#------------------------------------------------------------------------------ #$Date: 2024-08-05 21:11:07 +0300 (Mon, 05 Aug 2024) $ #$Revision: 293772 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/19/1571948.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_1571948 loop_ _publ_author_name 'Arnold, Robert E.' 'Saska, Jan' 'Mesquita-Ribeiro, Raquel' 'Dajas-Bailador, Federico' 'Taylor, Laurence' 'Lewis, William' 'Argent, Stephen' 'Shao, Huiling' 'Houk, Kendall N.' 'Denton, Ross M.' _publ_section_title ; Total synthesis, biological evaluation and biosynthetic re-evaluation of Illicium-derived neolignans. ; _journal_issue 30 _journal_name_full 'Chemical science' _journal_page_first 11783 _journal_page_last 11793 _journal_paper_doi 10.1039/d4sc03232b _journal_volume 15 _journal_year 2024 _chemical_formula_moiety 'C19 H19 Br O3' _chemical_formula_sum 'C19 H19 Br O3' _chemical_formula_weight 375.25 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _atom_sites_solution_secondary difmap _audit_creation_date 2018-02-12 _audit_creation_method ; Olex2 1.2 (compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381) ; _audit_update_record ; 2024-01-23 deposited with the CCDC. 2024-06-13 downloaded from the CCDC. ; _cell_angle_alpha 66.361(5) _cell_angle_beta 82.591(4) _cell_angle_gamma 75.387(4) _cell_formula_units_Z 4 _cell_length_a 11.1367(5) _cell_length_b 12.0896(6) _cell_length_c 14.1443(7) _cell_measurement_reflns_used 9461 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 74.0210 _cell_measurement_theta_min 3.4000 _cell_volume 1687.31(16) _computing_cell_refinement 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _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 'olex2.solve (Bourhis et al., 2015)' _diffrn_ambient_environment 'N2 gas' _diffrn_ambient_temperature 120(2) _diffrn_crystal_treatment 'flash frozen in gaseous N2' _diffrn_detector 'CCD area detector' _diffrn_detector_area_resol_mean 4.2207 _diffrn_detector_type 'Agilent Diffraction Titan S2 detector' _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.969 _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 -27.00 67.00 1.00 1.00 -- 42.81 -57.00 90.00 94 2 \w 38.00 65.00 1.00 3.00 -- 103.32-125.00 150.00 27 3 \w 38.00 64.00 1.00 3.00 -- 103.32-125.00 120.00 26 4 \w 96.00 121.00 1.00 3.00 -- 103.32-125.00 120.00 25 5 \w 61.00 124.00 1.00 3.00 -- 103.32 -77.00 0.00 63 6 \w 92.00 120.00 1.00 3.00 -- 103.32-125.00 -90.00 28 7 \w 70.00 108.00 1.00 3.00 -- 103.32 -94.00 -60.00 38 8 \w 47.00 87.00 1.00 3.00 -- 103.32 -94.00 -90.00 40 9 \w 39.00 98.00 1.00 3.00 -- 103.32 -45.00-120.00 59 10 \w 34.00 77.00 1.00 3.00 -- 103.32 -30.00 -60.00 43 11 \w 34.00 83.00 1.00 3.00 -- 103.32 -30.00-180.00 49 12 \w 20.00 112.00 1.00 1.00 -- 42.81 57.00-120.00 92 13 \w 76.00 168.00 1.00 3.00 -- 103.32 77.00-180.00 92 14 \w 78.00 124.00 1.00 3.00 -- 103.32 125.00 -90.00 46 15 \w 91.00 171.00 1.00 3.00 -- 103.32 30.00 90.00 80 16 \w 135.00 160.00 1.00 3.00 -- 103.32 125.00 120.00 25 17 \w 84.00 117.00 1.00 3.00 -- 103.32 125.00 120.00 33 18 \w 38.00 74.00 1.00 3.00 -- 103.32 -30.00 90.00 36 19 \w 32.00 133.00 1.00 3.00 -- 103.32 -77.00 120.00 101 20 \w -17.00 70.00 1.00 1.00 -- 42.81 -77.00 -30.00 87 ; _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'SuperNova, Titan S2' _diffrn_measurement_method '\w scans' _diffrn_measurement_specimen_support 'MiTeGen micromount' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0749829000 _diffrn_orient_matrix_UB_12 -0.1019315000 _diffrn_orient_matrix_UB_13 0.0438369000 _diffrn_orient_matrix_UB_21 -0.0419095000 _diffrn_orient_matrix_UB_22 0.0361342000 _diffrn_orient_matrix_UB_23 0.0938547000 _diffrn_orient_matrix_UB_31 -0.1143579000 _diffrn_orient_matrix_UB_32 0.0929788000 _diffrn_orient_matrix_UB_33 -0.0584743000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0214 _diffrn_reflns_av_unetI/netI 0.0249 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.969 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 12597 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.969 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 73.677 _diffrn_reflns_theta_min 3.413 _diffrn_source 'microfocus sealed tube' _diffrn_source_type 'Agilent Diffraction microfocus tube' _exptl_absorpt_coefficient_mu 3.421 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.437 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.477 _exptl_crystal_description block _exptl_crystal_F_000 768 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: diethyl ether, petroleum ether' _exptl_crystal_size_max 0.345 _exptl_crystal_size_mid 0.254 _exptl_crystal_size_min 0.105 _refine_diff_density_max 0.599 _refine_diff_density_min -0.516 _refine_diff_density_rms 0.082 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 445 _refine_ls_number_reflns 6604 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.075 _refine_ls_R_factor_all 0.0383 _refine_ls_R_factor_gt 0.0357 _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^)+(0.0406P)^2^+3.5368P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1009 _refine_ls_wR_factor_ref 0.1022 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6212 _reflns_number_total 6604 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc03232b2.cif _cod_data_source_block 42b _cod_depositor_comments 'Adding full bibliography for 1571943--1571950.cif.' _cod_original_cell_volume 1687.30(16) _cod_database_code 1571948 _nottingham_internal_coll_name REARDF _nottingham_internal_coll_number 17454 _nottingham_internal_coll_client REA/RD _nottingham_internal_coll_type custom _nottingham_internal_coll_frame_method '\w scans' _nottingham_internal_coll_frame_time '1.00, 3.00' _nottingham_internal_coll_frame_width 1.00 _nottingham_internal_coll_user pczwl _nottingham_internal_coll_date 18/01/2018 _nottingham_internal_coll_location NOTTS _nottingham_internal_coll_instrument 'GVA, PL13110002' _nottingham_internal_process_date 23/01/2018 _nottingham_internal_process_user pczwl _nottingham_internal_solution_date 23/1/2018 _nottingham_internal_solution_user pczwl _nottingham_internal_refinement_date 12/2/2018 _nottingham_internal_refinement_user pczwl _nottingham_internal_validation_date 12/2/2018 _nottingham_internal_validation_user pczwl _nottingham_internal_archive_date 12/2/2018 _shelx_shelxl_version_number 2018/1 _chemical_oxdiff_formula 'C19 H19 Br O3' _chemical_oxdiff_usercomment 'REARDF #17454 GVA-1359 IN FOMBLIN FILM ON A MICROMOUNT FOR REA/RD' _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_max 0.715 _shelx_estimated_absorpt_t_min 0.385 _reflns_odcompleteness_completeness 99.88 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 67.13 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Others Sof(C49)=Sof(H49C)=Sof(H49D)=Sof(C50)=Sof(H50)=Sof(C51)=Sof(H51C)=Sof(H51D)=1- FVAR(1) Sof(C49A)=Sof(H49A)=Sof(H49B)=Sof(C50A)=Sof(H50A)=Sof(C51A)=Sof(H51A)= Sof(H51B)=FVAR(1) 3.a Ternary CH refined with riding coordinates: C6(H6), C36(H36) 3.b Secondary CH2 refined with riding coordinates: C5(H5A,H5B), C17(H17A,H17B), C19(H19A,H19B), C35(H35A,H35B), C47(H47A,H47B), C49(H49C,H49D), C49A(H49A,H49B) 3.c Aromatic/amide H refined with riding coordinates: C7(H7), C8(H8), C10(H10), C11(H11), C14(H14), C15(H15), C20(H20), C37(H37), C38(H38), C40(H40), C41(H41), C44(H44), C45(H45), C50(H50), C50A(H50A) 3.d X=CH2 refined with riding coordinates: C21(H21A,H21B), C51(H51C,H51D), C51A(H51A,H51B) 3.e Idealised Me refined as rotating group: C18(H18A,H18B,H18C), C48(H48A,H48B,H48C) ; _shelx_res_file ; TITL reardf.res created by SHELXL-2018/1 at 09:51:22 on 12-Feb-2018 CELL 1.54184 11.136737 12.089557 14.144294 66.3612 82.5907 75.3866 ZERR 4 0.000534 0.0006 0.000711 0.0048 0.0041 0.0043 LATT 1 SFAC C H O Br UNIT 76 76 12 4 L.S. 12 0 0 PLAN 40 SIZE 0.105 0.254 0.345 TEMP -153(2) bond $h conf fmap -2 53 acta OMIT 1 8 4 OMIT 0 9 3 OMIT -7 6 2 OMIT 7 11 5 OMIT 1 -4 9 OMIT 4 5 12 OMIT 5 10 4 OMIT 6 11 5 OMIT -6 6 2 OMIT 3 5 12 OMIT 3 -3 10 OMIT -2 8 4 OMIT -8 6 3 OMIT 1 9 3 OMIT -9 6 2 OMIT -1 9 3 OMIT -2 9 4 OMIT 10 12 6 OMIT -1 8 4 OMIT -1 9 4 OMIT 0 -4 10 OMIT 7 -1 10 REM REM REM WGHT 0.040600 3.536800 FVAR 5.28865 0.48968 O1 3 0.487522 0.866616 0.259414 11.00000 0.02632 0.06985 = 0.03511 0.01800 -0.01222 -0.00736 C2 1 0.599257 0.885859 0.274580 11.00000 0.02158 0.05156 = 0.02719 0.00721 -0.00355 -0.00083 C3 1 0.694688 0.791781 0.332186 11.00000 0.02418 0.03551 = 0.01735 0.00059 -0.00309 0.00045 C4 1 0.679652 0.658016 0.385666 11.00000 0.02439 0.03688 = 0.01711 -0.00375 -0.00525 -0.00600 C5 1 0.571568 0.644264 0.333847 11.00000 0.02929 0.06417 = 0.02693 -0.01606 -0.00831 -0.00919 AFIX 23 H5A 2 0.601194 0.641391 0.265628 11.00000 -1.20000 H5B 2 0.547646 0.564988 0.377045 11.00000 -1.20000 AFIX 0 C6 1 0.458632 0.749332 0.319701 11.00000 0.02890 0.06432 = 0.02844 -0.00644 -0.01210 -0.01179 AFIX 13 H6 2 0.395278 0.737113 0.282876 11.00000 -1.20000 AFIX 0 C7 1 0.615948 1.006315 0.226763 11.00000 0.02970 0.04706 = 0.03470 0.01719 -0.00086 0.00694 AFIX 43 H7 2 0.551756 1.069635 0.186316 11.00000 -1.20000 AFIX 0 C8 1 0.724099 1.035457 0.237039 11.00000 0.03555 0.03199 = 0.03236 0.00872 0.00860 0.00240 AFIX 43 H8 2 0.732983 1.118757 0.204610 11.00000 -1.20000 AFIX 0 C9 1 0.821157 0.943681 0.294760 11.00000 0.03174 0.03081 = 0.02090 -0.00381 0.00322 0.00013 C10 1 0.804466 0.823453 0.339981 11.00000 0.02524 0.03045 = 0.01895 -0.00454 -0.00158 0.00081 AFIX 43 H10 2 0.870271 0.759806 0.377880 11.00000 -1.20000 AFIX 0 C11 1 0.794891 0.572123 0.367358 11.00000 0.02723 0.03772 = 0.01821 -0.00832 -0.00153 -0.01016 AFIX 43 H11 2 0.823008 0.585657 0.298106 11.00000 -1.20000 AFIX 0 C12 1 0.859590 0.478303 0.442725 11.00000 0.02417 0.02761 = 0.02231 -0.01048 -0.00369 -0.00788 C13 1 0.824828 0.448239 0.553180 11.00000 0.03328 0.02203 = 0.01877 -0.00642 -0.00607 -0.01046 C14 1 0.716962 0.534737 0.573980 11.00000 0.02939 0.02939 = 0.01822 -0.00681 -0.00101 -0.01299 AFIX 43 H14 2 0.692527 0.522504 0.643699 11.00000 -1.20000 AFIX 0 C15 1 0.651849 0.629772 0.499073 11.00000 0.02133 0.03333 = 0.02069 -0.00765 -0.00206 -0.01003 AFIX 43 H15 2 0.583782 0.682995 0.518206 11.00000 -1.20000 AFIX 0 O16 3 0.409240 0.743538 0.416381 11.00000 0.02205 0.04239 = 0.03209 -0.00551 -0.00716 -0.00894 C17 1 0.287711 0.822359 0.414617 11.00000 0.02555 0.02945 = 0.04551 -0.00737 -0.00836 -0.01012 AFIX 23 H17A 2 0.228107 0.800009 0.382861 11.00000 -1.20000 H17B 2 0.290667 0.910097 0.374055 11.00000 -1.20000 AFIX 0 C18 1 0.248940 0.803234 0.524533 11.00000 0.04053 0.03632 = 0.05097 -0.01220 0.00121 -0.01175 AFIX 137 H18A 2 0.253681 0.714906 0.565119 11.00000 -1.50000 H18B 2 0.163468 0.849576 0.527307 11.00000 -1.50000 H18C 2 0.304318 0.832713 0.553050 11.00000 -1.50000 AFIX 0 C19 1 0.940487 0.975843 0.304487 11.00000 0.04254 0.03156 = 0.02921 -0.00983 0.00005 -0.00835 AFIX 23 H19A 2 0.919191 1.051754 0.319696 11.00000 -1.20000 H19B 2 0.985034 0.908157 0.364324 11.00000 -1.20000 AFIX 0 C20 1 1.026881 0.996459 0.211817 11.00000 0.03705 0.04262 = 0.03815 -0.01090 -0.00034 -0.01460 AFIX 43 H20 2 1.097618 1.026350 0.212883 11.00000 -1.20000 AFIX 0 C21 1 1.013958 0.977161 0.129801 11.00000 0.04335 0.06706 = 0.04657 -0.02618 0.01658 -0.02685 AFIX 93 H21A 2 0.944644 0.947281 0.125271 11.00000 -1.20000 H21B 2 1.073851 0.992971 0.074537 11.00000 -1.20000 AFIX 0 BR22 4 1.003254 0.373133 0.413025 11.00000 0.02884 0.03467 = 0.02857 -0.01682 -0.00676 -0.00375 O23 3 0.881892 0.357960 0.621690 11.00000 0.05256 0.02277 = 0.02279 -0.00494 -0.01000 -0.00195 O31 3 0.502462 0.602893 0.129368 11.00000 0.01756 0.02402 = 0.03040 -0.00600 -0.00663 -0.00729 C32 1 0.447170 0.503891 0.165108 11.00000 0.01678 0.02191 = 0.01690 -0.00838 0.00043 -0.00513 C33 1 0.327214 0.510749 0.141086 11.00000 0.01622 0.02163 = 0.01433 -0.00733 -0.00135 -0.00428 C34 1 0.246019 0.634058 0.072702 11.00000 0.01539 0.02014 = 0.01718 -0.00686 -0.00296 -0.00399 C35 1 0.309351 0.741335 0.056632 11.00000 0.01722 0.02068 = 0.02316 -0.00801 -0.00195 -0.00374 AFIX 23 H35A 2 0.273816 0.815016 -0.003839 11.00000 -1.20000 H35B 2 0.291774 0.763492 0.118015 11.00000 -1.20000 AFIX 0 C36 1 0.448367 0.706189 0.039659 11.00000 0.01776 0.01989 = 0.02626 -0.00644 -0.00141 -0.00541 AFIX 13 H36 2 0.467761 0.684958 -0.022886 11.00000 -1.20000 AFIX 0 C37 1 0.517342 0.392676 0.231516 11.00000 0.01447 0.02921 = 0.02022 -0.00995 -0.00124 -0.00116 AFIX 43 H37 2 0.598435 0.388744 0.248686 11.00000 -1.20000 AFIX 0 C38 1 0.468419 0.288948 0.271888 11.00000 0.02364 0.02444 = 0.02520 0.00051 -0.00175 0.00059 AFIX 43 H38 2 0.516048 0.213577 0.317671 11.00000 -1.20000 AFIX 0 C39 1 0.349449 0.292217 0.246787 11.00000 0.02635 0.02444 = 0.03554 -0.00204 0.00123 -0.00850 C40 1 0.280755 0.403184 0.181624 11.00000 0.01927 0.02513 = 0.02653 -0.00772 -0.00112 -0.00827 AFIX 43 H40 2 0.200111 0.406469 0.163962 11.00000 -1.20000 AFIX 0 C41 1 0.233376 0.627229 -0.029461 11.00000 0.01676 0.02473 = 0.01518 -0.00612 0.00014 -0.00479 AFIX 43 H41 2 0.306643 0.613450 -0.069524 11.00000 -1.20000 AFIX 0 C42 1 0.124778 0.639529 -0.066326 11.00000 0.02304 0.02658 = 0.01537 -0.00733 -0.00221 -0.00668 C43 1 0.004520 0.658877 -0.009812 11.00000 0.01838 0.02661 = 0.02554 -0.00961 -0.00367 -0.00550 C44 1 0.013971 0.668956 0.088760 11.00000 0.01807 0.02862 = 0.02238 -0.00932 0.00335 -0.00538 AFIX 43 H44 2 -0.060162 0.684629 0.127301 11.00000 -1.20000 AFIX 0 C45 1 0.122098 0.657062 0.126504 11.00000 0.02206 0.02313 = 0.01803 -0.00874 0.00080 -0.00570 AFIX 43 H45 2 0.120980 0.663490 0.191400 11.00000 -1.20000 AFIX 0 O46 3 0.498522 0.804112 0.027743 11.00000 0.01798 0.02207 = 0.04507 -0.01305 0.00283 -0.00765 C47 1 0.630013 0.785409 0.002266 11.00000 0.01960 0.02645 = 0.04819 -0.01252 0.00523 -0.00891 AFIX 23 H47A 2 0.647065 0.766345 -0.060657 11.00000 -1.20000 H47B 2 0.676441 0.715192 0.059593 11.00000 -1.20000 AFIX 0 C48 1 0.669891 0.902576 -0.015721 11.00000 0.02603 0.03187 = 0.07108 -0.01949 0.00599 -0.01404 AFIX 137 H48A 2 0.623171 0.971517 -0.072360 11.00000 -1.50000 H48B 2 0.758860 0.892421 -0.033750 11.00000 -1.50000 H48C 2 0.653594 0.920041 0.047242 11.00000 -1.50000 AFIX 0 PART 2 C49 1 0.296887 0.179662 0.310345 -21.00000 0.02695 0.01997 = 0.03000 -0.01162 -0.00565 -0.00427 AFIX 23 H49C 2 0.208226 0.199147 0.294218 -21.00000 -1.20000 H49D 2 0.340147 0.111390 0.288146 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 C49A 1 0.298358 0.172062 0.274380 21.00000 0.03494 0.02137 = 0.03322 -0.01115 0.00972 -0.01137 AFIX 23 H49A 2 0.231801 0.188762 0.227170 21.00000 -1.20000 H49B 2 0.365818 0.104090 0.267807 21.00000 -1.20000 AFIX 0 PART 0 PART 2 C50 1 0.306122 0.134160 0.424817 -21.00000 0.03134 0.02130 = 0.02545 -0.00954 0.00348 -0.00998 AFIX 43 H50 2 0.245226 0.175260 0.460393 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 C50A 1 0.248861 0.137369 0.382667 21.00000 0.03919 0.01832 = 0.02499 -0.00476 0.00469 -0.00809 AFIX 43 H50A 2 0.301172 0.129249 0.434148 21.00000 -1.20000 AFIX 0 PART 0 PART 2 C51 1 0.392036 0.041636 0.480059 -21.00000 0.04350 0.02411 = 0.02488 -0.00664 -0.00035 -0.00548 AFIX 93 H51C 2 0.454557 -0.001797 0.447309 -21.00000 -1.20000 H51D 2 0.391584 0.018223 0.552721 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 C51A 1 0.136159 0.117232 0.411163 21.00000 0.04413 0.02538 = 0.03595 -0.01403 0.01260 -0.00959 AFIX 93 H51A 2 0.081893 0.124704 0.361281 21.00000 -1.20000 H51B 2 0.109306 0.095268 0.481554 21.00000 -1.20000 AFIX 0 PART 0 BR52 4 0.112517 0.631559 -0.195612 11.00000 0.02738 0.04180 = 0.02018 -0.01446 -0.00523 -0.00864 O53 3 -0.093774 0.665613 -0.042865 11.00000 0.01740 0.05658 = 0.03830 -0.02306 -0.00552 -0.00819 HKLF 4 REM REM R1 = 0.0357 for 6212 Fo > 4sig(Fo) and 0.0383 for all 6604 data REM 445 parameters refined using 0 restraints END WGHT 0.0406 3.5368 REM Highest difference 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54362.4 2031.62 12 -3 3 8 10902.6 845.977 12 -3 3 7 21514.6 1092.27 12 -3 3 6 56973.1 1653.55 12 -3 3 5 682.532 175.282 12 -3 3 5 654.124 182.494 1 -3 3 4 20857.5 913.068 1 -3 3 3 33972.0 1063.58 1 -3 3 2 126733. 1964.97 1 -3 3 1 262525. 2868.41 1 -3 3 0 8118.24 553.369 1 -3 3 -1 4232.25 433.424 1 -3 3 -2 40301.4 1385.33 1 -3 3 -3 64693.1 1884.51 1 3 -3 4 18917.7 1091.78 12 3 -3 5 14077.4 1022.89 12 -3 3 -6 55681.9 1482.59 4 -3 3 -6 56581.7 1457.91 19 3 -3 6 54221.1 2116.51 12 -3 3 -7 33076.1 1202.02 4 -3 3 -7 29105.9 1107.13 19 3 -3 7 30407.7 1683.58 12 3 -3 8 9706.09 1225.55 12 -3 3 -8 12146.7 1520.66 19 -3 3 -9 24198.4 1124.14 19 -3 3 -10 24184.7 1231.39 19 -3 3 -11 32770.4 932.619 8 -3 3 -11 34408.4 1255.24 19 -3 3 -12 32758.6 832.299 8 -3 3 -12 30845.2 1069.46 19 -3 3 -13 4081.00 246.574 8 -3 3 -13 3905.59 322.432 19 3 -2 -16 81.2799 62.4567 11 3 -2 -15 27065.8 827.816 11 3 -2 -14 1674.04 235.498 15 3 -2 -14 1828.95 252.399 11 3 -2 -13 2000.07 297.780 15 3 -2 -13 2309.78 302.798 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20 3 -1 3 55893.6 1264.48 12 -3 1 -4 155397. 1916.05 20 3 -1 4 155693. 2325.52 12 3 -1 5 34603.4 1230.90 12 -3 1 -5 35684.3 921.273 20 3 -1 6 3660.29 439.052 12 3 -1 7 84814.4 2338.51 12 -3 1 -8 166960. 2760.34 4 -3 1 -8 177904. 2520.62 19 3 -1 8 173979. 3685.57 12 -3 1 -9 59149.1 1412.75 11 -3 1 -9 57464.7 1543.23 19 3 -1 9 56904.8 2263.69 12 -3 1 -10 62.2809 92.3777 11 -3 1 -10 266.603 137.137 19 -3 1 -11 214.230 156.619 19 -3 1 -11 295.472 160.196 11 -3 1 -12 32431.1 1214.71 19 -3 1 -12 30260.3 952.878 11 -3 1 -13 25870.1 763.006 11 -3 1 -13 25830.6 1019.36 19 -3 1 -14 5898.71 431.439 19 -3 1 -14 5895.09 362.536 8 -3 1 -15 412.910 91.9716 8 3 0 -15 1042.13 168.474 11 3 0 -14 14257.6 702.373 11 3 0 -13 6372.80 511.170 11 3 0 -12 16346.9 860.504 11 3 0 -12 15726.7 715.235 15 3 0 -11 50183.7 1379.03 15 -3 0 10 31149.1 1800.78 12 3 0 -10 29363.3 1007.82 19 3 0 -9 55740.2 1348.05 19 -3 0 9 56247.1 1245.12 13 -3 0 8 27072.8 1466.82 12 3 0 -8 26868.2 892.075 19 -3 0 7 5966.19 627.634 12 -3 0 6 112169. 2455.29 12 -3 0 5 34339.2 1217.59 12 -3 0 4 5822.95 444.003 12 -3 0 3 81398.8 1456.86 12 -3 0 3 81447.2 1518.26 20 -3 0 2 34225.6 815.992 12 -3 0 2 35934.7 963.446 20 -3 0 1 165771. 1456.05 12 -3 0 1 171617. 2027.35 20 -3 0 0 35579.9 628.032 1 -3 0 0 35645.0 934.250 20 -3 0 -1 1526.78 190.563 20 -3 0 -1 2219.55 162.038 1 -3 0 -2 292931. 2643.85 20 3 0 2 289402. 1787.37 12 -3 0 -2 292651. 1736.05 1 -3 0 -3 22868.2 762.539 20 3 0 3 22956.0 622.247 12 3 0 4 111566. 1628.65 12 -3 0 -4 115560. 1768.33 20 3 0 5 16397.1 723.579 12 -3 0 -5 16362.7 681.344 20 -3 0 -6 35744.5 1018.40 20 3 0 6 35144.1 1214.57 12 3 0 7 102710. 2336.34 12 -3 0 -8 3820.72 354.464 19 -3 0 -8 3997.49 399.114 4 3 0 8 3635.33 484.726 12 -3 0 -9 92603.6 1839.93 19 3 0 9 96165.4 2728.09 12 -3 0 -10 3735.13 395.420 19 3 0 10 3882.49 591.440 12 -3 0 -10 3870.21 382.605 11 -3 0 -11 29073.9 1060.70 11 -3 0 -11 28176.0 1114.26 19 -3 0 -12 114122. 2055.25 11 -3 0 -12 111520. 2232.17 19 -3 0 -13 4222.79 422.250 19 -3 0 -13 4392.96 369.560 11 -3 0 -14 586.515 177.402 19 -3 0 -14 597.023 117.894 11 -3 0 -15 1298.99 169.025 8 3 1 -15 3891.97 261.003 11 3 1 -14 10539.5 571.221 11 3 1 -13 268.224 140.499 11 3 1 -12 23955.2 1058.83 11 3 1 -11 7267.10 531.924 19 -3 -1 10 25342.7 885.940 13 3 1 -10 24123.0 929.224 19 -3 -1 9 2630.71 293.327 13 -3 -1 9 2767.48 523.804 12 3 1 -9 2909.56 313.148 19 -3 -1 8 12816.6 614.604 13 -3 -1 8 13773.5 1107.88 12 3 1 -8 12001.5 609.580 19 -3 -1 7 47670.5 1894.12 12 -3 -1 6 36927.1 1501.40 12 -3 -1 5 75988.7 1912.19 12 -3 -1 4 102859. 1965.38 12 -3 -1 3 37572.6 949.299 20 -3 -1 3 38917.4 1060.88 12 -3 -1 2 322351. 2775.22 20 -3 -1 2 313791. 2572.99 12 -3 -1 1 203503. 2136.44 20 -3 -1 1 209561. 1722.73 12 -3 -1 0 141763. 1060.19 12 -3 -1 0 155929. 2148.73 20 -3 -1 -1 1439.69 218.601 20 -3 -1 -2 133170. 1898.56 20 3 1 3 133291. 1089.55 12 -3 -1 -3 135668. 1990.24 20 3 1 4 41694.8 828.759 12 -3 -1 -4 41245.0 1141.47 20 -3 -1 -5 15865.3 730.945 20 3 1 5 14550.6 602.653 12 -3 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58745.4 1820.71 12 -3 -2 4 35024.3 1258.68 12 -3 -2 3 56750.1 1037.82 20 -3 -2 3 55451.2 1397.40 12 -3 -2 2 361430. 3076.05 12 -3 -2 2 357846. 2846.72 20 -3 -2 1 3459.27 288.389 20 -3 -2 1 3525.65 260.052 12 -3 -2 0 86601.3 1493.07 20 -3 -2 0 84823.6 1007.86 12 -3 -2 -1 52652.8 1383.30 20 -3 -2 -1 47309.3 547.026 12 -3 -2 -2 189730. 2529.31 20 -3 -2 -3 839187. 5392.30 20 -3 -2 -4 27804.0 1016.61 20 3 2 4 28867.6 603.747 12 3 2 5 99075.1 1404.76 12 -3 -2 -5 98404.2 2001.19 20 -3 -2 -6 32523.9 1187.18 20 3 2 6 33665.3 967.654 12 -3 -2 -7 15240.8 846.597 20 3 2 7 14717.3 745.367 12 3 2 8 167096. 2845.92 12 -3 -2 -8 174250. 2934.52 20 3 2 9 4000.39 494.866 12 -3 -2 -9 3928.75 338.677 19 -3 -2 -9 3853.47 347.086 11 -3 -2 -10 4504.86 387.374 11 3 2 10 5025.66 604.944 12 -3 -2 -10 5218.00 420.334 19 -3 -2 -11 90513.8 1819.38 19 -3 -2 -11 89135.0 1818.49 11 -3 -2 -12 332.568 125.637 11 -3 -2 -12 263.457 99.5748 19 -3 -2 -13 16691.2 814.382 19 -3 -2 -13 17933.7 827.225 11 -3 -2 -14 5578.30 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43839.3 2101.31 12 3 4 -6 40251.1 1156.31 19 -3 -4 5 292.080 114.596 13 -3 -4 5 376.118 155.853 12 -3 -4 4 21467.6 1240.87 12 -3 -4 3 202064. 3486.10 12 -3 -4 2 11789.8 767.027 12 -3 -4 1 431842. 3525.72 20 -3 -4 1 440495. 4209.58 12 3 4 0 155.102 97.5912 1 -3 -4 0 181.317 101.976 20 -3 -4 -1 51619.7 1463.04 20 3 4 1 52560.2 1193.03 1 3 4 2 156970. 2016.52 1 3 4 3 779.498 150.436 1 3 4 4 91790.4 1392.04 1 3 4 5 1471.69 178.204 1 3 4 6 6443.78 393.383 1 3 4 7 181711. 2343.22 1 3 4 8 30269.7 1097.46 12 -3 -4 -8 30023.0 1469.11 20 3 4 8 29828.0 1057.12 1 -3 -4 -9 106877. 1736.85 11 -3 -4 -9 107051. 2835.15 20 3 4 9 110419. 2327.79 12 -3 -4 -10-33.6372 113.720 11 -3 -4 -10 17.9106 79.9354 19 3 4 10 51.1156 66.8706 12 -3 -4 -10 211.803 169.750 20 -3 -4 -11 10316.9 717.080 11 -3 -4 -11 9706.78 579.710 15 -3 -4 -12 101054. 1940.41 11 -3 -4 -12 97894.6 1800.05 15 -3 -4 -13 63.3326 94.1582 11 -3 -4 -14 17288.9 784.546 11 -3 -4 -15 11373.0 590.920 11 -3 -4 -16 5285.50 356.149 11 -3 -4 -16 5190.88 355.821 8 -3 -4 -17 18125.5 516.395 9 3 5 -12 17651.4 582.236 11 3 5 -11 4753.31 344.827 19 -3 -5 10 6671.97 425.432 13 3 5 -10 5250.01 448.614 19 3 5 -9 4604.46 681.516 19 -3 -5 9 7267.28 549.484 13 -3 -5 8 33947.2 1178.03 13 3 5 -8 34046.0 1277.80 19 3 5 -7 51074.3 1498.91 19 -3 -5 7 50351.5 1445.00 13 -3 -5 6 25999.7 1697.62 12 -3 -5 6 24964.1 991.740 13 3 5 -6 25389.5 994.049 19 3 5 -5 5382.72 470.890 18 -3 -5 5 5464.34 738.164 12 3 5 -4 1906.57 265.461 18 -3 -5 4 2222.81 455.167 12 -3 -5 3 6309.37 682.771 12 -3 -5 2 42197.5 1631.82 12 -3 -5 1 278244. 2903.36 20 -3 -5 1 267432. 3723.49 12 3 5 0 3896.06 449.051 1 -3 -5 0 3970.70 405.021 20 3 5 1 24596.8 1036.65 1 -3 -5 -1 25056.3 1089.30 20 3 5 2 70810.8 1664.48 1 3 5 3 80467.1 1709.29 1 3 5 4 28102.0 953.176 1 3 5 5 1553.76 216.909 1 3 5 6 52020.2 1212.65 1 3 5 7 53399.7 1292.78 1 3 5 8 22967.5 913.951 1 -3 -5 -9 33761.2 966.829 11 -3 -5 -9 34631.8 1064.68 15 -3 -5 -10 3107.23 318.900 11 -3 -5 -10 3295.96 561.278 20 -3 -5 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39784.9 1850.91 1 -5 3 7 229712. 2430.96 13 -5 3 7 230816. 4146.51 1 -5 3 6 2575.04 250.228 13 -5 3 6 1991.77 368.026 1 -5 3 5 14274.3 902.460 1 -5 3 4 6562.86 564.615 1 -5 3 3 3731.23 405.248 1 -5 3 2 225712. 3068.84 1 -5 3 1 11254.2 722.369 1 -5 3 0 38801.3 1389.41 1 -5 3 -1 109173. 2366.57 20 -5 3 -1 109082. 2338.77 1 -5 3 -2 8080.34 632.169 20 -5 3 -2 7372.33 610.727 1 -5 3 -3 69402.9 1984.00 1 -5 3 -4 9387.08 579.784 8 -5 3 -4 9627.27 551.396 19 -5 3 -5 2398.71 283.334 19 -5 3 -5 2314.90 282.381 8 -5 3 -6 88823.5 1673.35 8 -5 3 -6 89484.8 1926.05 4 -5 3 -6 90230.9 1862.63 19 -5 3 -7-91.5684 144.331 8 -5 3 -7 223.653 154.388 4 -5 3 -7-39.6396 131.514 19 -5 3 -8 17576.4 766.955 8 -5 3 -8 19327.5 979.227 4 -5 3 -8 18634.3 985.128 19 -5 3 -9 22609.0 822.328 8 -5 3 -9 21745.9 986.689 19 -5 3 -10 17782.9 684.027 8 -5 3 -10 18001.1 839.038 19 -5 3 -11 34150.1 851.219 8 -5 3 -11 33116.9 1031.86 19 -5 3 -12 7009.20 325.959 8 -5 3 -12 7783.53 426.723 19 5 -2 -14 195.383 76.4751 11 5 -2 -14 421.813 127.788 15 5 -2 -13 10552.0 507.329 11 5 -2 -13 11193.6 653.684 15 5 -2 -12 25144.9 852.750 11 5 -2 -12 25078.3 1079.75 15 -5 2 11 20870.6 784.512 13 5 -2 -11 19139.6 826.512 11 -5 2 10 6619.05 438.330 13 -5 2 10 7374.01 824.461 12 5 -2 -10 6421.39 456.947 11 -5 2 9 1305.33 202.637 13 -5 2 9 1149.25 279.264 12 -5 2 8 76101.7 1451.29 13 -5 2 8 79227.6 2416.80 12 -5 2 7 128767. 1827.25 13 -5 2 7 135714. 2934.48 12 -5 2 6 47361.3 1062.67 13 -5 2 6 49132.8 1632.86 12 -5 2 5 26233.3 1221.15 1 -5 2 4 1038.49 234.686 1 -5 2 3 154368. 2477.76 1 -5 2 2 56159.8 1381.29 1 -5 2 2 59649.1 1779.39 20 -5 2 1 252.571 107.348 1 -5 2 1 226.061 135.050 20 -5 2 0 5829.96 466.955 1 -5 2 0 5698.38 530.039 20 -5 2 -1 27291.6 1118.21 20 -5 2 -1 26889.9 1026.96 1 -5 2 -2 115089. 2119.38 1 -5 2 -2 119708. 2294.10 20 -5 2 -3 29831.5 1142.17 20 -5 2 -4 29362.8 1125.07 20 -5 2 -5 11212.9 592.951 8 -5 2 -5 11311.0 694.152 20 -5 2 -6 31293.3 1009.49 8 -5 2 -6 31648.4 1140.71 4 -5 2 -6 31070.2 1010.36 19 -5 2 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4958.05 20 -5 1 2 52826.5 1284.74 1 -5 1 2 56122.3 1636.40 20 -5 1 1 76454.9 1826.57 20 -5 1 1 71745.7 1379.06 1 -5 1 0 75.6232 76.0274 20 -5 1 0 234.367 89.0195 1 -5 1 -1 26962.7 1066.25 20 -5 1 -1 25972.0 854.477 1 -5 1 -2 259863. 2496.60 1 -5 1 -2 263067. 3337.07 20 -5 1 -3 2479.82 318.138 20 -5 1 -4 17450.3 853.696 20 -5 1 -5 5948.68 510.468 20 -5 1 -6 19425.0 918.286 20 -5 1 -6 18520.6 767.113 8 -5 1 -6 19126.8 877.209 4 -5 1 -6 20045.0 715.420 16 -5 1 -7 80400.8 1675.64 8 -5 1 -7 85807.4 1956.71 4 -5 1 -7 85279.1 1642.93 19 -5 1 -8 6315.77 493.336 8 -5 1 -8 5638.80 544.031 4 -5 1 -8 6018.44 475.141 19 -5 1 -9 1271.77 292.536 8 -5 1 -9 1292.20 285.909 4 -5 1 -9 1296.56 236.592 19 -5 1 -10 11992.1 696.305 8 -5 1 -10 12057.4 708.163 19 -5 1 -11 5636.95 446.019 8 -5 1 -11 4603.43 437.517 19 -5 1 -12 87737.5 1572.95 8 -5 1 -12 80843.3 1689.92 19 -5 1 -13 1061.74 161.867 8 -5 1 -13 1037.56 174.647 19 -5 1 -14 439.073 87.9339 8 5 0 -14 140.180 78.2342 11 5 0 -13 782.480 151.480 11 5 0 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276.477 104.675 16 -12 -4 -2 46231.7 943.207 10 -12 -4 -2 46480.8 1128.60 16 -12 -4 -3 3971.88 330.498 7 -12 -4 -3 4313.46 272.354 10 -12 -4 -3 4508.01 363.375 16 -12 -4 -4 7250.88 421.167 7 -12 -4 -4 7574.23 479.434 16 -12 -4 -5 293.175 103.807 7 -12 -4 -5 284.776 102.962 16 -12 -4 -6 4002.61 306.388 7 -12 -4 -6 3903.56 310.099 16 -12 -4 -7 50817.0 1055.83 7 -12 -4 -7 49371.4 1035.67 16 -12 -4 -8 93.7637 72.8878 7 -12 -4 -9 1296.63 153.607 7 -12 -4 -10 201.370 66.2129 7 -12 -5 4 2183.56 169.864 13 -12 -5 3 1756.89 181.947 10 -12 -5 2 24676.7 698.698 10 -12 -5 1 4109.22 299.157 10 -12 -5 1 4131.08 287.593 16 -12 -5 0 1859.43 208.913 10 -12 -5 -1 6488.65 410.430 10 -12 -5 -2 4376.18 305.820 10 -12 -5 -3 30151.8 778.644 10 -12 -5 -3 29251.0 953.468 16 -12 -5 -4 12787.3 470.248 10 -12 -5 -4 19091.7 732.576 16 -12 -5 -5 2169.91 212.854 7 -12 -5 -5 2165.58 241.672 16 -12 -5 -6 9547.65 443.500 7 -12 -5 -6 9761.71 516.011 16 -12 -5 -7 4623.42 305.537 7 -12 -5 -7 4880.56 336.549 16 -12 -5 -8 27256.7 703.316 7 -12 -5 -8 28630.1 734.657 16 -12 -5 -9 1168.07 137.522 7 -12 -6 3 7436.83 321.525 10 -12 -6 2 31620.1 730.857 10 -12 -6 1 679.068 125.056 10 -12 -6 0 415.994 119.604 10 -12 -6 -1 2411.40 245.501 10 -12 -6 -2 13304.3 535.961 10 -12 -6 -3 38968.6 923.336 10 -12 -6 -4 2961.52 235.679 10 -12 -6 -5 1529.57 160.557 10 -12 -6 -5 1479.22 210.051 16 -12 -6 -6 16991.1 662.938 16 -12 -6 -7 2477.62 248.274 16 -12 -6 -8 29670.4 752.533 16 -12 -6 -9 1400.22 144.261 7 -12 -6 -9 1382.95 144.654 16 -12 -7 2 5884.23 276.145 10 -12 -7 1 7593.66 347.451 10 -12 -7 0 350.663 86.4591 10 -12 -7 -1 148.504 60.1707 10 -12 -7 -2 39301.4 894.740 10 -12 -7 -3 4216.56 294.600 10 -12 -7 -4 5165.14 314.307 10 -12 -7 -5 265.296 79.1791 10 -12 -7 -6 1413.31 153.428 10 -12 -7 -6 1322.02 183.242 16 -12 -7 -7 23476.3 712.866 16 -12 -7 -8 15084.2 529.464 16 -12 -7 -9 1665.29 156.059 16 -12 -7 -9 1767.12 169.242 9 -12 -8 1 11388.2 364.514 10 -12 -8 0 311.036 75.6648 10 -12 -8 -1 3590.02 245.679 10 -12 -8 -2 30423.9 731.086 10 -12 -8 -3 2730.00 224.685 10 -12 -8 -4 13202.5 488.293 10 -12 -8 -5 1075.52 135.393 10 -12 -8 -6 9653.57 385.221 10 -12 -8 -7 38731.5 704.007 10 -12 -8 -7 37648.5 871.237 16 -12 -8 -8 2332.22 201.598 16 -12 -9 0 162.256 48.1739 10 -12 -9 -1 2142.20 161.362 10 -12 -9 -2 3758.37 228.814 10 -12 -9 -3 5775.32 292.434 10 -12 -9 -4 1894.43 168.956 10 -12 -9 -5 4353.45 254.209 10 -12 -9 -6 18268.5 500.645 10 -12 -9 -7 5383.72 255.278 10 -12 -9 -7 5056.06 297.222 16 -12 -9 -8 16626.4 482.749 16 -12 -10 -3 12469.3 360.738 10 -12 -10 -4 1835.12 144.283 10 -12 -10 -5 3453.59 199.834 10 -12 -10 -6 7545.48 287.030 10 -12 -10 -7 6567.17 253.363 10 -13 1 2 3815.19 202.781 5 -13 1 1 2940.88 187.025 5 -13 1 0 55.0784 53.9668 5 -13 1 -1 50.9325 39.2655 5 -13 0 2 8362.31 324.048 5 -13 0 1 3687.53 225.381 5 -13 0 0 177.481 57.5792 5 -13 0 -1 3336.71 205.922 5 -13 0 -2 15578.8 427.806 5 -13 0 -3 1656.08 129.284 5 -13 -1 2 17492.8 481.571 5 -13 -1 1 1387.23 144.511 5 -13 -1 0 1263.37 141.659 5 -13 -1 -1 2193.70 180.076 5 -13 -1 -2 1322.66 138.704 5 -13 -1 -3 18283.4 473.235 5 -13 -1 -4 3585.56 191.578 5 -13 -2 2 13970.5 433.182 5 -13 -2 1 409.535 84.3307 5 -13 -2 0 1510.11 158.077 5 -13 -2 -1 4403.99 269.223 5 -13 -2 -2 6755.58 325.383 5 -13 -2 -3 11320.9 397.066 5 -13 -2 -4 193.996 59.3943 5 -13 -2 -5 451.620 100.990 7 -13 -2 -6 7357.98 331.259 7 -13 -3 2 38.4793 57.5694 5 -13 -3 1 85.2851 63.3135 5 -13 -3 0 27.9508 40.7449 16 -13 -3 -1 619.625 106.237 16 -13 -3 -2 23416.4 666.385 16 -13 -3 -3 2890.64 237.050 16 -13 -3 -4 5958.13 333.185 16 -13 -3 -5 884.525 102.360 5 -13 -3 -5 693.270 111.896 7 -13 -3 -6 722.703 113.067 7 -13 -4 0 87.1148 38.5880 10 -13 -4 0 109.200 63.9802 16 -13 -4 -1 5227.27 312.045 16 -13 -4 -2 17313.1 593.024 16 -13 -4 -3 5844.91 352.927 16 -13 -4 -4 4443.81 299.115 16 -13 -4 -5 103.343 53.6261 16 -13 -4 -6 26783.5 612.794 7 -13 -4 -6 27953.6 676.232 16 -13 -5 1 10522.9 370.895 10 -13 -5 0 266.840 68.3590 10 -13 -5 0 212.879 55.2919 16 -13 -5 -1 11846.8 420.146 10 -13 -5 -1 9552.67 418.177 16 -13 -5 -2 365.595 82.6427 10 -13 -5 -2 479.357 109.390 16 -13 -5 -3 29195.1 770.352 16 -13 -5 -4 2429.58 239.474 16 -13 -5 -5 6116.24 347.476 16 -13 -5 -6 30753.5 743.198 16 -13 -5 -7 4077.33 241.721 16 -13 -6 1 1715.18 143.425 10 -13 -6 0 874.259 110.512 10 -13 -6 -1 4675.11 263.474 10 -13 -6 -1 4147.78 254.132 16 -13 -6 -2 4120.85 242.641 10 -13 -6 -2 2863.15 225.360 16 -13 -6 -3 13995.6 429.044 10 -13 -6 -3 11295.0 464.596 16 -13 -6 -4 850.972 134.848 16 -13 -6 -5 2577.46 240.705 16 -13 -6 -6 9232.31 396.186 16 -13 -6 -7 7435.49 326.909 16 -13 -7 0 91.2184 44.1827 10 -13 -7 -1 144.993 49.9056 10 -13 -7 -1 186.318 70.0804 16 -13 -7 -2 7179.80 305.677 10 -13 -7 -2 6895.48 325.194 16 -13 -7 -3 5301.55 255.611 10 -13 -7 -3 4821.83 283.903 16 -13 -7 -4 1526.51 134.644 10 -13 -7 -4 1622.46 171.972 16 -13 -7 -5 83.1769 39.7249 16 -13 -7 -6 2540.21 200.899 16 -13 -7 -7 28698.4 616.575 16 -13 -8 -2 6835.13 263.741 10 -13 -8 -3 3013.17 180.325 10 -13 -8 -3 2997.52 206.046 16 -13 -8 -4 1676.28 130.672 10 -13 -8 -4 1710.43 159.873 16 -13 -8 -5 253.580 73.9510 16 -13 -8 -6 5428.55 271.271 16 0 0 0 0.00 0.00 0 TITL REARDF in P-1 REM P-1 (#2 in standard setting) CELL 1.54184 11.136737 12.089557 14.144294 66.3612 82.5907 75.3866 ZERR 4.00 0.000534 0.000600 0.000711 0.0048 0.0041 0.0043 LATT 1 SFAC C H O Br UNIT 76.00 76.00 12.00 4.00 TREF HKLF 4 END ; _shelx_hkl_checksum 6747 _olex2_date_sample_data_collection 2018-01-19 _olex2_date_sample_submission 2018-01-16 _olex2_exptl_crystal_mounting_method "'in fomblin film on a micromount" _olex2_submission_original_sample_id RA-203-006 _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 1.325 _oxdiff_exptl_absorpt_empirical_full_min 0.715 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -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 O1 O 0.4875(2) 0.8666(3) 0.2594(2) 0.0558(8) Uani 1 1 d . . . . . C2 C 0.5993(3) 0.8859(4) 0.2746(3) 0.0419(9) Uani 1 1 d . . . . . C3 C 0.6947(3) 0.7918(3) 0.3322(2) 0.0303(7) Uani 1 1 d . . . . . C4 C 0.6797(3) 0.6580(3) 0.3857(2) 0.0280(6) Uani 1 1 d . . . . . C5 C 0.5716(3) 0.6443(4) 0.3338(3) 0.0401(8) Uani 1 1 d . . . . . H5A H 0.601194 0.641391 0.265628 0.048 Uiso 1 1 calc R . . . . H5B H 0.547646 0.564988 0.377045 0.048 Uiso 1 1 calc R . . . . C6 C 0.4586(3) 0.7493(4) 0.3197(3) 0.0429(9) Uani 1 1 d . . . . . H6 H 0.395278 0.737113 0.282876 0.051 Uiso 1 1 calc R . . . . C7 C 0.6159(3) 1.0063(4) 0.2268(3) 0.0509(11) Uani 1 1 d . . . . . H7 H 0.551756 1.069635 0.186316 0.061 Uiso 1 1 calc R . . . . C8 C 0.7241(3) 1.0355(3) 0.2370(3) 0.0430(9) Uani 1 1 d . . . . . H8 H 0.732983 1.118757 0.204610 0.052 Uiso 1 1 calc R . . . . C9 C 0.8212(3) 0.9437(3) 0.2948(2) 0.0316(7) Uani 1 1 d . . . . . C10 C 0.8045(3) 0.8235(3) 0.3400(2) 0.0278(6) Uani 1 1 d . . . . . H10 H 0.870271 0.759806 0.377880 0.033 Uiso 1 1 calc R . . . . C11 C 0.7949(3) 0.5721(3) 0.3674(2) 0.0278(6) Uani 1 1 d . . . . . H11 H 0.823008 0.585657 0.298106 0.033 Uiso 1 1 calc R . . . . C12 C 0.8596(3) 0.4783(3) 0.4427(2) 0.0237(6) Uani 1 1 d . . . . . C13 C 0.8248(3) 0.4482(3) 0.5532(2) 0.0238(6) Uani 1 1 d . . . . . C14 C 0.7170(3) 0.5347(3) 0.5740(2) 0.0251(6) Uani 1 1 d . . . . . H14 H 0.692527 0.522504 0.643699 0.030 Uiso 1 1 calc R . . . . C15 C 0.6518(3) 0.6298(3) 0.4991(2) 0.0251(6) Uani 1 1 d . . . . . H15 H 0.583782 0.682995 0.518206 0.030 Uiso 1 1 calc R . . . . O16 O 0.4092(2) 0.7435(2) 0.41638(18) 0.0341(5) Uani 1 1 d . . . . . C17 C 0.2877(3) 0.8224(3) 0.4146(3) 0.0343(7) Uani 1 1 d . . . . . H17A H 0.228107 0.800009 0.382861 0.041 Uiso 1 1 calc R . . . . H17B H 0.290667 0.910097 0.374055 0.041 Uiso 1 1 calc R . . . . C18 C 0.2489(4) 0.8032(4) 0.5245(3) 0.0437(8) Uani 1 1 d . . . . . H18A H 0.253681 0.714906 0.565119 0.066 Uiso 1 1 calc GR . . . . H18B H 0.163468 0.849576 0.527307 0.066 Uiso 1 1 calc GR . . . . H18C H 0.304318 0.832713 0.553050 0.066 Uiso 1 1 calc GR . . . . C19 C 0.9405(3) 0.9758(3) 0.3045(3) 0.0351(7) Uani 1 1 d . . . . . H19A H 0.919191 1.051754 0.319696 0.042 Uiso 1 1 calc R . . . . H19B H 0.985034 0.908157 0.364324 0.042 Uiso 1 1 calc R . . . . C20 C 1.0269(3) 0.9965(3) 0.2118(3) 0.0397(8) Uani 1 1 d . . . . . H20 H 1.097618 1.026350 0.212883 0.048 Uiso 1 1 calc R . . . . C21 C 1.0140(4) 0.9772(4) 0.1298(3) 0.0498(10) Uani 1 1 d . . . . . H21A H 0.944644 0.947281 0.125271 0.060 Uiso 1 1 calc R . . . . H21B H 1.073851 0.992971 0.074537 0.060 Uiso 1 1 calc R . . . . Br22 Br 1.00325(3) 0.37313(3) 0.41303(2) 0.02923(10) Uani 1 1 d . . . . . O23 O 0.8819(2) 0.3580(2) 0.62169(17) 0.0343(5) Uani 1 1 d . . . . . O31 O 0.50246(17) 0.60289(18) 0.12937(16) 0.0244(4) Uani 1 1 d . . . . . C32 C 0.4472(2) 0.5039(2) 0.1651(2) 0.0182(5) Uani 1 1 d . . . . . C33 C 0.3272(2) 0.5107(2) 0.1411(2) 0.0171(5) Uani 1 1 d . . . . . C34 C 0.2460(2) 0.6341(2) 0.0727(2) 0.0174(5) Uani 1 1 d . . . . . C35 C 0.3094(2) 0.7413(2) 0.0566(2) 0.0204(5) Uani 1 1 d . . . . . H35A H 0.273816 0.815016 -0.003839 0.025 Uiso 1 1 calc R . . . . H35B H 0.291774 0.763492 0.118015 0.025 Uiso 1 1 calc R . . . . C36 C 0.4484(2) 0.7062(3) 0.0397(2) 0.0218(5) Uani 1 1 d . . . . . H36 H 0.467761 0.684958 -0.022886 0.026 Uiso 1 1 calc R . . . . C37 C 0.5173(2) 0.3927(3) 0.2315(2) 0.0218(5) Uani 1 1 d . . . . . H37 H 0.598435 0.388744 0.248686 0.026 Uiso 1 1 calc R . . . . C38 C 0.4684(3) 0.2889(3) 0.2719(2) 0.0288(6) Uani 1 1 d . . . . . H38 H 0.516048 0.213577 0.317671 0.035 Uiso 1 1 calc R . . . . C39 C 0.3494(3) 0.2922(3) 0.2468(3) 0.0315(7) Uani 1 1 d . . . . . C40 C 0.2808(3) 0.4032(3) 0.1816(2) 0.0237(6) Uani 1 1 d . . . . . H40 H 0.200111 0.406469 0.163962 0.028 Uiso 1 1 calc R . . . . C41 C 0.2334(2) 0.6272(3) -0.0295(2) 0.0194(5) Uani 1 1 d . . . . . H41 H 0.306643 0.613450 -0.069524 0.023 Uiso 1 1 calc R . . . . C42 C 0.1248(3) 0.6395(3) -0.0663(2) 0.0215(5) Uani 1 1 d . . . . . C43 C 0.0045(3) 0.6589(3) -0.0098(2) 0.0232(6) Uani 1 1 d . . . . . C44 C 0.0140(3) 0.6690(3) 0.0888(2) 0.0235(6) Uani 1 1 d . . . . . H44 H -0.060162 0.684629 0.127301 0.028 Uiso 1 1 calc R . . . . C45 C 0.1221(3) 0.6571(3) 0.1265(2) 0.0208(5) Uani 1 1 d . . . . . H45 H 0.120980 0.663490 0.191400 0.025 Uiso 1 1 calc R . . . . O46 O 0.49852(18) 0.80411(19) 0.02774(18) 0.0281(5) Uani 1 1 d . . . . . C47 C 0.6300(3) 0.7854(3) 0.0023(3) 0.0319(7) Uani 1 1 d . . . . . H47A H 0.647065 0.766345 -0.060657 0.038 Uiso 1 1 calc R . . . . H47B H 0.676441 0.715192 0.059593 0.038 Uiso 1 1 calc R . . . . C48 C 0.6699(3) 0.9026(3) -0.0157(3) 0.0423(9) Uani 1 1 d . . . . . H48A H 0.623171 0.971517 -0.072360 0.063 Uiso 1 1 calc GR . . . . H48B H 0.758860 0.892421 -0.033750 0.063 Uiso 1 1 calc GR . . . . H48C H 0.653594 0.920041 0.047242 0.063 Uiso 1 1 calc GR . . . . C49 C 0.2969(10) 0.1797(10) 0.3103(8) 0.025(2) Uani 0.510(8) 1 d . . P A 2 H49C H 0.208226 0.199147 0.294218 0.030 Uiso 0.510(8) 1 calc R . P A 2 H49D H 0.340147 0.111390 0.288146 0.030 Uiso 0.510(8) 1 calc R . P A 2 C49A C 0.2984(11) 0.1721(11) 0.2744(9) 0.030(2) Uani 0.490(8) 1 d . . P A 1 H49A H 0.231801 0.188762 0.227170 0.036 Uiso 0.490(8) 1 calc R . P A 1 H49B H 0.365818 0.104090 0.267807 0.036 Uiso 0.490(8) 1 calc R . P A 1 C50 C 0.3061(6) 0.1342(5) 0.4248(5) 0.0255(14) Uani 0.510(8) 1 d . . P A 2 H50 H 0.245226 0.175260 0.460393 0.031 Uiso 0.510(8) 1 calc R . P A 2 C50A C 0.2489(7) 0.1374(6) 0.3827(6) 0.0289(17) Uani 0.490(8) 1 d . . P A 1 H50A H 0.301172 0.129249 0.434148 0.035 Uiso 0.490(8) 1 calc R . P A 1 C51 C 0.3920(6) 0.0416(6) 0.4801(5) 0.0322(16) Uani 0.510(8) 1 d . . P A 2 H51C H 0.454557 -0.001797 0.447309 0.039 Uiso 0.510(8) 1 calc R . P A 2 H51D H 0.391584 0.018223 0.552721 0.039 Uiso 0.510(8) 1 calc R . P A 2 C51A C 0.1362(7) 0.1172(6) 0.4112(6) 0.0354(18) Uani 0.490(8) 1 d . . P A 1 H51A H 0.081893 0.124704 0.361281 0.042 Uiso 0.490(8) 1 calc R . P A 1 H51B H 0.109306 0.095268 0.481554 0.042 Uiso 0.490(8) 1 calc R . P A 1 Br52 Br 0.11252(3) 0.63156(3) -0.19561(2) 0.02832(10) Uani 1 1 d . . . . . O53 O -0.09377(19) 0.6656(2) -0.04287(19) 0.0354(5) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0263(12) 0.0698(19) 0.0351(14) 0.0180(13) -0.0122(10) -0.0074(12) C2 0.0216(15) 0.052(2) 0.0272(16) 0.0072(15) -0.0036(13) -0.0008(14) C3 0.0242(14) 0.0355(17) 0.0173(14) 0.0006(12) -0.0031(11) 0.0004(12) C4 0.0244(14) 0.0369(17) 0.0171(14) -0.0038(12) -0.0053(11) -0.0060(12) C5 0.0293(17) 0.064(2) 0.0269(17) -0.0161(16) -0.0083(13) -0.0092(16) C6 0.0289(17) 0.064(2) 0.0284(17) -0.0064(17) -0.0121(13) -0.0118(16) C7 0.0297(18) 0.047(2) 0.0347(19) 0.0172(17) -0.0009(14) 0.0069(15) C8 0.0356(18) 0.0320(17) 0.0324(18) 0.0087(14) 0.0086(14) 0.0024(14) C9 0.0317(16) 0.0308(16) 0.0209(14) -0.0038(12) 0.0032(12) 0.0001(13) C10 0.0252(14) 0.0304(15) 0.0189(14) -0.0045(12) -0.0016(11) 0.0008(12) C11 0.0272(15) 0.0377(17) 0.0182(14) -0.0083(12) -0.0015(11) -0.0102(13) C12 0.0242(14) 0.0276(14) 0.0223(14) -0.0105(12) -0.0037(11) -0.0079(11) C13 0.0333(15) 0.0220(13) 0.0188(13) -0.0064(11) -0.0061(11) -0.0105(11) C14 0.0294(15) 0.0294(15) 0.0182(13) -0.0068(12) -0.0010(11) -0.0130(12) C15 0.0213(13) 0.0333(15) 0.0207(14) -0.0076(12) -0.0021(11) -0.0100(11) O16 0.0221(10) 0.0424(13) 0.0321(12) -0.0055(10) -0.0072(9) -0.0089(9) C17 0.0256(15) 0.0294(16) 0.046(2) -0.0074(14) -0.0084(14) -0.0101(12) C18 0.0405(19) 0.0363(19) 0.051(2) -0.0122(17) 0.0012(16) -0.0118(15) C19 0.0425(19) 0.0316(16) 0.0292(16) -0.0098(14) 0.0001(14) -0.0084(14) C20 0.0371(18) 0.0426(19) 0.0381(19) -0.0109(16) -0.0003(15) -0.0146(15) C21 0.043(2) 0.067(3) 0.047(2) -0.026(2) 0.0166(17) -0.0268(19) Br22 0.02884(17) 0.03467(18) 0.02857(17) -0.01682(14) -0.00676(12) -0.00375(13) O23 0.0526(14) 0.0228(11) 0.0228(11) -0.0049(9) -0.0100(10) -0.0019(10) O31 0.0176(9) 0.0240(10) 0.0304(11) -0.0060(9) -0.0066(8) -0.0073(8) C32 0.0168(12) 0.0219(13) 0.0169(12) -0.0084(10) 0.0004(10) -0.0051(10) C33 0.0162(12) 0.0216(13) 0.0143(12) -0.0073(10) -0.0013(9) -0.0043(10) C34 0.0154(12) 0.0201(13) 0.0172(12) -0.0069(10) -0.0030(9) -0.0040(10) C35 0.0172(13) 0.0207(13) 0.0232(13) -0.0080(11) -0.0019(10) -0.0037(10) C36 0.0178(13) 0.0199(13) 0.0263(14) -0.0064(11) -0.0014(10) -0.0054(10) C37 0.0145(12) 0.0292(14) 0.0202(13) -0.0100(11) -0.0012(10) -0.0012(10) C38 0.0236(14) 0.0244(14) 0.0252(15) 0.0005(12) -0.0018(11) 0.0006(11) C39 0.0264(15) 0.0244(15) 0.0355(17) -0.0020(13) 0.0012(13) -0.0085(12) C40 0.0193(13) 0.0251(14) 0.0265(14) -0.0077(12) -0.0011(11) -0.0083(11) C41 0.0168(12) 0.0247(13) 0.0152(12) -0.0061(10) 0.0001(10) -0.0048(10) C42 0.0230(13) 0.0266(14) 0.0154(12) -0.0073(11) -0.0022(10) -0.0067(11) C43 0.0184(13) 0.0266(14) 0.0255(14) -0.0096(12) -0.0037(11) -0.0055(11) C44 0.0181(13) 0.0286(14) 0.0224(14) -0.0093(12) 0.0034(10) -0.0054(11) C45 0.0221(13) 0.0231(13) 0.0180(13) -0.0087(11) 0.0008(10) -0.0057(10) O46 0.0180(9) 0.0221(10) 0.0451(13) -0.0131(9) 0.0028(9) -0.0076(8) C47 0.0196(14) 0.0265(15) 0.048(2) -0.0125(14) 0.0052(13) -0.0089(12) C48 0.0260(16) 0.0319(17) 0.071(3) -0.0195(18) 0.0060(16) -0.0140(14) C49 0.027(4) 0.020(3) 0.030(6) -0.012(4) -0.006(4) -0.004(3) C49A 0.035(4) 0.021(4) 0.033(6) -0.011(4) 0.010(5) -0.011(3) C50 0.031(3) 0.021(3) 0.025(3) -0.010(2) 0.003(3) -0.010(2) C50A 0.039(4) 0.018(3) 0.025(4) -0.005(3) 0.005(3) -0.008(3) C51 0.044(4) 0.024(3) 0.025(3) -0.007(2) 0.000(3) -0.005(3) C51A 0.044(4) 0.025(3) 0.036(4) -0.014(3) 0.013(3) -0.010(3) Br52 0.02738(16) 0.04180(19) 0.02018(16) -0.01446(13) -0.00523(11) -0.00864(13) O53 0.0174(10) 0.0566(15) 0.0383(13) -0.0231(11) -0.0055(9) -0.0082(10) 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' O O 0.0492 0.0322 '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' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 -1 0 0.0692 -3 5 0 0.0770 4 -4 2 0.0987 -5 4 -2 0.0949 -6 -3 -6 0.1530 0 -7 -3 0.0956 2 5 -4 0.0969 -7 1 -2 0.1228 -7 -3 0 0.1239 -7 -3 -4 0.1437 1 0 -5 0.1558 5 -2 1 0.1193 2 -1 3 0.0804 -2 1 5 0.1545 0 0 -1 0.1534 -2 1 -3 0.1376 -5 2 3 0.1254 -1 -5 4 0.1042 1 0 1 0.0999 0 0 -1 0.1459 0 1 0 0.0362 7 -1 2 0.1182 5 6 7 0.1178 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 O1 C6 118.1(3) . . ? O1 C2 C3 123.9(3) . . ? O1 C2 C7 116.4(3) . . ? C7 C2 C3 119.7(3) . . ? C2 C3 C4 121.1(3) . . ? C2 C3 C10 118.2(3) . . ? C10 C3 C4 120.7(3) . . ? C3 C4 C5 108.0(3) . . ? C11 C4 C3 109.7(3) . . ? C11 C4 C5 106.9(3) . . ? C11 C4 C15 111.9(2) . . ? C15 C4 C3 109.0(3) . . ? C15 C4 C5 111.3(3) . . ? C4 C5 H5A 109.1 . . ? C4 C5 H5B 109.1 . . ? H5A C5 H5B 107.8 . . ? C6 C5 C4 112.5(3) . . ? C6 C5 H5A 109.1 . . ? C6 C5 H5B 109.1 . . ? O1 C6 C5 111.8(3) . . ? O1 C6 H6 108.3 . . ? C5 C6 H6 108.3 . . ? O16 C6 O1 111.5(3) . . ? O16 C6 C5 108.6(3) . . ? O16 C6 H6 108.3 . . ? C2 C7 H7 119.5 . . ? C8 C7 C2 121.0(3) . . ? C8 C7 H7 119.5 . . ? C7 C8 H8 119.6 . . ? C7 C8 C9 120.8(3) . . ? C9 C8 H8 119.6 . . ? C8 C9 C19 120.5(3) . . ? C10 C9 C8 117.6(3) . . ? C10 C9 C19 121.8(3) . . ? C3 C10 H10 118.6 . . ? C9 C10 C3 122.7(3) . . ? C9 C10 H10 118.6 . . ? C4 C11 H11 118.3 . . ? C12 C11 C4 123.5(3) . . ? C12 C11 H11 118.3 . . ? C11 C12 C13 123.1(3) . . ? C11 C12 Br22 120.8(2) . . ? C13 C12 Br22 116.1(2) . . ? C14 C13 C12 114.8(2) . . ? O23 C13 C12 122.4(3) . . ? O23 C13 C14 122.8(3) . . ? C13 C14 H14 118.7 . . ? C15 C14 C13 122.6(3) . . ? C15 C14 H14 118.7 . . ? C4 C15 H15 118.1 . . ? C14 C15 C4 123.9(3) . . ? C14 C15 H15 118.1 . . ? C6 O16 C17 114.2(3) . . ? O16 C17 H17A 110.3 . . ? O16 C17 H17B 110.3 . . ? O16 C17 C18 106.9(3) . . ? H17A C17 H17B 108.6 . . ? C18 C17 H17A 110.3 . . ? C18 C17 H17B 110.3 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C9 C19 H19A 108.4 . . ? C9 C19 H19B 108.4 . . ? H19A C19 H19B 107.5 . . ? C20 C19 C9 115.5(3) . . ? C20 C19 H19A 108.4 . . ? C20 C19 H19B 108.4 . . ? C19 C20 H20 117.0 . . ? C21 C20 C19 126.0(3) . . ? C21 C20 H20 117.0 . . ? C20 C21 H21A 120.0 . . ? C20 C21 H21B 120.0 . . ? H21A C21 H21B 120.0 . . ? C32 O31 C36 115.6(2) . . ? O31 C32 C33 123.8(2) . . ? O31 C32 C37 115.7(2) . . ? C33 C32 C37 120.5(2) . . ? C32 C33 C34 121.2(2) . . ? C32 C33 C40 118.7(2) . . ? C40 C33 C34 120.1(2) . . ? C33 C34 C35 109.2(2) . . ? C41 C34 C33 108.2(2) . . ? C41 C34 C35 110.2(2) . . ? C45 C34 C33 109.5(2) . . ? C45 C34 C35 107.6(2) . . ? C45 C34 C41 112.1(2) . . ? C34 C35 H35A 109.3 . . ? C34 C35 H35B 109.3 . . ? H35A C35 H35B 107.9 . . ? C36 C35 C34 111.8(2) . . ? C36 C35 H35A 109.3 . . ? C36 C35 H35B 109.3 . . ? O31 C36 C35 110.0(2) . . ? O31 C36 H36 110.3 . . ? C35 C36 H36 110.3 . . ? O46 C36 O31 107.2(2) . . ? O46 C36 C35 108.7(2) . . ? O46 C36 H36 110.3 . . ? C32 C37 H37 120.2 . . ? C38 C37 C32 119.6(3) . . ? C38 C37 H37 120.2 . . ? C37 C38 H38 119.4 . . ? C37 C38 C39 121.2(3) . . ? C39 C38 H38 119.4 . . ? C38 C39 C49 116.1(5) . . ? C38 C39 C49A 123.1(5) . . ? C40 C39 C38 118.5(3) . . ? C40 C39 C49 124.2(5) . . ? C40 C39 C49A 117.6(5) . . ? C33 C40 H40 119.3 . . ? C39 C40 C33 121.5(3) . . ? C39 C40 H40 119.3 . . ? C34 C41 H41 118.4 . . ? C42 C41 C34 123.2(2) . . ? C42 C41 H41 118.4 . . ? C41 C42 C43 123.2(3) . . ? C41 C42 Br52 122.0(2) . . ? C43 C42 Br52 114.77(19) . . ? C44 C43 C42 114.6(2) . . ? O53 C43 C42 122.5(3) . . ? O53 C43 C44 122.9(3) . . ? C43 C44 H44 118.6 . . ? C45 C44 C43 122.8(3) . . ? C45 C44 H44 118.6 . . ? C34 C45 H45 118.0 . . ? C44 C45 C34 124.0(3) . . ? C44 C45 H45 118.0 . . ? C36 O46 C47 113.8(2) . . ? O46 C47 H47A 110.1 . . ? O46 C47 H47B 110.1 . . ? O46 C47 C48 107.9(3) . . ? H47A C47 H47B 108.4 . . ? C48 C47 H47A 110.1 . . ? C48 C47 H47B 110.1 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48B 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C39 C49 H49C 108.2 . . ? C39 C49 H49D 108.2 . . ? H49C C49 H49D 107.4 . . ? C50 C49 C39 116.2(7) . . ? C50 C49 H49C 108.2 . . ? C50 C49 H49D 108.2 . . ? C39 C49A H49A 110.3 . . ? C39 C49A H49B 110.3 . . ? H49A C49A H49B 108.6 . . ? C50A C49A C39 107.0(7) . . ? C50A C49A H49A 110.3 . . ? C50A C49A H49B 110.3 . . ? C49 C50 H50 117.5 . . ? C51 C50 C49 125.0(7) . . ? C51 C50 H50 117.5 . . ? C49A C50A H50A 118.2 . . ? C51A C50A C49A 123.5(9) . . ? C51A C50A H50A 118.2 . . ? C50 C51 H51C 120.0 . . ? C50 C51 H51D 120.0 . . ? H51C C51 H51D 120.0 . . ? C50A C51A H51A 120.0 . . ? C50A C51A H51B 120.0 . . ? H51A C51A H51B 120.0 . . ? 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 O1 C2 1.380(5) . ? O1 C6 1.425(5) . ? C2 C3 1.399(4) . ? C2 C7 1.388(6) . ? C3 C4 1.529(5) . ? C3 C10 1.399(5) . ? C4 C5 1.562(4) . ? C4 C11 1.500(4) . ? C4 C15 1.507(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C5 C6 1.513(5) . ? C6 H6 1.0000 . ? C6 O16 1.388(4) . ? C7 H7 0.9500 . ? C7 C8 1.377(6) . ? C8 H8 0.9500 . ? C8 C9 1.401(5) . ? C9 C10 1.384(5) . ? C9 C19 1.512(5) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C11 C12 1.326(4) . ? C12 C13 1.477(4) . ? C12 Br22 1.892(3) . ? C13 C14 1.465(4) . ? C13 O23 1.223(4) . ? C14 H14 0.9500 . ? C14 C15 1.330(4) . ? C15 H15 0.9500 . ? O16 C17 1.442(4) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C17 C18 1.499(5) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C19 C20 1.497(5) . ? C20 H20 0.9500 . ? C20 C21 1.303(6) . ? C21 H21A 0.9500 . ? C21 H21B 0.9500 . ? O31 C32 1.369(3) . ? O31 C36 1.442(3) . ? C32 C33 1.395(4) . ? C32 C37 1.395(4) . ? C33 C34 1.538(4) . ? C33 C40 1.397(4) . ? C34 C35 1.554(4) . ? C34 C41 1.506(4) . ? C34 C45 1.505(4) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C35 C36 1.513(4) . ? C36 H36 1.0000 . ? C36 O46 1.375(3) . ? C37 H37 0.9500 . ? C37 C38 1.373(4) . ? C38 H38 0.9500 . ? C38 C39 1.402(4) . ? C39 C40 1.381(4) . ? C39 C49 1.512(12) . ? C39 C49A 1.578(12) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? C41 C42 1.329(4) . ? C42 C43 1.484(4) . ? C42 Br52 1.893(3) . ? C43 C44 1.466(4) . ? C43 O53 1.217(3) . ? C44 H44 0.9500 . ? C44 C45 1.331(4) . ? C45 H45 0.9500 . ? O46 C47 1.445(3) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C47 C48 1.506(4) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49C 0.9900 . ? C49 H49D 0.9900 . ? C49 C50 1.495(11) . ? C49A H49A 0.9900 . ? C49A H49B 0.9900 . ? C49A C50A 1.486(11) . ? C50 H50 0.9500 . ? C50 C51 1.315(9) . ? C50A H50A 0.9500 . ? C50A C51A 1.320(11) . ? C51 H51C 0.9500 . ? C51 H51D 0.9500 . ? C51A H51A 0.9500 . ? C51A H51B 0.9500 . ? 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 O1 C2 C3 C4 -1.4(6) . . . . ? O1 C2 C3 C10 178.8(3) . . . . ? O1 C2 C7 C8 180.0(4) . . . . ? O1 C6 O16 C17 68.2(3) . . . . ? C2 O1 C6 C5 -39.0(5) . . . . ? C2 O1 C6 O16 82.9(4) . . . . ? C2 C3 C4 C5 19.1(4) . . . . ? C2 C3 C4 C11 135.2(3) . . . . ? C2 C3 C4 C15 -102.0(3) . . . . ? C2 C3 C10 C9 1.2(5) . . . . ? C2 C7 C8 C9 1.1(6) . . . . ? C3 C2 C7 C8 -1.5(6) . . . . ? C3 C4 C5 C6 -46.0(4) . . . . ? C3 C4 C11 C12 124.8(3) . . . . ? C3 C4 C15 C14 -125.8(3) . . . . ? C4 C3 C10 C9 -178.6(3) . . . . ? C4 C5 C6 O1 57.8(4) . . . . ? C4 C5 C6 O16 -65.7(4) . . . . ? C4 C11 C12 C13 0.1(5) . . . . ? C4 C11 C12 Br22 179.4(2) . . . . ? C5 C4 C11 C12 -118.4(3) . . . . ? C5 C4 C15 C14 115.2(3) . . . . ? C5 C6 O16 C17 -168.1(3) . . . . ? C6 O1 C2 C3 11.2(6) . . . . ? C6 O1 C2 C7 -170.3(4) . . . . ? C6 O16 C17 C18 179.4(3) . . . . ? C7 C2 C3 C4 -179.8(3) . . . . ? C7 C2 C3 C10 0.4(5) . . . . ? C7 C8 C9 C10 0.5(5) . . . . ? C7 C8 C9 C19 179.1(3) . . . . ? C8 C9 C10 C3 -1.6(5) . . . . ? C8 C9 C19 C20 -76.4(4) . . . . ? C9 C19 C20 C21 -7.3(6) . . . . ? C10 C3 C4 C5 -161.2(3) . . . . ? C10 C3 C4 C11 -45.1(4) . . . . ? C10 C3 C4 C15 77.8(4) . . . . ? C10 C9 C19 C20 102.2(4) . . . . ? C11 C4 C5 C6 -163.9(3) . . . . ? C11 C4 C15 C14 -4.3(4) . . . . ? C11 C12 C13 C14 -3.5(4) . . . . ? C11 C12 C13 O23 176.4(3) . . . . ? C12 C13 C14 C15 3.0(4) . . . . ? C13 C14 C15 C4 1.0(5) . . . . ? C15 C4 C5 C6 73.6(4) . . . . ? C15 C4 C11 C12 3.7(4) . . . . ? C19 C9 C10 C3 179.8(3) . . . . ? Br22 C12 C13 C14 177.11(19) . . . . ? Br22 C12 C13 O23 -3.0(4) . . . . ? O23 C13 C14 C15 -177.0(3) . . . . ? O31 C32 C33 C34 -1.3(4) . . . . ? O31 C32 C33 C40 179.6(2) . . . . ? O31 C32 C37 C38 179.3(3) . . . . ? O31 C36 O46 C47 66.1(3) . . . . ? C32 O31 C36 C35 50.2(3) . . . . ? C32 O31 C36 O46 168.2(2) . . . . ? C32 C33 C34 C35 -10.2(3) . . . . ? C32 C33 C34 C41 109.7(3) . . . . ? C32 C33 C34 C45 -127.8(3) . . . . ? C32 C33 C40 C39 1.9(4) . . . . ? C32 C37 C38 C39 0.7(5) . . . . ? C33 C32 C37 C38 1.2(4) . . . . ? C33 C34 C35 C36 40.6(3) . . . . ? C33 C34 C41 C42 120.5(3) . . . . ? C33 C34 C45 C44 -119.5(3) . . . . ? C34 C33 C40 C39 -177.2(3) . . . . ? C34 C35 C36 O31 -61.9(3) . . . . ? C34 C35 C36 O46 -179.0(2) . . . . ? C34 C41 C42 C43 -1.2(4) . . . . ? C34 C41 C42 Br52 179.5(2) . . . . ? C35 C34 C41 C42 -120.2(3) . . . . ? C35 C34 C45 C44 121.9(3) . . . . ? C35 C36 O46 C47 -175.0(2) . . . . ? C36 O31 C32 C33 -19.3(4) . . . . ? C36 O31 C32 C37 162.6(2) . . . . ? C36 O46 C47 C48 176.1(3) . . . . ? C37 C32 C33 C34 176.7(2) . . . . ? C37 C32 C33 C40 -2.4(4) . . . . ? C37 C38 C39 C40 -1.2(5) . . . . ? C37 C38 C39 C49 -169.3(5) . . . . ? C37 C38 C39 C49A 168.7(5) . . . . ? C38 C39 C40 C33 -0.1(5) . . . . ? C38 C39 C49 C50 47.9(9) . . . . ? C38 C39 C49A C50A 83.8(8) . . . . ? C39 C49 C50 C51 -98.6(9) . . . . ? C39 C49A C50A C51A 127.8(7) . . . . ? C40 C33 C34 C35 168.9(2) . . . . ? C40 C33 C34 C41 -71.2(3) . . . . ? C40 C33 C34 C45 51.3(3) . . . . ? C40 C39 C49 C50 -119.5(7) . . . . ? C40 C39 C49A C50A -106.3(7) . . . . ? C41 C34 C35 C36 -78.1(3) . . . . ? C41 C34 C45 C44 0.5(4) . . . . ? C41 C42 C43 C44 2.6(4) . . . . ? C41 C42 C43 O53 -177.3(3) . . . . ? C42 C43 C44 C45 -2.4(4) . . . . ? C43 C44 C45 C34 1.0(5) . . . . ? C45 C34 C35 C36 159.4(2) . . . . ? C45 C34 C41 C42 -0.4(4) . . . . ? C49 C39 C40 C33 167.0(5) . . . . ? C49A C39 C40 C33 -170.6(5) . . . . ? Br52 C42 C43 C44 -178.1(2) . . . . ? Br52 C42 C43 O53 1.9(4) . . . . ? O53 C43 C44 C45 177.5(3) . . . . ? 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 -0.0004 -0.5001 -0.0019 0.0509 -0.0182 -0.0463 -2.9950 5.4999 0.0185 -0.3352 0.3260 0.8528 3.9911 -4.0017 1.9857 0.1957 -0.1255 -0.9446 -4.9912 3.5011 -1.9884 -0.0698 0.1491 1.0126 -5.9866 -3.4956 -6.0112 0.5417 -0.4396 0.7111 0.0015 -7.4977 -3.0250 0.6315 -0.5549 -0.5204 2.0128 5.0072 -3.9744 -0.8355 -0.2764 0.4678 -6.9925 0.9997 -1.9996 0.3348 0.1415 1.0095 -6.9999 -2.5037 -0.0154 0.7794 0.2014 0.5686 -6.9907 -2.9985 -4.0125 0.6539 -0.1920 0.7553 1.0113 -0.4931 -4.9951 -0.2445 -0.5290 0.1306 4.9947 -1.9995 0.9953 -0.1271 -0.1882 -0.8153 1.9915 -1.0033 2.9942 0.0842 0.1613 -0.4961 -2.0106 0.9928 4.9961 0.2686 0.5890 0.0301 0.0024 0.0013 -0.9988 -0.0441 -0.0938 0.0583 -1.9915 1.0033 -2.9942 -0.0842 -0.1613 0.4961 -5.0042 1.9943 2.9998 0.3035 0.5633 0.5823 -1.0130 -5.0068 3.9752 0.7606 0.2346 -0.5821 0.9977 0.4992 1.0015 -0.0818 0.0702 -0.1262 0.0020 -0.4988 -1.0007 0.0068 -0.1120 0.0119 0.0004 0.5001 0.0019 -0.0509 0.0182 0.0463 6.9925 -0.9997 1.9996 -0.3348 -0.1415 -1.0095 4.9867 6.4945 7.0206 -0.7281 0.6846 -0.3769