 0.05 1.21 Q3 1 0.3220 0.6922 0.4628 11.00000 0.05 1.17 Q4 1 0.3181 0.2725 0.4424 11.00000 0.05 1.05 Q5 1 0.3238 0.5124 0.4242 11.00000 0.05 0.96 REM The information below was added by Olex2. REM REM R1 = 0.0503 for 2141 Fo > 4sig(Fo) and 0.0685 for all 5572 data REM 181 parameters refined using n/a restraints REM Highest difference peak 1.42, deepest hole -2.13 REM Mean Shift 0, Max Shift -0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0685 REM R1_gt = 0.0503 REM wR_ref = 0.1369 REM GOOF = 1.053 REM Shift_max = -0.001 REM Shift_mean = 0 REM Reflections_all = 5572 REM Reflections_gt = 2141 REM Parameters = 181 REM Hole = -2.13 REM Peak = 1.42 REM Flack = n/a ; _cod_data_source_file d4sc06590e2.cif _cod_data_source_block 3d-needle _cod_database_code 1573230 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula CHSAs _chemical_oxdiff_usercomment ' ' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.901 _shelx_estimated_absorpt_t_min 0.353 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups 2.a Aromatic/amide H refined with riding coordinates: C3(H3), C14(H14), C11(H11), C10(H10), C9(H9), C8(H8), C15(H15), C17(H17), C16(H16) ; _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.334 _oxdiff_exptl_absorpt_empirical_full_min 0.738 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group As1 As 0.32922(3) 0.44672(13) 0.46628(2) 0.01851(19) Uani 1 1 d . . . . . S2 S 0.04342(8) 0.8676(3) 0.42105(5) 0.0217(3) Uani 1 1 d . . . . . S1 S 0.20890(8) 0.3231(3) 0.62529(5) 0.0218(3) Uani 1 1 d . . . . . C1 C 0.2997(3) 0.3588(11) 0.53790(19) 0.0161(9) Uani 1 1 d . . . . . C3 C 0.1369(3) 0.5922(12) 0.5201(2) 0.0204(10) Uani 1 1 d . . . . . H3 H 0.082206 0.637265 0.535786 0.025 Uiso 1 1 calc R U . . . C4 C 0.1399(3) 0.6785(12) 0.4639(2) 0.0191(10) Uani 1 1 d . . . . . C14 C 0.0706(3) 1.0503(12) 0.3110(2) 0.0235(11) Uani 1 1 d . . . . . H14 H 0.009398 1.140615 0.302994 0.028 Uiso 1 1 calc R U . . . C2 C 0.2127(3) 0.4409(12) 0.55398(19) 0.0175(9) Uani 1 1 d . . . . . C11 C 0.4527(3) 0.0821(12) 0.5838(2) 0.0222(11) Uani 1 1 d . . . . . H11 H 0.480330 0.102710 0.550413 0.027 Uiso 1 1 calc R U . . . C10 C 0.5021(3) -0.0651(13) 0.6325(2) 0.0258(11) Uani 1 1 d . . . . . H10 H 0.563279 -0.148090 0.632365 0.031 Uiso 1 1 calc R U . . . C5 C 0.2159(3) 0.6359(12) 0.43432(19) 0.0180(10) Uani 1 1 d . . . . . C12 C 0.1947(3) 0.7671(12) 0.37651(19) 0.0191(10) Uani 1 1 d . . . . . C13 C 0.1039(3) 0.9043(12) 0.3639(2) 0.0201(10) Uani 1 1 d . . . . . C6 C 0.3624(3) 0.1996(12) 0.58393(19) 0.0190(10) Uani 1 1 d . . . . . C9 C 0.4617(4) -0.0911(13) 0.6818(2) 0.0259(11) Uani 1 1 d . . . . . H9 H 0.496294 -0.190050 0.714976 0.031 Uiso 1 1 calc R U . . . C7 C 0.3230(3) 0.1683(13) 0.6339(2) 0.0203(10) Uani 1 1 d . . . . . C8 C 0.3727(3) 0.0236(13) 0.6832(2) 0.0233(11) Uani 1 1 d . . . . . H8 H 0.345925 0.004775 0.716919 0.028 Uiso 1 1 calc R U . . . C15 C 0.1284(4) 1.0600(13) 0.2707(2) 0.0257(11) Uani 1 1 d . . . . . H15 H 0.106937 1.159466 0.234650 0.031 Uiso 1 1 calc R U . . . C17 C 0.2519(3) 0.7829(13) 0.3345(2) 0.0223(10) Uani 1 1 d . . . . . H17 H 0.313417 0.695586 0.342097 0.027 Uiso 1 1 calc R U . . . C16 C 0.2189(4) 0.9250(13) 0.2822(2) 0.0246(11) Uani 1 1 d . . . . . H16 H 0.257494 0.931708 0.253637 0.029 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 As1 0.0073(3) 0.0276(3) 0.0198(3) 0.0000(2) -0.00040(18) 0.00130(19) S2 0.0089(5) 0.0291(7) 0.0258(6) 0.0014(5) -0.0014(5) 0.0027(5) S1 0.0143(6) 0.0314(7) 0.0191(6) -0.0004(5) 0.0009(4) 0.0004(5) C1 0.009(2) 0.018(2) 0.019(2) -0.0018(18) -0.0028(17) -0.0033(17) C3 0.012(2) 0.024(3) 0.025(2) -0.002(2) 0.0020(19) -0.003(2) C4 0.010(2) 0.020(2) 0.025(2) -0.001(2) -0.0028(18) 0.0004(18) C14 0.015(2) 0.024(3) 0.027(3) 0.001(2) -0.008(2) -0.002(2) C2 0.012(2) 0.022(2) 0.017(2) -0.0019(19) -0.0015(18) -0.0020(19) C11 0.012(2) 0.026(3) 0.026(3) -0.004(2) -0.0031(19) -0.004(2) C10 0.012(2) 0.030(3) 0.032(3) -0.003(2) -0.007(2) 0.002(2) C5 0.017(2) 0.018(2) 0.018(2) -0.0036(18) -0.0009(18) -0.0001(19) C12 0.014(2) 0.020(2) 0.021(2) 0.000(2) -0.0026(18) -0.0008(19) C13 0.014(2) 0.021(2) 0.025(2) 0.000(2) 0.0001(19) -0.0010(19) C6 0.014(2) 0.023(2) 0.019(2) -0.002(2) -0.0029(18) -0.0027(19) C9 0.022(3) 0.028(3) 0.024(3) 0.001(2) -0.008(2) 0.000(2) C7 0.013(2) 0.024(3) 0.022(2) -0.004(2) -0.0002(18) -0.0031(19) C8 0.020(3) 0.030(3) 0.019(2) 0.000(2) -0.002(2) -0.005(2) C15 0.028(3) 0.024(3) 0.022(3) 0.003(2) -0.006(2) -0.004(2) C17 0.016(2) 0.024(3) 0.026(3) -0.002(2) 0.0011(19) 0.001(2) C16 0.023(3) 0.026(3) 0.024(3) 0.000(2) 0.003(2) -0.001(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _diffrn_refln_index_h _diffrn_refln_index_k _diffrn_refln_index_l _diffrn_refln_intensity_net _diffrn_refln_intensity_u 0 0 3 -0.26 1.62 0 0 4 119.23 5.4 0 0 4 129.19 5.67 0 0 5 0.54 3.14 0 0 5 1.27 3.11 0 0 6 12.43 4.01 0 0 7 -2.98 3.76 0 0 8 116.05 7.39 0 0 9 4.84 3.99 0 0 9 1.42 3.07 0 0 10 603.09 20.16 0 0 10 601.33 21.73 0 0 11 -5.23 4.61 0 0 11 -2.69 3.21 0 0 12 1587.68 43.12 0 0 12 1557.53 45.31 0 0 13 -1.76 3.77 0 0 13 2.86 4.36 0 0 14 339.27 15.47 0 0 14 348.1 17.38 0 0 15 -3.07 4.34 0 0 15 -2.63 4.82 0 0 16 121.18 9.36 0 0 16 127.62 11.02 0 0 17 -1.56 4.32 0 0 17 -10.79 6.35 0 0 18 1181.51 41.28 0 0 18 1201.25 38.2 0 0 19 9.51 5.88 0 0 19 -2.24 5.79 0 0 20 1488.51 45.85 0 0 20 1432.78 49.29 0 0 21 0.14 5.86 0 0 21 2.61 6.7 0 0 22 101.04 12.13 0 0 22 85.6 10.16 0 0 23 6.05 6.96 0 0 24 379.79 23.51 0 0 25 -4.65 7.91 0 0 26 213.63 18.53 0 0 27 3.25 7.71 0 0 28 60.09 12.7 0 0 29 -6.81 8.96 0 1 0 -0.2 1.61 0 1 1 625.91 17.14 0 1 -1 620.59 17.62 0 1 -2 2679.93 62.79 0 1 2 2624.9 61.72 0 1 3 5312.09 119.47 0 1 -3 5259.09 121.47 0 1 -4 395.25 14.14 0 1 4 436.73 13.12 0 1 -5 217.21 9.96 0 1 5 228.62 8.81 0 1 6 695.86 19.79 0 1 -6 675.54 21.7 0 1 7 414.25 14.07 0 1 -7 413 15.92 0 1 8 167.51 8.54 0 1 -8 171.47 9.85 0 -1 9 238.7 12.35 0 1 -9 235.95 12.12 0 1 9 224.89 10.52 0 1 -10 31.02 5 0 -1 10 28.49 5.15 0 1 10 31.99 4.78 0 1 -11 1183.58 36.19 0 -1 11 1146.58 35.64 0 1 11 1142 33.8 0 1 -12 308.93 15.64 0 1 12 281.03 13.33 0 -1 12 301.91 15.14 0 -1 13 1468.77 43.86 0 1 -13 1466.13 44.76 0 1 13 1473.46 42.39 0 -1 14 63.59 8.12 0 1 -14 70.61 8.18 0 1 14 67.75 7.12 0 1 -15 810.12 30.82 0 1 15 829.78 28.6 0 -1 15 784.52 29.85 0 -1 16 70.8 8.9 0 1 16 81.18 8.75 0 1 -16 72.03 8.57 0 -1 17 219.03 15.19 0 1 17 228.99 14.26 0 -1 18 181.8 14.16 0 1 18 183.98 13.2 0 -1 19 6.8 7.2 0 1 19 -0.56 5.5 0 1 20 3.42 6.8 0 -1 20 0.53 5.76 0 -1 20 4.62 7.8 0 1 21 80.03 10.03 0 -1 21 82.06 11.37 0 -1 21 70.37 11.06 0 -1 22 192.16 17.65 0 -1 22 214.57 16.17 0 1 22 195.61 15.33 0 1 23 9.44 6.75 0 -1 23 -4.8 8.03 0 -1 23 17.89 8.57 0 -1 24 2.83 7.31 0 1 24 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5.03 -13 1 18 -3.27 9.88 13 1 -17 23.2 6.04 -13 1 17 38.71 12.14 13 1 -16 27.9 6.97 -13 1 16 31.56 12.13 13 1 -15 24.66 5.78 -13 1 15 18.2 10.82 13 1 -14 8.1 4.85 -13 1 14 -4.06 9.47 13 1 -13 35.85 7.23 -13 1 13 20.59 10.2 -13 1 12 22.79 9.93 13 1 -12 4.18 5.17 -13 1 11 372.29 24.68 13 1 -11 362.51 20.39 13 1 -10 89.81 10.5 13 -1 -10 87.93 9.08 13 1 -9 500.72 24.83 13 -1 -9 462.95 20.86 13 1 -8 177.91 14.53 13 -1 -8 155.74 11.92 13 1 -7 431.01 23.69 13 -1 -7 428.5 21.25 13 1 -6 21.17 7.27 13 -1 -6 18.09 6.25 13 -1 -5 1004.69 36.85 13 1 -5 968.21 38.48 13 -1 -4 265.75 17.43 13 1 -4 247.88 17.71 13 -1 -3 218.26 16.14 13 1 -3 188.72 16.1 13 -1 -2 341.71 20.58 13 1 -2 339.4 22.13 13 1 -1 69.61 11.42 13 -1 -1 43.36 8.94 13 1 0 4.85 6.77 13 -1 0 5.1 6.75 13 1 1 120.09 14.53 13 -1 1 107.07 12.56 13 1 2 13.19 8.09 13 -1 2 5.24 7.25 13 1 3 239.79 19.93 13 -1 3 229.59 18.01 13 1 4 114.77 14.27 13 -1 4 122.94 14.19 13 1 5 150.37 16.44 13 -1 5 119.47 14.78 13 1 6 24.96 9.55 13 -1 6 7.78 8.36 13 1 7 241.56 20.8 13 -1 7 233.94 18.97 13 1 8 3.76 8.16 13 -1 8 8.6 8.13 13 1 9 414.78 27.72 13 -1 9 402.98 25.86 13 1 10 14.8 9.14 13 -1 10 3.03 8.07 13 1 11 181.11 19.09 13 -1 11 148.9 17.12 13 1 12 -4.52 9.79 13 -1 12 14.82 9.38 13 1 13 78.88 14.19 13 -1 13 95.65 14.56 13 1 14 -0.27 9.54 13 -1 14 28.28 11.33 13 1 15 -2.33 10.25 13 -1 15 16.37 10.35 13 -1 16 121.4 17.25 13 1 16 120.62 18.07 13 2 -20 65.63 10.22 13 2 -19 5.8 5.55 13 2 -18 99.73 12.19 13 2 -17 165.69 14.89 13 2 -16 42.16 8.32 13 2 -15 235.58 17.78 13 2 -14 -10.53 6.46 13 2 -13 72.07 10.2 13 2 -12 7.72 5.45 13 2 -11 1.12 5.39 13 2 -10 22.61 6.9 13 2 -9 -0.48 6.1 13 2 -8 370 23.09 13 2 -7 31.56 8.38 13 2 -6 371.16 23.59 13 2 -5 31.19 8.6 13 -2 -4 321.16 18.52 13 2 -4 342.99 23.22 13 2 -3 18.46 8.21 13 -2 -3 26.41 8.21 13 2 -2 60.18 11.31 13 -2 -2 49.86 9.55 13 2 -1 33.98 9.01 13 -2 -1 19.35 7.98 13 2 0 13.13 7.75 13 -2 0 16.42 8.29 13 2 1 146.98 15.77 13 -2 1 151.59 14.7 13 2 2 -2.89 7.36 13 -2 2 2.85 7.83 13 -2 3 458.65 25.56 13 2 3 436.01 27.8 13 2 4 94.96 13.83 13 -2 4 83.97 12.46 13 -2 5 352.35 23.3 13 2 5 334.15 24.99 13 -2 6 212.96 19.16 13 2 6 224.76 20.79 13 -2 7 13.55 9.24 13 2 7 15.45 8.56 13 -2 8 194.09 18.9 13 2 8 200.83 20.66 13 -2 9 158.27 17.71 13 2 9 112.06 16.43 13 -2 10 163.91 17.29 13 2 10 193.43 20.63 13 -2 11 1.37 10.13 13 2 11 7.48 9.44 13 -2 12 99.99 15.35 13 2 12 101.16 15.77 13 -2 13 -3.42 10.32 13 2 13 -0.8 10.65 13 3 -13 45.53 10.03 13 3 -12 23.49 8.36 13 3 -11 -2.84 7.63 13 3 -10 120.94 14.51 13 3 -9 1.97 6.28 13 3 -8 10.77 7.23 13 3 -7 39.76 10.08 13 3 -6 -6.74 7.98 13 3 -5 149.67 16.06 13 3 -4 34.64 9.95 13 3 -3 4.6 7.79 13 3 -2 148.02 17.35 13 3 -1 41.2 10.43 13 3 0 174.05 18.39 13 3 1 93.94 14.47 13 3 2 179.84 19.31 13 3 3 -10.66 10.02 13 -3 4 59.88 11.85 13 3 4 63.37 12.65 13 -3 5 141.88 16.69 13 3 5 156.21 18.41 13 -3 6 7.39 9.91 13 3 6 0.63 8.4 -14 0 22 147.38 19.24 -14 0 21 -29.38 13.25 -14 0 20 150.27 18.05 -14 0 19 -1.76 10.26 -14 0 18 50.98 13.37 -14 0 17 1.33 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-1 21 12.23 10.58 14 1 -21 21.42 7.76 -14 -1 20 16.87 11.13 14 1 -20 -1.03 5.9 14 1 -19 44.81 8.79 -14 -1 19 35.45 10.44 14 1 -18 -10.57 6.33 -14 -1 18 5.57 10.06 14 1 -17 -6.27 6.18 -14 1 17 -0.05 10.57 14 1 -16 33.56 7.8 -14 1 16 34.19 12.24 -14 1 15 174.42 19.49 14 1 -15 175.68 14.34 -14 1 14 126.4 16.75 14 1 -14 127.6 12.31 -14 1 13 233.46 21.02 14 1 -13 235.05 16.81 14 1 -12 11.43 6.38 14 1 -11 367.85 21.61 14 1 -10 59.76 9.42 14 -1 -10 73.89 8.74 14 1 -9 326.65 20.6 14 -1 -9 312.89 17.54 14 1 -8 121.45 13.09 14 -1 -8 100.76 10.11 14 1 -7 148.26 14.23 14 -1 -7 157.83 13.15 14 1 -6 112.19 12.69 14 -1 -6 99.24 11.44 14 1 -5 25.45 7.62 14 -1 -5 49.9 8.93 14 1 -4 61.62 10 14 -1 -4 68.76 10.59 14 1 -3 60.56 10.93 14 -1 -3 63.38 10.76 14 1 -2 2.8 6.45 14 -1 -2 8.37 8.03 14 1 -1 21.77 7.48 14 -1 -1 50.92 9.91 14 1 0 -9.37 7.81 14 -1 0 -5.77 7.94 14 1 1 11.24 8.6 14 -1 1 9.78 7.71 14 1 2 26.8 9.79 14 -1 2 13.48 8.94 14 1 3 165.13 17.45 14 -1 3 164.98 16.48 14 1 4 16.75 9.5 14 -1 4 1.2 8.8 14 1 5 532.56 31.47 14 -1 5 548.34 30.01 14 1 6 3.41 8.5 14 -1 6 -2.98 8.19 14 1 7 243.2 21.35 14 -1 7 252.54 21.4 14 1 8 -0.44 9.06 14 -1 8 0.57 8.4 14 1 9 193.28 19.65 14 -1 9 184.88 18.17 14 1 10 149.11 18.19 14 -1 10 143.25 17.1 14 1 11 6.01 10.46 14 -1 11 -4.11 9.92 14 1 12 101.81 15.76 14 -1 12 93.91 14.88 14 1 13 83.33 14.94 14 -1 13 83.11 14.48 14 1 14 -3.32 10.13 14 -1 14 11.67 10.48 14 2 -18 31.11 7.77 14 2 -17 -0.22 6.55 14 2 -16 10.06 5.6 14 2 -15 9.83 6.33 14 2 -14 81.77 11.13 14 2 -13 38.32 8.88 14 2 -12 166.46 15.07 14 2 -11 12.83 7.05 14 2 -10 93.79 12.35 14 2 -9 57.05 10.58 14 2 -8 24.04 7.96 14 2 -7 4.13 6.34 14 2 -6 68.12 11.67 14 2 -5 10.19 7.54 14 2 -4 5.71 7.57 14 -2 -3 489.87 25.47 14 2 -3 593.97 32 14 2 -2 55.64 10.93 14 -2 -2 67.69 11.37 14 -2 -1 450.64 24.92 14 2 -1 470.46 28.64 14 2 0 95.56 13.49 14 -2 0 94.25 12.93 14 2 1 1 7.61 14 -2 1 -0.8 8.71 14 -2 2 276.99 21.05 14 2 2 254.88 21.19 14 -2 3 323.16 22.82 14 2 3 309.86 24.02 14 2 4 67.02 12.98 14 -2 4 67.05 12.72 14 2 5 152.92 17.91 14 -2 5 144.1 15.59 14 2 6 64.67 13.26 14 -2 6 88.04 13.92 14 2 7 66.32 13.17 14 -2 7 44.05 11.83 14 2 8 87.82 15.79 14 -2 8 70.91 13.38 14 -2 9 105.55 15.32 14 2 9 122.88 17.45 14 -2 10 -0.04 9.61 14 2 10 11.2 10.23 14 3 -9 3.97 7.17 14 3 -8 160.27 17.33 14 3 -7 9.96 7.4 14 3 -6 240.86 20.9 14 3 -5 18.4 7.96 14 3 -4 62.94 12.01 14 3 -3 51.29 11.29 14 3 -2 -1.45 7.99 14 3 -1 151.01 17.86 14 3 0 29.09 9.58 14 3 1 302.62 24.78 14 3 2 5.01 8.79 -15 0 20 150.75 19.39 -15 0 19 -24.69 12.82 -15 0 18 23.98 11.9 -15 0 17 -10.24 10.44 -15 0 16 49.45 13.81 15 0 -15 -1.03 5 -15 0 15 -0.47 11.2 15 0 -14 433.68 22.43 -15 0 14 475.18 30.2 -15 0 13 21.16 11.01 15 0 -13 4.44 5.24 15 0 -12 473.49 24.01 -15 0 12 477.44 30.02 -15 0 11 10.58 11.07 15 0 -11 1.6 5.84 -15 0 10 1.13 10.09 15 0 -10 4.73 5.54 -15 0 9 -9.19 10.32 15 0 -9 1.29 5.61 -15 0 8 135.3 17.05 15 0 -8 121.7 12.3 -15 0 7 -8.05 10.34 15 0 -7 -0.2 6.13 15 0 -6 159.67 14.17 -15 0 6 153.58 17.06 15 0 -5 4.3 6.01 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16 1 -15 38.53 9.05 -16 -1 15 28.86 11.94 16 1 -14 2.71 6.64 -16 -1 14 -7.76 10.75 16 1 -13 6.83 7.17 -16 -1 13 2.36 10.29 16 1 -12 56.75 9.48 16 1 -11 3.53 6.79 16 1 -10 0.1 6.52 16 1 -9 82.28 12.18 16 1 -8 1.42 6.89 16 1 -7 273.26 21.02 16 -1 -7 260.6 18.35 16 1 -6 28.3 9.68 16 -1 -6 25.6 8.24 16 1 -5 337.25 23.11 16 -1 -5 332.4 22.12 16 1 -4 -0.97 7.73 16 -1 -4 5.09 7.81 16 -1 -3 193.58 17.45 16 1 -3 205.66 18.7 16 1 -2 57.09 11.56 16 -1 -2 47.7 10.84 16 1 -1 97.86 14.04 16 -1 -1 88.29 13.99 16 1 0 157.67 17.91 16 -1 0 131.34 16.21 16 1 1 -9.42 9.51 16 -1 1 -0.76 8.98 16 1 2 -1.67 8.57 16 -1 2 -9.72 9.14 16 1 3 325.18 25.31 16 -1 3 290.1 23.18 16 1 4 82.79 14.43 16 -1 4 73.31 14.15 16 1 5 295.73 24.61 16 -1 5 271.06 23.05 16 1 6 17.37 10.34 16 -1 6 12.07 9.43 16 1 7 162.56 19.05 16 -1 7 140.71 17.29 16 1 8 20.84 11.37 16 -1 8 22.42 10.73 16 2 -11 63.24 10.87 16 2 -10 68.73 11.83 16 2 -9 -2.08 7.39 16 2 -8 72.7 12.87 16 2 -7 55.57 11.1 16 2 -6 67.55 12.68 16 2 -5 -10.39 9.44 16 2 -4 40.18 10.35 16 2 -3 21.51 9.25 16 2 -2 38.56 10.33 16 2 -1 -5.74 8.18 16 2 0 -2.9 7.9 16 2 1 11.96 8.66 16 -2 1 -4.36 10.15 16 2 2 -0.55 8.22 16 -2 2 5.9 9.55 16 2 3 -30.26 11.57 16 -2 3 -6.27 9.93 -17 0 15 6.47 11.62 -17 0 14 328.28 27.36 -17 0 13 0.9 11.71 17 0 -12 442.08 24.88 -17 0 12 424.41 30.24 17 0 -11 4.32 7.48 -17 0 11 5.06 12.26 17 0 -10 145 15.08 -17 0 10 108.64 17.2 17 0 -9 -8.61 7.44 -17 0 9 1.39 11.99 17 0 -8 -1.25 6.74 -17 0 8 -3.34 11.22 17 0 -7 10.66 7.86 -17 0 7 -9.39 12.28 17 0 -6 74.06 11.3 -17 0 6 76.19 15.3 17 0 -5 10.49 7.92 -17 0 5 -5.21 10.93 17 0 -4 291.14 22.72 17 0 -3 -4.36 8.85 17 0 -2 99.07 14.85 17 0 -1 -26.56 11.94 17 0 0 726.48 38.32 17 0 1 17.04 10.83 17 0 2 490.21 31.32 17 0 3 -5.37 9.73 17 0 4 258.58 23.49 17 0 5 -1.32 9.43 17 0 6 238.77 22.24 -17 -1 13 338.28 27.36 17 1 -13 322.69 22.13 -17 -1 12 -5.76 12.15 17 1 -12 10.2 6.76 -17 -1 11 269.29 24.46 17 1 -11 301.26 21.77 17 1 -10 12.73 7.6 -17 -1 10 16.75 11.98 -17 -1 9 196.47 21.56 17 1 -9 227.15 19.51 -17 -1 8 108.13 17.31 17 1 -8 106.57 13.67 -17 -1 7 116.11 18.73 17 1 -7 140.66 16.2 -17 -1 6 324.85 26.93 17 1 -6 336.39 24.24 17 1 -5 -2.4 8.18 17 -1 -5 4.26 7.84 -17 -1 5 -7.37 12.86 17 1 -4 37.23 10.61 17 -1 -4 39.03 10.74 -17 -1 4 16.25 13.05 17 1 -3 104.12 14.92 17 -1 -3 97.65 14.28 17 1 -2 10.16 7.74 17 -1 -2 10.41 8.83 17 -1 -1 224.58 20.57 17 1 -1 241.02 21.68 17 1 0 2.37 8.92 17 -1 0 5.09 8.84 17 1 1 218.81 21.19 17 -1 1 218.63 20.98 17 1 2 57.44 13.49 17 -1 2 49.09 12.84 17 1 3 107.34 16.04 17 -1 3 116.47 16.02 17 1 4 0.25 9.55 17 -1 4 -6.58 10.15 18 0 -9 -2.15 7.26 -18 0 9 -54.76 15.56 18 0 -8 9.26 7.99 -18 0 8 10.3 12.75 18 0 -7 11.92 8.55 18 0 -6 147.76 16.13 18 0 -5 -6.26 8.14 18 0 -4 411.22 27.2 18 0 -3 -0.17 9.32 18 0 -2 215.88 21.19 18 0 -1 -2.97 9.17 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -1 0 1 0.0300 1 0 -1 0.0134 -1 1 -2 0.1939 1 -1 2 0.2040 0 0 1 0.0175 0 0 -1 0.0206 2 0 1 0.0190 -2 0 -1 0.0437 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 As1 C5 97.4(2) . . ? C13 S2 C4 91.7(2) . . ? C7 S1 C2 91.5(2) . . ? C2 C1 As1 123.7(3) . . ? C2 C1 C6 112.1(4) . . ? C6 C1 As1 124.2(3) . . ? C4 C3 C2 121.2(4) . . ? C3 C4 S2 121.0(4) . . ? C3 C4 C5 126.8(4) . . ? C5 C4 S2 112.2(4) . . ? C15 C14 C13 118.4(5) . . ? C1 C2 S1 111.5(3) . . ? C3 C2 S1 121.5(4) . . ? C3 C2 C1 126.9(4) . . ? C10 C11 C6 119.9(5) . . ? C11 C10 C9 119.9(5) . . ? C4 C5 As1 124.0(4) . . ? C4 C5 C12 111.4(4) . . ? C12 C5 As1 124.6(3) . . ? C13 C12 C5 112.6(4) . . ? C17 C12 C5 129.0(4) . . ? C17 C12 C13 118.4(4) . . ? C14 C13 S2 126.2(4) . . ? C14 C13 C12 121.6(4) . . ? C12 C13 S2 112.1(4) . . ? C11 C6 C1 128.4(4) . . ? C11 C6 C7 119.2(4) . . ? C7 C6 C1 112.5(4) . . ? C8 C9 C10 121.5(5) . . ? C6 C7 S1 112.4(4) . . ? C8 C7 S1 126.4(4) . . ? C8 C7 C6 121.2(4) . . ? C9 C8 C7 118.3(5) . . ? C14 C15 C16 121.0(5) . . ? C16 C17 C12 120.1(5) . . ? C17 C16 C15 120.5(5) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag As1 C1 1.857(5) . ? As1 C5 1.859(5) . ? S2 C4 1.762(5) . ? S2 C13 1.742(5) . ? S1 C2 1.769(5) . ? S1 C7 1.752(5) . ? C1 C2 1.419(6) . ? C1 C6 1.451(6) . ? C3 C4 1.389(7) . ? C3 C2 1.391(7) . ? C4 C5 1.415(6) . ? C14 C13 1.400(7) . ? C14 C15 1.374(7) . ? C11 C10 1.389(7) . ? C11 C6 1.395(7) . ? C10 C9 1.399(7) . ? C5 C12 1.456(6) . ? C12 C13 1.414(6) . ? C12 C17 1.403(6) . ? C6 C7 1.407(6) . ? C9 C8 1.378(7) . ? C7 C8 1.398(7) . ? C15 C16 1.406(7) . ? C17 C16 1.379(7) . ? loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -1.0010 -0.0004 0.9988 0.0127 0.0507 0.0117 1.0010 0.0004 -0.9988 -0.0127 -0.0507 -0.0117 -1.0038 1.0017 -1.9902 -0.0168 -0.0243 0.1966 1.0038 -1.0017 1.9902 0.0168 0.0243 -0.1966 -0.0006 -0.0003 1.0009 -0.0200 0.0205 -0.0097 0.0006 0.0003 -1.0009 0.0200 -0.0205 0.0097 2.0004 -0.0001 1.0051 -0.0853 -0.0399 -0.0525 -2.0004 0.0001 -1.0051 0.0853 0.0399 0.0525