#------------------------------------------------------------------------------ #$Date: 2024-11-21 01:10:52 +0200 (Thu, 21 Nov 2024) $ #$Revision: 296021 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/32/1573234.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_1573234 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 'C23 H13 As S2' _chemical_formula_sum 'C23 H13 As S2' _chemical_formula_weight 428.37 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-I 2ya' _space_group_name_H-M_alt 'I 1 2/a 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2024-06-23 _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 90.732(3) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 16.1897(5) _cell_length_b 7.1373(3) _cell_length_c 31.4478(9) _cell_measurement_reflns_used 6237 _cell_measurement_temperature 100.00 _cell_measurement_theta_max 32.8100 _cell_measurement_theta_min 2.8810 _cell_volume 3633.5(2) _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 0.999 _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 -68.00 114.00 0.10 1.75 -- 30.00 54.00-180.00 1820 2 \w 41.00 79.00 0.10 1.75 -- 30.00 54.00 90.00 380 3 \w -17.00 19.00 0.10 1.75 -- 30.00 54.00 120.00 360 4 \w 41.00 66.00 0.10 1.75 -- 30.00 54.00 30.00 250 ; _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 0.0412406000 _diffrn_orient_matrix_UB_12 -0.0332215000 _diffrn_orient_matrix_UB_13 0.0006042000 _diffrn_orient_matrix_UB_21 -0.0008111000 _diffrn_orient_matrix_UB_22 -0.0010570000 _diffrn_orient_matrix_UB_23 0.0225387000 _diffrn_orient_matrix_UB_31 -0.0146949000 _diffrn_orient_matrix_UB_32 -0.0937458000 _diffrn_orient_matrix_UB_33 -0.0004696000 _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 0.0240 _diffrn_reflns_av_unetI/netI 0.0274 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_number 8410 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.373 _diffrn_reflns_theta_min 2.591 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Rigaku (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 2.104 _exptl_absorpt_correction_T_max 0.122 _exptl_absorpt_correction_T_min 0.015 _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 colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.566 _exptl_crystal_description block _exptl_crystal_F_000 1728 _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.15 _refine_diff_density_max 0.653 _refine_diff_density_min -0.353 _refine_diff_density_rms 0.078 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 235 _refine_ls_number_reflns 3705 _refine_ls_number_restraints 36 _refine_ls_restrained_S_all 1.082 _refine_ls_R_factor_all 0.0359 _refine_ls_R_factor_gt 0.0345 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0462P)^2^+7.1908P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0909 _refine_ls_wR_factor_ref 0.0919 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3540 _reflns_number_total 3705 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL 3c-benzyne_a.res in I2/a 3c-benzyne.res created by SHELXL-2018/3 at 15:16:14 on 23-Jun-2024 REM Old TITL 3c-benzyne in I2/a REM SHELXT solution in I2/a: R1 0.122, Rweak 0.027, Alpha 0.026 REM 1.452 for 308 systematic absences, Orientation as input REM Formula found by SHELXT: C23 S2 As CELL 0.71073 16.1897 7.1373 31.4478 90 90.732 90 ZERR 8 0.0005 0.0003 0.0009 0 0.003 0 LATT 2 SYMM 0.5-X,+Y,-Z SFAC C H As S UNIT 184 104 8 16 RIGU 0.002 0.002 C8 C1 C7 C4 C6 C5 L.S. 20 0 0 PLAN 1 SIZE 0.15 0.33 0.54 TEMP -173.15 BOND list 4 fmap 2 53 ACTA OMIT 1 1 0 OMIT 0 1 1 REM REM REM WGHT 0.046200 7.190800 FVAR 0.22038 AS1 3 0.314316 0.722637 0.657929 11.00000 0.03634 0.02227 = 0.02124 -0.00163 -0.00103 -0.01375 S2 4 0.199661 0.553304 0.735777 11.00000 0.02986 0.01753 = 0.01983 -0.00263 -0.00057 -0.00402 S1 4 0.214710 0.855037 0.569587 11.00000 0.04489 0.01772 = 0.02617 0.00162 -0.00022 0.00314 C22 1 0.137222 0.081348 0.678075 11.00000 0.02030 0.01759 = 0.02214 -0.00198 -0.00337 0.00023 AFIX 43 H22 2 0.148601 0.025962 0.651313 11.00000 -1.20000 AFIX 0 C17 1 0.171725 0.256312 0.688898 11.00000 0.01507 0.01740 = 0.02093 0.00232 -0.00389 0.00248 C16 1 0.223915 0.378897 0.665058 11.00000 0.01690 0.01660 = 0.02007 0.00113 -0.00363 -0.00059 C9 1 0.231181 0.510109 0.592674 11.00000 0.02093 0.01667 = 0.02028 -0.00124 0.00016 -0.00009 C3 1 0.242945 0.540334 0.685857 11.00000 0.02550 0.01868 = 0.01982 0.00024 -0.00126 -0.00395 C23 1 0.258631 0.347883 0.620863 11.00000 0.01832 0.01519 = 0.02036 -0.00001 -0.00219 -0.00104 AFIX 13 H23 2 0.239465 0.225505 0.608804 11.00000 -1.20000 AFIX 0 C18 1 0.153258 0.334372 0.729030 11.00000 0.01886 0.01664 = 0.02160 -0.00013 -0.00419 0.00066 C21 1 0.086705 -0.009465 0.706581 11.00000 0.02364 0.01960 = 0.02717 0.00059 -0.00469 -0.00471 AFIX 43 H21 2 0.063096 -0.127041 0.699159 11.00000 -1.20000 AFIX 0 C19 1 0.102897 0.242051 0.758169 11.00000 0.02071 0.02305 = 0.02082 -0.00035 -0.00128 0.00214 AFIX 43 H19 2 0.091713 0.295552 0.785151 11.00000 -1.20000 AFIX 0 C20 1 0.069843 0.070345 0.746499 11.00000 0.02083 0.02555 = 0.02475 0.00437 0.00085 -0.00247 AFIX 43 H20 2 0.035257 0.005381 0.765719 11.00000 -1.20000 AFIX 0 C10 1 0.184503 0.502204 0.553516 11.00000 0.02108 0.02358 = 0.01925 0.00020 0.00088 0.00460 C8 1 0.353183 0.354349 0.624213 11.00000 0.01811 0.03037 = 0.01902 0.00701 -0.00210 -0.00253 C15 1 0.153121 0.347407 0.531298 11.00000 0.02427 0.02622 = 0.02403 -0.00277 -0.00202 0.00089 AFIX 43 H15 2 0.162125 0.224195 0.541802 11.00000 -1.20000 AFIX 0 C2 1 0.250632 0.687739 0.605018 11.00000 0.03123 0.01823 = 0.02245 0.00336 -0.00140 -0.00202 C1 1 0.388720 0.518042 0.640543 11.00000 0.02548 0.03435 = 0.02029 0.00555 -0.00210 -0.00902 C7 1 0.402810 0.206940 0.611404 11.00000 0.02315 0.03572 = 0.02441 0.01087 0.00110 0.00554 AFIX 43 H7 2 0.378503 0.095192 0.600625 11.00000 -1.20000 AFIX 0 C4 1 0.475129 0.537337 0.643329 11.00000 0.01988 0.05227 = 0.02080 0.00689 -0.00615 -0.01193 AFIX 43 H4 2 0.499710 0.649843 0.653514 11.00000 -1.20000 AFIX 0 C11 1 0.170409 0.683902 0.537009 11.00000 0.03084 0.02570 = 0.02380 0.00022 0.00107 0.00538 C14 1 0.108884 0.375264 0.493916 11.00000 0.02803 0.04076 = 0.02513 -0.00615 -0.00481 -0.00003 AFIX 43 H14 2 0.087298 0.270467 0.478827 11.00000 -1.20000 AFIX 0 C12 1 0.125586 0.711653 0.499192 11.00000 0.03554 0.03441 = 0.02737 0.00654 0.00051 0.01356 AFIX 43 H12 2 0.116131 0.834211 0.488398 11.00000 -1.20000 AFIX 0 C13 1 0.095547 0.556517 0.478044 11.00000 0.02937 0.05247 = 0.02213 -0.00025 -0.00419 0.00833 AFIX 43 H13 2 0.065241 0.572579 0.452234 11.00000 -1.20000 AFIX 0 C6 1 0.488933 0.223381 0.614416 11.00000 0.02387 0.05824 = 0.03445 0.01615 0.00144 0.01032 AFIX 43 H6 2 0.523167 0.123341 0.605340 11.00000 -1.20000 AFIX 0 C5 1 0.523943 0.384969 0.630572 11.00000 0.02272 0.06799 = 0.03395 0.01979 -0.00287 -0.00276 AFIX 43 H5 2 0.582353 0.393496 0.633137 11.00000 -1.20000 AFIX 0 HKLF 4 REM 3c-benzyne_a.res in I2/a REM wR2 = 0.0919, GooF = S = 1.084, Restrained GooF = 1.082 for all data REM R1 = 0.0345 for 3540 Fo > 4sig(Fo) and 0.0359 for all 3705 data REM 235 parameters refined using 36 restraints END WGHT 0.0462 7.1907 REM Highest difference peak 0.653, deepest hole -0.353, 1-sigma level 0.078 Q1 1 0.3632 0.6668 0.6553 11.00000 0.05 0.65 REM The information below was added by Olex2. REM REM R1 = 0.0345 for 3540 Fo > 4sig(Fo) and 0.0359 for all 8904 data REM 235 parameters refined using n/a restraints REM Highest difference peak 0.65, deepest hole -0.35 REM Mean Shift 0, Max Shift 0.003. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0359 REM R1_gt = 0.0345 REM wR_ref = 0.0919 REM GOOF = 1.084 REM Shift_max = 0.003 REM Shift_mean = 0 REM Reflections_all = 8904 REM Reflections_gt = 3540 REM Parameters = 235 REM Hole = -0.35 REM Peak = 0.65 REM Flack = n/a ; _cod_data_source_file d4sc06590e2.cif _cod_data_source_block 3c-benzyne _cod_database_code 1573234 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula CHAsS _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 0.743 _shelx_estimated_absorpt_t_min 0.396 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups 2. Rigid body (RIGU) restrains C8, C1, C7, C4, C6, C5 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002 3.a Ternary CH refined with riding coordinates: C23(H23) 3.b Aromatic/amide H refined with riding coordinates: C22(H22), C21(H21), C19(H19), C20(H20), C15(H15), C7(H7), C4(H4), C14(H14), C12(H12), C13(H13), C6(H6), C5(H5) ; _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 1.826 _oxdiff_exptl_absorpt_empirical_full_min 0.510 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' '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 0.31432(2) 0.72264(4) 0.65793(2) 0.02663(11) Uani 1 1 d . . . . . S2 S 0.19966(4) 0.55330(9) 0.73578(2) 0.02241(15) Uani 1 1 d . . . . . S1 S 0.21471(4) 0.85504(9) 0.56959(2) 0.02960(16) Uani 1 1 d . . . . . C22 C 0.13722(14) 0.0813(3) 0.67808(7) 0.0200(5) Uani 1 1 d . . . . . H22 H 0.148601 0.025962 0.651313 0.024 Uiso 1 1 calc R U . . . C17 C 0.17173(13) 0.2563(3) 0.68890(7) 0.0178(5) Uani 1 1 d . . . . . C16 C 0.22392(13) 0.3789(3) 0.66506(7) 0.0179(4) Uani 1 1 d . . . . . C9 C 0.23118(14) 0.5101(3) 0.59267(7) 0.0193(5) Uani 1 1 d . . . . . C3 C 0.24295(14) 0.5403(3) 0.68586(7) 0.0213(5) Uani 1 1 d . . . . . C23 C 0.25863(13) 0.3479(3) 0.62086(7) 0.0180(4) Uani 1 1 d . . . . . H23 H 0.239465 0.225505 0.608804 0.022 Uiso 1 1 calc R U . . . C18 C 0.15326(13) 0.3344(3) 0.72903(7) 0.0191(4) Uani 1 1 d . . . . . C21 C 0.08670(14) -0.0095(4) 0.70658(8) 0.0235(5) Uani 1 1 d . . . . . H21 H 0.063096 -0.127041 0.699159 0.028 Uiso 1 1 calc R U . . . C19 C 0.10290(14) 0.2421(4) 0.75817(8) 0.0215(5) Uani 1 1 d . . . . . H19 H 0.091713 0.295552 0.785151 0.026 Uiso 1 1 calc R U . . . C20 C 0.06984(14) 0.0703(4) 0.74650(8) 0.0237(5) Uani 1 1 d . . . . . H20 H 0.035257 0.005381 0.765719 0.028 Uiso 1 1 calc R U . . . C10 C 0.18450(14) 0.5022(4) 0.55352(7) 0.0213(5) Uani 1 1 d . . . . . C8 C 0.35318(14) 0.3543(4) 0.62421(7) 0.0225(5) Uani 1 1 d . . . . . C15 C 0.15312(15) 0.3474(4) 0.53130(8) 0.0249(5) Uani 1 1 d . . . . . H15 H 0.162125 0.224195 0.541802 0.030 Uiso 1 1 calc R U . . . C2 C 0.25063(16) 0.6877(4) 0.60502(8) 0.0240(5) Uani 1 1 d . . . . . C1 C 0.38872(15) 0.5180(4) 0.64054(7) 0.0267(5) Uani 1 1 d . . . . . C7 C 0.40281(15) 0.2069(4) 0.61140(8) 0.0278(5) Uani 1 1 d . . . . . H7 H 0.378503 0.095192 0.600625 0.033 Uiso 1 1 calc R U . . . C4 C 0.47513(15) 0.5373(5) 0.64333(8) 0.0310(6) Uani 1 1 d . . . . . H4 H 0.499710 0.649843 0.653514 0.037 Uiso 1 1 calc R U . . . C11 C 0.17041(16) 0.6839(4) 0.53701(8) 0.0268(5) Uani 1 1 d . . . . . C14 C 0.10888(16) 0.3753(4) 0.49392(8) 0.0314(6) Uani 1 1 d . . . . . H14 H 0.087298 0.270467 0.478827 0.038 Uiso 1 1 calc R U . . . C12 C 0.12559(17) 0.7117(4) 0.49919(9) 0.0324(6) Uani 1 1 d . . . . . H12 H 0.116131 0.834211 0.488398 0.039 Uiso 1 1 calc R U . . . C13 C 0.09555(16) 0.5565(5) 0.47804(8) 0.0347(6) Uani 1 1 d . . . . . H13 H 0.065241 0.572579 0.452234 0.042 Uiso 1 1 calc R U . . . C6 C 0.48893(17) 0.2234(5) 0.61442(9) 0.0388(7) Uani 1 1 d . . . . . H6 H 0.523167 0.123341 0.605340 0.047 Uiso 1 1 calc R U . . . C5 C 0.52394(16) 0.3850(5) 0.63057(9) 0.0416(7) Uani 1 1 d . . . . . H5 H 0.582353 0.393496 0.633137 0.050 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 0.03634(17) 0.02227(17) 0.02124(15) -0.00163(10) -0.00103(11) -0.01375(11) S2 0.0299(3) 0.0175(3) 0.0198(3) -0.0026(2) -0.0006(2) -0.0040(2) S1 0.0449(4) 0.0177(3) 0.0262(3) 0.0016(3) -0.0002(3) 0.0031(3) C22 0.0203(10) 0.0176(12) 0.0221(11) -0.0020(9) -0.0034(8) 0.0002(9) C17 0.0151(10) 0.0174(11) 0.0209(11) 0.0023(9) -0.0039(8) 0.0025(8) C16 0.0169(10) 0.0166(12) 0.0201(10) 0.0011(9) -0.0036(8) -0.0006(9) C9 0.0209(10) 0.0167(12) 0.0203(10) -0.0012(9) 0.0002(8) -0.0001(9) C3 0.0255(11) 0.0187(12) 0.0198(10) 0.0002(9) -0.0013(8) -0.0040(9) C23 0.0183(10) 0.0152(11) 0.0204(10) 0.0000(9) -0.0022(8) -0.0010(9) C18 0.0189(10) 0.0166(12) 0.0216(11) -0.0001(9) -0.0042(8) 0.0007(9) C21 0.0236(11) 0.0196(12) 0.0272(12) 0.0006(10) -0.0047(9) -0.0047(10) C19 0.0207(11) 0.0230(13) 0.0208(11) -0.0003(9) -0.0013(9) 0.0021(9) C20 0.0208(11) 0.0256(13) 0.0248(11) 0.0044(10) 0.0008(9) -0.0025(10) C10 0.0211(11) 0.0236(13) 0.0193(10) 0.0002(9) 0.0009(8) 0.0046(9) C8 0.0181(10) 0.0304(13) 0.0190(10) 0.0070(10) -0.0021(8) -0.0025(9) C15 0.0243(11) 0.0262(14) 0.0240(11) -0.0028(10) -0.0020(9) 0.0009(10) C2 0.0312(12) 0.0182(12) 0.0225(11) 0.0034(10) -0.0014(9) -0.0020(10) C1 0.0255(11) 0.0343(14) 0.0203(11) 0.0056(10) -0.0021(9) -0.0090(10) C7 0.0231(11) 0.0357(15) 0.0244(12) 0.0109(11) 0.0011(9) 0.0055(10) C4 0.0199(11) 0.0523(17) 0.0208(11) 0.0069(11) -0.0061(9) -0.0119(11) C11 0.0308(13) 0.0257(14) 0.0238(12) 0.0002(10) 0.0011(9) 0.0054(11) C14 0.0280(12) 0.0408(17) 0.0251(12) -0.0061(12) -0.0048(10) 0.0000(12) C12 0.0355(14) 0.0344(16) 0.0274(13) 0.0065(11) 0.0005(11) 0.0136(12) C13 0.0294(13) 0.0525(19) 0.0221(12) -0.0002(12) -0.0042(10) 0.0083(13) C6 0.0239(12) 0.0582(19) 0.0344(15) 0.0161(13) 0.0014(11) 0.0103(12) C5 0.0227(12) 0.068(2) 0.0339(14) 0.0198(14) -0.0029(10) -0.0028(12) 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 4 977.25 6.46 0 0 -4 1065.12 6.46 0 0 6 755.77 7.91 0 0 -6 747.89 10.46 0 0 8 1923.92 16.87 0 0 -8 1890.94 17.89 0 0 -8 1944.19 20.68 0 0 10 2547.54 21.96 0 0 -10 2525.3 23.07 0 0 -10 2540.96 26.27 0 0 -12 1491.48 16.74 0 0 -12 1503.72 19.51 0 0 12 1528.12 15.75 0 0 -14 43.53 3.04 0 0 14 43.68 2.3 0 0 -14 41.66 2.44 0 0 -16 36.67 2.41 0 0 16 42.25 2.4 0 0 -16 37.41 2.98 0 0 -18 341.22 9.4 0 0 18 342.47 7.28 0 0 -18 345.21 8.02 0 0 -20 86.92 4.05 0 0 -20 99.45 5.03 0 0 20 91.3 3.79 0 0 -22 956.11 15.2 0 0 -22 950.32 14.45 0 0 -22 946.29 17.25 0 0 -24 15.74 1.73 0 0 -24 14.4 2.11 0 0 -26 1082.9 19.41 0 0 -26 1125.93 16.74 0 0 -28 229.29 7.31 0 0 -28 205.79 8.19 0 0 -30 162.66 7.33 0 0 -30 175.99 6.44 0 0 -32 225.83 8.67 0 0 -34 9.54 1.77 0 0 -36 227.31 8.91 0 0 -38 337.63 10.88 0 -1 1 1210.4 15.09 0 -1 -1 1529.71 14.75 0 -1 -3 387.41 5.75 0 -1 3 479.56 7.21 0 -1 5 233.42 5.44 0 -1 -5 195.04 4.08 0 -1 7 1875.54 19.43 0 -1 -9 295.9 6.1 0 -1 9 304.43 6.91 0 -1 -11 1316.59 11.31 0 -1 11 1291.59 16.3 0 -1 -13 248.72 7.16 0 -1 -13 237.53 3.97 0 -1 13 255.23 6.7 0 -1 -15 707.43 8.77 0 -1 -15 714.11 13.84 0 -1 -17 66.67 2.67 0 -1 17 54.06 3.23 0 1 -17 55.31 3.03 0 -1 -17 60.99 4.3 0 -1 -19 189.24 8.57 0 -1 -19 176.57 4.63 0 -1 19 149.29 5.62 0 1 -19 150.5 5.23 0 1 -21 670.79 15.4 0 -1 -21 640.8 15.06 0 -1 -21 652.93 9.71 0 1 -21 681.16 12.2 0 1 -23 9.96 1.47 0 -1 -23 6.6 0.78 0 -1 -23 6.62 1.44 0 1 -23 8.73 1.67 0 -1 23 11.03 1.7 0 -1 -25 44.82 3.73 0 -1 25 55.99 3.86 0 1 -25 52.54 3.39 0 1 -25 48.16 4.04 0 1 -27 148.64 7.19 0 -1 27 166.72 6.84 0 1 -27 156.7 6.15 0 -1 -27 140.38 6.78 0 1 -29 83.34 5.45 0 -1 29 92.34 5.21 0 1 -29 89.38 5.22 0 -1 -29 80.24 5.28 0 1 -29 91.2 4.77 0 1 -31 22.92 2.56 0 1 -31 17.92 2.43 0 -1 -31 20.58 2.74 0 1 -33 7.76 1.68 0 1 -33 9.31 1.92 0 -1 -33 7.12 1.5 0 1 -35 11.53 1.93 0 -1 -35 16.38 2.51 0 1 -37 34.35 3.62 0 -1 -37 34.11 3.62 0 1 -39 5.53 1.66 0 -1 -39 6.95 1.72 0 -2 0 1106.7 14.19 0 -2 -2 162.66 4.49 0 -2 2 157.5 4.92 0 -2 -4 1681.34 18.01 0 -2 4 1637.76 20.03 0 -2 -6 1908.88 17.7 0 -2 6 1903.91 23 0 -2 -8 31.78 2.14 0 -2 8 35.28 2.76 0 -2 10 113.95 5.11 0 -2 -10 127.54 4.62 0 -2 -12 416.89 8.98 0 -2 12 441.77 10.59 0 -2 14 13.09 1.74 0 -2 -14 11.37 1.53 0 -2 16 590.86 12.78 0 -2 18 1075.44 17.9 0 -2 20 99.43 5.21 0 -2 22 1668.18 24.21 0 2 -24 165.2 5.69 0 -2 24 175.42 7.29 0 2 -26 1088.38 16.64 0 -2 26 1188.74 20.95 0 2 -28 56.19 4.77 0 -2 28 61.5 4.65 0 2 -28 57.4 3.53 0 2 -30 1.87 0.75 0 -2 30 3.29 1.03 0 2 -32 690.24 13.73 0 2 -32 671.88 17.22 0 2 -34 380.82 12.14 0 2 -34 373.83 12.59 0 2 -36 1.22 0.88 0 2 -36 0.43 0.87 0 2 -38 64.72 5.15 0 -3 -1 35.33 2.7 0 -3 1 35.94 2.79 0 -3 -3 422.36 9.54 0 -3 3 390.84 10 0 -3 -5 810.7 13.44 0 -3 5 687.77 14.14 0 -3 7 1832.47 24.79 0 -3 -7 1834.4 19.68 0 -3 -9 20.48 1.35 0 -3 9 22.47 2.48 0 -3 -11 4.95 0.62 0 -3 11 4.71 1.27 0 -3 -11 5.76 1.13 0 -3 13 20.28 2.53 0 -3 -13 18.88 2.15 0 -3 -13 14.71 0.9 0 -3 15 400.91 11.61 0 -3 -15 397.64 10.36 0 -3 -17 103.24 5.31 0 -3 17 112.86 6.27 0 -3 19 607.74 14.87 0 -3 -19 595.33 14 0 -3 21 196.18 8.4 0 -3 -21 174.83 7.56 0 -3 23 100.77 5.92 0 -3 -23 87.96 5.64 0 -3 25 585.88 14.96 0 -3 -25 534.58 14.92 0 -3 27 7.47 1.81 0 3 -27 7.97 1.25 0 -3 -27 4.54 1.47 0 -3 29 168.25 8.23 0 -3 -29 156.05 9.06 0 -3 31 260.48 10.45 0 -3 -31 240.53 12.37 0 -3 -33 24.26 3.62 0 -3 33 23.95 3.27 0 3 -33 25.98 3.67 0 -3 -35 17.48 3.06 0 3 -35 21.92 3.68 0 -3 35 22.27 3.07 0 3 -37 19.23 2.83 0 3 -37 28.87 4.18 0 -3 -37 21.25 3.23 0 -4 0 922.32 18.46 0 -4 2 899.05 18.08 0 -4 -2 961.46 18.62 0 -4 4 129.07 6.42 0 -4 -4 148.12 6.5 0 -4 6 519.66 12.97 0 -4 -6 529.97 11.07 0 -4 -8 6.24 1.11 0 -4 8 4.86 1.19 0 -4 10 244.78 9.31 0 -4 -10 254.49 8.28 0 -4 -12 181.66 7.23 0 -4 12 179.79 8.03 0 -4 -12 167.42 4.71 0 -4 -14 15.6 2.2 0 -4 14 17.13 2.53 0 -4 -16 688.18 15.33 0 -4 16 667.33 16.59 0 -4 -18 13.44 2.19 0 -4 18 18.41 2.76 0 -4 -20 1052.6 20.71 0 -4 20 1035.04 21.49 0 -4 22 35.28 3.84 0 -4 -22 37.27 3.76 0 -4 24 6.11 1.78 0 -4 -24 3.67 1.38 0 -4 -26 67.34 5.44 0 -4 26 78.26 5.94 0 -4 -28 237.55 11.02 0 -4 28 282.9 11.67 0 -4 30 136.74 8.13 0 -4 -30 118.11 8.19 0 -4 32 39.15 4.66 0 -4 -32 34.54 4.68 0 -4 -34 0.56 1.13 0 -4 34 2.58 1.12 0 -5 -1 555.47 15.43 0 -5 1 484.5 14.32 0 -5 -3 341.57 10.84 0 -5 3 356.09 12.09 0 -5 -5 12.66 2.04 0 -5 5 14.99 2.67 0 -5 -7 125.31 5.58 0 -5 7 133.31 7.42 0 -5 -9 549.55 11.71 0 -5 9 597.83 16.16 0 -5 11 4.79 1.43 0 -5 -11 3.33 0.82 0 -5 -13 389.18 8.89 0 -5 -13 406.97 12.31 0 -5 13 377.93 13 0 -5 15 217.53 9.88 0 -5 -15 215.09 8.92 0 -5 -17 38.4 3.98 0 -5 17 29.77 3.72 0 -5 19 150.47 8.44 0 -5 -19 163.93 8.2 0 -5 21 15.62 2.77 0 -5 -21 22.38 3.17 0 -5 23 51.35 5.02 0 -5 -23 52.06 4.91 0 -5 -25 55.56 5.22 0 -5 25 59.22 5.56 0 -5 27 6.88 2.13 0 -5 -27 7.6 2.1 0 -5 -29 50.19 5.3 0 -5 29 62.42 5.9 0 -5 31 105.86 7.86 0 -5 -31 89.09 7.37 0 -6 0 5.43 2.21 0 -6 -2 545.77 16.19 0 -6 2 541.75 17.08 0 -6 -4 5.96 1.33 0 -6 4 7.22 1.92 0 -6 -6 347.17 11.27 0 -6 6 340.92 12.96 0 -6 -8 47.96 4.03 0 -6 8 41.19 4.52 0 -6 -10 152.61 6.97 0 -6 10 129.36 8.05 0 -6 12 339.59 13.34 0 -6 -12 358.57 10.12 0 -6 14 74.04 6.39 0 -6 16 29.64 3.99 0 -6 -18 1.91 1.26 0 -6 18 0.21 1.16 0 -6 20 61.82 5.94 0 -6 -20 68.73 5.94 0 -6 -22 13.6 2.59 0 -6 22 14.33 2.85 0 -6 -24 0.03 1.27 0 -6 24 3.08 1.7 0 -6 26 28.9 4.21 0 -6 -26 32.02 4.34 0 -6 -28 69.77 6.73 0 -6 28 79.69 7.25 0 -7 1 119.88 8.94 0 -7 -1 118.69 8.45 0 -7 -3 158.87 9.17 0 -7 3 163.36 10.12 0 -7 5 97.58 7.64 0 -7 -5 96.43 6.9 0 -7 -7 4.5 1.69 0 -7 7 3.34 1.1 0 -7 9 290.62 13.06 0 -7 -9 329.18 11.96 0 -7 11 7 2.51 0 -7 13 806.23 22.42 0 -7 15 20.91 3.53 0 -7 17 18.4 3.48 0 -7 19 66.6 6.6 0 -7 21 29.34 4.42 0 -7 23 408.01 16.68 0 -8 0 18 3.97 0 -8 2 45.56 5.85 0 -8 -2 45.65 5.48 0 -8 -4 130.8 8.99 0 -8 4 133.31 10.03 0 -8 -6 40.35 4.94 0 -8 6 38.65 5.45 0 -8 8 104.72 8.67 0 -8 10 0.02 1.45 0 -8 12 0.41 1.47 0 -8 14 124.07 9.36 0 -8 16 3.38 1.86 1 0 -39 -0.57 0.77 1 0 -37 0.63 0.78 1 0 -35 -2.52 1.23 1 0 -33 1.52 0.89 1 0 -31 -1.03 0.88 1 0 -31 0.88 0.8 1 0 -29 -0.28 0.47 1 0 -29 -0.51 0.82 1 0 -27 0.07 0.44 1 0 -27 0.15 0.63 1 0 -25 -0.24 0.63 1 0 -25 -0.78 0.69 1 0 -23 -0.03 0.52 1 0 -23 -1.44 0.82 1 0 -21 0.02 0.42 1 0 -21 0.19 0.42 1 0 -19 1.83 0.76 1 0 -19 1.24 0.51 1 0 -17 1.69 0.53 1 0 -17 0.15 0.31 1 0 -15 -0.07 0.51 1 0 -15 0.28 0.31 1 0 -13 0.38 0.4 1 0 -13 1.13 0.55 1 0 -11 -0.05 0.33 1 0 -11 0.64 0.33 1 0 -9 -0.2 0.45 1 0 -9 0.22 0.19 1 0 -7 2.55 0.67 1 0 -7 3.1 0.58 1 0 -5 1.38 0.53 1 0 -5 1.41 0.34 -1 0 5 1.67 0.28 -1 0 -5 1.72 0.32 1 0 5 1.04 0.27 1 0 7 1.55 0.38 -1 0 -9 3.02 0.69 -1 0 -9 3.62 0.71 1 0 9 2.48 0.45 -1 0 -11 0.81 0.42 1 0 11 1.19 0.38 -1 0 -13 0.55 0.45 1 0 13 -0.11 0.44 -1 0 -13 0.29 0.32 -1 0 -15 1.14 0.54 1 0 15 -0.09 0.31 -1 0 -15 1.46 0.62 -1 0 -17 0.63 0.37 1 0 17 0.45 0.33 -1 0 -17 0.07 0.32 1 0 19 2.84 0.68 -1 0 -19 0.96 0.66 -1 0 -19 1.61 0.69 1 0 21 0.13 0.45 -1 0 -21 0.66 0.46 -1 0 -21 0.56 0.41 -1 0 -23 0.54 0.44 -1 0 -23 0.18 0.52 1 0 23 0.34 0.45 1 0 25 1.32 0.63 -1 0 -25 1.56 0.72 -1 0 -25 0.31 0.44 -1 0 -27 0.39 0.61 -1 0 -27 -1.62 0.95 -1 0 -27 -0.91 0.81 -1 0 -29 0.18 0.53 -1 0 -29 0.25 0.52 -1 0 -31 0.66 0.63 -1 0 -33 -0.98 0.88 -1 0 -35 0.5 0.67 -1 0 -37 -0.48 0.98 -1 0 -39 0.49 0.59 1 -1 -38 160.66 7.96 1 1 -38 147.56 7.3 1 -1 -36 337.41 11.55 1 1 -36 320.41 10.92 1 1 -34 145.03 6.91 1 1 -34 132.89 6.95 1 -1 -34 139.09 7.26 1 -1 -32 206.83 8.65 1 1 -32 198.71 8.48 1 -1 -30 14.6 2.29 1 1 -30 12.38 2.12 1 1 -30 18.35 2.48 1 1 -28 19.65 2.4 1 1 -28 16.59 2.5 1 -1 -28 12.72 2.13 1 -1 -26 383 11.45 1 1 -26 418.58 12.33 1 1 -26 437.96 11.5 1 -1 -26 397.91 8.09 1 1 -26 443.38 9.92 -1 -1 24 32.8 2.89 1 -1 -24 27.72 3.02 1 1 -24 29.04 3.18 1 -1 -24 27.39 1.94 1 1 -24 29.44 2.41 -1 -1 22 719.86 13.77 1 1 -22 703.63 12.01 1 1 -22 716.82 16.11 1 -1 -22 701.28 10.96 1 -1 -20 550.62 15.09 -1 -1 20 498.27 10.87 1 -1 -20 556.06 9.74 1 1 -20 502.52 9.66 1 1 -20 503.84 13.35 1 1 -18 11.27 1.24 1 -1 -18 11.36 1.16 -1 -1 18 10.34 1.41 1 1 -16 915.19 12.51 1 -1 -16 940.42 11.63 1 -1 -16 957.37 17.21 -1 -1 16 932.14 14.51 1 1 -14 2924.52 26.56 1 -1 -14 2935.19 24.72 -1 -1 14 2901.39 29.24 1 -1 -12 837.34 9.35 -1 -1 12 820.38 12.31 1 -1 -10 4482.09 37.19 1 -1 -10 4341.1 31.82 -1 -1 8 188.92 5.12 1 -1 -8 205.52 3.43 -1 -1 6 1710.94 18.15 1 -1 -6 1670.97 13.74 1 -1 -6 1689.09 16.58 -1 1 4 3161.32 23.39 1 -1 -4 3138.77 23.53 1 -1 -4 3080.89 25.37 1 -1 -2 70.31 2 -1 -1 2 68.68 2.58 1 -1 -2 64.46 2.16 1 -1 0 804.39 9.14 -1 -1 0 850.66 9.18 -1 -1 -2 245.36 4 -1 -1 -2 246.7 3.83 1 -1 4 45.25 2.1 -1 -1 -4 44.57 1.7 1 -1 6 52.67 2.51 1 -1 8 3463.43 30.97 -1 -1 -10 200.38 5.11 1 -1 10 211.92 5.85 -1 -1 -12 3310.78 24.29 1 -1 12 3268.02 32.01 -1 -1 -14 21.62 1.08 1 -1 14 21.37 1.94 -1 -1 -14 21.54 2.12 -1 -1 -16 1486.31 21.98 -1 -1 -16 1464.23 14.01 1 -1 16 1480.01 19.38 1 -1 18 1216.29 17.58 -1 -1 -18 1177.23 12.67 -1 1 -20 226.01 6.87 -1 -1 -20 232.13 8.88 1 -1 20 223.47 7.02 -1 -1 -20 213.54 4.67 -1 -1 -22 962.26 18.24 -1 -1 -22 984.58 12.07 -1 1 -22 1063.92 16.54 1 -1 22 1087.09 16.97 -1 1 -22 1063.49 19.66 -1 1 -24 7.53 1.34 1 -1 24 5.52 1.21 -1 1 -24 4.42 1.38 -1 1 -26 349.3 11.05 -1 -1 -26 320.14 10.13 -1 1 -26 363.92 9.74 1 -1 26 390.4 10.51 -1 1 -28 146.76 7.1 -1 1 -28 159.06 6.42 -1 -1 -28 146.1 6.98 1 -1 30 553 12.98 -1 1 -30 493.11 13.48 -1 1 -30 542.31 12.49 -1 -1 -30 470.45 12.99 -1 -1 -32 96.96 5.79 1 -1 32 104.75 5.59 -1 1 -32 93.86 5.3 -1 1 -32 89.59 5.52 -1 1 -32 100.29 5.29 -1 -1 -34 217.73 8.78 -1 1 -34 214.03 8.7 -1 -1 -36 49.23 4.26 -1 1 -36 43.52 3.94 -1 1 -38 231.17 9.23 -1 -1 -38 230.35 9.28 1 2 -37 80.03 5.67 1 2 -35 41.62 3.99 1 2 -35 38.6 3.98 1 2 -33 2.13 0.66 1 2 -33 2.95 1.16 1 2 -31 53.44 4.66 1 2 -31 59.19 4.93 1 2 -29 57.4 3.54 1 2 -29 48.67 4.45 -1 -2 29 55.77 4.5 1 2 -27 34.07 3.68 -1 -2 27 40.83 3.77 1 2 -27 35.99 2.71 -1 -2 25 86.22 5.27 1 2 -25 79.23 3.78 1 2 -23 86.25 3.87 -1 -2 23 94.65 5.45 1 2 -21 956.54 13.86 -1 -2 21 1023.12 18.18 -1 -2 19 86.17 4.74 1 -2 -17 405.92 5.36 -1 -2 17 372.28 9.71 1 -2 -15 254.32 7.58 1 -2 -15 267.58 4.12 -1 -2 13 0.86 0.41 1 -2 -13 1.83 0.28 1 -2 -13 1.3 0.28 1 -2 -11 4.87 0.99 1 -2 -11 4.74 0.57 -1 -2 11 4.36 0.96 -1 -2 9 27.48 2.33 1 -2 -9 31.14 2.23 1 -2 -9 30.35 1.46 1 -2 -7 656.45 10.35 1 -2 -7 647.02 8.21 1 -2 -5 199.02 5.35 1 -2 -5 186.59 4.32 -1 -2 5 205.07 6.31 1 -2 -3 47.6 2.4 1 -2 -3 48.53 2.3 1 -2 -1 81.52 3.18 -1 -2 1 113.16 4.7 -1 -2 -1 161.25 5.07 1 -2 1 139.01 4.46 1 -2 3 1122.3 15.13 -1 -2 -3 1082.36 12.78 -1 -2 -3 1108.57 13.23 -1 -2 -5 415.85 7.52 1 -2 5 409.19 8.78 -1 -2 -7 7.14 0.65 -1 -2 -7 6.18 0.91 1 -2 9 85.07 4.2 -1 -2 -9 90.08 3.65 -1 -2 -11 6.74 1.08 1 -2 11 7.48 1.29 -1 -2 -13 1.56 0.51 1 -2 13 1.46 0.58 1 -2 15 2367.37 28.85 1 -2 17 50.05 3.7 1 -2 19 63.91 4.19 1 -2 21 195.58 7.66 1 -2 23 6.8 1.5 1 -2 25 238.55 8.58 -1 2 -25 222.74 7.1 1 -2 27 22.56 2.66 -1 2 -27 22.53 2.21 -1 2 -29 18.67 2.84 -1 2 -29 16.91 2.02 1 -2 29 22.93 2.84 -1 2 -31 32.65 2.85 -1 2 -31 32.48 3.72 1 -2 31 37.37 3.69 -1 2 -33 17.55 2.12 1 -2 33 19.09 2.68 -1 2 -33 16.85 2.75 -1 2 -35 5 1.45 1 -2 35 4.94 1.5 -1 2 -37 74.62 5.64 1 -3 -36 2.94 1.45 1 3 -36 1.74 0.89 1 3 -34 15.35 2.62 1 -3 -34 12.18 2.5 -1 -3 34 14.45 2.66 1 3 -34 18.02 3.19 -1 -3 32 891.34 19.9 1 -3 -32 854.24 23.25 1 3 -32 841.88 21.46 1 -3 -30 217.01 10.92 -1 -3 30 240.16 9.89 -1 -3 28 32.26 3.6 1 -3 -28 27.13 3.73 1 3 -26 200.47 6.03 1 -3 -26 215.85 9.62 1 -3 -24 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16 1 5 9.13 1.78 16 -1 5 8.46 1.96 16 -1 7 -0.29 1.04 16 1 7 1.94 1.08 16 -1 9 179.22 8.5 16 1 9 185.04 8.2 16 -1 11 5.88 1.59 16 1 11 9.19 1.98 16 -1 13 8.51 1.98 16 1 13 6.22 1.7 -16 -1 -13 4.92 1.85 16 -1 15 1.92 1.02 16 1 15 1.89 0.91 -16 -1 -15 2.93 1.74 16 -1 17 25.34 3.44 16 1 17 17.98 2.63 -16 -1 -17 26.83 3.92 16 -1 19 4.23 1.33 16 1 19 6.7 1.72 -16 -1 -19 7 2.09 16 -1 21 2.83 1.5 -16 -1 -21 4.53 2.07 16 -1 23 42.22 4.4 -16 -1 -23 46.5 5.59 16 2 -22 146.62 8.8 16 -2 -22 124.01 7.56 16 2 -22 147.24 8.25 16 2 -20 142.32 8.46 16 -2 -20 125.97 7.44 16 2 -20 152.89 7.92 16 -2 -18 2.17 1.02 16 2 -18 4.38 1.32 16 2 -18 2.74 0.72 16 2 -16 157.02 8.49 16 -2 -16 136.3 7.68 16 2 -16 149.73 7 16 2 -14 68.04 5.48 16 -2 -14 61.25 5.01 16 2 -12 78.78 5.98 16 -2 -12 65.26 5.22 16 2 -10 104.03 6.8 16 -2 -10 96.33 6.36 16 2 -8 14.19 2.6 16 -2 -8 14.74 2.53 16 2 -6 212.71 9.74 16 -2 -6 185.16 8.75 16 -2 -4 60.75 5.08 -16 -2 4 61.57 5.1 16 2 -4 77.15 5.82 16 2 -2 6.98 1.55 16 -2 -2 5.75 1.43 -16 -2 2 5.87 1.59 16 -2 0 99.84 6.54 16 2 0 100.66 6.2 -16 -2 0 93.72 6.97 16 2 2 3.54 1.44 16 -2 2 3.36 1.4 -16 -2 -2 1.53 0.78 16 -2 4 310.95 11.46 16 2 4 306.26 10.34 16 -2 6 499.41 14.87 16 2 6 523.3 13.89 16 2 8 0.84 0.59 16 -2 8 2.47 1.03 -16 -2 -8 0.24 1.2 16 -2 10 4.24 1.27 -16 -2 -10 5.48 1.86 16 2 10 6.86 1.57 16 -2 12 67.47 5.71 16 2 12 71.55 5.12 -16 -2 -12 64.86 6.14 16 -2 14 39.53 4.58 16 2 14 37.88 3.73 -16 -2 -14 30.98 4.28 16 -2 16 357.39 13.6 16 2 16 342.29 11.04 -16 -2 -16 322.62 13.78 16 -2 18 130.98 8.19 -16 -2 -18 131.73 9.15 16 -2 20 10.32 2.38 -16 -2 -20 7.65 2.08 16 3 -19 23.9 3.64 16 -3 -19 18.89 2.97 16 3 -19 27.88 3.51 16 3 -17 27.34 3.76 16 -3 -17 19.63 2.88 16 3 -17 26.37 3.26 16 3 -15 13.67 2.14 16 -3 -15 10.05 2.06 16 3 -15 13.75 2.82 16 3 -13 96.15 6.91 16 -3 -13 81.04 6.03 16 3 -13 94.86 5.67 16 3 -11 66.26 5.83 16 -3 -11 55.25 4.87 16 3 -9 40.4 4.52 16 -3 -9 33.31 3.84 16 3 -7 53.12 5.02 16 -3 -7 44.49 4.44 16 3 -5 171.33 8.98 16 -3 -5 147.94 8.1 16 3 -3 4.46 1.4 16 -3 -3 2.59 0.93 16 3 -1 62.9 5.15 16 -3 -1 56.23 5.19 -16 -3 1 65.51 5.61 16 3 1 20.41 2.98 16 -3 1 19.71 3.07 -16 -3 -1 28.03 4.1 16 3 3 24.57 3.03 16 -3 3 26.3 3.59 -16 -3 -3 33.96 4.8 16 3 5 1.82 0.96 16 -3 5 -0.79 1.13 -16 -3 -5 1.04 1.47 16 3 7 12.09 2.18 16 -3 7 7.1 1.71 -16 -3 -7 11.74 3.44 16 3 9 6.29 1.45 16 -3 9 6.5 2.05 -16 -3 -9 5.1 2.38 16 3 11 7.58 1.56 16 -3 11 10.08 2.34 -16 -3 -11 11.04 2.94 16 -3 13 33.85 4.45 16 3 13 32.75 3.46 -16 -3 -13 32.8 4.76 16 -3 15 3.94 1.75 -16 -3 -15 7.04 2.3 16 -3 17 3.03 1.57 -16 -3 -17 6.57 2.49 16 -3 19 68.01 6.38 -16 -3 -19 66.14 6.73 16 -4 -16 36.42 4.41 16 4 -16 40.79 4.8 16 -4 -14 47.13 4.83 16 4 -14 55.87 5.65 16 4 -12 13.12 2.86 16 -4 -12 11.82 2.71 16 4 -10 60.78 5.73 16 -4 -10 49.59 5.01 16 4 -8 25.36 3.64 16 -4 -8 25 3.74 16 4 -6 71.67 6.08 16 -4 -6 61.96 5.57 16 4 -4 117.23 7.72 16 -4 -4 104.48 7.38 16 -4 -2 14.56 2.82 16 4 -2 16.74 2.82 16 4 0 297.2 11.47 16 -4 0 273.92 12.16 16 4 2 38.88 3.99 16 -4 2 44.59 5.05 16 -4 4 21.02 3.48 16 4 4 17.87 2.69 16 -4 6 94.19 7.44 16 4 6 87.89 5.71 16 -4 8 27.26 4.1 16 4 8 30.44 3.38 16 -4 10 251.81 12.33 16 4 10 244.82 9.3 16 -4 12 185.53 10.88 16 -4 14 8.29 2.34 16 5 -9 10.95 2.61 16 -5 -9 8.54 2.12 16 -5 -7 95.39 7.83 16 5 -7 99.44 7.5 16 5 -5 18.15 3.2 16 -5 -5 17.39 3.18 16 -5 -3 129.05 9.39 16 5 -3 129.68 8.35 16 -5 -1 156.14 10.3 16 5 -1 154.99 8.78 16 5 1 31.75 3.96 16 -5 1 30.56 4.64 16 5 3 73.36 5.66 16 -5 3 78.2 7.27 16 5 5 88.27 6 16 -5 5 89.93 7.82 16 -5 7 50.45 5.78 16 5 7 43.5 4.26 16 -5 9 91.6 7.89 17 0 -21 1.72 0.97 17 0 -19 3.79 1.6 17 0 -17 1.03 0.82 17 0 -15 -0.92 1.06 17 0 -13 1.01 1 17 0 -11 0.08 0.85 17 0 -9 -0.18 0.89 17 0 -7 0.01 0.91 17 0 -5 -1.13 1.28 17 0 -3 0.31 0.83 17 0 -1 0.11 0.84 17 0 1 -1.1 1.04 17 0 3 -1.54 1.32 17 0 5 0.48 0.7 17 0 7 -0.13 0.74 17 0 9 2.11 1.1 17 0 11 -3.24 1.79 17 0 13 -0.36 1.14 17 0 15 1.46 0.97 17 0 17 -0.98 1.09 17 0 19 -0.97 1.14 17 -1 -20 176.36 9.1 17 1 -20 184.73 9.58 17 -1 -18 41.67 4.31 17 1 -18 44.23 4.69 17 -1 -16 97.89 6.71 17 1 -16 102.59 6.98 17 -1 -14 7.74 1.99 17 1 -14 6.89 1.67 17 -1 -12 19.74 2.99 17 1 -12 17.95 2.89 17 -1 -10 187.78 9.2 17 1 -10 186.22 9.15 17 -1 -8 67.43 5.48 17 1 -8 68.07 5.49 17 -1 -6 77.52 5.84 17 1 -6 78.17 5.83 17 -1 -4 74.76 5.66 17 1 -4 79.94 5.78 17 1 -2 2.81 1.04 17 -1 -2 4.17 1.48 17 -1 0 230.18 9.94 17 1 0 238.25 9.89 17 -1 2 345.48 12.13 17 1 2 352.97 11.91 17 1 4 18.04 2.7 17 -1 4 17.12 2.64 17 -1 6 247.6 10.19 17 1 6 258.64 9.9 17 -1 8 4.3 1.64 17 1 8 3.39 1.2 17 -1 10 2.93 1.36 17 1 10 2.28 1.27 -17 -1 -10 2.08 1.24 17 -1 12 316.39 12.06 17 1 12 332.09 11.72 -17 -1 -12 316.4 14.1 17 -1 14 16.12 2.94 17 1 14 18.42 2.89 -17 -1 -14 18.46 3.52 17 -1 16 125.17 7.83 17 1 16 124.37 7.14 -17 -1 -16 126.05 9.33 17 -1 18 57.01 5.32 17 1 18 50.44 4.49 -17 -1 -18 60.8 6.75 17 -1 20 18.17 3.15 -17 -1 -20 14.67 3.33 17 -2 -19 2.63 0.98 17 2 -19 3.14 1.5 17 2 -17 5.28 1.68 17 -2 -17 5.04 1.39 17 2 -15 8.34 2 17 -2 -15 5.59 1.59 17 2 -13 118.55 7.58 17 -2 -13 105.26 6.75 17 2 -11 12.39 2.41 17 -2 -11 11.16 2.26 17 2 -9 1.25 1.18 17 -2 -9 -0.86 1.41 17 2 -7 10.98 2.3 17 -2 -7 10.23 2.29 17 2 -5 28 3.66 17 -2 -5 25.19 3.36 17 -2 -3 82.46 6.07 -17 -2 3 76.17 5.67 17 2 -3 88.21 6.22 17 -2 -1 142.52 8.07 17 2 -1 143.95 7.74 -17 -2 1 124.89 7.65 17 2 1 15.4 2.46 17 -2 1 15.66 2.54 -17 -2 -1 14.25 2.64 17 -2 3 1.29 0.77 -17 -2 -3 2.99 1.25 17 -2 5 153.27 8.3 17 2 5 157.89 7.72 -17 -2 -5 132.33 8.07 17 2 7 -0.25 0.63 17 -2 7 -0.43 0.98 -17 -2 -7 -1.23 1.25 17 -2 9 42.25 4.44 17 2 9 46.14 4.17 -17 -2 -9 42.21 4.85 17 -2 11 25.73 3.5 17 2 11 27.8 3.3 -17 -2 -11 21.4 3.48 17 -2 13 84.24 6.61 17 2 13 84.03 5.7 -17 -2 -13 79.7 6.98 17 -2 15 5.85 1.87 17 2 15 7.53 1.7 -17 -2 -15 7.22 2.06 17 -2 17 89.64 6.94 -17 -2 -17 91.18 7.79 17 -3 -16 4.51 1.48 17 3 -16 6.92 1.85 17 -3 -14 5.34 1.61 17 3 -14 4.38 1.63 17 3 -12 212.35 10.42 17 -3 -12 183.44 9.19 17 3 -10 167.89 9.22 17 -3 -10 146.78 8.29 17 3 -8 24.94 3.57 17 -3 -8 20.78 3.27 17 3 -6 44.87 4.73 17 -3 -6 38.29 4.09 17 3 -4 116.62 7.48 17 -3 -4 102.37 6.95 17 3 -2 2.36 1.33 17 -3 -2 2.87 1.14 17 -3 0 115.29 7.4 -17 -3 0 140.35 8.77 17 3 0 126.32 7.33 17 -3 2 45.96 4.83 -17 -3 -2 62.35 6.41 17 3 2 50.68 4.56 17 3 4 0.7 0.69 17 -3 4 4.25 1.54 -17 -3 -4 3.22 1.74 17 -3 6 65.1 5.77 17 3 6 59.28 4.72 -17 -3 -6 76.4 7.88 17 -3 8 107.05 7.43 17 3 8 113.66 6.6 -17 -3 -8 112.18 9.59 17 3 10 2.15 0.97 17 -3 10 2.73 1.07 -17 -3 -10 2.26 1.06 17 -3 12 9.78 2.25 -17 -3 -12 10.41 2.9 17 3 12 13.99 2.39 17 -3 14 4.73 1.85 -17 -3 -14 2.06 1.58 17 -3 16 51.42 5.58 -17 -3 -16 52.17 5.81 17 -4 -11 0.52 1.14 17 4 -11 0.44 0.91 17 -4 -9 15.71 2.84 17 4 -9 21.12 3.47 17 4 -7 110.76 7.76 17 -4 -7 95.54 6.98 17 4 -5 182.26 9.71 17 -4 -5 146.66 8.81 17 -4 -3 6.9 1.94 17 4 -3 6.67 1.9 17 -4 -1 16.91 3.18 17 4 -1 15.28 2.73 17 -4 1 11.71 2.35 17 4 1 12.21 2.27 17 -4 3 7.14 2.09 17 4 3 5.27 1.6 17 -4 5 104.33 7.83 17 4 5 95.13 6.18 17 4 7 6.4 1.5 17 -4 7 8.18 2.14 17 4 9 8.8 1.98 17 -4 9 8.72 2.27 17 -4 11 21.02 3.69 18 0 -18 2.46 1.19 18 0 -16 18.5 2.88 18 0 -14 76.95 5.79 18 0 -12 174.3 8.91 18 0 -10 60.35 5.28 18 0 -8 133.85 8 18 0 -6 10.69 2.6 18 0 -4 111.17 7.14 18 0 -2 8.28 1.97 18 0 0 109.58 6.9 18 0 2 365.31 12.4 18 0 4 5.51 1.8 18 0 6 24.25 3.24 18 0 8 -0.23 0.98 18 0 10 18.16 2.73 18 0 12 180.05 9 18 0 14 187.21 9.34 18 0 16 10.96 2.33 18 -1 -17 9.19 2.12 18 1 -17 6.92 1.79 18 -1 -15 0.95 1 18 1 -15 -0.04 1.01 18 -1 -13 31.08 3.79 18 1 -13 36.63 4.2 18 -1 -11 101.28 6.81 18 1 -11 104.01 7.02 18 -1 -9 99.97 6.79 18 1 -9 95.19 6.59 18 -1 -7 50.31 4.8 18 1 -7 47.94 4.75 18 1 -5 14.04 2.49 18 -1 -5 14.33 2.6 18 -1 -3 84.28 6.16 18 1 -3 90.02 6.31 18 1 -1 24.46 3.17 18 -1 -1 28.83 3.74 18 1 1 2.94 1.33 18 -1 1 5.23 1.75 18 -1 3 59.02 5.19 18 1 3 54.49 4.68 18 -1 5 8.65 1.94 18 1 5 10.79 2.16 18 -1 7 4.45 1.36 18 1 7 3.81 1.18 18 -1 9 22.36 3.35 18 1 9 21.92 3.1 -18 -1 -9 22.54 3.68 18 -1 11 11.71 2.41 18 1 11 16.05 2.78 -18 -1 -11 11.42 2.59 18 -1 13 1.99 1.27 18 1 13 0.98 0.85 -18 -1 -13 -1.16 2.12 18 -1 15 -1.63 1.35 18 1 15 0.11 0.79 -18 -1 -15 1.58 1.46 18 2 -16 81.52 6.47 18 -2 -16 63.88 5.43 18 2 -14 87.84 6.63 18 -2 -14 79.43 6.07 18 2 -12 2 1.45 18 -2 -12 2.11 1.22 18 -2 -10 68.57 5.76 18 2 -10 71.07 6.05 18 -2 -8 118.37 7.47 18 2 -8 129.56 8.06 18 2 -6 27.23 3.65 18 -2 -6 23.12 3.28 18 -2 -4 155.89 8.57 18 2 -4 160.08 8.64 18 -2 -2 186.62 9.57 18 2 -2 199.44 9.33 18 2 0 14.63 2.4 18 -2 0 14.37 2.59 -18 -2 0 9.44 2.01 18 -2 2 32.67 4.09 18 2 2 34.54 3.82 -18 -2 -2 25.69 3.7 18 -2 4 101.14 6.86 18 2 4 97.31 6.24 -18 -2 -4 86.34 6.7 18 -2 6 74.72 6.02 18 2 6 75.36 5.49 -18 -2 -6 63.28 5.84 18 -2 8 59.61 5.46 18 2 8 65.7 5.15 -18 -2 -8 54.41 5.45 18 -2 10 18.47 3.38 -18 -2 -10 12.62 2.83 18 2 10 16.79 2.69 18 -2 12 41.03 4.65 18 2 12 47.51 4.48 -18 -2 -12 42.7 5.08 18 -2 14 7.24 2.12 18 2 14 4.2 1.47 -18 -2 -14 9.02 2.76 18 3 -11 3.96 1.89 18 -3 -11 5.2 1.68 18 3 -9 11.77 2.57 18 -3 -9 10.22 2.32 18 3 -7 18.6 3.1 18 -3 -7 19.32 3.28 18 -3 -5 148.31 8.57 18 3 -5 164.25 9.22 18 3 -3 7.79 2.12 18 -3 -3 6.07 1.7 18 -3 -1 52.31 5.15 18 3 -1 53.07 4.93 18 3 1 5.49 1.86 18 -3 1 4.95 1.86 18 -3 3 31.97 4.11 18 3 3 33.83 3.81 -18 -3 -3 32.12 4.45 18 3 5 6.41 1.72 18 -3 5 4.89 1.7 -18 -3 -5 1.37 1.64 18 -3 7 31.97 4.13 18 3 7 30.11 3.46 -18 -3 -7 28.74 4.67 18 3 9 2.85 1.27 18 -3 9 2.06 1.23 -18 -3 -9 0.35 1.6 18 -3 11 0.26 1.11 -18 -3 -11 -0.16 1.3 18 3 11 0.73 0.86 18 -4 -2 1.31 1.24 18 4 -2 3.26 1.32 18 -4 0 52.7 5.52 18 4 0 59.05 5.4 18 4 2 2.73 1.07 18 -4 2 2.99 1.61 19 0 -13 -1.75 1.23 19 0 -11 -1.33 1.61 19 0 -9 2.43 1.33 19 0 -7 -0.12 0.73 19 0 -5 -0.22 1.33 19 0 -3 -0.09 0.74 19 0 -1 1.51 1.32 19 0 1 -1.15 0.99 19 0 3 -0.45 0.97 19 0 5 -1.32 1.06 19 0 7 0.43 0.74 19 0 9 0.76 0.82 19 0 11 -0.1 1.09 19 0 13 -1.52 1.41 19 -1 -12 4.3 1.63 19 1 -12 7.08 1.97 19 -1 -10 77.37 6.12 19 1 -10 80.08 6.19 19 -1 -8 47.4 4.85 19 1 -8 44.81 4.7 19 1 -6 3.74 1.57 19 -1 -6 3.74 1.7 19 1 -4 30.64 3.84 19 -1 -4 28.81 3.59 19 1 -2 28.59 3.75 19 -1 -2 24.29 3.42 19 1 0 2.85 1.51 19 -1 0 5.16 1.46 19 -1 2 283.18 11.57 19 1 2 264.01 10.82 19 -1 4 21.99 3.29 19 1 4 25.34 3.25 19 -1 6 24.41 3.42 19 1 6 24.01 3.2 -19 -1 -6 21.35 3.43 19 -1 8 82.58 6.28 19 1 8 79.74 5.85 -19 -1 -8 84.57 6.97 19 -1 10 86.72 6.58 19 1 10 82.87 6.03 -19 -1 -10 83.77 7.52 19 -1 12 145 8.6 19 1 12 150.93 8.25 -19 -1 -12 159.95 10.96 19 2 -9 1.85 1.07 19 -2 -9 -0.6 1.38 19 2 -7 1.51 1.02 19 -2 -7 2.09 0.97 19 2 -5 9.66 1.98 19 -2 -5 10.15 2.3 19 2 -3 18.48 3 19 -2 -3 19.48 3.23 19 2 -1 3.29 1.06 19 -2 -1 3.67 1.43 19 2 1 7.7 2.09 19 -2 1 9.7 2.11 19 2 3 11.86 2.35 19 -2 3 7.32 2.1 -19 -2 -3 5.86 1.86 19 -2 5 58.47 5.4 19 2 5 55.95 4.84 -19 -2 -5 44.54 4.94 19 2 7 36.02 3.8 19 -2 7 32.75 4.12 -19 -2 -7 24.53 3.7 19 -2 9 20.14 3.36 -19 -2 -9 19.39 3.42 19 2 9 20.18 2.97 19 -3 -2 97.37 7.42 19 3 -2 103.06 7.12 19 3 0 2.88 1.23 19 -3 0 5.51 1.7 19 3 2 26.56 3.38 19 -3 2 26.87 3.88 20 0 -6 128.81 8 20 0 -4 31.26 3.96 20 0 -2 14.89 2.75 20 0 0 4.17 1.09 20 0 2 122.85 7.76 20 0 4 68.41 5.72 20 1 -3 1.6 1.36 20 -1 -3 2.46 1.64 20 1 -1 -0.8 1.02 20 -1 -1 -1.54 1.46 20 1 1 1.78 1.31 20 -1 1 0 1.04 20 -1 3 27.87 3.78 -20 -1 -3 16.53 2.72 20 1 3 26.36 3.42 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 2 0 1 0.1514 -2 0 -1 0.1277 0 -2 1 0.2824 0 2 -1 0.2370 0 0 1 0.0781 0 0 -1 0.0716 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 C3 As1 C2 89.39(10) . . ? C3 As1 C1 89.91(10) . . ? C2 As1 C1 89.26(10) . . ? C3 S2 C18 91.17(11) . . ? C2 S1 C11 91.57(13) . . ? C21 C22 C17 119.7(2) . . ? C22 C17 C16 130.5(2) . . ? C22 C17 C18 118.5(2) . . ? C18 C17 C16 111.0(2) . . ? C17 C16 C23 128.0(2) . . ? C3 C16 C17 113.4(2) . . ? C3 C16 C23 118.6(2) . . ? C10 C9 C23 128.0(2) . . ? C2 C9 C23 118.5(2) . . ? C2 C9 C10 113.4(2) . . ? S2 C3 As1 128.35(14) . . ? C16 C3 As1 118.67(17) . . ? C16 C3 S2 112.98(18) . . ? C16 C23 C8 108.23(18) . . ? C9 C23 C16 108.23(19) . . ? C9 C23 C8 107.52(18) . . ? C17 C18 S2 111.43(17) . . ? C19 C18 S2 126.54(19) . . ? C19 C18 C17 122.0(2) . . ? C22 C21 C20 120.8(2) . . ? C20 C19 C18 118.0(2) . . ? C19 C20 C21 121.0(2) . . ? C15 C10 C9 130.0(2) . . ? C15 C10 C11 119.0(2) . . ? C11 C10 C9 111.0(2) . . ? C1 C8 C23 117.2(2) . . ? C7 C8 C23 122.6(2) . . ? C7 C8 C1 120.3(2) . . ? C14 C15 C10 119.5(3) . . ? S1 C2 As1 128.88(15) . . ? C9 C2 As1 118.49(18) . . ? C9 C2 S1 112.62(18) . . ? C8 C1 As1 118.06(18) . . ? C8 C1 C4 120.6(3) . . ? C4 C1 As1 121.3(2) . . ? C8 C7 C6 119.8(3) . . ? C5 C4 C1 117.9(3) . . ? C10 C11 S1 111.32(18) . . ? C12 C11 S1 127.3(2) . . ? C12 C11 C10 121.4(3) . . ? C15 C14 C13 120.7(3) . . ? C13 C12 C11 118.2(3) . . ? C12 C13 C14 121.2(2) . . ? C5 C6 C7 119.9(3) . . ? C6 C5 C4 121.5(2) . . ? 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 C3 1.956(2) . ? As1 C2 1.962(2) . ? As1 C1 1.975(3) . ? S2 C3 1.730(2) . ? S2 C18 1.746(3) . ? S1 C2 1.729(3) . ? S1 C11 1.743(3) . ? C22 C17 1.408(3) . ? C22 C21 1.383(3) . ? C17 C16 1.434(3) . ? C17 C18 1.415(3) . ? C16 C3 1.358(3) . ? C16 C23 1.522(3) . ? C9 C23 1.521(3) . ? C9 C10 1.438(3) . ? C9 C2 1.362(4) . ? C23 C8 1.534(3) . ? C18 C19 1.399(3) . ? C21 C20 1.408(3) . ? C19 C20 1.385(4) . ? C10 C15 1.399(4) . ? C10 C11 1.414(4) . ? C8 C1 1.397(4) . ? C8 C7 1.387(4) . ? C15 C14 1.383(3) . ? C1 C4 1.407(3) . ? C7 C6 1.401(4) . ? C4 C5 1.406(5) . ? C11 C12 1.399(4) . ? C14 C13 1.402(4) . ? C12 C13 1.377(4) . ? C6 C5 1.379(5) . ? 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 1.9989 0.0001 1.0016 0.0830 0.0210 -0.0299 -1.9989 -0.0001 -1.0016 -0.0830 -0.0210 0.0299 -0.0015 -1.9997 0.9981 0.0670 0.0246 0.1870 0.0015 1.9997 -0.9981 -0.0670 -0.0246 -0.1870 -0.0005 0.0001 1.0001 0.0006 0.0225 -0.0005 0.0005 -0.0001 -1.0001 -0.0006 -0.0225 0.0005