#------------------------------------------------------------------------------ #$Date: 2019-11-07 23:23:23 +0200 (Thu, 07 Nov 2019) $ #$Revision: 224003 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/83/7048319.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_7048319 loop_ _publ_author_name 'Bartalucci, Niccol\`o' 'Bortoluzzi, Marco' 'Zacchini, Stefano' 'Pampaloni, Guido' 'Marchetti, Fabio' _publ_section_title ; Straightforward formation of carbocations from tertiary carboxylic acids via CO release at room temperature. ; _journal_issue 5 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 1574 _journal_page_last 1577 _journal_paper_doi 10.1039/c8dt04416c _journal_volume 48 _journal_year 2019 _chemical_formula_sum 'C19 H15 Cl5 O W' _chemical_formula_weight 620.41 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2018-09-26 deposited with the CCDC. 2018-11-23 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 103.080(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.275(2) _cell_length_b 7.9205(11) _cell_length_c 18.698(3) _cell_measurement_reflns_used 5470 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 27.8955 _cell_measurement_theta_min 2.2365 _cell_volume 2059.2(5) _computing_cell_refinement 'APEX3 (Bruker AXS, 2015)' _computing_data_collection 'APEX3 (Bruker AXS, 2015)' _computing_data_reduction 'SAINT (Bruker AXS, 2015)' _computing_molecular_graphics 'ORTEPIII (Johnson, 1996)' _computing_publication_material 'XCIF 2014/2 (Bruker AXS, 2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0568 _diffrn_reflns_av_unetI/netI 0.0461 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 16758 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 25.049 _diffrn_reflns_theta_max 25.049 _diffrn_reflns_theta_min 1.465 _exptl_absorpt_coefficient_mu 6.265 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.3935 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details ; Data were corrected for Lorentz polarization and absorption effects (empirical absorption correction SADABS). R(int) = 0.1360 (selected reflections only, before parameter refinement) R(int) = 0.0657(selected reflections only, after parameter refinement) ; _exptl_crystal_colour orange _exptl_crystal_density_diffrn 2.001 _exptl_crystal_description plate _exptl_crystal_F_000 1184 _exptl_crystal_size_max 0.180 _exptl_crystal_size_mid 0.160 _exptl_crystal_size_min 0.110 _refine_diff_density_max 2.845 _refine_diff_density_min -1.399 _refine_diff_density_rms 0.165 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 235 _refine_ls_number_reflns 3654 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.094 _refine_ls_R_factor_all 0.0441 _refine_ls_R_factor_gt 0.0374 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0262P)^2^+14.2528P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0845 _refine_ls_wR_factor_ref 0.0875 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3244 _reflns_number_total 3654 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c8dt04416c3.cif _cod_data_source_block 1 _cod_depositor_comments 'Adding full bibliography for 7048319--7048320.cif.' _cod_database_code 7048319 _shelx_shelxl_version_number 2014/7 _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_min 0.398 _shelx_estimated_absorpt_t_max 0.546 _shelx_res_file ; p21c.res created by SHELXL-2014/7 TITL p21c in P2(1)/c CELL 0.71073 14.2746 7.9205 18.6983 90.000 103.080 90.000 ZERR 4.00 0.0021 0.0011 0.0027 0.000 0.002 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H O Cl W UNIT 76 60 4 20 4 OMIT -3 50.1 L.S. 16 ACTA BOND bond $h eqiv $1 1-x, 2-y, 1-z dfix -3 .01 o1 o1_$1 conf htab FMAP 2 PLAN 20 size 0.18 0.16 0.11 TEMP -173 WGHT 0.026200 14.252800 FVAR 0.06689 C1 1 0.778290 0.396591 0.354868 11.00000 0.02021 0.02921 = 0.00712 0.00478 0.00290 0.00369 C2 1 0.783653 0.234208 0.320599 11.00000 0.02223 0.01731 = 0.00919 0.00192 0.00370 0.00216 C3 1 0.870593 0.144494 0.332528 11.00000 0.01480 0.02210 = 0.01127 -0.00340 0.00502 0.00134 AFIX 43 H3 2 0.926960 0.192045 0.362731 11.00000 -1.20000 AFIX 0 C4 1 0.875128 -0.006004 0.302158 11.00000 0.02939 0.04296 = 0.02484 -0.00414 0.01036 0.01142 AFIX 43 H4 2 0.934616 -0.064971 0.311666 11.00000 -1.20000 AFIX 0 C5 1 0.792950 -0.080690 0.255767 11.00000 0.03607 0.02301 = 0.01827 0.00589 0.01219 0.00361 AFIX 43 H5 2 0.797416 -0.187406 0.233584 11.00000 -1.20000 AFIX 0 C6 1 0.706192 0.004993 0.243482 11.00000 0.02644 0.02661 = 0.01470 -0.00466 0.00084 -0.00384 AFIX 43 H6 2 0.650288 -0.044078 0.213302 11.00000 -1.20000 AFIX 0 C7 1 0.700535 0.161342 0.274868 11.00000 0.01825 0.02173 = 0.01412 0.00654 0.00521 0.00477 AFIX 43 H7 2 0.641002 0.220123 0.265845 11.00000 -1.20000 AFIX 0 C8 1 0.687739 0.453930 0.369335 11.00000 0.01776 0.02879 = 0.00769 -0.00474 -0.00254 -0.00224 C9 1 0.624430 0.340984 0.392538 11.00000 0.01717 0.02684 = 0.01839 -0.00180 0.00350 -0.00229 AFIX 43 H9 2 0.639219 0.223957 0.396826 11.00000 -1.20000 AFIX 0 C10 1 0.541286 0.400023 0.408973 11.00000 0.02137 0.04674 = 0.01628 -0.00473 0.00357 -0.00388 AFIX 43 H10 2 0.500199 0.324164 0.426680 11.00000 -1.20000 AFIX 0 C11 1 0.516895 0.568580 0.399993 11.00000 0.01526 0.04926 = 0.02220 -0.01842 0.00333 0.00308 AFIX 43 H11 2 0.458431 0.607043 0.410528 11.00000 -1.20000 AFIX 0 C12 1 0.576534 0.682037 0.375856 11.00000 0.02576 0.03165 = 0.01297 -0.00655 -0.00094 0.00762 AFIX 43 H12 2 0.558524 0.797358 0.368782 11.00000 -1.20000 AFIX 0 C13 1 0.662930 0.626353 0.362018 11.00000 0.02822 0.02280 = 0.01231 -0.00448 -0.00008 0.00269 AFIX 43 H13 2 0.705510 0.704753 0.347558 11.00000 -1.20000 AFIX 0 C14 1 0.862445 0.501168 0.377569 11.00000 0.01925 0.02087 = 0.01740 0.00415 0.00774 0.00127 C15 1 0.873839 0.602650 0.441065 11.00000 0.02009 0.02600 = 0.01709 0.00271 0.00566 0.01003 AFIX 43 H15 2 0.824182 0.606017 0.467355 11.00000 -1.20000 AFIX 0 C16 1 0.954892 0.695523 0.465039 11.00000 0.02170 0.01762 = 0.01888 0.00005 0.00238 0.00440 AFIX 43 H16 2 0.961392 0.761733 0.508249 11.00000 -1.20000 AFIX 0 C17 1 1.028518 0.695320 0.427396 11.00000 0.02095 0.02212 = 0.02769 0.00536 0.00030 -0.00523 AFIX 43 H17 2 1.085057 0.760154 0.444880 11.00000 -1.20000 AFIX 0 C18 1 1.018385 0.598638 0.363544 11.00000 0.02313 0.02723 = 0.02774 0.00314 0.01397 -0.00300 AFIX 43 H18 2 1.067626 0.600022 0.336835 11.00000 -1.20000 AFIX 0 C19 1 0.937479 0.501402 0.339115 11.00000 0.02250 0.02397 = 0.01890 0.00194 0.01085 0.00219 AFIX 43 H19 2 0.931886 0.434135 0.296290 11.00000 -1.20000 AFIX 0 CL1 4 0.869977 0.931062 0.647218 11.00000 0.02099 0.03261 = 0.02298 0.00476 -0.00067 -0.00249 CL2 4 0.704208 0.676657 0.561477 11.00000 0.03096 0.02455 = 0.02023 -0.00400 0.01146 -0.00765 CL3 4 0.644257 0.948244 0.673531 11.00000 0.03765 0.03256 = 0.02330 -0.00333 0.02110 -0.00343 CL4 4 0.729775 1.254407 0.591217 11.00000 0.03544 0.02356 = 0.03288 0.00015 0.01751 0.00652 CL5 4 0.786161 0.987409 0.472787 11.00000 0.02848 0.02605 = 0.01751 0.00217 0.01135 0.00389 O1 3 0.602987 0.994758 0.508058 11.00000 0.03410 0.06919 = 0.02526 0.00779 0.00309 0.00455 W1 5 0.705936 0.968741 0.567991 11.00000 0.01732 0.02488 = 0.01518 -0.00008 0.00695 0.00032 HKLF 4 REM p21c in P2(1)/c REM R1 = 0.0374 for 3244 Fo > 4sig(Fo) and 0.0441 for all 3654 data REM 235 parameters refined using 1 restraints END WGHT 0.0263 14.2448 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 2.845, deepest hole -1.399, 1-sigma level 0.165 Q1 1 0.7536 0.9596 0.6073 11.00000 0.05 2.85 Q2 1 0.6264 1.0390 0.5601 11.00000 0.05 1.37 Q3 1 0.7780 1.0469 0.5712 11.00000 0.05 1.31 Q4 1 0.7189 1.0869 0.5914 11.00000 0.05 1.27 Q5 1 0.7014 0.8380 0.5720 11.00000 0.05 1.24 Q6 1 0.7753 0.8922 0.5723 11.00000 0.05 1.22 Q7 1 0.5735 0.9999 0.5016 11.00000 0.05 1.22 Q8 1 0.5292 0.5377 0.3417 11.00000 0.05 1.10 Q9 1 0.6379 0.8906 0.5684 11.00000 0.05 1.00 Q10 1 0.8860 -0.1113 0.2927 11.00000 0.05 0.87 Q11 1 0.6171 0.9625 0.6316 11.00000 0.05 0.78 Q12 1 0.6796 1.1861 0.5940 11.00000 0.05 0.68 Q13 1 0.7599 0.7519 0.5675 11.00000 0.05 0.62 Q14 1 0.8338 1.0384 0.5903 11.00000 0.05 0.58 Q15 1 0.8398 0.9327 0.5787 11.00000 0.05 0.56 Q16 1 0.6582 0.7598 0.5748 11.00000 0.05 0.55 Q17 1 0.8652 0.0140 0.2750 11.00000 0.05 0.50 Q18 1 0.7861 0.6214 0.5637 11.00000 0.05 0.50 Q19 1 0.6537 0.8796 0.5237 11.00000 0.05 0.49 Q20 1 0.8734 0.7984 0.6441 11.00000 0.05 0.49 ; _shelx_res_checksum 20998 _shelx_hkl_file ; 1 0 0 11.03 0.83 1 0 0 11.46 0.92 -1 0 0 12.67 0.85 2 0 0 634.90 43.85 -2 0 0 679.97 41.12 2 0 0 700.89 39.15 3 0 0 262.57 17.56 -3 0 0 270.49 16.45 -4 0 0 43.86 2.97 4 0 0 45.58 3.25 5 0 0 408.48 27.17 -5 0 0 416.46 25.45 -6 0 0 5.40 0.73 6 0 0 4.30 0.84 -7 0 0 246.86 16.04 7 0 0 268.32 17.18 -8 0 0 29.26 2.25 8 0 0 31.91 2.54 -9 0 0 36.47 2.67 9 0 0 36.18 2.92 -10 0 0 139.45 8.95 -11 0 0 6.91 1.02 -12 0 0 285.46 18.96 -12 0 0 277.26 17.67 -13 0 0 8.22 1.38 -13 0 0 8.21 1.18 -14 0 0 103.85 7.57 -14 0 0 106.18 7.04 -15 0 0 25.20 2.30 -15 0 0 27.90 2.61 -16 0 0 4.60 1.23 -16 0 0 5.18 1.11 -17 0 0 55.61 4.59 -18 0 0 10.33 1.83 0 -1 0 -0.03 0.32 0 -1 0 0.01 0.15 0 1 0 -0.50 0.09 0 1 0 -0.36 0.13 -1 -1 0 9.29 0.92 1 -1 0 7.46 0.99 -1 -1 0 7.35 0.71 1 1 0 9.28 0.67 -1 1 0 8.67 0.69 1 1 0 9.35 0.60 -2 -1 0 4.32 0.59 -2 -1 0 6.70 0.63 2 -1 0 5.68 0.79 2 1 0 5.46 0.50 -2 1 0 6.15 0.42 -2 1 0 5.62 0.53 2 1 0 6.12 0.45 3 -1 0 1.85 0.47 -3 -1 0 3.68 0.54 -3 -1 0 3.56 0.40 3 1 0 2.85 0.35 -3 1 0 2.94 0.35 3 1 0 2.93 0.39 -3 1 0 3.84 0.46 -4 -1 0 12.88 1.09 4 -1 0 12.99 1.28 4 1 0 11.21 0.88 -4 1 0 9.58 0.91 -4 1 0 12.54 1.09 4 1 0 11.15 0.99 -5 -1 0 14.37 1.21 5 -1 0 14.48 1.39 -5 1 0 11.73 1.07 5 1 0 14.61 1.10 5 1 0 12.19 1.20 -5 1 0 14.44 1.31 6 -1 0 22.00 1.84 -6 -1 0 21.04 1.63 6 1 0 17.69 1.55 -6 1 0 20.19 1.52 -6 1 0 18.33 1.76 6 1 0 18.63 1.72 7 -1 0 9.55 1.05 -7 -1 0 11.55 1.14 -7 1 0 6.05 1.09 7 1 0 7.99 1.13 7 1 0 10.03 1.29 -7 1 0 9.09 0.96 -8 -1 0 2.68 0.64 8 -1 0 3.10 0.59 8 1 0 4.01 0.96 -8 1 0 2.55 0.56 -8 1 0 2.61 0.79 8 1 0 3.13 0.84 -9 -1 0 12.86 1.38 -9 1 0 11.56 1.24 -9 1 0 12.76 1.66 9 1 0 13.69 1.58 -10 -1 0 -0.28 0.47 10 1 0 0.78 0.78 -10 1 0 2.15 0.89 -10 1 0 1.68 0.61 -11 -1 0 4.47 0.87 11 1 0 6.77 1.22 -11 1 0 4.10 0.83 -11 1 0 5.48 1.17 -12 -1 0 3.20 0.81 -12 1 0 2.87 0.80 -12 1 0 3.21 1.05 12 1 0 4.67 1.12 -13 -1 0 8.59 1.22 13 1 0 5.53 1.24 -13 1 0 7.33 1.13 -13 1 0 8.26 1.52 -14 -1 0 1.01 0.69 -14 1 0 -0.59 0.85 -15 -1 0 -1.08 0.59 -15 -1 0 0.24 0.77 -15 1 0 0.83 0.92 -16 -1 0 8.27 1.52 -16 -1 0 7.77 1.38 -16 1 0 13.06 1.85 -17 -1 0 2.10 1.15 -17 -1 0 -0.69 0.79 -17 1 0 1.85 1.14 -18 -1 0 4.81 1.38 -18 -1 0 4.16 1.22 0 -2 0 516.05 42.54 0 -2 0 524.76 33.82 0 2 0 596.61 32.15 0 2 0 568.79 36.07 -1 -2 0 11.59 1.32 1 -2 0 10.69 0.68 -1 -2 0 7.91 0.88 1 -2 0 9.69 1.38 -1 2 0 9.33 0.89 1 2 0 9.35 0.73 1 2 0 9.29 0.87 -2 -2 0 173.52 12.46 2 -2 0 143.07 12.57 -2 -2 0 141.31 9.97 -2 2 0 162.45 10.56 2 2 0 164.09 10.50 2 2 0 167.35 9.37 -3 -2 0 27.68 2.05 3 -2 0 26.95 2.63 -3 -2 0 27.91 2.37 3 2 0 27.47 1.77 3 2 0 27.98 1.98 -3 2 0 27.36 2.04 -4 -2 0 3.08 0.59 4 -2 0 3.57 0.85 -4 -2 0 2.65 0.49 -4 2 0 2.49 0.30 -4 2 0 2.29 0.48 4 2 0 2.42 0.38 4 2 0 2.06 0.42 -5 -2 0 135.13 8.08 -5 -2 0 126.09 9.74 5 2 0 119.87 7.47 -5 2 0 125.11 7.80 -5 2 0 126.10 8.48 5 2 0 123.02 8.38 -6 -2 0 14.32 1.33 6 -2 0 15.16 1.60 6 2 0 14.09 1.24 -6 2 0 13.75 1.37 -6 2 0 13.92 1.12 6 2 0 13.54 1.11 -7 -2 0 58.64 3.81 7 -2 0 59.85 4.59 7 2 0 56.25 3.49 -7 2 0 47.09 3.57 7 2 0 54.13 3.88 -7 2 0 52.29 4.04 -8 -2 0 24.49 1.89 8 -2 0 22.69 2.12 8 2 0 21.55 1.95 8 2 0 20.20 1.72 -8 2 0 23.07 2.10 -8 2 0 20.20 1.70 9 -2 0 7.15 1.06 -9 -2 0 7.49 1.06 -9 2 0 6.06 0.88 -9 2 0 6.66 1.23 9 2 0 6.83 1.14 9 2 0 7.33 1.25 -10 -2 0 90.57 5.21 10 2 0 72.07 5.57 -10 2 0 59.66 5.53 -10 2 0 78.08 4.99 10 2 0 71.82 5.03 -11 -2 0 4.65 0.91 11 2 0 4.74 1.32 11 2 0 6.32 1.22 -11 2 0 4.96 1.33 -12 -2 0 90.18 6.30 12 2 0 94.81 6.82 -12 2 0 97.43 7.05 -13 -2 0 16.96 1.89 13 2 0 17.16 2.08 -13 2 0 18.52 2.30 -14 -2 0 39.72 3.29 14 2 0 41.32 3.59 -14 2 0 51.23 3.98 -15 -2 0 13.56 1.76 15 2 0 15.95 2.03 -15 2 0 16.92 2.28 -16 -2 0 2.93 1.02 -16 2 0 1.21 1.05 -17 -2 0 43.93 3.81 -17 -2 0 38.80 3.46 -17 2 0 46.37 3.97 -18 -2 0 4.83 1.37 -18 -2 0 4.95 1.32 0 -3 0 0.28 0.65 0 -3 0 0.94 0.26 0 3 0 -0.62 0.23 0 3 0 -0.06 0.35 -1 -3 0 274.93 20.28 1 -3 0 276.92 15.88 -1 -3 0 234.14 16.02 1 -3 0 216.06 20.27 1 3 0 271.26 15.19 -1 3 0 250.00 17.06 1 3 0 283.84 17.07 -2 -3 0 11.01 1.29 2 -3 0 6.14 1.25 -2 -3 0 6.93 0.88 2 3 0 7.19 0.70 -2 3 0 7.26 0.85 2 3 0 8.11 0.81 3 -3 0 42.61 3.75 -3 -3 0 42.79 3.48 -3 -3 0 36.15 2.82 3 3 0 40.29 2.83 -3 3 0 40.34 2.93 3 3 0 39.63 2.53 4 -3 0 51.86 4.37 -4 -3 0 48.20 4.03 -4 -3 0 50.07 3.41 4 3 0 46.02 3.02 -4 3 0 48.96 3.49 4 3 0 47.52 3.38 5 -3 0 4.03 1.07 -5 -3 0 4.15 0.77 -5 -3 0 3.78 0.70 5 3 0 4.08 0.61 -5 3 0 3.59 0.66 5 3 0 4.10 0.56 6 -3 0 71.05 5.38 -6 -3 0 67.35 4.32 -6 -3 0 59.16 4.99 -6 3 0 62.80 4.46 6 3 0 58.49 3.85 -6 3 0 60.61 3.90 6 3 0 60.71 4.33 -7 -3 0 0.62 0.53 -7 -3 0 1.53 0.47 7 -3 0 0.88 0.76 -7 3 0 1.09 0.60 7 3 0 0.15 0.43 -7 3 0 0.80 0.37 7 3 0 1.25 0.54 -8 -3 0 17.08 1.71 8 -3 0 9.98 1.64 8 3 0 16.22 1.50 8 3 0 17.17 1.36 -8 3 0 18.67 1.83 9 -3 0 0.93 0.74 -9 -3 0 1.72 0.67 9 3 0 0.58 0.61 -9 3 0 1.75 0.83 9 3 0 0.01 0.67 -10 -3 0 4.74 0.94 -10 3 0 4.57 1.26 10 3 0 4.71 1.14 10 3 0 4.72 1.05 -11 -3 0 25.03 2.16 11 3 0 23.59 2.60 11 3 0 26.99 2.50 -11 3 0 22.98 2.70 -12 -3 0 1.28 0.68 12 3 0 1.50 1.11 -12 3 0 0.63 0.97 12 3 0 0.13 0.94 -13 -3 0 32.12 2.68 13 3 0 35.53 3.16 -13 3 0 26.76 3.27 13 3 0 34.89 3.18 -14 -3 0 -1.40 0.60 -14 3 0 1.89 1.26 14 3 0 -0.90 0.96 -15 -3 0 11.96 1.66 -15 3 0 10.35 2.01 15 3 0 12.61 2.02 -16 -3 0 5.06 1.22 16 3 0 6.71 1.65 -16 3 0 5.03 1.59 -17 -3 0 -1.27 0.88 17 3 0 1.47 1.24 -17 3 0 0.80 1.26 0 -4 0 220.02 12.60 0 -4 0 196.73 16.22 0 4 0 196.30 11.99 0 4 0 198.10 13.49 -1 -4 0 5.99 0.69 1 -4 0 5.42 1.29 -1 -4 0 5.08 1.13 1 -4 0 6.16 0.49 -1 4 0 3.64 0.71 1 4 0 3.44 0.70 1 4 0 4.54 0.61 -1 4 0 3.68 0.57 -2 -4 0 142.23 9.33 -2 -4 0 162.57 11.87 2 -4 0 119.76 11.90 2 4 0 153.13 8.78 2 4 0 151.40 9.86 -2 4 0 150.17 9.91 -3 -4 0 43.79 3.49 -3 -4 0 55.08 4.43 3 -4 0 49.30 4.70 -3 4 0 54.42 3.71 3 4 0 51.96 3.19 3 4 0 48.11 3.57 -4 -4 0 35.06 2.83 -4 -4 0 39.61 3.42 4 -4 0 43.71 3.87 4 4 0 37.66 2.50 -4 4 0 38.66 2.96 4 4 0 37.13 2.79 5 -4 0 57.05 4.95 -5 -4 0 50.49 4.49 -5 -4 0 52.93 3.82 5 4 0 52.60 3.40 5 4 0 53.85 3.79 -5 4 0 56.15 3.97 6 -4 0 6.15 1.39 -6 -4 0 4.19 0.88 -6 -4 0 6.70 1.04 6 4 0 4.25 0.70 6 4 0 5.38 0.81 -6 4 0 5.48 0.95 -7 -4 0 38.10 3.43 -7 -4 0 46.65 3.16 7 -4 0 40.25 3.81 -7 4 0 36.90 3.16 7 4 0 39.83 2.68 7 4 0 40.86 2.99 8 -4 0 21.39 2.30 -8 -4 0 21.08 2.07 8 4 0 16.99 1.58 8 4 0 19.38 1.78 -8 4 0 23.29 2.10 9 -4 0 28.99 3.01 -9 -4 0 31.81 2.60 9 4 0 34.16 2.58 9 4 0 30.92 2.28 -9 4 0 28.26 2.76 -10 -4 0 37.01 3.08 -10 4 0 42.36 3.53 10 4 0 39.63 3.20 10 4 0 40.73 2.89 -11 -4 0 0.27 0.67 11 4 0 -0.01 0.88 11 4 0 0.77 0.78 -11 4 0 0.92 0.96 -12 -4 0 35.42 2.83 -12 4 0 28.58 3.43 12 4 0 36.73 2.93 12 4 0 33.46 3.15 -13 -4 0 3.72 0.97 13 4 0 2.93 1.42 -13 4 0 3.80 1.48 13 4 0 1.54 1.22 -14 -4 0 20.55 2.24 14 4 0 26.69 3.00 14 4 0 19.38 2.57 -14 4 0 16.28 2.74 -15 -4 0 8.80 1.49 -15 4 0 7.45 1.94 15 4 0 8.69 1.97 -16 -4 0 5.70 1.32 -16 4 0 3.50 1.65 0 -5 0 1.26 0.34 0 -5 0 2.06 1.10 0 5 0 1.21 0.59 0 5 0 -0.47 0.36 1 -5 0 95.02 5.80 -1 -5 0 100.70 5.97 1 -5 0 78.23 7.93 -1 -5 0 102.55 7.98 -1 5 0 89.74 6.41 -1 5 0 89.92 5.65 1 5 0 95.74 6.41 1 5 0 88.88 5.66 2 -5 0 8.05 1.86 -2 -5 0 8.42 1.06 -2 -5 0 11.26 1.73 2 5 0 10.50 1.18 -2 5 0 9.42 1.18 2 5 0 9.33 0.99 -2 5 0 11.88 1.02 3 -5 0 3.56 1.45 -3 -5 0 5.82 0.96 -3 -5 0 3.35 1.12 3 5 0 6.46 0.93 -3 5 0 4.36 0.92 3 5 0 5.85 0.76 4 -5 0 30.89 3.63 -4 -5 0 35.56 3.27 -4 -5 0 31.21 2.67 4 5 0 35.82 2.36 4 5 0 34.30 2.63 -4 5 0 36.29 2.86 -5 -5 0 11.19 1.51 -5 -5 0 7.97 1.28 5 -5 0 11.25 1.96 -5 5 0 7.60 1.24 5 5 0 8.20 0.96 5 5 0 7.45 1.05 -6 -5 0 37.72 3.00 6 -5 0 44.44 3.95 -6 -5 0 34.45 3.36 6 5 0 39.19 2.56 6 5 0 35.40 2.83 -6 5 0 36.00 3.08 -7 -5 0 4.06 1.08 7 -5 0 5.16 1.46 -7 5 0 4.90 1.07 7 5 0 4.43 0.85 7 5 0 4.78 0.78 8 -5 0 9.78 1.80 -8 -5 0 11.89 1.60 8 5 0 10.33 1.34 -8 5 0 11.92 1.62 8 5 0 12.61 1.29 9 -5 0 6.12 1.44 -9 -5 0 6.60 1.26 -9 5 0 6.60 1.30 9 5 0 6.60 1.08 9 5 0 5.72 0.95 10 -5 0 0.57 0.93 -10 -5 0 0.57 0.72 10 5 0 0.46 0.70 10 5 0 1.59 0.72 -10 5 0 0.41 0.97 -11 -5 0 45.70 3.58 11 5 0 44.23 3.31 11 5 0 45.32 3.69 -11 5 0 48.27 4.07 -12 -5 0 4.83 1.18 -12 5 0 3.58 1.51 12 5 0 3.77 1.20 12 5 0 8.45 1.58 -13 -5 0 36.83 3.14 13 5 0 36.57 3.24 -13 5 0 34.22 3.97 13 5 0 39.25 3.58 -14 -5 0 6.16 1.35 -14 5 0 6.22 1.95 14 5 0 8.03 1.76 -15 -5 0 6.37 1.36 -15 5 0 2.78 1.79 15 5 0 5.76 1.77 0 -6 0 25.23 3.18 0 6 0 19.51 1.53 0 6 0 20.15 1.86 -1 -6 0 2.82 1.38 1 -6 0 3.05 1.56 -1 6 0 2.83 0.56 1 6 0 1.52 0.52 1 6 0 1.29 0.73 -1 6 0 3.04 0.80 -2 -6 0 13.00 2.12 2 -6 0 11.01 2.31 -2 -6 0 13.29 1.34 2 6 0 12.50 1.21 2 6 0 11.01 1.37 -2 6 0 13.40 1.50 -2 6 0 11.16 1.14 3 -6 0 13.50 2.74 -3 -6 0 18.97 2.42 3 6 0 16.66 1.43 -3 6 0 20.51 1.91 3 6 0 18.61 1.70 -3 6 0 15.47 1.40 -4 -6 0 2.26 0.85 -4 -6 0 1.07 0.97 4 -6 0 0.00 1.24 -4 6 0 2.82 0.96 4 6 0 2.19 0.75 4 6 0 1.12 0.57 5 -6 0 9.35 2.05 -5 -6 0 9.94 1.64 -5 -6 0 7.75 1.41 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5.60 -3 -7 0 62.21 5.48 3 7 0 56.04 3.80 3 7 0 59.29 4.31 -3 7 0 63.34 3.84 -3 7 0 60.68 4.47 4 -7 0 44.67 5.65 -4 -7 0 65.62 4.33 -4 -7 0 57.71 5.34 4 7 0 56.44 3.84 -4 7 0 60.57 4.58 4 7 0 62.76 4.36 -4 7 0 57.93 3.86 -5 -7 0 14.20 1.90 5 -7 0 10.03 2.44 -5 -7 0 13.28 2.13 -5 7 0 17.61 2.02 -5 7 0 21.40 1.54 5 7 0 13.79 1.69 5 7 0 13.92 1.48 -6 -7 0 60.17 5.43 -6 -7 0 51.29 4.51 6 -7 0 59.17 5.90 6 7 0 66.86 4.55 -6 7 0 69.64 4.89 6 7 0 56.85 4.00 -7 -7 0 5.21 1.41 7 -7 0 4.82 1.70 7 7 0 6.66 1.13 7 7 0 5.85 0.94 -7 7 0 5.91 1.43 8 -7 0 36.11 3.86 -8 -7 0 33.24 3.10 -8 7 0 34.33 3.23 8 7 0 32.63 2.52 9 -7 0 19.33 2.91 -9 -7 0 20.44 2.57 9 7 0 22.41 1.91 -9 7 0 26.49 2.79 -10 -7 0 9.33 1.79 10 -7 0 5.84 1.68 -10 7 0 10.11 1.85 -11 -7 0 37.85 3.48 -11 7 0 39.56 3.81 -12 -7 0 -0.31 1.10 -12 7 0 -0.20 1.39 -13 -7 0 38.81 3.35 -13 7 0 26.86 3.73 0 -8 0 -0.66 1.31 0 8 0 0.20 0.75 0 8 0 0.28 0.49 1 -8 0 -0.21 1.41 -1 -8 0 0.48 1.34 1 8 0 0.15 0.51 -1 8 0 -0.01 0.47 -1 8 0 -0.23 0.75 1 8 0 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4.35 0.60 -2 4 -4 5.09 0.86 -2 4 -4 4.46 0.47 -3 -4 -4 37.95 2.67 -3 -4 -4 41.42 3.40 3 -4 4 36.53 3.93 -3 4 -4 39.22 2.98 3 4 4 39.20 2.55 3 4 4 37.02 2.66 -3 4 -4 35.22 2.40 4 -4 4 58.84 5.21 -4 -4 -4 57.29 3.77 -4 -4 -4 53.50 4.55 4 4 4 53.41 3.73 -4 4 -4 55.88 4.08 4 4 4 48.62 3.46 5 -4 4 45.80 4.46 -5 -4 -4 44.29 3.85 -5 -4 -4 45.27 3.34 5 4 4 46.23 3.02 5 4 4 44.59 3.21 -5 4 -4 44.84 3.51 6 -4 4 80.45 6.95 -6 -4 -4 78.35 6.43 -6 -4 -4 81.64 5.54 -6 4 -4 81.27 5.76 6 4 4 80.40 5.46 6 4 4 75.06 4.97 -7 -4 -4 2.11 0.90 7 -4 4 1.38 1.11 -7 4 -4 2.76 0.94 7 4 4 2.47 0.67 7 4 4 1.44 0.66 -8 -4 -4 42.42 3.83 8 -4 4 50.63 4.67 -8 4 -4 52.57 4.01 8 4 4 51.31 3.39 8 4 4 50.76 3.77 -9 -4 -4 2.77 1.12 9 -4 4 2.88 1.21 -9 4 -4 1.01 0.95 9 4 4 2.88 0.81 -10 -4 -4 5.37 1.37 10 4 4 7.44 1.18 -10 4 -4 6.94 1.53 -11 -4 -4 12.96 1.88 11 4 4 13.67 1.69 -11 4 -4 12.16 2.08 -12 -4 -4 0.71 0.96 12 4 4 0.43 0.97 -12 4 -4 0.63 1.15 -13 -4 -4 9.48 1.65 -13 4 -4 12.55 2.29 13 4 4 7.60 1.77 -14 -4 -4 2.80 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7.57 2.03 -7 -2 22 18.67 3.42 7 -2 -22 18.90 1.96 7 2 -22 21.28 2.08 -7 2 22 15.71 2.93 6 -2 -22 0.91 0.65 -6 -2 22 0.59 1.47 6 2 -22 1.01 0.69 -6 2 22 1.60 1.23 -5 -2 22 28.14 4.34 5 -2 -22 28.51 2.43 5 2 -22 28.90 2.49 -5 2 22 29.86 4.00 -4 -2 22 5.72 2.24 4 -2 -22 12.15 1.49 4 2 -22 9.15 1.35 -4 2 22 8.63 2.06 -3 -2 22 13.29 2.84 3 -2 -22 9.98 1.49 -3 2 22 10.70 2.25 3 2 -22 10.56 1.52 -2 -2 22 28.97 4.47 2 -2 -22 35.07 2.82 2 2 -22 32.13 2.74 -2 2 22 32.61 3.77 1 -2 -22 -0.80 0.61 -1 -2 22 1.83 1.52 -1 2 22 0.82 1.08 1 2 -22 0.43 0.75 0 -2 -22 54.22 3.89 0 -2 22 49.89 5.42 0 2 22 46.13 4.96 0 2 -22 48.21 3.81 -1 -2 -22 3.59 1.02 1 -2 22 1.98 1.68 -1 2 -22 2.33 0.96 1 2 22 5.23 1.60 -2 -2 -22 42.44 3.67 2 -2 22 50.11 5.25 2 2 22 43.47 4.74 -2 2 -22 53.42 3.79 3 -2 22 12.49 2.63 3 2 22 7.95 1.97 -3 2 -22 10.64 1.61 -10 3 22 0.81 1.15 -9 -3 22 9.62 2.65 9 -3 -22 13.38 1.60 -9 3 22 12.84 2.50 8 -3 -22 4.81 1.01 -8 -3 22 2.99 2.02 -8 3 22 1.95 1.38 8 3 -22 5.44 1.09 -7 -3 22 2.53 1.89 7 -3 -22 1.24 0.76 -7 3 22 2.75 1.39 7 3 -22 3.01 0.89 -6 -3 22 2.03 2.01 6 -3 -22 4.74 1.02 -6 3 22 4.28 1.67 6 3 -22 4.22 1.05 -5 -3 22 -1.45 1.51 5 -3 -22 0.36 0.65 5 3 -22 1.10 0.78 -5 3 22 -0.24 1.03 4 -3 -22 5.02 1.10 -4 -3 22 4.02 2.15 -4 3 22 4.71 1.64 4 3 -22 3.08 0.96 -3 -3 22 -0.64 1.50 3 -3 -22 1.00 0.71 3 3 -22 -0.33 0.71 -3 3 22 0.89 1.13 -2 -3 22 0.83 1.69 2 -3 -22 1.05 0.77 -2 3 22 0.62 1.04 2 3 -22 1.05 0.76 1 -3 -22 3.85 1.05 -1 -3 22 3.40 1.94 -1 3 22 2.21 1.26 1 3 -22 3.04 0.99 0 -3 22 1.02 1.57 0 -3 -22 1.20 0.78 0 3 -22 -0.11 0.73 0 3 22 0.07 1.04 1 -3 22 8.42 2.46 -1 -3 -22 11.08 1.61 1 3 22 8.46 1.98 -1 3 -22 12.70 1.65 -2 3 -22 1.81 0.90 2 3 22 0.14 1.14 -8 -4 22 15.92 3.55 -7 -4 22 6.57 2.65 6 -4 -22 3.81 0.99 -6 -4 22 3.41 2.27 6 4 -22 2.73 1.01 -5 -4 22 4.51 2.36 5 -4 -22 9.33 1.36 5 4 -22 5.53 1.24 4 -4 -22 1.76 0.87 -4 -4 22 0.53 2.02 4 4 -22 2.02 0.91 3 -4 -22 2.83 0.99 3 4 -22 2.87 0.95 2 -4 -22 6.22 1.26 2 4 -22 4.87 1.15 1 -4 -22 0.66 0.84 1 4 -22 1.86 0.89 0 4 -22 19.61 2.13 -10 0 23 -0.02 1.27 -9 0 23 -0.86 1.15 9 0 -23 -0.07 0.65 8 0 -23 0.67 0.67 -8 0 23 0.57 1.40 7 0 -23 0.17 0.60 -7 0 23 -1.05 1.22 -6 0 23 -0.36 1.26 6 0 -23 -0.22 0.56 5 0 -23 -0.02 0.58 -5 0 23 0.37 1.37 4 0 -23 0.19 0.64 -4 0 23 -0.57 1.18 3 0 -23 -0.13 0.61 -3 0 23 0.28 1.24 2 0 -23 1.47 0.78 -2 0 23 0.07 1.12 1 0 -23 -0.07 0.65 -1 0 23 0.63 1.20 0 0 23 1.11 1.26 0 0 -23 0.78 0.77 -1 0 -23 0.74 0.81 1 0 23 -0.14 1.10 2 0 23 1.78 1.47 -10 -1 23 62.64 6.63 -10 1 23 70.43 6.67 -9 -1 23 -0.33 1.29 9 -1 -23 1.11 0.73 -9 1 23 -0.26 1.11 -8 -1 23 42.76 5.57 8 -1 -23 45.39 3.41 8 1 -23 45.61 3.44 -8 1 23 41.60 4.95 -7 -1 23 17.13 3.32 7 -1 -23 16.59 1.80 7 1 -23 13.49 1.67 -7 1 23 16.51 3.07 6 -1 -23 4.83 1.06 -6 -1 23 6.99 2.19 -6 1 23 11.49 2.58 6 1 -23 8.53 1.26 5 -1 -23 38.12 2.94 -5 -1 23 35.35 4.98 -5 1 23 40.36 4.99 5 1 -23 32.49 2.86 -4 -1 23 0.76 1.47 4 -1 -23 0.35 0.64 -4 1 23 0.21 1.10 4 1 -23 1.13 0.72 -3 -1 23 13.82 2.77 3 -1 -23 12.92 1.69 -3 1 23 14.05 2.69 3 1 -23 13.68 1.72 2 -1 -23 10.69 1.54 -2 -1 23 10.31 2.47 -2 1 23 10.62 2.35 2 1 -23 8.89 1.43 -1 -1 23 1.17 1.38 1 -1 -23 1.62 0.87 1 1 -23 2.13 0.90 -1 1 23 1.27 1.30 0 -1 -23 36.05 3.06 0 -1 23 34.64 4.61 0 1 -23 34.87 3.03 0 1 23 37.64 4.21 1 -1 23 -0.04 1.25 1 1 23 0.42 1.14 -1 1 -23 0.47 0.77 -9 -2 23 9.16 2.54 9 -2 -23 7.85 1.26 -9 2 23 6.55 1.99 8 -2 -23 0.16 0.64 -8 -2 23 -0.94 1.39 -8 2 23 0.20 1.13 7 -2 -23 0.10 0.67 -7 -2 23 1.20 1.75 7 2 -23 0.58 0.71 -7 2 23 1.07 1.27 6 -2 -23 5.03 1.03 -6 -2 23 3.17 1.90 -6 2 23 4.25 1.75 6 2 -23 4.12 1.02 -5 -2 23 -1.05 1.49 5 -2 -23 1.11 0.71 5 2 -23 -0.01 0.64 -5 2 23 1.10 1.19 -4 -2 23 2.49 1.90 4 -2 -23 2.97 0.95 -4 2 23 2.58 1.40 4 2 -23 2.88 0.92 3 -2 -23 0.17 0.66 -3 -2 23 1.01 1.54 3 2 -23 -0.22 0.67 -3 2 23 0.25 1.06 2 -2 -23 0.39 0.74 -2 -2 23 0.50 1.58 -2 2 23 -0.04 1.00 2 2 -23 -1.18 0.62 1 -2 -23 2.51 0.96 -1 -2 23 2.20 1.66 -1 2 23 0.03 1.10 1 2 -23 2.13 0.86 0 2 -23 0.57 0.79 0 2 23 0.88 1.13 -1 2 -23 6.84 1.35 -8 -3 23 19.47 3.77 8 -3 -23 20.23 2.08 7 -3 -23 21.28 2.19 -7 -3 23 20.73 4.00 -6 -3 23 2.94 2.35 6 -3 -23 6.44 1.18 5 -3 -23 22.44 2.14 -5 -3 23 11.13 3.36 5 3 -23 17.53 2.03 4 -3 -23 0.39 0.77 4 3 -23 1.22 0.79 3 -3 -23 9.46 1.45 3 3 -23 6.26 1.26 2 -3 -23 26.99 2.37 2 3 -23 20.41 2.31 1 3 -23 2.49 0.96 0 3 -23 34.05 2.93 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 9759 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp C1 C 0.7783(5) 0.3966(9) 0.3549(3) 0.0189(14) Uani 1 1 d . . C2 C 0.7837(5) 0.2342(8) 0.3206(3) 0.0162(13) Uani 1 1 d . . C3 C 0.8706(4) 0.1445(8) 0.3325(3) 0.0157(13) Uani 1 1 d . . H3 H 0.9270 0.1920 0.3627 0.019 Uiso 1 1 calc R U C4 C 0.8751(6) -0.0060(10) 0.3022(4) 0.0317(18) Uani 1 1 d . . H4 H 0.9346 -0.0650 0.3117 0.038 Uiso 1 1 calc R U C5 C 0.7930(5) -0.0807(9) 0.2558(4) 0.0248(16) Uani 1 1 d . . H5 H 0.7974 -0.1874 0.2336 0.030 Uiso 1 1 calc R U C6 C 0.7062(5) 0.0050(8) 0.2435(4) 0.0232(15) Uani 1 1 d . . H6 H 0.6503 -0.0441 0.2133 0.028 Uiso 1 1 calc R U C7 C 0.7005(5) 0.1613(8) 0.2749(3) 0.0178(14) Uani 1 1 d . . H7 H 0.6410 0.2201 0.2658 0.021 Uiso 1 1 calc R U C8 C 0.6877(5) 0.4539(9) 0.3693(3) 0.0189(14) Uani 1 1 d . . C9 C 0.6244(5) 0.3410(9) 0.3925(3) 0.0209(14) Uani 1 1 d . . H9 H 0.6392 0.2240 0.3968 0.025 Uiso 1 1 calc R U C10 C 0.5413(5) 0.4000(10) 0.4090(4) 0.0282(17) Uani 1 1 d . . H10 H 0.5002 0.3242 0.4267 0.034 Uiso 1 1 calc R U C11 C 0.5169(5) 0.5686(10) 0.4000(4) 0.0290(18) Uani 1 1 d . . H11 H 0.4584 0.6070 0.4105 0.035 Uiso 1 1 calc R U C12 C 0.5765(5) 0.6820(9) 0.3759(3) 0.0243(16) Uani 1 1 d . . H12 H 0.5585 0.7974 0.3688 0.029 Uiso 1 1 calc R U C13 C 0.6629(5) 0.6264(9) 0.3620(3) 0.0218(15) Uani 1 1 d . . H13 H 0.7055 0.7048 0.3476 0.026 Uiso 1 1 calc R U C14 C 0.8624(5) 0.5012(8) 0.3776(3) 0.0186(14) Uani 1 1 d . . C15 C 0.8738(5) 0.6027(9) 0.4411(3) 0.0208(14) Uani 1 1 d . . H15 H 0.8242 0.6060 0.4674 0.025 Uiso 1 1 calc R U C16 C 0.9549(5) 0.6955(8) 0.4650(3) 0.0198(14) Uani 1 1 d . . H16 H 0.9614 0.7617 0.5082 0.024 Uiso 1 1 calc R U C17 C 1.0285(5) 0.6953(9) 0.4274(4) 0.0244(15) Uani 1 1 d . . H17 H 1.0851 0.7602 0.4449 0.029 Uiso 1 1 calc R U C18 C 1.0184(5) 0.5986(9) 0.3635(4) 0.0247(15) Uani 1 1 d . . H18 H 1.0676 0.6000 0.3368 0.030 Uiso 1 1 calc R U C19 C 0.9375(5) 0.5014(8) 0.3391(4) 0.0208(15) Uani 1 1 d . . H19 H 0.9319 0.4341 0.2963 0.025 Uiso 1 1 calc R U Cl1 Cl 0.86998(12) 0.9311(2) 0.64722(9) 0.0264(4) Uani 1 1 d . . Cl2 Cl 0.70421(12) 0.6767(2) 0.56148(8) 0.0243(4) Uani 1 1 d . . Cl3 Cl 0.64426(14) 0.9482(2) 0.67353(9) 0.0289(4) Uani 1 1 d . . Cl4 Cl 0.72977(13) 1.2544(2) 0.59122(10) 0.0291(4) Uani 1 1 d . . Cl5 Cl 0.78616(12) 0.9874(2) 0.47279(8) 0.0230(4) Uani 1 1 d . . O1 O 0.6030(3) 0.9948(8) 0.5081(3) 0.0434(15) Uani 1 1 d D . W1 W 0.70594(2) 0.96874(3) 0.56799(2) 0.01860(11) 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 C1 0.020(4) 0.029(4) 0.007(3) 0.005(3) 0.003(3) 0.004(3) C2 0.022(4) 0.017(3) 0.009(3) 0.002(2) 0.004(3) 0.002(3) C3 0.015(3) 0.022(3) 0.011(3) -0.003(2) 0.005(2) 0.001(3) C4 0.029(4) 0.043(5) 0.025(4) -0.004(3) 0.010(3) 0.011(4) C5 0.036(4) 0.023(4) 0.018(3) 0.006(3) 0.012(3) 0.004(3) C6 0.026(4) 0.027(4) 0.015(3) -0.005(3) 0.001(3) -0.004(3) C7 0.018(3) 0.022(3) 0.014(3) 0.007(3) 0.005(3) 0.005(3) C8 0.018(3) 0.029(4) 0.008(3) -0.005(3) -0.003(3) -0.002(3) C9 0.017(3) 0.027(4) 0.018(3) -0.002(3) 0.003(3) -0.002(3) C10 0.021(4) 0.047(5) 0.016(3) -0.005(3) 0.004(3) -0.004(3) C11 0.015(4) 0.049(5) 0.022(4) -0.018(3) 0.003(3) 0.003(3) C12 0.026(4) 0.032(4) 0.013(3) -0.007(3) -0.001(3) 0.008(3) C13 0.028(4) 0.023(4) 0.012(3) -0.004(3) 0.000(3) 0.003(3) C14 0.019(4) 0.021(4) 0.017(3) 0.004(3) 0.008(3) 0.001(3) C15 0.020(4) 0.026(4) 0.017(3) 0.003(3) 0.006(3) 0.010(3) C16 0.022(4) 0.018(3) 0.019(3) 0.000(3) 0.002(3) 0.004(3) C17 0.021(4) 0.022(4) 0.028(4) 0.005(3) 0.000(3) -0.005(3) C18 0.023(4) 0.027(4) 0.028(4) 0.003(3) 0.014(3) -0.003(3) C19 0.022(4) 0.024(4) 0.019(3) 0.002(3) 0.011(3) 0.002(3) Cl1 0.0210(9) 0.0326(10) 0.0230(8) 0.0048(7) -0.0007(7) -0.0025(7) Cl2 0.0310(9) 0.0245(9) 0.0202(8) -0.0040(7) 0.0115(7) -0.0077(7) Cl3 0.0376(11) 0.0326(10) 0.0233(8) -0.0033(7) 0.0211(8) -0.0034(8) Cl4 0.0354(10) 0.0236(9) 0.0329(9) 0.0002(7) 0.0175(8) 0.0065(8) Cl5 0.0285(9) 0.0261(9) 0.0175(8) 0.0022(6) 0.0114(7) 0.0039(7) O1 0.034(3) 0.069(4) 0.025(3) 0.008(3) 0.003(3) 0.005(3) W1 0.01732(17) 0.02488(17) 0.01518(15) -0.00008(11) 0.00695(11) 0.00032(12) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 '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 C14 C1 C2 121.1(6) C14 C1 C8 118.9(6) C2 C1 C8 119.9(6) C3 C2 C7 118.6(6) C3 C2 C1 120.9(6) C7 C2 C1 120.5(6) C4 C3 C2 120.9(6) C4 C3 H3 119.6 C2 C3 H3 119.6 C3 C4 C5 121.4(7) C3 C4 H4 119.3 C5 C4 H4 119.3 C6 C5 C4 118.8(7) C6 C5 H5 120.6 C4 C5 H5 120.6 C7 C6 C5 120.3(7) C7 C6 H6 119.8 C5 C6 H6 119.8 C6 C7 C2 120.0(6) C6 C7 H7 120.0 C2 C7 H7 120.0 C9 C8 C13 118.7(6) C9 C8 C1 121.3(6) C13 C8 C1 120.0(6) C10 C9 C8 120.0(7) C10 C9 H9 120.0 C8 C9 H9 120.0 C9 C10 C11 120.6(7) C9 C10 H10 119.7 C11 C10 H10 119.7 C10 C11 C12 120.8(6) C10 C11 H11 119.6 C12 C11 H11 119.6 C11 C12 C13 119.6(7) C11 C12 H12 120.2 C13 C12 H12 120.2 C12 C13 C8 120.3(7) C12 C13 H13 119.9 C8 C13 H13 119.9 C15 C14 C19 118.0(6) C15 C14 C1 120.3(6) C19 C14 C1 121.7(6) C16 C15 C14 120.9(6) C16 C15 H15 119.6 C14 C15 H15 119.6 C15 C16 C17 121.1(6) C15 C16 H16 119.4 C17 C16 H16 119.4 C16 C17 C18 119.3(6) C16 C17 H17 120.4 C18 C17 H17 120.4 C19 C18 C17 120.4(6) C19 C18 H18 119.8 C17 C18 H18 119.8 C18 C19 C14 120.3(6) C18 C19 H19 119.8 C14 C19 H19 119.8 O1 W1 Cl4 94.4(2) O1 W1 Cl2 95.3(2) Cl4 W1 Cl2 170.24(6) O1 W1 Cl5 89.39(17) Cl4 W1 Cl5 90.26(6) Cl2 W1 Cl5 91.40(6) O1 W1 Cl3 97.72(18) Cl4 W1 Cl3 88.68(6) Cl2 W1 Cl3 88.48(6) Cl5 W1 Cl3 172.87(6) O1 W1 Cl1 173.85(17) Cl4 W1 Cl1 85.81(6) Cl2 W1 Cl1 84.78(6) Cl5 W1 Cl1 84.46(6) Cl3 W1 Cl1 88.43(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 C14 1.442(9) C1 C2 1.447(9) C1 C8 1.452(9) C2 C3 1.403(9) C2 C7 1.419(9) C3 C4 1.328(10) C3 H3 0.9500 C4 C5 1.421(11) C4 H4 0.9500 C5 C6 1.385(10) C5 H5 0.9500 C6 C7 1.381(9) C6 H6 0.9500 C7 H7 0.9500 C8 C9 1.408(9) C8 C13 1.410(10) C9 C10 1.374(10) C9 H9 0.9500 C10 C11 1.380(11) C10 H10 0.9500 C11 C12 1.382(10) C11 H11 0.9500 C12 C13 1.388(10) C12 H12 0.9500 C13 H13 0.9500 C14 C15 1.412(9) C14 C19 1.419(9) C15 C16 1.359(10) C15 H15 0.9500 C16 C17 1.391(9) C16 H16 0.9500 C17 C18 1.398(10) C17 H17 0.9500 C18 C19 1.377(10) C18 H18 0.9500 C19 H19 0.9500 Cl1 W1 2.4893(17) Cl2 W1 2.3165(17) Cl3 W1 2.3414(16) Cl4 W1 2.3145(18) Cl5 W1 2.3292(16) O1 W1 1.647(4) 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 C14 C1 C2 C3 24.3(9) C8 C1 C2 C3 -153.4(6) C14 C1 C2 C7 -156.5(6) C8 C1 C2 C7 25.8(8) C7 C2 C3 C4 -0.5(9) C1 C2 C3 C4 178.7(6) C2 C3 C4 C5 0.9(10) C3 C4 C5 C6 -1.3(10) C4 C5 C6 C7 1.1(10) C5 C6 C7 C2 -0.7(9) C3 C2 C7 C6 0.3(9) C1 C2 C7 C6 -178.9(6) C14 C1 C8 C9 -140.0(6) C2 C1 C8 C9 37.8(8) C14 C1 C8 C13 38.3(8) C2 C1 C8 C13 -143.9(6) C13 C8 C9 C10 -1.3(9) C1 C8 C9 C10 177.1(6) C8 C9 C10 C11 2.8(10) C9 C10 C11 C12 -1.4(10) C10 C11 C12 C13 -1.4(10) C11 C12 C13 C8 2.8(9) C9 C8 C13 C12 -1.5(9) C1 C8 C13 C12 -179.9(6) C2 C1 C14 C15 -145.6(6) C8 C1 C14 C15 32.2(9) C2 C1 C14 C19 32.1(9) C8 C1 C14 C19 -150.2(6) C19 C14 C15 C16 -1.0(9) C1 C14 C15 C16 176.8(6) C14 C15 C16 C17 0.8(10) C15 C16 C17 C18 0.4(10) C16 C17 C18 C19 -1.6(10) C17 C18 C19 C14 1.4(10) C15 C14 C19 C18 -0.2(10) C1 C14 C19 C18 -177.9(6)