#------------------------------------------------------------------------------ #$Date: 2021-06-05 22:28:01 +0300 (Sat, 05 Jun 2021) $ #$Revision: 266163 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/15/80/7158031.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_7158031 loop_ _publ_author_name 'Warghude, Prakash K.' 'Sabale, Abhijeet S.' 'Dixit, Ruchi' 'Vanka, Kumar' 'Bhat, Ramakrishna G.' _publ_section_title ; An easy and practical approach to access multifunctional cylcopentadiene- and cyclopentene-spirooxindoles via [3 + 2] annulation. ; _journal_issue 19 _journal_name_full 'Organic & biomolecular chemistry' _journal_page_first 4338 _journal_page_last 4345 _journal_paper_doi 10.1039/d1ob00514f _journal_volume 19 _journal_year 2021 _chemical_formula_sum 'C29 H22 Cl3 N O5' _chemical_formula_weight 570.82 _chemical_melting_point 445.0(10) _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2021-03-03 deposited with the CCDC. 2021-04-20 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 94.36(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.170(14) _cell_length_b 29.30(4) _cell_length_c 9.624(15) _cell_measurement_reflns_used 3099 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 20.14 _cell_measurement_theta_min 2.53 _cell_volume 2578(7) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2014 (Sheldrick 2014)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method 'Omega and phi scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1421 _diffrn_reflns_av_unetI/netI 0.1100 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 38011 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.473 _diffrn_reflns_theta_min 1.390 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 0.398 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.6099 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.471 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1176 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Chloroform-Hexane' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.09 _refine_diff_density_max 0.625 _refine_diff_density_min -0.603 _refine_diff_density_rms 0.093 _refine_ls_extinction_coef 0.0127(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2014/7 (Sheldrick 2014' _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 347 _refine_ls_number_reflns 6463 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.029 _refine_ls_R_factor_all 0.1200 _refine_ls_R_factor_gt 0.0599 _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^)+(0.0571P)^2^+1.1427P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1314 _refine_ls_wR_factor_ref 0.1580 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3866 _reflns_number_total 6463 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1ob00514f2.cif _cod_data_source_block TRI_a _cod_depositor_comments ; The following automatic conversions were performed: data item '_chemical_melting_point' value '444-446' was changed to '445.0(10)' -- the average value was taken and precision was estimated. Automatic conversion script Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas Adding full bibliography for 7158031--7158034.cif. ; _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 7158031 _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_res_file ; TRI_a.res created by SHELXL-2014/7 TITL TRI_a.res in P2(1)/n CELL 0.71073 9.1699 29.3010 9.6237 90.000 94.355 90.000 ZERR 4.000 0.0142 0.0417 0.0148 0.000 0.024 0.000 LATT 1 SYMM 1/2-X, 1/2+Y, 1/2-Z SFAC C H N O Cl UNIT 116 88 4 20 12 LIST 6 ! automatically inserted. Change 6 to 4 for CHECKCIF!! REM Old TITL TRI in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.183, Rweak 0.015, Alpha 0.029, Orientation as input REM Formula found by SHELXT: C29 N O5 Cl3 L.S. 10 ACTA BOND $H FMAP 2 PLAN 20 TEMP -173.000 WGHT 0.057100 1.142700 EXTI 0.012727 FVAR 0.44388 CL1 5 0.529576 0.421942 0.201725 11.00000 0.02756 0.03348 = 0.02998 -0.00754 0.01003 -0.00668 CL2 5 0.824289 0.432409 0.128314 11.00000 0.02186 0.05609 = 0.05218 -0.02384 0.00394 -0.00298 CL3 5 0.587762 0.444230 -0.080490 11.00000 0.06296 0.11635 = 0.03120 0.02769 0.00871 0.04676 O3 4 0.438861 0.398436 0.488762 11.00000 0.01383 0.02604 = 0.01975 -0.00063 0.00064 0.00030 O1 4 0.171620 0.392737 0.067255 11.00000 0.02707 0.01830 = 0.01113 0.00197 -0.00005 -0.00150 O2 4 0.159322 0.445562 0.235413 11.00000 0.02698 0.01599 = 0.01862 0.00189 0.00147 0.00144 O4 4 0.274352 0.348513 0.727519 11.00000 0.03328 0.01854 = 0.01552 -0.00236 -0.00292 -0.00206 O5 4 0.318445 0.293934 0.934417 11.00000 0.02745 0.02376 = 0.01420 -0.00090 -0.00469 -0.00160 AFIX 147 H5 2 0.323248 0.318700 0.891036 11.00000 -1.50000 AFIX 0 N1 3 0.254021 0.440530 0.573402 11.00000 0.01436 0.01691 = 0.01417 -0.00110 -0.00206 -0.00193 C8 1 0.310566 0.404735 0.506526 11.00000 0.01658 0.01785 = 0.01295 0.00199 -0.00166 0.00059 C4 1 0.194729 0.323238 0.265759 11.00000 0.01594 0.01869 = 0.01058 -0.00083 -0.00175 -0.00162 AFIX 43 H4 2 0.194999 0.311203 0.174117 11.00000 -1.20000 AFIX 0 C14 1 0.052526 0.398241 0.505048 11.00000 0.01794 0.01357 = 0.01026 0.00239 -0.00079 0.00174 C5 1 0.212371 0.296212 0.393205 11.00000 0.01447 0.01683 = 0.01301 0.00061 -0.00101 0.00127 C6 1 0.201463 0.324724 0.502962 11.00000 0.01335 0.01712 = 0.01298 0.00288 -0.00244 0.00031 C2 1 0.167798 0.406291 0.199816 11.00000 0.01285 0.01953 = 0.01390 0.00018 -0.00033 0.00000 C9 1 0.102109 0.436948 0.576967 11.00000 0.01491 0.01787 = 0.01096 0.00328 -0.00168 0.00118 C3 1 0.178059 0.367529 0.296385 11.00000 0.01021 0.02122 = 0.01211 0.00093 -0.00092 -0.00106 C16 1 0.178064 0.274080 0.720005 11.00000 0.01469 0.02131 = 0.01216 0.00001 0.00126 0.00269 C22 1 0.243698 0.246896 0.384970 11.00000 0.01763 0.01951 = 0.01011 -0.00006 0.00133 -0.00038 C17 1 0.234649 0.264081 0.856763 11.00000 0.01634 0.02096 = 0.01475 -0.00264 0.00134 0.00405 C7 1 0.181305 0.373348 0.451866 11.00000 0.01503 0.01553 = 0.01153 -0.00003 -0.00094 -0.00040 C21 1 0.082887 0.242682 0.651926 11.00000 0.01616 0.02308 = 0.01597 -0.00097 0.00325 0.00213 AFIX 43 H21 2 0.040330 0.249421 0.561161 11.00000 -1.20000 AFIX 0 C15 1 0.220102 0.316687 0.654950 11.00000 0.01744 0.01927 = 0.01548 -0.00212 -0.00003 0.00329 C20 1 0.049905 0.202164 0.714380 11.00000 0.01726 0.01992 = 0.02173 -0.00107 0.00291 -0.00202 AFIX 43 H20 2 -0.016717 0.181405 0.667806 11.00000 -1.20000 AFIX 0 C23 1 0.363155 0.227901 0.460086 11.00000 0.02000 0.02182 = 0.01590 0.00212 -0.00059 0.00014 AFIX 43 H23 2 0.421122 0.246109 0.524597 11.00000 -1.20000 AFIX 0 C00Q 1 0.341375 0.476812 0.638821 11.00000 0.02001 0.01656 = 0.01958 -0.00174 -0.00060 -0.00432 AFIX 137 H00A 2 0.444056 0.472483 0.620200 11.00000 -1.50000 H00B 2 0.332361 0.476265 0.739627 11.00000 -1.50000 H00C 2 0.306900 0.506275 0.600967 11.00000 -1.50000 AFIX 0 C10 1 0.007411 0.466040 0.638316 11.00000 0.02085 0.01715 = 0.01530 -0.00084 -0.00020 0.00168 AFIX 43 H10 2 0.041960 0.492417 0.687908 11.00000 -1.20000 AFIX 0 C13 1 -0.093862 0.388020 0.491239 11.00000 0.01905 0.01888 = 0.01705 0.00192 -0.00283 -0.00039 AFIX 43 H13 2 -0.128087 0.361634 0.441507 11.00000 -1.20000 AFIX 0 C12 1 -0.191327 0.417093 0.551573 11.00000 0.01552 0.02090 = 0.02180 0.00423 0.00056 -0.00075 AFIX 43 H12 2 -0.293171 0.410701 0.542464 11.00000 -1.20000 AFIX 0 C11 1 -0.140431 0.455160 0.624551 11.00000 0.02021 0.02062 = 0.01669 0.00365 0.00354 0.00825 AFIX 43 H11 2 -0.208133 0.474380 0.666370 11.00000 -1.20000 AFIX 0 C18 1 0.205900 0.222550 0.917234 11.00000 0.02235 0.02575 = 0.01551 0.00375 0.00109 0.00364 AFIX 43 H18 2 0.248915 0.215285 1.007438 11.00000 -1.20000 AFIX 0 C26 1 0.191977 0.173844 0.276331 11.00000 0.03366 0.02139 = 0.01665 -0.00291 0.00122 -0.00363 AFIX 43 H26 2 0.132159 0.155242 0.214497 11.00000 -1.20000 AFIX 0 C24 1 0.398785 0.182422 0.441757 11.00000 0.02158 0.02448 = 0.02271 0.00544 0.00227 0.00577 AFIX 43 H24 2 0.481931 0.169728 0.492610 11.00000 -1.20000 AFIX 0 C27 1 0.157702 0.219508 0.293448 11.00000 0.02363 0.02181 = 0.01361 -0.00055 -0.00190 -0.00009 AFIX 43 H27 2 0.074776 0.232196 0.242230 11.00000 -1.20000 AFIX 0 C19 1 0.114295 0.191675 0.845787 11.00000 0.02249 0.02162 = 0.02559 0.00451 0.00455 0.00201 AFIX 43 H19 2 0.095189 0.163025 0.886901 11.00000 -1.20000 AFIX 0 C25 1 0.313786 0.155518 0.349808 11.00000 0.03608 0.01800 = 0.02159 -0.00098 0.00655 0.00222 AFIX 43 H25 2 0.338919 0.124428 0.336982 11.00000 -1.20000 AFIX 0 C1 1 0.168567 0.429057 -0.034565 11.00000 0.03700 0.02564 = 0.01429 0.00815 0.00172 0.00342 AFIX 137 H1A 2 0.073836 0.444645 -0.037371 11.00000 -1.50000 H1B 2 0.182916 0.416235 -0.126586 11.00000 -1.50000 H1C 2 0.246879 0.450914 -0.008772 11.00000 -1.50000 AFIX 0 C1S 1 0.648611 0.414649 0.069704 11.00000 0.01964 0.03150 = 0.02138 0.00100 0.00028 0.00041 AFIX 13 H1S 2 0.652466 0.381417 0.046607 11.00000 -1.20000 AFIX 0 HKLF 4 REM TRI_a.res in P2(1)/n REM R1 = 0.0599 for 3866 Fo > 4sig(Fo) and 0.1200 for all 6463 data REM 347 parameters refined using 0 restraints END WGHT 0.0571 1.1286 REM Highest difference peak 0.625, deepest hole -0.603, 1-sigma level 0.093 Q1 1 0.7891 0.4453 0.0440 11.00000 0.05 0.62 Q2 1 0.5351 0.4095 -0.0821 11.00000 0.05 0.53 Q3 1 0.7779 0.4108 0.1828 11.00000 0.05 0.41 Q4 1 0.7483 0.4611 -0.0141 11.00000 0.05 0.38 Q5 1 0.6042 0.4305 0.0957 11.00000 0.05 0.37 Q6 1 0.1782 0.3057 0.3371 11.00000 0.05 0.37 Q7 1 0.6891 0.4513 -0.0623 11.00000 0.05 0.37 Q8 1 0.7178 0.4205 0.1095 11.00000 0.05 0.36 Q9 1 0.2508 0.2346 0.4550 11.00000 0.05 0.35 Q10 1 0.1829 0.4373 0.5816 11.00000 0.05 0.35 Q11 1 0.1848 0.3687 0.3720 11.00000 0.05 0.35 Q12 1 -0.1269 0.4123 0.5055 11.00000 0.05 0.34 Q13 1 0.3287 0.2339 0.3971 11.00000 0.05 0.34 Q14 1 0.2356 0.3853 0.7624 11.00000 0.05 0.34 Q15 1 0.1983 0.2686 0.7917 11.00000 0.05 0.33 Q16 1 0.2854 0.3896 0.1925 11.00000 0.05 0.33 Q17 1 0.3826 0.2561 0.3494 11.00000 0.05 0.32 Q18 1 0.1814 0.4042 0.1374 11.00000 0.05 0.32 Q19 1 -0.0560 0.2390 0.4770 11.00000 0.05 0.32 Q20 1 0.1527 0.4315 0.6777 11.00000 0.05 0.32 ; _shelx_res_checksum 69958 _shelx_hkl_file ; -1 0 0 2.10 2.50 1 0 0 1.10 2.50 1 0 0 -1.40 2.30 -1 0 0 3.30 2.70 -1 0 0 1.20 2.10 1 0 0 0.80 2.30 -1 0 0 2.10 3.10 1 0 0 3.10 1.70 1 0 0 2.10 2.70 -1 0 0 0.60 1.50 2 0 0 7455.35 854.01 2 0 0 7315.47 855.11 -2 0 0 7240.98 853.91 2 0 0 7650.03 855.41 -2 0 0 8527.65 855.41 -2 0 0 8186.88 855.01 2 0 0 8106.49 855.01 -3 0 0 3.50 7.00 -3 0 0 -9.60 2.90 3 0 0 1.40 5.50 3 0 0 0.90 6.50 3 0 0 -1.60 4.70 -3 0 0 -1.50 5.20 3 0 0 -2.90 5.80 -3 0 0 -3.10 5.60 4 0 0 179.58 27.30 -4 0 0 203.28 26.30 -4 0 0 194.68 24.10 4 0 0 221.08 29.70 -4 0 0 196.28 29.60 4 0 0 228.48 26.10 -5 0 0 5.00 4.20 -5 0 0 -5.50 7.80 5 0 0 4.10 6.70 5 0 0 -0.90 6.40 -5 0 0 0.20 6.30 -6 0 0 943.21 100.69 -6 0 0 798.32 105.19 6 0 0 922.81 105.29 6 0 0 880.71 102.89 -7 0 0 3.80 5.20 7 0 0 -8.40 9.60 -7 0 0 16.30 13.10 8 0 0 1058.29 125.69 -9 0 0 14.90 20.90 9 0 0 3.70 14.90 -10 0 0 23.10 21.40 10 0 0 -9.80 16.90 11 0 0 5.10 17.70 -11 0 0 -5.40 22.90 12 0 0 60.59 34.20 -12 0 0 126.79 40.10 0 -1 0 0.20 0.30 0 -1 0 0.30 0.40 0 -1 0 0.00 0.20 0 1 0 -0.10 0.20 0 1 0 0.10 0.20 0 1 0 -0.10 0.40 1 -1 0 38.40 5.70 -1 -1 0 40.00 6.00 1 -1 0 33.40 5.80 1 -1 0 29.00 5.40 -1 -1 0 33.70 5.00 1 -1 0 28.50 5.20 -1 -1 0 30.50 4.50 -1 -1 0 31.80 6.30 1 1 0 27.90 4.80 -1 1 0 40.20 5.80 1 1 0 32.60 5.90 -1 1 0 30.90 5.70 1 1 0 43.10 6.30 -1 1 0 23.50 5.00 -1 1 0 34.50 5.70 -2 -1 0 2497.65 256.77 -2 -1 0 2432.86 258.17 2 -1 0 2321.87 257.37 -2 -1 0 2219.98 256.87 2 -1 0 2174.48 257.67 -2 -1 0 2145.29 257.67 2 -1 0 2393.76 257.57 2 -1 0 2534.95 257.77 -2 1 0 2315.17 257.37 -2 1 0 2384.16 257.67 2 1 0 2347.47 257.87 2 1 0 2438.26 256.77 2 1 0 2046.70 256.67 -2 1 0 2580.64 257.87 2 1 0 2298.67 257.47 -2 1 0 2198.28 256.37 -3 -1 0 4252.77 444.06 3 -1 0 4111.09 445.36 3 -1 0 3535.75 445.36 -3 -1 0 4215.48 445.96 -3 -1 0 3922.11 446.16 -3 -1 0 4346.37 444.96 3 -1 0 3712.43 445.66 3 1 0 3863.01 444.46 -3 1 0 3936.61 445.56 3 1 0 3916.51 445.36 -3 1 0 4128.89 445.86 -3 1 0 4101.19 443.76 3 1 0 4507.45 446.56 -3 1 0 4056.99 445.36 -3 1 0 3995.70 445.16 3 1 0 4187.68 445.96 3 1 0 3817.42 443.96 4 -1 0 137.69 22.00 -4 -1 0 135.49 23.80 -4 -1 0 153.28 19.60 4 -1 0 135.09 22.20 -4 -1 0 173.48 21.30 4 -1 0 172.18 24.10 4 1 0 128.29 21.30 -4 1 0 161.98 24.60 4 1 0 144.89 23.60 -4 1 0 203.18 22.30 4 1 0 171.68 19.70 4 1 0 169.38 23.20 -4 1 0 135.99 18.80 -4 1 0 213.18 23.00 -5 -1 0 655.93 71.99 -5 -1 0 589.04 70.09 5 -1 0 608.74 71.99 -5 -1 0 710.23 75.09 5 -1 0 628.64 73.59 5 1 0 522.35 72.69 -5 1 0 589.54 73.89 -5 1 0 618.64 69.59 5 1 0 664.53 71.69 -6 -1 0 510.95 56.49 6 -1 0 571.04 61.69 6 -1 0 484.45 59.19 -6 -1 0 477.65 61.89 -6 1 0 447.56 55.69 6 1 0 484.35 60.69 -6 1 0 504.35 61.59 -7 -1 0 88.49 23.70 7 -1 0 88.09 21.50 -7 -1 0 69.09 13.30 7 -1 0 90.49 18.50 -7 1 0 79.39 21.70 7 1 0 73.49 19.60 -7 1 0 99.69 13.30 -8 -1 0 6.20 18.30 8 -1 0 6.20 13.60 -8 -1 0 6.20 5.80 -8 1 0 -36.90 14.00 8 1 0 11.20 14.60 -9 -1 0 25.70 22.90 9 -1 0 80.09 21.50 9 1 0 62.09 21.40 -9 1 0 31.70 23.40 -10 -1 0 4.00 22.40 10 -1 0 27.30 19.30 -10 1 0 -7.30 19.40 10 1 0 13.00 21.70 -11 -1 0 206.08 45.40 11 -1 0 241.18 45.70 -11 1 0 300.47 52.69 11 1 0 142.09 39.80 12 -1 0 15.10 28.10 -12 -1 0 -26.10 27.40 12 1 0 46.10 27.80 12 1 0 22.00 26.40 -12 1 0 16.40 30.40 0 -2 0 0.90 1.30 0 -2 0 -0.10 0.50 0 -2 0 0.30 1.30 0 -2 0 0.80 1.20 0 2 0 0.50 1.40 0 2 0 -0.10 1.20 0 2 0 0.40 0.50 0 2 0 0.10 1.10 -1 -2 0 992.10 132.69 1 -2 0 1150.78 132.19 1 -2 0 1150.08 132.59 1 -2 0 1165.98 132.29 1 -2 0 1230.68 132.89 -1 -2 0 1322.27 132.49 1 2 0 1226.48 132.59 -1 2 0 1128.29 132.19 -1 2 0 1271.97 132.79 -1 2 0 1255.17 132.39 1 2 0 1162.38 132.39 1 2 0 1330.87 132.89 2 -2 0 2098.49 244.38 -2 -2 0 2093.59 244.98 2 -2 0 2128.29 244.18 2 -2 0 2256.97 244.48 -2 -2 0 2129.39 243.78 -2 -2 0 2137.59 244.78 2 2 0 2167.08 243.78 2 2 0 2208.78 244.78 -2 2 0 2091.09 244.58 -2 2 0 2096.19 244.18 2 2 0 2577.14 245.48 -2 2 0 2582.84 244.78 3 -2 0 2692.13 283.97 -3 -2 0 2671.43 282.97 3 -2 0 2739.33 284.37 3 -2 0 2707.93 284.47 -3 -2 0 2390.06 282.87 -3 -2 0 2885.31 285.47 -3 -2 0 2435.36 284.47 -3 2 0 2826.12 284.57 -3 2 0 2348.27 283.97 -3 2 0 2538.85 283.77 3 2 0 2450.95 284.37 3 2 0 2544.15 282.87 3 2 0 2501.15 284.07 -3 2 0 2318.07 282.17 3 2 0 2565.54 284.87 -3 2 0 2509.25 284.17 4 -2 0 278.67 39.20 4 -2 0 255.67 33.60 -4 -2 0 295.47 32.90 4 -2 0 369.06 34.90 4 -2 0 268.47 36.30 -4 -2 0 233.58 31.90 -4 -2 0 252.67 35.10 4 2 0 236.18 35.10 4 2 0 237.18 31.70 -4 2 0 271.07 31.10 4 2 0 274.67 37.20 -4 2 0 309.57 34.00 -4 2 0 301.67 34.80 -4 2 0 240.98 33.80 -5 -2 0 20.30 7.30 5 -2 0 4.80 9.10 -5 -2 0 20.50 6.70 -5 -2 0 -7.60 8.80 5 -2 0 11.50 7.80 -5 2 0 9.50 4.20 5 2 0 2.20 9.30 5 2 0 12.30 5.70 -5 2 0 11.50 10.40 -5 2 0 16.60 8.20 -6 -2 0 296.97 35.80 -6 -2 0 337.57 38.00 -6 -2 0 252.47 42.70 6 -2 0 316.27 42.40 6 -2 0 331.87 39.10 6 2 0 288.17 42.50 -6 2 0 277.67 34.30 -6 2 0 267.47 42.50 -7 -2 0 30.40 9.00 -7 -2 0 11.20 13.20 7 -2 0 70.29 17.40 7 -2 0 33.70 12.80 -7 2 0 7.00 13.00 7 2 0 33.60 14.60 -7 2 0 34.50 7.20 -8 -2 0 -6.40 5.90 8 -2 0 23.00 14.80 -8 -2 0 -35.70 15.80 8 2 0 14.60 14.00 -8 2 0 -33.00 14.90 -9 -2 0 55.99 24.80 9 -2 0 47.10 21.00 9 2 0 55.49 21.90 -9 2 0 60.69 25.10 -10 -2 0 34.10 23.00 10 -2 0 8.30 18.20 -10 2 0 36.10 24.40 10 2 0 25.20 21.60 -11 -2 0 21.50 22.60 11 -2 0 15.60 23.10 -11 2 0 61.89 29.00 11 2 0 70.89 29.30 12 -2 0 91.29 34.90 -12 -2 0 122.39 41.10 -12 2 0 62.49 32.90 12 2 0 48.20 28.80 12 2 0 120.59 38.30 0 -3 0 4.60 2.90 0 -3 0 12.20 3.40 0 -3 0 2.10 2.50 0 -3 0 0.00 1.60 0 3 0 -1.20 2.70 0 3 0 4.00 2.70 0 3 0 2.70 2.70 0 3 0 0.30 0.80 -1 -3 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2 12 21.00 31.40 -5 2 12 70.19 36.80 -4 -2 12 10.50 27.80 -4 -2 12 19.10 24.00 -4 2 12 -14.00 25.20 -4 2 12 -19.30 26.80 -3 -2 12 15.20 20.50 -3 -2 12 5.20 28.20 -3 -2 12 22.00 27.40 -3 2 12 -37.80 21.60 -3 2 12 9.60 24.80 -2 -2 12 2.60 24.20 -2 -2 12 36.50 27.80 -2 -2 12 32.50 27.80 -2 2 12 32.70 28.00 -2 2 12 25.60 21.00 -1 -2 12 -13.10 22.30 -1 -2 12 21.20 24.80 -1 -2 12 36.30 26.40 -1 2 12 67.89 29.40 -1 2 12 25.80 27.80 -1 2 12 74.29 32.10 0 -2 12 -4.10 18.60 0 -2 12 14.30 22.20 0 -2 12 37.20 23.80 0 -2 -12 15.10 23.50 0 2 12 7.10 19.10 0 2 -12 28.20 21.10 0 2 12 6.60 21.20 0 2 12 6.60 21.90 1 -2 12 35.90 22.50 1 -2 12 4.00 19.30 -1 -2 -12 -12.20 18.60 1 2 12 -22.90 13.70 -1 2 -12 25.50 24.00 1 2 12 -15.60 18.30 1 2 12 -7.60 19.20 1 2 12 -10.00 20.40 2 -2 12 -1.20 19.20 2 -2 12 10.20 20.10 -2 -2 -12 -4.30 25.10 2 2 12 -9.20 18.50 2 2 12 14.60 18.70 2 2 12 6.10 20.90 -2 2 -12 5.80 22.90 2 2 12 17.50 22.20 3 -2 12 -8.60 16.70 3 -2 12 -10.10 16.90 -3 2 -12 17.50 27.50 3 2 12 10.00 20.60 3 2 12 2.60 20.60 3 2 12 26.10 21.00 3 2 12 -4.90 18.90 -5 -3 12 15.80 28.30 -5 -3 12 11.40 26.40 -5 3 12 10.40 25.20 -5 3 12 3.60 27.30 -4 -3 12 -8.90 27.00 -4 -3 12 0.70 24.00 -4 3 12 6.70 27.40 -4 3 12 10.50 27.70 -3 -3 12 39.00 29.50 -3 -3 12 55.99 29.90 -3 -3 12 17.10 24.80 -3 3 12 37.00 25.50 -3 3 12 9.30 30.20 -2 -3 12 22.80 25.70 -2 -3 12 -7.10 22.50 -2 -3 12 18.80 20.50 -2 3 12 -12.60 18.80 -2 3 12 -5.40 23.90 -1 -3 12 24.30 21.80 -1 -3 12 -16.40 15.50 -1 -3 12 6.10 23.30 -1 3 12 -2.30 22.60 -1 3 12 7.80 18.10 0 -3 12 60.39 26.20 0 -3 12 52.99 28.20 0 -3 12 27.80 23.50 0 3 12 42.00 28.00 0 3 -12 45.60 23.70 0 3 12 29.20 23.30 0 3 12 45.90 24.60 1 -3 12 15.40 20.10 1 -3 12 27.70 23.70 1 3 12 20.80 23.30 1 3 12 20.80 23.40 -1 3 -12 23.00 20.70 1 3 12 8.50 22.30 2 -3 12 54.89 29.70 2 -3 12 87.69 27.60 2 3 12 46.90 30.60 -2 3 -12 35.70 27.40 2 3 12 42.20 21.40 2 3 12 65.29 27.90 2 3 12 43.80 29.70 3 -3 12 26.30 19.80 3 -3 12 2.50 22.30 -3 3 -12 -6.10 19.50 3 3 12 44.70 24.90 3 3 12 -4.20 20.90 3 3 12 -14.60 18.50 3 3 12 21.60 21.30 -5 -4 12 -57.99 23.10 -5 4 12 30.40 31.90 -4 -4 12 -14.50 18.60 -4 -4 12 -59.99 19.10 -4 -4 12 24.20 31.20 -4 4 12 15.50 27.30 -4 4 12 -11.40 21.10 -3 -4 12 6.90 27.90 -3 -4 12 -1.10 22.70 -3 -4 12 8.70 21.60 -3 4 12 14.10 26.00 -3 4 12 -10.50 21.10 -2 -4 12 -6.80 19.70 -2 -4 12 0.50 20.20 -2 -4 12 -14.30 22.20 -2 4 12 2.10 19.00 -2 4 12 -21.80 22.50 -1 -4 12 44.70 26.70 -1 -4 12 91.09 30.60 -1 -4 12 42.50 25.00 -1 4 12 43.50 29.60 1 4 -12 59.29 30.50 -1 4 12 17.70 26.00 0 -4 12 29.30 22.80 0 -4 12 17.60 24.80 0 4 12 -11.40 20.20 0 4 -12 20.90 20.50 0 4 12 1.80 22.90 0 4 12 27.80 26.20 1 -4 12 -1.70 19.00 1 -4 12 23.30 19.90 1 4 12 -3.20 18.90 -1 4 -12 7.40 26.00 1 4 12 42.30 26.00 1 4 12 31.00 23.30 2 -4 12 -20.30 12.70 2 -4 12 4.50 19.10 2 4 12 15.70 21.20 2 4 12 -5.40 15.90 -2 4 -12 2.10 22.20 2 4 12 12.80 23.10 2 4 12 -5.80 21.40 3 -4 12 -10.60 14.60 3 -4 12 24.80 23.90 -3 4 -12 14.30 26.20 3 4 12 -11.70 17.20 3 4 12 21.20 21.80 3 4 12 21.80 28.60 3 4 12 27.00 27.30 -5 -5 12 35.60 30.00 -4 -5 12 4.80 24.90 -4 -5 12 -10.00 25.90 -4 -5 12 15.60 31.90 -4 5 12 -26.40 22.10 -4 5 12 64.39 39.60 -3 -5 12 115.19 36.80 -3 -5 12 32.70 29.20 -3 -5 12 111.09 39.90 -3 5 12 76.69 34.30 -3 5 12 32.70 27.10 -2 -5 12 58.09 28.60 -2 -5 12 32.90 28.70 -2 -5 12 17.60 26.00 -2 5 12 42.80 29.40 -2 5 12 43.90 31.50 -1 -5 12 20.40 25.30 -1 -5 12 67.69 31.80 -1 -5 12 72.09 26.80 -1 5 12 -3.70 23.00 -1 5 12 49.20 24.40 1 5 -12 26.50 23.30 0 -5 12 52.89 27.20 0 -5 12 42.80 25.70 0 5 12 50.19 25.70 0 5 12 72.29 29.60 0 5 12 118.69 36.10 1 -5 12 -4.60 20.30 1 -5 12 -2.50 18.50 1 5 12 -3.90 18.30 -1 5 -12 18.70 21.50 1 5 12 -9.40 23.10 1 5 12 14.40 22.70 2 -5 12 167.38 36.60 2 -5 12 113.29 37.90 2 5 12 152.58 40.10 -2 5 -12 79.69 30.90 2 5 12 94.49 33.20 2 5 12 137.19 34.60 3 -5 12 130.29 31.90 3 5 12 74.69 37.20 -3 5 -12 83.99 30.90 3 5 12 39.80 29.10 3 5 12 33.50 29.30 3 5 12 62.69 31.80 3 5 12 76.39 29.40 -4 -6 12 -10.40 28.10 -4 -6 12 -8.90 20.00 -4 -6 12 -52.79 20.10 -4 6 12 2.30 22.10 -4 6 12 27.20 27.60 -3 -6 12 81.99 30.60 -3 -6 12 1.60 23.90 -3 -6 12 -1.50 25.70 -3 6 12 47.50 25.70 -3 6 12 53.79 29.00 -2 -6 12 22.00 25.60 -2 -6 12 -45.80 21.30 -2 -6 12 -30.40 20.50 -2 6 12 -16.00 17.80 -2 6 12 -6.30 21.60 -1 -6 12 114.59 35.60 -1 -6 12 177.48 43.70 -1 -6 12 41.70 34.20 -1 6 12 115.89 36.80 1 6 -12 130.09 38.30 -1 6 12 218.28 52.49 0 -6 12 20.80 20.30 0 -6 12 25.90 22.40 0 6 12 29.50 26.40 0 6 12 -9.60 18.10 0 6 -12 14.40 22.80 0 6 12 45.60 30.60 1 -6 12 -19.00 16.90 1 -6 12 33.40 22.80 1 6 12 6.40 25.30 -1 6 -12 -2.60 20.80 1 6 12 8.70 22.90 1 6 12 -12.80 18.80 2 -6 12 79.89 30.80 2 -6 12 106.89 33.10 2 6 12 39.00 28.50 -2 6 -12 70.49 33.50 2 6 12 38.40 25.30 2 6 12 87.19 34.30 3 -6 12 25.90 21.10 3 6 12 -19.30 20.00 3 6 12 -8.70 26.00 3 6 12 13.20 23.60 -3 6 -12 55.39 32.80 3 6 12 -8.10 19.40 -4 -7 12 -30.60 22.60 -4 -7 12 -22.30 22.90 -4 -7 12 -35.20 24.70 -4 7 12 28.00 30.00 -4 7 12 12.50 24.60 -3 -7 12 99.19 37.20 -3 -7 12 95.79 30.80 -3 -7 12 6.90 26.80 -3 7 12 104.19 39.70 -3 7 12 57.19 30.30 -2 -7 12 75.89 31.20 -2 -7 12 121.29 35.20 -2 -7 12 78.19 29.10 -2 7 12 171.28 49.00 -2 7 12 26.00 25.80 -1 -7 12 -8.50 18.60 -1 -7 12 -3.10 18.50 -1 7 12 22.40 20.90 -1 7 12 -5.40 23.00 1 7 -12 -14.50 20.70 0 -7 12 46.80 24.80 0 -7 12 25.70 24.60 0 7 -12 31.00 27.00 0 7 12 63.29 28.00 0 7 12 90.39 34.20 1 -7 12 36.10 23.20 1 -7 12 9.60 22.40 1 7 12 13.20 22.00 1 7 12 24.00 25.40 1 7 12 -15.50 18.90 -1 7 -12 28.80 24.50 2 -7 12 78.19 35.30 2 -7 12 89.79 32.00 2 7 12 191.38 48.00 2 7 12 77.09 36.00 -2 7 -12 123.69 34.40 2 7 12 115.89 33.10 -4 -8 12 -28.80 25.30 -4 -8 12 1.00 30.10 -4 -8 12 -30.00 24.50 -4 8 12 7.70 26.00 -4 8 12 -2.20 32.00 -3 -8 12 1.40 25.50 -3 -8 12 49.90 27.40 -3 -8 12 -24.10 24.50 -3 8 12 10.00 23.50 -3 8 12 19.60 26.10 -2 -8 12 127.09 46.60 -2 -8 12 112.89 35.00 -2 -8 12 135.09 40.70 -2 8 12 89.49 34.50 -2 8 12 50.79 28.60 -1 -8 12 -16.40 20.80 -1 -8 12 25.30 21.40 -1 8 12 -7.20 22.50 1 8 -12 -10.90 19.20 -1 8 12 13.90 24.80 0 -8 12 0.50 16.70 0 -8 12 59.29 29.80 0 8 -12 42.20 23.70 0 8 12 9.00 25.20 0 8 12 46.90 30.40 1 -8 12 40.00 25.60 1 -8 12 -6.80 21.10 1 8 12 6.30 21.60 1 8 12 11.90 21.40 1 8 12 -19.80 19.20 -1 8 -12 -3.20 22.70 2 -8 12 2.80 24.40 2 -8 12 85.39 30.20 2 8 12 105.29 37.90 2 8 12 34.60 24.50 -2 8 -12 42.10 31.90 2 8 12 56.39 31.00 -4 -9 12 14.80 27.60 -4 -9 12 1.70 23.90 -4 -9 12 36.00 30.30 -4 9 12 44.40 36.10 -4 9 12 50.39 33.30 -3 -9 12 -15.00 22.90 -3 -9 12 4.50 24.70 -3 -9 12 -3.80 25.50 -3 9 12 23.80 27.80 -3 9 12 -20.20 18.40 -2 -9 12 8.30 25.60 -2 -9 12 -31.10 24.20 -2 9 12 -7.10 22.00 -2 9 12 23.10 23.70 -1 -9 12 96.59 30.30 -1 -9 12 106.99 35.50 -1 9 12 91.69 33.20 1 9 -12 28.90 25.50 -1 9 12 72.99 35.00 0 -9 12 23.20 22.00 0 -9 12 23.20 24.00 0 9 -12 -4.80 22.00 0 9 12 17.40 22.70 0 9 12 3.20 26.10 1 -9 12 24.20 23.70 1 -9 12 40.10 26.30 1 9 12 58.39 28.40 1 9 12 -24.40 19.40 -1 9 -12 32.70 27.90 1 9 12 12.70 24.00 2 -9 12 -12.90 21.20 2 -9 12 42.90 32.20 2 9 12 -2.90 25.50 -2 9 -12 13.00 24.30 2 9 12 -24.70 18.40 2 9 12 4.00 28.90 -3 -10 12 2.40 27.60 -3 -10 12 47.80 27.40 -3 -10 12 -16.90 21.20 -3 10 12 47.10 39.20 -3 10 12 -12.00 23.50 -2 -10 12 -30.60 20.10 -2 -10 12 1.90 21.80 -2 10 12 -0.70 23.70 -2 10 12 -34.40 23.50 -1 -10 12 107.29 36.50 -1 -10 12 126.59 35.40 1 10 -12 80.89 36.00 -1 10 12 145.59 37.20 -1 10 12 105.19 39.80 0 -10 12 -3.70 21.70 0 -10 12 -5.40 20.80 0 10 -12 -13.60 19.70 0 10 12 -22.20 22.40 0 10 12 9.20 27.20 1 -10 12 151.38 36.50 1 -10 12 51.09 26.70 1 10 12 128.29 34.90 1 10 12 83.79 35.10 -1 10 -12 78.49 36.00 1 10 12 65.29 32.10 2 -10 12 -2.70 26.50 2 -10 12 14.60 22.70 2 10 12 -25.40 25.50 2 10 12 -16.00 19.90 -2 10 -12 17.10 25.00 2 10 12 11.10 25.40 -3 -11 12 -5.30 25.00 -3 -11 12 3.40 23.90 -3 11 12 -13.40 24.50 -3 11 12 37.30 36.90 -2 -11 12 -11.60 27.30 -2 -11 12 -10.40 24.70 -2 11 12 -8.20 26.70 -2 11 12 8.80 26.20 -1 -11 12 53.29 35.70 -1 -11 12 170.28 40.20 -1 11 12 85.69 42.00 -1 11 12 219.38 49.00 1 11 -12 99.79 38.40 0 -11 12 -20.30 19.50 0 -11 12 72.69 31.40 0 11 12 -16.10 23.50 0 11 12 -21.60 24.80 0 11 -12 7.60 25.20 1 -11 12 -9.20 19.70 1 -11 12 25.50 25.20 1 11 12 26.30 28.90 1 11 12 26.80 30.80 -1 11 -12 6.10 26.70 -3 -12 12 46.70 34.60 -3 12 12 27.70 33.00 -2 -12 12 6.80 26.30 -2 -12 12 -14.20 23.70 2 12 -12 -2.20 20.70 -2 12 12 -7.30 31.80 -2 12 12 0.90 25.00 -1 -12 12 -35.50 24.20 -1 -12 12 31.40 24.00 -1 12 12 14.30 30.90 -1 12 12 -4.00 28.20 1 12 -12 -19.10 23.10 0 -12 12 20.30 21.00 0 -12 12 5.10 22.00 0 12 -12 -13.70 19.50 0 12 12 39.40 28.40 0 12 12 -12.30 19.30 1 -12 12 25.50 27.80 1 -12 12 18.20 23.20 -1 12 -12 34.60 28.00 1 12 12 12.90 23.90 1 12 12 74.39 35.10 -2 -13 12 9.00 35.10 -2 -13 12 6.80 24.70 -2 13 12 26.70 31.00 -2 13 12 -21.50 22.30 2 13 -12 1.10 25.20 -1 -13 12 -19.40 20.70 -1 -13 12 17.80 26.30 -1 13 12 7.70 28.00 -1 13 12 38.20 29.20 1 13 -12 12.80 24.20 0 -13 12 -2.20 24.30 0 -13 12 -2.30 21.00 0 13 -12 12.00 27.60 0 13 12 33.70 31.40 0 13 12 2.50 24.40 -1 14 12 6.80 30.20 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 58502 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -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 Cl1 Cl 0.52958(9) 0.42194(3) 0.20172(8) 0.0299(2) Uani 1 1 d . . . . . Cl2 Cl 0.82429(9) 0.43241(4) 0.12831(10) 0.0433(3) Uani 1 1 d . . . . . Cl3 Cl 0.58776(13) 0.44423(5) -0.08049(11) 0.0699(4) Uani 1 1 d . . . . . O3 O 0.4389(2) 0.39844(7) 0.4888(2) 0.0199(5) Uani 1 1 d . . . . . O1 O 0.1716(2) 0.39274(7) 0.06726(19) 0.0189(5) Uani 1 1 d . . . . . O2 O 0.1593(2) 0.44556(7) 0.2354(2) 0.0205(5) Uani 1 1 d . . . . . O4 O 0.2744(2) 0.34851(7) 0.7275(2) 0.0227(5) Uani 1 1 d . . . . . O5 O 0.3184(2) 0.29393(7) 0.9344(2) 0.0221(5) Uani 1 1 d . . . . . H5 H 0.3232 0.3187 0.8910 0.033 Uiso 1 1 calc R U . . . N1 N 0.2540(3) 0.44053(8) 0.5734(2) 0.0153(5) Uani 1 1 d . . . . . C8 C 0.3106(3) 0.40474(10) 0.5065(3) 0.0159(6) Uani 1 1 d . . . . . C4 C 0.1947(3) 0.32324(10) 0.2658(3) 0.0152(6) Uani 1 1 d . . . . . H4 H 0.1950 0.3112 0.1741 0.018 Uiso 1 1 calc R U . . . C14 C 0.0525(3) 0.39824(9) 0.5050(3) 0.0140(6) Uani 1 1 d . . . . . C5 C 0.2124(3) 0.29621(10) 0.3932(3) 0.0149(6) Uani 1 1 d . . . . . C6 C 0.2015(3) 0.32472(10) 0.5030(3) 0.0147(6) Uani 1 1 d . . . . . C2 C 0.1678(3) 0.40629(10) 0.1998(3) 0.0155(6) Uani 1 1 d . . . . . C9 C 0.1021(3) 0.43695(10) 0.5770(3) 0.0147(6) Uani 1 1 d . . . . . C3 C 0.1781(3) 0.36753(10) 0.2964(3) 0.0146(6) Uani 1 1 d . . . . . C16 C 0.1781(3) 0.27408(10) 0.7200(3) 0.0160(6) Uani 1 1 d . . . . . C22 C 0.2437(3) 0.24690(10) 0.3850(3) 0.0157(6) Uani 1 1 d . . . . . C17 C 0.2346(3) 0.26408(10) 0.8568(3) 0.0173(6) Uani 1 1 d . . . . . C7 C 0.1813(3) 0.37335(10) 0.4519(3) 0.0141(6) Uani 1 1 d . . . . . C21 C 0.0829(3) 0.24268(10) 0.6519(3) 0.0183(6) Uani 1 1 d . . . . . H21 H 0.0403 0.2494 0.5612 0.022 Uiso 1 1 calc R U . . . C15 C 0.2201(3) 0.31669(10) 0.6550(3) 0.0175(6) Uani 1 1 d . . . . . C20 C 0.0499(3) 0.20216(10) 0.7144(3) 0.0196(6) Uani 1 1 d . . . . . H20 H -0.0167 0.1814 0.6678 0.023 Uiso 1 1 calc R U . . . C23 C 0.3632(3) 0.22790(10) 0.4601(3) 0.0193(6) Uani 1 1 d . . . . . H23 H 0.4211 0.2461 0.5246 0.023 Uiso 1 1 calc R U . . . C00Q C 0.3414(3) 0.47681(10) 0.6388(3) 0.0188(6) Uani 1 1 d . . . . . H00A H 0.4441 0.4725 0.6202 0.028 Uiso 1 1 calc R U . . . H00B H 0.3324 0.4763 0.7396 0.028 Uiso 1 1 calc R U . . . H00C H 0.3069 0.5063 0.6010 0.028 Uiso 1 1 calc R U . . . C10 C 0.0074(3) 0.46604(10) 0.6383(3) 0.0179(6) Uani 1 1 d . . . . . H10 H 0.0420 0.4924 0.6879 0.021 Uiso 1 1 calc R U . . . C13 C -0.0939(3) 0.38802(10) 0.4912(3) 0.0185(6) Uani 1 1 d . . . . . H13 H -0.1281 0.3616 0.4415 0.022 Uiso 1 1 calc R U . . . C12 C -0.1913(3) 0.41709(10) 0.5516(3) 0.0194(6) Uani 1 1 d . . . . . H12 H -0.2932 0.4107 0.5425 0.023 Uiso 1 1 calc R U . . . C11 C -0.1404(3) 0.45516(10) 0.6246(3) 0.0191(6) Uani 1 1 d . . . . . H11 H -0.2081 0.4744 0.6664 0.023 Uiso 1 1 calc R U . . . C18 C 0.2059(3) 0.22255(10) 0.9172(3) 0.0212(7) Uani 1 1 d . . . . . H18 H 0.2489 0.2153 1.0074 0.025 Uiso 1 1 calc R U . . . C26 C 0.1920(4) 0.17384(11) 0.2763(3) 0.0239(7) Uani 1 1 d . . . . . H26 H 0.1322 0.1552 0.2145 0.029 Uiso 1 1 calc R U . . . C24 C 0.3988(3) 0.18242(11) 0.4418(3) 0.0229(7) Uani 1 1 d . . . . . H24 H 0.4819 0.1697 0.4926 0.027 Uiso 1 1 calc R U . . . C27 C 0.1577(3) 0.21951(10) 0.2934(3) 0.0198(7) Uani 1 1 d . . . . . H27 H 0.0748 0.2322 0.2422 0.024 Uiso 1 1 calc R U . . . C19 C 0.1143(3) 0.19168(11) 0.8458(3) 0.0231(7) Uani 1 1 d . . . . . H19 H 0.0952 0.1630 0.8869 0.028 Uiso 1 1 calc R U . . . C25 C 0.3138(4) 0.15552(11) 0.3498(3) 0.0250(7) Uani 1 1 d . . . . . H25 H 0.3389 0.1244 0.3370 0.030 Uiso 1 1 calc R U . . . C1 C 0.1686(4) 0.42906(11) -0.0346(3) 0.0257(7) Uani 1 1 d . . . . . H1A H 0.0738 0.4446 -0.0374 0.038 Uiso 1 1 calc R U . . . H1B H 0.1829 0.4162 -0.1266 0.038 Uiso 1 1 calc R U . . . H1C H 0.2469 0.4509 -0.0088 0.038 Uiso 1 1 calc R U . . . C1S C 0.6486(3) 0.41465(12) 0.0697(3) 0.0242(7) Uani 1 1 d . . . . . H1S H 0.6525 0.3814 0.0466 0.029 Uiso 1 1 calc R U . . . 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 Cl1 0.0276(4) 0.0335(5) 0.0300(4) -0.0075(4) 0.0100(3) -0.0067(4) Cl2 0.0219(5) 0.0561(6) 0.0522(6) -0.0238(5) 0.0039(4) -0.0030(4) Cl3 0.0630(8) 0.1163(11) 0.0312(5) 0.0277(6) 0.0087(5) 0.0468(7) O3 0.0138(11) 0.0260(12) 0.0198(10) -0.0006(9) 0.0006(8) 0.0003(9) O1 0.0271(12) 0.0183(11) 0.0111(9) 0.0020(8) 0.0000(8) -0.0015(9) O2 0.0270(12) 0.0160(11) 0.0186(10) 0.0019(9) 0.0015(9) 0.0014(9) O4 0.0333(13) 0.0185(11) 0.0155(10) -0.0024(9) -0.0029(9) -0.0021(9) O5 0.0274(12) 0.0238(12) 0.0142(10) -0.0009(9) -0.0047(9) -0.0016(10) N1 0.0144(12) 0.0169(13) 0.0142(11) -0.0011(10) -0.0021(9) -0.0019(10) C8 0.0166(15) 0.0178(15) 0.0129(13) 0.0020(11) -0.0017(11) 0.0006(12) C4 0.0159(15) 0.0187(15) 0.0106(13) -0.0008(11) -0.0018(11) -0.0016(12) C14 0.0179(15) 0.0136(14) 0.0103(12) 0.0024(11) -0.0008(11) 0.0017(11) C5 0.0145(14) 0.0168(15) 0.0130(13) 0.0006(11) -0.0010(11) 0.0013(11) C6 0.0134(14) 0.0171(15) 0.0130(13) 0.0029(11) -0.0024(11) 0.0003(11) C2 0.0129(14) 0.0195(16) 0.0139(13) 0.0002(12) -0.0003(11) 0.0000(12) C9 0.0149(14) 0.0179(15) 0.0110(13) 0.0033(11) -0.0017(11) 0.0012(11) C3 0.0102(14) 0.0212(16) 0.0121(13) 0.0009(12) -0.0009(11) -0.0011(11) C16 0.0147(15) 0.0213(16) 0.0122(13) 0.0000(12) 0.0013(11) 0.0027(12) C22 0.0176(15) 0.0195(16) 0.0101(13) -0.0001(11) 0.0013(11) -0.0004(12) C17 0.0163(15) 0.0210(16) 0.0148(13) -0.0026(12) 0.0013(11) 0.0041(12) C7 0.0150(14) 0.0155(15) 0.0115(13) 0.0000(11) -0.0009(11) -0.0004(11) C21 0.0162(15) 0.0231(16) 0.0160(14) -0.0010(12) 0.0032(12) 0.0021(12) C15 0.0174(15) 0.0193(16) 0.0155(14) -0.0021(12) 0.0000(12) 0.0033(12) C20 0.0173(15) 0.0199(16) 0.0217(15) -0.0011(13) 0.0029(12) -0.0020(12) C23 0.0200(16) 0.0218(16) 0.0159(14) 0.0021(12) -0.0006(12) 0.0001(13) C00Q 0.0200(16) 0.0166(15) 0.0196(15) -0.0017(12) -0.0006(12) -0.0043(12) C10 0.0209(16) 0.0172(15) 0.0153(14) -0.0008(12) -0.0002(12) 0.0017(12) C13 0.0191(16) 0.0189(16) 0.0171(14) 0.0019(12) -0.0028(12) -0.0004(12) C12 0.0155(15) 0.0209(16) 0.0218(15) 0.0042(13) 0.0006(12) -0.0008(12) C11 0.0202(16) 0.0206(16) 0.0167(14) 0.0037(12) 0.0035(12) 0.0082(12) C18 0.0224(16) 0.0257(17) 0.0155(14) 0.0037(13) 0.0011(12) 0.0036(13) C26 0.0337(19) 0.0214(17) 0.0166(15) -0.0029(13) 0.0012(13) -0.0036(14) C24 0.0216(16) 0.0245(18) 0.0227(16) 0.0054(13) 0.0023(13) 0.0058(13) C27 0.0236(16) 0.0218(17) 0.0136(14) -0.0006(12) -0.0019(12) -0.0001(13) C19 0.0225(17) 0.0216(17) 0.0256(16) 0.0045(13) 0.0045(13) 0.0020(13) C25 0.036(2) 0.0180(17) 0.0216(16) -0.0010(13) 0.0066(14) 0.0022(14) C1 0.037(2) 0.0256(18) 0.0143(14) 0.0082(13) 0.0017(13) 0.0034(15) C1S 0.0196(16) 0.0315(19) 0.0214(16) 0.0010(14) 0.0003(13) 0.0004(13) 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' N N 0.0061 0.0033 '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' 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 C2 O1 C1 115.3(2) . . ? C17 O5 H5 109.5 . . ? C8 N1 C9 111.8(2) . . ? C8 N1 C00Q 123.8(3) . . ? C9 N1 C00Q 124.3(2) . . ? O3 C8 N1 126.4(3) . . ? O3 C8 C7 125.6(3) . . ? N1 C8 C7 108.0(3) . . ? C3 C4 C5 110.3(3) . . ? C3 C4 H4 124.8 . . ? C5 C4 H4 124.8 . . ? C13 C14 C9 120.5(3) . . ? C13 C14 C7 130.3(3) . . ? C9 C14 C7 109.2(3) . . ? C6 C5 C4 108.1(3) . . ? C6 C5 C22 132.1(3) . . ? C4 C5 C22 119.7(2) . . ? C5 C6 C15 131.5(3) . . ? C5 C6 C7 109.9(3) . . ? C15 C6 C7 118.2(2) . . ? O2 C2 O1 124.1(3) . . ? O2 C2 C3 124.2(3) . . ? O1 C2 C3 111.7(3) . . ? C10 C9 C14 121.7(3) . . ? C10 C9 N1 128.6(3) . . ? C14 C9 N1 109.8(2) . . ? C4 C3 C2 127.8(3) . . ? C4 C3 C7 109.5(2) . . ? C2 C3 C7 122.6(3) . . ? C21 C16 C17 118.3(3) . . ? C21 C16 C15 122.5(3) . . ? C17 C16 C15 119.2(3) . . ? C23 C22 C27 119.2(3) . . ? C23 C22 C5 121.0(3) . . ? C27 C22 C5 119.7(3) . . ? O5 C17 C18 117.1(3) . . ? O5 C17 C16 122.4(3) . . ? C18 C17 C16 120.5(3) . . ? C3 C7 C14 115.8(2) . . ? C3 C7 C6 102.1(2) . . ? C14 C7 C6 115.1(2) . . ? C3 C7 C8 111.1(2) . . ? C14 C7 C8 101.2(2) . . ? C6 C7 C8 112.0(2) . . ? C20 C21 C16 120.9(3) . . ? C20 C21 H21 119.5 . . ? C16 C21 H21 119.5 . . ? O4 C15 C16 120.4(3) . . ? O4 C15 C6 116.5(3) . . ? C16 C15 C6 123.1(3) . . ? C21 C20 C19 119.8(3) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C22 C23 C24 120.4(3) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? N1 C00Q H00A 109.5 . . ? N1 C00Q H00B 109.5 . . ? H00A C00Q H00B 109.5 . . ? N1 C00Q H00C 109.5 . . ? H00A C00Q H00C 109.5 . . ? H00B C00Q H00C 109.5 . . ? C9 C10 C11 117.3(3) . . ? C9 C10 H10 121.4 . . ? C11 C10 H10 121.4 . . ? C14 C13 C12 118.7(3) . . ? C14 C13 H13 120.7 . . ? C12 C13 H13 120.7 . . ? C11 C12 C13 120.2(3) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C12 C11 C10 121.6(3) . . ? C12 C11 H11 119.2 . . ? C10 C11 H11 119.2 . . ? C19 C18 C17 119.7(3) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C25 C26 C27 119.7(3) . . ? C25 C26 H26 120.2 . . ? C27 C26 H26 120.2 . . ? C25 C24 C23 120.2(3) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C26 C27 C22 120.6(3) . . ? C26 C27 H27 119.7 . . ? C22 C27 H27 119.7 . . ? C18 C19 C20 120.6(3) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? C24 C25 C26 120.0(3) . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Cl3 C1S Cl2 110.47(19) . . ? Cl3 C1S Cl1 111.3(2) . . ? Cl2 C1S Cl1 109.9(2) . . ? Cl3 C1S H1S 108.4 . . ? Cl2 C1S H1S 108.4 . . ? Cl1 C1S H1S 108.4 . . ? 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 Cl1 C1S 1.750(4) . ? Cl2 C1S 1.745(4) . ? Cl3 C1S 1.741(4) . ? O3 C8 1.216(4) . ? O1 C2 1.339(4) . ? O1 C1 1.445(4) . ? O2 C2 1.205(4) . ? O4 C15 1.246(4) . ? O5 C17 1.352(4) . ? O5 H5 0.8400 . ? N1 C8 1.354(4) . ? N1 C9 1.400(4) . ? N1 C00Q 1.446(4) . ? C8 C7 1.560(4) . ? C4 C3 1.342(4) . ? C4 C5 1.459(4) . ? C4 H4 0.9500 . ? C14 C13 1.372(4) . ? C14 C9 1.387(4) . ? C14 C7 1.510(4) . ? C5 C6 1.356(4) . ? C5 C22 1.477(4) . ? C6 C15 1.479(4) . ? C6 C7 1.514(4) . ? C2 C3 1.466(4) . ? C9 C10 1.381(4) . ? C3 C7 1.504(4) . ? C16 C21 1.397(4) . ? C16 C17 1.408(4) . ? C16 C15 1.461(4) . ? C22 C23 1.383(4) . ? C22 C27 1.391(4) . ? C17 C18 1.383(4) . ? C21 C20 1.375(4) . ? C21 H21 0.9500 . ? C20 C19 1.389(5) . ? C20 H20 0.9500 . ? C23 C24 1.386(5) . ? C23 H23 0.9500 . ? C00Q H00A 0.9800 . ? C00Q H00B 0.9800 . ? C00Q H00C 0.9800 . ? C10 C11 1.389(5) . ? C10 H10 0.9500 . ? C13 C12 1.393(4) . ? C13 H13 0.9500 . ? C12 C11 1.380(4) . ? C12 H12 0.9500 . ? C11 H11 0.9500 . ? C18 C19 1.382(5) . ? C18 H18 0.9500 . ? C26 C25 1.384(5) . ? C26 C27 1.387(5) . ? C26 H26 0.9500 . ? C24 C25 1.381(5) . ? C24 H24 0.9500 . ? C27 H27 0.9500 . ? C19 H19 0.9500 . ? C25 H25 0.9500 . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C1S H1S 1.0000 . ?