#------------------------------------------------------------------------------ #$Date: 2024-07-28 01:36:44 +0300 (Sun, 28 Jul 2024) $ #$Revision: 293571 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/91/7249126.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_7249126 loop_ _publ_author_name 'D'Agostino, Simone' 'Ocak, Samet' 'Braga, Dario' _publ_section_title ; Effect of Supramolecular Complexation of Alkali Hydrogenselenates with Crown Ethers and solid-solutions with their Hydrogensulfate Counterparts on the Solid-to-Solid Phase Transition Behaviors ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D4CE00514G _journal_year 2024 _chemical_formula_moiety 'C12 H24 Cs O11 Se' _chemical_formula_sum 'C12 H24 Cs O11 Se' _chemical_formula_weight 556.18 _chemical_name_systematic Cr6CsHSeO4_H2O _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 _audit_creation_date 2024-02-06 _audit_creation_method ; Olex2 1.5 (compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817) ; _audit_update_record ; 2024-04-22 deposited with the CCDC. 2024-07-23 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 109.486(9) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 23.7101(16) _cell_length_b 8.4597(7) _cell_length_c 21.3553(18) _cell_measurement_reflns_used 1090 _cell_measurement_temperature 300 _cell_measurement_theta_max 20.7300 _cell_measurement_theta_min 2.2260 _cell_volume 4038.1(6) _computing_cell_refinement 'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)' _computing_data_collection 'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)' _computing_data_reduction 'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2016/6 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 300 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.1385 _diffrn_detector_type Sapphire3 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.837 _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 -3.00 51.00 1.00 105.00 -- -16.52 38.00-120.00 54 2 \w -86.00 6.00 1.00 105.00 -- -16.52 -38.00 60.00 92 3 \w -7.00 18.00 1.00 105.00 -- 17.30 77.00 90.00 25 4 \w 10.00 56.00 1.00 105.00 -- 17.30 -99.00-180.00 46 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0025662000 _diffrn_orient_matrix_UB_12 -0.0438046000 _diffrn_orient_matrix_UB_13 -0.0291582000 _diffrn_orient_matrix_UB_21 0.0062399000 _diffrn_orient_matrix_UB_22 0.0693589000 _diffrn_orient_matrix_UB_23 -0.0151784000 _diffrn_orient_matrix_UB_31 0.0309916000 _diffrn_orient_matrix_UB_32 -0.0175527000 _diffrn_orient_matrix_UB_33 0.0126677000 _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 0.1111 _diffrn_reflns_av_unetI/netI 0.4332 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.837 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 8935 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.837 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 29.182 _diffrn_reflns_theta_min 1.822 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 3.685 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.75999 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.42.85a (Rigaku Oxford Diffraction, 2023) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear light colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.830 _exptl_crystal_description plate _exptl_crystal_F_000 2184 _exptl_crystal_preparation solution _exptl_crystal_recrystallization_method 'slow evaporation' _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.943 _refine_diff_density_min -0.558 _refine_diff_density_rms 0.154 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.809 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 226 _refine_ls_number_reflns 4576 _refine_ls_number_restraints 304 _refine_ls_restrained_S_all 0.798 _refine_ls_R_factor_all 0.2828 _refine_ls_R_factor_gt 0.0794 _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^)+(0.0625P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1312 _refine_ls_wR_factor_ref 0.1888 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1224 _reflns_number_total 4576 _reflns_threshold_expression 'I > 2\s(I)' _twin_special_details ; Component 2 rotated by 177.2725\% around [-0.01 1.00 0.00] (reciprocal) or [-0.00 1.00 -0.00] (direct) ; _cod_data_source_file d4ce00514g2.cif _cod_data_source_block Cs-hydrated _cod_database_code 7249126 _shelx_shelxl_version_number 2016/6 _chemical_oxdiff_formula 'C12 O10 Se1 Cs1' _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 0.837 _shelx_estimated_absorpt_t_min 0.837 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H,H) groups 2. Restrained distances C4-Cs1 3.95 with sigma of 0.02 Cs1-C4 4 with sigma of 0.02 C5-Cs1 4 with sigma of 0.02 Cs1-C8 3.9 with sigma of 0.02 3. Rigid body (RIGU) restrains O7, Se1, O10, O8, O9 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C8, Cs1, O2, O4, O6, O1, O3, O5, C1, C9, C3, C2, C6, C7, C10, C11, C12, C5, C4 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 4.a Secondary CH2 refined with riding coordinates: C3(H3A,H3B), C11(H11A,H11B), C6(H6A,H6B), C5(H5A,H5B), C1(H1A,H1B), C2(H2A, H2B), C12(H12A,H12B), C4(H4A,H4B), C10(H10A,H10B), C7(H7A,H7B), C9(H9A,H9B), C8(H8A,H8B) ; _shelx_res_file ; TITL pppp_twin1_hklf4_a.res in I2/a pppp_twin1_hklf4.res created by SHELXL-2016/6 at 09:23:05 on 14-Feb-2024 REM Old TITL pppp_twin1_hklf4 in Ia REM SHELXT solution in I2/a REM R1 0.181, Rweak 0.075, Alpha 0.116, Orientation as input REM Formula found by SHELXT: C16 O9 Se Cs CELL 0.71073 23.7101 8.4597 21.3553 90 109.486 90 ZERR 8 0.0016 0.0007 0.0018 0 0.009 0 LATT 2 SYMM 0.5-X,+Y,-Z SFAC C H Cs O Se UNIT 96 192 8 88 8 DFIX 3.95 C4 Cs1 DFIX 4 Cs1 C4 DFIX 4 C5 Cs1 RIGU O7 Se1 O10 O8 O9 RIGU C8 Cs1 O2 O4 O6 O1 O3 O5 C1 C9 C3 C2 C6 C7 C10 C11 C12 C5 C4 DFIX 3.9 Cs1 C8 L.S. 99 PLAN 5 SIZE 0.05 0.05 0.05 TEMP 26.85 CONF list 4 MORE -1 BOND $H fmap 2 53 acta 50 REM REM REM WGHT 0.062500 FVAR 0.14212 CS1 3 0.644838 0.139643 0.368180 11.00000 0.04263 0.04272 = 0.04823 0.00022 0.01745 0.00037 SE1 5 0.687399 0.888970 0.567951 11.00000 0.05552 0.11389 = 0.04613 0.00031 0.01725 -0.01115 O4 4 0.667053 0.273077 0.244433 11.00000 0.07072 0.04190 = 0.05917 -0.00245 0.04324 -0.00149 O3 4 0.593195 0.006447 0.217131 11.00000 0.03391 0.04831 = 0.04918 -0.01668 0.00918 -0.00002 O6 4 0.590154 0.424870 0.424956 11.00000 0.06921 0.02832 = 0.07209 0.00187 0.04251 0.02100 O1 4 0.518247 0.147702 0.394302 11.00000 0.06755 0.04147 = 0.06599 0.01054 0.03850 0.01487 O2 4 0.539511 -0.090414 0.312709 11.00000 0.04176 0.03908 = 0.06507 -0.00483 0.01675 -0.00696 O5 4 0.641881 0.509665 0.325542 11.00000 0.05287 0.04617 = 0.06444 -0.00870 0.03344 -0.00811 C3 1 0.526942 -0.160718 0.249735 11.00000 0.06477 0.03132 = 0.06683 -0.00727 0.01532 -0.00576 AFIX 23 H3A 2 0.493959 -0.104484 0.218152 11.00000 -1.20000 H3B 2 0.514116 -0.268837 0.251950 11.00000 -1.20000 AFIX 0 O10 4 0.745794 0.916715 0.628244 11.00000 0.07819 0.08798 = 0.06437 -0.02301 0.02045 -0.01344 C11 1 0.536775 0.404235 0.440472 11.00000 0.08517 0.05298 = 0.08698 -0.01710 0.06405 0.00447 AFIX 23 H11A 2 0.502897 0.442418 0.403905 11.00000 -1.20000 H11B 2 0.539187 0.465710 0.479624 11.00000 -1.20000 AFIX 0 C6 1 0.653555 0.186467 0.185004 11.00000 0.05080 0.07162 = 0.07313 -0.02593 0.05109 0.00062 AFIX 23 H6A 2 0.686551 0.196118 0.167970 11.00000 -1.20000 H6B 2 0.618360 0.231717 0.152352 11.00000 -1.20000 AFIX 0 C5 1 0.642485 0.016761 0.193469 11.00000 0.03474 0.06632 = 0.07159 -0.02257 0.01443 -0.00143 AFIX 23 H5A 2 0.633406 -0.038191 0.151390 11.00000 -1.20000 H5B 2 0.677664 -0.031319 0.225061 11.00000 -1.20000 AFIX 0 C1 1 0.503677 -0.011193 0.398039 11.00000 0.05209 0.04791 = 0.07824 0.01905 0.03493 0.00673 AFIX 23 H1A 2 0.469511 -0.018796 0.413227 11.00000 -1.20000 H1B 2 0.537077 -0.065049 0.430052 11.00000 -1.20000 AFIX 0 C2 1 0.489695 -0.087315 0.334013 11.00000 0.04434 0.04476 = 0.08219 0.01050 0.02254 -0.00202 AFIX 23 H2A 2 0.476395 -0.194619 0.336994 11.00000 -1.20000 H2B 2 0.457279 -0.030963 0.301669 11.00000 -1.20000 AFIX 0 C12 1 0.527865 0.238523 0.452586 11.00000 0.06375 0.06481 = 0.05791 0.00777 0.03808 0.00959 AFIX 23 H12A 2 0.562771 0.198826 0.487446 11.00000 -1.20000 H12B 2 0.493630 0.228145 0.467516 11.00000 -1.20000 AFIX 0 C4 1 0.577979 -0.161520 0.225051 11.00000 0.08087 0.03807 = 0.07333 0.00846 0.02438 0.02140 AFIX 23 H4A 2 0.567374 -0.216195 0.182772 11.00000 -1.20000 H4B 2 0.611917 -0.214983 0.256404 11.00000 -1.20000 AFIX 0 C10 1 0.593936 0.579007 0.404400 11.00000 0.10385 0.02526 = 0.07043 -0.00572 0.05209 0.01919 AFIX 23 H10A 2 0.595726 0.652304 0.439942 11.00000 -1.20000 H10B 2 0.559007 0.604201 0.366424 11.00000 -1.20000 AFIX 0 O8 4 0.632101 0.803510 0.578808 11.00000 0.11201 0.25662 = 0.13019 -0.02059 0.05307 -0.08638 C7 1 0.680239 0.437107 0.240903 11.00000 0.02920 0.04309 = 0.07714 0.01011 0.03495 0.00886 AFIX 23 H7A 2 0.646819 0.486849 0.207282 11.00000 -1.20000 H7B 2 0.714990 0.446731 0.226835 11.00000 -1.20000 AFIX 0 C9 1 0.648592 0.592303 0.386274 11.00000 0.09598 0.03681 = 0.05490 -0.00392 0.02937 -0.00408 AFIX 23 H9A 2 0.656909 0.702903 0.381123 11.00000 -1.20000 H9B 2 0.682235 0.548691 0.421640 11.00000 -1.20000 AFIX 0 C8 1 0.691645 0.520733 0.302265 11.00000 0.05982 0.03893 = 0.08951 -0.00060 0.04524 0.00174 AFIX 23 H8A 2 0.726899 0.477059 0.335378 11.00000 -1.20000 H8B 2 0.699525 0.631009 0.295868 11.00000 -1.20000 AFIX 0 O11 4 0.710970 1.315950 0.534617 11.00000 0.19403 0.14546 = 0.07941 0.03112 0.00072 0.00652 O7 4 0.698410 0.831850 0.508949 11.00000 0.09953 0.70054 = 0.15501 -0.24787 0.07081 -0.15062 O9 4 0.649895 1.049026 0.545992 11.00000 0.21088 0.21407 = 0.31698 0.12071 -0.05128 0.06365 HKLF 4 REM pppp_twin1_hklf4_a.res in I2/a REM R1 = 0.0794 for 1224 Fo > 4sig(Fo) and 0.2828 for all 4576 data REM 226 parameters refined using 304 restraints END WGHT 0.0625 0.0000 REM Highest difference peak 0.943, deepest hole -0.558, 1-sigma level 0.154 Q1 1 0.6049 0.1381 0.3282 11.00000 0.05 0.94 Q2 1 0.6804 0.1382 0.4057 11.00000 0.05 0.82 Q3 1 0.6545 0.1276 0.3275 11.00000 0.05 0.65 Q4 1 0.6469 0.1444 0.4148 11.00000 0.05 0.65 Q5 1 0.5931 -0.1281 0.2413 11.00000 0.05 0.65 ; _shelx_res_checksum 38464 _shelx_hkl_file ; 1 1 24 112.86 113.73 4 1 17 13.68 92.43 3 1 20 16.51 107.08 10 -1 15 69.48 96.13 -3 2 23 28.79 118.35 -8 3 19 102.80 89.33 6 0 20 5.10 115.13 0 1 25 -26.87 133.73 8 -1 21 64.01 124.39 14 -3 11 91.32 76.68 -4 2 24 19.06 116.32 -7 -1 -4 0.88 61.75 12 -2 14 44.38 91.20 9 -1 18 -32.28 99.51 -5 2 25 34.36 108.94 10 -1 13 14.67 78.78 -6 2 26 15.24 114.76 2 1 21 11.30 98.78 12 -2 8 31.99 58.54 -9 3 20 88.23 88.71 15 -4 13 17.62 86.23 -14 3 25 14.60 109.58 10 -1 11 86.40 72.97 13 -3 16 31.32 100.35 -10 3 21 48.82 90.43 -13 3 24 -3.71 102.84 10 -2 20 28.68 121.74 0 2 14 37.26 71.39 -9 3 18 -10.30 79.10 12 -2 12 6.59 80.37 12 -3 19 65.43 120.17 7 -1 22 330.73 139.84 -11 3 22 20.57 94.33 -12 3 23 73.74 103.85 15 -4 7 41.10 57.04 11 -2 17 6.75 105.74 12 -2 10 10.25 70.44 -8 3 15 67.61 69.67 1 1 22 29.52 107.89 -3 2 21 66.91 97.51 -10 3 13 243.31 58.72 6 0 18 282.29 98.75 15 -4 11 -35.35 72.02 -1 2 19 54.07 99.84 6 -4 -6 228.69 37.76 -1 2 11 225.48 72.33 -9 3 14 212.71 67.18 -8 3 17 212.63 82.61 15 -4 9 44.21 62.08 4 1 11 51.38 72.13 9 -1 16 144.05 90.27 8 -1 19 60.38 105.11 13 -4 19 -1.86 118.51 14 -4 16 -3.13 104.65 4 0 22 63.79 121.01 3 1 8 99.63 58.88 -10 3 19 61.55 83.51 -14 3 13 -3.70 48.84 -10 3 17 57.46 77.37 4 1 15 170.32 83.12 -4 2 22 33.47 107.56 -15 3 24 -15.50 99.75 6 -1 23 -50.43 128.92 0 1 23 -36.89 121.24 10 -1 9 203.16 69.32 4 1 13 5.23 69.13 9 -2 21 91.86 125.59 -11 3 20 118.17 89.66 -14 3 23 144.68 102.23 -5 2 23 127.94 118.47 -9 2 27 10.12 130.58 13 -3 14 26.90 93.01 -1 2 17 84.28 88.42 -2 2 20 5.74 98.30 -13 3 22 7.12 93.84 -12 3 21 134.10 92.69 -1 1 24 44.14 122.00 -9 3 16 149.87 77.02 -8 2 26 47.29 123.85 -6 2 24 53.07 112.52 -2 2 10 391.81 64.45 11 -3 20 46.21 121.60 -17 3 14 39.23 49.81 -7 2 25 37.66 115.55 3 -3 -6 7.49 46.20 11 -2 15 133.16 93.98 -2 1 3 106.71 28.28 -11 3 16 40.39 68.29 6 0 6 390.46 57.79 -5 2 7 1778.56 58.91 3 1 18 122.75 101.70 6 0 16 76.11 81.02 -1 2 15 56.23 82.30 -2 1 25 96.02 109.62 9 -1 14 77.09 81.60 10 -2 18 -3.04 101.81 -5 -1 -4 20.35 72.21 12 -3 17 65.97 105.89 0 -1 -3 93.72 38.83 -10 3 15 23.61 65.16 -11 3 18 53.86 76.95 -11 3 14 12.67 62.90 0 -3 -7 248.08 60.32 -16 3 23 111.63 99.09 7 -1 20 121.72 116.07 -15 3 14 65.69 53.66 -3 2 9 63.77 50.73 2 0 24 132.53 134.69 2 1 7 67.11 55.48 8 -2 22 78.26 132.45 -4 -2 -6 98.11 64.42 5 -2 -3 6866.72 46.63 10 -6 -6 37.99 35.42 -18 1 3 29.97 37.39 13 -3 12 -18.09 78.92 9 -1 6 35.48 55.31 -4 2 8 164.82 50.84 1 -2 -5 1588.63 67.80 12 -4 20 -7.17 129.63 7 -1 2 1476.47 50.64 -15 3 22 20.38 93.03 -12 3 19 123.36 86.05 14 -4 14 15.65 89.96 -2 2 18 45.03 91.21 -4 2 20 60.05 100.65 8 -1 17 88.65 105.80 -14 3 21 28.37 91.53 9 -1 12 302.42 82.65 -13 3 20 73.40 85.83 3 1 16 567.82 101.57 -8 2 6 15.40 32.42 3 1 10 10.34 72.39 11 -2 13 48.88 83.18 4 0 20 197.90 99.23 10 -3 21 145.80 123.82 2 1 19 69.15 106.80 0 1 21 -24.87 91.99 -16 3 15 34.48 55.62 13 -4 17 24.95 108.54 -11 2 27 -26.06 115.21 13 -3 10 30.60 72.09 -5 2 21 8.91 92.28 13 -3 8 67.58 58.76 -13 3 14 47.12 54.34 -12 3 17 178.27 74.91 -2 2 12 70.91 63.78 6 -1 21 96.61 120.41 -2 2 16 47.63 73.12 3 1 14 28.68 69.22 -12 3 15 31.42 63.18 -10 2 26 14.08 119.92 9 -2 19 78.98 112.12 -6 2 22 97.96 110.72 1 1 6 1327.23 64.46 -3 2 19 252.91 86.54 -16 3 21 129.27 87.09 -13 3 18 11.45 72.88 -2 2 14 92.94 75.02 -1 1 22 82.05 116.36 -9 2 25 41.97 117.92 11 -2 11 460.69 84.99 -3 -1 -4 368.00 49.59 -7 2 23 94.73 109.20 5 -4 -7 90.42 40.08 10 -2 16 39.29 100.00 -8 2 24 -47.35 112.92 -15 3 20 76.61 82.38 -14 3 19 63.74 80.36 12 -3 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8 20.23 81.99 2 -2 12 87.35 60.94 24 1 -5 86.09 71.39 15 -2 9 42.34 90.30 13 -2 7 31.72 71.70 6 -2 20 -24.28 100.95 23 -1 8 142.24 101.92 10 -2 6 9.65 79.05 4 -2 20 -6.67 90.37 24 2 -8 16.30 57.52 2 -2 18 68.92 78.94 12 -2 6 119.24 88.04 3 -2 19 95.38 85.53 1 -2 15 22.90 61.74 23 2 -9 73.76 53.22 14 -2 16 -72.60 115.73 8 -2 20 20.10 116.54 16 -2 12 20.16 107.03 12 -2 18 105.29 126.51 16 -2 10 99.01 103.50 10 1 -7 98.79 23.96 -1 2 -5 263.89 57.66 17 -1 0 45.96 74.88 23 -1 6 64.21 121.01 15 -2 15 67.82 111.31 -3 -1 8 -5.75 36.29 11 -2 19 74.01 121.06 8 -2 6 17.32 71.51 1 -2 19 92.81 77.42 1 -2 17 242.08 73.59 2 -2 20 54.58 83.32 16 -2 14 168.27 97.67 1 -2 13 32.55 58.71 15 -2 7 180.78 94.13 21 -1 2 246.63 97.81 -5 -1 10 -2.63 26.45 16 -2 8 31.73 89.32 5 -2 21 26.90 103.04 22 -1 3 7.67 96.74 10 -2 20 -8.50 115.89 14 -1 -1 32.16 59.05 17 -2 11 114.00 93.03 7 -2 21 161.06 111.88 20 -1 1 19.38 79.91 28 1 -3 32.24 93.50 29 1 -2 46.81 99.28 26 0 0 -0.64 91.79 14 -2 6 8.29 72.08 8 4 -12 54.92 32.05 17 -2 9 343.27 101.18 17 -2 13 346.21 116.62 18 2 -10 84.71 35.83 4 -2 8 67.98 62.86 11 -2 5 368.00 85.28 -12 1 9 18.31 40.31 23 -1 4 -4.29 99.47 24 -1 7 44.72 120.47 3 -2 9 317.12 68.75 3 -2 21 54.76 91.75 27 1 -4 72.31 87.90 3 -1 2 3982.29 71.32 30 1 -1 100.83 120.18 22 1 -7 55.41 55.72 16 -1 -1 11.46 70.44 23 1 -6 115.85 63.75 14 -2 18 137.32 123.92 9 -2 21 -12.28 125.76 15 -2 17 107.12 124.07 19 -1 0 35.51 84.38 13 -2 19 52.29 134.47 24 0 -2 66.34 82.94 16 -2 16 76.41 116.80 2 -2 10 118.68 59.84 18 -2 10 167.41 102.60 0 -2 16 46.10 62.71 18 -2 12 50.24 98.36 7 -1 0 37.86 57.95 24 -1 5 10.37 116.73 12 -2 20 25.33 122.56 17 -2 15 77.77 106.24 17 -2 7 128.60 85.62 6 -2 22 -34.00 110.69 28 0 2 -38.76 104.74 16 -2 6 20.07 89.67 16 2 -10 7.49 27.74 6 -2 6 61.65 54.05 1 3 -8 311.97 49.82 4 3 -9 57.89 34.77 26 1 -5 56.71 80.23 0 -2 14 65.09 57.43 18 -2 8 69.12 83.95 8 -2 22 -46.06 119.29 0 -2 20 56.91 77.65 1 -2 21 100.17 88.22 10 -1 -1 459.61 69.21 4 -2 22 113.93 104.18 18 -2 14 25.18 122.17 11 -2 21 52.83 133.22 20 2 -10 2.20 39.17 15 -2 5 237.09 81.94 0 -2 18 20.55 68.96 25 -1 6 90.93 125.43 22 0 -4 35.03 71.12 19 -2 11 52.87 114.69 12 -2 4 13.10 78.37 19 -2 9 185.73 109.11 -2 2 -4 46.34 49.06 23 -1 2 36.25 104.05 2 -2 22 -24.31 89.44 18 -1 -1 12.38 76.83 22 -1 1 103.97 99.78 19 -2 13 9.04 113.35 14 -2 4 32.79 78.18 17 1 -8 29.07 41.91 10 -2 22 10.51 132.52 24 -1 3 -70.47 110.66 10 -2 4 46.40 61.15 7 -2 5 1145.94 70.64 21 -1 0 110.21 91.27 18 -2 6 44.32 84.12 19 1 -8 106.05 46.00 17 -2 5 153.29 82.57 19 -2 7 234.29 86.65 20 -2 10 20.38 105.82 25 -1 4 65.12 100.60 28 0 0 101.10 113.74 5 -2 23 8.52 110.84 0 1 -3 95.19 33.69 25 1 -6 -6.15 71.28 -12 2 6 17.28 55.30 9 -2 23 95.52 137.12 -1 -2 19 147.52 68.60 20 -2 8 132.94 109.72 26 0 -2 65.01 91.38 16 -2 4 5.97 90.71 0 -2 12 -0.76 51.24 -1 -2 17 30.85 59.82 7 -2 23 36.85 119.70 30 1 -3 -28.85 105.58 15 -1 -2 388.27 72.88 20 -1 -1 21.80 83.73 -1 -2 15 31.90 55.01 22 2 -10 7.02 45.04 29 1 -4 59.42 95.29 17 -1 -2 504.23 76.45 13 -1 -2 69.77 59.89 13 -2 3 222.01 69.53 7 1 2 1625.22 85.71 5 1 8 813.71 80.42 -2 1 -9 1007.63 63.60 7 1 -2 385.55 48.28 2 1 13 654.52 73.89 3 1 12 718.24 78.89 0 1 15 640.81 76.45 11 2 -5 2106.53 59.50 3 2 17 605.95 94.06 14 3 -7 786.36 47.98 7 1 6 1241.70 78.07 1 1 -8 1176.25 51.93 -2 0 10 418.48 54.44 -4 0 12 648.76 50.35 -1 1 -8 1200.01 63.90 15 3 0 515.03 69.90 8 1 5 687.97 76.02 -10 0 0 489.63 60.65 16 4 -10 375.83 42.76 -16 0 12 555.10 40.63 -14 0 4 4138.49 103.20 -12 0 2 1021.48 71.12 -16 0 8 447.89 54.69 9 1 0 2082.99 81.02 -16 0 10 634.85 50.24 5 2 -11 390.37 29.94 13 2 1 781.55 75.28 3 3 -14 504.23 49.94 8 1 -3 1991.05 61.01 -14 0 6 1351.59 66.15 13 2 5 1208.44 93.56 2 1 -7 349.26 38.75 -1 2 -11 1040.05 64.57 10 1 3 1258.75 83.11 -4 0 14 577.04 53.04 6 1 13 645.67 81.99 13 3 -10 576.19 30.48 13 2 -5 428.02 45.21 -14 0 8 1454.57 58.85 2 0 10 2061.04 87.19 10 1 -1 474.93 64.40 18 3 -3 486.08 68.42 17 3 -6 374.18 54.01 4 0 8 764.41 78.46 15 2 3 642.83 85.42 11 1 0 415.30 60.40 -8 0 2 3748.03 82.79 -6 0 16 1567.67 64.63 -14 0 12 237.20 28.96 -12 0 6 1804.13 64.96 11 1 6 573.40 85.94 6 3 -13 413.89 34.43 15 2 -1 1885.76 87.40 4 0 10 580.79 72.22 -10 0 4 1510.10 64.88 11 1 10 547.90 82.78 2 0 14 1005.44 83.33 9 1 -4 1453.21 50.41 12 1 -1 428.70 64.45 2 2 -10 337.93 42.90 15 2 -5 619.03 53.17 6 0 10 653.34 79.15 0 0 16 1005.89 82.67 13 1 4 685.55 80.60 -12 0 8 687.67 44.33 13 2 -7 593.03 40.05 -6 0 2 1919.82 56.04 16 3 -9 786.17 46.24 17 2 -3 435.11 63.83 8 0 8 1667.90 100.66 8 0 4 2388.13 99.76 8 0 10 918.45 94.01 -10 0 16 389.39 31.52 -10 0 6 1526.79 54.14 12 1 -3 873.57 60.77 -8 0 4 2032.89 58.34 1 3 -12 731.65 55.89 8 0 2 878.10 85.16 3 1 -6 1308.13 33.14 10 0 6 496.73 70.13 10 0 8 1215.41 90.51 -12 0 10 339.52 31.81 10 0 4 1750.31 97.33 17 2 -5 1003.51 66.37 1 2 -9 1840.70 62.16 6 0 0 8686.69 103.82 15 1 0 870.65 73.69 10 0 2 1988.61 85.05 -14 1 5 451.84 63.84 0 3 -11 373.68 53.49 -10 1 1 480.29 56.97 -12 1 3 895.54 69.04 -16 1 9 576.92 62.93 12 0 2 2140.91 100.39 5 2 -9 1344.47 36.13 0 2 -8 479.99 51.97 10 0 0 489.44 65.17 17 2 -7 588.96 51.43 -10 0 8 1392.07 43.02 15 1 -4 626.68 59.39 2 -1 11 1301.64 81.62 3 -1 12 655.22 78.19 -14 1 7 626.37 59.13 1 -1 10 494.57 65.54 2 -1 9 1026.38 74.87 2 -1 13 690.93 76.48 5 -1 8 805.57 81.27 -1 -1 12 1022.64 65.15 -13 1 6 1014.06 65.67 14 1 -5 477.44 50.84 6 -1 13 646.49 84.63 1 -1 8 1079.23 71.85 -1 2 -7 3939.26 90.97 0 -1 15 643.11 72.34 -12 0 12 879.29 29.06 -8 0 6 3468.41 55.88 7 -1 6 1249.47 90.27 19 2 -7 628.03 60.32 11 2 -9 1454.05 28.59 16 0 2 1021.09 92.19 11 1 -6 942.02 42.32 8 0 -2 4079.03 84.91 8 -1 5 822.75 87.89 -3 -1 14 760.73 56.94 6 3 -11 465.44 35.33 4 3 -11 1328.40 53.44 6 0 -2 2036.06 56.72 13 1 -6 898.89 49.38 0 -1 7 683.58 64.94 12 0 -2 1002.89 72.97 -1 -1 8 1147.18 59.77 2 1 -5 4119.71 51.07 -14 1 9 405.04 52.76 9 -1 4 457.13 67.58 4 4 -12 500.77 48.10 -2 -1 9 1073.25 56.15 -16 1 13 675.42 51.27 14 0 -2 537.15 65.72 13 2 -9 771.13 32.35 10 -1 3 1361.46 89.32 4 2 -8 314.19 30.99 18 0 0 997.28 94.50 13 -1 4 748.45 78.82 17 1 -6 735.13 57.33 17 2 -9 295.35 39.61 20 1 -5 425.18 66.50 1 2 -7 719.07 53.34 7 -1 2 1606.77 83.50 -4 -1 11 1676.84 52.83 -6 -1 15 260.51 37.66 8 3 -11 397.41 26.76 -11 1 6 1069.29 61.98 6 4 -12 846.07 49.96 -6 -1 17 353.18 46.74 23 2 -7 502.27 70.79 14 1 -7 614.25 43.94 -6 1 1 4382.22 81.77 -9 1 4 1479.23 67.45 14 0 -4 4181.09 99.12 -8 1 3 1978.05 74.53 -4 -1 9 444.72 35.65 5 -2 11 1221.49 90.49 3 -2 13 694.00 77.09 -13 1 10 1121.56 55.68 -2 -1 7 404.65 45.11 2 3 -9 701.14 50.25 10 0 -4 1360.14 59.41 15 -1 0 909.42 85.03 3 -2 17 616.17 91.04 9 -1 0 2091.71 90.52 3 2 -7 396.89 37.80 18 0 -4 772.62 72.10 7 -2 7 1443.92 85.47 5 4 -11 279.42 44.81 20 0 -4 977.46 83.30 12 -1 -1 468.41 69.02 13 -2 5 1376.87 108.17 5 -2 7 1674.19 90.57 9 -2 5 1399.86 91.42 -13 2 7 596.07 64.88 1 -2 11 962.48 70.63 2 4 -10 767.85 58.58 -7 -1 14 846.13 34.65 8 0 -4 2030.22 57.67 -11 1 8 462.33 50.40 -2 -2 18 15.14 59.53 28 1 -5 51.50 89.25 0 3 -7 235.97 55.72 15 1 -8 3.93 33.71 2 -2 8 17.98 57.48 -1 -2 13 1087.29 66.45 24 1 -7 26.00 62.82 -14 1 13 71.67 37.81 -2 -2 16 36.08 56.92 14 2 -10 43.01 20.68 0 0 0 0.00 0.00 TITL pppp_twin1_hklf4 in Ia REM Ia (#9 in standard setting) CELL 0.71073 23.710091 8.459690 21.355331 90.0000 109.4864 90.0000 ZERR 9.00 0.001598 0.000706 0.001802 0.0000 0.0086 0.0000 LATT -2 SYMM x+1/2,-y, z SFAC C O Se Cs UNIT 108.00 90.00 9.00 9.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 51633 _olex2_submission_original_sample_id Cr6CsSe _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 1.227 _oxdiff_exptl_absorpt_empirical_full_min 0.879 _oxdiff_twin_integration_method simultaneous _oxdiff_twin_items 2 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 Cs1 Cs 0.64484(4) 0.13964(14) 0.36818(5) 0.0440(4) Uani 1 1 d D . . . . Se1 Se 0.68740(7) 0.8890(3) 0.56795(9) 0.0718(7) Uani 1 1 d . . . . . O4 O 0.6671(5) 0.2731(13) 0.2444(6) 0.052(3) Uani 1 1 d . . . . . O3 O 0.5932(4) 0.0064(13) 0.2171(5) 0.045(3) Uani 1 1 d . . . . . O6 O 0.5902(4) 0.4249(12) 0.4250(5) 0.052(3) Uani 1 1 d . . . . . O1 O 0.5182(4) 0.1477(14) 0.3943(5) 0.054(3) Uani 1 1 d . . . . . O2 O 0.5395(4) -0.0904(12) 0.3127(5) 0.049(3) Uani 1 1 d . . . . . O5 O 0.6419(4) 0.5097(13) 0.3255(5) 0.051(3) Uani 1 1 d . . . . . C3 C 0.5269(7) -0.161(2) 0.2497(8) 0.056(4) Uani 1 1 d . . . . . H3A H 0.493959 -0.104484 0.218152 0.067 Uiso 1 1 calc R U . . . H3B H 0.514116 -0.268837 0.251950 0.067 Uiso 1 1 calc R U . . . O10 O 0.7458(5) 0.9167(15) 0.6282(5) 0.078(4) Uani 1 1 d . . . . . C11 C 0.5368(8) 0.404(2) 0.4405(9) 0.066(5) Uani 1 1 d . . . . . H11A H 0.502897 0.442418 0.403905 0.079 Uiso 1 1 calc R U . . . H11B H 0.539187 0.465710 0.479624 0.079 Uiso 1 1 calc R U . . . C6 C 0.6536(7) 0.186(2) 0.1850(9) 0.058(5) Uani 1 1 d . . . . . H6A H 0.686551 0.196118 0.167970 0.069 Uiso 1 1 calc R U . . . H6B H 0.618360 0.231717 0.152352 0.069 Uiso 1 1 calc R U . . . C5 C 0.6425(6) 0.017(2) 0.1935(7) 0.058(4) Uani 1 1 d D . . . . H5A H 0.633406 -0.038191 0.151390 0.070 Uiso 1 1 calc R U . . . H5B H 0.677664 -0.031319 0.225061 0.070 Uiso 1 1 calc R U . . . C1 C 0.5037(7) -0.011(2) 0.3980(9) 0.056(4) Uani 1 1 d . . . . . H1A H 0.469511 -0.018796 0.413227 0.067 Uiso 1 1 calc R U . . . H1B H 0.537077 -0.065049 0.430052 0.067 Uiso 1 1 calc R U . . . C2 C 0.4897(6) -0.087(2) 0.3340(8) 0.057(4) Uani 1 1 d . . . . . H2A H 0.476395 -0.194619 0.336994 0.068 Uiso 1 1 calc R U . . . H2B H 0.457279 -0.030963 0.301669 0.068 Uiso 1 1 calc R U . . . C12 C 0.5279(8) 0.239(2) 0.4526(9) 0.058(4) Uani 1 1 d . . . . . H12A H 0.562771 0.198826 0.487446 0.069 Uiso 1 1 calc R U . . . H12B H 0.493630 0.228145 0.467516 0.069 Uiso 1 1 calc R U . . . C4 C 0.5780(7) -0.1615(17) 0.2251(7) 0.064(4) Uani 1 1 d D . . . . H4A H 0.567374 -0.216195 0.182772 0.077 Uiso 1 1 calc R U . . . H4B H 0.611917 -0.214983 0.256404 0.077 Uiso 1 1 calc R U . . . C10 C 0.5939(8) 0.5790(19) 0.4044(9) 0.061(5) Uani 1 1 d . . . . . H10A H 0.595726 0.652304 0.439942 0.073 Uiso 1 1 calc R U . . . H10B H 0.559007 0.604201 0.366424 0.073 Uiso 1 1 calc R U . . . O8 O 0.6321(7) 0.804(3) 0.5788(8) 0.163(8) Uani 1 1 d . . . . . C7 C 0.6802(6) 0.437(2) 0.2409(9) 0.046(4) Uani 1 1 d . . . . . H7A H 0.646819 0.486849 0.207282 0.055 Uiso 1 1 calc R U . . . H7B H 0.714990 0.446731 0.226835 0.055 Uiso 1 1 calc R U . . . C9 C 0.6486(7) 0.592(2) 0.3863(8) 0.062(5) Uani 1 1 d . . . . . H9A H 0.656909 0.702903 0.381123 0.074 Uiso 1 1 calc R U . . . H9B H 0.682235 0.548691 0.421640 0.074 Uiso 1 1 calc R U . . . C8 C 0.6916(7) 0.5207(17) 0.3023(8) 0.058(4) Uani 1 1 d D . . . . H8A H 0.726899 0.477059 0.335378 0.069 Uiso 1 1 calc R U . . . H8B H 0.699525 0.631009 0.295868 0.069 Uiso 1 1 calc R U . . . O11 O 0.7110(8) 1.316(2) 0.5346(7) 0.151(7) Uani 1 1 d . . . . . O7 O 0.6984(7) 0.832(5) 0.5089(9) 0.311(16) Uani 1 1 d . . . . . O9 O 0.6499(10) 1.049(3) 0.5460(14) 0.282(12) 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 Cs1 0.0426(5) 0.0427(6) 0.0482(7) 0.0002(8) 0.0174(5) 0.0004(7) Se1 0.0555(11) 0.114(2) 0.0461(12) 0.0003(15) 0.0173(10) -0.0112(13) O4 0.071(7) 0.042(6) 0.059(7) -0.002(6) 0.043(6) -0.001(6) O3 0.034(5) 0.048(6) 0.049(6) -0.017(6) 0.009(5) 0.000(5) O6 0.069(6) 0.028(5) 0.072(8) 0.002(6) 0.043(6) 0.021(5) O1 0.068(6) 0.041(6) 0.066(7) 0.011(6) 0.039(6) 0.015(6) O2 0.042(5) 0.039(7) 0.065(6) -0.005(6) 0.017(5) -0.007(5) O5 0.053(6) 0.046(7) 0.064(7) -0.009(6) 0.033(6) -0.008(5) C3 0.065(9) 0.031(11) 0.067(9) -0.007(8) 0.015(8) -0.006(8) O10 0.078(7) 0.088(11) 0.064(7) -0.023(8) 0.020(5) -0.013(7) C11 0.085(10) 0.053(9) 0.087(14) -0.017(10) 0.064(10) 0.004(9) C6 0.051(10) 0.072(10) 0.073(10) -0.026(8) 0.051(9) 0.001(8) C5 0.035(8) 0.066(9) 0.072(12) -0.023(9) 0.014(8) -0.001(8) C1 0.052(9) 0.048(8) 0.078(10) 0.019(9) 0.035(9) 0.007(8) C2 0.044(8) 0.045(11) 0.082(10) 0.010(8) 0.023(8) -0.002(8) C12 0.064(11) 0.065(9) 0.058(10) 0.008(8) 0.038(9) 0.010(8) C4 0.081(10) 0.038(8) 0.073(11) 0.008(9) 0.024(9) 0.021(8) C10 0.104(12) 0.025(7) 0.070(12) -0.006(9) 0.052(10) 0.019(9) O8 0.112(11) 0.26(2) 0.130(13) -0.021(14) 0.053(10) -0.086(13) C7 0.029(8) 0.043(7) 0.077(10) 0.010(8) 0.035(8) 0.009(7) C9 0.096(11) 0.037(9) 0.055(10) -0.004(8) 0.029(9) -0.004(9) C8 0.060(10) 0.039(9) 0.090(11) -0.001(8) 0.045(9) 0.002(8) O11 0.194(17) 0.145(17) 0.079(11) 0.031(13) 0.001(11) 0.007(13) O7 0.100(12) 0.70(5) 0.155(14) -0.25(2) 0.071(11) -0.15(2) O9 0.21(2) 0.21(2) 0.32(3) 0.12(2) -0.051(19) 0.064(15) 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' Cs Cs -0.3680 2.1192 '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' Se Se -0.0929 2.2259 '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 O4 Cs1 O3 52.4(3) . . ? O4 Cs1 O6 105.0(3) . . ? O4 Cs1 O1 125.1(3) . . ? O4 Cs1 O5 53.2(3) . . ? O4 Cs1 O10 82.3(3) . 2_646 ? O4 Cs1 C1 132.5(3) . . ? O4 Cs1 C9 73.5(3) . . ? O4 Cs1 C8 38.9(3) . . ? O4 Cs1 O11 86.7(3) . 2_646 ? O4 Cs1 O11 122.7(4) . 1_545 ? O3 Cs1 O5 95.2(3) . . ? O3 Cs1 C1 89.4(3) . . ? O3 Cs1 C9 115.7(3) . . ? O3 Cs1 C8 89.2(3) . . ? O3 Cs1 O11 132.4(3) . 2_646 ? O3 Cs1 O11 175.1(3) . 1_545 ? O6 Cs1 O3 125.3(3) . . ? O6 Cs1 O1 52.8(3) . . ? O6 Cs1 O5 53.2(3) . . ? O6 Cs1 O10 151.1(3) . 2_646 ? O6 Cs1 C1 72.4(3) . . ? O6 Cs1 C9 37.0(3) . . ? O6 Cs1 C8 72.8(3) . . ? O6 Cs1 O11 54.5(3) . 1_545 ? O6 Cs1 O11 84.1(3) . 2_646 ? O1 Cs1 O3 96.6(3) . . ? O1 Cs1 O5 95.4(3) . . ? O1 Cs1 C1 20.7(3) . . ? O1 Cs1 C9 87.3(3) . . ? O1 Cs1 C8 116.5(3) . . ? O1 Cs1 O11 129.6(3) . 2_646 ? O1 Cs1 O11 86.9(4) . 1_545 ? O2 Cs1 O4 104.5(3) . . ? O2 Cs1 O3 53.8(3) . . ? O2 Cs1 O6 104.3(3) . . ? O2 Cs1 O1 53.0(3) . . ? O2 Cs1 O5 124.2(3) . . ? O2 Cs1 O10 100.6(3) . 2_646 ? O2 Cs1 C1 37.9(3) . . ? O2 Cs1 C9 131.1(3) . . ? O2 Cs1 C8 133.6(3) . . ? O2 Cs1 O11 131.1(4) . 1_545 ? O2 Cs1 O11 163.4(3) . 2_646 ? O5 Cs1 C1 115.4(3) . . ? O5 Cs1 C9 21.3(3) . . ? O5 Cs1 C8 21.4(3) . . ? O5 Cs1 O11 72.3(3) . 2_646 ? O5 Cs1 O11 81.0(3) . 1_545 ? O10 Cs1 O3 81.5(3) 2_646 . ? O10 Cs1 O1 143.5(3) 2_646 . ? O10 Cs1 O5 121.2(3) 2_646 . ? O10 Cs1 C1 123.3(3) 2_646 . ? O10 Cs1 C9 126.5(3) 2_646 . ? O10 Cs1 C8 100.0(3) 2_646 . ? O10 Cs1 O11 97.8(4) 2_646 1_545 ? O10 Cs1 O11 68.3(4) 2_646 2_646 ? C1 Cs1 C9 107.9(3) . . ? C8 Cs1 C1 136.0(3) . . ? C8 Cs1 C9 36.7(3) . . ? O11 Cs1 C1 95.1(4) 1_545 . ? O11 Cs1 C1 137.9(4) 2_646 . ? O11 Cs1 C9 63.4(4) 2_646 . ? O11 Cs1 C9 60.8(4) 1_545 . ? O11 Cs1 C8 62.4(4) 2_646 . ? O11 Cs1 C8 86.1(4) 1_545 . ? O11 Cs1 O11 43.5(5) 2_646 1_545 ? O10 Se1 Cs1 36.3(4) . 2_666 ? O10 Se1 O8 119.9(8) . . ? O10 Se1 O9 111.5(11) . . ? O8 Se1 Cs1 154.4(6) . 2_666 ? O8 Se1 O9 91.3(12) . . ? O7 Se1 Cs1 91.4(8) . 2_666 ? O7 Se1 O10 113.5(8) . . ? O7 Se1 O8 111.9(11) . . ? O7 Se1 O9 105.7(18) . . ? O9 Se1 Cs1 92.3(10) . 2_666 ? C6 O4 Cs1 122.1(9) . . ? C6 O4 C7 116.5(13) . . ? C7 O4 Cs1 120.3(10) . . ? C5 O3 Cs1 104.4(7) . . ? C5 O3 C4 111.0(11) . . ? C4 O3 Cs1 104.1(7) . . ? C11 O6 Cs1 120.4(8) . . ? C10 O6 Cs1 121.1(8) . . ? C10 O6 C11 110.2(12) . . ? C1 O1 Cs1 104.5(8) . . ? C1 O1 C12 116.3(13) . . ? C12 O1 Cs1 106.1(9) . . ? C3 O2 Cs1 121.4(8) . . ? C2 O2 Cs1 121.8(9) . . ? C2 O2 C3 112.7(11) . . ? C9 O5 Cs1 103.3(8) . . ? C8 O5 Cs1 102.5(8) . . ? C8 O5 C9 115.3(11) . . ? O2 C3 H3A 108.8 . . ? O2 C3 H3B 108.8 . . ? O2 C3 C4 114.0(12) . . ? H3A C3 H3B 107.7 . . ? C4 C3 H3A 108.8 . . ? C4 C3 H3B 108.8 . . ? Se1 O10 Cs1 126.8(6) . 2_666 ? O6 C11 H11A 109.5 . . ? O6 C11 H11B 109.5 . . ? O6 C11 C12 110.7(13) . . ? H11A C11 H11B 108.1 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? O4 C6 H6A 109.0 . . ? O4 C6 H6B 109.0 . . ? O4 C6 C5 113.0(14) . . ? H6A C6 H6B 107.8 . . ? C5 C6 H6A 109.0 . . ? C5 C6 H6B 109.0 . . ? Cs1 C5 H5A 162.3 . . ? Cs1 C5 H5B 73.1 . . ? O3 C5 Cs1 54.6(6) . . ? O3 C5 C6 107.6(12) . . ? O3 C5 H5A 110.2 . . ? O3 C5 H5B 110.2 . . ? C6 C5 Cs1 84.9(9) . . ? C6 C5 H5A 110.2 . . ? C6 C5 H5B 110.2 . . ? H5A C5 H5B 108.5 . . ? Cs1 C1 H1A 162.1 . . ? Cs1 C1 H1B 73.8 . . ? O1 C1 Cs1 54.8(7) . . ? O1 C1 H1A 109.4 . . ? O1 C1 H1B 109.4 . . ? O1 C1 C2 111.0(15) . . ? H1A C1 H1B 108.0 . . ? C2 C1 Cs1 85.9(9) . . ? C2 C1 H1A 109.4 . . ? C2 C1 H1B 109.4 . . ? O2 C2 C1 111.3(13) . . ? O2 C2 H2A 109.4 . . ? O2 C2 H2B 109.4 . . ? C1 C2 H2A 109.4 . . ? C1 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? Cs1 C12 H12A 73.9 . . ? Cs1 C12 H12B 160.4 . . ? O1 C12 Cs1 53.4(7) . . ? O1 C12 C11 110.9(15) . . ? O1 C12 H12A 109.5 . . ? O1 C12 H12B 109.5 . . ? C11 C12 Cs1 87.5(9) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 108.0 . . ? Cs1 C4 H4A 162.8 . . ? Cs1 C4 H4B 74.7 . . ? O3 C4 Cs1 54.1(6) . . ? O3 C4 H4A 110.3 . . ? O3 C4 H4B 110.3 . . ? C3 C4 Cs1 83.3(8) . . ? C3 C4 O3 107.2(12) . . ? C3 C4 H4A 110.3 . . ? C3 C4 H4B 110.3 . . ? H4A C4 H4B 108.5 . . ? O6 C10 H10A 110.1 . . ? O6 C10 H10B 110.1 . . ? O6 C10 C9 108.0(13) . . ? H10A C10 H10B 108.4 . . ? C9 C10 H10A 110.1 . . ? C9 C10 H10B 110.1 . . ? O4 C7 H7A 108.7 . . ? O4 C7 H7B 108.7 . . ? O4 C7 C8 114.1(14) . . ? H7A C7 H7B 107.6 . . ? C8 C7 H7A 108.7 . . ? C8 C7 H7B 108.7 . . ? Cs1 C9 H9A 161.4 . . ? Cs1 C9 H9B 71.6 . . ? O5 C9 Cs1 55.4(7) . . ? O5 C9 C10 111.0(14) . . ? O5 C9 H9A 109.4 . . ? O5 C9 H9B 109.4 . . ? C10 C9 Cs1 87.6(9) . . ? C10 C9 H9A 109.4 . . ? C10 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? Cs1 C8 H8A 72.3 . . ? Cs1 C8 H8B 162.7 . . ? O5 C8 Cs1 56.1(6) . . ? O5 C8 C7 111.1(12) . . ? O5 C8 H8A 109.4 . . ? O5 C8 H8B 109.4 . . ? C7 C8 Cs1 86.0(9) . . ? C7 C8 H8A 109.4 . . ? C7 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? Cs1 O11 Cs1 113.4(5) 2_666 1_565 ? 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 Cs1 O4 3.076(10) . ? Cs1 O3 3.246(9) . ? Cs1 O6 3.166(9) . ? Cs1 O1 3.231(9) . ? Cs1 O2 3.075(9) . ? Cs1 O5 3.254(11) . ? Cs1 O10 3.187(11) 2_646 ? Cs1 C1 3.829(15) . ? Cs1 C9 3.847(17) . ? Cs1 C8 3.827(13) . ? Cs1 O11 3.672(17) 2_646 ? Cs1 O11 3.688(16) 1_545 ? Se1 O10 1.562(11) . ? Se1 O8 1.581(14) . ? Se1 O7 1.452(17) . ? Se1 O9 1.60(2) . ? O4 C6 1.407(18) . ? O4 C7 1.430(17) . ? O3 C5 1.422(15) . ? O3 C4 1.489(17) . ? O6 C11 1.422(16) . ? O6 C10 1.388(17) . ? O1 C1 1.397(19) . ? O1 C12 1.415(19) . ? O2 C3 1.408(17) . ? O2 C2 1.400(15) . ? O5 C9 1.435(16) . ? O5 C8 1.428(14) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C3 C4 1.472(19) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 C12 1.45(2) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 C5 1.48(2) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C1 C2 1.45(2) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 C9 1.475(19) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 C8 1.43(2) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? 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 Cs1 O4 C6 C5 -14.1(16) . . . . ? Cs1 O4 C7 C8 9.9(16) . . . . ? Cs1 O3 C5 C6 -70.1(13) . . . . ? Cs1 O3 C4 C3 68.0(11) . . . . ? Cs1 O6 C11 C12 22.9(19) . . . . ? Cs1 O6 C10 C9 -29.2(17) . . . . ? Cs1 O1 C1 C2 -68.6(13) . . . . ? Cs1 O1 C12 C11 69.9(14) . . . . ? Cs1 O2 C3 C4 20.6(18) . . . . ? Cs1 O2 C2 C1 -21.1(17) . . . . ? Cs1 O5 C9 C10 -71.4(13) . . . . ? Cs1 O5 C8 C7 69.6(13) . . . . ? Cs1 C1 C2 O2 14.3(12) . . . . ? O4 C6 C5 Cs1 9.5(11) . . . . ? O4 C6 C5 O3 59.9(17) . . . . ? O4 C7 C8 Cs1 -6.9(11) . . . . ? O4 C7 C8 O5 -58.1(17) . . . . ? O6 C11 C12 Cs1 -16.0(13) . . . . ? O6 C11 C12 O1 -65.0(19) . . . . ? O6 C10 C9 Cs1 20.2(12) . . . . ? O6 C10 C9 O5 71.5(17) . . . . ? O1 C1 C2 O2 64.0(18) . . . . ? O2 C3 C4 Cs1 -13.9(12) . . . . ? O2 C3 C4 O3 -63.0(17) . . . . ? C3 O2 C2 C1 -178.7(14) . . . . ? C11 O6 C10 C9 -177.7(14) . . . . ? C6 O4 C7 C8 178.0(12) . . . . ? C5 O3 C4 Cs1 111.8(10) . . . . ? C5 O3 C4 C3 179.8(11) . . . . ? C1 O1 C12 Cs1 115.7(12) . . . . ? C1 O1 C12 C11 -174.4(13) . . . . ? C2 O2 C3 C4 178.3(13) . . . . ? C12 O1 C1 Cs1 -116.6(13) . . . . ? C12 O1 C1 C2 174.8(13) . . . . ? C4 O3 C5 Cs1 -111.6(10) . . . . ? C4 O3 C5 C6 178.3(13) . . . . ? C10 O6 C11 C12 171.6(16) . . . . ? O8 Se1 O10 Cs1 -167.2(10) . . . 2_666 ? C7 O4 C6 C5 178.0(12) . . . . ? C9 O5 C8 Cs1 111.5(12) . . . . ? C9 O5 C8 C7 -178.9(13) . . . . ? C8 O5 C9 Cs1 -111.0(11) . . . . ? C8 O5 C9 C10 177.6(13) . . . . ? O7 Se1 O10 Cs1 56.9(19) . . . 2_666 ? O9 Se1 O10 Cs1 -62.4(14) . . . 2_666 ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined _oxdiff_twin_reflns_isolated _oxdiff_twin_reflns_overlapped _twin_individual_twin_lattice_type _twin_individual_twin_matrix_11 _twin_individual_twin_matrix_12 _twin_individual_twin_matrix_13 _twin_individual_twin_matrix_21 _twin_individual_twin_matrix_22 _twin_individual_twin_matrix_23 _twin_individual_twin_matrix_31 _twin_individual_twin_matrix_32 _twin_individual_twin_matrix_33 1 0.9182 6916 2106 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 2 0.0818 7058 2106 nmt -0.9823 -0.0285 0.0472 -0.0035 1.0048 -0.0005 -0.0455 0.0055 -1.0012