#------------------------------------------------------------------------------ #$Date: 2021-07-25 01:20:33 +0300 (Sun, 25 Jul 2021) $ #$Revision: 267735 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/89/4518919.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_4518919 loop_ _publ_author_name 'Doma\'nski, Mateusz A.' 'Kraszewski, Karol' 'Paluch, Piotr' 'Gu\'nka, Piotr A.' _publ_section_title ; Arsenic(III)-oxide Intercalates with Potassium Chloride: Water-Induced Varieties and New Synthesis Methods ; _journal_name_full 'Crystal Growth & Design' _journal_paper_doi 10.1021/acs.cgd.1c00555 _journal_year 2021 _chemical_formula_moiety 'As4 O6, 2(K), 2(Cl), 1(O)' _chemical_formula_sum 'As4 Cl2 K2 O7' _chemical_formula_weight 560.78 _space_group_crystal_system hexagonal _space_group_IT_number 191 _space_group_name_Hall '-P 6 2' _space_group_name_H-M_alt 'P 6/m m m' _atom_sites_solution_primary iterative _audit_creation_date 2021-01-27 _audit_creation_method ; Olex2 1.3-dev (compiled 2020.12.01 svn.r5f60950 for OlexSys, GUI svn.r6226) ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 1 _cell_length_a 5.24015(14) _cell_length_b 5.24015(14) _cell_length_c 12.2944(4) _cell_measurement_reflns_used 3325 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 32.3190 _cell_measurement_theta_min 4.4690 _cell_volume 292.365(15) _computing_cell_refinement 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_molecular_graphics 'Olex2 1.3-dev (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3-dev (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'olex2.solve 1.3-dev (Bourhis et al., 2015)' _diffrn_ambient_temperature 293(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 10.3347 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.985 _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 -45.00 35.00 1.00 4.50 -- -19.50 38.00 -60.00 80 2 \w -13.00 25.00 1.00 4.50 -- 19.81 77.00 150.00 38 3 \w -95.00 7.00 1.00 4.50 -- -19.50 -38.00 120.00 102 4 \w -98.00 -40.00 1.00 4.50 -- -19.50 -77.00 -60.00 58 5 \w -108.00 -32.00 1.00 4.50 -- -19.50 179.00 30.00 76 6 \w -95.00 7.00 1.00 4.50 -- -19.50 -38.00 -30.00 102 7 \w -93.00 10.00 1.00 4.50 -- -19.50 -57.00-120.00 103 8 \w 45.00 87.00 1.00 4.50 -- 19.97-166.00 -45.00 42 9 \w -4.00 62.00 1.00 4.50 -- 19.97 -99.00 30.00 66 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.1541029000 _diffrn_orient_matrix_UB_12 -0.0659466000 _diffrn_orient_matrix_UB_13 0.0083702000 _diffrn_orient_matrix_UB_21 0.0114746000 _diffrn_orient_matrix_UB_22 0.1404462000 _diffrn_orient_matrix_UB_23 -0.0037406000 _diffrn_orient_matrix_UB_31 -0.0233666000 _diffrn_orient_matrix_UB_32 -0.0188574000 _diffrn_orient_matrix_UB_33 -0.0569657000 _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 0.0445 _diffrn_reflns_av_unetI/netI 0.0148 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.985 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 6016 _diffrn_reflns_point_group_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.985 _diffrn_reflns_theta_full 26.000 _diffrn_reflns_theta_max 32.709 _diffrn_reflns_theta_min 3.314 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 12.506 _exptl_absorpt_correction_T_max 0.586 _exptl_absorpt_correction_T_min 0.157 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015) 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 3.185 _exptl_crystal_description plate _exptl_crystal_F_000 260 _exptl_crystal_size_max 0.218 _exptl_crystal_size_mid 0.181 _exptl_crystal_size_min 0.039 _refine_diff_density_max 0.499 _refine_diff_density_min -0.777 _refine_diff_density_rms 0.099 _refine_ls_extinction_coef 0.119(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.130 _refine_ls_hydrogen_treatment undef _refine_ls_matrix_type full _refine_ls_number_parameters 17 _refine_ls_number_reflns 267 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.130 _refine_ls_R_factor_all 0.0166 _refine_ls_R_factor_gt 0.0153 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0170P)^2^+0.1336P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0335 _refine_ls_wR_factor_ref 0.0339 _reflns_Friedel_coverage 0.000 _reflns_number_gt 260 _reflns_number_total 267 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file cg1c00555_si_002.cif _cod_data_source_block pg48intercalateY_KCl _cod_original_cell_volume 292.365(18) _cod_database_code 4518919 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'K1 As2 O3 Cl1' _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 0.641 _shelx_estimated_absorpt_t_min 0.171 _reflns_odcompleteness_completeness 99.57 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 30.44 _olex2_refinement_description ; 1. Uiso/Uaniso restraints and constraints Uanis(K2) = Uanis(O2) 2. Others Fixed Sof: K2(0.04167) O2(0.04167) ; _shelx_res_file ; TITL pg48.res created by SHELXL-2018/3 at 14:45:46 on 27-Jan-2021 CELL 0.71073 5.240153 5.240153 12.294398 90 90 120 ZERR 1 0.00014 0.00014 0.000399 0 0 0 LATT 1 SYMM -Y+X,+X,+Z SYMM -Y,+X-Y,+Z SYMM -X,-Y,+Z SYMM +Y-X,-X,+Z SYMM +Y,-X+Y,+Z SYMM -Y+X,-Y,-Z SYMM -X,-X+Y,-Z SYMM +Y,+X,-Z SYMM -Y,-X,-Z SYMM +Y-X,+Y,-Z SYMM +X,+X-Y,-Z SFAC As Cl K O UNIT 4 2 2 7 EADP K2 O2 L.S. 10 PLAN 2 SIZE 0.039 0.181 0.218 CONF CONN 3 $As CONN 0 $K LIST 4 more -3 fmap 2 acta 52 BOND $H REM REM REM WGHT 0.017000 0.133600 EXTI 0.119043 FVAR 9.69909 AS1 1 0.333333 0.666667 0.210262 10.16667 0.00876 0.00876 = 0.01562 0.00000 0.00000 0.00438 K1 3 0.000000 0.000000 0.000000 10.04167 0.02684 0.02684 = 0.02851 0.00000 0.00000 0.01342 CL1 2 0.000000 0.000000 0.324243 10.08333 0.02692 0.02692 = 0.03695 0.00000 0.00000 0.01346 O1 4 0.500000 0.500000 0.132256 10.25000 0.01483 0.01483 = 0.01988 0.00000 0.00000 0.01147 PART 1 K2 3 0.500000 0.000000 0.500000 10.04167 0.08547 0.06012 = 0.03327 0.00000 0.00000 0.03006 PART 2 O2 4 0.500000 0.000000 0.500000 10.04167 0.08547 0.06012 = 0.03327 0.00000 0.00000 0.03006 HKLF 4 REM REM wR2 = 0.0339, GooF = S = 1.130, Restrained GooF = 1.130 for all data REM R1 = 0.0153 for 260 Fo > 4sig(Fo) and 0.0166 for all 267 data REM 17 parameters refined using 0 restraints END WGHT 0.0170 0.1335 REM Highest difference peak 0.499, deepest hole -0.777, 1-sigma level 0.099 Q1 1 0.5093 -0.1762 0.5000 10.50000 0.05 0.30 Q2 1 0.0000 0.0000 0.2120 10.08333 0.05 0.29 ; _shelx_res_checksum 26155 _shelx_hkl_file ; 0 0 -2 366351. 7974.60 1 0 0 3 437711. 11126.5 9 0 0 3 448454. 10129.2 3 0 0 -3 451496. 11034.5 5 0 0 -3 441933. 9876.15 1 0 0 3 444472. 10048.9 7 0 0 3 444028. 11032.9 8 0 0 3 460061. 9998.88 1 0 0 -4 190936. 5338.09 1 0 0 4 197880. 5607.55 3 0 0 4 200513. 6481.77 8 0 0 4 196236. 5533.27 7 0 0 -4 196075. 6455.71 5 0 0 4 196968. 5444.15 1 0 0 4 187788. 6454.54 9 0 0 -5 256683. 8136.26 5 0 0 5 260177. 6926.72 1 0 0 5 255631. 6978.29 7 0 0 5 258748. 7103.29 3 0 0 -5 253142. 6821.47 1 0 0 5 256109. 8259.46 9 0 0 5 265181. 8243.84 8 0 0 5 253843. 7923.69 2 0 0 6 173794. 5320.76 1 0 0 -6 176561. 6615.13 5 0 0 6 168479. 6466.79 8 0 0 6 165429. 5457.43 3 0 0 6 175558. 6630.98 9 0 0 6 163739. 6231.84 2 0 0 6 165958. 5343.36 7 0 0 7 358948. 9418.93 7 0 0 -7 369042. 11049.5 5 0 0 7 363627. 8928.12 6 0 0 7 362960. 10740.3 2 0 0 7 352840. 9286.43 1 0 0 7 371656. 9665.17 3 0 0 8 4321.40 859.875 7 0 0 8 3609.69 1080.80 2 0 0 8 4380.17 794.131 1 0 0 -8 3081.14 1058.55 9 0 0 8 3828.32 838.061 3 0 0 -8 2536.59 987.920 5 0 0 8 4863.49 764.223 6 0 0 9 394077. 10361.3 7 0 0 9 386100. 10154.3 1 0 0 -9 404193. 12302.0 5 0 0 9 391127. 10555.2 3 0 0 9 394205. 11875.5 2 0 0 9 391691. 9699.82 6 0 0 10 288934. 8341.44 1 0 0 10 293357. 8675.65 3 0 0 10 301836. 10101.9 2 0 0 -10 297948. 10418.7 5 0 0 10 294291. 8541.15 7 0 0 10 290990. 7871.70 6 0 0 11 158673. 5763.13 7 0 0 11 156928. 5513.68 1 0 0 -11 164250. 7368.56 5 0 0 11 158412. 7035.21 2 0 0 11 158751. 5088.59 6 0 0 11 152303. 5792.85 3 0 0 12 171807. 6103.28 7 0 0 12 150791. 7194.36 2 0 0 12 175329. 6283.01 3 0 0 -12 170586. 7791.07 5 0 0 12 173297. 5333.00 6 0 0 -13 2691.35 1182.70 5 0 0 13 4675.18 1308.44 2 0 0 13 5058.58 991.346 7 0 0 13 4591.87 933.052 3 0 0 14 180693. 8261.74 2 0 0 14 187847. 6657.30 3 0 0 -14 189856. 8739.21 5 0 0 15 74781.8 5219.35 2 0 0 -15 86984.9 5847.41 5 0 0 16 8601.88 1768.94 2 0 0 17 71698.6 5242.91 2 0 0 18 4581.64 1246.69 2 1 -1 0 95043.8 3168.18 1 -1 1 0 97598.7 2813.48 7 -1 1 0 98868.3 2668.78 4 -1 0 0 93876.3 3115.81 3 0 1 0 89267.2 3220.31 7 0 1 0 94144.8 2524.88 2 0 -1 0 93613.1 2708.41 3 0 1 0 90942.6 2664.88 4 1 0 0 97310.5 2948.46 6 -1 1 -1 17776.2 928.490 1 -1 1 -1 18039.5 990.996 7 0 1 -1 19532.1 1057.78 7 1 -1 -1 20408.7 1479.59 1 -1 0 1 19298.7 1484.30 3 -1 1 1 18037.3 1093.06 7 1 0 -1 19312.1 1105.13 6 1 0 -1 17359.0 818.772 5 0 1 1 18804.7 1125.23 6 1 0 1 18557.3 1203.39 6 0 -1 1 21617.8 1417.36 7 0 1 -1 16294.5 934.392 4 1 -1 1 19166.6 1105.08 1 0 1 -1 18798.6 1166.06 2 0 -1 1 19022.1 1063.64 3 0 1 1 17306.6 1536.45 7 -1 1 1 19887.9 919.796 4 0 -1 -1 17236.4 945.580 3 1 0 1 20808.1 1238.07 3 -1 0 -1 20031.2 982.073 3 1 -1 1 17503.5 871.523 9 -1 1 -1 17402.2 722.587 5 1 -1 2 149340. 4085.42 9 -1 0 2 172315. 5677.56 3 1 -1 -2 150165. 3819.92 6 0 -1 2 154471. 4015.30 7 1 0 -2 151091. 3987.73 6 1 0 -2 149232. 3709.16 7 1 -1 2 149776. 3745.34 5 0 1 -2 162517. 3440.12 7 1 0 -2 142823. 3875.97 8 1 -1 -2 151742. 5051.22 1 0 1 -2 150578. 4013.57 5 0 1 2 157040. 4035.03 6 0 -1 -2 141562. 3768.79 6 1 -1 2 156769. 3776.81 1 -1 1 -2 159349. 3870.25 5 1 0 2 165298. 3884.42 3 0 1 2 155648. 5698.99 7 0 -1 -2 146136. 3609.99 9 -1 1 2 153736. 4349.90 7 1 0 -2 151678. 4026.71 5 0 -1 -2 151096. 3887.76 8 -1 0 -2 157031. 3351.56 3 0 1 -2 151012. 3853.20 4 0 -1 -2 153153. 4081.20 1 -1 1 -2 145640. 3611.03 3 -1 1 2 155392. 3671.90 4 0 -1 2 157257. 4254.11 3 0 1 -2 156599. 4819.13 2 1 0 2 154907. 4547.18 6 -1 0 3 526335. 10636.9 7 1 -1 3 495942. 11178.0 5 -1 1 -3 503000. 11315.0 5 1 0 -3 528610. 11322.9 2 0 1 -3 577006. 11426.6 5 -1 1 3 512070. 11681.3 7 1 -1 -3 504855. 10614.4 2 0 -1 -3 522027. 11190.8 1 -1 0 -3 494347. 11557.6 6 0 1 -3 519284. 12617.3 2 -1 0 3 491097. 13385.6 3 1 -1 3 524952. 10507.6 3 1 0 -3 492642. 11493.6 5 1 -1 -3 449180. 12372.3 1 0 -1 -3 507545. 11477.1 8 1 0 -3 493953. 11499.5 8 1 0 3 488685. 11305.9 5 0 -1 3 472936. 11906.9 9 0 1 3 518575. 10844.6 6 0 1 3 580822. 10964.1 9 1 0 -3 522347. 10521.6 7 0 -1 3 571452. 11122.8 4 1 0 -3 528465. 10848.9 6 0 -1 3 511140. 11466.5 3 1 -1 3 482040. 11610.2 9 -1 0 3 513095. 11139.2 6 1 -1 3 540256. 11078.5 7 1 -1 -3 507492. 10112.6 6 0 1 3 492404. 13186.8 7 0 -1 -3 491125. 11002.0 9 0 -1 -3 522751. 10609.9 6 1 0 3 480764. 11753.8 6 -1 1 -3 527922. 10399.3 3 1 -1 3 503810. 10283.9 1 1 -1 -4 26551.8 1657.30 7 1 -1 4 22424.0 1608.24 5 1 -1 4 25529.5 1125.01 3 1 -1 -4 22502.2 2037.94 1 1 0 -4 22789.9 1098.24 7 0 -1 -4 27299.0 1880.14 8 0 1 -4 30536.5 2344.29 2 0 -1 -4 24304.8 1623.84 9 0 1 -4 25132.5 1635.70 5 0 -1 -4 23649.7 1102.41 6 1 -1 -4 28039.5 1917.57 5 0 1 -4 25574.0 1595.89 3 -1 0 4 27565.9 2400.58 3 1 0 -4 25994.7 1611.96 2 -1 1 4 26550.3 1790.49 7 -1 0 4 23925.2 1673.86 8 1 -1 -4 25456.4 1388.77 2 -1 0 4 23592.4 1166.38 7 0 1 4 27289.2 2302.89 7 1 0 -4 24760.3 1269.97 6 -1 1 -4 24556.3 1706.23 5 1 0 -4 25950.1 1839.21 5 1 -1 4 24281.8 1854.33 9 1 0 -4 25144.2 1864.44 8 0 1 4 26726.6 1597.99 1 0 -1 -4 25836.3 1513.71 1 1 0 4 25246.7 1578.89 9 1 0 4 25779.1 1785.90 5 -1 1 4 25669.3 1682.96 9 1 0 4 26015.6 1819.27 6 0 1 4 26500.4 1771.30 8 0 -1 4 26343.2 2037.18 9 -1 1 -4 24002.1 1084.71 3 -1 0 -4 24633.3 933.033 1 0 -1 4 22080.3 1350.44 4 0 -1 4 25426.8 1658.67 3 -1 0 -4 24387.4 1617.67 6 -1 0 4 25635.0 1440.57 6 0 1 4 27812.9 1306.37 6 0 1 4 25314.4 1483.10 9 1 -1 -5 126320. 4362.53 7 1 0 5 120723. 4615.06 6 0 1 5 121035. 3470.58 6 1 0 5 121559. 4877.94 8 -1 1 5 116330. 3890.48 2 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3 0 5 9 6937.37 2186.07 7 0 -5 9 5354.81 1777.97 3 0 5 9 5895.15 2145.42 4 -5 5 9 4671.24 1858.82 7 5 -5 10 4610.59 1797.60 6 5 0 10 10495.6 2446.55 6 0 -5 -10 10008.0 2115.43 1 -5 5 -10 11308.2 2472.46 9 -5 0 -10 10379.5 2241.11 9 0 5 -10 8052.69 1937.07 5 5 0 -10 7458.02 1722.84 5 5 -5 -10 11845.6 2293.29 8 -5 0 10 6806.70 2132.60 3 5 -5 -10 11690.0 2862.31 1 0 5 10 8275.07 2158.21 7 0 -5 10 7448.62 2115.04 3 0 5 10 6596.19 2244.38 4 -5 5 10 10094.4 2564.75 7 5 -5 11 1910.93 1155.43 6 5 -5 -11 4173.40 1657.67 1 5 0 11 6876.03 1882.87 6 0 -5 -11 5023.23 1598.07 1 -5 5 -11 5391.76 1839.82 9 -5 0 -11 5299.95 1657.57 9 0 5 -11 4736.59 1683.53 5 5 -5 -11 6239.66 1918.88 8 -5 0 11 4618.89 1755.83 3 0 5 11 6816.58 1947.58 7 0 -5 11 2508.14 1330.67 3 0 5 11 7812.09 2406.52 4 -5 5 11 2560.39 1319.51 7 0 -5 -12 36090.6 4064.43 1 5 0 12 34952.6 4175.15 6 -5 5 -12 37213.3 4426.32 9 0 -5 12 31803.0 4180.82 3 -5 5 12 29012.2 4050.88 7 6 -3 0 256744. 10723.9 6 -6 3 0 236709. 12216.7 3 3 3 0 266714. 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4160.63 4 -2 7 4 39142.8 4682.41 7 -5 7 4 39877.6 4621.20 7 -2 7 4 44843.0 4634.06 4 2 -7 -4 40769.8 4630.19 1 2 5 -4 41284.2 3619.84 4 -5 7 -4 46106.4 3959.90 7 2 5 4 44046.7 5915.51 7 -2 7 -4 46470.0 4375.17 4 5 -7 4 40826.1 5273.46 1 7 -5 5 98248.7 8782.12 6 -7 5 5 106987. 9197.99 3 7 -2 -5 99346.5 6244.43 6 5 2 5 102714. 8325.17 6 -7 2 5 91170.0 8610.53 3 5 2 -5 93744.9 6794.09 6 5 -7 -5 107598. 8866.08 1 -5 -2 5 88297.8 7098.83 3 -2 7 -5 96118.1 6109.89 5 2 5 -5 92004.5 6212.95 5 -2 -5 5 88421.3 6918.37 3 -7 5 -5 101619. 6524.87 9 -7 2 -5 100575. 6454.27 9 -5 -2 -5 94307.3 5964.44 9 -2 -5 -5 96735.2 6451.55 1 2 -7 5 100075. 7841.73 1 2 5 5 83164.7 8239.71 7 2 5 5 81875.1 6353.62 4 -2 7 5 92926.0 7597.91 7 -5 7 5 93363.2 7458.55 7 -2 7 5 104179. 7242.73 4 -5 7 5 94538.8 6826.53 4 2 -7 6-2693.02 1473.98 1 -5 7 6 2125.71 1657.50 4 7 -2 -6-150.203 776.674 6 -7 5 -6 2313.69 1160.25 9 -2 7 -6-209.068 905.014 5 -5 -2 -6 3214.08 1235.49 9 -7 2 6 2950.23 1708.67 3 -2 -5 -6 1586.85 1089.75 1 -7 5 -7 92078.3 6738.44 9 -2 -5 -7 84080.8 5990.78 1 2 -7 7 77393.6 7225.64 1 6 -7 0 20270.8 3533.05 6 7 -6 0 18209.5 3063.60 6 7 -1 0 19325.1 3213.42 6 7 -6 0 24757.8 4384.28 1 6 -7 0 10555.0 3319.85 1 -6 -1 0 20121.9 2707.19 3 1 6 0 23398.5 3333.31 7 -1 7 0 16382.4 2493.54 7 -6 7 0 18131.7 2844.00 7 1 6 0 17302.6 2688.62 4 6 -7 1 742.732 1041.73 6 6 -7 -1 1046.27 986.021 6 7 -6 1 1313.57 1105.70 6 7 -6 -1 2434.62 1339.53 6 7 -1 -1 2158.38 1374.95 6 6 -7 1 116.862 1714.53 1 6 -7 -1 3938.15 1631.96 1 -7 1 1 2563.49 1159.20 3 7 -6 -1 4153.51 2402.45 1 -6 -1 1 3019.35 1210.04 3 1 6 1 2588.75 1579.11 7 -1 7 1 1387.72 1074.68 7 -6 7 1 2552.03 1217.06 7 -6 7 -1 2362.85 1206.76 7 1 6 1 4009.12 1292.77 4 1 6 -1 1729.49 1144.69 4 6 -7 2 18656.4 3692.03 6 6 -7 -2 18824.8 3058.82 6 7 -6 2 27881.7 4235.29 6 7 -6 -2 19992.2 2977.71 6 7 -1 -2 20920.2 3108.39 6 7 -6 -2 24840.4 4876.40 1 6 -7 2 17864.0 3887.38 1 6 -7 -2 22837.5 4758.65 1 -7 1 2 20269.6 3169.42 3 -6 -1 2 21395.8 3048.46 3 1 6 2 20881.7 3523.53 7 -1 7 2 22567.3 3340.61 7 1 6 2 18407.9 2867.25 4 -6 7 -2 18564.5 2753.17 7 1 6 -2 14752.7 2419.65 4 7 -1 -3 32365.0 3839.92 6 6 -7 3 33340.9 5344.17 6 -7 1 3 33434.0 4308.19 3 -6 -1 3 30639.5 3840.00 3 7 -6 -3 46214.6 6408.02 1 6 -7 -3 45248.9 6466.74 1 -1 7 3 39601.4 4719.45 7 1 6 -3 34214.7 3609.41 4 1 6 3 33717.5 4665.23 7 1 6 -4 3875.70 1422.57 4 7 -1 -4 2076.52 1098.40 6 -7 1 4 1899.19 1266.22 3 -6 -1 4 1172.08 1291.11 3 1 6 4 3924.10 1721.62 7 -1 7 4 1990.19 1330.90 7 1 6 -5 17200.9 2481.44 4 7 -1 -5 18077.2 2746.47 6 0 0 0 0.00 0.00 0 TITL pg48 in P6/mmm REM P6/mmm (#191 in standard setting) CELL 0.71073 5.240153 5.240153 12.294398 90.0000 90.0000 120.0000 ZERR 2.00 0.000140 0.000140 0.000399 0.0000 0.0000 0.0000 LATT 1 SYMM -y, x-y, z SYMM -x+y,-x, z SYMM -x,-y, z SYMM y,-x+y, z SYMM x-y, x, z SYMM y, x,-z SYMM x-y,-y,-z SYMM -x,-x+y,-z SYMM -y,-x,-z SYMM -x+y, y,-z SYMM x, x-y,-z SFAC O Cl K As UNIT 6.00 2.00 2.00 4.00 TREF HKLF 4 END ; _shelx_hkl_checksum 2593 _olex2_date_sample_data_collection 2018-12-05 _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 1.104 _oxdiff_exptl_absorpt_empirical_full_min 0.891 loop_ _space_group_symop_operation_xyz 'x, y, z' 'x-y, x, z' '-y, x-y, z' '-x, -y, z' '-x+y, -x, z' 'y, -x+y, z' 'x-y, -y, -z' '-x, -x+y, -z' 'y, x, -z' '-y, -x, -z' '-x+y, y, -z' 'x, x-y, -z' '-x, -y, -z' '-x+y, -x, -z' 'y, -x+y, -z' 'x, y, -z' 'x-y, x, -z' '-y, x-y, -z' '-x+y, y, z' 'x, x-y, z' '-y, -x, z' 'y, x, z' 'x-y, -y, z' '-x, -x+y, z' 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 0.333333 0.666667 0.21026(2) 0.01105(12) Uani 1 6 d S T P . . K1 K 0.000000 0.000000 0.000000 0.0274(3) Uani 1 24 d S T P . . Cl1 Cl 0.000000 0.000000 0.32424(12) 0.0303(3) Uani 1 12 d S T P . . O1 O 0.500000 0.500000 0.13226(13) 0.0147(3) Uani 1 4 d S T P . . K2 K 0.500000 0.000000 0.500000 0.0624(9) Uani 0.3334 8 d S T P A 1 O2 O 0.500000 0.000000 0.500000 0.0624(9) Uani 0.3334 8 d S T P B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 As1 0.00876(13) 0.00876(13) 0.01562(18) 0.000 0.000 0.00438(7) K1 0.0268(5) 0.0268(5) 0.0285(7) 0.000 0.000 0.0134(2) Cl1 0.0269(4) 0.0269(4) 0.0370(6) 0.000 0.000 0.01346(19) O1 0.0148(6) 0.0148(6) 0.0199(8) 0.000 0.000 0.0115(6) K2 0.085(2) 0.060(2) 0.0333(13) 0.000 0.000 0.0301(10) O2 0.085(2) 0.060(2) 0.0333(13) 0.000 0.000 0.0301(10) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 -1 0.0196 0 1 0 0.1013 0 -1 0 0.0857 -1 1 0 0.0827 1 -1 0 0.0983 -1 0 0 0.1034 1 0 0 0.0878 0 0 1 0.0196 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 O1 As1 O1 94.01(6) 2 3_665 ? O1 As1 O1 94.01(6) 3_665 . ? O1 As1 O1 94.01(6) 2 . ? As1 O1 As1 115.25(9) 2_655 . ? 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 O1 1.7911(9) 2 ? As1 O1 1.7911(9) . ? As1 O1 1.7911(9) 3_665 ? 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 O1 As1 O1 As1 -132.84(4) 2 . . 2_655 ? O1 As1 O1 As1 132.84(4) 3_665 . . 2_655 ? 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 -0.0001 0.0000 -0.9985 -0.0083 0.0037 0.0569 -0.0009 0.9980 0.0001 -0.0657 0.1402 -0.0188 0.0009 -0.9980 -0.0001 0.0657 -0.1402 0.0188 -0.9983 0.9979 0.0004 0.0880 0.1287 0.0045 0.9983 -0.9979 -0.0004 -0.0880 -0.1287 -0.0045 -0.9975 -0.0001 0.0003 0.1537 -0.0115 0.0233 0.9975 0.0001 -0.0003 -0.1537 0.0115 -0.0233 0.0001 -0.0000 0.9985 0.0083 -0.0037 -0.0569