#------------------------------------------------------------------------------ #$Date: 2021-10-07 07:41:56 +0300 (Thu, 07 Oct 2021) $ #$Revision: 269817 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/48/1564853.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_1564853 loop_ _publ_author_name 'Aitken, R. Alan' 'Saab, Elizabeth A.' 'Slawin, Alexandra M. Z.' _publ_section_title ; 2,6-Dimethoxybenzyl Bromide ; _journal_issue 3 _journal_name_full Molbank _journal_page_first M1277 _journal_paper_doi 10.3390/M1277 _journal_volume 2021 _journal_year 2021 _chemical_absolute_configuration ad _chemical_formula_moiety 'C9 H11 Br O2' _chemical_formula_sum 'C9 H11 Br O2' _chemical_formula_weight 231.09 _space_group_crystal_system orthorhombic _space_group_IT_number 33 _space_group_name_Hall 'P 2c -2n' _space_group_name_H-M_alt 'P n a 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_date 2021-06-09 _audit_creation_method 'by CrystalStructure 4.3' _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 90.0000 _cell_formula_units_Z 4 _cell_length_a 13.297(8) _cell_length_b 5.033(3) _cell_length_c 13.789(9) _cell_measurement_reflns_used 2220 _cell_measurement_temperature 93 _cell_measurement_theta_max 27.40 _cell_measurement_theta_min 3.00 _cell_volume 922.8(10) _computing_cell_refinement 'CrystalClear-SM Expert 2.1 b32' _computing_data_collection 'CrystalClear-SM Expert 2.1 b32 (Rigaku, 2014)' _computing_data_reduction 'CrystalClear-SM Expert 2.1 b32' _computing_molecular_graphics 'CrystalStructure 4.3' _computing_publication_material 'CrystalStructure 4.3 (Rigaku, 2019)' _computing_structure_refinement 'SHELXL Version 2018/3 (Sheldrick, 2008)' _computing_structure_solution 'SIR2011 (Burla, et al., 2012)' _diffrn_ambient_temperature 93 _diffrn_detector_area_resol_mean 5.814 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Rigaku XtaLAB P200' _diffrn_measurement_method \w _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_reflns_av_R_equivalents 0.0537 _diffrn_reflns_av_unetI/netI 0.0379 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 9253 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.215 _diffrn_reflns_theta_max 25.215 _diffrn_reflns_theta_min 2.955 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 4.424 _exptl_absorpt_correction_T_max 0.915 _exptl_absorpt_correction_T_min 0.608 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.663 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 464.00 _exptl_crystal_size_max 0.180 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.020 _refine_diff_density_max 0.95 _refine_diff_density_min -0.48 _refine_ls_abs_structure_details ; Flack x determined using 707 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.007(7) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_hydrogen_treatment constr _refine_ls_number_parameters 111 _refine_ls_number_reflns 1647 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0281 _refine_ls_R_factor_gt 0.0269 _refine_ls_shift/su_max 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0395P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0654 _refine_ls_wR_factor_ref 0.0658 _reflns_Friedel_coverage 0.913 _reflns_Friedel_fraction_full 0.996 _reflns_Friedel_fraction_max 0.996 _reflns_number_gt 1554 _reflns_number_total 1647 _reflns_threshold_expression F^2^>2.0\s(F^2^) _cod_data_source_file s5.cif _cod_data_source_block 1 _cod_database_code 1564853 _shelx_res_file ; TITL LSAA1 shelxl.res created by SHELXL-2018/3 at 16:08:42 on 09-Jun-2021 CELL 0.71075 13.29700 5.03300 13.78900 90.00000 90.00000 90.00000 ZERR 4 0.00800 0.00300 0.00900 0.00000 0.00000 0.00000 LATT -1 SYMM -X, -Y, .50+Z SYMM .50-X, .50+Y, .50+Z SYMM .50+X, .50-Y, +Z SFAC C H BR O UNIT 36 44 4 8 L.S. 20 FMAP 2 PLAN 5 WPDB -2 HTAB BOND $H CONF LIST 4 TEMP -180.0 ACTA SIZE 0.020 0.100 0.180 WGHT 0.039500 FVAR 0.87578 BR7 3 0.107898 0.167000 0.229081 11.00000 0.02538 0.02230 = 0.02353 0.00399 -0.00438 -0.00651 O2 4 0.141993 0.028270 0.487424 11.00000 0.02025 0.01860 = 0.02633 0.00908 -0.00103 -0.00145 O6 4 0.294219 0.675862 0.294414 11.00000 0.01882 0.01528 = 0.02253 0.00518 -0.00156 -0.00314 C1 1 0.220719 0.359389 0.395179 11.00000 0.01843 0.01158 = 0.01792 -0.00209 -0.00320 0.00186 C2 1 0.227465 0.173614 0.471307 11.00000 0.01985 0.01181 = 0.02045 -0.00106 0.00462 0.00374 C3 1 0.315174 0.149982 0.526099 11.00000 0.02210 0.01578 = 0.01780 0.00174 0.00031 0.00351 AFIX 43 H3 2 0.318894 0.027839 0.578502 11.00000 -1.20000 AFIX 0 C4 1 0.397684 0.310269 0.502190 11.00000 0.02020 0.01743 = 0.02173 -0.00354 -0.00352 0.00063 AFIX 43 H4 2 0.457459 0.296158 0.539572 11.00000 -1.20000 AFIX 0 C5 1 0.394812 0.488795 0.425689 11.00000 0.01866 0.01338 = 0.02238 -0.00231 0.00085 0.00040 AFIX 43 H5 2 0.451869 0.594335 0.410349 11.00000 -1.20000 AFIX 0 C6 1 0.306190 0.510493 0.371491 11.00000 0.02050 0.01010 = 0.01900 -0.00257 0.00156 0.00162 C7 1 0.124129 0.405071 0.343433 11.00000 0.02182 0.01497 = 0.02153 0.00307 -0.00244 -0.00105 AFIX 23 H7A 2 0.121129 0.592309 0.321622 11.00000 -1.20000 H7B 2 0.067646 0.375146 0.388915 11.00000 -1.20000 AFIX 0 C8 1 0.144727 -0.157381 0.566328 11.00000 0.02634 0.01639 = 0.02412 0.00734 0.00495 0.00099 AFIX 137 H8A 2 0.153844 -0.061059 0.627465 11.00000 -1.20000 H8B 2 0.200807 -0.281096 0.556979 11.00000 -1.20000 H8C 2 0.081396 -0.256807 0.568440 11.00000 -1.20000 AFIX 0 C9 1 0.374024 0.858489 0.271904 11.00000 0.02231 0.01222 = 0.03075 0.00341 0.00495 -0.00270 AFIX 137 H9A 2 0.353372 0.973162 0.218028 11.00000 -1.20000 H9B 2 0.434363 0.758848 0.253393 11.00000 -1.20000 H9C 2 0.388730 0.967937 0.328949 11.00000 -1.20000 AFIX 0 HKLF 4 REM LSAA1 REM wR2 = 0.0658, GooF = S = 1.084, Restrained GooF = 1.084 for all data REM R1 = 0.0269 for 1554 Fo > 4sig(Fo) and 0.0281 for all 1647 data REM 111 parameters refined using 1 restraints END WGHT 0.0392 0.0000 REM Instructions for potential hydrogen bonds EQIV $1 -x+1/2, y-1/2, z+1/2 HTAB C3 Br7_$1 REM Highest difference peak 0.948, deepest hole -0.479, 1-sigma level 0.091 Q1 1 0.1118 0.1665 0.1626 11.00000 0.05 0.95 Q2 1 0.1084 0.1654 0.2966 11.00000 0.05 0.94 Q3 1 0.1748 0.0931 0.2278 11.00000 0.05 0.55 Q4 1 0.1683 0.2565 0.2270 11.00000 0.05 0.54 Q5 1 0.0460 0.2464 0.2270 11.00000 0.05 0.48 ; _shelx_res_checksum 84956 _shelx_hkl_file ; 1 0 -1 1.87 6.25 1 0 1 10.80 7.01 1 0 1 6.55 7.63 1 0 -1 3.86 7.55 -1 0 1 4.92 7.89 0 0 2 6039.77 321.73 0 0 2 6172.08 321.59 0 0 -2 4846.49 255.57 2 0 0 3442.08 179.37 2 0 0 3935.24 204.77 2 0 0 3852.88 201.58 2 0 0 4623.82 240.56 -1 0 -2 3.95 5.30 1 0 -2 0.02 9.81 -1 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476.17 48.33 9 -2 -12 23.31 16.72 -9 -2 -12 4.98 13.51 -9 -2 -12 6.13 19.94 9 -2 -12 -2.83 15.31 -9 -2 12 -9.23 16.38 9 2 12 -6.01 17.61 -9 -2 12 -6.31 15.46 9 -2 12 -2.99 20.03 -9 2 12 -5.76 18.52 -9 2 -12 8.59 11.63 9 2 -12 11.55 18.12 3 -5 8 70.93 17.26 -3 5 -8 67.10 17.22 -3 -5 8 71.35 13.10 -3 -5 -8 70.47 17.76 -3 -5 8 73.53 20.25 3 5 -8 80.02 17.17 -3 -5 -8 85.47 18.26 -3 5 8 84.52 19.09 3 -5 8 55.76 18.45 -11 3 -8 298.47 31.12 11 3 -8 273.93 31.28 11 -3 -8 254.89 30.33 11 -3 -8 263.49 28.88 -11 -3 -8 284.86 33.36 -11 -3 -8 244.98 26.06 -11 -3 8 341.55 40.55 -11 -3 8 296.85 33.86 11 3 8 323.73 37.66 -11 3 8 279.49 39.24 11 -3 8 343.98 35.57 -12 1 -10 558.85 50.37 12 -1 -10 564.28 53.93 12 1 10 717.85 75.24 -12 -1 -10 580.82 57.45 -12 1 10 653.46 76.40 -12 -1 10 710.33 71.18 -12 -1 10 700.93 75.60 -12 1 -10 608.69 59.59 -12 -1 -10 602.13 55.70 12 -1 10 659.48 68.58 6 5 6 555.18 53.57 -6 -5 -6 632.02 57.77 6 -5 -6 639.83 59.01 6 -5 6 582.44 54.25 -6 5 6 571.52 52.56 -6 -5 -6 548.47 54.34 -6 -5 6 633.30 60.88 6 5 -6 501.43 47.31 6 5 -6 598.09 55.86 -6 5 6 593.44 58.03 -6 5 -6 606.19 56.65 -13 0 -9 -8.42 13.02 13 0 9 -2.81 23.82 -13 0 9 11.32 19.45 -5 -3 -13 98.51 20.01 5 3 13 69.55 19.12 -5 3 13 78.32 23.71 5 -3 13 76.68 22.41 -5 3 -13 96.58 17.58 5 3 -13 85.17 20.05 -5 -3 13 62.03 19.00 5 -3 -13 87.64 19.65 -5 -3 -13 94.81 20.10 -5 3 -13 92.99 22.73 0 -1 16 7.50 19.39 0 1 16 4.59 19.35 0 1 -16 -3.03 17.77 0 -1 -16 3.51 19.54 0 1 -16 0.59 15.17 -5 -5 7 21.38 17.62 -5 -5 -7 14.13 17.98 -5 -5 -7 10.34 13.83 5 -5 7 9.67 16.04 5 -5 -7 14.20 17.38 -5 5 7 7.38 14.07 5 5 -7 13.56 17.59 -5 5 -7 9.15 17.91 0 -3 -14 6.86 19.51 0 3 14 4.19 15.83 0 3 14 -5.21 16.72 0 3 -14 0.20 18.12 0 3 -14 -2.31 18.16 0 -3 14 4.88 20.60 -9 1 -13 23.76 15.04 9 -1 -13 10.04 14.50 -9 -1 -13 36.32 15.98 -9 1 13 15.02 18.10 -9 -1 13 7.26 18.26 9 -1 13 12.38 22.37 -9 -1 13 5.27 15.15 9 1 13 24.79 23.51 9 -1 -13 26.07 16.15 9 1 -13 23.18 16.00 10 4 -6 37.79 22.91 -10 4 -6 49.91 17.18 10 4 -6 42.95 20.82 10 4 6 5.86 20.99 -10 -4 6 6.65 19.91 -10 4 6 20.86 16.86 10 -4 -6 38.51 17.68 10 -4 6 12.04 18.79 -10 4 6 16.35 18.81 -10 -4 -6 43.21 20.42 6 0 15 1245.91 121.95 6 0 -15 1247.86 109.90 -6 0 -15 1186.44 104.75 -6 0 15 1136.28 103.60 6 0 -15 1139.47 104.83 -6 0 15 1142.21 109.93 0 -4 12 219.46 29.21 0 4 12 188.97 27.69 0 4 -12 227.74 27.13 0 4 12 202.97 25.74 0 4 -12 252.46 29.58 7 -3 -12 0.92 15.54 -7 -3 -12 8.57 17.18 7 -3 -12 5.16 14.36 -7 -3 -12 2.08 18.62 -7 3 -12 8.71 14.29 7 3 12 5.81 19.59 -7 3 12 12.79 23.06 -7 3 -12 7.82 16.60 7 -3 12 9.14 21.13 7 3 -12 4.58 15.12 -7 -3 12 1.82 16.44 1 -1 -16 252.24 30.40 -1 1 -16 215.62 27.58 -1 1 16 286.84 32.40 -1 1 -16 221.58 26.88 1 1 -16 262.15 31.91 1 -1 16 298.06 35.89 1 1 -16 213.92 27.94 -1 -1 -16 270.10 31.81 1 1 16 283.57 35.11 -1 1 16 274.97 31.72 -1 -1 16 311.57 36.24 -1 3 -14 722.91 66.73 1 3 -14 700.90 65.24 1 3 14 686.92 66.70 1 -3 14 706.72 71.65 1 3 14 760.57 72.90 1 -3 -14 845.77 77.49 -1 3 -14 937.39 84.50 -1 3 14 713.15 72.92 1 3 -14 610.81 57.59 -1 3 14 692.54 65.44 -1 -3 14 675.74 65.83 3 -2 -15 191.73 26.94 3 2 -15 142.54 24.15 -3 2 -15 184.58 26.02 3 2 -15 175.86 27.48 -3 2 -15 151.18 20.46 3 2 15 160.17 23.88 -3 2 15 154.03 25.50 3 2 15 146.50 23.36 3 -2 15 159.59 27.93 -3 2 15 143.59 23.28 -3 -2 15 158.98 23.47 -6 2 -14 111.77 17.53 -6 2 14 116.99 23.98 -6 -2 14 109.64 20.39 6 2 14 116.33 27.13 6 2 -14 78.98 16.84 6 -2 -14 84.79 16.28 6 2 14 100.62 20.50 -6 2 -14 121.70 22.78 -6 -2 -14 124.18 21.11 6 -2 14 112.94 24.07 6 -2 -14 115.99 21.81 -8 0 14 106.28 19.70 8 0 -14 227.77 25.96 -8 0 14 121.49 24.49 -8 0 -14 261.40 29.94 8 0 14 119.54 26.44 1 -4 12 225.31 29.57 -1 -4 -12 293.99 30.76 -1 -4 12 211.10 28.24 -1 4 12 196.38 26.79 -1 4 12 190.44 25.05 1 4 12 218.96 28.40 -1 4 -12 290.32 30.86 1 4 -12 298.73 33.30 -1 4 -12 266.13 30.67 13 3 -4 680.65 66.40 13 -3 -4 731.93 67.32 13 -3 4 689.00 62.60 -13 3 -4 707.20 64.22 -13 3 4 708.57 68.56 13 3 4 646.14 69.29 -13 -3 4 612.65 59.45 -13 3 4 607.92 65.71 -13 3 -4 493.32 58.05 -13 -3 4 716.62 69.49 -13 -3 -4 706.77 70.74 -7 -5 5 117.13 22.58 7 -5 -5 158.61 23.95 -7 5 5 107.00 18.70 -7 5 5 111.61 20.30 -7 -5 -5 154.53 19.94 7 -5 5 116.45 21.27 7 5 5 106.77 20.61 7 5 -5 150.92 23.89 7 5 -5 145.48 20.17 -7 5 -5 155.48 22.99 -7 -5 -5 139.79 22.20 -15 -1 4 154.85 26.27 -15 1 4 151.91 28.21 15 -1 4 136.83 22.77 15 -1 -4 185.37 26.55 15 1 -4 158.61 25.59 15 1 4 158.31 30.48 -15 -1 -4 190.75 25.94 -15 1 -4 134.52 25.39 -15 -1 4 140.91 21.39 8 5 -3 191.55 24.64 8 5 3 205.67 25.50 -8 5 3 197.77 25.70 8 -5 -3 208.71 25.65 -8 -5 3 249.36 31.01 -8 -5 -3 196.46 25.90 -8 5 -3 194.57 24.08 -8 5 3 207.80 25.17 8 5 -3 211.76 26.74 -3 0 16 -6.03 18.14 3 0 16 7.37 20.73 -3 0 -16 4.42 18.39 3 0 -16 10.34 18.94 3 0 -16 -0.63 13.49 -14 2 -5 33.31 16.92 14 2 5 56.48 24.98 14 2 -5 46.80 20.89 14 -2 5 47.37 16.80 -14 -2 5 33.01 20.52 -14 2 -5 44.84 14.74 -14 2 5 30.60 19.74 -14 -2 5 27.36 16.15 -14 -2 -5 49.41 19.05 12 2 9 246.45 33.16 12 -2 -9 216.37 25.49 12 -2 -9 229.28 28.38 -12 2 9 214.04 33.29 -12 -2 9 216.06 29.73 -12 -2 -9 247.47 27.84 12 -2 9 225.30 28.83 -12 -2 9 183.14 32.81 -12 2 -9 240.55 28.07 12 2 -9 235.06 28.71 -12 2 -9 220.04 24.80 11 -4 4 490.02 46.98 -11 -4 4 511.63 51.25 11 4 -4 416.43 42.76 -11 4 4 429.56 48.01 -11 -4 -4 418.46 44.81 11 -4 -4 380.25 37.47 11 4 4 447.74 51.68 11 4 -4 456.36 48.68 -11 4 4 477.05 46.21 -15 0 -5 11.02 14.14 -15 0 5 -12.23 21.39 15 0 -5 2.10 19.71 -14 -1 7 620.60 68.74 -14 -1 7 667.95 71.85 -14 -1 -7 625.28 62.64 -14 -1 -7 614.88 59.50 -14 1 -7 615.13 56.31 14 -1 7 662.97 60.35 14 1 -7 648.30 62.19 -14 1 7 550.62 66.45 2 -1 -16 1192.12 106.55 -2 -1 16 961.82 90.20 2 1 -16 1017.19 100.20 -2 1 -16 1043.67 93.36 -2 1 16 975.74 92.52 -2 1 16 962.37 95.71 2 1 16 943.72 94.21 -2 -1 -16 1313.87 116.77 -8 -2 13 164.70 26.70 8 2 13 208.61 26.70 -8 -2 -13 187.24 25.35 8 -2 13 192.44 28.54 8 -2 -13 131.97 21.31 8 2 -13 171.81 25.03 -8 2 -13 151.30 19.18 -8 2 13 170.30 28.81 -8 2 -13 171.51 25.34 -2 3 -14 71.82 20.77 2 3 14 73.67 21.90 2 3 14 83.73 21.28 -2 3 14 83.64 22.00 2 -3 14 76.24 19.87 2 3 -14 97.59 21.76 2 -3 -14 96.56 20.86 -2 3 14 78.97 18.10 -2 3 -14 89.09 19.63 5 4 11 826.21 78.15 -5 4 -11 748.14 67.13 -5 4 11 830.76 81.85 5 -4 11 679.33 65.50 -5 -4 -11 758.93 71.72 -5 -4 11 832.48 77.35 5 -4 -11 803.60 73.10 -5 -4 -11 852.78 77.36 2 -4 -12 -0.40 19.19 2 -4 12 -5.79 19.21 -2 4 -12 2.68 17.16 2 4 12 -5.24 18.09 -2 -4 12 -4.22 18.51 -2 4 12 -5.40 20.20 -2 -4 -12 5.95 17.50 2 4 -12 1.03 18.47 -2 -4 -12 4.97 16.35 0 -5 -9 573.27 52.56 0 -5 9 532.42 49.02 0 -5 9 545.20 52.74 0 5 -9 607.28 55.85 4 5 -8 103.65 21.14 -4 -5 -8 118.64 19.70 4 -5 8 103.28 19.74 -4 5 -8 114.23 21.39 -4 -5 -8 104.60 21.65 -4 -5 8 105.43 19.75 4 -5 8 95.98 19.46 -4 5 8 108.53 20.14 -1 -5 -9 323.72 33.60 1 -5 -9 312.36 32.85 1 5 -9 316.44 34.60 1 -5 9 305.96 33.78 -1 5 -9 326.21 35.25 -1 -5 9 317.52 34.55 -1 -5 9 307.05 30.91 1 -5 9 313.75 32.11 -1 5 9 302.76 33.53 -8 4 -9 18.68 15.70 -8 -4 -9 23.18 15.34 8 4 9 21.89 19.64 -8 4 9 10.41 20.52 8 4 -9 19.43 18.57 8 4 -9 26.76 19.28 8 -4 -9 16.75 14.53 -8 -4 -9 14.59 19.74 8 -4 -9 15.80 14.22 0 6 0 2839.70 243.53 0 6 0 2897.53 248.22 0 -6 0 2947.05 252.52 13 -1 9 51.03 22.21 -13 -1 9 46.70 18.16 13 -1 -9 66.22 17.10 -13 1 -9 69.77 17.57 -13 -1 -9 66.16 15.76 -13 -1 -9 53.87 16.72 -13 1 9 52.06 19.83 13 1 9 49.31 20.94 -13 1 -9 65.97 14.10 13 1 -9 71.90 22.56 -13 -1 9 43.95 18.19 -9 -4 8 2.34 15.72 -9 4 8 5.81 17.00 9 -4 -8 0.03 15.44 9 4 8 14.03 20.27 -9 4 -8 -2.97 16.28 9 4 -8 -2.11 19.19 -9 -4 -8 -0.92 18.99 -9 -4 -8 1.76 14.80 9 -4 8 7.72 19.23 9 4 -8 6.47 20.98 0 -6 -1 -5.52 14.53 0 6 1 -10.06 14.17 0 6 -1 -1.38 13.23 0 6 1 0.86 13.45 0 -6 1 -12.00 14.95 6 -1 -15 351.52 35.86 6 -1 15 377.50 43.19 6 1 -15 394.20 40.31 -6 1 15 348.21 36.58 6 -1 -15 371.18 39.80 -6 1 -15 450.46 46.31 -6 -1 15 368.11 38.20 1 -6 0 79.54 17.28 -1 6 0 72.00 15.76 1 6 0 73.15 14.88 1 6 0 66.87 17.98 -1 6 0 81.22 18.62 -1 -6 0 93.33 20.83 -1 -6 0 92.03 16.29 -12 3 -7 62.41 16.83 12 3 7 31.32 21.77 -12 -3 7 37.21 20.40 12 -3 -7 56.86 16.05 -12 3 7 39.72 20.87 -12 -3 7 43.46 20.68 12 -3 7 45.10 17.51 12 3 -7 62.40 21.74 12 -3 -7 50.86 18.30 -15 -2 0 366.96 43.58 -15 2 0 250.96 42.09 15 2 0 328.07 37.38 -15 -2 0 365.46 39.01 4 -2 -15 81.04 18.20 4 2 15 52.45 17.99 -4 2 -15 89.66 16.56 4 2 -15 78.96 20.13 -4 2 -15 80.65 22.95 4 -2 15 40.67 24.40 -4 2 15 68.27 21.34 -4 2 15 64.27 18.33 4 2 15 63.65 24.58 -4 -2 15 52.90 19.42 1 6 1 56.17 13.77 -1 6 1 51.45 16.58 -1 6 -1 42.58 17.71 1 6 1 45.68 15.94 1 6 -1 43.58 17.19 1 -6 -1 48.38 16.06 -1 -6 1 51.71 14.40 1 -6 1 52.70 16.15 -1 6 -1 49.07 13.37 -1 -6 1 50.96 19.04 -1 -6 -1 46.26 14.23 -1 6 1 41.21 13.78 1 6 -1 41.82 12.86 -8 -1 14 357.20 41.38 8 1 14 397.89 48.25 -8 -1 -14 371.36 38.02 8 1 -14 397.84 41.06 8 -1 -14 354.69 38.56 -8 1 14 373.71 45.02 8 -1 14 415.46 46.46 8 -1 -14 348.78 35.85 8 5 4 346.20 37.01 8 5 -4 353.17 37.18 -8 5 4 349.89 35.45 -8 5 -4 375.13 38.16 8 -5 -4 393.55 41.32 -8 5 4 353.74 38.21 8 5 -4 356.42 37.32 -8 -5 -4 366.63 40.08 -8 -5 4 387.99 39.45 7 4 -10 716.11 66.30 7 -4 -10 565.07 55.47 -7 -4 -10 686.24 63.20 7 -4 10 710.35 65.21 7 -4 10 624.42 60.19 -7 -4 -10 645.90 63.68 7 4 10 668.47 65.39 7 -4 -10 642.03 60.52 -7 4 -10 662.57 62.76 -2 -5 9 28.65 11.92 2 -5 9 36.61 14.99 -2 5 9 42.02 17.15 2 -5 9 32.68 17.68 -2 5 -9 36.96 19.55 2 -5 -9 34.58 14.10 -2 -5 9 28.37 17.06 -2 -5 -9 46.06 16.54 2 5 -9 33.10 18.37 3 1 -16 183.62 26.15 -3 -1 16 232.78 29.11 3 -1 -16 197.28 27.72 3 1 -16 170.67 24.04 -3 -1 -16 190.98 25.49 -3 1 -16 172.82 24.49 -3 1 16 219.02 27.75 3 1 16 220.41 31.18 -3 1 16 215.84 28.38 4 0 -16 686.67 64.19 -4 0 16 725.49 68.78 4 0 -16 599.91 57.27 -4 0 -16 615.94 56.87 3 -3 14 243.59 32.40 3 3 14 255.36 34.19 -3 3 14 254.26 34.52 3 3 14 237.69 29.40 -3 3 -14 306.68 32.77 3 -3 -14 294.16 33.48 -3 -3 -14 305.29 33.18 -3 3 -14 253.63 30.96 3 3 -14 308.69 35.23 ; _shelx_hkl_checksum 20915 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 +X,+Y,+Z 2 -X,-Y,1/2+Z 3 1/2-X,1/2+Y,1/2+Z 4 1/2+X,1/2-Y,+Z 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 Br7 Br 0.10790(3) 0.16700(7) 0.22908(4) 0.02374(17) Uani 1 1 d . . . . . O2 O 0.1420(2) 0.0283(5) 0.4874(2) 0.0217(6) Uani 1 1 d . . . . . O6 O 0.2942(2) 0.6759(5) 0.2944(2) 0.0189(7) Uani 1 1 d . . . . . C1 C 0.2207(3) 0.3594(7) 0.3952(3) 0.0160(9) Uani 1 1 d . . . . . C2 C 0.2275(3) 0.1736(7) 0.4713(3) 0.0174(9) Uani 1 1 d . . . . . C3 C 0.3152(4) 0.1500(8) 0.5261(3) 0.0186(10) Uani 1 1 d . . . . . H3 H 0.318894 0.027839 0.578502 0.022 Uiso 1 1 calc R U . . . C4 C 0.3977(3) 0.3103(8) 0.5022(4) 0.0198(11) Uani 1 1 d . . . . . H4 H 0.457459 0.296158 0.539572 0.024 Uiso 1 1 calc R U . . . C5 C 0.3948(3) 0.4888(8) 0.4257(4) 0.0181(9) Uani 1 1 d . . . . . H5 H 0.451869 0.594335 0.410349 0.022 Uiso 1 1 calc R U . . . C6 C 0.3062(3) 0.5105(7) 0.3715(3) 0.0165(8) Uani 1 1 d . . . . . C7 C 0.1241(4) 0.4051(9) 0.3434(3) 0.0194(9) Uani 1 1 d . . . . . H7A H 0.121129 0.592309 0.321622 0.023 Uiso 1 1 calc R U . . . H7B H 0.067646 0.375146 0.388915 0.023 Uiso 1 1 calc R U . . . C8 C 0.1447(4) -0.1574(7) 0.5663(4) 0.0223(10) Uani 1 1 d . . . . . H8A H 0.153844 -0.061059 0.627465 0.027 Uiso 1 1 calc R U . . . H8B H 0.200807 -0.281096 0.556979 0.027 Uiso 1 1 calc R U . . . H8C H 0.081396 -0.256807 0.568440 0.027 Uiso 1 1 calc R U . . . C9 C 0.3740(4) 0.8585(8) 0.2719(4) 0.0218(10) Uani 1 1 d . . . . . H9A H 0.353372 0.973162 0.218028 0.026 Uiso 1 1 calc R U . . . H9B H 0.434363 0.758848 0.253393 0.026 Uiso 1 1 calc R U . . . H9C H 0.388730 0.967937 0.328949 0.026 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 Br7 0.0254(3) 0.0223(2) 0.0235(2) 0.0040(3) -0.0044(2) -0.00651(14) O2 0.0203(15) 0.0186(15) 0.0263(16) 0.0091(14) -0.0010(14) -0.0015(14) O6 0.0188(16) 0.0153(15) 0.0225(16) 0.0052(12) -0.0016(13) -0.0031(10) C1 0.018(2) 0.0116(18) 0.018(2) -0.0021(15) -0.0032(18) 0.0019(15) C2 0.020(2) 0.012(2) 0.020(2) -0.0011(16) 0.0046(18) 0.0037(15) C3 0.022(2) 0.016(2) 0.018(2) 0.0017(15) 0.0003(19) 0.0035(17) C4 0.020(3) 0.017(2) 0.022(3) -0.0035(18) -0.0035(18) 0.0006(15) C5 0.019(2) 0.013(2) 0.022(2) -0.002(2) 0.0008(16) 0.0004(16) C6 0.021(2) 0.0101(16) 0.019(2) -0.0026(16) 0.0016(17) 0.0016(16) C7 0.022(2) 0.0150(19) 0.022(2) 0.0031(18) -0.0024(18) -0.0011(16) C8 0.026(3) 0.016(2) 0.024(2) 0.0073(17) 0.005(2) 0.0010(18) C9 0.022(2) 0.012(2) 0.031(3) 0.0034(17) 0.005(2) -0.0027(17) 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 for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (Vol. C, Table 6.1.1.4) ; Br Br -0.2901 2.4595 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.0106 0.0060 ; International Tables for Crystallography (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 O2 C8 116.7(4) . . ? C6 O6 C9 118.3(3) . . ? C6 C1 C2 118.7(4) . . ? C6 C1 C7 120.2(4) . . ? C2 C1 C7 121.0(4) . . ? O2 C2 C3 124.1(4) . . ? O2 C2 C1 115.0(4) . . ? C3 C2 C1 120.9(4) . . ? C2 C3 C4 118.6(4) . . ? C2 C3 H3 120.7 . . ? C4 C3 H3 120.7 . . ? C5 C4 C3 122.1(4) . . ? C5 C4 H4 119.0 . . ? C3 C4 H4 119.0 . . ? C4 C5 C6 118.7(4) . . ? C4 C5 H5 120.7 . . ? C6 C5 H5 120.7 . . ? O6 C6 C5 124.3(4) . . ? O6 C6 C1 114.7(4) . . ? C5 C6 C1 121.0(4) . . ? C1 C7 Br7 112.4(3) . . ? C1 C7 H7A 109.1 . . ? Br7 C7 H7A 109.1 . . ? C1 C7 H7B 109.1 . . ? Br7 C7 H7B 109.1 . . ? H7A C7 H7B 107.9 . . ? O2 C8 H8A 109.5 . . ? O2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O6 C9 H9A 109.5 . . ? O6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? O6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? 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 Br7 C7 1.992(5) . ? O2 C2 1.370(5) . ? O2 C8 1.435(5) . ? O6 C6 1.359(5) . ? O6 C9 1.438(5) . ? C1 C6 1.406(6) . ? C1 C2 1.409(6) . ? C1 C7 1.487(6) . ? C2 C3 1.395(7) . ? C3 C4 1.401(7) . ? C3 H3 0.9500 . ? C4 C5 1.386(7) . ? C4 H4 0.9500 . ? C5 C6 1.400(6) . ? C5 H5 0.9500 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C8 O2 C2 C3 0.3(6) . . . . ? C8 O2 C2 C1 -178.1(3) . . . . ? C6 C1 C2 O2 -177.8(4) . . . . ? C7 C1 C2 O2 5.0(5) . . . . ? C6 C1 C2 C3 3.7(6) . . . . ? C7 C1 C2 C3 -173.5(4) . . . . ? O2 C2 C3 C4 180.0(4) . . . . ? C1 C2 C3 C4 -1.7(6) . . . . ? C2 C3 C4 C5 -0.5(7) . . . . ? C3 C4 C5 C6 0.6(7) . . . . ? C9 O6 C6 C5 -5.9(6) . . . . ? C9 O6 C6 C1 173.3(4) . . . . ? C4 C5 C6 O6 -179.4(4) . . . . ? C4 C5 C6 C1 1.5(6) . . . . ? C2 C1 C6 O6 177.2(3) . . . . ? C7 C1 C6 O6 -5.6(5) . . . . ? C2 C1 C6 C5 -3.6(6) . . . . ? C7 C1 C6 C5 173.7(4) . . . . ? C6 C1 C7 Br7 92.7(4) . . . . ? C2 C1 C7 Br7 -90.1(4) . . . . ?