#------------------------------------------------------------------------------ #$Date: 2023-12-06 16:50:21 +0100 (Wed, 06 Dec 2023) $ #$Revision: 288091 $ #$URL: svn://www.crystallography.net/cod/cif/2/02/28/2022876.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2022876 loop_ _publ_author_name 'Poreba, Tomasz' 'Garbarino, Gaston' 'Comboni, Davide' 'Mezouar, Mohamed' _publ_section_title ; Deformation of polyiodides in Cs2I8 crystals at high pressure ; _journal_issue 6 _journal_name_full 'Acta Crystallographica Section B Structural Science, Crystal Engineering and Materials' _journal_page_first 934 _journal_page_last 939 _journal_paper_doi 10.1107/S2052520621010192 _journal_volume 77 _journal_year 2021 _chemical_formula_moiety 'Cs I4' _chemical_formula_sum 'Cs I4' _chemical_formula_weight 640.51 _chemical_name_common 'Cesium Tetraiodide' _chemical_name_systematic 'dicesium octaiodide' _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' _audit_creation_date 2021-07-19 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2021-07-20 deposited with the CCDC. 2021-07-23 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 115.28(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.997(3) _cell_length_b 8.8025(3) _cell_length_c 10.9003(8) _cell_measurement_pressure 910000 _cell_measurement_reflns_used 1172 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 20.7870 _cell_measurement_theta_min 2.1750 _cell_volume 867.3(3) _computing_cell_refinement 'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _diffrn_ambient_environment Helium _diffrn_ambient_pressure 910000 _diffrn_ambient_temperature 296(2) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 13.3333 _diffrn_detector_type 'Eiger 9M CdTe' _diffrn_measured_fraction_theta_full 0.378 _diffrn_measured_fraction_theta_max 0.260 _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 -32.00 32.00 0.50 0.20 -- 0.00 0.00 0.00 128 ; _diffrn_measurement_device '1-circle goniometer' _diffrn_measurement_device_type 'esperanto-CrysAlisPro-abstract goniometer imported esperanto images' _diffrn_measurement_method 'phi scan' _diffrn_measurement_specimen_support 'diamond anvil cell' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0430290000 _diffrn_orient_matrix_UB_12 -0.0108681000 _diffrn_orient_matrix_UB_13 -0.0085931000 _diffrn_orient_matrix_UB_21 0.0119439000 _diffrn_orient_matrix_UB_22 -0.0081543000 _diffrn_orient_matrix_UB_23 0.0404447000 _diffrn_orient_matrix_UB_31 -0.0083185000 _diffrn_orient_matrix_UB_32 0.0446550000 _diffrn_orient_matrix_UB_33 0.0052885000 _diffrn_radiation_collimation '0.02 mm double pinhole' _diffrn_radiation_monochromator synchrotron _diffrn_radiation_probe x-ray _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.41077 _diffrn_reflns_av_R_equivalents 0.0147 _diffrn_reflns_av_unetI/netI 0.0175 _diffrn_reflns_Laue_measured_fraction_full 0.378 _diffrn_reflns_Laue_measured_fraction_max 0.260 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 2040 _diffrn_reflns_point_group_measured_fraction_full 0.378 _diffrn_reflns_point_group_measured_fraction_max 0.260 _diffrn_reflns_theta_full 14.268 _diffrn_reflns_theta_max 19.990 _diffrn_reflns_theta_min 2.178 _diffrn_source 'undulator, ID15B, ESRF' _exptl_absorpt_coefficient_mu 4.197 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.61661 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'dark red' _exptl_crystal_colour_modifier dark _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 4.905 _exptl_crystal_description plate _exptl_crystal_F_000 1068 _exptl_crystal_size_max 0.035 _exptl_crystal_size_mid 0.015 _exptl_crystal_size_min 0.01 _refine_diff_density_max 0.921 _refine_diff_density_min -0.564 _refine_diff_density_rms 0.160 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.108 _refine_ls_hydrogen_treatment undef _refine_ls_matrix_type full _refine_ls_number_parameters 46 _refine_ls_number_reflns 1090 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.108 _refine_ls_R_factor_all 0.0379 _refine_ls_R_factor_gt 0.0355 _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^)+(0.0712P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1048 _refine_ls_wR_factor_ref 0.1067 _reflns_Friedel_coverage 0.000 _reflns_number_gt 975 _reflns_number_total 1090 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file bm5146sup1.cif _cod_data_source_block CsI4_0p91GPa _cod_depositor_comments ; The following automatic conversions were performed: data name '__exptl_crystal_size_max' was replaced with '_exptl_crystal_size_max'. Automatic conversion script Id: cif_correct_tags 8170 2020-07-09 18:12:32Z antanas The following automatic conversions were performed: data name '_diffrn_measurement_specimen_suport' was replaced with '_diffrn_measurement_specimen_support' as specified in the replacement file 'data/replacement-values/replacement_tags.lst'. Automatic conversion script Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas ; _cod_database_code 2022876 _cod_database_fobs_code 2022876 _shelx_shelxl_version_number 2017/1 _chemical_oxdiff_formula 'Cs I4' _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. ; _reflns_odcompleteness_completeness 35.84 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 14.88 _olex2_refinement_description ; ; _shelx_res_file ; TITL csi4_0097 in P2(1)/c csi4_0097.res created by SHELXL-2018/3 at 14:30:24 on 19-Jul-2021 REM P2(1)/c (#14 in standard setting) CELL 0.41077 9.996751 8.802525 10.900312 90 115.2788 90 ZERR 4 0.002813 0.000345 0.000827 0 0.0198 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC Cs I DISP Cs -1.803 0.7961 2042.8949 DISP I -2.2298 0.677 1764.6088 UNIT 4 16 L.S. 4 0 0 PLAN 10 CONF list 4 MORE -1 fmap 2 53 acta SHEL 0.6 1000 REM REM REM WGHT 0.071200 FVAR 2.67707 I2 2 0.383290 0.710591 0.393500 11.00000 0.04384 0.04231 = 0.03787 -0.00180 0.02024 0.00421 CS1 1 0.777910 0.876455 0.693859 11.00000 0.05108 0.05103 = 0.04058 0.00409 0.01964 0.00550 I1 2 0.561079 0.904605 0.316969 11.00000 0.04681 0.05416 = 0.04505 0.00334 0.02444 -0.00147 I3 2 0.173318 0.509113 0.451819 11.00000 0.04497 0.04224 = 0.05273 0.00424 0.02517 -0.00053 I4 2 0.051226 0.855120 0.496524 11.00000 0.04119 0.04607 = 0.04607 -0.00251 0.01829 -0.00720 HKLF 4 REM csi4_0097 in P2(1)/c REM wR2 = 0.1067, GooF = S = 1.108, Restrained GooF = 1.108 for all data REM R1 = 0.0355 for 975 Fo > 4sig(Fo) and 0.0379 for all 1090 data REM 46 parameters refined using 0 restraints END WGHT 0.0712 0.0000 REM Highest difference peak 0.921, deepest hole -0.564, 1-sigma level 0.160 Q1 1 0.7404 0.8133 0.7172 11.00000 0.05 0.92 Q2 1 0.7398 0.9352 0.7182 11.00000 0.05 0.90 Q3 1 0.6240 0.9672 0.2977 11.00000 0.05 0.88 Q4 1 0.8432 0.8184 0.6801 11.00000 0.05 0.82 Q5 1 0.1099 0.7973 0.4787 11.00000 0.05 0.78 Q6 1 0.4538 0.6595 0.3821 11.00000 0.05 0.78 Q7 1 0.3057 0.7644 0.4028 11.00000 0.05 0.75 Q8 1 0.2058 0.5535 0.4172 11.00000 0.05 0.74 Q9 1 0.6161 0.8476 0.3028 11.00000 0.05 0.74 Q10 1 0.1114 0.9134 0.4826 11.00000 0.05 0.69 ; _shelx_res_checksum 7335 _shelx_hkl_file ; 0 0 2 83190.3 1119.58 1 0 0 -2 84633.7 1130.73 1 0 0 3 8.09442 19.0673 1 0 0 4 31551.9 648.285 1 0 0 5 21.9451 54.3836 1 0 0 6 153521. 2214.36 1 0 0 -6 150483. 2243.77 1 0 0 7 97.7639 73.2303 1 0 0 -7 8.36782 66.7250 1 0 0 8 40255.2 970.814 1 0 0 -8 40616.9 993.941 1 0 0 -9 98.0950 88.8687 1 0 0 -10 103038. 1945.73 1 0 0 10 101458. 1954.26 1 0 0 -11 104.431 108.480 1 0 0 -12 469.196 123.452 1 0 0 12 197.184 129.732 1 0 0 -13 267.564 106.809 1 0 -1 -2 212884. 2566.51 1 0 -1 2 213651. 2598.61 1 0 1 -2 214347. 2604.00 1 0 1 2 210386. 2580.87 1 0 1 3 343221. 4080.26 1 0 -1 -3 335262. 4076.75 1 0 1 -3 336536. 4123.33 1 0 1 -4 76016.7 1215.56 1 0 -1 -4 72931.6 1160.79 1 0 1 4 77125.3 1172.33 1 0 -1 -5 543471. 6594.29 1 0 1 5 536750. 6557.66 1 0 1 -5 549143. 6624.94 1 0 -1 -6 64526.8 1173.35 1 0 1 -6 65143.2 1212.78 1 0 1 6 61949.3 1162.94 1 0 1 -7 9666.46 424.691 1 0 1 7 9496.51 406.140 1 0 -1 -7 8558.10 394.546 1 0 -1 7 9372.47 410.550 1 0 1 -8 3161.42 260.243 1 0 1 8 3684.35 271.788 1 0 -1 8 3328.30 259.073 1 0 -1 -8 3379.62 262.318 1 0 -1 -9 8141.90 433.033 1 0 1 9 7914.03 417.420 1 0 1 -9 7615.13 438.434 1 0 -1 9 8517.73 443.878 1 0 1 -10 2514.59 274.330 1 0 1 10 2594.62 256.913 1 0 -1 10 2635.26 268.832 1 0 -1 -10 2899.00 271.466 1 0 -1 11 50820.1 1342.09 1 0 1 11 50920.8 1254.56 1 0 -1 -11 52492.5 1289.95 1 0 -1 -12 6509.97 446.917 1 0 1 12 5476.05 390.412 1 0 -1 12 6006.14 443.318 1 0 -1 -13 209.847 103.910 1 0 -1 13 8.13521 112.936 1 0 1 13 256.326 125.027 1 0 -2 1 40766.2 587.232 1 0 2 -1 41572.3 583.389 1 0 -2 2 2515.81 119.725 1 0 2 -2 2306.19 116.334 1 0 -2 -2 2228.60 98.8530 1 0 2 -3 7627.00 259.176 1 0 2 3 7912.72 232.258 1 0 -2 -3 7603.58 229.487 1 0 -2 3 7273.06 250.009 1 0 2 -4 85820.9 1388.62 1 0 -2 -4 89465.3 1310.95 1 0 2 4 87879.4 1298.39 1 0 2 5 2604.19 168.329 1 0 2 -5 2578.66 185.956 1 0 -2 -5 2870.69 182.138 1 0 2 -6 9879.11 410.426 1 0 -2 6 9912.09 395.068 1 0 -2 -6 10316.1 388.351 1 0 2 6 10867.1 383.222 1 0 -2 7 16482.1 565.064 1 0 2 -7 16560.0 584.470 1 0 -2 -7 16604.0 534.600 1 0 2 7 16249.3 519.088 1 0 2 -8 103292. 1852.25 1 0 -2 -8 101427. 1752.96 1 0 -2 8 100340. 1806.73 1 0 2 8 101562. 1712.59 1 0 2 9 8240.97 396.184 1 0 -2 9 7687.62 419.391 1 0 2 -9 7894.44 445.838 1 0 -2 -9 8381.46 430.562 1 0 2 -10 35372.1 1044.51 1 0 -2 -10 41052.5 1047.03 1 0 2 10 38842.0 976.204 1 0 -2 10 36974.1 1052.11 1 0 -2 -11 8351.57 468.218 1 0 -2 11 7345.25 477.041 1 0 2 -11 7701.94 515.766 1 0 -2 -12 2164.64 252.143 1 0 2 -12 2004.33 269.032 1 0 2 12 1951.39 238.372 1 0 2 13 908.036 189.795 1 0 -2 -13 1249.84 205.519 1 0 2 -13 1181.32 215.462 1 0 3 -1 453913. 5282.82 1 0 -3 1 455640. 5266.08 1 0 -3 2 21108.2 426.133 1 0 3 -2 22007.0 424.018 1 0 -3 -3 112242. 1507.72 1 0 3 -3 115307. 1596.14 1 0 -3 3 113795. 1592.76 1 0 3 -4 10585.3 357.320 1 0 -3 4 10940.0 354.744 1 0 -3 -4 11229.0 317.874 1 0 -3 -5 481102. 5814.67 1 0 3 -5 473305. 5950.28 1 0 -3 5 480437. 5921.90 1 0 3 6 28038.9 646.571 1 0 -3 6 26186.0 694.543 1 0 -3 -6 26224.3 636.339 1 0 3 -6 25310.3 712.347 1 0 3 7 142.022 66.1787 1 0 -3 -7 147.170 65.2827 1 0 -3 7 237.251 86.1299 1 0 3 -7 195.580 95.9708 1 0 -3 8 43632.8 1060.77 1 0 -3 -8 45763.3 999.487 1 0 3 8 45324.6 970.571 1 0 3 -8 46192.9 1138.11 1 0 3 -9 9632.46 516.408 1 0 -3 -9 10628.9 459.755 1 0 3 9 10584.7 444.311 1 0 -3 9 10458.1 499.524 1 0 -3 10 4767.35 359.987 1 0 3 -10 5420.25 404.298 1 0 -3 -11 1469.22 193.910 1 0 -3 11 1033.83 193.085 1 0 3 -11 1219.06 206.306 1 0 -3 12 1305.46 230.523 1 0 -3 -12 1536.89 204.073 1 0 3 -12 1197.82 222.621 1 0 -3 13 16.9269 124.326 1 0 3 -13 82.5819 113.919 1 0 -4 1 126984. 1606.29 1 0 4 -2 185116. 2306.98 1 0 -4 2 182824. 2326.22 1 0 -4 3 18917.5 454.218 1 0 4 -3 18844.9 450.220 1 0 4 -4 96406.4 1466.98 1 0 -4 -4 94326.0 1338.11 1 0 -4 4 94860.6 1458.70 1 0 4 -5 33092.0 753.698 1 0 -4 5 32402.0 764.558 1 0 -4 6 270616. 3657.22 1 0 4 -6 270178. 3641.74 1 0 -4 -6 270994. 3516.25 1 0 -4 7 6600.60 355.579 1 0 -4 -7 6684.71 312.728 1 0 4 -7 6548.57 354.346 1 0 -4 -8 6711.28 329.810 1 0 -4 8 6598.65 371.339 1 0 4 -8 6163.15 371.388 1 0 -4 9 9331.59 472.493 1 0 4 -10 44153.2 1185.69 1 0 -4 10 43564.2 1123.28 1 0 -4 -11 2342.72 234.827 1 0 -4 11 2251.61 271.714 1 0 4 -11 1957.40 261.052 1 0 4 -12 4170.91 393.090 1 0 -4 -12 4962.40 360.028 1 0 -5 1 520680. 6072.10 1 0 5 -2 77426.5 1120.65 1 0 -5 2 74862.2 1108.50 1 0 -5 3 88895.0 1326.17 1 0 -5 4 12387.2 393.256 1 0 -5 -5 23082.1 520.633 1 0 -5 5 22313.8 603.532 1 0 -5 -6 7219.80 289.275 1 0 -5 6 6398.18 322.039 1 0 -5 7 23417.9 692.051 1 0 -5 -7 21479.0 573.853 1 0 5 -7 21954.6 663.581 1 0 5 -8 1021.20 159.868 1 0 -5 -8 1205.00 138.876 1 0 -5 8 1178.21 166.658 1 0 -5 -9 242.493 83.7140 1 0 5 -9 189.890 97.4708 1 0 -5 9 156.885 99.6232 1 0 -5 10 812.416 162.812 1 0 5 -10 782.755 163.206 1 0 -5 -10 1081.62 155.650 1 0 -5 -11 6832.32 384.665 1 0 -5 11 5850.05 421.269 1 0 5 -11 5567.40 417.873 1 0 -5 12 1797.46 250.711 1 0 5 -12 1527.70 248.854 1 0 -6 1 2004.37 109.001 1 0 -6 2 205843. 2607.03 1 0 -6 3 104127. 1488.38 1 0 6 -3 96213.7 1447.27 1 0 -6 4 40211.5 811.235 1 0 6 -4 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146.002 1 0 -8 3 8256.23 292.605 1 0 -8 4 24169.2 592.107 1 0 -8 5 131.383 69.3799 1 0 8 -5 185.936 71.6144 1 0 -8 6 10015.1 418.062 1 0 8 -6 10279.9 412.113 1 0 8 -7 26405.3 741.743 1 0 -8 7 28380.8 773.155 1 0 -8 8 9428.60 445.915 1 0 8 -8 8180.96 420.419 1 0 8 -9 140.539 94.9152 1 0 -8 9 112.122 92.0829 1 0 -8 10 136.045 99.2194 1 0 8 -10 165.752 107.798 1 0 8 -11 1320.80 209.551 1 0 -8 11 1455.95 225.531 1 0 -8 12 369.028 153.204 1 0 8 -12 261.628 130.861 1 0 -9 0 66.9849 24.8826 1 0 -9 1 21778.2 424.020 1 0 -9 2 15268.1 377.924 1 0 -9 3 22216.1 514.241 1 0 -9 4 16034.0 457.978 1 0 -9 5 18804.1 545.065 1 0 9 -6 459.214 105.811 1 0 -9 6 419.828 99.8540 1 0 -9 7 847.583 133.973 1 0 9 -7 1001.32 148.097 1 0 9 -8 2900.12 256.762 1 0 -9 8 2827.22 247.775 1 0 9 -9 653.523 138.890 1 0 -9 9 826.686 149.032 1 0 -9 10 1369.49 202.038 1 0 9 -10 1587.93 211.445 1 0 9 -11 470.805 145.048 1 0 -9 11 490.279 140.931 1 0 -10 0 16744.0 314.573 1 0 -10 -1 13796.3 246.251 1 0 -10 1 14431.0 317.225 1 0 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4267.18 332.908 1 -5 3 13 8163.91 444.479 1 5 3 -13 7545.44 502.200 1 5 -3 -13 7553.72 412.536 1 -5 -3 12 2375.14 284.199 1 -5 3 12 2891.70 254.907 1 5 3 -12 2871.83 302.258 1 5 -3 -12 2959.83 248.814 1 5 -3 -11 21326.8 667.070 1 -5 3 11 20180.6 674.035 1 -5 3 10 2582.51 226.364 1 -5 3 9 14499.9 507.731 1 -5 3 8 261182. 3499.55 1 -5 4 16 769.427 156.345 1 5 -4 -15 477.076 133.698 1 -5 4 15 472.839 130.464 1 -5 4 14 2285.99 244.860 1 5 4 -14 1958.18 288.435 1 5 -4 -14 2356.32 245.291 1 -5 4 13 4551.89 324.397 1 5 -4 -13 4446.63 302.274 1 -5 -4 13 3818.05 377.041 1 5 -4 -12 175.223 84.6164 1 -5 4 12 174.135 88.6343 1 5 -4 -11 5875.93 325.165 1 -5 4 11 5146.49 314.325 1 -5 4 10 851.926 128.877 1 5 -4 -10 1083.45 141.221 1 -5 4 9 18890.8 550.997 1 -5 4 8 21166.7 566.481 1 5 -5 -16 185.005 104.155 1 -5 5 15 4180.42 325.901 1 5 -5 -15 4453.10 328.139 1 -5 5 14 2034.68 221.361 1 5 -5 -14 2002.06 215.350 1 -5 5 13 4949.41 329.138 1 5 -5 -13 4620.66 302.068 1 -5 5 12 50.4612 72.0419 1 -5 5 11 2977.64 230.256 1 5 -5 -11 2997.45 232.873 1 -5 5 10 1533.62 158.010 1 -5 5 9 31.4173 55.8472 1 -5 5 8 35025.1 726.669 1 -5 5 7 891.782 95.3325 1 -5 6 16 221.054 115.397 1 5 -6 -16 99.7311 87.0252 1 -5 6 15 29.8378 89.9792 1 -5 6 14 191.923 96.1436 1 5 -6 -14 172.589 89.7379 1 -5 6 13 23325.0 727.243 1 5 -6 -13 22052.7 691.009 1 5 -6 -12 10270.7 440.575 1 5 -6 -11 114.825 71.6865 1 -5 6 11 140.649 80.4477 1 -5 6 10 561.015 104.084 1 -5 6 9 11286.7 394.308 1 -5 6 8 747.145 100.743 1 -5 6 7 433.858 71.6413 1 -5 6 6 1558.35 105.228 1 -5 7 16 1051.92 180.872 1 5 -7 -16 1115.73 164.202 1 -5 7 15 46.5458 92.0807 1 5 -7 -15 34.4905 79.1704 1 5 -7 -14 749.473 137.869 1 -5 7 14 727.910 145.507 1 -5 7 13 914.259 149.269 1 5 -7 -13 779.147 136.013 1 -5 7 12 1218.06 152.701 1 5 -7 -12 1186.27 150.209 1 -5 7 11 8893.46 380.889 1 -5 7 10 7027.03 309.495 1 -5 7 9 23172.1 571.870 1 -5 7 6 36757.1 636.765 1 -5 7 5 21231.8 393.386 1 5 -8 -16 171.063 82.6465 1 -5 8 16 105.933 84.7901 1 5 -8 -15 378.721 107.798 1 -5 8 15 411.585 113.187 1 -5 8 14 106.246 83.1152 1 5 -8 -14 90.4333 73.7022 1 -5 8 13 686.624 126.905 1 5 -8 -13 442.320 102.816 1 -5 8 12 9166.21 399.006 1 -5 8 11 9612.43 390.192 1 -5 8 10 55.0506 50.9772 1 -5 8 9 2687.49 164.577 1 -5 8 8 2860.28 153.905 1 -5 8 7 6807.74 217.426 1 -5 8 6 7497.37 199.663 1 -5 8 5 28950.6 432.704 1 5 -9 -15 1317.67 169.624 1 5 -9 -14 23.5121 65.7236 1 -5 9 13 878.787 129.664 1 -5 9 12 35.7287 52.9636 1 -5 9 1 6815.83 192.654 1 -5 9 0 6581.66 220.108 1 -5 9 -1 636.112 83.0376 1 -5 9 -2 8319.00 316.608 1 -5 9 -3 218.139 70.0540 1 -5 10 0 9188.59 251.539 1 -5 10 -1 11100.0 328.706 1 -5 10 -2 2294.67 161.034 1 -5 10 -3 3564.53 227.590 1 -5 10 -4 489.725 93.2422 1 -5 11 -2 2283.57 154.973 1 -5 11 -3 50.8167 52.1571 1 -5 11 -4 2355.01 193.052 1 6 0 -15 31.4093 106.792 1 6 0 -14 8075.16 496.960 1 -6 0 14 7247.76 497.239 1 6 -1 -15 133.325 121.651 1 -6 -1 15 26.9628 107.319 1 6 -1 -14 4031.27 349.977 1 -6 1 14 3911.46 358.546 1 -6 -1 14 3477.05 350.896 1 -6 1 13 2514.74 283.591 1 6 -2 -15 746.703 163.952 1 -6 2 15 725.177 172.199 1 -6 2 14 21.1487 87.5205 1 -6 2 13 5786.19 402.927 1 -6 2 12 28.2731 80.0433 1 -6 3 16 442.040 150.624 1 -6 3 15 1101.29 192.247 1 6 -3 -15 1263.44 197.508 1 6 -3 -14 395.240 129.724 1 -6 3 14 325.369 121.660 1 -6 3 11 19211.9 681.646 1 -6 4 16 5573.65 401.398 1 6 -4 -16 5942.49 407.251 1 -6 4 15 311.834 119.248 1 6 -4 -15 468.199 141.798 1 -6 4 14 3037.66 276.326 1 6 -4 -14 3379.03 296.992 1 -6 4 13 9136.48 449.801 1 -6 4 12 1166.76 164.185 1 -6 4 11 1451.60 172.552 1 -6 4 10 10478.4 424.804 1 -6 5 16 105.129 70.7875 1 6 -5 -16 30.4638 87.8910 1 6 -5 -15 3335.47 298.716 1 -6 5 14 2112.93 228.930 1 6 -5 -14 2767.54 254.509 1 -6 5 13 636.015 129.537 1 -6 5 12 8955.44 415.045 1 -6 5 11 68581.5 1297.13 1 -6 5 10 673.554 110.074 1 -6 5 9 4699.34 247.906 1 6 -6 -16 11.9971 84.9111 1 -6 6 16 23.3984 77.0284 1 -6 6 15 1398.42 187.094 1 6 -6 -15 1384.76 194.507 1 -6 6 14 2984.78 260.085 1 -6 6 13 255.465 95.2349 1 -6 6 10 13018.7 441.888 1 -6 6 9 20757.6 539.318 1 -6 7 16 429.276 124.953 1 -6 7 15 21.0827 74.6082 1 -6 7 14 34.9581 74.0133 1 -6 7 12 142.822 77.6784 1 -6 7 11 5083.72 290.889 1 -6 7 10 313.487 79.6796 1 -6 7 9 1453.77 136.662 1 -6 8 16 868.804 157.384 1 -6 8 15 64.0682 83.1888 1 -6 8 14 623.547 128.376 1 -6 8 13 443.936 108.247 1 -6 8 12 1286.21 150.215 1 -6 8 11 32.8818 50.8253 1 -6 8 10 4621.11 246.502 1 -6 8 9 9724.17 341.420 1 -6 8 8 2226.04 145.395 1 -6 8 7 11925.3 321.758 1 -6 8 6 32184.5 570.903 1 -6 9 12 2461.73 193.094 1 -6 9 11 963.600 116.845 1 -6 9 10 2327.26 158.641 1 -6 9 9 17619.9 422.581 1 -6 9 8 10684.7 291.469 1 -6 9 7 739.630 63.7576 1 -6 9 6 10700.6 224.287 1 -6 10 2 42.1883 18.2129 1 -6 10 1 22.1157 31.0561 1 -6 10 0 894.864 90.0874 1 -7 2 15 2680.08 291.048 1 -7 3 16 438.420 137.502 1 -7 3 15 466.375 139.124 1 -7 3 14 4646.05 346.635 1 -7 4 16 449.591 128.004 1 -7 4 15 272.075 109.575 1 -7 4 14 10605.2 508.823 1 -7 4 13 2538.85 238.358 1 -7 5 16 1154.38 168.396 1 -7 5 14 602.635 126.978 1 -7 5 13 6612.30 364.349 1 -7 5 12 4445.73 282.803 1 -7 6 16 118.191 61.5064 1 -7 6 15 388.953 107.343 1 -7 6 14 1723.01 193.282 1 -7 6 13 430.108 105.465 1 -7 6 12 2999.09 227.529 1 -7 7 16 187.293 68.9140 1 -7 7 15 2362.61 216.577 1 -7 7 14 373.762 99.3206 1 -7 7 13 381.214 101.233 1 -7 7 12 6485.22 324.270 1 -7 7 11 1183.42 132.124 1 -7 7 10 386.204 78.4005 1 -7 8 15 2997.25 241.386 1 -7 8 14 216.170 68.7794 1 -7 8 13 364.493 90.4706 1 -7 8 12 25.7703 61.3209 1 -7 8 11 215.583 75.9053 1 -7 8 10 4067.97 221.576 1 -7 8 9 332.457 67.9594 1 -7 9 12 243.217 70.2878 1 -7 9 11 54.9513 53.9378 1 -7 9 10 4677.33 229.724 1 -7 9 9 1035.90 105.584 1 -7 9 8 615.058 75.9737 1 -7 9 7 26120.5 488.495 1 0 0 0 0.00 0.00 0 TITL csi4_0097 in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 0.41077 9.996751 8.802525 10.900312 90.0000 115.2788 90.0000 ZERR 5.00 0.002813 0.000345 0.000827 0.0000 0.0198 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC I Cs UNIT 20.00 5.00 TREF HKLF 4 END ; _shelx_hkl_checksum 25306 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_diffrn_reflns_filtered 57 _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.483 _oxdiff_exptl_absorpt_empirical_full_min 0.753 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 I2 I 0.38329(14) 0.71059(6) 0.39350(5) 0.0404(6) Uani 1 1 d . . . . . Cs1 Cs 0.77791(16) 0.87646(6) 0.69386(5) 0.0475(6) Uani 1 1 d . . . . . I1 I 0.56108(18) 0.90461(7) 0.31697(6) 0.0470(6) Uani 1 1 d . . . . . I3 I 0.17332(16) 0.50911(7) 0.45182(6) 0.0451(6) Uani 1 1 d . . . . . I4 I 0.05123(16) 0.85512(7) 0.49652(6) 0.0446(6) Uani 1 1 d . . . . . 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 I2 0.0438(17) 0.0423(3) 0.0379(3) -0.00180(14) 0.0202(5) 0.0042(3) Cs1 0.0511(19) 0.0510(3) 0.0406(3) 0.00409(15) 0.0196(5) 0.0055(3) I1 0.047(2) 0.0542(4) 0.0450(3) 0.00334(18) 0.0244(6) -0.0015(4) I3 0.0450(18) 0.0422(3) 0.0527(3) 0.00424(17) 0.0252(6) -0.0005(4) I4 0.0412(19) 0.0461(3) 0.0461(3) -0.00251(16) 0.0183(6) -0.0072(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cs Cs -1.8030 0.7961 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -2.2298 0.6770 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Cs1 I2 Cs1 91.09(3) 3_676 . ? I1 I2 Cs1 61.20(3) . . ? I1 I2 Cs1 67.34(4) . 3_676 ? I1 I2 I3 175.20(4) . . ? I3 I2 Cs1 123.42(2) . . ? I3 I2 Cs1 110.19(4) . 3_676 ? I2 Cs1 I2 88.91(3) 3_676 . ? I2 Cs1 Cs1 42.76(2) . 3_676 ? I2 Cs1 Cs1 46.151(18) 3_676 3_676 ? I2 Cs1 I4 63.05(3) 3_676 3_676 ? I2 Cs1 I4 102.10(2) 3_676 1_655 ? I1 Cs1 I2 116.20(4) 4_576 3_676 ? I1 Cs1 I2 64.41(3) 4_576 . ? I1 Cs1 I2 71.779(19) . 3_676 ? I1 Cs1 I2 68.07(3) 3_676 . ? I1 Cs1 I2 42.72(2) 3_676 3_676 ? I1 Cs1 I2 41.55(3) . . ? I1 Cs1 Cs1 41.22(3) . 3_676 ? I1 Cs1 Cs1 89.33(4) 4_576 3_676 ? I1 Cs1 Cs1 39.80(2) 3_676 3_676 ? I1 Cs1 I1 81.02(3) . 3_676 ? I1 Cs1 I1 73.52(3) 3_676 4_576 ? I1 Cs1 I1 105.90(4) . 4_576 ? I1 Cs1 I3 67.26(3) 3_676 2_656 ? I1 Cs1 I3 120.16(3) 3_676 4_676 ? I1 Cs1 I3 135.31(4) . 4_676 ? I1 Cs1 I3 147.54(4) . 2_656 ? I1 Cs1 I3 133.60(4) 3_676 3_666 ? I1 Cs1 I3 73.916(19) . 3_666 ? I1 Cs1 I4 104.75(3) 3_676 3_676 ? I1 Cs1 I4 68.56(3) . 1_655 ? I1 Cs1 I4 140.62(2) 3_676 1_655 ? I1 Cs1 I4 64.21(3) . 3_676 ? I1 Cs1 I4 170.05(3) 4_576 3_676 ? I1 Cs1 I4 147.33(3) . 4_676 ? I1 Cs1 I4 137.69(2) 4_576 1_655 ? I3 Cs1 I2 145.51(2) 3_666 3_676 ? I3 Cs1 I2 79.98(2) 2_656 3_676 ? I3 Cs1 I2 171.71(3) 4_676 . ? I3 Cs1 I2 124.36(5) 2_656 . ? I3 Cs1 I2 96.95(3) 4_676 3_676 ? I3 Cs1 I2 67.23(3) 3_666 . ? I3 Cs1 Cs1 106.29(3) 3_666 3_676 ? I3 Cs1 Cs1 142.75(2) 4_676 3_676 ? I3 Cs1 Cs1 106.79(4) 2_656 3_676 ? I3 Cs1 I1 76.68(2) 3_666 4_576 ? I3 Cs1 I1 72.42(2) 2_656 4_576 ? I3 Cs1 I1 117.44(3) 4_676 4_576 ? I3 Cs1 I3 104.92(3) 3_666 4_676 ? I3 Cs1 I3 62.75(4) 2_656 4_676 ? I3 Cs1 I3 133.811(19) 2_656 3_666 ? I3 Cs1 I4 72.19(3) 4_676 1_655 ? I3 Cs1 I4 72.09(3) 4_676 3_676 ? I3 Cs1 I4 98.60(3) 3_666 3_676 ? I3 Cs1 I4 61.30(2) 3_666 1_655 ? I3 Cs1 I4 116.30(3) 2_656 3_676 ? I3 Cs1 I4 134.73(5) 2_656 1_655 ? I4 Cs1 I2 125.11(3) 4_676 . ? I4 Cs1 I2 105.74(2) 3_676 . ? I4 Cs1 I2 140.02(2) 4_676 3_676 ? I4 Cs1 I2 100.90(3) 1_655 . ? I4 Cs1 Cs1 159.26(4) 4_676 3_676 ? I4 Cs1 Cs1 106.19(2) 1_655 3_676 ? I4 Cs1 Cs1 83.57(3) 3_676 3_676 ? I4 Cs1 I1 125.73(3) 4_676 3_676 ? I4 Cs1 I1 70.32(3) 4_676 4_576 ? I4 Cs1 I3 64.05(2) 4_676 2_656 ? I4 Cs1 I3 73.69(2) 4_676 3_666 ? I4 Cs1 I3 52.08(3) 4_676 4_676 ? I4 Cs1 I4 39.70(2) 3_676 1_655 ? I4 Cs1 I4 117.12(4) 4_676 3_676 ? I4 Cs1 I4 92.11(4) 4_676 1_655 ? I2 I1 Cs1 69.94(4) . 3_676 ? I2 I1 Cs1 103.31(3) . 4_575 ? I2 I1 Cs1 77.25(3) . . ? Cs1 I1 Cs1 100.94(4) . 4_575 ? Cs1 I1 Cs1 98.98(3) . 3_676 ? Cs1 I1 Cs1 156.92(3) 3_676 4_575 ? I2 I3 Cs1 125.92(4) . 2_646 ? I2 I3 Cs1 106.26(3) . 4_475 ? I2 I3 Cs1 102.04(4) . 3_666 ? Cs1 I3 Cs1 117.25(4) 2_646 4_475 ? Cs1 I3 Cs1 99.275(15) 2_646 3_666 ? Cs1 I3 Cs1 101.45(3) 3_666 4_475 ? Cs1 I4 Cs1 140.30(2) 3_676 1_455 ? Cs1 I4 Cs1 94.87(4) 4_475 1_455 ? Cs1 I4 Cs1 99.97(2) 4_475 3_676 ? I4 I4 Cs1 66.99(4) 3_576 1_455 ? I4 I4 Cs1 112.14(6) 3_576 4_475 ? I4 I4 Cs1 73.30(4) 3_576 3_676 ? 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 I2 Cs1 3.9251(9) 3_676 ? I2 Cs1 4.1692(19) . ? I2 I1 2.8351(16) . ? I2 I3 3.0158(14) . ? Cs1 Cs1 5.780(3) 3_676 ? Cs1 I1 3.856(2) 3_676 ? Cs1 I1 3.7459(12) . ? Cs1 I1 3.8864(15) 4_576 ? Cs1 I3 3.8652(9) 3_666 ? Cs1 I3 3.880(2) 4_676 ? Cs1 I3 3.8613(8) 2_656 ? Cs1 I4 4.1409(18) 1_655 ? Cs1 I4 3.8479(14) 4_676 ? Cs1 I4 3.9793(13) 3_676 ? I4 I4 2.7617(16) 3_576 ?