#------------------------------------------------------------------------------ #$Date: 2024-08-17 04:50:03 +0300 (Sat, 17 Aug 2024) $ #$Revision: 294162 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/32/2023238.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_2023238 loop_ _publ_author_name 'Song, Xueqing' 'Li, William' 'Torres, Yolanda' 'Greaves, Tazena' _publ_section_title ; Crystal structure of (1,4,7,10,13,16-hexaoxacyclooctadecane-\k6 O)potassium-\m-oxalato-triphenylstannate(IV), the first reported 18-crown-6-stabilized potassium salt of triphenyloxalatostannate ; _journal_coeditor_code NY2007 _journal_issue 9 _journal_name_full 'Acta Crystallographica Section E Crystallographic Communications' _journal_paper_doi 10.1107/S2056989024007758 _journal_volume 80 _journal_year 2024 _chemical_formula_iupac '[K Sn (C6 H5)3 (C2 O4) (C12 H24 O6)]' _chemical_formula_moiety 'C32 H39 K O10 Sn' _chemical_formula_sum 'C32 H39 K O10 Sn' _chemical_formula_weight 741.42 _chemical_name_systematic (1,4,7,10,13,16-Hexaoxacyclooctadecane-1\k^6^O)(\m-oxalato-1\k^2^O^1^,O^2^:2\k^2^O^1'^,O^2'^)triphenyl-2\k^3^C-potassium(I)tin(IV) _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_method ; FinalCif V138 by Daniel Kratzert, Freiburg 2024, https://dkratzert.de/finalcif.html ; _cell_angle_alpha 90 _cell_angle_beta 97.925(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 9.4060(3) _cell_length_b 19.3779(4) _cell_length_c 9.4225(3) _cell_measurement_reflns_used 9822 _cell_measurement_temperature 100.00(10) _cell_measurement_theta_max 31.0600 _cell_measurement_theta_min 2.8560 _cell_volume 1701.02(8) _computing_cell_refinement ; CrysAlisPro 1.171.42.62a (Rigaku OD, 2022) ; _computing_data_collection ; CrysAlisPro 1.171.42.62a (Rigaku OD, 2022) ; _computing_data_reduction ; CrysAlisPro 1.171.42.62a (Rigaku OD, 2022) ; _computing_molecular_graphics ; Olex2 1.5-beta (Dolomanov et al., 2009) ; _computing_publication_material ; Olex2 1.5-beta (Dolomanov et al., 2009) ; _computing_structure_refinement ; SHELXL2018/3 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 100.15 _diffrn_detector 'hybrid photon counting' _diffrn_detector_area_resol_mean 10.0000 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.987 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Rigaku XtaLAB Synergy-S dual wavelength Mo/Cu' _diffrn_measurement_method '\w scans' _diffrn_measurement_specimen_support 'MiTeGen micromount' _diffrn_radiation_monochromator 'mirror optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0396 _diffrn_reflns_av_unetI/netI 0.0498 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 15412 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.484 _diffrn_reflns_theta_min 2.869 _diffrn_source 'microfocus sealed X-ray tube' _exptl_absorpt_coefficient_mu 0.926 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.91248 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (CrysAlis PRO; Rigaku OD, 2022) ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.448 _exptl_crystal_description block _exptl_crystal_F_000 760 _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.055 _exptl_crystal_size_min 0.032 _exptl_crystal_size_rad 0.021 _refine_diff_density_max 1.280 _refine_diff_density_min -0.520 _refine_ls_abs_structure_details ; Flack x determined using 2807 quotients [(I^+^)-(I^-^)]/[(I^+^)+(I^-^)] (Parsons et al., 2013) ; _refine_ls_abs_structure_Flack -0.08(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 398 _refine_ls_number_reflns 7113 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.077 _refine_ls_R_factor_all 0.0368 _refine_ls_R_factor_gt 0.0327 _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^)+(0.0708P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0848 _refine_ls_wR_factor_ref 0.1049 _reflns_number_gt 6792 _reflns_number_total 7113 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ny2007.cif _cod_data_source_block I _cod_database_code 2023238 _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_hkl_file ; 0 -20 3 17.6829 2.04008 4 0 -19 3 28.8722 2.35547 4 0 -19 -4 61.3677 2.22162 2 0 -19 4 66.0554 3.46278 4 0 -18 -3 31.6235 1.37317 2 0 -18 3 36.3121 2.47715 4 0 -18 -4 22.1481 1.26854 2 0 -18 4 20.8288 2.04782 4 0 -18 -5 16.1934 1.32199 2 0 -18 5 17.0863 2.03697 4 0 -18 -6 5.26157 1.10419 2 0 -18 -8 4.45762 1.78818 4 0 -17 -3 155.613 4.42735 2 0 -17 3 161.901 5.70056 4 0 -17 -4 49.0050 2.02336 2 0 -17 4 51.9362 2.98286 4 0 -17 5 51.1340 2.94529 4 0 -17 -5 44.8826 2.09018 2 0 -17 -6 52.6868 2.44303 2 0 -17 -7 23.9272 1.81169 2 0 -17 -8 24.0493 2.58578 4 0 -16 -2 52.2011 1.81521 2 0 -16 -3 44.6039 1.76373 2 0 -16 3 46.8581 2.68633 4 0 -16 -4 25.7271 1.42746 2 0 -16 4 26.0387 2.10434 4 0 -16 5 10.7882 1.66284 4 0 -16 -5 13.3501 1.27549 2 0 -16 6 11.4589 1.83215 4 0 -16 -6 11.0696 1.29069 2 0 -16 -7 5.11644 1.19550 2 0 -16 -8 13.1761 2.06864 4 0 -16 -8 10.1636 1.55731 2 0 -16 -9 18.8570 2.38525 4 0 -15 -2 102.642 3.03831 2 0 -15 -3 27.9791 1.37658 2 0 -15 3 30.0016 2.13205 4 0 -15 4 66.6471 3.21650 4 0 -15 -4 63.9091 2.43402 2 0 -15 5 36.9308 2.51137 4 0 -15 -5 35.3994 1.83327 2 0 -15 6 58.1974 3.24861 4 0 -15 -6 58.7014 2.59343 2 0 -15 -7 23.0649 1.78054 2 0 -15 -8 19.4822 2.27311 4 0 -15 -8 15.7302 1.71166 2 0 -15 -9 22.4817 2.59644 4 0 -14 -2 81.3367 2.53987 2 0 -14 -3 43.4874 1.74361 2 0 -14 3 42.3190 2.41012 4 0 -14 4 21.5771 1.83742 4 0 -14 -4 18.2119 1.27656 2 0 -14 5 29.5989 2.17531 4 0 -14 -5 26.2555 1.61750 2 0 -14 6 35.3801 2.47030 4 0 -14 -6 29.9759 1.90570 2 0 -14 7 7.06898 1.55577 4 0 -14 -7 5.73605 1.57449 4 0 -14 -7 7.73760 1.30947 2 0 -14 -8 3.42212 1.59439 4 0 -14 -8 6.75803 1.41403 2 0 -14 -9 11.5388 2.12597 4 0 -14 -9 13.6166 1.80081 2 0 -13 -2 41.7891 1.59348 2 0 -13 3 99.7684 3.78684 4 0 -13 -3 90.4232 2.95660 2 0 -13 4 119.143 4.43837 4 0 -13 -4 116.841 3.74209 2 0 -13 5 64.0339 3.10159 4 0 -13 -5 58.5454 2.50184 2 0 -13 6 55.3715 3.07099 4 0 -13 -6 55.4531 2.55886 2 0 -13 -7 45.2724 2.85134 4 0 -13 7 41.8217 2.74176 4 0 -13 -7 43.4690 2.42390 2 0 -13 -8 33.1718 2.69161 4 0 -13 -8 33.7047 2.31419 2 0 -13 -9 17.4414 2.22560 4 0 -13 -9 16.5896 1.89735 2 0 -13 -10 10.6256 2.13714 4 0 -12 -1 57.6702 1.86225 2 0 -12 -2 163.956 4.52333 2 0 -12 3 23.2153 1.69348 4 0 -12 -3 23.2458 1.23953 2 0 -12 4 34.2830 2.12029 4 0 -12 -4 30.3450 1.57580 2 0 -12 5 72.7380 3.29649 4 0 -12 -5 71.3871 2.79971 2 0 -12 6 95.5737 4.00914 4 0 -12 -6 86.1761 3.41467 2 0 -12 7 8.50403 1.60418 4 0 -12 -7 5.82121 1.19201 2 0 -12 -7 6.74165 1.42248 4 0 -12 -8 5.41460 1.51331 4 0 -12 -8 3.58542 1.27711 2 0 -12 -9 21.6439 2.35485 4 0 -12 -9 21.1555 2.05101 2 0 -12 -10 8.80028 2.08479 4 0 -11 -1 11.0493 0.69600 2 0 -11 -2 40.3432 1.53810 2 0 -11 3 86.4528 3.31129 4 0 -11 -3 79.2893 2.67793 2 0 -11 4 130.519 4.64338 4 0 -11 -4 134.018 4.13268 2 0 -11 5 92.6531 3.69081 4 0 -11 -5 83.4559 3.18445 2 0 -11 6 21.9489 1.94669 4 0 -11 -6 22.3911 1.66421 2 0 -11 7 25.6534 2.14352 4 0 -11 -7 25.4766 2.11774 4 0 -11 -7 25.6547 1.88624 2 0 -11 8 27.9955 2.31013 4 0 -11 -8 32.7247 2.57319 4 0 -11 -8 30.6550 2.16816 2 0 -11 -9 28.3837 2.57851 4 0 -11 -9 25.5871 2.20330 2 0 -11 -10 8.69960 2.04451 4 0 -10 -1 201.385 5.24431 2 0 -10 -2 62.0817 2.05193 2 0 -10 3 0.19502 0.66787 4 0 -10 -3 66.7005 1.71050 2 0 -10 4 44.1434 2.25616 4 0 -10 -4 40.8086 1.87938 2 0 -10 5 80.1887 3.39808 4 0 -10 -5 71.3612 2.88482 2 0 -10 6 39.3455 2.37142 4 0 -10 -6 36.7555 2.06226 2 0 -10 7 22.2204 1.97631 4 0 -10 -7 19.7260 1.96468 4 0 -10 -8 16.2723 1.92356 4 0 -10 8 16.9351 1.93403 4 0 -10 -9 4.74637 1.67848 4 0 -10 -10 25.5333 2.62765 4 0 -9 -1 150.420 4.00979 2 0 -9 -2 61.4304 2.03253 2 0 -9 -3 91.7176 2.94876 2 0 -9 4 92.1748 3.54949 4 0 -9 -4 97.8176 3.23813 2 0 -9 5 70.1393 3.04775 4 0 -9 6 162.263 5.31106 4 0 -9 -6 133.386 5.12476 4 0 -9 7 23.9730 2.07443 4 0 -9 -7 25.5235 2.15470 4 0 -9 -8 29.3956 2.42019 4 0 -9 8 30.1217 2.38332 4 0 -9 -9 19.0157 2.20021 4 0 -9 -10 7.54778 1.88154 4 0 -8 -1 194.280 5.01523 2 0 -8 -2 220.945 5.96743 1 0 -8 -2 215.250 5.74158 2 0 -8 -3 45.2233 1.73691 1 0 -8 -3 45.5346 1.79530 2 0 -8 6 42.5642 2.43472 4 0 -8 7 2.95518 1.19337 4 0 -8 8 7.67293 1.54124 4 0 -8 -10 4.59090 1.80210 4 0 -8 -11 15.9113 2.44309 4 0 -7 -1 17.8039 0.78993 2 0 -7 -1 17.4746 1.08022 1 0 -7 -2 206.510 5.57178 1 0 -7 -2 205.366 5.47289 2 0 -7 -3 99.9541 2.98148 1 0 -7 -4 81.0307 2.43560 1 0 -7 -7 37.3687 1.15909 3 0 -7 8 59.5928 3.12635 4 0 -7 -8 58.9075 1.76614 3 0 -7 -9 17.6013 0.85074 3 0 -6 -1 261.233 6.91154 1 0 -6 -1 266.805 6.63318 2 0 -6 -2 188.161 5.01862 1 0 -6 -2 185.603 4.98469 2 0 -6 -3 20.2367 0.93655 1 0 -6 -4 56.1080 1.73610 1 0 -6 -5 27.0434 0.87097 3 0 -6 -6 26.7796 0.98523 3 0 -6 -7 3.90830 0.51040 3 0 -6 -8 29.5271 1.24896 3 0 -6 -9 3.84447 0.65271 3 0 -5 0 0.24602 0.52160 1 0 -5 0 0.18335 0.28191 2 0 -5 -1 153.652 4.18620 1 0 -5 -1 155.064 3.99433 2 0 -5 -2 43.8409 1.49374 1 0 -5 -3 162.240 4.23631 1 0 -5 -4 66.5104 1.88700 1 0 -5 -8 53.9835 1.98543 3 0 -5 -9 19.3483 1.19449 3 0 -5 -10 8.61612 0.93373 3 0 -4 0 327.080 8.14598 1 0 -4 0 321.903 7.86066 2 0 -4 -1 375.848 9.36637 1 0 -4 -1 379.771 9.26220 2 0 -4 -2 114.686 3.06633 1 0 -4 -3 11.3630 0.53240 1 0 -4 -4 60.4380 1.65861 1 0 -4 -9 39.1154 1.80910 3 0 -4 -10 19.4408 1.37067 3 0 -3 0-0.11552 0.31443 1 0 -3 -1 97.6231 2.59505 1 0 -3 1 95.7279 2.73104 4 0 -3 -2 265.361 6.56635 1 0 -3 2 272.107 6.98755 4 0 -3 -3 39.1625 1.15142 1 0 -3 -3 45.4101 1.80220 4 0 -3 3 41.6920 1.74890 4 0 -3 -4 173.255 5.20008 4 0 -3 -5 71.2706 2.89375 4 0 -3 -6 90.7160 3.62433 4 0 -3 -7 57.3716 3.03567 4 0 -3 -8 31.9362 2.41498 4 0 -3 -10 7.57287 1.08732 3 0 -2 -1 639.196 15.3052 1 0 -2 -3 72.3640 2.50610 4 0 -2 -4 119.998 3.88661 4 0 -2 -5 51.2786 2.28121 4 0 -2 -5 40.8012 1.22132 1 0 -2 -6 10.1561 0.43992 1 0 -2 -6 11.7078 0.45540 1 0 -2 6 14.9239 1.30574 4 0 -2 -6 15.5504 1.49292 4 0 -2 7 27.6264 1.94314 4 0 -2 -7 25.3239 1.98134 4 0 -2 8 17.1845 1.75870 4 0 -2 -8 19.7805 1.94803 4 0 -2 -9 18.6425 2.10679 4 0 -2 -10 18.3679 2.20095 4 0 -2 -10 13.9354 1.34370 3 0 -2 -11 5.77983 1.96750 4 0 -1 -2 701.127 17.1626 4 0 -1 -3 251.884 6.77342 4 0 -1 -4 206.647 5.98513 4 0 -1 -5 122.785 4.21071 4 0 -1 -6 130.507 2.64826 1 0 -1 -6 140.185 4.18102 4 0 -1 -7 90.5947 2.58106 1 0 -1 -7 98.0822 2.58277 1 0 -1 -7 103.440 4.07026 4 0 -1 7 101.750 3.84442 4 0 -1 -8 32.6208 0.99855 1 0 -1 -8 30.0141 0.97444 1 0 -1 8 40.4922 2.43003 4 0 -1 -8 39.9269 2.54349 4 0 -1 9 18.1313 1.85444 4 0 -1 -9 19.5955 2.13932 4 0 -1 -10 17.3740 2.15418 4 0 -1 -11 5.90812 1.82827 4 0 0 -2 71.3759 2.23784 4 0 0 -3 25.0434 1.29275 4 0 0 -4 63.6457 2.51222 4 0 0 -5 130.233 4.38550 4 0 0 -6 40.7340 1.10836 1 0 0 -6 55.6286 2.41122 4 0 0 -7 27.7382 1.13831 1 0 0 -7 36.3982 2.26238 4 0 0 7 30.7356 1.94693 4 0 0 -8 15.9678 0.79074 1 0 0 -8 14.9417 1.75478 4 0 0 8 16.0360 1.62617 4 0 0 -9 7.42401 0.51250 1 0 0 -9 7.57775 0.52240 1 0 0 -9 11.3428 1.76346 4 0 0 -10 16.4144 2.28075 4 0 0 -11 56.9134 3.66400 4 0 0 -11 55.1755 2.79469 3 0 1 -2 695.042 17.0288 4 0 1 -3 242.140 6.58407 4 0 1 -4 204.838 5.92196 4 0 1 -5 114.326 3.29909 1 0 1 -5 126.922 4.14225 4 0 1 -6 138.387 2.95281 1 0 1 -6 133.528 4.07679 4 0 1 -7 101.406 3.01516 1 0 1 -7 104.569 4.15082 4 0 1 -8 41.9068 1.56129 1 0 1 -8 41.3945 2.70874 4 0 1 -9 16.5707 0.88585 1 0 1 -9 19.0132 2.14109 4 0 1 -10 12.4164 0.70409 1 0 1 -10 14.7726 0.72842 1 0 1 -10 17.6472 2.24951 4 0 1 -11 2.41324 1.80979 4 0 1 -11 3.19642 1.23277 3 0 2 -1 680.061 16.4642 4 0 2 -2 197.005 5.27286 4 0 2 -3 67.9098 2.40749 4 0 2 -4 125.085 4.06412 4 0 2 -5 44.6034 1.71524 1 0 2 -5 52.6601 2.38535 4 0 2 -6 14.6576 0.91845 1 0 2 -6 17.0923 1.57231 4 0 2 -7 26.4005 1.25547 1 0 2 -7 27.2105 2.05021 4 0 2 -8 17.5969 1.03652 1 0 2 -8 18.8941 1.93268 4 0 2 -9 16.6021 1.00602 1 0 2 -9 16.6577 2.02379 4 0 2 -10 14.5302 0.89366 1 0 2 -10 15.9610 2.06860 4 0 2 -11 6.00153 1.94041 4 0 2 -11 5.16715 1.37413 3 0 3 -2 297.946 7.43108 4 0 3 2 279.976 6.97698 1 0 3 -3 48.1044 1.93688 4 0 3 3 46.6849 1.30360 1 0 3 -4 177.891 4.86446 1 0 3 -4 172.356 5.28757 4 0 3 -5 76.8655 2.56113 1 0 3 -5 80.5623 3.14011 4 0 3 -6 93.9676 3.00896 1 0 3 -6 93.4030 3.74806 4 0 3 -7 65.8025 2.34217 1 0 3 -7 60.7630 3.13014 4 0 3 -8 36.2416 1.64154 1 0 3 -8 39.3077 2.66380 4 0 3 -9 13.9164 1.04872 1 0 3 -9 13.1945 1.83390 4 0 3 -10 8.73702 1.85371 4 0 3 -10 6.21378 0.81575 1 0 3 -11 9.36142 2.00262 4 0 4 -2 106.913 3.02754 1 0 4 -2 104.409 3.11167 4 0 4 2 93.5129 2.69911 1 0 4 -3 12.4295 0.86778 1 0 4 -3 11.9752 1.03047 4 0 4 3 12.1505 0.57247 1 0 4 -4 62.5561 2.30733 1 0 4 -4 71.4184 2.70608 4 0 4 -5 68.2549 2.43575 1 0 4 -5 68.4768 2.88717 4 0 4 -6 35.9879 1.67003 1 0 4 -6 36.6941 2.20639 4 0 4 -7 8.74388 0.90865 1 0 4 -7 8.65173 1.41628 4 0 4 -8 16.6848 1.18569 1 0 4 -8 17.9785 1.89430 4 0 4 -9 40.5377 1.84757 1 0 4 -9 42.6053 2.87271 4 0 4 -10 23.4974 2.50966 4 0 4 -10 19.2143 1.28833 1 0 4 -11 14.2326 2.26196 4 0 5 0-0.10533 0.31332 2 0 5 0 0.05519 0.49808 1 0 5 1 152.358 3.91430 3 0 5 -2 50.7139 1.88844 1 0 5 2 50.5642 1.63765 1 0 5 -3 161.613 4.69448 1 0 5 -3 168.159 4.88087 4 0 5 3 162.604 4.27547 1 0 5 -4 75.4548 2.58297 1 0 5 -4 74.1451 2.80347 4 0 5 4 69.5354 2.01534 1 0 5 -5 86.2910 2.92282 1 0 5 -5 79.2939 3.25488 4 0 5 -6 68.4433 2.55309 1 0 5 -6 63.1663 3.00666 4 0 5 -7 74.0018 2.77294 1 0 5 -7 74.1764 3.47405 4 0 5 -8 57.8699 2.41653 1 0 5 -8 57.8587 3.22102 4 0 5 -9 21.5026 1.43256 1 0 5 -9 24.3682 2.32228 4 0 5 -10 6.19765 1.71008 4 0 5 -10 9.41606 1.09132 1 0 5 -11 4.67801 1.93833 4 0 6 0 87.3129 2.39011 2 0 6 1 253.511 6.40979 3 0 6 1 254.257 6.38138 2 0 6 -2 194.657 5.42709 1 0 6 2 190.357 5.11373 1 0 6 -3 22.6609 1.34423 1 0 6 -3 23.6329 1.42239 4 0 6 3 22.8920 1.01728 1 0 6 -4 60.3424 2.33496 1 0 6 -4 56.0235 2.48504 4 0 6 4 58.2373 1.81001 1 0 6 -5 32.8690 1.69564 1 0 6 -5 36.0512 2.05374 4 0 6 -6 29.6445 1.65906 1 0 6 -6 31.4194 2.06332 4 0 6 -7 3.78458 0.87554 1 0 6 -7 4.58393 1.22261 4 0 6 -8 30.0565 1.75426 1 0 6 -8 32.5853 2.42285 4 0 6 -9 4.97616 1.51694 4 0 6 -9 4.52778 0.95158 1 0 6 -10 24.0215 1.58073 1 0 6 -10 24.9993 2.49863 4 0 6 -11 10.6926 2.16995 4 0 7 0 0.04809 0.32275 2 0 7 1 17.9804 0.80169 2 0 7 -2 198.964 5.64130 1 0 7 2 192.568 5.34370 1 0 7 2 198.243 4.96614 3 0 7 -3 112.346 3.68151 1 0 7 3 111.502 3.27474 1 0 7 -4 80.9827 3.00738 1 0 7 -4 83.9825 3.19127 4 0 7 4 84.0982 2.51070 1 0 7 -5 66.8723 2.72556 1 0 7 -5 69.3600 3.02124 4 0 7 5 72.5708 2.11625 1 0 7 -6 83.1333 3.10434 1 0 7 -6 78.3649 3.45383 4 0 7 -7 43.8772 2.16860 1 0 7 -7 43.7807 2.59008 4 0 7 -8 67.0476 2.80555 1 0 7 -8 62.9860 3.40066 4 0 7 -9 20.9062 1.55769 1 0 7 -9 20.8144 2.22343 4 0 7 -10 18.4220 1.53749 1 0 7 -10 21.4972 2.38317 4 0 7 -11 3.34515 1.79180 4 0 8 0 510.843 12.4996 2 0 8 -1 179.584 4.80244 2 0 8 1 168.489 5.07881 1 0 8 1 184.871 4.71165 2 0 8 1 182.571 4.85003 3 0 8 2 218.889 6.05635 1 0 8 2 223.419 5.64475 3 0 8 -3 52.6193 2.24621 1 0 8 3 50.3872 1.88029 1 0 8 -4 48.6876 2.33206 1 0 8 4 56.7548 1.94363 1 0 8 -5 22.6467 1.51025 1 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2.61413 2 -2 -10 7 15.3693 1.87546 4 2 -10 -7 12.7327 1.66413 4 2 -10 -7 14.8057 1.66257 2 -2 -10 6 74.1711 3.43219 4 2 -10 -6 70.5930 3.20839 4 2 -10 -6 69.9234 3.10144 2 2 -10 -5 62.7801 2.85556 4 -2 -10 5 72.3661 3.18919 4 2 -10 -5 67.5812 2.86342 2 -2 -10 4 92.8808 3.47848 1 -2 -10 4 87.2445 3.53472 4 2 -10 -4 86.1381 3.23349 2 -2 -10 3-0.29101 0.54709 4 2 -10 -3 160.510 3.11350 2 2 -10 -2 2.31554 0.73011 2 -2 -10 2 1.23408 0.77715 1 -2 -10 1 225.549 6.52690 1 2 -10 -1 215.587 6.17348 2 2 -10 0 24.4503 1.38800 2 -2 -10 0 22.9043 1.53219 1 -2 -10 -1 13.6767 1.20293 1 -2 -10 -2 20.9705 1.37582 1 2 -10 2 23.7843 1.40513 4 -2 -10 -2 21.6749 1.17664 3 -2 -10 -2 21.3021 0.82630 2 -2 -10 -3 138.017 4.28707 1 -2 -10 -3 132.715 3.90825 3 -2 -10 -4 32.0667 1.57004 1 2 -10 4 15.5298 1.43528 4 -2 -10 -4 30.1246 1.21338 3 -2 -10 -5 30.6136 1.52973 1 2 -10 5 32.9160 2.03067 4 -2 -10 -5 28.9817 1.20643 3 -2 -10 -6 54.5564 2.11430 1 2 -10 6 56.5364 2.79029 4 -2 -10 -6 49.9802 1.71126 3 -2 -10 -7 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354.333 8.78731 4 2 3 2 332.019 8.77878 1 -2 3 -3 131.633 3.99916 4 -2 3 -4 36.3326 1.83030 4 -2 3 -5 78.6255 3.15176 4 -2 3 -6 37.0528 2.24286 4 -2 3 -7 26.5202 2.09658 4 -2 3 -8 12.0690 1.69448 4 -2 3 -9 18.5783 2.15089 4 -2 3 -10 8.51259 1.07299 1 -2 3 -10 9.20593 1.98642 4 -2 3 -11 9.61370 2.12873 4 2 4 -11 3.26306 1.36165 3 2 4 -10 4.61461 0.73695 1 2 4 -10 5.56346 1.31999 3 2 4 -9 6.09689 0.82734 1 2 4 -9 5.11933 1.29438 3 2 4 -8 17.0523 1.15487 1 2 4 -8 15.0670 1.56046 3 2 4 -7 89.4874 3.03217 1 2 4 -7 94.3624 3.56309 3 2 4 -6 64.3008 2.36464 1 2 4 -6 65.8616 2.78399 3 2 4 -5 31.1567 1.47296 1 2 4 -5 28.4300 1.67094 3 2 4 -4 178.369 4.94421 1 -2 4 4 171.005 4.36782 1 2 4 -4 176.801 5.21339 3 2 4 -3 54.9101 2.05246 1 2 4 -3 55.4699 2.18691 3 -2 4 3 55.3374 1.71622 3 2 4 -2 384.933 9.89498 1 2 4 -1 66.9376 1.98082 2 2 4 0 97.5504 2.59631 2 -2 4 -1 21.4402 0.89963 4 -2 4 -2 115.892 3.40186 4 2 4 2 116.413 3.47887 1 -2 4 -3 16.7609 1.12352 4 2 4 3 15.4124 0.96388 1 -2 4 -4 149.234 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1.46888 1 -2 5 -10 19.9275 2.33912 4 -2 5 -11 10.1016 2.15323 4 2 6 -11 1.66186 1.85692 4 2 6 -10 5.94407 0.96445 1 2 6 -10 5.50911 1.74340 4 2 6 -10 5.21611 1.43815 3 2 6 -9 3.57995 0.87283 1 2 6 -9 5.47811 1.55326 4 2 6 -9 2.92017 1.24484 3 2 6 -8 55.9721 2.36280 1 2 6 -8 55.8435 3.14716 4 2 6 -8 53.4638 2.79638 3 2 6 -7 23.1115 1.50876 1 2 6 -7 29.5726 2.19084 4 2 6 -7 23.4297 1.83370 3 2 6 -6 98.7780 3.40102 1 2 6 -6 96.6645 3.94233 4 2 6 -6 103.729 3.80487 3 -2 6 5 128.475 3.32767 1 2 6 -5 137.003 4.18415 1 2 6 -5 140.422 4.67308 4 2 6 -5 132.945 4.44210 3 2 6 -4 119.074 3.76249 1 -2 6 4 118.925 3.23021 1 2 6 -4 110.715 3.92409 3 2 6 -3 56.3156 2.23108 1 2 6 -2 15.0497 1.04995 1 -2 6 2 10.6655 0.97288 2 2 6 -1 449.297 10.9838 2 2 6 0 113.297 3.54641 1 -2 6 -2 97.3638 3.06211 4 2 6 2 99.5631 3.18577 1 -2 6 -3 10.8341 0.98816 4 2 6 3 10.5936 0.90213 1 -2 6 -4 16.7310 1.32997 4 2 6 4 19.0307 1.12038 1 -2 6 -5 64.9814 2.86922 4 -2 6 -6 121.840 4.53165 4 -2 6 -7 59.7702 3.09884 4 -2 6 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2.82402 1 -2 9 -6 32.0315 2.19249 4 -2 9 -7 12.9065 1.67846 4 -2 9 -8 12.5066 1.53857 1 -2 9 -8 14.0896 1.87890 4 -2 9 -9 8.62455 1.55301 1 -2 9 -9 12.7667 2.01740 4 -2 9 -10 54.1741 6.32077 1 -2 9 -10 15.0359 2.20496 4 2 10 -10 3.64968 1.19840 1 2 10 -9 2.52231 1.07100 1 2 10 -8 38.2210 2.21681 1 2 10 -8 40.6086 2.63133 3 2 10 -7 13.4725 1.39921 1 2 10 -7 14.2246 1.72423 3 -2 10 6 66.4877 2.07334 1 2 10 -6 66.2850 2.92816 1 2 10 -6 64.9700 3.12414 3 2 10 -5 64.7648 2.88532 1 -2 10 5 65.1015 2.25951 1 2 10 -5 71.7778 3.09677 3 2 10 -4 79.4998 3.21208 1 -2 10 4 80.6403 2.74809 1 2 10 -4 86.0182 3.34992 3 2 10 -3 156.708 5.08230 1 -2 10 3 158.553 4.70982 1 2 10 -2-0.06349 0.39310 1 -2 10 2 4.02413 0.78454 2 -2 10 1 213.429 5.99080 2 2 10 -1 209.080 5.19385 2 -2 10 0 25.1313 1.44190 2 -2 10 -1 12.5315 1.09080 2 -2 10 -2 22.5992 1.43740 2 -2 10 -3 148.455 4.83628 2 -2 10 -6 52.7236 2.80226 4 -2 10 -7 17.8444 1.67089 1 -2 10 -7 18.0897 1.88293 4 -2 10 -8 96.9799 4.02483 1 -2 10 -8 94.5654 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7.15045 1.94559 4 2 12 -10 3.35786 1.29267 1 2 12 -9 15.6939 1.70819 1 2 12 -8 13.3463 1.53970 1 2 12 -7 17.9798 1.69724 1 -2 12 7 18.1280 0.85699 1 2 12 -7 17.0827 1.87823 3 -2 12 6 62.8380 2.19310 1 2 12 -6 63.1735 3.02445 1 2 12 -6 57.8223 3.03697 3 2 12 -5 67.1684 3.06678 1 -2 12 5 64.4163 2.40490 1 2 12 -5 63.5829 3.06905 3 2 12 -4 92.0292 3.70238 1 2 12 -3 15.5025 1.42719 1 2 12 -2 51.4986 2.11356 1 2 12 -2 47.1186 2.02345 3 -2 12 2 49.2150 1.83642 2 2 12 -1 38.7281 1.87152 1 -2 12 1 3.57605 0.77191 1 2 12 -1 0.31383 0.61878 3 -2 12 1 44.1949 1.67287 2 -2 12 0 100.002 3.39441 2 2 12 1 40.7627 2.11980 1 -2 12 -1 42.8818 1.99144 2 2 12 2 77.8469 3.07728 1 -2 12 -2 76.8540 2.96991 2 2 12 3 0.19585 0.56015 1 -2 12 -3 4.16697 0.90890 2 2 12 4-0.25015 0.56174 1 -2 12 -5 27.0156 2.02282 1 -2 12 -6 20.4085 1.86975 1 -2 12 -7 66.0213 3.27382 1 -2 12 -8 29.7980 2.30519 1 -2 12 -9 33.2096 2.46076 1 -2 12 -10 10.4072 1.69806 1 2 13 -10 24.8187 2.10295 1 2 13 -9 20.7288 1.97569 1 2 13 -8 23.2180 1.95078 1 2 13 -7 17.3338 1.73864 1 -2 13 7 20.7806 1.02219 1 2 13 -7 18.9124 1.93471 3 -2 13 6 13.3052 0.98906 1 2 13 -6 14.5320 1.56462 1 2 13 -6 12.2712 1.57457 3 2 13 -5 7.22007 1.26089 1 2 13 -5 5.50285 1.30691 3 2 13 -4 37.0855 2.16319 1 -2 13 4 23.4307 0.83270 3 2 13 -3 26.2416 1.73150 1 2 13 -3 21.5788 1.64491 3 2 13 -2 14.7921 1.31180 1 -2 13 2 14.8510 1.27305 1 -2 13 2 13.6433 1.15972 2 2 13 -2 12.1295 1.30087 3 -2 13 1 31.8551 1.84764 1 -2 13 1 29.1785 1.58296 2 2 13 -1 29.9420 1.77666 3 -2 13 0 92.4316 3.50484 1 -2 13 0 81.8998 3.04950 2 2 13 1 127.500 4.49185 1 -2 13 -1 128.799 4.23178 2 2 13 2 97.1450 3.63616 1 -2 13 -2 96.3491 3.46440 2 -2 13 -2 90.4328 3.71319 1 2 13 3 54.1468 2.46384 1 -2 13 -3 48.4156 2.59309 1 -2 13 -3 49.5890 2.41179 2 2 13 4 38.7897 2.04941 1 -2 13 -4 39.2907 2.23026 2 -2 13 -4 38.4951 2.36083 1 2 13 5 14.1125 1.25688 1 -2 13 -5 26.3125 1.96915 1 2 13 6-0.41945 0.61322 1 -2 13 -6 27.3659 2.04814 1 -2 13 -7 13.0538 1.73766 1 -2 13 -8 10.3285 1.71610 1 -2 13 -9 2.98734 1.41168 1 -2 13 -10 9.35422 1.70565 1 2 14 -10 1.89491 1.35074 1 2 14 -9 3.57362 1.37981 1 2 14 -8 27.7687 2.15596 1 2 14 -7 22.4394 1.94140 1 -2 14 7 17.3911 1.08257 1 2 14 -6 27.6865 2.15191 1 2 14 -6 26.6483 2.17689 3 2 14 -5 55.6341 2.94785 1 2 14 -4 83.6534 3.07097 1 -2 14 4 76.0976 1.16426 3 2 14 -3 89.8862 3.73402 1 -2 14 3 90.0008 3.40728 1 2 14 -3 91.6773 3.72260 3 2 14 -2 19.3560 1.58060 1 -2 14 2 20.0586 1.50942 1 2 14 -2 20.9628 0.93483 2 -2 14 2 20.9203 1.41698 2 2 14 -2 18.9190 1.55243 3 -2 14 1 76.6888 3.21369 1 -2 14 1 78.2136 2.88986 2 2 14 -1 76.3041 3.11706 3 -2 14 0 45.7415 2.18774 1 -2 14 0 47.4033 1.87541 2 2 14 1 4.13249 0.93360 1 -2 14 -1 3.97281 0.88648 2 2 14 2 9.74488 1.20722 1 -2 14 -2 8.15983 1.04692 2 -2 14 -2 9.53630 1.26428 1 2 14 3 63.4855 2.80416 1 -2 14 -3 62.1145 2.76066 2 -2 14 -3 52.5938 2.87415 1 2 14 4 12.9076 1.32923 1 -2 14 -4 12.9601 1.41462 2 -2 14 -4 13.0863 1.58413 1 2 14 5 28.4445 1.76391 1 -2 14 -5 29.0417 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-1 4 16.0637 2.13094 2 -11 -1 3 8.70551 1.81870 2 -11 -1 2 12.3842 1.98096 2 -11 -1 1 13.5608 2.04282 2 -11 -1 0 5.44420 1.62362 2 -11 -1 -1 1.81659 1.52817 2 -11 -1 -2 7.35829 1.83079 2 -11 -1 -3 8.59569 1.87392 2 -11 -1 -4 9.75025 2.02154 2 -11 0 7 2.19647 1.66448 3 -11 0 6 3.83964 1.72742 3 -11 0 5 0.69394 1.52029 3 -11 0 4 11.5180 2.02870 2 -11 0 4 14.1868 2.05252 3 -11 0 3 9.50741 1.95662 2 -11 0 2 1.05512 1.44485 2 -11 0 1 25.1838 2.40690 2 -11 0 0 26.3735 2.53229 2 -11 0 -1 26.8757 2.54619 2 -11 0 -2 22.8522 2.43271 2 -11 0 -3 5.64739 1.74912 2 -11 0 -4 15.4034 2.25323 2 -11 1 8 6.60377 1.87579 3 -11 1 7 4.58075 1.67042 3 -11 1 6 9.56014 1.89614 3 -11 1 5 7.46609 1.86184 2 -11 1 5 7.35314 1.77130 3 -11 1 4 16.8251 2.23103 2 -11 1 4 14.8734 2.06877 3 -11 1 3 10.4800 1.97397 2 -11 1 2 12.1215 2.01021 2 -11 1 1 12.7768 2.04823 2 -11 1 0 8.01118 1.80630 2 -11 1 -1 1.50018 1.55109 2 -11 1 -2 6.18853 1.85069 2 -11 1 -3 7.74798 1.95725 2 -11 2 8 1.96835 1.57408 3 -11 2 7 2.38237 1.66591 3 -11 2 6 1.32768 1.46085 3 -11 2 5 5.80991 1.82960 2 -11 2 5 5.89722 1.76163 3 -11 2 4 6.49208 1.87376 2 -11 2 3 10.5208 1.94589 2 -11 2 2 25.4188 2.45844 2 -11 2 1 9.90592 1.93149 2 -11 2 0 18.0801 2.18676 2 -11 2 -1 22.9840 2.58803 2 -11 2 -2 16.2827 2.29425 2 -11 2 -3 16.7284 2.35248 2 -11 3 9 3.27562 1.66252 3 -11 3 8 6.25703 1.75341 3 -11 3 7 8.15094 1.86615 3 -11 3 6 10.7792 1.97678 3 -11 3 5 7.71844 1.90166 2 -11 3 5 8.95837 1.82814 3 -11 3 4 7.21391 1.86586 2 -11 3 3 11.8546 2.05282 2 -11 3 2 8.53299 1.82748 2 -11 3 1 1.10827 1.53714 2 -11 3 0 1.96339 1.62058 2 -11 3 -1 4.12343 1.74399 2 -11 3 -2 6.16557 1.94005 2 -11 3 -3 11.1981 2.16698 2 -11 4 9 4.87024 1.73296 3 -11 4 8-0.37275 1.56305 3 -11 4 7 2.14499 1.64408 3 -11 4 6 2.33139 1.58711 3 -11 4 5 2.15231 1.73457 2 -11 4 5 1.69422 1.47061 3 -11 4 4 6.76096 1.89676 2 -11 4 3 7.56619 1.86864 2 -11 4 2 10.1227 1.99194 2 -11 4 1 18.5217 2.28846 2 -11 4 0 13.6496 2.18641 2 -11 4 -1 11.9005 2.20723 2 -11 4 -2 30.6664 2.86397 2 -11 5 9 2.70220 1.55001 3 -11 5 8 7.96470 1.85867 3 -11 5 7 6.77277 1.72459 3 -11 5 6 6.48469 1.75125 3 -11 5 5 7.03369 1.95300 2 -11 5 5 6.17937 1.66330 3 -11 5 4 18.6708 2.43646 2 -11 5 3 14.5165 2.18411 2 -11 5 2 10.0209 2.00664 2 -11 5 1 5.47878 1.70860 2 -11 5 0 1.75794 1.76958 2 -11 5 -1 8.58617 1.99630 2 -11 5 -2 2.23421 1.79310 2 -11 6 8 3.15487 1.51434 3 -11 6 7 0.47982 1.38024 3 -11 6 6 1.74091 1.50756 3 -11 6 4 4.51246 1.79354 2 -11 6 3 5.57394 1.81757 2 -11 6 2 21.7106 2.43448 2 -11 6 1 7.18867 1.84129 2 -11 6 0 6.71946 1.96888 2 -11 6 -1 23.2276 2.64282 2 -11 6 -2 16.0854 2.40121 2 -11 7 8 8.92316 1.78098 3 -11 7 7 4.91888 1.65020 3 -11 7 6 9.62438 1.82252 3 -11 7 4 9.97312 2.19655 2 -11 7 3 7.35140 1.94695 2 11 7 -2 6.02093 1.44323 2 -11 7 2 7.80996 1.93849 2 -11 7 1 5.67705 1.83447 2 -11 7 0 3.95287 1.87059 2 -11 7 -1-0.30721 1.76737 2 -11 8 8 0.21800 1.37116 3 -11 8 7 1.02872 1.44276 3 -11 8 6 0.95471 1.49649 3 -11 8 3 15.7119 2.28458 2 11 8 -2 4.09835 1.30815 2 -11 8 2 2.13756 1.68146 2 -11 8 1 11.9981 2.11431 2 -11 8 0 12.8347 2.30448 2 -11 9 7 9.14568 1.81003 3 -11 9 6 8.41818 1.70168 3 11 9 -3 3.78870 1.29509 2 11 9 -2 6.13287 1.43089 2 -11 10 7 0.32613 1.39846 3 -11 10 6 0.80332 1.44375 3 -11 11 6 6.29760 1.67969 3 -11 12 6 4.72952 1.59766 3 -12 -8 2 15.7328 2.03680 2 -12 -7 2 4.80155 1.57965 2 -12 -7 1 4.19231 1.60955 2 -12 -7 0 6.50529 1.68901 2 -12 -7 -1 5.02034 1.56564 2 -12 -6 3 20.6819 2.28398 2 -12 -6 2 7.54161 1.72339 2 -12 -6 1 8.97918 1.80203 2 -12 -6 0 12.8171 1.98804 2 -12 -6 -1 3.08692 1.54331 2 -12 -6 -2 4.45786 1.61043 2 -12 -5 3 6.43333 1.79586 2 -12 -5 2 1.52155 1.53705 2 -12 -5 1 3.09078 1.55694 2 -12 -5 0 8.57853 1.84715 2 -12 -5 -1 8.49405 1.80375 2 -12 -5 -2 11.6028 1.90925 2 -12 -5 -3 5.56598 1.63893 2 -12 -4 3 3.57226 1.66649 2 -12 -4 2 19.8966 2.36463 2 -12 -4 1 10.3455 1.90262 2 -12 -4 0 7.59800 1.83468 2 -12 -4 -1 19.7012 2.28697 2 -12 -4 -2 3.67987 1.69816 2 -12 -4 -3 6.00204 1.69474 2 -12 -3 4 2.37376 1.66914 2 -12 -3 3 4.07253 1.82366 2 -12 -3 2 1.86681 1.54682 2 -12 -3 1 2.75810 1.64806 2 -12 -3 0 12.5038 2.03056 2 -12 -3 -1 9.57659 1.94662 2 -12 -3 -2 10.0031 1.96337 2 -12 -2 4 1.99926 1.61139 2 -12 -2 3 7.40240 1.83845 2 -12 -2 2 3.54691 1.63197 2 -12 -2 1 14.2723 2.08608 2 -12 -2 0 22.0068 2.38553 2 -12 -2 -1 7.85612 1.89789 2 -12 -2 -2 7.92681 1.87500 2 -12 -1 4-0.14609 1.59323 2 -12 -1 3 0.57455 1.59357 2 -12 -1 2 3.48954 1.72892 2 -12 -1 1 5.78586 1.73834 2 -12 -1 0 2.33495 1.69448 2 -12 -1 -1 9.48872 1.97917 2 -12 -1 -2 13.8222 2.21254 2 -12 0 4 13.8692 2.25817 2 -12 0 3 3.10037 1.73961 2 -12 0 2 11.7281 2.11609 2 -12 0 1 15.9084 2.28146 2 -12 0 0 13.3634 2.15959 2 -12 0 -1 4.74559 1.82426 2 -12 1 3 1.80107 1.65864 2 -12 1 2 2.62625 1.64681 2 -12 1 1 8.07003 1.97552 2 -12 1 0 3.16245 1.73753 2 -12 1 -1 6.49196 1.95672 2 -12 2 3 5.92726 1.90449 2 -12 2 2 4.61209 1.76140 2 -12 2 1 14.8537 2.26594 2 -12 2 0 24.2390 2.62087 2 -12 3 2 5.15871 1.96172 2 -12 3 1 4.04616 1.78642 2 0 0 0 0.00 0.00 0 TITL SX22-17_Mo_auto in P2(1) REM P2(1) (#4 in standard setting) CELL 0.71073 9.406047 19.377926 9.422486 90.0000 97.9255 90.0000 ZERR 2.00 0.000267 0.000446 0.000297 0.0000 0.0024 0.0000 LATT -1 SYMM -x, y+1/2,-z SFAC C H O K Sn UNIT 64.00 78.00 20.00 2.00 2.00 REM CrysAlisPro recorded range (K): Min=100.0; max=100.0; aver:100.0 TEMP -173 SIZE 0.03 0.05 0.06 TREF HKLF 4 END ; _shelx_hkl_checksum 92943 _shelx_res_file ; TITL sx22-17_mo_auto_a.res in P2(1) sx22-17_mo_auto.res created by SHELXL-2018/3 at 18:42:22 on 30-May-2024 REM Old TITL SX22-17_Mo_auto in P2(1)/m REM SHELXT solution in P2(1): R1 0.180, Rweak 0.140, Alpha 0.080 REM 0.215 for 11 systematic absences, Orientation as input REM Flack x = 0.205 ( 0.015 ) from 2802 Parsons' quotients REM Formula found by SHELXT: C32 O10 K Sn CELL 0.71073 9.406 19.3779 9.4225 90 97.925 90 ZERR 2 0.0003 0.0004 0.0003 0 0.002 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H K O Sn UNIT 64 78 2 20 2 EQIV $1 +X,+Y,1+Z EQIV $2 1+X,+Y,+Z L.S. 10 PLAN 7 TEMP -173 CONF HTAB C4 O1_$2 HTAB C16 O1_$1 BIND O3 K1 BIND O4 K1 BIND O6 K1 BIND O7 K1 BIND K1 O5 BIND K1 O10 BIND K1 O9 FREE K1 C20 FREE K1 C19 FREE K1 C24 BIND O8 K1 BOND list 4 MORE -1 BOND $H fmap 2 53 acta SHEL 90 0.77 TWIN 0 0 1 0 -1 0 1 0 0 2 REM REM REM WGHT 0.070800 BASF 0.19728 FVAR 0.18983 SN1 5 0.410083 0.583760 0.459355 11.00000 0.02583 0.01459 = 0.02423 0.00108 -0.00227 0.00236 O1 4 0.251713 0.555174 0.294980 11.00000 0.02561 0.01566 = 0.02418 0.00113 -0.00183 0.00162 O2 4 0.396862 0.465808 0.465111 11.00000 0.04475 0.01643 = 0.04289 -0.00094 -0.01788 -0.00102 O3 4 0.284745 0.376000 0.346960 11.00000 0.06109 0.02226 = 0.05290 -0.00197 -0.02374 -0.00397 O4 4 0.148168 0.471973 0.156228 11.00000 0.03433 0.02515 = 0.03114 -0.00196 -0.00661 -0.00340 C1 1 0.623253 0.574111 0.407747 11.00000 0.02651 0.02115 = 0.02671 -0.00100 -0.00544 0.01363 C2 1 0.711518 0.517617 0.449220 11.00000 0.03796 0.02028 = 0.03036 -0.00339 -0.00675 0.00567 AFIX 43 H2 2 0.677139 0.480378 0.500564 11.00000 -1.20000 AFIX 0 C3 1 0.853563 0.516613 0.413523 11.00000 0.03640 0.03433 = 0.04330 -0.01157 -0.00780 0.02339 AFIX 43 H3 2 0.913985 0.478341 0.441871 11.00000 -1.20000 AFIX 0 C4 1 0.904612 0.569124 0.339878 11.00000 0.02950 0.04633 = 0.04398 -0.02213 0.00490 0.00147 AFIX 43 H4 2 1.000617 0.568146 0.319164 11.00000 -1.20000 AFIX 0 C5 1 0.816327 0.623813 0.295401 11.00000 0.03937 0.03226 = 0.04335 -0.01034 0.01337 0.00183 AFIX 43 H5 2 0.850759 0.659627 0.240293 11.00000 -1.20000 AFIX 0 C6 1 0.678786 0.627444 0.329536 11.00000 0.02763 0.02027 = 0.03499 -0.00301 -0.00006 0.01243 AFIX 43 H6 2 0.620610 0.666331 0.300060 11.00000 -1.20000 AFIX 0 C7 1 0.359191 0.691144 0.401254 11.00000 0.02154 0.01229 = 0.02980 0.00468 0.00446 0.00204 C8 1 0.444995 0.742394 0.474772 11.00000 0.02434 0.02270 = 0.02440 0.00081 0.00469 0.00650 AFIX 43 H8 2 0.519593 0.729495 0.548454 11.00000 -1.20000 AFIX 0 C9 1 0.422492 0.812582 0.441279 11.00000 0.02773 0.01963 = 0.02287 -0.00119 0.00588 -0.00115 AFIX 43 H9 2 0.480264 0.846932 0.492962 11.00000 -1.20000 AFIX 0 C10 1 0.313681 0.831424 0.330580 11.00000 0.03212 0.00777 = 0.02652 0.00156 0.00015 0.00169 AFIX 43 H10 2 0.298609 0.878641 0.305833 11.00000 -1.20000 AFIX 0 C11 1 0.227806 0.780604 0.257075 11.00000 0.03465 0.01761 = 0.02396 0.00222 -0.00803 0.00241 AFIX 43 H11 2 0.152693 0.793270 0.183718 11.00000 -1.20000 AFIX 0 C12 1 0.252532 0.710607 0.291673 11.00000 0.03019 0.01317 = 0.02841 0.00160 -0.00306 0.00388 AFIX 43 H12 2 0.195505 0.676187 0.239377 11.00000 -1.20000 AFIX 0 C13 1 0.370792 0.579510 0.677286 11.00000 0.02587 0.02753 = 0.02733 0.00093 -0.00079 -0.00460 C14 1 0.297405 0.634323 0.729667 11.00000 0.03813 0.02229 = 0.02269 0.00404 -0.00059 -0.00425 AFIX 43 H14 2 0.262058 0.670815 0.667257 11.00000 -1.20000 AFIX 0 C15 1 0.275441 0.636006 0.873198 11.00000 0.03879 0.03970 = 0.03807 -0.00530 0.01222 -0.01020 AFIX 43 H15 2 0.226304 0.673758 0.908593 11.00000 -1.20000 AFIX 0 C16 1 0.325607 0.582393 0.963761 11.00000 0.03944 0.03422 = 0.03224 0.00947 0.00412 -0.01618 AFIX 43 H16 2 0.310981 0.583366 1.061508 11.00000 -1.20000 AFIX 0 C17 1 0.396304 0.527966 0.912429 11.00000 0.03831 0.04103 = 0.03042 0.01706 -0.00594 -0.01458 AFIX 43 H17 2 0.429710 0.491448 0.975628 11.00000 -1.20000 AFIX 0 C18 1 0.420739 0.524729 0.768571 11.00000 0.02741 0.02905 = 0.03477 0.00026 0.00105 -0.00775 AFIX 43 H18 2 0.469574 0.486627 0.734140 11.00000 -1.20000 AFIX 0 C19 1 0.227659 0.490788 0.259886 11.00000 0.02143 0.01985 = 0.02659 0.00425 0.00286 0.00090 C20 1 0.310071 0.437910 0.367178 11.00000 0.03233 0.02033 = 0.02937 0.00427 -0.01000 -0.00109 K1 3 0.108665 0.338952 0.096307 11.00000 0.02405 0.01680 = 0.02398 -0.00038 0.00008 -0.00055 O5 4 -0.091087 0.427547 -0.097109 11.00000 0.02565 0.01729 = 0.02555 -0.00005 0.00273 -0.00041 O6 4 -0.156184 0.382803 0.168201 11.00000 0.02233 0.01992 = 0.03195 0.00125 0.00344 -0.00244 O7 4 -0.035612 0.258683 0.285166 11.00000 0.03294 0.02644 = 0.02270 0.00115 0.00212 0.00285 O8 4 0.222958 0.210809 0.200460 11.00000 0.03854 0.01730 = 0.02988 -0.00131 -0.00204 -0.00022 O9 4 0.291826 0.259338 -0.062120 11.00000 0.02571 0.02580 = 0.03740 0.00313 0.00678 0.00438 O10 4 0.175253 0.384538 -0.171375 11.00000 0.02993 0.01819 = 0.02636 -0.00161 0.00245 0.00174 C21 1 -0.174377 0.468221 -0.012325 11.00000 0.02334 0.02092 = 0.03099 -0.00076 -0.00379 0.00918 AFIX 23 H21A 2 -0.241853 0.497889 -0.075143 11.00000 -1.20000 H21B 2 -0.110542 0.498315 0.053253 11.00000 -1.20000 AFIX 0 C22 1 -0.255849 0.420860 0.072029 11.00000 0.02708 0.03222 = 0.02934 -0.00158 0.00588 0.00048 AFIX 23 H22A 2 -0.319867 0.447871 0.126044 11.00000 -1.20000 H22B 2 -0.315664 0.389015 0.006764 11.00000 -1.20000 AFIX 0 C23 1 -0.222995 0.341964 0.264810 11.00000 0.03851 0.02775 = 0.04212 -0.00068 0.01826 -0.00750 AFIX 23 H23A 2 -0.286849 0.307414 0.211248 11.00000 -1.20000 H23B 2 -0.281701 0.371518 0.319785 11.00000 -1.20000 AFIX 0 C24 1 -0.108862 0.306432 0.364534 11.00000 0.04131 0.01485 = 0.02707 -0.00428 0.00676 -0.00640 AFIX 23 H24A 2 -0.040179 0.340835 0.411697 11.00000 -1.20000 H24B 2 -0.152538 0.281731 0.439726 11.00000 -1.20000 AFIX 0 C25 1 0.066207 0.217241 0.375212 11.00000 0.04825 0.03052 = 0.02546 0.01230 0.00090 -0.00171 AFIX 23 H25A 2 0.016438 0.190038 0.442444 11.00000 -1.20000 H25B 2 0.137948 0.247248 0.431986 11.00000 -1.20000 AFIX 0 C26 1 0.138932 0.170130 0.283648 11.00000 0.04549 0.01807 = 0.03497 0.01081 -0.00535 0.00318 AFIX 23 H26A 2 0.201246 0.137366 0.344216 11.00000 -1.20000 H26B 2 0.066709 0.143313 0.219869 11.00000 -1.20000 AFIX 0 C27 1 0.298264 0.170722 0.110815 11.00000 0.04673 0.02926 = 0.03965 -0.00174 -0.00403 0.01446 AFIX 23 H27A 2 0.229728 0.144494 0.041901 11.00000 -1.20000 H27B 2 0.361344 0.137377 0.168962 11.00000 -1.20000 AFIX 0 C28 1 0.387150 0.217963 0.031130 11.00000 0.02840 0.02959 = 0.04949 0.00286 0.00073 0.01439 AFIX 23 H28A 2 0.449335 0.247442 0.099552 11.00000 -1.20000 H28B 2 0.449059 0.190529 -0.024455 11.00000 -1.20000 AFIX 0 C29 1 0.369438 0.306511 -0.141751 11.00000 0.02866 0.02500 = 0.05414 -0.00507 0.01095 0.00024 AFIX 23 H29A 2 0.439272 0.280956 -0.191382 11.00000 -1.20000 H29B 2 0.422566 0.340498 -0.076177 11.00000 -1.20000 AFIX 0 C30 1 0.261809 0.342702 -0.249086 11.00000 0.04148 0.03089 = 0.02509 -0.00292 0.01341 0.00488 AFIX 23 H30A 2 0.311547 0.371631 -0.313522 11.00000 -1.20000 H30B 2 0.201563 0.308548 -0.307951 11.00000 -1.20000 AFIX 0 C31 1 0.076342 0.423948 -0.265993 11.00000 0.03211 0.01946 = 0.02690 0.00124 -0.00036 -0.00734 AFIX 23 H31A 2 0.010250 0.392884 -0.326933 11.00000 -1.20000 H31B 2 0.128454 0.452511 -0.329063 11.00000 -1.20000 AFIX 0 C32 1 -0.007349 0.469551 -0.178047 11.00000 0.02848 0.02550 = 0.02036 0.00321 -0.00231 -0.00280 AFIX 23 H32A 2 0.059398 0.498412 -0.112634 11.00000 -1.20000 H32B 2 -0.070902 0.500531 -0.241853 11.00000 -1.20000 AFIX 0 HKLF 4 REM sx22-17_mo_auto_a.res in P2(1) REM wR2 = 0.1049, GooF = S = 1.077, Restrained GooF = 1.077 for all data REM R1 = 0.0327 for 6792 Fo > 4sig(Fo) and 0.0368 for all 7113 data REM 398 parameters refined using 1 restraints END WGHT 0.0708 0.0000 REM Highest difference peak 1.280, deepest hole -0.520, 1-sigma level 0.073 Q1 1 0.4774 0.5835 0.4036 11.00000 0.05 1.28 Q2 1 0.3594 0.5621 0.3988 11.00000 0.05 1.09 Q3 1 0.3547 0.6013 0.3906 11.00000 0.05 0.80 Q4 1 0.2944 0.0841 0.3297 11.00000 0.05 0.49 Q5 1 0.4840 0.5594 0.5290 11.00000 0.05 0.43 Q6 1 -0.0026 0.3391 0.0423 11.00000 0.05 0.37 Q7 1 0.5219 0.5905 0.5037 11.00000 0.05 0.37 ; _shelx_res_checksum 50789 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Sn Sn1 0.41008(5) 0.58376(2) 0.45935(5) 0.02209(12) Uani d 1 . . O O1 0.2517(6) 0.5552(3) 0.2950(6) 0.0223(10) Uani d 1 . . O O2 0.3969(8) 0.4658(3) 0.4651(8) 0.0369(16) Uani d 1 . . O O3 0.2847(9) 0.3760(4) 0.3470(9) 0.0484(19) Uani d 1 . . O O4 0.1482(7) 0.4720(3) 0.1562(7) 0.0312(14) Uani d 1 . . C C1 0.6233(8) 0.5741(5) 0.4077(8) 0.0256(19) Uani d 1 . . C C2 0.7115(10) 0.5176(4) 0.4492(9) 0.0306(18) Uani d 1 . . H H2 0.677139 0.480378 0.500564 0.037 Uiso calc 1 . . C C3 0.8536(11) 0.5166(5) 0.4135(11) 0.039(2) Uani d 1 . . H H3 0.913985 0.478341 0.441871 0.047 Uiso calc 1 . . C C4 0.9046(10) 0.5691(5) 0.3399(10) 0.040(3) Uani d 1 . . H H4 1.000617 0.568146 0.319164 0.048 Uiso calc 1 . . C C5 0.8163(11) 0.6238(5) 0.2954(12) 0.038(2) Uani d 1 . . H H5 0.850759 0.659627 0.240293 0.045 Uiso calc 1 . . C C6 0.6788(9) 0.6274(4) 0.3295(10) 0.0280(17) Uani d 1 . . H H6 0.620610 0.666331 0.300060 0.034 Uiso calc 1 . . C C7 0.3592(8) 0.6911(4) 0.4013(9) 0.0211(15) Uani d 1 . . C C8 0.4450(8) 0.7424(4) 0.4748(8) 0.0237(15) Uani d 1 . . H H8 0.519593 0.729495 0.548454 0.028 Uiso calc 1 . . C C9 0.4225(8) 0.8126(4) 0.4413(8) 0.0232(14) Uani d 1 . . H H9 0.480264 0.846932 0.492962 0.028 Uiso calc 1 . . C C10 0.3137(8) 0.8314(4) 0.3306(8) 0.0225(15) Uani d 1 . . H H10 0.298609 0.878641 0.305833 0.027 Uiso calc 1 . . C C11 0.2278(9) 0.7806(4) 0.2571(9) 0.0265(16) Uani d 1 . . H H11 0.152693 0.793270 0.183718 0.032 Uiso calc 1 . . C C12 0.2525(9) 0.7106(4) 0.2917(9) 0.0246(16) Uani d 1 . . H H12 0.195505 0.676187 0.239377 0.030 Uiso calc 1 . . C C13 0.3708(7) 0.5795(7) 0.6773(8) 0.0273(15) Uani d 1 . . C C14 0.2974(10) 0.6343(5) 0.7297(9) 0.0282(17) Uani d 1 . . H H14 0.262058 0.670815 0.667257 0.034 Uiso calc 1 . . C C15 0.2754(11) 0.6360(5) 0.8732(11) 0.038(2) Uani d 1 . . H H15 0.226304 0.673758 0.908593 0.046 Uiso calc 1 . . C C16 0.3256(8) 0.5824(8) 0.9638(8) 0.0354(17) Uani d 1 . . H H16 0.310981 0.583366 1.061508 0.042 Uiso calc 1 . . C C17 0.3963(10) 0.5280(6) 0.9124(10) 0.038(2) Uani d 1 . . H H17 0.429710 0.491448 0.975628 0.045 Uiso calc 1 . . C C18 0.4207(9) 0.5247(5) 0.7686(9) 0.0307(18) Uani d 1 . . H H18 0.469574 0.486627 0.734140 0.037 Uiso calc 1 . . C C19 0.2277(8) 0.4908(4) 0.2599(9) 0.0227(15) Uani d 1 . . C C20 0.3101(10) 0.4379(4) 0.3672(10) 0.0287(16) Uani d 1 . . K K1 0.10867(17) 0.33895(8) 0.09631(17) 0.0219(3) Uani d 1 . . O O5 -0.0911(6) 0.4275(3) -0.0971(6) 0.0229(11) Uani d 1 . . O O6 -0.1562(6) 0.3828(3) 0.1682(6) 0.0248(12) Uani d 1 . . O O7 -0.0356(7) 0.2587(4) 0.2852(7) 0.0275(15) Uani d 1 . . O O8 0.2230(7) 0.2108(3) 0.2005(7) 0.0292(12) Uani d 1 . . O O9 0.2918(8) 0.2593(4) -0.0621(8) 0.0294(16) Uani d 1 . . O O10 0.1753(6) 0.3845(3) -0.1714(6) 0.0250(12) Uani d 1 . . C C21 -0.1744(9) 0.4682(4) -0.0123(9) 0.0258(16) Uani d 1 . . H H21A -0.241853 0.497889 -0.075143 0.031 Uiso calc 1 . . H H21B -0.110542 0.498315 0.053253 0.031 Uiso calc 1 . . C C22 -0.2558(11) 0.4209(6) 0.0720(11) 0.029(2) Uani d 1 . . H H22A -0.319867 0.447871 0.126044 0.035 Uiso calc 1 . . H H22B -0.315664 0.389015 0.006764 0.035 Uiso calc 1 . . C C23 -0.2230(12) 0.3420(6) 0.2648(12) 0.035(2) Uani d 1 . . H H23A -0.286849 0.307414 0.211248 0.042 Uiso calc 1 . . H H23B -0.281701 0.371518 0.319785 0.042 Uiso calc 1 . . C C24 -0.1089(10) 0.3064(4) 0.3645(9) 0.0276(17) Uani d 1 . . H H24A -0.040179 0.340835 0.411697 0.033 Uiso calc 1 . . H H24B -0.152538 0.281731 0.439726 0.033 Uiso calc 1 . . C C25 0.0662(11) 0.2172(5) 0.3752(10) 0.035(2) Uani d 1 . . H H25A 0.016438 0.190038 0.442444 0.042 Uiso calc 1 . . H H25B 0.137948 0.247248 0.431986 0.042 Uiso calc 1 . . C C26 0.1389(11) 0.1701(4) 0.2836(10) 0.0339(19) Uani d 1 . . H H26A 0.201246 0.137366 0.344216 0.041 Uiso calc 1 . . H H26B 0.066709 0.143313 0.219869 0.041 Uiso calc 1 . . C C27 0.2983(11) 0.1707(5) 0.1108(11) 0.039(2) Uani d 1 . . H H27A 0.229728 0.144494 0.041901 0.047 Uiso calc 1 . . H H27B 0.361344 0.137377 0.168962 0.047 Uiso calc 1 . . C C28 0.3872(10) 0.2180(5) 0.0311(11) 0.036(2) Uani d 1 . . H H28A 0.449335 0.247442 0.099552 0.044 Uiso calc 1 . . H H28B 0.449059 0.190529 -0.024455 0.044 Uiso calc 1 . . C C29 0.3694(10) 0.3065(5) -0.1418(11) 0.035(2) Uani d 1 . . H H29A 0.439272 0.280956 -0.191382 0.043 Uiso calc 1 . . H H29B 0.422566 0.340498 -0.076177 0.043 Uiso calc 1 . . C C30 0.2618(11) 0.3427(5) -0.2491(10) 0.032(2) Uani d 1 . . H H30A 0.311547 0.371631 -0.313522 0.038 Uiso calc 1 . . H H30B 0.201563 0.308548 -0.307951 0.038 Uiso calc 1 . . C C31 0.0763(10) 0.4239(5) -0.2660(10) 0.027(2) Uani d 1 . . H H31A 0.010250 0.392884 -0.326933 0.032 Uiso calc 1 . . H H31B 0.128454 0.452511 -0.329063 0.032 Uiso calc 1 . . C C32 -0.0073(9) 0.4696(4) -0.1780(8) 0.0253(16) Uani d 1 . . H H32A 0.059398 0.498412 -0.112634 0.030 Uiso calc 1 . . H H32B -0.070902 0.500531 -0.241853 0.030 Uiso calc 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Sn1 0.0258(2) 0.01459(18) 0.0242(2) 0.0024(3) -0.00227(13) 0.0011(3) O1 0.026(3) 0.016(2) 0.024(3) 0.002(2) -0.0018(19) 0.001(2) O2 0.045(4) 0.016(3) 0.043(4) -0.001(3) -0.018(3) -0.001(3) O3 0.061(5) 0.022(3) 0.053(5) -0.004(3) -0.024(3) -0.002(3) O4 0.034(3) 0.025(3) 0.031(3) -0.003(2) -0.007(2) -0.002(2) C1 0.027(3) 0.021(5) 0.027(3) 0.014(3) -0.005(3) -0.001(3) C2 0.038(5) 0.020(4) 0.030(5) 0.006(3) -0.007(3) -0.003(3) C3 0.036(5) 0.034(5) 0.043(5) 0.023(4) -0.008(4) -0.012(4) C4 0.030(4) 0.046(8) 0.044(5) 0.001(4) 0.005(3) -0.022(5) C5 0.039(5) 0.032(5) 0.043(6) 0.002(4) 0.013(4) -0.010(4) C6 0.028(4) 0.020(4) 0.035(5) 0.012(3) 0.000(3) -0.003(3) C7 0.022(4) 0.012(3) 0.030(5) 0.002(3) 0.004(3) 0.005(3) C8 0.024(4) 0.023(4) 0.024(4) 0.006(3) 0.005(3) 0.001(3) C9 0.028(4) 0.020(3) 0.023(4) -0.001(3) 0.006(3) -0.001(3) C10 0.032(4) 0.008(3) 0.027(4) 0.002(3) 0.000(3) 0.002(3) C11 0.035(4) 0.018(3) 0.024(4) 0.002(3) -0.008(3) 0.002(3) C12 0.030(4) 0.013(4) 0.028(5) 0.004(3) -0.003(3) 0.002(3) C13 0.026(3) 0.028(4) 0.027(3) -0.005(5) -0.001(2) 0.001(5) C14 0.038(5) 0.022(4) 0.023(4) -0.004(3) -0.001(3) 0.004(3) C15 0.039(5) 0.040(5) 0.038(5) -0.010(4) 0.012(4) -0.005(4) C16 0.039(4) 0.034(4) 0.032(4) -0.016(6) 0.004(3) 0.009(6) C17 0.038(5) 0.041(5) 0.030(4) -0.015(4) -0.006(3) 0.017(4) C18 0.027(4) 0.029(4) 0.035(5) -0.008(3) 0.001(3) 0.000(4) C19 0.021(4) 0.020(4) 0.027(4) 0.001(3) 0.003(3) 0.004(3) C20 0.032(5) 0.020(4) 0.029(5) -0.001(3) -0.010(3) 0.004(3) K1 0.0241(7) 0.0168(7) 0.0240(8) -0.0005(5) 0.0001(5) -0.0004(5) O5 0.026(3) 0.017(2) 0.026(3) 0.000(2) 0.0027(19) -0.0001(19) O6 0.022(3) 0.020(3) 0.032(3) -0.002(2) 0.003(2) 0.001(2) O7 0.033(4) 0.026(3) 0.023(3) 0.003(3) 0.002(2) 0.001(3) O8 0.039(3) 0.017(3) 0.030(3) 0.000(2) -0.002(2) -0.001(2) O9 0.026(3) 0.026(3) 0.037(4) 0.004(3) 0.007(3) 0.003(3) O10 0.030(3) 0.018(3) 0.026(3) 0.002(2) 0.002(2) -0.002(2) C21 0.023(4) 0.021(4) 0.031(4) 0.009(3) -0.004(3) -0.001(3) C22 0.027(5) 0.032(5) 0.029(5) 0.000(4) 0.006(4) -0.002(4) C23 0.039(5) 0.028(5) 0.042(5) -0.007(4) 0.018(4) -0.001(4) C24 0.041(5) 0.015(4) 0.027(4) -0.006(3) 0.007(3) -0.004(3) C25 0.048(5) 0.031(4) 0.025(4) -0.002(4) 0.001(4) 0.012(4) C26 0.045(5) 0.018(4) 0.035(5) 0.003(4) -0.005(4) 0.011(3) C27 0.047(6) 0.029(5) 0.040(5) 0.014(4) -0.004(4) -0.002(4) C28 0.028(4) 0.030(4) 0.049(6) 0.014(4) 0.001(4) 0.003(4) C29 0.029(4) 0.025(4) 0.054(6) 0.000(4) 0.011(4) -0.005(4) C30 0.041(5) 0.031(5) 0.025(4) 0.005(4) 0.013(4) -0.003(4) C31 0.032(5) 0.019(4) 0.027(5) -0.007(3) 0.000(4) 0.001(3) C32 0.028(4) 0.026(4) 0.020(4) -0.003(3) -0.002(3) 0.003(3) 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' 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' Sn Sn -0.6537 1.4246 '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 -1 0 0.0247 2 -1 2 0.0155 2 -1 -2 0.0163 0 1 2 0.0048 -3 -5 2 0.0352 1 -2 1 0.0149 1 5 0 0.0202 0 -2 -1 0.0293 0 2 1 0.0136 -1 1 1 0.0218 -2 0 -3 0.0224 0 -1 1 0.0122 1 2 -1 0.0137 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 Sn1 O2 . . 73.4(2) ? O1 Sn1 C1 . . 114.0(3) ? O1 Sn1 C7 . . 87.6(3) ? O1 Sn1 C13 . . 120.4(3) ? C1 Sn1 O2 . . 88.5(3) ? C1 Sn1 C7 . . 101.9(3) ? C1 Sn1 C13 . . 120.5(3) ? C7 Sn1 O2 . . 160.8(3) ? C13 Sn1 O2 . . 85.5(4) ? C13 Sn1 C7 . . 102.5(4) ? C19 O1 Sn1 . . 121.9(5) ? C20 O2 Sn1 . . 116.1(5) ? C20 O3 K1 . . 117.5(6) ? C19 O4 K1 . . 121.4(5) ? C2 C1 Sn1 . . 123.1(7) ? C2 C1 C6 . . 118.1(7) ? C6 C1 Sn1 . . 118.8(6) ? C1 C2 H2 . . 120.5 ? C1 C2 C3 . . 119.1(8) ? C3 C2 H2 . . 120.5 ? C2 C3 H3 . . 119.3 ? C4 C3 C2 . . 121.4(8) ? C4 C3 H3 . . 119.3 ? C3 C4 H4 . . 120.2 ? C3 C4 C5 . . 119.5(9) ? C5 C4 H4 . . 120.2 ? C4 C5 H5 . . 119.5 ? C4 C5 C6 . . 121.0(9) ? C6 C5 H5 . . 119.5 ? C1 C6 H6 . . 119.6 ? C5 C6 C1 . . 120.8(8) ? C5 C6 H6 . . 119.6 ? C8 C7 Sn1 . . 117.3(5) ? C12 C7 Sn1 . . 123.7(6) ? C12 C7 C8 . . 118.9(7) ? C7 C8 H8 . . 119.5 ? C7 C8 C9 . . 121.1(7) ? C9 C8 H8 . . 119.5 ? C8 C9 H9 . . 120.3 ? C10 C9 C8 . . 119.3(7) ? C10 C9 H9 . . 120.3 ? C9 C10 H10 . . 120.1 ? C11 C10 C9 . . 119.8(7) ? C11 C10 H10 . . 120.1 ? C10 C11 H11 . . 120.0 ? C10 C11 C12 . . 120.0(7) ? C12 C11 H11 . . 120.0 ? C7 C12 C11 . . 120.9(8) ? C7 C12 H12 . . 119.6 ? C11 C12 H12 . . 119.6 ? C14 C13 Sn1 . . 118.1(7) ? C14 C13 C18 . . 119.9(7) ? C18 C13 Sn1 . . 122.0(7) ? C13 C14 H14 . . 119.8 ? C13 C14 C15 . . 120.5(8) ? C15 C14 H14 . . 119.8 ? C14 C15 H15 . . 120.1 ? C16 C15 C14 . . 119.7(9) ? C16 C15 H15 . . 120.1 ? C15 C16 H16 . . 120.0 ? C17 C16 C15 . . 120.0(8) ? C17 C16 H16 . . 120.0 ? C16 C17 H17 . . 119.1 ? C16 C17 C18 . . 121.7(9) ? C18 C17 H17 . . 119.1 ? C13 C18 C17 . . 118.1(9) ? C13 C18 H18 . . 121.0 ? C17 C18 H18 . . 121.0 ? O1 C19 C20 . . 114.2(7) ? O4 C19 O1 . . 124.3(8) ? O4 C19 C20 . . 121.5(8) ? O2 C20 C19 . . 113.8(7) ? O3 C20 O2 . . 128.3(8) ? O3 C20 C19 . . 117.9(8) ? O3 K1 O5 . . 128.47(19) ? O3 K1 O6 . . 99.3(2) ? O3 K1 O7 . . 83.7(2) ? O3 K1 O8 . . 77.22(19) ? O3 K1 O9 . . 104.4(2) ? O3 K1 O10 . . 119.8(2) ? O4 K1 O3 . . 61.30(19) ? O4 K1 O5 . . 68.16(17) ? O4 K1 O6 . . 75.94(18) ? O4 K1 O7 . . 117.6(2) ? O4 K1 O8 . . 138.06(19) ? O4 K1 O9 . . 123.7(2) ? O4 K1 O10 . . 81.05(18) ? O6 K1 O5 . . 57.71(16) ? O6 K1 O7 . . 59.86(18) ? O6 K1 O8 . . 119.38(18) ? O6 K1 O9 . . 154.6(2) ? O6 K1 O10 . . 115.80(18) ? O7 K1 O5 . . 112.53(18) ? O7 K1 O9 . . 113.74(19) ? O8 K1 O5 . . 153.77(17) ? O8 K1 O7 . . 59.61(19) ? O8 K1 O9 . . 58.88(19) ? O9 K1 O5 . . 111.35(18) ? O10 K1 O5 . . 58.09(15) ? O10 K1 O7 . . 156.01(19) ? O10 K1 O8 . . 117.67(18) ? O10 K1 O9 . . 58.80(19) ? C21 O5 K1 . . 108.9(4) ? C32 O5 K1 . . 108.0(4) ? C32 O5 C21 . . 111.7(6) ? C22 O6 K1 . . 122.3(5) ? C23 O6 K1 . . 118.3(6) ? C23 O6 C22 . . 112.9(7) ? C24 O7 K1 . . 106.3(5) ? C24 O7 C25 . . 112.6(7) ? C25 O7 K1 . . 109.8(5) ? C26 O8 K1 . . 117.6(5) ? C27 O8 K1 . . 118.3(5) ? C27 O8 C26 . . 112.8(6) ? C28 O9 K1 . . 110.8(5) ? C28 O9 C29 . . 111.0(7) ? C29 O9 K1 . . 108.2(5) ? C30 O10 K1 . . 119.7(5) ? C31 O10 K1 . . 121.5(5) ? C31 O10 C30 . . 110.8(7) ? O5 C21 H21A . . 110.0 ? O5 C21 H21B . . 110.0 ? O5 C21 C22 . . 108.6(7) ? H21A C21 H21B . . 108.3 ? C22 C21 H21A . . 110.0 ? C22 C21 H21B . . 110.0 ? O6 C22 C21 . . 108.5(7) ? O6 C22 H22A . . 110.0 ? O6 C22 H22B . . 110.0 ? C21 C22 H22A . . 110.0 ? C21 C22 H22B . . 110.0 ? H22A C22 H22B . . 108.4 ? O6 C23 H23A . . 110.0 ? O6 C23 H23B . . 110.0 ? O6 C23 C24 . . 108.5(8) ? H23A C23 H23B . . 108.4 ? C24 C23 H23A . . 110.0 ? C24 C23 H23B . . 110.0 ? O7 C24 C23 . . 109.1(7) ? O7 C24 H24A . . 109.9 ? O7 C24 H24B . . 109.9 ? C23 C24 H24A . . 109.9 ? C23 C24 H24B . . 109.9 ? H24A C24 H24B . . 108.3 ? O7 C25 H25A . . 109.9 ? O7 C25 H25B . . 109.9 ? O7 C25 C26 . . 108.9(7) ? H25A C25 H25B . . 108.3 ? C26 C25 H25A . . 109.9 ? C26 C25 H25B . . 109.9 ? O8 C26 C25 . . 108.3(7) ? O8 C26 H26A . . 110.0 ? O8 C26 H26B . . 110.0 ? C25 C26 H26A . . 110.0 ? C25 C26 H26B . . 110.0 ? H26A C26 H26B . . 108.4 ? O8 C27 H27A . . 109.9 ? O8 C27 H27B . . 109.9 ? O8 C27 C28 . . 108.8(8) ? H27A C27 H27B . . 108.3 ? C28 C27 H27A . . 109.9 ? C28 C27 H27B . . 109.9 ? O9 C28 C27 . . 107.8(8) ? O9 C28 H28A . . 110.1 ? O9 C28 H28B . . 110.1 ? C27 C28 H28A . . 110.1 ? C27 C28 H28B . . 110.1 ? H28A C28 H28B . . 108.5 ? O9 C29 H29A . . 110.2 ? O9 C29 H29B . . 110.2 ? O9 C29 C30 . . 107.7(8) ? H29A C29 H29B . . 108.5 ? C30 C29 H29A . . 110.2 ? C30 C29 H29B . . 110.2 ? O10 C30 C29 . . 107.5(7) ? O10 C30 H30A . . 110.2 ? O10 C30 H30B . . 110.2 ? C29 C30 H30A . . 110.2 ? C29 C30 H30B . . 110.2 ? H30A C30 H30B . . 108.5 ? O10 C31 H31A . . 110.0 ? O10 C31 H31B . . 110.0 ? O10 C31 C32 . . 108.5(7) ? H31A C31 H31B . . 108.4 ? C32 C31 H31A . . 110.0 ? C32 C31 H31B . . 110.0 ? O5 C32 C31 . . 109.2(6) ? O5 C32 H32A . . 109.8 ? O5 C32 H32B . . 109.8 ? C31 C32 H32A . . 109.8 ? C31 C32 H32B . . 109.8 ? H32A C32 H32B . . 108.3 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Sn1 O1 . 2.071(5) ? Sn1 O2 . 2.290(6) ? Sn1 C1 . 2.136(7) ? Sn1 C7 . 2.188(7) ? Sn1 C13 . 2.138(7) ? O1 C19 . 1.303(10) ? O2 C20 . 1.266(11) ? O3 C20 . 1.233(11) ? O3 K1 . 2.785(7) ? O4 C19 . 1.202(10) ? O4 K1 . 2.654(6) ? C1 C2 . 1.397(12) ? C1 C6 . 1.411(13) ? C2 H2 . 0.9500 ? C2 C3 . 1.422(14) ? C3 H3 . 0.9500 ? C3 C4 . 1.356(15) ? C4 H4 . 0.9500 ? C4 C5 . 1.376(14) ? C5 H5 . 0.9500 ? C5 C6 . 1.377(13) ? C6 H6 . 0.9500 ? C7 C8 . 1.401(11) ? C7 C12 . 1.389(11) ? C8 H8 . 0.9500 ? C8 C9 . 1.406(10) ? C9 H9 . 0.9500 ? C9 C10 . 1.405(11) ? C10 H10 . 0.9500 ? C10 C11 . 1.396(11) ? C11 H11 . 0.9500 ? C11 C12 . 1.407(10) ? C12 H12 . 0.9500 ? C13 C14 . 1.394(15) ? C13 C18 . 1.406(14) ? C14 H14 . 0.9500 ? C14 C15 . 1.396(13) ? C15 H15 . 0.9500 ? C15 C16 . 1.385(16) ? C16 H16 . 0.9500 ? C16 C17 . 1.370(18) ? C17 H17 . 0.9500 ? C17 C18 . 1.407(13) ? C18 H18 . 0.9500 ? C19 C20 . 1.567(11) ? K1 O5 . 2.976(6) ? K1 O6 . 2.802(6) ? K1 O7 . 2.845(7) ? K1 O8 . 2.827(6) ? K1 O9 . 2.878(7) ? K1 O10 . 2.823(6) ? O5 C21 . 1.430(9) ? O5 C32 . 1.425(9) ? O6 C22 . 1.418(12) ? O6 C23 . 1.417(11) ? O7 C24 . 1.426(10) ? O7 C25 . 1.435(11) ? O8 C26 . 1.425(11) ? O8 C27 . 1.408(11) ? O9 C28 . 1.415(11) ? O9 C29 . 1.443(12) ? O10 C30 . 1.421(11) ? O10 C31 . 1.419(11) ? C21 H21A . 0.9900 ? C21 H21B . 0.9900 ? C21 C22 . 1.493(13) ? C22 H22A . 0.9900 ? C22 H22B . 0.9900 ? C23 H23A . 0.9900 ? C23 H23B . 0.9900 ? C23 C24 . 1.494(14) ? C24 H24A . 0.9900 ? C24 H24B . 0.9900 ? C25 H25A . 0.9900 ? C25 H25B . 0.9900 ? C25 C26 . 1.486(13) ? C26 H26A . 0.9900 ? C26 H26B . 0.9900 ? C27 H27A . 0.9900 ? C27 H27B . 0.9900 ? C27 C28 . 1.508(15) ? C28 H28A . 0.9900 ? C28 H28B . 0.9900 ? C29 H29A . 0.9900 ? C29 H29B . 0.9900 ? C29 C30 . 1.502(14) ? C30 H30A . 0.9900 ? C30 H30B . 0.9900 ? C31 H31A . 0.9900 ? C31 H31B . 0.9900 ? C31 C32 . 1.506(13) ? C32 H32A . 0.9900 ? C32 H32B . 0.9900 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C4 H4 O1 1_655 0.95 2.42 3.360(11) 172.0 yes C16 H16 O1 1_556 0.95 2.41 3.332(9) 164.8 yes 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Sn1 O1 C19 O4 . . . . -171.7(6) ? Sn1 O1 C19 C20 . . . . 9.4(10) ? Sn1 O2 C20 O3 . . . . 179.5(10) ? Sn1 O2 C20 C19 . . . . 0.0(11) ? Sn1 C1 C2 C3 . . . . -178.2(6) ? Sn1 C1 C6 C5 . . . . 179.2(7) ? Sn1 C7 C8 C9 . . . . 178.1(5) ? Sn1 C7 C12 C11 . . . . -178.2(7) ? Sn1 C13 C14 C15 . . . . -176.6(7) ? Sn1 C13 C18 C17 . . . . 176.8(6) ? O1 C19 C20 O2 . . . . -5.7(12) ? O1 C19 C20 O3 . . . . 174.8(9) ? O4 C19 C20 O2 . . . . 175.4(9) ? O4 C19 C20 O3 . . . . -4.2(14) ? C1 C2 C3 C4 . . . . -0.2(13) ? C2 C1 C6 C5 . . . . -0.1(13) ? C2 C3 C4 C5 . . . . -1.7(14) ? C3 C4 C5 C6 . . . . 2.7(15) ? C4 C5 C6 C1 . . . . -1.8(14) ? C6 C1 C2 C3 . . . . 1.1(12) ? C7 C8 C9 C10 . . . . -1.1(11) ? C8 C7 C12 C11 . . . . -1.7(13) ? C8 C9 C10 C11 . . . . 1.1(11) ? C9 C10 C11 C12 . . . . -1.5(13) ? C10 C11 C12 C7 . . . . 1.8(14) ? C12 C7 C8 C9 . . . . 1.4(12) ? C13 C14 C15 C16 . . . . -0.7(14) ? C14 C13 C18 C17 . . . . -1.0(12) ? C14 C15 C16 C17 . . . . -0.1(14) ? C15 C16 C17 C18 . . . . 0.3(14) ? C16 C17 C18 C13 . . . . 0.2(13) ? C18 C13 C14 C15 . . . . 1.3(13) ? K1 O3 C20 O2 . . . . -172.6(9) ? K1 O3 C20 C19 . . . . 6.8(13) ? K1 O4 C19 O1 . . . . 179.9(6) ? K1 O4 C19 C20 . . . . -1.3(11) ? K1 O5 C21 C22 . . . . -59.3(7) ? K1 O5 C32 C31 . . . . 60.9(7) ? K1 O6 C22 C21 . . . . -35.7(10) ? K1 O6 C23 C24 . . . . 29.9(9) ? K1 O7 C24 C23 . . . . 65.7(7) ? K1 O7 C25 C26 . . . . -60.8(8) ? K1 O8 C26 C25 . . . . -37.5(9) ? K1 O8 C27 C28 . . . . 38.8(9) ? K1 O9 C28 C27 . . . . 59.3(8) ? K1 O9 C29 C30 . . . . -64.4(8) ? K1 O10 C30 C29 . . . . -34.4(9) ? K1 O10 C31 C32 . . . . 33.9(8) ? O5 C21 C22 O6 . . . . 63.9(9) ? O6 C23 C24 O7 . . . . -65.8(9) ? O7 C25 C26 O8 . . . . 66.3(9) ? O8 C27 C28 O9 . . . . -66.0(10) ? O9 C29 C30 O10 . . . . 66.4(9) ? O10 C31 C32 O5 . . . . -64.5(8) ? C21 O5 C32 C31 . . . . -179.4(7) ? C22 O6 C23 C24 . . . . -177.8(7) ? C23 O6 C22 C21 . . . . 173.2(8) ? C24 O7 C25 C26 . . . . -179.0(7) ? C25 O7 C24 C23 . . . . -174.0(7) ? C26 O8 C27 C28 . . . . -178.2(8) ? C27 O8 C26 C25 . . . . 179.2(8) ? C28 O9 C29 C30 . . . . 173.8(7) ? C29 O9 C28 C27 . . . . 179.6(8) ? C30 O10 C31 C32 . . . . -177.4(7) ? C31 O10 C30 C29 . . . . 176.3(7) ? C32 O5 C21 C22 . . . . -178.5(7) ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.80272 2 0.19728