#------------------------------------------------------------------------------ #$Date: 2024-07-05 21:00:30 +0300 (Fri, 05 Jul 2024) $ #$Revision: 293277 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/15/98/7159882.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_7159882 loop_ _publ_author_name 'Tsutsui, Yuya' 'Yanaka, Issei' 'Takeda, Kazuhiro' 'Kondo, Masaru' 'Takizawa, Shinobu' 'Kojima, Ryosuke' 'Konishi, Akihito' 'Yasuda, Makoto' _publ_section_title ; Selective recognition between aromatics and aliphatics by cage-shaped borates supported by a machine learning approach. ; _journal_issue 21 _journal_name_full 'Organic & biomolecular chemistry' _journal_page_first 4283 _journal_page_last 4291 _journal_paper_doi 10.1039/d4ob00408f _journal_volume 22 _journal_year 2024 _chemical_formula_moiety 'C48 H28 B Br2 N O6, C H Cl3' _chemical_formula_sum 'C49 H29 B Br2 Cl3 N O6' _chemical_formula_weight 1004.71 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2022-04-05 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2023-09-27 deposited with the CCDC. 2024-04-04 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 103.3290(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.39030(10) _cell_length_b 32.0048(2) _cell_length_c 10.89300(10) _cell_measurement_reflns_used 29084 _cell_measurement_temperature 190 _cell_measurement_theta_max 74.3070 _cell_measurement_theta_min 3.6450 _cell_volume 4203.25(6) _computing_cell_refinement 'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 190 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -60.00 -12.00 0.50 0.79 -- -42.93 71.00-105.00 96 2 \w -76.00 -34.00 0.50 3.67 -- -106.00 77.00-180.00 84 3 \w -61.00 -32.00 0.50 3.67 -- -106.00 77.00-120.00 58 4 \w -53.00 -28.00 0.50 3.67 -- -106.00 19.00-150.00 50 5 \w -88.00 -51.00 0.50 3.67 -- -106.00 37.00-120.00 74 6 \w -87.00 -37.00 0.50 3.67 -- -106.00 0.00 -90.00 100 7 \w -106.00 -81.00 0.50 3.67 -- -106.00 71.00-105.00 50 8 \w -110.00 -84.00 0.50 3.67 -- -106.00 80.00-115.13 52 9 \w -126.00-100.00 0.50 3.67 -- -106.00 77.00-180.00 52 10 \w -135.00 -79.00 0.50 3.67 -- -106.00 77.00-120.00 112 11 \w -116.00 -51.00 0.50 3.67 -- -106.00 125.00 -90.00 130 12 \w -68.00 -43.00 0.50 3.67 -- -106.00 125.00 -30.00 50 13 \w -94.00 -36.00 0.50 3.67 -- -106.00 77.00 60.00 116 14 \w -95.00 -69.00 0.50 3.67 -- -106.00 57.00 30.00 52 15 \w -121.00 -85.00 0.50 3.67 -- -106.00 -19.00 90.00 72 16 \w -106.00 -79.00 0.50 3.67 -- -106.00 -77.00 150.00 54 17 \w -103.00 -78.00 0.50 3.67 -- -106.00 -77.00 120.00 50 18 \w -102.00 -71.00 0.50 3.67 -- -106.00-125.00 120.00 62 19 \w -117.00 -86.00 0.50 3.67 -- -106.00 -96.00 28.76 62 20 \w -124.00 -94.00 0.50 3.67 -- -106.00 -57.00 -60.00 60 21 \w -119.00 -89.00 0.50 3.67 -- -106.00 -67.00 -85.80 60 22 \w -124.00 -91.00 0.50 3.67 -- -106.00 -77.00-150.00 66 23 \w -115.00 -71.00 0.50 0.79 -- -42.93-125.00-150.00 88 24 \w -149.00-123.00 0.50 3.67 -- -106.00 -19.00 0.00 52 25 \w -166.00-140.00 0.50 3.67 -- -106.00 -57.00 -60.00 52 26 \w -151.00-125.00 0.50 3.67 -- -106.00 -67.00 -85.80 52 27 \w -174.00 -68.00 0.50 3.67 -- -106.00 -9.00 -57.84 212 28 \w -135.00 -39.00 0.50 3.67 -- -106.00 77.00 30.00 192 29 \w -119.00 -42.00 0.50 3.67 -- -106.00 77.00 -30.00 154 30 \w -124.00 -45.00 0.50 3.67 -- -106.00 60.00 -59.10 158 31 \w -100.00 -16.00 0.50 0.79 -- -42.93 -71.00 124.00 168 32 \w 59.00 96.00 0.50 0.79 -- 42.93 71.00-105.00 74 33 \w 76.00 101.00 0.50 3.67 -- 76.50 71.00-105.00 50 34 \w 22.00 117.00 0.50 0.79 -- 42.93 57.00-150.00 190 35 \w 15.00 43.00 0.50 0.79 -- 42.93 -71.00 124.00 56 36 \w 18.00 43.00 0.50 3.67 -- 76.50 -71.00 124.00 50 37 \w 73.00 111.00 0.50 0.79 -- 42.93 125.00 120.00 76 38 \w -117.00 -91.00 0.50 3.67 -- -106.00 -19.00 150.00 52 39 \w -123.00 -92.00 0.50 3.67 -- -106.00 -71.00 124.00 62 40 \w -120.00 -95.00 0.50 3.67 -- -106.00 -57.00 120.00 50 41 \w -146.00-121.00 0.50 3.67 -- -106.00-125.00 120.00 50 42 \w -134.00-108.00 0.50 3.67 -- -106.00-125.00 90.00 52 43 \w -139.00-113.00 0.50 3.67 -- -106.00-125.00 30.00 52 44 \w -166.00-135.00 0.50 3.67 -- -106.00 -96.00 28.76 62 45 \w -158.00-122.00 0.50 3.67 -- -106.00 -77.00 150.00 72 46 \w -171.00-113.00 0.50 3.67 -- -106.00 -37.00 150.00 116 47 \w -175.00-150.00 0.50 3.67 -- -106.00 -19.00 150.00 50 48 \w -120.00 -80.00 0.50 3.67 -- -106.00 37.00 -60.00 80 49 \w -163.00-138.00 0.50 3.67 -- -106.00 0.00 -90.00 50 50 \w -176.00-122.00 0.50 3.67 -- -106.00 -99.00 -90.00 108 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Single source at offset/far, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0037212000 _diffrn_orient_matrix_UB_12 0.0379967000 _diffrn_orient_matrix_UB_13 -0.0858595000 _diffrn_orient_matrix_UB_21 -0.1256851000 _diffrn_orient_matrix_UB_22 0.0063680000 _diffrn_orient_matrix_UB_23 -0.0155909000 _diffrn_orient_matrix_UB_31 0.0227083000 _diffrn_orient_matrix_UB_32 0.0288751000 _diffrn_orient_matrix_UB_33 0.1161890000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0447 _diffrn_reflns_av_unetI/netI 0.0324 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 54661 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 74.276 _diffrn_reflns_theta_min 3.666 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 4.642 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.57360 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.43a (Rigaku Oxford Diffraction, 2019) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'translucent intense colourless' _exptl_crystal_density_diffrn 1.588 _exptl_crystal_description block _exptl_crystal_F_000 2016 _exptl_crystal_size_max 0.099 _exptl_crystal_size_mid 0.068 _exptl_crystal_size_min 0.066 _refine_diff_density_max 0.696 _refine_diff_density_min -0.816 _refine_diff_density_rms 0.061 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 578 _refine_ls_number_reflns 8499 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.053 _refine_ls_R_factor_all 0.0361 _refine_ls_R_factor_gt 0.0334 _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^)+(0.0525P)^2^+1.6670P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0917 _refine_ls_wR_factor_ref 0.0939 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7796 _reflns_number_total 8499 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4ob00408f2.cif _cod_data_source_block 1121 _cod_depositor_comments 'Adding full bibliography for 7159882--7159883.cif.' _cod_database_code 7159882 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'C30 H30 O B Br Cl' _chemical_oxdiff_usercomment CHCl3/hexane _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. ; _reflns_odcompleteness_completeness 98.83 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 74.33 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups 2. Others Sof(Br1)=Sof(Br2)=1-FVAR(1) Sof(Br01)=Sof(Br02)=FVAR(1) 3.a Ternary CH refined with riding coordinates: C1(H1), C49(H49) 3.b Aromatic/amide H refined with riding coordinates: C7(H7), C21(H21), C44(H44), C5(H5), C48(H48), C19(H19), C6(H6), C13(H13), C46(H46), C17(H17), C29(H29), C18(H18), C11(H11), C37(H37), C12(H12), C26(H26), C23(H23), C24(H24), C42(H42), C25(H25), C34(H34), C41(H41), C31(H31), C40(H40), C39(H39), C33(H33), C32(H32) ; _shelx_res_file ; TITL 1121_a.res in P2(1)/c 1121.res created by SHELXL-2018/3 at 20:07:01 on 05-Apr-2022 REM Old TITL 1121 in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.229, Rweak 0.019, Alpha 0.041 REM 0.540 for 178 systematic absences, Orientation as input REM Formula found by SHELXT: C50 B O6 Cl3 Br2 CELL 1.54184 12.3903 32.0048 10.893 90 103.329 90 ZERR 4 0.0001 0.0002 0.0001 0 0.001 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H B Br Cl N O UNIT 196 116 4 8 12 4 24 L.S. 45 PLAN 20 TEMP -83.15 BOND list 4 fmap 2 ACTA REM REM REM WGHT 0.052500 1.667000 FVAR 0.19569 0.53287 PART 1 BR01 4 0.455882 0.669794 0.485740 21.00000 0.03793 0.03874 = 0.08034 0.00948 0.03741 -0.00016 BR02 4 0.266886 0.519043 0.610128 21.00000 0.04655 0.02220 = 0.08187 -0.00341 0.02543 0.00390 PART 0 CL2 5 0.627583 0.568219 0.516798 11.00000 0.05187 0.06456 = 0.06064 -0.02204 0.02086 0.00220 CL1 5 0.604559 0.599171 0.758785 11.00000 0.05162 0.09053 = 0.05206 -0.01355 0.02286 0.00186 CL3 5 0.817967 0.572632 0.725155 11.00000 0.04407 0.08354 = 0.08838 -0.01046 0.00871 0.01042 O1 7 0.086758 0.710216 0.605430 11.00000 0.02661 0.01983 = 0.01924 -0.00145 0.00891 0.00070 O3 7 -0.016041 0.644872 0.598618 11.00000 0.02169 0.02274 = 0.02146 -0.00066 0.00481 -0.00039 O2 7 0.106147 0.667088 0.794044 11.00000 0.02339 0.02669 = 0.01867 -0.00051 0.00741 -0.00150 O4 7 0.322857 0.804860 0.653300 11.00000 0.03047 0.03438 = 0.02107 -0.00087 0.00258 -0.00872 O6 7 -0.204325 0.597513 0.254896 11.00000 0.04147 0.03443 = 0.02220 -0.00103 0.00129 -0.00607 O5 7 0.166722 0.586617 1.108805 11.00000 0.04328 0.03419 = 0.02546 0.00734 0.00634 -0.00151 N1 6 0.183456 0.643092 0.621150 11.00000 0.02227 0.02371 = 0.01849 -0.00065 0.00525 0.00064 C20 1 0.231357 0.780389 0.599700 11.00000 0.02467 0.02063 = 0.02135 0.00283 0.00165 -0.00216 C15 1 -0.113641 0.662919 0.541929 11.00000 0.02099 0.02508 = 0.02166 0.00372 0.00709 -0.00228 C3 1 0.072750 0.745597 0.669939 11.00000 0.02543 0.02067 = 0.01783 0.00023 0.00498 0.00294 C4 1 0.145661 0.779550 0.672229 11.00000 0.02934 0.02220 = 0.01782 0.00206 0.00415 0.00254 C9 1 0.026410 0.660588 0.859571 11.00000 0.02625 0.02646 = 0.01948 -0.00385 0.00837 -0.00523 C8 1 -0.074748 0.681906 0.829177 11.00000 0.02903 0.02695 = 0.02212 -0.00250 0.00997 -0.00201 C7 1 -0.022383 0.784124 0.803201 11.00000 0.03231 0.02722 = 0.02223 -0.00088 0.00888 0.00728 AFIX 43 H7 2 -0.080184 0.786012 0.847055 11.00000 -1.20000 AFIX 0 C21 1 0.239570 0.765389 0.486294 11.00000 0.02640 0.02385 = 0.02300 -0.00014 0.00611 -0.00349 AFIX 43 H21 2 0.187594 0.747859 0.432122 11.00000 -1.20000 AFIX 0 C16 1 -0.175831 0.645103 0.428768 11.00000 0.02307 0.02885 = 0.02415 0.00290 0.00646 -0.00492 C36 1 -0.140857 0.607038 0.374264 11.00000 0.02722 0.03143 = 0.02016 -0.00149 0.00477 -0.00975 C14 1 -0.154343 0.698128 0.594087 11.00000 0.02226 0.02799 = 0.02505 0.00228 0.00930 -0.00068 C44 1 0.260638 0.662481 0.574253 11.00000 0.02700 0.02583 = 0.02850 0.00360 0.01018 0.00104 AFIX 43 H44 2 0.258467 0.692006 0.564999 11.00000 -1.20000 AFIX 0 C5 1 0.134396 0.814827 0.745102 11.00000 0.03627 0.02242 = 0.02215 0.00036 0.00401 0.00001 AFIX 43 H5 2 0.184354 0.837570 0.749056 11.00000 -1.20000 AFIX 0 C1 1 -0.102786 0.715081 0.725938 11.00000 0.02460 0.02715 = 0.02479 -0.00082 0.01113 0.00369 AFIX 13 H1 2 -0.165315 0.730806 0.748311 11.00000 -1.20000 AFIX 0 C2 1 -0.014004 0.748435 0.732400 11.00000 0.02758 0.02407 = 0.01952 0.00037 0.00713 0.00374 C48 1 0.186827 0.601593 0.638054 11.00000 0.02521 0.02368 = 0.02724 0.00118 0.00698 0.00066 AFIX 43 H48 2 0.133588 0.588369 0.675318 11.00000 -1.20000 AFIX 0 C28 1 0.157539 0.611683 1.002032 11.00000 0.03688 0.02539 = 0.01828 0.00084 0.00169 -0.00534 C10 1 0.050649 0.632844 0.963117 11.00000 0.03023 0.02829 = 0.01962 -0.00202 0.00571 -0.00575 C19 1 -0.250764 0.717411 0.526011 11.00000 0.02454 0.03205 = 0.03515 0.00420 0.01001 0.00281 AFIX 43 H19 2 -0.277378 0.741730 0.559436 11.00000 -1.20000 AFIX 0 C22 1 0.341784 0.780968 0.463129 11.00000 0.02678 0.02432 = 0.02672 0.00332 0.00638 -0.00043 C6 1 0.052167 0.816912 0.810737 11.00000 0.04015 0.02370 = 0.02287 -0.00341 0.00594 0.00565 AFIX 43 H6 2 0.046393 0.840690 0.861032 11.00000 -1.20000 AFIX 0 C45 1 0.343943 0.639730 0.538993 11.00000 0.02721 0.03491 = 0.03572 0.00710 0.01506 0.00466 C27 1 0.389400 0.804758 0.568824 11.00000 0.02612 0.03290 = 0.02686 0.00516 0.00364 -0.00159 C13 1 -0.152515 0.674452 0.901219 11.00000 0.03080 0.04102 = 0.02962 0.00000 0.01430 -0.00075 AFIX 43 H13 2 -0.221540 0.688754 0.881227 11.00000 -1.20000 AFIX 0 C46 1 0.347157 0.596876 0.549654 11.00000 0.03056 0.03346 = 0.04102 -0.00100 0.01461 0.00698 AFIX 43 H46 2 0.401937 0.580891 0.522501 11.00000 -1.20000 AFIX 0 C17 1 -0.272557 0.665413 0.364710 11.00000 0.02468 0.03952 = 0.02876 0.00186 0.00162 -0.00393 AFIX 43 H17 2 -0.314376 0.653916 0.287997 11.00000 -1.20000 AFIX 0 C29 1 0.252906 0.610534 0.961534 11.00000 0.03147 0.03557 = 0.02827 0.00447 0.00240 -0.00136 AFIX 43 H29 2 0.267558 0.625211 0.891327 11.00000 -1.20000 AFIX 0 C18 1 -0.308551 0.701866 0.410723 11.00000 0.02332 0.03929 = 0.03550 0.00686 0.00236 0.00334 AFIX 43 H18 2 -0.372122 0.716081 0.363872 11.00000 -1.20000 AFIX 0 C47 1 0.267378 0.577938 0.601542 11.00000 0.03021 0.02325 = 0.04174 0.00011 0.00991 0.00311 C11 1 -0.030346 0.626099 1.032133 11.00000 0.03701 0.04017 = 0.02332 0.00422 0.00883 -0.00707 AFIX 43 H11 2 -0.015735 0.607144 1.101101 11.00000 -1.20000 AFIX 0 C37 1 -0.060163 0.578269 0.411257 11.00000 0.03081 0.03400 = 0.03016 -0.00797 0.00401 -0.00437 AFIX 43 H37 2 -0.007091 0.577648 0.489611 11.00000 -1.20000 AFIX 0 C38 1 -0.069677 0.548680 0.309536 11.00000 0.03548 0.03555 = 0.03506 -0.01059 0.01073 -0.01006 C43 1 -0.159658 0.561979 0.217484 11.00000 0.04383 0.03149 = 0.02839 -0.00486 0.01097 -0.01199 C12 1 -0.130972 0.646600 1.001306 11.00000 0.03597 0.05057 = 0.02998 0.00444 0.01667 -0.00449 AFIX 43 H12 2 -0.185284 0.641636 1.048541 11.00000 -1.20000 AFIX 0 C30 1 0.328193 0.582916 1.044627 11.00000 0.03652 0.03538 = 0.03657 0.00463 0.00034 -0.00037 C35 1 0.270692 0.569672 1.133552 11.00000 0.04316 0.03125 = 0.03056 0.00236 -0.00192 -0.00290 C26 1 0.488620 0.826140 0.584146 11.00000 0.03072 0.05161 = 0.03976 0.00099 0.00052 -0.01322 AFIX 43 H26 2 0.518562 0.841985 0.657880 11.00000 -1.20000 AFIX 0 C23 1 0.397392 0.778648 0.364197 11.00000 0.03852 0.03413 = 0.03687 -0.00099 0.01744 -0.00337 AFIX 43 H23 2 0.367350 0.762916 0.290259 11.00000 -1.20000 AFIX 0 C24 1 0.496599 0.799767 0.377142 11.00000 0.03761 0.04499 = 0.05162 0.00546 0.02386 -0.00215 AFIX 43 H24 2 0.534874 0.798418 0.311050 11.00000 -1.20000 AFIX 0 B1 3 0.080398 0.669415 0.658821 11.00000 0.02135 0.02077 = 0.01916 -0.00100 0.00727 0.00096 C42 1 -0.196601 0.542094 0.101910 11.00000 0.06203 0.04799 = 0.03007 -0.00883 0.00550 -0.01454 AFIX 43 H42 2 -0.258840 0.551891 0.040511 11.00000 -1.20000 AFIX 0 C25 1 0.542015 0.823091 0.485295 11.00000 0.02697 0.05425 = 0.05708 0.00696 0.01111 -0.01010 AFIX 43 H25 2 0.610620 0.837117 0.491364 11.00000 -1.20000 AFIX 0 C34 1 0.314303 0.542240 1.230841 11.00000 0.06105 0.04281 = 0.04172 0.01222 0.00009 0.00045 AFIX 43 H34 2 0.273352 0.533814 1.290378 11.00000 -1.20000 AFIX 0 C49 1 0.692493 0.595599 0.653640 11.00000 0.04349 0.03710 = 0.05554 -0.00572 0.01952 -0.00263 AFIX 13 H49 2 0.708037 0.624603 0.628227 11.00000 -1.20000 AFIX 0 C41 1 -0.137300 0.507256 0.081880 11.00000 0.07242 0.05547 = 0.04415 -0.02569 0.01498 -0.01638 AFIX 43 H41 2 -0.158840 0.492754 0.003969 11.00000 -1.20000 AFIX 0 C31 1 0.435271 0.567796 1.052335 11.00000 0.04273 0.06283 = 0.06141 0.01968 0.00771 0.00884 AFIX 43 H31 2 0.476419 0.576217 0.992985 11.00000 -1.20000 AFIX 0 C40 1 -0.047384 0.492855 0.172035 11.00000 0.05931 0.05593 = 0.06869 -0.03339 0.01826 -0.00347 AFIX 43 H40 2 -0.009123 0.468613 0.154873 11.00000 -1.20000 AFIX 0 C39 1 -0.011849 0.513058 0.287035 11.00000 0.04343 0.04826 = 0.05996 -0.02328 0.00779 0.00020 AFIX 43 H39 2 0.049904 0.502981 0.348589 11.00000 -1.20000 AFIX 0 C33 1 0.420477 0.527793 1.236672 11.00000 0.06237 0.04933 = 0.05947 0.01899 -0.01083 0.00605 AFIX 43 H33 2 0.453526 0.509000 1.302075 11.00000 -1.20000 AFIX 0 C32 1 0.480224 0.540091 1.149091 11.00000 0.04677 0.06472 = 0.07983 0.02359 -0.00192 0.01425 AFIX 43 H32 2 0.552836 0.529399 1.155489 11.00000 -1.20000 AFIX 0 PART 2 BR1 4 0.267333 0.520884 0.635881 -21.00000 0.06788 0.02117 = 0.12566 0.00894 0.05545 0.01114 BR2 4 0.449095 0.666949 0.469393 -21.00000 0.04914 0.05500 = 0.06795 0.03014 0.04011 0.01569 HKLF 4 REM 1121_a.res in P2(1)/c REM wR2 = 0.0939, GooF = S = 1.053, Restrained GooF = 1.053 for all data REM R1 = 0.0334 for 7796 Fo > 4sig(Fo) and 0.0361 for all 8499 data REM 578 parameters refined using 0 restraints END WGHT 0.0525 1.6670 REM Highest difference peak 0.696, deepest hole -0.816, 1-sigma level 0.061 Q1 1 0.7799 0.5557 0.7665 11.00000 0.05 0.70 Q2 1 0.6368 0.5441 0.5507 11.00000 0.05 0.44 Q3 1 0.3577 0.5119 0.6619 11.00000 0.05 0.35 Q4 1 0.5236 0.6486 0.5116 11.00000 0.05 0.34 Q5 1 -0.2112 0.6564 0.4037 11.00000 0.05 0.33 Q6 1 -0.0632 0.7313 0.7249 11.00000 0.05 0.32 Q7 1 0.5389 0.6731 0.5345 11.00000 0.05 0.31 Q8 1 -0.1485 0.6537 0.4826 11.00000 0.05 0.30 Q9 1 0.1048 0.6242 0.9793 11.00000 0.05 0.29 Q10 1 -0.1987 0.7058 0.5585 11.00000 0.05 0.28 Q11 1 0.1769 0.5242 0.5779 11.00000 0.05 0.28 Q12 1 0.0153 0.8005 0.8019 11.00000 0.05 0.28 Q13 1 0.3005 0.5966 1.0004 11.00000 0.05 0.28 Q14 1 -0.0819 0.6964 0.7784 11.00000 0.05 0.27 Q15 1 0.3615 0.6763 0.4209 11.00000 0.05 0.26 Q16 1 0.0188 0.7477 0.6931 11.00000 0.05 0.25 Q17 1 0.3444 0.5351 0.6625 11.00000 0.05 0.25 Q18 1 0.3823 0.6888 0.4426 11.00000 0.05 0.25 Q19 1 -0.0216 0.6822 0.8582 11.00000 0.05 0.24 Q20 1 -0.1241 0.5500 0.2615 11.00000 0.05 0.24 ; _shelx_res_checksum 10449 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 2.571 _oxdiff_exptl_absorpt_empirical_full_min 0.605 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Br01 Br 0.4559(3) 0.66979(12) 0.4857(5) 0.0485(5) Uani 0.533(18) 1 d . . P A 1 Br02 Br 0.2669(2) 0.51904(9) 0.6101(4) 0.0485(4) Uani 0.533(18) 1 d . . P A 1 Cl2 Cl 0.62758(5) 0.56822(2) 0.51680(6) 0.05775(15) Uani 1 1 d . . . . . Cl1 Cl 0.60456(5) 0.59917(2) 0.75878(6) 0.06297(17) Uani 1 1 d . . . . . Cl3 Cl 0.81797(5) 0.57263(3) 0.72515(8) 0.0731(2) Uani 1 1 d . . . . . O1 O 0.08676(9) 0.71022(3) 0.60543(9) 0.0213(2) Uani 1 1 d . . . . . O3 O -0.01604(9) 0.64487(3) 0.59862(9) 0.0220(2) Uani 1 1 d . . . . . O2 O 0.10615(9) 0.66709(3) 0.79404(10) 0.0225(2) Uani 1 1 d . . . . . O4 O 0.32286(10) 0.80486(4) 0.65330(10) 0.0292(2) Uani 1 1 d . . . . . O6 O -0.20432(11) 0.59751(4) 0.25490(11) 0.0337(3) Uani 1 1 d . . . . . O5 O 0.16672(11) 0.58662(4) 1.10881(11) 0.0346(3) Uani 1 1 d . . . . . N1 N 0.18346(10) 0.64309(4) 0.62115(11) 0.0214(2) Uani 1 1 d . . . . . C20 C 0.23136(13) 0.78039(5) 0.59970(14) 0.0228(3) Uani 1 1 d . . . . . C15 C -0.11364(12) 0.66292(5) 0.54193(14) 0.0222(3) Uani 1 1 d . . . . . C3 C 0.07275(12) 0.74560(5) 0.66994(13) 0.0213(3) Uani 1 1 d . . . . . C4 C 0.14566(13) 0.77955(5) 0.67223(13) 0.0233(3) Uani 1 1 d . . . . . C9 C 0.02641(13) 0.66059(5) 0.85957(14) 0.0236(3) Uani 1 1 d . . . . . C8 C -0.07475(13) 0.68191(5) 0.82918(14) 0.0254(3) Uani 1 1 d . . . . . C7 C -0.02238(14) 0.78412(5) 0.80320(14) 0.0268(3) Uani 1 1 d . . . . . H7 H -0.080184 0.786012 0.847055 0.032 Uiso 1 1 calc R . . . . C21 C 0.23957(13) 0.76539(5) 0.48629(14) 0.0243(3) Uani 1 1 d . . . . . H21 H 0.187594 0.747859 0.432122 0.029 Uiso 1 1 calc R . . . . C16 C -0.17583(13) 0.64510(5) 0.42877(14) 0.0252(3) Uani 1 1 d . . . . . C36 C -0.14086(13) 0.60704(5) 0.37426(14) 0.0264(3) Uani 1 1 d . . . . . C14 C -0.15434(13) 0.69813(5) 0.59409(14) 0.0245(3) Uani 1 1 d . . . . . C44 C 0.26064(13) 0.66248(5) 0.57425(15) 0.0265(3) Uani 1 1 d . . . . . H44 H 0.258467 0.692006 0.564999 0.032 Uiso 1 1 calc R . . . . C5 C 0.13440(14) 0.81483(5) 0.74510(14) 0.0274(3) Uani 1 1 d . . . . . H5 H 0.184354 0.837570 0.749056 0.033 Uiso 1 1 calc R . . . . C1 C -0.10279(13) 0.71508(5) 0.72594(14) 0.0246(3) Uani 1 1 d . . . . . H1 H -0.165315 0.730806 0.748311 0.030 Uiso 1 1 calc R . . . . C2 C -0.01400(13) 0.74844(5) 0.73240(13) 0.0234(3) Uani 1 1 d . . . . . C48 C 0.18683(13) 0.60159(5) 0.63805(15) 0.0252(3) Uani 1 1 d . . . . . H48 H 0.133588 0.588369 0.675318 0.030 Uiso 1 1 calc R . . . . C28 C 0.15754(14) 0.61168(5) 1.00203(14) 0.0276(3) Uani 1 1 d . . . . . C10 C 0.05065(14) 0.63284(5) 0.96312(14) 0.0261(3) Uani 1 1 d . . . . . C19 C -0.25076(14) 0.71741(6) 0.52601(16) 0.0301(3) Uani 1 1 d . . . . . H19 H -0.277378 0.741730 0.559436 0.036 Uiso 1 1 calc R . . . . C22 C 0.34178(13) 0.78097(5) 0.46313(15) 0.0259(3) Uani 1 1 d . . . . . C6 C 0.05217(15) 0.81691(5) 0.81074(15) 0.0291(3) Uani 1 1 d . . . . . H6 H 0.046393 0.840690 0.861032 0.035 Uiso 1 1 calc R . . . . C45 C 0.34394(14) 0.63973(6) 0.53899(17) 0.0313(3) Uani 1 1 d . . . . . C27 C 0.38940(14) 0.80476(6) 0.56882(15) 0.0290(3) Uani 1 1 d . . . . . C13 C -0.15251(15) 0.67445(6) 0.90122(16) 0.0326(4) Uani 1 1 d . . . . . H13 H -0.221540 0.688754 0.881227 0.039 Uiso 1 1 calc R . . . . C46 C 0.34716(15) 0.59688(6) 0.54965(17) 0.0340(4) Uani 1 1 d . . . . . H46 H 0.401937 0.580891 0.522501 0.041 Uiso 1 1 calc R . . . . C17 C -0.27256(14) 0.66541(6) 0.36471(16) 0.0317(4) Uani 1 1 d . . . . . H17 H -0.314376 0.653916 0.287997 0.038 Uiso 1 1 calc R . . . . C29 C 0.25291(15) 0.61053(6) 0.96153(16) 0.0325(4) Uani 1 1 d . . . . . H29 H 0.267558 0.625211 0.891327 0.039 Uiso 1 1 calc R . . . . C18 C -0.30855(14) 0.70187(6) 0.41072(17) 0.0334(4) Uani 1 1 d . . . . . H18 H -0.372122 0.716081 0.363872 0.040 Uiso 1 1 calc R . . . . C47 C 0.26738(14) 0.57794(5) 0.60154(17) 0.0315(3) Uani 1 1 d . . . . . C11 C -0.03035(15) 0.62610(6) 1.03213(15) 0.0332(4) Uani 1 1 d . . . . . H11 H -0.015735 0.607144 1.101101 0.040 Uiso 1 1 calc R . . . . C37 C -0.06016(15) 0.57827(6) 0.41126(16) 0.0321(4) Uani 1 1 d . . . . . H37 H -0.007091 0.577648 0.489611 0.039 Uiso 1 1 calc R . . . . C38 C -0.06968(15) 0.54868(6) 0.30954(17) 0.0349(4) Uani 1 1 d . . . . . C43 C -0.15966(16) 0.56198(6) 0.21748(16) 0.0341(4) Uani 1 1 d . . . . . C12 C -0.13097(16) 0.64660(7) 1.00131(17) 0.0374(4) Uani 1 1 d . . . . . H12 H -0.185284 0.641636 1.048541 0.045 Uiso 1 1 calc R . . . . C30 C 0.32819(16) 0.58292(6) 1.04463(18) 0.0375(4) Uani 1 1 d . . . . . C35 C 0.27069(17) 0.56967(6) 1.13355(17) 0.0367(4) Uani 1 1 d . . . . . C26 C 0.48862(16) 0.82614(7) 0.58415(19) 0.0419(4) Uani 1 1 d . . . . . H26 H 0.518562 0.841985 0.657880 0.050 Uiso 1 1 calc R . . . . C23 C 0.39739(16) 0.77865(6) 0.36420(18) 0.0351(4) Uani 1 1 d . . . . . H23 H 0.367350 0.762916 0.290259 0.042 Uiso 1 1 calc R . . . . C24 C 0.49660(17) 0.79977(7) 0.3771(2) 0.0425(4) Uani 1 1 d . . . . . H24 H 0.534874 0.798418 0.311050 0.051 Uiso 1 1 calc R . . . . B1 B 0.08040(14) 0.66942(5) 0.65882(15) 0.0200(3) Uani 1 1 d . . . . . C42 C -0.1966(2) 0.54209(7) 0.10191(19) 0.0475(5) Uani 1 1 d . . . . . H42 H -0.258840 0.551891 0.040511 0.057 Uiso 1 1 calc R . . . . C25 C 0.54202(16) 0.82309(7) 0.4853(2) 0.0459(5) Uani 1 1 d . . . . . H25 H 0.610620 0.837117 0.491364 0.055 Uiso 1 1 calc R . . . . C34 C 0.3143(2) 0.54224(7) 1.2308(2) 0.0504(5) Uani 1 1 d . . . . . H34 H 0.273352 0.533814 1.290378 0.061 Uiso 1 1 calc R . . . . C49 C 0.69249(18) 0.59560(7) 0.6536(2) 0.0441(4) Uani 1 1 d . . . . . H49 H 0.708037 0.624603 0.628227 0.053 Uiso 1 1 calc R . . . . C41 C -0.1373(2) 0.50726(8) 0.0819(2) 0.0571(6) Uani 1 1 d . . . . . H41 H -0.158840 0.492754 0.003969 0.069 Uiso 1 1 calc R . . . . C31 C 0.4353(2) 0.56780(9) 1.0523(3) 0.0564(6) Uani 1 1 d . . . . . H31 H 0.476419 0.576217 0.992985 0.068 Uiso 1 1 calc R . . . . C40 C -0.0474(2) 0.49286(9) 0.1720(3) 0.0607(7) Uani 1 1 d . . . . . H40 H -0.009123 0.468613 0.154873 0.073 Uiso 1 1 calc R . . . . C39 C -0.01185(19) 0.51306(8) 0.2870(2) 0.0512(5) Uani 1 1 d . . . . . H39 H 0.049904 0.502981 0.348589 0.061 Uiso 1 1 calc R . . . . C33 C 0.4205(2) 0.52779(8) 1.2367(3) 0.0611(7) Uani 1 1 d . . . . . H33 H 0.453526 0.509000 1.302075 0.073 Uiso 1 1 calc R . . . . C32 C 0.4802(2) 0.54009(9) 1.1491(3) 0.0665(7) Uani 1 1 d . . . . . H32 H 0.552836 0.529399 1.155489 0.080 Uiso 1 1 calc R . . . . Br1 Br 0.2673(3) 0.52088(12) 0.6359(9) 0.0662(9) Uani 0.467(18) 1 d . . P A 2 Br2 Br 0.4491(4) 0.66695(15) 0.4694(6) 0.0530(7) Uani 0.467(18) 1 d . . P A 2 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 Br01 0.0379(5) 0.0387(7) 0.0803(13) 0.0095(8) 0.0374(6) -0.0002(5) Br02 0.0465(7) 0.0222(4) 0.0819(10) -0.0034(4) 0.0254(8) 0.0039(4) Cl2 0.0519(3) 0.0646(4) 0.0606(3) -0.0220(3) 0.0209(2) 0.0022(3) Cl1 0.0516(3) 0.0905(5) 0.0521(3) -0.0135(3) 0.0229(2) 0.0019(3) Cl3 0.0441(3) 0.0835(5) 0.0884(5) -0.0105(4) 0.0087(3) 0.0104(3) O1 0.0266(5) 0.0198(5) 0.0192(4) -0.0014(4) 0.0089(4) 0.0007(4) O3 0.0217(5) 0.0227(5) 0.0215(5) -0.0007(4) 0.0048(4) -0.0004(4) O2 0.0234(5) 0.0267(5) 0.0187(5) -0.0005(4) 0.0074(4) -0.0015(4) O4 0.0305(6) 0.0344(6) 0.0211(5) -0.0009(4) 0.0026(4) -0.0087(5) O6 0.0415(7) 0.0344(7) 0.0222(5) -0.0010(5) 0.0013(5) -0.0061(5) O5 0.0433(7) 0.0342(7) 0.0255(5) 0.0073(5) 0.0063(5) -0.0015(5) N1 0.0223(6) 0.0237(6) 0.0185(5) -0.0007(4) 0.0052(5) 0.0006(5) C20 0.0247(7) 0.0206(7) 0.0214(6) 0.0028(5) 0.0016(5) -0.0022(6) C15 0.0210(7) 0.0251(7) 0.0217(7) 0.0037(5) 0.0071(5) -0.0023(6) C3 0.0254(7) 0.0207(7) 0.0178(6) 0.0002(5) 0.0050(5) 0.0029(5) C4 0.0293(7) 0.0222(7) 0.0178(6) 0.0021(5) 0.0041(5) 0.0025(6) C9 0.0263(7) 0.0265(7) 0.0195(6) -0.0039(6) 0.0084(5) -0.0052(6) C8 0.0290(8) 0.0270(8) 0.0221(7) -0.0025(6) 0.0100(6) -0.0020(6) C7 0.0323(8) 0.0272(8) 0.0222(7) -0.0009(6) 0.0089(6) 0.0073(6) C21 0.0264(7) 0.0238(7) 0.0230(7) -0.0001(5) 0.0061(6) -0.0035(6) C16 0.0231(7) 0.0288(8) 0.0241(7) 0.0029(6) 0.0065(6) -0.0049(6) C36 0.0272(7) 0.0314(8) 0.0202(7) -0.0015(6) 0.0048(6) -0.0098(6) C14 0.0223(7) 0.0280(8) 0.0250(7) 0.0023(6) 0.0093(6) -0.0007(6) C44 0.0270(8) 0.0258(8) 0.0285(7) 0.0036(6) 0.0102(6) 0.0010(6) C5 0.0363(8) 0.0224(7) 0.0222(7) 0.0004(6) 0.0040(6) 0.0000(6) C1 0.0246(7) 0.0271(8) 0.0248(7) -0.0008(6) 0.0111(6) 0.0037(6) C2 0.0276(7) 0.0241(7) 0.0195(6) 0.0004(5) 0.0071(5) 0.0037(6) C48 0.0252(7) 0.0237(7) 0.0272(7) 0.0012(6) 0.0070(6) 0.0007(6) C28 0.0369(9) 0.0254(8) 0.0183(6) 0.0008(6) 0.0017(6) -0.0053(6) C10 0.0302(8) 0.0283(8) 0.0196(6) -0.0020(6) 0.0057(6) -0.0058(6) C19 0.0245(7) 0.0320(9) 0.0351(8) 0.0042(7) 0.0100(6) 0.0028(6) C22 0.0268(7) 0.0243(7) 0.0267(7) 0.0033(6) 0.0064(6) -0.0004(6) C6 0.0401(9) 0.0237(8) 0.0229(7) -0.0034(6) 0.0059(6) 0.0057(7) C45 0.0272(8) 0.0349(9) 0.0357(8) 0.0071(7) 0.0151(7) 0.0047(7) C27 0.0261(8) 0.0329(8) 0.0269(7) 0.0052(6) 0.0036(6) -0.0016(6) C13 0.0308(8) 0.0410(10) 0.0296(8) 0.0000(7) 0.0143(7) -0.0007(7) C46 0.0306(8) 0.0335(9) 0.0410(9) -0.0010(7) 0.0146(7) 0.0070(7) C17 0.0247(8) 0.0395(10) 0.0288(8) 0.0019(7) 0.0016(6) -0.0039(7) C29 0.0315(8) 0.0356(9) 0.0283(8) 0.0045(7) 0.0024(6) -0.0014(7) C18 0.0233(7) 0.0393(10) 0.0355(8) 0.0069(7) 0.0024(6) 0.0033(7) C47 0.0302(8) 0.0233(8) 0.0417(9) 0.0001(7) 0.0099(7) 0.0031(6) C11 0.0370(9) 0.0402(10) 0.0233(7) 0.0042(7) 0.0088(6) -0.0071(7) C37 0.0308(8) 0.0340(9) 0.0302(8) -0.0080(7) 0.0040(6) -0.0044(7) C38 0.0355(9) 0.0355(9) 0.0351(9) -0.0106(7) 0.0107(7) -0.0101(7) C43 0.0438(10) 0.0315(9) 0.0284(8) -0.0049(7) 0.0110(7) -0.0120(7) C12 0.0360(9) 0.0506(11) 0.0300(8) 0.0044(7) 0.0167(7) -0.0045(8) C30 0.0365(9) 0.0354(9) 0.0366(9) 0.0046(7) 0.0003(7) -0.0004(8) C35 0.0432(10) 0.0313(9) 0.0306(8) 0.0024(7) -0.0019(7) -0.0029(7) C26 0.0307(9) 0.0516(12) 0.0398(10) 0.0010(8) 0.0005(7) -0.0132(8) C23 0.0385(9) 0.0341(9) 0.0369(9) -0.0010(7) 0.0174(7) -0.0034(7) C24 0.0376(10) 0.0450(11) 0.0516(11) 0.0055(9) 0.0239(9) -0.0022(8) B1 0.0214(7) 0.0208(8) 0.0192(7) -0.0010(6) 0.0073(6) 0.0010(6) C42 0.0620(13) 0.0480(12) 0.0301(9) -0.0088(8) 0.0055(9) -0.0145(10) C25 0.0270(9) 0.0542(13) 0.0571(12) 0.0070(10) 0.0111(8) -0.0101(8) C34 0.0611(14) 0.0428(11) 0.0417(10) 0.0122(9) 0.0001(10) 0.0005(10) C49 0.0435(11) 0.0371(10) 0.0555(12) -0.0057(9) 0.0195(9) -0.0026(8) C41 0.0724(16) 0.0555(14) 0.0442(11) -0.0257(10) 0.0150(11) -0.0164(12) C31 0.0427(11) 0.0628(15) 0.0614(14) 0.0197(11) 0.0077(10) 0.0088(10) C40 0.0593(14) 0.0559(14) 0.0687(15) -0.0334(12) 0.0183(12) -0.0035(11) C39 0.0434(11) 0.0483(12) 0.0600(13) -0.0233(10) 0.0078(10) 0.0002(9) C33 0.0624(15) 0.0493(13) 0.0595(14) 0.0190(11) -0.0108(12) 0.0060(11) C32 0.0468(13) 0.0647(16) 0.0798(18) 0.0236(14) -0.0019(12) 0.0143(12) Br1 0.0679(10) 0.0212(6) 0.126(2) 0.0089(10) 0.0555(12) 0.0111(5) Br2 0.0491(10) 0.0550(15) 0.0680(10) 0.0301(11) 0.0401(7) 0.0157(9) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -6 13 4 0.0223 -5 -4 -4 0.0079 5 -14 -4 0.0448 7 0 3 0.0514 -1 -6 7 0.0211 0 -20 -2 0.0119 0 -1 -7 0.0334 1 21 -1 0.0499 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 C3 O1 B1 121.30(11) . . ? C15 O3 B1 122.01(12) . . ? C9 O2 B1 121.97(12) . . ? C27 O4 C20 105.98(12) . . ? C43 O6 C36 106.30(14) . . ? C35 O5 C28 106.54(14) . . ? C44 N1 C48 120.69(14) . . ? C44 N1 B1 121.22(13) . . ? C48 N1 B1 118.09(12) . . ? O4 C20 C4 113.99(13) . . ? C21 C20 O4 110.98(14) . . ? C21 C20 C4 134.80(14) . . ? O3 C15 C16 118.39(14) . . ? O3 C15 C14 121.55(13) . . ? C14 C15 C16 120.06(14) . . ? O1 C3 C4 119.45(13) . . ? O1 C3 C2 120.44(14) . . ? C2 C3 C4 120.11(14) . . ? C3 C4 C20 123.14(14) . . ? C5 C4 C20 117.99(14) . . ? C5 C4 C3 118.85(14) . . ? O2 C9 C8 121.37(14) . . ? O2 C9 C10 117.92(14) . . ? C8 C9 C10 120.66(14) . . ? C9 C8 C1 123.57(14) . . ? C13 C8 C9 118.73(15) . . ? C13 C8 C1 117.60(15) . . ? C6 C7 C2 121.22(15) . . ? C20 C21 C22 107.02(14) . . ? C15 C16 C36 122.43(14) . . ? C17 C16 C15 118.62(15) . . ? C17 C16 C36 118.92(15) . . ? O6 C36 C16 113.92(14) . . ? C37 C36 O6 110.49(15) . . ? C37 C36 C16 135.59(15) . . ? C15 C14 C1 123.51(14) . . ? C19 C14 C15 118.82(15) . . ? C19 C14 C1 117.56(14) . . ? N1 C44 C45 120.37(15) . . ? C6 C5 C4 120.98(16) . . ? C8 C1 C14 114.80(13) . . ? C2 C1 C8 114.46(13) . . ? C2 C1 C14 115.64(12) . . ? C3 C2 C1 123.98(14) . . ? C7 C2 C3 118.98(15) . . ? C7 C2 C1 117.02(14) . . ? N1 C48 C47 120.33(15) . . ? O5 C28 C10 113.74(14) . . ? C29 C28 O5 110.26(15) . . ? C29 C28 C10 135.99(15) . . ? C9 C10 C28 122.34(14) . . ? C11 C10 C9 118.57(15) . . ? C11 C10 C28 119.08(15) . . ? C18 C19 C14 121.49(16) . . ? C27 C22 C21 105.49(14) . . ? C27 C22 C23 118.20(16) . . ? C23 C22 C21 136.28(16) . . ? C5 C6 C7 119.71(15) . . ? C44 C45 Br01 117.65(19) . . ? C44 C45 Br2 120.0(2) . . ? C46 C45 Br01 121.69(18) . . ? C46 C45 C44 120.56(16) . . ? C46 C45 Br2 119.3(2) . . ? O4 C27 C22 110.53(14) . . ? O4 C27 C26 125.01(17) . . ? C26 C27 C22 124.44(17) . . ? C12 C13 C8 121.29(17) . . ? C45 C46 C47 117.43(16) . . ? C18 C17 C16 121.42(16) . . ? C28 C29 C30 107.39(16) . . ? C17 C18 C19 119.23(16) . . ? C48 C47 Br02 121.47(17) . . ? C48 C47 C46 120.52(16) . . ? C48 C47 Br1 116.4(2) . . ? C46 C47 Br02 117.88(17) . . ? C46 C47 Br1 122.9(2) . . ? C12 C11 C10 120.95(16) . . ? C36 C37 C38 107.14(15) . . ? C43 C38 C37 105.33(17) . . ? C43 C38 C39 118.93(18) . . ? C39 C38 C37 135.73(19) . . ? O6 C43 C38 110.72(15) . . ? O6 C43 C42 125.39(19) . . ? C38 C43 C42 123.9(2) . . ? C11 C12 C13 119.78(16) . . ? C35 C30 C29 105.19(17) . . ? C35 C30 C31 118.91(19) . . ? C31 C30 C29 135.9(2) . . ? O5 C35 C30 110.60(15) . . ? O5 C35 C34 125.9(2) . . ? C34 C35 C30 123.5(2) . . ? C27 C26 C25 116.11(19) . . ? C24 C23 C22 118.48(18) . . ? C23 C24 C25 121.53(18) . . ? O1 B1 O3 115.08(12) . . ? O1 B1 N1 104.12(11) . . ? O3 B1 N1 102.33(11) . . ? O2 B1 O1 116.23(13) . . ? O2 B1 O3 113.58(12) . . ? O2 B1 N1 103.06(11) . . ? C41 C42 C43 115.9(2) . . ? C26 C25 C24 121.24(18) . . ? C33 C34 C35 116.5(2) . . ? Cl2 C49 Cl1 110.75(12) . . ? Cl3 C49 Cl2 110.95(12) . . ? Cl3 C49 Cl1 111.18(13) . . ? C42 C41 C40 121.9(2) . . ? C32 C31 C30 118.4(2) . . ? C41 C40 C39 121.4(2) . . ? C40 C39 C38 118.0(2) . . ? C34 C33 C32 121.7(2) . . ? C31 C32 C33 121.1(2) . . ? 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 Br01 C45 1.886(4) . ? Br02 C47 1.887(3) . ? Cl2 C49 1.756(2) . ? Cl1 C49 1.757(2) . ? Cl3 C49 1.734(2) . ? O1 C3 1.3647(18) . ? O1 B1 1.4390(19) . ? O3 C15 1.3539(19) . ? O3 B1 1.4538(19) . ? O2 C9 1.3616(19) . ? O2 B1 1.4354(19) . ? O4 C20 1.3908(19) . ? O4 C27 1.370(2) . ? O6 C36 1.3895(19) . ? O6 C43 1.367(2) . ? O5 C28 1.3958(19) . ? O5 C35 1.366(2) . ? N1 C44 1.336(2) . ? N1 C48 1.340(2) . ? N1 B1 1.658(2) . ? C20 C4 1.463(2) . ? C20 C21 1.351(2) . ? C15 C16 1.414(2) . ? C15 C14 1.407(2) . ? C3 C4 1.410(2) . ? C3 C2 1.401(2) . ? C4 C5 1.406(2) . ? C9 C8 1.398(2) . ? C9 C10 1.412(2) . ? C8 C1 1.527(2) . ? C8 C13 1.396(2) . ? C7 C2 1.395(2) . ? C7 C6 1.388(3) . ? C21 C22 1.437(2) . ? C16 C36 1.464(2) . ? C16 C17 1.400(2) . ? C36 C37 1.351(3) . ? C14 C1 1.530(2) . ? C14 C19 1.396(2) . ? C44 C45 1.388(2) . ? C5 C6 1.375(2) . ? C1 C2 1.523(2) . ? C48 C47 1.382(2) . ? C28 C10 1.461(2) . ? C28 C29 1.354(3) . ? C10 C11 1.402(2) . ? C19 C18 1.387(3) . ? C22 C27 1.393(2) . ? C22 C23 1.409(2) . ? C45 C46 1.376(3) . ? C45 Br2 1.867(4) . ? C27 C26 1.383(3) . ? C13 C12 1.386(3) . ? C46 C47 1.386(3) . ? C17 C18 1.384(3) . ? C29 C30 1.443(3) . ? C47 Br1 1.864(4) . ? C11 C12 1.380(3) . ? C37 C38 1.442(2) . ? C38 C43 1.384(3) . ? C38 C39 1.398(3) . ? C43 C42 1.391(3) . ? C30 C35 1.394(3) . ? C30 C31 1.396(3) . ? C35 C34 1.386(3) . ? C26 C25 1.391(3) . ? C23 C24 1.381(3) . ? C24 C25 1.399(3) . ? C42 C41 1.380(4) . ? C34 C33 1.382(4) . ? C41 C40 1.383(4) . ? C31 C32 1.392(3) . ? C40 C39 1.388(3) . ? C33 C32 1.392(4) . ? loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -5.5999 13.0901 3.5001 0.1760 0.7326 0.6575 -5.1396 -4.3635 -4.0524 0.1630 0.6814 -0.7136 4.6704 -13.7877 -4.1924 -0.1466 -0.6094 -0.7792 6.6083 -0.3150 2.5821 -0.2091 -0.8728 0.4410 -0.6209 -5.5785 6.7318 -0.7923 -0.0624 0.6070 -0.4147 -20.0296 -1.7089 -0.6159 -0.0488 -0.7863 0.4605 -1.0181 -6.9559 0.5603 0.0441 -0.8271 0.6002 20.6356 -0.7062 0.8470 0.0670 0.5274