#------------------------------------------------------------------------------ #$Date: 2021-06-04 03:57:48 +0300 (Fri, 04 Jun 2021) $ #$Revision: 265748 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/86/4518688.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_4518688 loop_ _publ_author_name 'Ishihara, Hideyuki' 'Huang, Jianhao' 'Mochizuki, Takuya' 'Hatano, Manabu' 'Ishihara, Kazuaki' _publ_section_title ; Enantio- and Diastereoselective Carbonyl-Ene Cyclization--Acetalization Tandem Reaction Catalyzed by Tris(pentafluorophenyl)borane-Assisted Chiral Phosphoric Acids ; _journal_issue 10 _journal_name_full 'ACS Catalysis' _journal_page_first 6121 _journal_page_last 6127 _journal_paper_doi 10.1021/acscatal.1c01242 _journal_volume 11 _journal_year 2021 _chemical_absolute_configuration (2S,4aS,7aR) _chemical_formula_sum 'C17 H23 Br O2' _chemical_formula_weight 339.26 _chemical_name_common ; (2S,4aS,7aR)-2-(3-bromophenyl)-4,4,7,7- tetramethylhexahydrocyclopenta[d][1,3]dioxine ; _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2014/6 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 5.9557(9) _cell_length_b 10.9058(17) _cell_length_c 24.740(4) _cell_measurement_reflns_used 5613 _cell_measurement_temperature 93(2) _cell_measurement_theta_max 27.485 _cell_measurement_theta_min 3.097 _cell_volume 1606.9(4) _computing_cell_refinement 'Rigaku CrystalClear' _computing_data_collection 'Rigaku CrystalClear' _computing_data_reduction 'Rigaku CrystalClear' _computing_molecular_graphics 'Rigaku CrystalStructure' _computing_publication_material 'Rigaku CrystalStructure' _computing_structure_refinement 'SHELXL-2014/6 (Sheldrick, 2014)' _computing_structure_solution 'Rigaku CrystalStructure' _diffrn_ambient_temperature 93(2) _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type 'PILATUS 200K area detector' _diffrn_measurement_method 'phi and omega scan' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71075 _diffrn_reflns_av_R_equivalents 0.0471 _diffrn_reflns_av_unetI/netI 0.0553 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_number 12662 _diffrn_reflns_point_group_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.989 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.440 _diffrn_reflns_theta_min 3.097 _exptl_absorpt_coefficient_mu 2.558 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'Rigaku CrystalClear' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.402 _exptl_crystal_description prism _exptl_crystal_F_000 704 _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_transmission_factor_max 1.000 _exptl_transmission_factor_min 0.854 _refine_diff_density_max 0.490 _refine_diff_density_min -0.663 _refine_diff_density_rms 0.078 _refine_ls_abs_structure_details ; Flack x determined using 1189 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.005(5) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.954 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 189 _refine_ls_number_reflns 3624 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.954 _refine_ls_R_factor_all 0.0372 _refine_ls_R_factor_gt 0.0305 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0282P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0637 _refine_ls_wR_factor_ref 0.0646 _reflns_Friedel_coverage 0.705 _reflns_Friedel_fraction_full 0.991 _reflns_Friedel_fraction_max 0.981 _reflns_number_gt 3125 _reflns_number_total 3624 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file cs1c01242_si_002.cif _cod_data_source_block CrystalClear _cod_depositor_comments 'Adding full bibliography for 4518688.cif.' _cod_database_code 4518688 _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 0.629 _shelx_estimated_absorpt_t_max 0.629 _shelxl_version_number 2014/6 _shelx_res_file ; TITL _20161122-1 REM Yadorkari-X generated CELL 0.71075 5.9557 10.9058 24.7400 90.0000 90.0000 90.0000 ZERR 4.0 0.0009 0.0017 0.0040 0.0000 0.0000 0.0000 LATT -1 SYMM 1/2-X, -Y, 1/2+Z SYMM 1/2+X, 1/2-Y, -Z SYMM -X, 1/2+Y, 1/2-Z REM SPGR P212121 orthorhombic SFAC C H O Br UNIT 68 92 8 4 SIZE 0.20 0.20 0.20 TEMP -180.0 L.S. 10 FMAP 2 PLAN -25 ACTA CONF LIST 4 WPDB -1 MERG 2 WGHT 0.028200 FVAR 1.01196 BR1 4 0.412195 1.396615 0.622336 11.00000 0.04003 0.02243 = 0.03901 -0.00802 -0.00470 0.01375 O1 3 0.931113 1.006386 0.647821 11.00000 0.01593 0.01520 = 0.01706 -0.00273 -0.00448 0.00433 O2 3 0.808162 0.857545 0.586102 11.00000 0.01521 0.00986 = 0.01892 -0.00006 -0.00344 0.00169 C1 1 1.119393 0.930995 0.661576 11.00000 0.01210 0.01417 = 0.01609 -0.00111 -0.00274 0.00252 AFIX 13 H1 2 1.245948 0.951800 0.636646 11.00000 -1.20000 AFIX 0 C16 1 0.374565 1.104880 0.515904 11.00000 0.02038 0.01712 = 0.02101 0.00437 -0.00347 -0.00045 AFIX 43 H16 2 0.283159 1.081572 0.486159 11.00000 -1.20000 AFIX 0 C14 1 0.467431 1.245802 0.585617 11.00000 0.02289 0.01372 = 0.02351 0.00224 0.00350 0.00322 C12 1 0.682830 1.062281 0.576203 11.00000 0.01311 0.01332 = 0.01693 0.00471 0.00284 0.00037 C10 1 0.858554 0.644545 0.596629 11.00000 0.01917 0.01471 = 0.01815 0.00042 -0.00062 -0.00060 AFIX 137 H10 2 0.789584 0.633319 0.561007 11.00000 -1.50000 H10A 2 0.741491 0.644223 0.624466 11.00000 -1.50000 H10B 2 0.964542 0.577609 0.603519 11.00000 -1.50000 AFIX 0 C13 1 0.644075 1.172786 0.602934 11.00000 0.01763 0.01733 = 0.01624 0.00102 -0.00048 0.00220 AFIX 43 H13 2 0.736382 1.197494 0.632295 11.00000 -1.20000 AFIX 0 C2 1 1.203986 0.943078 0.719966 11.00000 0.01626 0.01844 = 0.01784 -0.00204 -0.00321 0.00064 C9 1 1.164561 0.769067 0.554854 11.00000 0.02113 0.01892 = 0.01992 -0.00196 0.00379 0.00158 AFIX 137 H9 2 1.253210 0.844225 0.558856 11.00000 -1.50000 H9A 2 1.095036 0.767546 0.518958 11.00000 -1.50000 H9B 2 1.262763 0.697577 0.558990 11.00000 -1.50000 AFIX 0 C11 1 0.875035 0.980006 0.593246 11.00000 0.01583 0.00869 = 0.01743 0.00072 0.00081 -0.00035 H11 2 1.003330 1.003842 0.570885 11.00000 0.01038 C15 1 0.331746 1.214483 0.542964 11.00000 0.01651 0.01806 = 0.02490 0.00817 -0.00037 0.00210 AFIX 43 H15 2 0.211578 1.266248 0.532150 11.00000 -1.20000 AFIX 0 C17 1 0.550118 1.029450 0.532151 11.00000 0.01790 0.01245 = 0.01763 0.00151 0.00104 -0.00246 AFIX 43 H17 2 0.579649 0.955428 0.513197 11.00000 -1.20000 AFIX 0 C3 1 1.008862 0.947146 0.759998 11.00000 0.02172 0.06751 = 0.01883 -0.00945 -0.00096 -0.00341 AFIX 137 H3 2 0.919257 1.021100 0.753592 11.00000 -1.50000 H3A 2 1.067781 0.948524 0.796978 11.00000 -1.50000 H3B 2 0.914364 0.874423 0.755106 11.00000 -1.50000 AFIX 0 C6 1 1.280404 0.739011 0.677190 11.00000 0.01988 0.01929 = 0.02587 0.00029 -0.00618 0.00760 AFIX 23 H6 2 1.401389 0.740155 0.649753 11.00000 -1.20000 H6A 2 1.254919 0.653411 0.689014 11.00000 -1.20000 AFIX 0 C7 1 1.065477 0.795523 0.654986 11.00000 0.01141 0.01563 = 0.01430 0.00011 -0.00009 0.00185 AFIX 13 H7 2 0.941524 0.775341 0.680759 11.00000 -1.20000 AFIX 0 C8 1 0.982145 0.765727 0.598011 11.00000 0.01538 0.01141 = 0.01578 -0.00106 0.00042 0.00225 C5 1 1.339496 0.822195 0.725679 11.00000 0.03076 0.02768 = 0.03348 -0.00446 -0.01512 0.00989 AFIX 23 H5 2 1.502483 0.840023 0.725928 11.00000 -1.20000 H5A 2 1.300231 0.780692 0.759990 11.00000 -1.20000 AFIX 0 C4 1 1.349167 1.056905 0.727238 11.00000 0.03226 0.02747 = 0.03310 -0.00149 -0.01135 -0.00986 AFIX 137 H4 2 1.402237 1.061167 0.764686 11.00000 -1.50000 H4A 2 1.260351 1.130175 0.718945 11.00000 -1.50000 H4B 2 1.478300 1.052595 0.702761 11.00000 -1.50000 AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM _20161122-1 REM R1 = 0.0305 for 3125 Fo > 4sig(Fo) and 0.0372 for all 3624 data REM 189 parameters refined using 0 restraints END WGHT 0.0282 0.0000 REM Highest difference peak 0.490, deepest hole -0.663, 1-sigma level 0.078 Q1 1 0.3110 1.3460 0.6264 11.00000 0.05 0.49 Q2 1 0.4194 1.3980 0.5859 11.00000 0.05 0.42 Q3 1 0.4245 1.3971 0.6624 11.00000 0.05 0.39 Q4 1 0.5467 1.4937 0.6251 11.00000 0.05 0.37 Q5 1 0.2358 1.2792 0.6313 11.00000 0.05 0.32 Q6 1 1.4611 0.6520 0.6433 11.00000 0.05 0.26 Q7 1 -0.1284 1.3463 0.6279 11.00000 0.05 0.26 Q8 1 1.3327 0.6610 0.6639 11.00000 0.05 0.26 Q9 1 1.4530 0.6447 0.6079 11.00000 0.05 0.26 Q10 1 1.1894 0.6445 0.6275 11.00000 0.05 0.26 Q11 1 1.4456 0.8603 0.5836 11.00000 0.05 0.25 Q12 1 -0.1129 1.3943 0.5938 11.00000 0.05 0.23 Q13 1 1.4751 0.8778 0.5940 11.00000 0.05 0.23 Q14 1 0.0166 1.3880 0.6282 11.00000 0.05 0.22 Q15 1 1.4612 0.7802 0.6601 11.00000 0.05 0.22 Q16 1 0.5816 1.0164 0.5665 11.00000 0.05 0.22 Q17 1 0.6636 1.1853 0.6278 11.00000 0.05 0.21 Q18 1 -0.0033 1.2395 0.6159 11.00000 0.05 0.21 Q19 1 0.5800 0.7444 0.6270 11.00000 0.05 0.21 Q20 1 0.6812 1.0860 0.6068 11.00000 0.05 0.21 Q21 1 1.1235 1.2213 0.6931 11.00000 0.05 0.21 Q22 1 1.0100 1.1397 0.6287 11.00000 0.05 0.21 Q23 1 0.6204 0.5990 0.6567 11.00000 0.05 0.20 Q24 1 1.6426 0.7421 0.6685 11.00000 0.05 0.20 Q25 1 0.0146 1.2277 0.6604 11.00000 0.05 0.20 ; _shelx_res_checksum 62098 _shelx_hkl_file ; 0 0 5 2.06 13.14 0 0 -612213.33 469.36 0 0 -611352.40 444.81 0 0 611118.53 457.65 0 0 -7 29.99 25.38 0 0 -811287.13 437.37 0 0 -810363.47 410.20 0 0 -810683.33 441.38 0 0 810401.02 423.75 0 0 -9 0.55 24.01 0 0 9 -0.59 19.69 0 0 -10 149.72 23.66 0 0 -10 120.13 27.35 0 0 -10 121.73 24.86 0 0 10 123.27 26.22 0 0 -11 0.36 22.14 0 0 -11 3.90 24.21 0 0 11 -5.57 27.35 0 0 -12 570.41 43.93 0 0 -12 596.46 48.71 0 0 -12 620.31 52.11 0 0 12 599.28 48.52 0 0 -13 1.19 33.76 0 0 13 30.51 32.27 0 0 -14 347.75 38.94 0 0 -14 339.81 46.38 0 0 -14 346.91 32.18 0 0 -15 -2.78 26.95 0 0 -15 -0.01 39.57 0 0 -15 3.58 24.90 0 0 -16 248.09 32.49 0 0 -16 225.57 46.80 0 0 -16 204.41 31.49 0 0 -16 228.30 29.39 0 0 -17 0.54 24.82 0 0 -17 -1.38 42.73 0 0 -17 1.52 25.89 0 0 -18 166.14 43.45 0 0 -18 168.31 32.72 0 0 -18 168.13 29.94 0 0 -19 4.06 40.38 0 0 -19 2.90 28.81 0 0 -20 1411.75 126.28 0 0 -20 1403.70 121.43 0 0 -20 1390.28 115.19 0 0 -21 2.68 52.30 0 0 -21 -8.93 32.43 0 0 -22 90.73 56.80 0 0 -22 89.90 35.83 0 0 -22 88.99 33.52 0 0 -23 0.59 55.62 0 0 -24 640.08 84.81 0 0 -24 612.95 58.06 0 0 -25 -9.29 64.98 0 0 -26 139.44 65.83 0 0 -26 129.71 36.94 0 0 -27 21.67 68.41 0 0 -28 1310.37 116.93 0 0 -29 13.35 65.79 0 0 -30 237.01 71.89 0 0 -31 2.26 70.41 0 0 -32 618.36 77.22 0 1 3 1091.87 60.39 0 -1 3 1044.31 59.77 0 1 -3 1036.27 55.29 0 -1 3 1092.85 60.29 0 1 4 87.52 20.13 0 -1 -4 72.43 17.08 0 -1 4 77.92 17.81 0 1 -4 81.95 19.24 0 -1 4 85.89 20.60 0 -1 -4 66.04 20.75 0 1 5 2600.13 128.48 0 -1 -5 2482.22 112.77 0 -1 5 2523.20 117.60 0 1 -5 2282.59 124.59 0 -1 5 2619.14 160.93 0 -1 -5 2352.03 144.22 0 1 5 2264.73 107.41 0 1 615113.33 571.30 0 -1 -614741.15 556.88 0 1 -613986.03 538.03 0 -1 615302.68 583.20 0 -1 -614948.52 626.39 0 1 614269.62 543.67 0 1 7 3701.37 155.50 0 -1 -7 3410.77 146.40 0 1 -7 3520.69 155.54 0 -1 7 3315.90 146.61 0 1 -7 3794.33 156.60 0 -1 7 3727.89 174.97 0 -1 -7 3488.74 189.69 0 1 7 3303.43 147.07 0 1 8 306.83 27.98 0 -1 -8 304.57 28.71 0 1 -8 305.98 32.61 0 -1 8 309.18 32.12 0 1 -8 347.99 28.77 0 -1 8 344.14 40.30 0 -1 -8 336.24 40.25 0 1 8 292.33 33.60 0 1 9 5417.90 218.62 0 -1 -9 5338.52 218.81 0 1 -9 5677.78 235.06 0 -1 9 5201.08 216.72 0 1 -9 5291.52 215.81 0 -1 -9 5401.95 240.25 0 -1 9 5436.88 258.62 0 1 10 3875.48 167.09 0 -1 -10 4034.81 164.74 0 1 -10 4279.83 180.53 0 -1 10 3964.10 163.55 0 1 -10 4220.95 199.56 0 -1 -10 4195.29 200.44 0 -1 10 4197.70 212.66 0 1 11 2702.54 116.35 0 -1 -11 2651.21 117.47 0 1 -11 2616.11 119.66 0 -1 11 2514.06 112.35 0 -1 -11 2405.58 120.20 0 1 -11 2493.45 113.42 0 -1 -11 2806.04 163.37 0 -1 11 2707.59 123.88 0 1 -12 1544.99 77.08 0 1 12 1436.17 70.98 0 -1 -12 1443.67 74.32 0 1 -12 1361.47 80.33 0 -1 -12 1382.75 74.40 0 1 -12 1386.83 71.27 0 -1 -12 1450.95 97.69 0 -1 12 1514.74 75.09 0 1 -13 4166.40 176.62 0 -1 -13 3951.71 171.78 0 1 -13 3801.26 170.46 0 -1 -13 3821.93 159.83 0 -1 -13 4161.83 196.56 0 -1 13 3954.51 177.86 0 1 -1413023.65 587.21 0 -1 -1412469.31 473.48 0 1 -1412006.07 464.49 0 -1 -1413291.44 606.54 0 -1 -1412115.91 459.83 0 1 -1412345.52 537.79 0 -1 -1412678.18 572.28 0 -1 1413210.49 597.31 0 1 -15 1331.41 84.25 0 -1 -15 1265.93 106.27 0 1 -15 1393.80 88.14 0 -1 -15 1357.48 91.21 0 -1 -15 1230.30 72.75 0 -1 -15 1323.08 96.87 0 -1 15 1424.38 86.09 0 1 -16 1583.83 80.03 0 -1 -16 1561.45 80.23 0 1 -16 1660.83 91.07 0 -1 -16 1498.76 87.39 0 1 -16 1543.13 75.87 0 -1 -16 1524.05 75.42 0 1 -16 1637.02 171.30 0 -1 -16 1605.00 101.64 0 1 -17 767.21 59.96 0 -1 -17 771.37 54.55 0 1 -17 749.56 65.87 0 -1 -17 857.03 76.72 0 1 -17 738.76 52.14 0 -1 -17 773.95 53.67 0 -1 -17 774.57 183.04 0 1 -18 4657.11 254.19 0 -1 -18 4519.33 250.75 0 1 -18 4330.95 233.68 0 -1 -18 4480.13 243.05 0 1 -18 4669.02 264.97 0 -1 -18 4672.43 248.17 0 1 -19 1180.62 112.29 0 -1 -19 1126.25 108.32 0 1 -19 1073.27 94.85 0 -1 -19 1121.43 97.95 0 1 -19 1093.45 231.68 0 -1 -19 1163.17 101.26 0 1 -20 156.50 53.90 0 -1 -20 144.92 55.26 0 1 -20 147.88 38.30 0 -1 -20 149.41 36.41 0 -1 -20 151.18 37.90 0 1 -21 891.93 84.01 0 -1 -21 964.94 89.12 0 1 -21 883.42 75.10 0 -1 -21 935.91 76.94 0 1 -21 865.94 116.97 0 -1 -21 930.25 109.91 0 1 -22 490.91 68.41 0 -1 -22 482.94 74.93 0 1 -22 497.60 52.55 0 -1 -22 512.73 54.41 0 1 -22 493.82 106.21 0 -1 -22 513.60 52.81 0 1 -23 41.63 59.78 0 -1 -23 45.34 48.18 0 -1 -23 35.97 35.25 0 -1 -23 48.18 41.36 0 1 -24 250.27 53.72 0 -1 -24 272.10 64.34 0 -1 -24 248.42 81.13 0 1 -25 1171.36 118.17 0 -1 -25 1131.77 116.05 0 1 -25 1071.16 101.42 0 -1 -25 1071.49 104.17 0 1 -26 1093.59 85.53 0 -1 -26 1086.02 91.98 0 -1 -26 961.66 74.11 0 1 -27 5.08 62.18 0 -1 -27 -13.78 65.41 0 -1 -27 8.92 37.30 0 1 -28 65.60 64.19 0 -1 -28 71.18 57.92 0 1 -29 2.36 58.21 0 -1 -29 29.23 66.72 0 1 -30 32.56 69.78 0 -1 -30 18.07 69.78 0 1 -31 95.93 77.15 0 -1 -31 39.78 71.17 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28.48 64.87 -6 3 16 51.53 37.23 -6 3 -16 26.14 40.89 -6 -3 -16 36.30 53.77 -6 3 -17 111.89 63.40 -6 -3 -17 64.33 68.48 -6 3 17 64.53 36.21 -6 3 -17 97.72 49.96 -6 -3 -17 61.01 53.86 -6 -3 -18 57.59 67.09 -6 3 18 37.80 32.94 -6 3 -18 61.64 41.24 -6 -3 -18 41.96 52.84 -6 -3 -19 91.12 67.66 6 4 0 335.37 74.36 -6 4 0 437.49 44.12 -6 -4 0 394.57 53.85 6 4 1 203.34 65.59 -6 4 1 217.89 35.67 -6 4 -1 195.34 45.00 -6 -4 1 196.13 45.80 -6 -4 -1 205.82 70.11 6 4 2 116.19 60.24 -6 4 2 105.09 37.85 -6 4 -2 93.63 36.75 -6 -4 2 103.20 40.83 -6 -4 -2 92.97 64.48 6 4 3 184.35 72.63 -6 4 3 195.05 49.59 -6 -4 3 192.54 43.12 -6 -4 -3 211.53 39.22 6 4 4 242.17 46.86 -6 4 4 305.28 39.97 -6 -4 4 269.70 44.08 -6 -4 -4 301.11 69.87 6 4 5 29.64 49.65 -6 4 5 41.00 36.86 -6 -4 5 28.92 36.78 6 4 6 101.42 84.70 -6 4 6 83.20 38.11 -6 4 -6 99.35 44.75 -6 -4 6 100.04 40.13 -6 -4 -6 90.48 46.62 6 4 7 293.91 91.16 -6 4 7 298.11 33.99 -6 4 -7 302.34 47.58 -6 -4 7 326.56 46.70 -6 -4 -7 313.68 47.82 6 4 8 410.77 57.16 -6 4 8 583.42 54.75 -6 4 -8 424.00 57.09 -6 -4 8 447.64 52.30 -6 -4 -8 601.56 68.47 6 4 9 25.70 44.70 -6 4 9 -0.26 34.79 -6 4 -9 25.81 37.44 -6 -4 9 30.05 37.12 -6 4 10 5.45 36.35 -6 4 -10 -3.23 47.16 -6 -4 -10 1.83 41.17 -6 4 -11 95.65 56.26 -6 4 11 74.24 30.35 -6 4 -11 109.97 46.73 -6 -4 -11 82.57 44.10 6 4 12 562.36 65.79 -6 4 -12 599.12 84.04 -6 4 12 647.55 56.50 -6 4 -12 640.80 62.58 -6 -4 -12 616.38 65.25 6 4 13 94.01 51.42 -6 4 -13 70.31 73.81 -6 4 13 121.37 39.24 -6 4 -13 88.99 48.11 -6 -4 -13 114.78 55.35 6 4 14 104.58 48.77 -6 4 -14 82.78 61.64 -6 4 14 120.14 39.71 -6 4 -14 106.67 41.58 -6 -4 -14 97.58 56.60 6 4 15 57.46 49.80 -6 4 -15 63.47 61.16 -6 4 15 98.23 41.50 -6 4 -15 69.61 47.64 -6 4 -16 546.52 85.09 -6 4 16 555.65 62.34 -6 4 -16 559.03 71.10 -6 4 -17 110.11 64.87 -6 -4 -17 110.44 72.39 -6 4 17 139.99 35.25 -6 4 -17 131.72 48.63 -6 -4 -18 130.56 73.82 -6 5 0 -18.67 38.44 -6 5 1 40.72 39.22 6 5 2 867.31 80.96 -6 5 2 880.77 74.67 -6 -5 2 884.08 75.53 -6 -5 -2 936.66 80.20 -6 5 3 46.27 32.75 -6 -5 3 37.90 38.71 6 5 4 26.48 46.47 -6 5 4 38.92 37.79 -6 5 -4 19.23 41.30 -6 -5 -4 38.69 48.32 -6 5 -5 37.33 42.55 6 5 6 1346.45 107.07 -6 5 6 1186.79 84.83 -6 5 -6 1475.71 112.84 -6 -5 6 1460.71 105.56 -6 -5 -6 1273.29 100.10 -6 5 7 47.27 36.58 -6 -5 7 50.14 38.29 6 5 8 83.11 49.38 -6 5 8 85.79 36.28 -6 5 -8 59.32 37.62 -6 -5 -8 80.13 49.96 -6 5 9 1.16 36.94 -6 5 -9 -0.62 44.40 -6 -5 -9 -2.55 52.18 6 5 10 451.59 63.64 -6 5 10 460.45 51.65 -6 5 -10 498.07 55.00 -6 -5 -10 436.65 64.44 6 5 11 24.30 49.76 -6 5 11 0.29 36.43 -6 5 12 30.40 34.38 -6 5 -12 8.73 47.96 -6 -5 -12 1.82 54.59 6 5 13 136.96 67.82 -6 5 -13 131.90 63.07 -6 5 13 114.18 42.07 -6 5 -13 158.48 47.97 -6 -5 -13 117.39 47.99 6 5 14 225.28 48.90 -6 5 -14 233.85 66.44 -6 5 14 459.68 58.03 -6 5 -14 245.55 56.28 -6 -5 -14 393.17 68.91 6 5 15 -16.27 49.01 -6 5 -15 14.30 61.45 -6 5 15 1.49 36.89 -6 5 -15 -13.66 46.27 -6 -5 -15 -3.07 50.79 6 5 16 72.63 52.48 -6 5 -16 48.74 69.67 -6 5 16 67.65 35.94 -6 5 -16 57.28 40.47 6 6 0 120.55 68.87 -6 -6 0 178.72 50.51 6 6 1 178.54 58.79 -6 6 1 159.12 39.61 -6 -6 1 192.25 43.63 -6 -6 -1 172.03 46.49 -6 6 2 11.04 33.39 -6 -6 -2 4.48 43.90 -6 6 3 118.20 48.23 -6 6 -3 83.42 42.12 -6 -6 3 77.32 42.07 -6 -6 -3 122.88 70.85 6 6 4 346.11 57.57 -6 6 4 398.93 48.23 -6 6 -4 432.08 52.93 -6 -6 4 408.06 52.63 -6 -6 -4 397.98 59.37 -6 6 5 78.55 38.21 -6 6 -5 107.91 43.07 -6 -6 5 113.60 40.75 -6 6 6 9.45 37.63 -6 6 -6 3.83 43.38 -6 -6 6 0.78 44.22 6 6 7 244.29 107.27 -6 6 7 252.65 45.49 -6 6 -7 307.99 50.77 -6 -6 -7 255.84 89.49 6 6 8 417.66 63.04 -6 6 8 537.67 51.53 -6 6 -8 485.14 54.16 -6 -6 -8 540.82 69.07 -6 6 9 132.51 40.75 -6 6 -9 90.05 45.14 6 6 10 248.83 87.98 -6 6 10 268.79 45.90 -6 6 -10 302.72 50.46 -6 -6 -10 220.99 59.90 6 6 11 299.34 86.52 -6 6 11 252.47 50.21 -6 6 -11 323.95 56.14 -6 -6 -11 261.25 62.98 6 6 12 227.23 53.53 -6 6 12 313.58 46.48 -6 6 -12 237.18 46.49 -6 -6 -12 278.88 65.16 -6 6 13 43.05 41.86 -6 -6 -13 21.88 58.53 6 6 14 258.37 96.87 -6 6 14 274.79 39.69 -6 6 -14 277.04 49.11 -6 -6 -14 239.49 61.39 -6 -7 0 249.07 100.13 6 7 1 595.69 86.08 -6 7 -1 630.44 56.55 -6 -7 1 611.57 68.28 -6 -7 -1 725.12 80.30 6 7 2 259.24 93.99 -6 7 -2 262.22 40.22 -6 -7 2 292.40 83.32 -6 -7 -2 276.42 106.44 6 7 3 300.48 62.66 -6 7 3 293.60 45.23 -6 7 -3 352.92 43.03 -6 -7 3 343.19 49.63 -6 -7 -3 308.00 78.04 -6 7 4 104.16 53.09 -6 7 -4 182.29 43.05 -6 -7 4 168.77 48.79 6 7 5 649.82 68.13 -6 7 5 605.74 50.53 -6 7 -5 783.71 63.45 -6 -7 -5 658.31 67.96 -6 7 6 -0.05 40.11 6 7 7 273.48 56.71 -6 7 7 233.28 49.41 -6 7 -7 332.20 49.03 -6 -7 -7 223.65 58.37 -6 7 8 64.01 42.10 -6 7 -8 75.01 43.64 -6 -7 -8 46.03 61.54 6 7 9 298.44 61.95 -6 7 9 310.07 52.62 -6 7 -9 378.61 56.69 -6 -7 -9 282.02 63.47 6 7 10 108.38 54.81 -6 7 10 120.51 45.81 -6 7 -10 138.44 39.26 -6 -7 -10 113.88 57.25 6 7 11 58.36 51.26 -6 7 11 119.28 42.74 -6 7 -11 84.87 44.43 -6 -7 -11 88.44 60.43 -6 -7 -12 -8.30 59.20 6 8 0 133.70 88.30 -6 8 0 215.03 46.06 -6 -8 0 226.53 82.04 6 8 1 270.40 77.81 -6 8 -1 327.62 53.29 -6 -8 1 302.87 55.60 -6 -8 -1 357.39 74.14 -6 8 -2 76.91 41.10 -6 -8 2 64.54 46.50 6 8 3 185.59 53.57 -6 8 -3 270.75 48.34 -6 -8 -3 165.82 52.20 -6 8 4 -8.46 42.53 -6 8 -4 12.66 35.59 6 8 5 173.33 52.36 -6 8 5 217.98 45.22 -6 8 -5 234.13 43.43 -6 -8 -5 221.24 47.76 -6 8 -6 14.53 41.38 6 8 7 245.16 62.24 -6 8 7 452.30 50.30 -6 8 -7 347.71 45.52 -6 -8 -7 419.25 55.47 6 8 8 135.88 100.75 -6 8 8 177.50 47.15 -6 8 -8 196.51 43.96 -6 -8 -8 152.73 103.15 -7 0 0 10.31 42.81 -7 0 1 90.11 42.57 -7 0 -1 48.36 38.03 -7 0 2 376.20 51.97 -7 0 -2 353.98 53.22 -7 0 3 323.96 49.57 -7 0 -3 352.43 48.24 -7 0 4 1.90 40.90 -7 0 5 54.98 40.42 -7 0 -5 76.98 47.24 -7 0 6 284.94 41.63 -7 0 -6 292.00 46.15 -7 0 7 184.53 40.76 -7 0 -7 228.83 49.33 -7 0 8 3.58 38.71 -7 0 -8 15.42 50.13 -7 0 9 -11.12 39.44 -7 0 -9 0.77 41.30 -7 0 10 50.47 38.76 -7 0 11 99.61 38.50 -7 0 12 84.63 36.87 -7 0 -13 38.50 52.98 -7 1 0 40.70 43.10 -7 -1 0 41.65 43.18 -7 1 1 242.93 50.45 -7 1 -1 320.90 51.69 -7 -1 1 275.48 51.07 -7 -1 -1 235.83 42.86 -7 1 2 65.57 44.94 -7 1 -2 128.18 70.05 -7 -1 2 98.62 43.71 -7 -1 -2 66.96 52.17 -7 1 3 380.93 53.40 -7 -1 3 272.77 48.13 -7 1 -3 331.84 52.99 -7 -1 -3 336.79 47.84 -7 1 4 71.77 42.14 -7 -1 4 114.74 41.18 -7 1 -4 178.14 52.58 -7 -1 -4 119.94 55.81 -7 1 5 80.42 36.30 -7 -1 5 70.39 41.56 -7 1 -5 125.65 47.92 -7 -1 -5 99.36 47.40 -7 1 6 134.77 42.57 -7 -1 6 98.61 42.18 -7 1 -6 82.38 47.26 -7 -1 -6 123.42 42.01 -7 1 7 60.80 40.47 -7 -1 7 67.09 42.52 -7 1 -7 61.12 51.59 -7 -1 -7 47.77 48.43 -7 1 8 182.21 41.47 -7 -1 8 227.87 42.58 -7 1 -8 192.61 43.91 -7 -1 -8 189.57 50.22 -7 1 9 525.82 61.70 -7 -1 9 546.05 64.20 -7 -1 -9 557.38 67.27 -7 1 10 101.97 37.91 -7 -1 10 112.39 40.45 -7 -1 -10 134.92 51.04 -7 1 11 223.28 43.47 -7 -1 11 182.19 42.75 -7 -1 -11 200.74 55.79 -7 1 12 258.96 39.49 -7 1 -12 343.60 55.46 -7 1 13 175.66 37.98 -7 1 -13 101.86 52.81 -7 2 0 235.76 48.54 -7 -2 0 213.07 42.37 -7 2 1 77.26 44.01 -7 2 -1 102.78 44.18 -7 -2 1 82.54 37.85 -7 2 2 87.95 42.82 -7 2 -2 119.86 46.98 -7 -2 2 82.26 46.37 -7 -2 -2 110.24 44.79 -7 2 3 236.58 44.77 -7 2 -3 296.90 45.24 -7 -2 3 269.38 47.21 -7 -2 -3 232.96 50.16 -7 2 4 224.62 43.50 -7 2 -4 192.74 49.28 -7 -2 4 163.43 43.02 -7 -2 -4 219.05 48.31 -7 2 5 144.78 41.97 -7 -2 5 205.48 45.51 -7 2 -5 229.20 50.68 -7 -2 -5 164.41 54.45 -7 2 6 65.88 40.14 -7 -2 6 50.49 41.42 -7 2 -6 52.92 41.68 -7 -2 -6 43.97 46.56 -7 2 7 100.22 40.42 -7 -2 7 136.32 44.16 -7 -2 -7 125.06 48.52 -7 2 8 429.32 55.93 -7 -2 8 555.00 66.14 -7 -2 -8 438.15 60.11 -7 2 9 67.36 33.50 -7 -2 9 53.18 40.66 -7 -2 -9 93.25 51.40 -7 2 10 -11.71 36.47 -7 2 -10 12.49 50.71 -7 -2 -10 -1.63 50.66 -7 2 11 33.11 36.89 -7 2 -11 54.26 53.88 -7 -2 -11 60.86 44.23 -7 2 12 188.44 38.66 -7 2 -12 268.56 53.63 -7 -2 -12 193.29 48.80 -7 3 0 55.64 53.80 -7 -3 0 43.68 48.51 -7 3 1 333.67 78.31 -7 3 -1 316.15 50.50 -7 -3 1 287.23 49.21 -7 -3 -1 347.84 64.04 -7 3 2 354.28 50.92 -7 3 -2 371.94 54.56 -7 -3 2 363.06 49.19 -7 -3 -2 384.25 91.68 -7 3 3 286.67 46.58 -7 3 -3 263.95 50.97 -7 -3 3 268.25 47.48 -7 -3 -3 269.85 87.66 -7 3 4 23.78 40.60 -7 3 -4 46.95 47.62 -7 -3 4 31.52 41.17 -7 3 5 150.31 41.37 -7 3 -5 101.06 48.44 -7 -3 5 88.62 44.15 -7 -3 -5 125.36 42.66 -7 3 6 153.01 41.85 -7 -3 6 89.01 42.85 -7 -3 -6 163.92 52.59 -7 3 7 189.17 43.52 -7 -3 7 160.85 44.88 -7 -3 -7 164.55 52.42 -7 3 8 71.44 39.11 -7 -3 8 112.27 42.10 -7 -3 -8 82.73 49.61 -7 3 9 69.06 38.58 -7 3 -9 48.41 42.44 -7 -3 -9 69.09 52.19 -7 3 10 285.60 39.77 -7 3 -10 219.92 52.83 -7 -3 -10 323.46 55.89 -7 3 11 349.88 40.71 -7 3 -11 305.22 53.05 -7 -3 -11 328.26 49.38 -7 4 0 362.67 51.00 -7 -4 0 346.28 51.35 -7 4 -1 87.86 43.94 -7 4 2 476.53 60.81 -7 4 -2 412.88 62.22 -7 -4 2 403.60 55.09 -7 -4 -2 455.32 63.33 -7 4 3 96.00 55.29 -7 4 -3 159.57 50.08 -7 -4 3 179.34 56.34 -7 4 4 185.63 44.81 -7 -4 4 276.51 50.46 -7 -4 -4 191.69 51.65 -7 4 5 229.81 46.04 -7 -4 5 313.35 52.36 -7 -4 -5 233.99 54.47 -7 4 6 107.63 40.13 -7 -4 6 63.81 42.08 -7 -4 -6 99.79 54.84 -7 4 7 120.16 43.09 -7 4 -7 201.31 43.81 -7 -4 -7 155.69 51.92 -7 4 8 161.01 35.34 -7 4 -8 197.93 52.64 -7 -4 -8 164.03 53.39 -7 4 9 126.81 39.17 -7 4 -9 180.28 44.60 -7 -4 -9 120.80 46.64 -7 5 0 -6.59 41.18 -7 -5 0 -3.23 44.38 -7 5 1 131.25 37.44 -7 5 -1 126.56 44.47 -7 -5 1 138.03 44.30 -7 -5 -1 132.56 40.88 -7 5 2 25.92 43.30 -7 5 -2 18.01 45.12 -7 -5 3 2.81 42.61 -7 -5 -3 3.26 45.83 -7 5 4 99.07 47.44 -7 -5 4 149.14 44.37 -7 -5 -4 117.94 51.06 -7 5 5 330.92 42.58 -7 -5 5 281.97 49.25 -7 -5 -5 340.76 53.74 -7 5 6 6.07 38.74 -7 5 -6 -14.24 47.06 -7 5 7 -2.00 39.49 -7 5 -7 -1.49 47.49 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 12809 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -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 _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 0.41220(7) 1.39662(4) 0.62234(2) 0.03382(12) Uani 1 1 d . . . . . O1 O 0.9311(4) 1.00639(19) 0.64782(8) 0.0161(5) Uani 1 1 d . . . . . O2 O 0.8082(4) 0.85754(19) 0.58610(8) 0.0147(5) Uani 1 1 d . . . . . C1 C 1.1194(5) 0.9310(3) 0.66158(12) 0.0141(7) Uani 1 1 d . . . . . H1 H 1.2459 0.9518 0.6366 0.017 Uiso 1 1 calc R U . . . C16 C 0.3746(6) 1.1049(3) 0.51590(12) 0.0195(7) Uani 1 1 d . . . . . H16 H 0.2832 1.0816 0.4862 0.023 Uiso 1 1 calc R U . . . C14 C 0.4674(6) 1.2458(3) 0.58562(14) 0.0200(8) Uani 1 1 d . . . . . C12 C 0.6828(5) 1.0623(3) 0.57620(12) 0.0145(7) Uani 1 1 d . . . . . C10 C 0.8586(6) 0.6445(3) 0.59663(13) 0.0173(7) Uani 1 1 d . . . . . H10 H 0.7896 0.6333 0.5610 0.026 Uiso 1 1 calc R U . . . H10A H 0.7415 0.6442 0.6245 0.026 Uiso 1 1 calc R U . . . H10B H 0.9645 0.5776 0.6035 0.026 Uiso 1 1 calc R U . . . C13 C 0.6441(5) 1.1728(3) 0.60293(13) 0.0171(7) Uani 1 1 d . . . . . H13 H 0.7364 1.1975 0.6323 0.020 Uiso 1 1 calc R U . . . C2 C 1.2040(6) 0.9431(3) 0.71997(13) 0.0175(7) Uani 1 1 d . . . . . C9 C 1.1646(6) 0.7691(3) 0.55485(13) 0.0200(7) Uani 1 1 d . . . . . H9 H 1.2532 0.8442 0.5589 0.030 Uiso 1 1 calc R U . . . H9A H 1.0950 0.7675 0.5190 0.030 Uiso 1 1 calc R U . . . H9B H 1.2628 0.6976 0.5590 0.030 Uiso 1 1 calc R U . . . C11 C 0.8750(6) 0.9800(3) 0.59325(12) 0.0140(7) Uani 1 1 d . . . . . H11 H 1.003(6) 1.004(3) 0.5709(12) 0.010(9) Uiso 1 1 d . . . . . C15 C 0.3317(6) 1.2145(3) 0.54296(13) 0.0198(7) Uani 1 1 d . . . . . H15 H 0.2116 1.2662 0.5321 0.024 Uiso 1 1 calc R U . . . C17 C 0.5501(6) 1.0295(3) 0.53215(12) 0.0160(7) Uani 1 1 d . . . . . H17 H 0.5796 0.9554 0.5132 0.019 Uiso 1 1 calc R U . . . C3 C 1.0089(7) 0.9471(5) 0.76000(14) 0.0360(11) Uani 1 1 d . . . . . H3 H 0.9193 1.0211 0.7536 0.054 Uiso 1 1 calc R U . . . H3A H 1.0678 0.9485 0.7970 0.054 Uiso 1 1 calc R U . . . H3B H 0.9144 0.8744 0.7551 0.054 Uiso 1 1 calc R U . . . C6 C 1.2804(6) 0.7390(3) 0.67719(13) 0.0217(8) Uani 1 1 d . . . . . H6 H 1.4014 0.7402 0.6498 0.026 Uiso 1 1 calc R U . . . H6A H 1.2549 0.6534 0.6890 0.026 Uiso 1 1 calc R U . . . C7 C 1.0655(6) 0.7955(3) 0.65499(12) 0.0138(6) Uani 1 1 d . . . . . H7 H 0.9415 0.7753 0.6808 0.017 Uiso 1 1 calc R U . . . C8 C 0.9821(5) 0.7657(3) 0.59801(13) 0.0142(7) Uani 1 1 d . . . . . C5 C 1.3395(7) 0.8222(4) 0.72568(15) 0.0306(9) Uani 1 1 d . . . . . H5 H 1.5025 0.8400 0.7259 0.037 Uiso 1 1 calc R U . . . H5A H 1.3002 0.7807 0.7600 0.037 Uiso 1 1 calc R U . . . C4 C 1.3492(7) 1.0569(4) 0.72724(15) 0.0309(9) Uani 1 1 d . . . . . H4 H 1.4022 1.0612 0.7647 0.046 Uiso 1 1 calc R U . . . H4A H 1.2604 1.1302 0.7189 0.046 Uiso 1 1 calc R U . . . H4B H 1.4783 1.0526 0.7028 0.046 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 Br1 0.0400(2) 0.02243(16) 0.0390(2) -0.00802(18) -0.0047(2) 0.01375(18) O1 0.0159(12) 0.0152(11) 0.0171(10) -0.0027(8) -0.0045(10) 0.0043(10) O2 0.0152(11) 0.0099(11) 0.0189(11) -0.0001(9) -0.0034(9) 0.0017(9) C1 0.0121(17) 0.0142(15) 0.0161(15) -0.0011(11) -0.0027(13) 0.0025(12) C16 0.0204(19) 0.0171(14) 0.0210(16) 0.0044(15) -0.0035(13) -0.0005(16) C14 0.023(2) 0.0137(16) 0.0235(18) 0.0022(14) 0.0035(14) 0.0032(13) C12 0.0131(15) 0.0133(15) 0.0169(16) 0.0047(12) 0.0028(13) 0.0004(13) C10 0.0192(19) 0.0147(15) 0.0182(16) 0.0004(13) -0.0006(13) -0.0006(13) C13 0.0176(18) 0.0173(17) 0.0162(16) 0.0010(12) -0.0005(12) 0.0022(13) C2 0.0163(17) 0.0184(16) 0.0178(16) -0.0020(13) -0.0032(14) 0.0006(14) C9 0.0211(18) 0.0189(17) 0.0199(17) -0.0020(14) 0.0038(14) 0.0016(14) C11 0.0158(18) 0.0087(14) 0.0174(16) 0.0007(12) 0.0008(14) -0.0003(13) C15 0.0165(17) 0.0181(17) 0.0249(18) 0.0082(14) -0.0004(14) 0.0021(13) C17 0.0179(19) 0.0124(15) 0.0176(16) 0.0015(12) 0.0010(13) -0.0025(13) C3 0.0217(19) 0.068(3) 0.0188(19) -0.0094(19) -0.0010(15) -0.003(2) C6 0.0199(19) 0.0193(18) 0.0259(19) 0.0003(15) -0.0062(15) 0.0076(15) C7 0.0114(16) 0.0156(15) 0.0143(15) 0.0001(12) -0.0001(13) 0.0018(14) C8 0.0154(17) 0.0114(15) 0.0158(16) -0.0011(12) 0.0004(12) 0.0022(12) C5 0.031(2) 0.028(2) 0.033(2) -0.0045(17) -0.0151(16) 0.0099(17) C4 0.032(2) 0.027(2) 0.033(2) -0.0015(16) -0.0114(17) -0.0099(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 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' Br Br -0.2901 2.4595 '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 C11 O1 C1 107.1(2) . . ? C11 O2 C8 115.0(2) . . ? O1 C1 C7 111.5(3) . . ? O1 C1 C2 115.6(2) . . ? C7 C1 C2 104.7(2) . . ? C17 C16 C15 120.4(3) . . ? C15 C14 C13 122.8(3) . . ? C15 C14 Br1 118.6(3) . . ? C13 C14 Br1 118.6(3) . . ? C17 C12 C13 120.0(3) . . ? C17 C12 C11 119.6(3) . . ? C13 C12 C11 120.4(3) . . ? C14 C13 C12 118.4(3) . . ? C4 C2 C3 109.4(3) . . ? C4 C2 C1 111.5(3) . . ? C3 C2 C1 111.3(3) . . ? C4 C2 C5 112.7(3) . . ? C3 C2 C5 111.2(3) . . ? C1 C2 C5 100.6(3) . . ? O2 C11 O1 112.3(2) . . ? O2 C11 C12 108.3(3) . . ? O1 C11 C12 108.8(3) . . ? C14 C15 C16 118.4(3) . . ? C16 C17 C12 120.1(3) . . ? C7 C6 C5 103.5(3) . . ? C1 C7 C6 100.2(3) . . ? C1 C7 C8 111.9(3) . . ? C6 C7 C8 121.3(3) . . ? O2 C8 C10 104.3(2) . . ? O2 C8 C9 110.2(3) . . ? C10 C8 C9 110.6(3) . . ? O2 C8 C7 105.6(2) . . ? C10 C8 C7 111.4(3) . . ? C9 C8 C7 114.2(3) . . ? C6 C5 C2 108.0(3) . . ? 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 Br1 C14 1.908(3) . ? O1 C11 1.420(4) . ? O1 C1 1.432(4) . ? O2 C11 1.405(4) . ? O2 C8 1.471(4) . ? C1 C7 1.521(4) . ? C1 C2 1.536(4) . ? C16 C17 1.390(5) . ? C16 C15 1.394(5) . ? C14 C15 1.372(5) . ? C14 C13 1.387(4) . ? C12 C17 1.393(4) . ? C12 C13 1.394(4) . ? C12 C11 1.514(4) . ? C10 C8 1.513(4) . ? C2 C4 1.523(5) . ? C2 C3 1.528(5) . ? C2 C5 1.552(5) . ? C9 C8 1.524(4) . ? C6 C7 1.523(5) . ? C6 C5 1.545(5) . ? C7 C8 1.529(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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 O1 C1 C7 -59.1(3) . . . . ? C11 O1 C1 C2 -178.5(3) . . . . ? C15 C14 C13 C12 -0.9(5) . . . . ? Br1 C14 C13 C12 179.6(2) . . . . ? C17 C12 C13 C14 2.0(5) . . . . ? C11 C12 C13 C14 179.4(3) . . . . ? O1 C1 C2 C4 -79.4(4) . . . . ? C7 C1 C2 C4 157.5(3) . . . . ? O1 C1 C2 C3 43.0(4) . . . . ? C7 C1 C2 C3 -80.1(4) . . . . ? O1 C1 C2 C5 160.8(3) . . . . ? C7 C1 C2 C5 37.7(3) . . . . ? C8 O2 C11 O1 -63.2(3) . . . . ? C8 O2 C11 C12 176.6(2) . . . . ? C1 O1 C11 O2 62.7(3) . . . . ? C1 O1 C11 C12 -177.4(2) . . . . ? C17 C12 C11 O2 -37.0(4) . . . . ? C13 C12 C11 O2 145.6(3) . . . . ? C17 C12 C11 O1 -159.3(3) . . . . ? C13 C12 C11 O1 23.3(4) . . . . ? C13 C14 C15 C16 -0.3(5) . . . . ? Br1 C14 C15 C16 179.3(2) . . . . ? C17 C16 C15 C14 0.3(5) . . . . ? C15 C16 C17 C12 0.9(5) . . . . ? C13 C12 C17 C16 -2.1(5) . . . . ? C11 C12 C17 C16 -179.4(3) . . . . ? O1 C1 C7 C6 -174.6(2) . . . . ? C2 C1 C7 C6 -49.0(3) . . . . ? O1 C1 C7 C8 55.5(3) . . . . ? C2 C1 C7 C8 -178.8(3) . . . . ? C5 C6 C7 C1 39.0(3) . . . . ? C5 C6 C7 C8 162.6(3) . . . . ? C11 O2 C8 C10 170.7(2) . . . . ? C11 O2 C8 C9 -70.6(3) . . . . ? C11 O2 C8 C7 53.2(3) . . . . ? C1 C7 C8 O2 -48.5(3) . . . . ? C6 C7 C8 O2 -166.4(3) . . . . ? C1 C7 C8 C10 -161.2(3) . . . . ? C6 C7 C8 C10 80.9(4) . . . . ? C1 C7 C8 C9 72.7(4) . . . . ? C6 C7 C8 C9 -45.2(4) . . . . ? C7 C6 C5 C2 -16.6(4) . . . . ? C4 C2 C5 C6 -131.4(3) . . . . ? C3 C2 C5 C6 105.4(4) . . . . ? C1 C2 C5 C6 -12.5(4) . . . . ?