#------------------------------------------------------------------------------ #$Date: 2024-01-06 10:21:58 +0200 (Sat, 06 Jan 2024) $ #$Revision: 288817 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/76/7247608.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_7247608 loop_ _publ_author_name 'Li, Chaoyang' 'Niu, Xinyue' 'Xu, Wan' 'Bu, Zhanwei' 'Zhang, Wenjing' 'Wang, Qilin' _publ_section_title ; Distinct reactivities of ortho-chalcone-substituted organophosphines with activated alkynes: skeletal editing or periphery modification ; _journal_issue 24 _journal_name_full 'Green Chemistry' _journal_page_first 10587 _journal_page_last 10595 _journal_paper_doi 10.1039/D3GC03165A _journal_volume 25 _journal_year 2023 _chemical_formula_moiety 'C54 H40 Br2 O2 P2' _chemical_formula_sum 'C54 H40 Br2 O2 P2' _chemical_formula_weight 942.62 _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 dual _audit_creation_date 2021-11-23 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408) ; _audit_update_record ; 2023-10-24 deposited with the CCDC. 2023-10-30 downloaded from the CCDC. ; _cell_angle_alpha 101.507(3) _cell_angle_beta 108.532(3) _cell_angle_gamma 108.298(4) _cell_formula_units_Z 3 _cell_length_a 14.3800(5) _cell_length_b 15.4793(7) _cell_length_c 17.3460(6) _cell_measurement_reflns_used 7811 _cell_measurement_temperature 149.99(10) _cell_measurement_theta_max 74.1800 _cell_measurement_theta_min 2.8590 _cell_volume 3278.1(3) _computing_cell_refinement 'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 149.99(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.2684 _diffrn_detector_type AtlasS2 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.964 _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 -65.00 34.00 1.00 1.00 -- -40.36 38.00 60.00 99 2 \w -60.00 32.00 1.00 1.00 -- -40.36 57.00 150.00 92 3 \w -88.00 -5.00 1.00 1.00 -- -40.36 125.00 150.00 83 4 \w 57.00 91.00 1.00 1.00 -- 40.36-125.00 30.00 34 5 \w 38.00 67.00 1.00 2.00 -- 108.83-125.00 -30.00 29 6 \w 82.00 109.00 1.00 2.00 -- 108.83-125.00 -30.00 27 7 \w 49.00 120.00 1.00 2.00 -- 108.83-125.00-150.00 71 8 \w 47.00 120.00 1.00 2.00 -- 108.83 -15.00 -60.00 73 9 \w 80.00 113.00 1.00 2.00 -- 108.83 61.00 0.00 33 10 \w 145.00 173.00 1.00 2.00 -- 108.83 61.00 0.00 28 11 \w 146.00 175.00 1.00 2.00 -- 108.83 77.00-120.00 29 12 \w 98.00 125.00 1.00 2.00 -- 108.83 125.00-120.00 27 13 \w 94.00 140.00 1.00 2.00 -- 108.83 125.00 -90.00 46 14 \w 80.00 178.00 1.00 2.00 -- 108.83 61.00 -30.00 98 15 \w 89.00 172.00 1.00 2.00 -- 108.83 45.00 90.00 83 16 \w 77.00 122.00 1.00 2.00 -- 108.83 77.00-120.00 45 17 \w 36.00 131.00 1.00 2.00 -- 108.83 -77.00 30.00 95 18 \w 40.00 116.00 1.00 2.00 -- 108.83-125.00 60.00 76 19 \w 36.00 140.00 1.00 2.00 -- 108.83 -77.00-150.00 104 20 \w -106.00 -16.00 1.00 1.00 -- -40.36 -38.00-120.00 90 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, AtlasS2' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0247570000 _diffrn_orient_matrix_UB_12 0.1083484000 _diffrn_orient_matrix_UB_13 0.0313067000 _diffrn_orient_matrix_UB_21 0.1088964000 _diffrn_orient_matrix_UB_22 0.0243251000 _diffrn_orient_matrix_UB_23 -0.0068249000 _diffrn_orient_matrix_UB_31 -0.0530833000 _diffrn_orient_matrix_UB_32 -0.0047215000 _diffrn_orient_matrix_UB_33 -0.0940094000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0417 _diffrn_reflns_av_unetI/netI 0.0570 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.964 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 23821 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.964 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 74.450 _diffrn_reflns_theta_min 2.849 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 3.372 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.47449 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.432 _exptl_crystal_description block _exptl_crystal_F_000 1440 _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _refine_diff_density_max 1.416 _refine_diff_density_min -1.099 _refine_diff_density_rms 0.084 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 830 _refine_ls_number_reflns 12906 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.038 _refine_ls_R_factor_all 0.0753 _refine_ls_R_factor_gt 0.0534 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0787P)^2^+2.4771P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1433 _refine_ls_wR_factor_ref 0.1573 _reflns_Friedel_coverage 0.000 _reflns_number_gt 9761 _reflns_number_total 12906 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3gc03165a2.cif _cod_data_source_block glj-p _cod_depositor_comments 'Adding full bibliography for 7247605--7247608.cif.' _cod_original_cell_volume 3278.1(2) _cod_database_code 7247608 _shelx_shelxl_version_number 2018/3 _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 0.708 _shelx_estimated_absorpt_t_min 0.650 _reflns_odcompleteness_completeness 99.75 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups 2. Others Sof(H47A)=Sof(C50)=Sof(H50)=Sof(C51)=Sof(H51)=1-FVAR(1) Sof(H47)=Sof(C48)=Sof(H48)=Sof(C49)=Sof(H49)=FVAR(1) 3.a Ternary CH refined with riding coordinates: C2(H2), C3(H3), C4(H4), C31(H31), C71(H71), C72(H72) 3.b Aromatic/amide H refined with riding coordinates: C7(H7), C8(H8), C10(H10), C11(H11), C14(H14), C15(H15), C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C33(H33), C34(H34), C36(H36), C37(H37), C39(H39), C40(H40), C41(H41), C42(H42), C45(H45), C46(H46), C47(H47), C47(H47A), C48(H48), C49(H49), C50(H50), C51(H51), C53(H53), C54(H54), C55(H55), C56(H56), C57(H57), C60(H60), C61(H61), C62(H62), C63(H63), C64(H64), C66(H66), C67(H67), C68(H68), C69(H69), C70(H70), C75(H75), C76(H76), C78(H78), C79(H79), C82(H82), C83(H83), C84(H84), C85(H85) ; _smtbx_masks_void_probe_radius 1.2 _smtbx_masks_void_truncation_radius 1.2 _shelx_res_file ; TITL glj-p_a.res in P-1 glj-p.res created by SHELXL-2018/3 at 18:27:15 on 23-Nov-2021 REM Old TITL GLJ-P in P-1 REM SHELXT solution in P-1: R1 0.240, Rweak 0.017, Alpha 0.048 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C81 O6 Br3 CELL 1.54184 14.380033 15.479341 17.345995 101.5068 108.5319 108.298 ZERR 3 0.000503 0.000723 0.000567 0.0033 0.0031 0.0036 LATT 1 SFAC C H Br O P UNIT 162 120 6 6 6 L.S. 20 PLAN 7 SIZE 0.11 0.12 0.14 CONF BOND list 4 ABIN fmap 2 53 acta MORE -1 BOND $H OMIT 9 5 8 OMIT 11 0 0 OMIT 12 2 2 OMIT 12 1 1 OMIT -3 1 20 REM REM REM WGHT 0.078700 2.477100 FVAR 2.75635 0.56546 BR1 3 0.597850 0.503514 0.707272 11.00000 0.06357 0.10701 = 0.05553 0.04283 0.04278 0.04123 BR2 3 1.425494 0.835529 0.321036 11.00000 0.03758 0.07061 = 0.05713 0.02582 0.02948 0.01486 P1 5 0.826098 0.543696 0.149101 11.00000 0.04034 0.03182 = 0.03662 0.01912 0.01780 0.01735 P2 5 0.994111 0.837834 0.601798 11.00000 0.03342 0.02583 = 0.02990 0.01136 0.01290 0.01584 O1 4 0.660447 0.424568 0.328794 11.00000 0.03819 0.04047 = 0.03856 0.00583 0.01751 0.00580 O2 4 1.086050 0.610429 0.486099 11.00000 0.03201 0.03792 = 0.04408 0.02460 0.01766 0.01988 C2 1 0.899713 0.645861 0.452882 11.00000 0.02622 0.02274 = 0.02704 0.00885 0.01082 0.01400 AFIX 13 H2 2 0.951957 0.667036 0.512613 11.00000 -1.20000 AFIX 0 C3 1 0.954085 0.643337 0.387503 11.00000 0.02482 0.02484 = 0.03201 0.01392 0.01238 0.01351 AFIX 13 H3 2 0.952599 0.691386 0.358446 11.00000 -1.20000 AFIX 0 C4 1 0.862837 0.538617 0.331802 11.00000 0.02832 0.02443 = 0.02903 0.01093 0.01217 0.01247 AFIX 13 H4 2 0.802492 0.546301 0.292011 11.00000 -1.20000 AFIX 0 C5 1 1.064041 0.642127 0.426651 11.00000 0.02775 0.02097 = 0.03026 0.00810 0.01198 0.01126 C6 1 1.146593 0.681396 0.393411 11.00000 0.02904 0.02498 = 0.03301 0.00961 0.01477 0.01455 C7 1 1.124012 0.708447 0.319915 11.00000 0.02620 0.03909 = 0.02969 0.00953 0.00934 0.01227 AFIX 43 H7 2 1.053762 0.697259 0.286429 11.00000 -1.20000 AFIX 0 C8 1 1.206483 0.752248 0.296454 11.00000 0.03750 0.05462 = 0.03409 0.01726 0.01849 0.01743 AFIX 43 H8 2 1.192045 0.769964 0.247193 11.00000 -1.20000 AFIX 0 C9 1 1.309900 0.768718 0.347884 11.00000 0.03307 0.04136 = 0.04302 0.01237 0.02408 0.01615 C10 1 1.334233 0.739729 0.419903 11.00000 0.02896 0.04005 = 0.05203 0.01828 0.01822 0.01843 AFIX 43 H10 2 1.404226 0.749165 0.452208 11.00000 -1.20000 AFIX 0 C11 1 1.251948 0.696711 0.442061 11.00000 0.03158 0.03320 = 0.04285 0.01741 0.01547 0.01912 AFIX 43 H11 2 1.266784 0.677428 0.490438 11.00000 -1.20000 AFIX 0 C12 1 0.833836 0.704965 0.441395 11.00000 0.02817 0.02509 = 0.03431 0.01353 0.01796 0.01616 C13 1 0.876477 0.799424 0.499880 11.00000 0.02907 0.02628 = 0.03292 0.01365 0.01699 0.01393 C14 1 0.821636 0.858460 0.482030 11.00000 0.03472 0.02647 = 0.03861 0.01137 0.01704 0.01744 AFIX 43 H14 2 0.849524 0.921103 0.519732 11.00000 -1.20000 AFIX 0 C15 1 0.726509 0.825561 0.409273 11.00000 0.03129 0.03592 = 0.04350 0.01813 0.01718 0.02155 AFIX 43 H15 2 0.692853 0.866778 0.397691 11.00000 -1.20000 AFIX 0 C16 1 0.682211 0.732240 0.354495 11.00000 0.02859 0.03664 = 0.03787 0.01308 0.01051 0.01866 AFIX 43 H16 2 0.616946 0.709122 0.307171 11.00000 -1.20000 AFIX 0 C17 1 0.736002 0.672247 0.370428 11.00000 0.02989 0.02862 = 0.03971 0.01086 0.01522 0.01581 AFIX 43 H17 2 0.706044 0.609202 0.332999 11.00000 -1.20000 AFIX 0 C18 1 1.106946 0.867145 0.569905 11.00000 0.03169 0.02841 = 0.03095 0.00747 0.01169 0.01743 C19 1 1.201916 0.866106 0.624462 11.00000 0.03849 0.04786 = 0.03439 0.01332 0.01132 0.02512 AFIX 43 H19 2 1.203313 0.845871 0.671671 11.00000 -1.20000 AFIX 0 C20 1 1.294117 0.894895 0.609038 11.00000 0.03676 0.05763 = 0.03997 0.01144 0.00993 0.02790 AFIX 43 H20 2 1.357280 0.895498 0.646541 11.00000 -1.20000 AFIX 0 C21 1 1.291516 0.922617 0.537734 11.00000 0.03453 0.03359 = 0.05300 0.00711 0.01971 0.01488 AFIX 43 H21 2 1.353552 0.943302 0.527994 11.00000 -1.20000 AFIX 0 C22 1 1.197345 0.919788 0.480849 11.00000 0.04268 0.02643 = 0.04264 0.01088 0.02053 0.01813 AFIX 43 H22 2 1.195263 0.935819 0.431611 11.00000 -1.20000 AFIX 0 C23 1 1.105544 0.892955 0.497178 11.00000 0.03071 0.02624 = 0.03332 0.00959 0.01096 0.01469 AFIX 43 H23 2 1.042625 0.892239 0.459177 11.00000 -1.20000 AFIX 0 C24 1 1.008223 0.958047 0.658492 11.00000 0.03251 0.03126 = 0.02795 0.01230 0.01191 0.01660 C25 1 1.087385 1.044281 0.668843 11.00000 0.03635 0.03236 = 0.02890 0.01400 0.01223 0.01859 AFIX 43 H25 2 1.135501 1.043160 0.643729 11.00000 -1.20000 AFIX 0 C26 1 1.095660 1.132296 0.716270 11.00000 0.04065 0.02620 = 0.03526 0.01081 0.00970 0.01461 AFIX 43 H26 2 1.149444 1.189393 0.723025 11.00000 -1.20000 AFIX 0 C27 1 1.024284 1.135108 0.753314 11.00000 0.05145 0.03584 = 0.03627 0.00914 0.01296 0.02655 AFIX 43 H27 2 1.029959 1.194017 0.784987 11.00000 -1.20000 AFIX 0 C28 1 0.943878 1.049753 0.743221 11.00000 0.03990 0.05093 = 0.03595 0.00784 0.01371 0.02627 AFIX 43 H28 2 0.894891 1.051605 0.767230 11.00000 -1.20000 AFIX 0 C29 1 0.936703 0.961540 0.697186 11.00000 0.03530 0.04133 = 0.03564 0.01161 0.01291 0.01663 AFIX 43 H29 2 0.884156 0.904510 0.692024 11.00000 -1.20000 AFIX 0 C30 1 0.728644 0.477358 0.400604 11.00000 0.02874 0.02656 = 0.03993 0.01207 0.01715 0.01400 C31 1 0.841604 0.532893 0.412661 11.00000 0.02787 0.02302 = 0.02850 0.00975 0.01366 0.01292 AFIX 13 H31 2 0.887743 0.505544 0.444446 11.00000 -1.20000 AFIX 0 C32 1 0.701018 0.486095 0.477455 11.00000 0.03706 0.03162 = 0.03856 0.01760 0.02162 0.02109 C33 1 0.776811 0.541824 0.560548 11.00000 0.03307 0.04220 = 0.03804 0.01345 0.01849 0.01367 AFIX 43 H33 2 0.847592 0.576067 0.569935 11.00000 -1.20000 AFIX 0 C34 1 0.747523 0.546807 0.630058 11.00000 0.04007 0.06177 = 0.03649 0.01739 0.01799 0.01998 AFIX 43 H34 2 0.798152 0.584574 0.685728 11.00000 -1.20000 AFIX 0 C35 1 0.641992 0.494740 0.615061 11.00000 0.05248 0.05683 = 0.05198 0.03261 0.03527 0.03278 C36 1 0.566227 0.437260 0.532773 11.00000 0.03315 0.04864 = 0.05237 0.02694 0.02454 0.02377 AFIX 43 H36 2 0.495869 0.401923 0.523738 11.00000 -1.20000 AFIX 0 C37 1 0.595470 0.432597 0.464248 11.00000 0.02780 0.03836 = 0.04143 0.01654 0.01444 0.01689 AFIX 43 H37 2 0.544753 0.393661 0.408902 11.00000 -1.20000 AFIX 0 C38 1 0.885661 0.464307 0.280022 11.00000 0.02191 0.02413 = 0.03150 0.01034 0.01268 0.00885 C39 1 0.924100 0.402621 0.314796 11.00000 0.03038 0.02913 = 0.03082 0.01232 0.01263 0.01593 AFIX 43 H39 2 0.934377 0.406355 0.371273 11.00000 -1.20000 AFIX 0 C40 1 0.947664 0.335149 0.266939 11.00000 0.03139 0.02921 = 0.03592 0.01376 0.01440 0.01683 AFIX 43 H40 2 0.974623 0.295389 0.291827 11.00000 -1.20000 AFIX 0 C41 1 0.930746 0.327718 0.182415 11.00000 0.03667 0.03452 = 0.04126 0.01287 0.02313 0.01976 AFIX 43 H41 2 0.945826 0.282676 0.150025 11.00000 -1.20000 AFIX 0 C42 1 0.891112 0.387884 0.146160 11.00000 0.03478 0.03416 = 0.03071 0.01331 0.01819 0.01626 AFIX 43 H42 2 0.879618 0.382287 0.089174 11.00000 -1.20000 AFIX 0 C43 1 0.868057 0.456574 0.193012 11.00000 0.02444 0.02808 = 0.03178 0.01251 0.01326 0.00990 C44 1 0.814727 0.506555 0.037900 11.00000 0.04473 0.04025 = 0.03755 0.02000 0.02054 0.01398 C45 1 0.731219 0.429814 -0.029587 11.00000 0.04279 0.04630 = 0.04290 0.01785 0.02214 0.01683 AFIX 43 H45 2 0.674924 0.391425 -0.019691 11.00000 -1.20000 AFIX 0 C46 1 0.728039 0.407621 -0.112152 11.00000 0.05798 0.04964 = 0.03645 0.01504 0.01937 0.02505 AFIX 43 H46 2 0.670338 0.354807 -0.156408 11.00000 -1.20000 AFIX 0 C47 1 0.807751 0.461945 -0.128453 11.00000 0.07583 0.10277 = 0.04560 0.02210 0.03507 0.01158 PART 1 AFIX 43 H47 2 0.819391 0.439555 -0.176932 21.00000 -1.20000 AFIX 43 PART 2 H47A 2 0.796771 0.470385 -0.181745 -21.00000 -1.20000 AFIX 0 PART 1 C48 1 0.875563 0.558981 -0.065057 21.00000 0.05934 0.06922 = 0.04491 0.02605 0.02953 -0.00013 AFIX 43 H48 2 0.916224 0.607155 -0.080005 21.00000 -1.20000 AFIX 0 C49 1 0.878209 0.577782 0.016838 21.00000 0.04067 0.04900 = 0.04160 0.01619 0.01541 0.00403 AFIX 43 H49 2 0.922655 0.638358 0.058079 21.00000 -1.20000 AFIX 0 PART 2 C50 1 0.914267 0.507370 -0.055483 -21.00000 0.08692 0.07443 = 0.09932 0.05121 0.07777 0.03957 AFIX 43 H50 2 0.976695 0.515873 -0.064125 -21.00000 -1.20000 AFIX 0 C51 1 0.917227 0.536793 0.026437 -21.00000 0.03734 0.06564 = 0.05923 0.03318 0.02639 0.01243 AFIX 43 H51 2 0.982197 0.574839 0.073565 -21.00000 -1.20000 AFIX 0 PART 0 C52 1 0.685344 0.505813 0.132659 11.00000 0.04130 0.03219 = 0.03063 0.01476 0.01499 0.02190 C53 1 0.642650 0.574708 0.129225 11.00000 0.04865 0.03760 = 0.04833 0.01534 0.01245 0.02463 AFIX 43 H53 2 0.686091 0.636994 0.135858 11.00000 -1.20000 AFIX 0 C54 1 0.536389 0.552097 0.116075 11.00000 0.05399 0.05525 = 0.05170 0.01268 0.01396 0.03910 AFIX 43 H54 2 0.508349 0.598395 0.111947 11.00000 -1.20000 AFIX 0 C55 1 0.472161 0.460782 0.109105 11.00000 0.04081 0.07154 = 0.04168 0.02123 0.01975 0.03353 AFIX 43 H55 2 0.401114 0.445965 0.101003 11.00000 -1.20000 AFIX 0 C56 1 0.512559 0.392040 0.114062 11.00000 0.04024 0.05401 = 0.05620 0.02851 0.02122 0.01866 AFIX 43 H56 2 0.469233 0.330813 0.109896 11.00000 -1.20000 AFIX 0 C57 1 0.619191 0.413899 0.125413 11.00000 0.04270 0.04048 = 0.05400 0.02575 0.02337 0.02514 AFIX 43 H57 2 0.646171 0.366767 0.128148 11.00000 -1.20000 AFIX 0 BR3 3 -0.479975 -0.180916 0.159161 11.00000 0.03916 0.06580 = 0.06896 0.03506 0.03679 0.02304 P3 5 0.315274 0.117063 0.142650 11.00000 0.02633 0.03283 = 0.03982 0.01399 0.01296 0.01411 O3 4 -0.029760 0.105068 0.133282 11.00000 0.03451 0.03744 = 0.04329 0.01501 0.01874 0.01476 C59 1 0.449426 0.137060 0.146895 11.00000 0.02659 0.03618 = 0.04520 0.02173 0.01418 0.01605 C60 1 0.458805 0.101263 0.070311 11.00000 0.03649 0.04769 = 0.04800 0.02268 0.01945 0.02273 AFIX 43 H60 2 0.397632 0.060395 0.020817 11.00000 -1.20000 AFIX 0 C61 1 0.559878 0.126771 0.068005 11.00000 0.04400 0.05688 = 0.06150 0.03406 0.02907 0.02835 AFIX 43 H61 2 0.565905 0.103267 0.016927 11.00000 -1.20000 AFIX 0 C62 1 0.649952 0.186345 0.140943 11.00000 0.03011 0.04280 = 0.08662 0.03707 0.02870 0.01960 AFIX 43 H62 2 0.717113 0.202568 0.139281 11.00000 -1.20000 AFIX 0 C63 1 0.642180 0.222510 0.216756 11.00000 0.03100 0.03590 = 0.06688 0.02183 0.01350 0.01254 AFIX 43 H63 2 0.703850 0.263135 0.265960 11.00000 -1.20000 AFIX 0 C64 1 0.542516 0.198349 0.219663 11.00000 0.03058 0.03512 = 0.05222 0.01646 0.01149 0.01321 AFIX 43 H64 2 0.537665 0.223400 0.270931 11.00000 -1.20000 AFIX 0 C65 1 0.337938 0.140405 0.256732 11.00000 0.03382 0.04187 = 0.04237 0.00983 0.01676 0.00695 C66 1 0.316881 0.215908 0.295686 11.00000 0.03638 0.05718 = 0.05925 -0.00199 0.01958 0.00868 AFIX 43 H66 2 0.294017 0.252813 0.263999 11.00000 -1.20000 AFIX 0 C67 1 0.329211 0.236119 0.378616 11.00000 0.04841 0.08836 = 0.06322 -0.00879 0.03220 0.01014 AFIX 43 H67 2 0.312643 0.285223 0.403165 11.00000 -1.20000 AFIX 0 C68 1 0.367128 0.182786 0.427720 11.00000 0.04683 0.12073 = 0.03907 0.00188 0.01989 -0.01032 AFIX 43 H68 2 0.378582 0.198425 0.485546 11.00000 -1.20000 AFIX 0 C69 1 0.387482 0.107084 0.390331 11.00000 0.05635 0.08434 = 0.04145 0.02130 0.01271 0.00305 AFIX 43 H69 2 0.411485 0.070945 0.422402 11.00000 -1.20000 AFIX 0 C70 1 0.371709 0.085831 0.304754 11.00000 0.05966 0.06076 = 0.04339 0.01946 0.01674 0.01325 AFIX 43 H70 2 0.383900 0.034200 0.278955 11.00000 -1.20000 AFIX 0 C71 1 0.071160 0.006644 0.054127 11.00000 0.02358 0.03291 = 0.03604 0.01489 0.01369 0.01348 AFIX 13 H71 2 0.107227 0.065586 0.104432 11.00000 -1.20000 AFIX 0 C72 1 -0.051491 -0.034714 0.030729 11.00000 0.02530 0.03330 = 0.03582 0.01504 0.01484 0.01512 AFIX 13 H72 2 -0.082453 -0.104630 0.018522 11.00000 -1.20000 AFIX 0 C73 1 -0.082322 0.018735 0.094357 11.00000 0.02647 0.03790 = 0.03637 0.02024 0.01475 0.01877 C74 1 -0.181910 -0.033642 0.105999 11.00000 0.02529 0.04191 = 0.03102 0.01716 0.01232 0.01785 C75 1 -0.219833 0.021612 0.151257 11.00000 0.03032 0.04238 = 0.03699 0.01211 0.01570 0.01699 AFIX 43 H75 2 -0.184202 0.088496 0.172325 11.00000 -1.20000 AFIX 0 C76 1 -0.310259 -0.022428 0.165075 11.00000 0.03402 0.05551 = 0.03639 0.01569 0.01896 0.02353 AFIX 43 H76 2 -0.337029 0.014370 0.193664 11.00000 -1.20000 AFIX 0 C77 1 -0.359672 -0.121424 0.135791 11.00000 0.02559 0.05482 = 0.04209 0.02540 0.02197 0.02036 C78 1 -0.325483 -0.178601 0.089743 11.00000 0.03257 0.04399 = 0.04588 0.02477 0.02149 0.01970 AFIX 43 H78 2 -0.361738 -0.245428 0.068842 11.00000 -1.20000 AFIX 0 C79 1 -0.235518 -0.133670 0.075464 11.00000 0.03669 0.03961 = 0.04347 0.02388 0.02324 0.02233 AFIX 43 H79 2 -0.210725 -0.170928 0.045073 11.00000 -1.20000 AFIX 0 C80 1 0.131590 -0.057303 0.067286 11.00000 0.02774 0.03654 = 0.02936 0.01480 0.01281 0.01673 C81 1 0.244560 -0.015968 0.101431 11.00000 0.02680 0.03421 = 0.03177 0.01309 0.01219 0.01498 C82 1 0.300439 -0.076206 0.108162 11.00000 0.02747 0.03853 = 0.05134 0.01908 0.01486 0.01955 AFIX 43 H82 2 0.374958 -0.049228 0.129507 11.00000 -1.20000 AFIX 0 C83 1 0.245519 -0.175291 0.083303 11.00000 0.03752 0.04003 = 0.04808 0.01767 0.01617 0.02531 AFIX 43 H83 2 0.283022 -0.214608 0.086660 11.00000 -1.20000 AFIX 0 C84 1 0.135512 -0.215396 0.053668 11.00000 0.03739 0.03034 = 0.04083 0.01214 0.01616 0.01386 AFIX 43 H84 2 0.098919 -0.281408 0.040267 11.00000 -1.20000 AFIX 0 C85 1 0.079178 -0.157357 0.043778 11.00000 0.02761 0.03420 = 0.04037 0.01226 0.01363 0.01417 AFIX 43 H85 2 0.004591 -0.185754 0.020910 11.00000 -1.20000 AFIX 0 HKLF 4 REM glj-p_a.res in P-1 REM wR2 = 0.1573, GooF = S = 1.038, Restrained GooF = 1.038 for all data REM R1 = 0.0534 for 9761 Fo > 4sig(Fo) and 0.0753 for all 12906 data REM 830 parameters refined using 0 restraints END WGHT 0.0791 2.4212 REM Highest difference peak 1.416, deepest hole -1.099, 1-sigma level 0.084 Q1 1 0.8766 0.6372 0.1873 11.00000 0.05 1.42 Q2 1 1.4271 0.7809 0.3168 11.00000 0.05 1.04 Q3 1 0.6066 0.4535 0.6922 11.00000 0.05 0.85 Q4 1 -0.3913 -0.1652 0.2027 11.00000 0.05 0.49 Q5 1 0.2847 0.1824 0.1186 11.00000 0.05 0.48 Q6 1 1.4459 0.8049 0.2525 11.00000 0.05 0.48 Q7 1 1.4527 0.8371 0.2974 11.00000 0.05 0.46 ; _shelx_res_checksum 83553 _shelx_fab_file ; -17 1 8 0.1121 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-11 5 0.0684 0.0110 12 -11 6 -0.0038 0.0053 12 -11 7 -0.0211 0.0037 12 -11 8 -0.0209 0.0077 12 -11 9 0.0188 0.0066 12 -11 10 0.0714 -0.0011 12 -10 0 0.5940 0.0016 12 -10 1 0.6455 -0.0016 12 -10 2 0.2903 0.0029 12 -10 3 -0.0813 0.0112 12 -10 4 -0.1725 0.0133 12 -10 5 -0.0760 0.0112 12 -10 6 -0.0067 0.0123 12 -10 7 0.0163 0.0134 12 -10 8 0.0849 0.0072 12 -10 9 0.1779 -0.0012 12 -10 10 0.1951 -0.0031 12 -9 0 -0.0177 0.0054 12 -9 1 -0.4487 0.0106 12 -9 2 -0.5614 0.0137 12 -9 3 -0.3548 0.0085 12 -9 4 -0.1313 0.0020 12 -9 5 -0.0650 -0.0003 12 -9 6 -0.0610 -0.0047 12 -9 7 -0.0114 -0.0161 12 -9 8 0.0255 -0.0271 12 -9 9 -0.0381 -0.0313 12 -9 10 -0.1590 -0.0327 12 -8 0 -0.3496 0.0033 12 -8 1 -0.1622 -0.0018 12 -8 2 0.0997 -0.0109 12 -8 3 0.2201 -0.0139 12 -8 4 0.1908 -0.0116 12 -8 5 0.1231 -0.0154 12 -8 6 0.0762 -0.0266 12 -8 7 0.0298 -0.0323 12 -8 8 -0.0315 -0.0247 12 -8 9 -0.0799 -0.0087 12 -8 10 -0.0840 0.0115 12 -7 0 0.2394 -0.0115 12 -7 1 0.3591 -0.0126 12 -7 2 0.4112 -0.0045 12 -7 3 0.3571 0.0028 12 -7 4 0.1946 -0.0030 12 -7 5 0.0510 -0.0125 12 -7 6 0.0514 -0.0061 12 -7 7 0.1386 0.0177 12 -7 8 0.1588 0.0424 12 -7 9 0.0898 0.0557 12 -7 10 0.0523 0.0542 12 -6 0 0.0856 0.0030 12 -6 1 0.1723 0.0130 12 -6 2 -0.0236 0.0122 12 -6 3 -0.4160 -0.0022 12 -6 4 -0.5704 -0.0083 12 -6 5 -0.3356 0.0094 12 -6 6 -0.0936 0.0344 12 -6 7 -0.1775 0.0401 12 -6 8 -0.3910 0.0215 12 -6 9 -0.3645 -0.0082 12 -6 10 -0.1088 -0.0372 12 -5 0 -0.0041 0.0099 12 -5 1 -0.5716 -0.0015 12 -5 2 -1.0365 -0.0165 12 -5 3 -0.7724 -0.0109 12 -5 4 -0.0775 0.0126 12 -5 5 0.1960 0.0225 12 -5 6 -0.1027 0.0018 12 -5 7 -0.2826 -0.0305 12 -5 8 0.0548 -0.0480 12 -5 9 0.4672 -0.0446 12 -5 10 0.4392 -0.0269 12 -4 0 -0.8797 -0.0134 12 -4 1 -0.7223 -0.0163 12 -4 2 0.3502 0.0019 12 -4 3 1.2447 0.0201 12 -4 4 1.0716 0.0108 12 -4 5 0.4239 -0.0170 12 -4 6 0.3802 -0.0290 12 -4 7 0.8521 -0.0125 12 -4 8 0.8921 0.0134 12 -4 9 0.2637 0.0297 12 -3 0 0.3438 -0.0013 12 -3 1 1.6096 0.0162 12 -3 2 1.7100 0.0177 12 -3 3 0.5935 -0.0028 12 -3 4 -0.2684 -0.0174 12 -3 5 -0.0778 -0.0037 12 -3 6 0.2178 0.0213 12 -3 7 -0.3463 0.0280 12 -3 8 -1.1705 0.0140 12 -3 9 -1.1544 -0.0012 12 -2 0 1.7183 0.0155 12 -2 1 0.5589 0.0021 12 -2 2 -0.9544 -0.0144 12 -2 3 -1.2573 -0.0100 12 -2 4 -0.6229 0.0092 12 -2 5 -0.5720 0.0131 12 -2 6 -1.2984 -0.0072 12 -2 7 -1.3973 -0.0265 12 -2 8 -0.2840 -0.0239 12 -1 0 -0.8357 -0.0106 12 -1 1 -1.5507 -0.0106 12 -1 2 -0.8882 0.0050 12 -1 3 -0.1585 0.0123 12 -1 4 -0.4645 -0.0034 12 -1 5 -0.8323 -0.0208 12 -1 6 0.1119 -0.0125 12 -1 7 1.6313 0.0136 12 -1 8 1.8415 0.0267 12 0 0 -1.3685 0.0013 12 0 1 -0.4720 0.0131 12 0 2 -0.2893 0.0041 12 0 3 -0.7181 -0.0129 12 0 4 -0.2493 -0.0078 12 0 5 1.3358 0.0190 12 0 6 2.0948 0.0328 12 0 7 0.7865 0.0140 12 1 0 -0.3143 0.0071 12 1 2 -0.0950 -0.0170 12 1 3 1.2722 0.0031 12 1 4 2.4725 0.0193 12 1 5 1.6104 0.0014 12 1 6 -0.7569 -0.0329 12 2 0 1.1762 -0.0159 12 2 1 2.1422 -0.0068 12 2 3 2.5669 0.0096 12 2 4 0.0465 -0.0210 12 2 5 -2.1563 -0.0338 12 2 6 -1.7848 -0.0051 12 3 0 2.2010 0.0113 12 3 1 1.5022 0.0225 12 3 2 -0.7833 0.0049 12 3 3 -3.2783 -0.0163 12 3 4 -3.5953 -0.0010 12 3 5 -1.3993 0.0376 12 4 0 -2.0710 0.0098 12 4 1 -3.8905 -0.0111 12 4 2 -4.1750 -0.0183 12 4 3 -2.0824 0.0076 12 4 4 0.8026 0.0287 12 5 0 -2.1598 -0.0272 12 5 1 -0.4827 -0.0217 12 5 2 2.0214 0.0047 12 6 0 2.1906 0.0021 13 -17 0 0.2192 -0.0068 13 -17 1 0.1472 -0.0474 13 -16 0 -0.1265 -0.0350 13 -16 1 -0.1074 -0.0160 13 -16 2 -0.1587 0.0310 13 -16 3 -0.2950 0.0681 13 -16 4 -0.3512 0.0742 13 -15 0 -0.1659 0.0474 13 -15 1 -0.1705 0.0649 13 -15 2 -0.1530 0.0552 13 -15 3 -0.0468 0.0246 13 -15 4 0.1088 -0.0056 13 -15 5 0.1696 -0.0317 13 -14 0 0.2210 0.0050 13 -14 1 0.2895 -0.0198 13 -14 2 0.2917 -0.0400 13 -14 3 0.2218 -0.0454 13 -14 4 0.1205 -0.0457 13 -14 5 0.0437 -0.0449 13 -14 6 0.0455 -0.0287 13 -14 7 0.1290 0.0054 13 -13 0 0.0643 -0.0377 13 -13 1 -0.1636 -0.0287 13 -13 2 -0.3096 -0.0152 13 -13 3 -0.2510 -0.0090 13 -13 4 -0.0832 -0.0060 13 -13 5 0.0292 0.0082 13 -13 6 0.0360 0.0279 13 -13 7 -0.0219 0.0306 13 -12 0 -0.4982 0.0117 13 -12 1 -0.3344 0.0131 13 -12 2 0.0430 0.0060 13 -12 3 0.2737 0.0022 13 -12 4 0.1904 0.0111 13 -12 5 -0.0251 0.0207 13 -12 6 -0.1463 0.0153 13 -12 7 -0.1554 0.0028 13 -12 8 -0.1345 0.0014 13 -11 0 0.3220 0.0005 13 -11 1 0.6376 -0.0050 13 -11 2 0.5053 -0.0003 13 -11 3 0.0958 0.0140 13 -11 4 -0.1609 0.0222 13 -11 5 -0.1168 0.0166 13 -11 6 0.0194 0.0098 13 -11 7 0.0722 0.0121 13 -11 8 0.0978 0.0137 13 -10 0 0.3656 0.0037 13 -10 1 -0.1005 0.0139 13 -10 2 -0.4566 0.0234 13 -10 3 -0.4004 0.0202 13 -10 4 -0.1184 0.0068 13 -10 5 0.0417 -0.0019 13 -10 6 0.0284 -0.0034 13 -10 7 0.0291 -0.0101 13 -10 8 0.1013 -0.0250 13 -10 9 0.1066 -0.0348 13 -9 0 -0.4751 0.0119 13 -9 1 -0.4446 0.0074 13 -9 2 -0.1417 -0.0067 13 -9 3 0.0866 -0.0205 13 -9 4 0.0779 -0.0227 13 -9 5 -0.0137 -0.0207 13 -9 6 -0.0193 -0.0278 13 -9 7 0.0074 -0.0383 13 -9 8 -0.0653 -0.0359 13 -9 9 -0.2066 -0.0181 13 -8 0 0.1171 -0.0135 13 -8 1 0.2958 -0.0216 13 -8 2 0.3121 -0.0209 13 -8 3 0.2505 -0.0094 13 -8 4 0.2124 -0.0034 13 -8 5 0.1892 -0.0106 13 -8 6 0.1307 -0.0132 13 -8 7 0.0499 0.0053 13 -8 8 0.0140 0.0353 13 -8 9 0.0598 0.0553 13 -7 0 0.1269 -0.0043 13 -7 1 0.1502 0.0052 13 -7 2 0.1924 0.0165 13 -7 3 0.0948 0.0121 13 -7 4 -0.1251 -0.0011 13 -7 5 -0.2504 0.0037 13 -7 6 -0.1854 0.0308 13 -7 7 -0.0702 0.0524 13 -7 8 -0.0381 0.0452 13 -6 0 -0.0476 0.0108 13 -6 1 -0.1392 0.0107 13 -6 2 -0.5600 -0.0056 13 -6 3 -0.8752 -0.0163 13 -6 4 -0.6774 0.0004 13 -6 5 -0.2126 0.0262 13 -6 6 -0.0015 0.0237 13 -6 7 -0.1002 -0.0113 13 -6 8 -0.1590 -0.0473 13 -5 0 -0.4031 -0.0073 13 -5 1 -0.8302 -0.0203 13 -5 2 -0.5763 -0.0144 13 -5 3 0.3433 0.0131 13 -5 4 1.0050 0.0261 13 -5 5 0.8554 0.0011 13 -5 6 0.4023 -0.0350 13 -5 7 0.3080 -0.0415 13 -5 8 0.4647 -0.0154 13 -4 0 -0.2349 -0.0078 13 -4 1 0.7817 0.0101 13 -4 2 1.7905 0.0308 13 -4 3 1.6461 0.0207 13 -4 4 0.5673 -0.0134 13 -4 5 -0.1989 -0.0275 13 -4 6 -0.1710 -0.0026 13 -4 7 -0.0375 0.0302 13 -3 0 1.5353 0.0220 13 -3 1 1.4733 0.0209 13 -3 2 0.0670 -0.0064 13 -3 3 -1.3791 -0.0296 13 -3 4 -1.5754 -0.0171 13 -3 5 -0.9496 0.0133 13 -3 6 -0.6795 0.0193 13 -3 7 -0.8337 -0.0054 13 -2 0 -0.1377 -0.0051 13 -2 1 -1.6861 -0.0262 13 -2 2 -2.0879 -0.0231 13 -2 3 -1.0621 0.0037 13 -2 4 -0.0197 0.0170 13 -2 5 0.1231 -0.0023 13 -2 6 0.0993 -0.0247 13 -1 0 -1.8037 -0.0190 13 -1 1 -0.9154 0.0031 13 -1 2 0.4665 0.0216 13 -1 3 0.9071 0.0110 13 -1 4 0.5416 -0.0111 13 -1 5 0.5990 -0.0073 13 -1 6 1.1422 0.0218 13 0 0 0.1741 0.0169 13 0 1 0.7826 0.0116 13 0 2 0.4306 -0.0113 13 0 3 0.0983 -0.0169 13 0 4 0.5396 0.0069 13 0 5 0.8391 0.0253 13 1 0 0.8319 -0.0070 13 1 1 0.5715 -0.0200 13 1 2 0.8408 -0.0040 13 1 3 1.3433 0.0196 13 1 4 0.8567 0.0112 13 2 0 1.0387 -0.0005 13 2 1 1.2696 0.0224 13 2 2 0.8753 0.0276 13 2 3 -0.5719 -0.0009 13 2 4 -1.8875 -0.0245 13 3 0 -0.3376 0.0200 13 3 1 -1.4575 0.0049 13 3 2 -2.6569 -0.0243 13 3 3 -2.5855 -0.0237 13 4 0 -1.8595 -0.0270 13 4 1 -1.7432 -0.0385 13 5 0 0.5683 -0.0123 14 -16 0 -0.1601 0.0446 14 -16 1 -0.1532 0.0611 14 -15 0 0.0226 0.0118 14 -15 1 0.0472 -0.0100 14 -15 2 0.0699 -0.0314 14 -15 3 0.1205 -0.0397 14 -14 0 0.1403 -0.0473 14 -14 1 0.0542 -0.0342 14 -14 2 -0.0224 -0.0189 14 -14 3 -0.0184 -0.0112 14 -14 4 0.0347 -0.0141 14 -14 5 0.0557 -0.0109 14 -13 0 -0.3140 0.0179 14 -13 1 -0.3129 0.0179 14 -13 2 -0.1180 0.0058 14 -13 3 0.0840 -0.0064 14 -13 4 0.0948 -0.0018 14 -13 5 -0.0408 0.0176 14 -13 6 -0.1350 0.0278 14 -12 0 0.0211 0.0013 14 -12 1 0.3474 -0.0139 14 -12 2 0.4258 -0.0130 14 -12 3 0.1802 0.0066 14 -12 4 -0.1016 0.0289 14 -12 5 -0.1475 0.0325 14 -12 6 -0.0268 0.0187 14 -11 0 0.4879 -0.0106 14 -11 1 0.2196 0.0085 14 -11 2 -0.1775 0.0311 14 -11 3 -0.3071 0.0400 14 -11 4 -0.1070 0.0257 14 -11 5 0.1088 0.0027 14 -11 6 0.1169 -0.0095 14 -10 0 -0.2948 0.0258 14 -10 1 -0.4551 0.0287 14 -10 2 -0.2617 0.0139 14 -10 3 0.0241 -0.0142 14 -10 4 0.0776 -0.0348 14 -10 5 -0.0717 -0.0365 14 -10 6 -0.1480 -0.0318 14 -9 0 -0.0792 -0.0043 14 -9 1 0.1499 -0.0230 14 -9 2 0.1889 -0.0403 14 -9 3 0.0341 -0.0378 14 -9 4 -0.0739 -0.0194 14 -9 5 0.0026 -0.0070 14 -9 6 0.1238 -0.0064 14 -9 7 0.1013 -0.0008 14 -8 0 0.1546 -0.0195 14 -8 1 0.0200 -0.0191 14 -8 2 -0.0055 0.0012 14 -8 3 0.1305 0.0219 14 -8 4 0.2448 0.0218 14 -8 5 0.1937 0.0127 14 -8 6 0.0545 0.0196 14 -8 7 -0.0052 0.0401 14 -7 0 -0.2498 0.0028 14 -7 1 -0.0409 0.0219 14 -7 2 0.0501 0.0243 14 -7 3 -0.1582 0.0038 14 -7 4 -0.4105 -0.0084 14 -7 5 -0.4038 0.0066 14 -7 6 -0.2005 0.0241 14 -6 0 0.0511 0.0115 14 -6 1 -0.1916 -0.0017 14 -6 2 -0.5559 -0.0237 14 -6 3 -0.4551 -0.0178 14 -6 4 0.0939 0.0107 14 -6 5 0.4811 0.0186 14 -6 6 0.3792 -0.0097 14 -5 0 -0.1421 -0.0103 14 -5 1 -0.0750 -0.0169 14 -5 2 0.6661 0.0093 14 -5 3 1.3320 0.0347 14 -5 4 1.1257 0.0201 14 -5 5 0.3296 -0.0165 14 -5 6 -0.1774 -0.0258 14 -4 0 0.5847 0.0035 14 -4 1 1.2484 0.0288 14 -4 2 1.0251 0.0286 14 -4 3 -0.2089 -0.0077 14 -4 4 -1.2700 -0.0342 14 -4 5 -1.2643 -0.0174 14 -3 0 0.4726 0.0186 14 -3 1 -0.6255 -0.0039 14 -3 2 -1.8883 -0.0358 14 -3 3 -1.9310 -0.0329 14 -3 4 -0.7768 0.0003 14 -2 0 -1.3973 -0.0224 14 -2 1 -1.5489 -0.0269 14 -2 2 -0.3313 0.0002 14 -2 3 1.1374 0.0249 14 -2 4 1.5213 0.0148 14 -1 0 -0.2462 -0.0028 14 -1 1 1.0200 0.0189 14 -1 2 1.5015 0.0161 14 -1 3 0.7777 -0.0075 14 -1 4 -0.0947 -0.0129 14 0 0 1.0529 0.0089 14 0 1 0.6320 -0.0093 14 0 2 -0.2252 -0.0196 14 0 3 -0.4691 -0.0005 14 1 0 0.2940 -0.0054 14 1 1 0.0216 0.0065 14 1 2 0.2936 0.0299 14 2 0 -0.0971 0.0233 14 2 1 -0.0597 0.0254 14 3 0 -0.6755 -0.0168 15 -14 0 -0.1461 0.0179 15 -14 1 -0.1321 0.0230 15 -14 2 -0.0520 0.0090 15 -13 0 -0.0856 0.0127 15 -13 1 0.1001 -0.0164 15 -13 2 0.2162 -0.0262 15 -13 3 0.1472 -0.0106 15 -12 0 0.3778 -0.0302 15 -12 1 0.3203 -0.0103 15 -12 2 0.0691 0.0229 15 -12 3 -0.1441 0.0490 15 -12 4 -0.1166 0.0484 15 -11 0 -0.0182 0.0276 15 -11 1 -0.2624 0.0457 15 -11 2 -0.2748 0.0424 15 -10 0 -0.2113 0.0177 15 -10 1 -0.0513 -0.0043 15 -10 2 0.0850 -0.0389 15 -10 3 0.0055 -0.0604 15 -9 0 0.0928 -0.0263 15 -9 1 0.0025 -0.0442 15 -9 2 -0.1524 -0.0347 15 -9 3 -0.1358 0.0021 15 -8 0 -0.2873 -0.0191 15 -8 1 -0.1877 0.0080 15 -8 2 0.1229 0.0415 15 -8 3 0.3456 0.0422 15 -7 0 0.0914 0.0226 15 -7 1 0.3028 0.0340 15 -7 2 0.1161 0.0033 15 -7 3 -0.2573 -0.0309 15 -6 0 0.3176 0.0125 15 -6 1 -0.0833 -0.0263 15 -6 2 -0.1992 -0.0333 15 -6 3 0.1753 0.0048 15 -5 0 -0.0631 -0.0281 15 -5 1 0.2511 -0.0032 15 -5 2 0.7141 0.0397 15 -5 3 0.5600 0.0392 15 -4 0 0.2118 0.0201 15 -4 1 0.1734 0.0361 15 -4 2 -0.6223 -0.0003 15 -3 0 -0.4297 0.0111 15 -3 1 -1.0997 -0.0296 15 -3 2 -0.9903 -0.0409 15 -2 0 -0.5047 -0.0300 15 -2 1 0.2577 -0.0111 15 -2 2 1.3120 0.0227 15 -1 0 0.6546 0.0035 15 -1 1 0.9413 0.0132 15 -1 2 0.2227 -0.0033 15 0 0 0.3695 0.0062 15 0 1 -0.3266 -0.0020 15 1 0 -0.2622 0.0185 16 -12 0 0.1516 0.0128 16 -11 0 -0.1810 0.0353 16 -11 1 -0.2131 0.0223 16 -10 0 -0.1008 -0.0155 16 -10 1 -0.0339 -0.0447 16 -9 0 -0.1564 -0.0353 16 -9 1 -0.1488 -0.0243 16 -9 2 -0.0256 0.0197 16 -8 0 0.0441 0.0070 16 -8 1 0.2856 0.0468 16 -8 2 0.4357 0.0444 16 -7 0 0.4361 0.0426 16 -7 1 0.2504 0.0046 16 -7 2 -0.1505 -0.0428 16 -6 0 -0.0595 -0.0300 16 -6 1 -0.2893 -0.0440 16 -6 2 -0.1314 0.0026 16 -5 0 -0.2703 -0.0154 16 -5 1 0.0395 0.0388 16 -4 0 0.0089 0.0459 16 -4 1 -0.1992 0.0108 16 -3 0 -0.1114 -0.0226 17 -8 0 0.2693 0.0419 17 -7 0 -0.0176 0.0046 0 0 0 0.0 0.0 ; _shelx_fab_checksum 5877 _olex2_date_sample_data_collection 2021-11-23 _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 1.727 _oxdiff_exptl_absorpt_empirical_full_min 0.444 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 Br1 Br 0.59785(5) 0.50351(5) 0.70727(3) 0.06593(18) Uani 1 1 d . . . . . Br2 Br 1.42549(4) 0.83553(4) 0.32104(3) 0.05350(14) Uani 1 1 d . . . . . P1 P 0.82610(8) 0.54370(7) 0.14910(6) 0.0337(2) Uani 1 1 d . . . . . P2 P 0.99411(7) 0.83783(6) 0.60180(6) 0.02836(19) Uani 1 1 d . . . . . O1 O 0.6604(2) 0.4246(2) 0.32879(18) 0.0425(6) Uani 1 1 d . . . . . O2 O 1.0860(2) 0.61043(19) 0.48610(17) 0.0341(6) Uani 1 1 d . . . . . C2 C 0.8997(3) 0.6459(2) 0.4529(2) 0.0242(6) Uani 1 1 d . . . . . H2 H 0.951957 0.667036 0.512613 0.029 Uiso 1 1 calc R U . . . C3 C 0.9541(3) 0.6433(2) 0.3875(2) 0.0253(6) Uani 1 1 d . . . . . H3 H 0.952599 0.691386 0.358446 0.030 Uiso 1 1 calc R U . . . C4 C 0.8628(3) 0.5386(2) 0.3318(2) 0.0263(7) Uani 1 1 d . . . . . H4 H 0.802492 0.546301 0.292011 0.032 Uiso 1 1 calc R U . . . C5 C 1.0640(3) 0.6421(2) 0.4267(2) 0.0260(7) Uani 1 1 d . . . . . C6 C 1.1466(3) 0.6814(2) 0.3934(2) 0.0275(7) Uani 1 1 d . . . . . C7 C 1.1240(3) 0.7084(3) 0.3199(2) 0.0328(7) Uani 1 1 d . . . . . H7 H 1.053762 0.697259 0.286429 0.039 Uiso 1 1 calc R U . . . C8 C 1.2065(3) 0.7522(3) 0.2965(3) 0.0409(9) Uani 1 1 d . . . . . H8 H 1.192045 0.769964 0.247193 0.049 Uiso 1 1 calc R U . . . C9 C 1.3099(3) 0.7687(3) 0.3479(3) 0.0368(8) Uani 1 1 d . . . . . C10 C 1.3342(3) 0.7397(3) 0.4199(3) 0.0382(8) Uani 1 1 d . . . . . H10 H 1.404226 0.749165 0.452208 0.046 Uiso 1 1 calc R U . . . C11 C 1.2519(3) 0.6967(3) 0.4421(3) 0.0334(8) Uani 1 1 d . . . . . H11 H 1.266784 0.677428 0.490438 0.040 Uiso 1 1 calc R U . . . C12 C 0.8338(3) 0.7050(2) 0.4414(2) 0.0257(6) Uani 1 1 d . . . . . C13 C 0.8765(3) 0.7994(2) 0.4999(2) 0.0269(7) Uani 1 1 d . . . . . C14 C 0.8216(3) 0.8585(3) 0.4820(2) 0.0313(7) Uani 1 1 d . . . . . H14 H 0.849524 0.921103 0.519732 0.038 Uiso 1 1 calc R U . . . C15 C 0.7265(3) 0.8256(3) 0.4093(2) 0.0334(8) Uani 1 1 d . . . . . H15 H 0.692853 0.866778 0.397691 0.040 Uiso 1 1 calc R U . . . C16 C 0.6822(3) 0.7322(3) 0.3545(2) 0.0336(8) Uani 1 1 d . . . . . H16 H 0.616946 0.709122 0.307171 0.040 Uiso 1 1 calc R U . . . C17 C 0.7360(3) 0.6722(3) 0.3704(2) 0.0315(7) Uani 1 1 d . . . . . H17 H 0.706044 0.609202 0.332999 0.038 Uiso 1 1 calc R U . . . C18 C 1.1069(3) 0.8671(3) 0.5699(2) 0.0296(7) Uani 1 1 d . . . . . C19 C 1.2019(3) 0.8661(3) 0.6245(2) 0.0392(9) Uani 1 1 d . . . . . H19 H 1.203313 0.845871 0.671671 0.047 Uiso 1 1 calc R U . . . C20 C 1.2941(3) 0.8949(3) 0.6090(3) 0.0448(10) Uani 1 1 d . . . . . H20 H 1.357280 0.895498 0.646541 0.054 Uiso 1 1 calc R U . . . C21 C 1.2915(3) 0.9226(3) 0.5377(3) 0.0408(9) Uani 1 1 d . . . . . H21 H 1.353552 0.943302 0.527994 0.049 Uiso 1 1 calc R U . . . C22 C 1.1973(3) 0.9198(3) 0.4808(3) 0.0354(8) Uani 1 1 d . . . . . H22 H 1.195263 0.935819 0.431611 0.042 Uiso 1 1 calc R U . . . C23 C 1.1055(3) 0.8930(2) 0.4972(2) 0.0299(7) Uani 1 1 d . . . . . H23 H 1.042625 0.892239 0.459177 0.036 Uiso 1 1 calc R U . . . C24 C 1.0082(3) 0.9580(3) 0.6585(2) 0.0293(7) Uani 1 1 d . . . . . C25 C 1.0874(3) 1.0443(3) 0.6688(2) 0.0310(7) Uani 1 1 d . . . . . H25 H 1.135501 1.043160 0.643729 0.037 Uiso 1 1 calc R U . . . C26 C 1.0957(3) 1.1323(3) 0.7163(2) 0.0353(8) Uani 1 1 d . . . . . H26 H 1.149444 1.189393 0.723025 0.042 Uiso 1 1 calc R U . . . C27 C 1.0243(4) 1.1351(3) 0.7533(3) 0.0406(9) Uani 1 1 d . . . . . H27 H 1.029959 1.194017 0.784987 0.049 Uiso 1 1 calc R U . . . C28 C 0.9439(3) 1.0498(3) 0.7432(3) 0.0417(9) Uani 1 1 d . . . . . H28 H 0.894891 1.051605 0.767230 0.050 Uiso 1 1 calc R U . . . C29 C 0.9367(3) 0.9615(3) 0.6972(2) 0.0378(8) Uani 1 1 d . . . . . H29 H 0.884156 0.904510 0.692024 0.045 Uiso 1 1 calc R U . . . C30 C 0.7286(3) 0.4774(3) 0.4006(2) 0.0300(7) Uani 1 1 d . . . . . C31 C 0.8416(3) 0.5329(2) 0.4127(2) 0.0250(6) Uani 1 1 d . . . . . H31 H 0.887743 0.505544 0.444446 0.030 Uiso 1 1 calc R U . . . C32 C 0.7010(3) 0.4861(3) 0.4775(2) 0.0312(7) Uani 1 1 d . . . . . C33 C 0.7768(3) 0.5418(3) 0.5605(2) 0.0371(8) Uani 1 1 d . . . . . H33 H 0.847592 0.576067 0.569935 0.045 Uiso 1 1 calc R U . . . C34 C 0.7475(4) 0.5468(4) 0.6301(3) 0.0455(10) Uani 1 1 d . . . . . H34 H 0.798152 0.584574 0.685728 0.055 Uiso 1 1 calc R U . . . C35 C 0.6420(4) 0.4947(3) 0.6151(3) 0.0447(10) Uani 1 1 d . . . . . C36 C 0.5662(3) 0.4373(3) 0.5328(3) 0.0392(9) Uani 1 1 d . . . . . H36 H 0.495869 0.401923 0.523738 0.047 Uiso 1 1 calc R U . . . C37 C 0.5955(3) 0.4326(3) 0.4642(3) 0.0343(8) Uani 1 1 d . . . . . H37 H 0.544753 0.393661 0.408902 0.041 Uiso 1 1 calc R U . . . C38 C 0.8857(3) 0.4643(2) 0.2800(2) 0.0253(6) Uani 1 1 d . . . . . C39 C 0.9241(3) 0.4026(3) 0.3148(2) 0.0286(7) Uani 1 1 d . . . . . H39 H 0.934377 0.406355 0.371273 0.034 Uiso 1 1 calc R U . . . C40 C 0.9477(3) 0.3351(3) 0.2669(2) 0.0303(7) Uani 1 1 d . . . . . H40 H 0.974623 0.295389 0.291827 0.036 Uiso 1 1 calc R U . . . C41 C 0.9307(3) 0.3277(3) 0.1824(2) 0.0340(8) Uani 1 1 d . . . . . H41 H 0.945826 0.282676 0.150025 0.041 Uiso 1 1 calc R U . . . C42 C 0.8911(3) 0.3879(3) 0.1462(2) 0.0309(7) Uani 1 1 d . . . . . H42 H 0.879618 0.382287 0.089174 0.037 Uiso 1 1 calc R U . . . C43 C 0.8681(3) 0.4566(2) 0.1930(2) 0.0274(7) Uani 1 1 d . . . . . C44 C 0.8147(3) 0.5066(3) 0.0379(3) 0.0395(9) Uani 1 1 d . . . . . C45 C 0.7312(4) 0.4298(3) -0.0296(3) 0.0426(9) Uani 1 1 d . . . . . H45 H 0.674924 0.391425 -0.019691 0.051 Uiso 1 1 calc R U . . . C46 C 0.7280(4) 0.4076(3) -0.1122(3) 0.0470(10) Uani 1 1 d . . . . . H46 H 0.670338 0.354807 -0.156408 0.056 Uiso 1 1 calc R U . . . C47 C 0.8078(5) 0.4619(5) -0.1285(4) 0.0790(19) Uani 1 1 d . . . . . H47 H 0.819391 0.439555 -0.176932 0.095 Uiso 0.565(14) 1 calc R U P A 1 H47A H 0.796771 0.470385 -0.181745 0.095 Uiso 0.435(14) 1 calc R U P A 2 C48 C 0.8756(8) 0.5590(8) -0.0651(5) 0.061(4) Uani 0.565(14) 1 d . . P A 1 H48 H 0.916224 0.607155 -0.080005 0.074 Uiso 0.565(14) 1 calc R U P A 1 C49 C 0.8782(7) 0.5778(7) 0.0168(5) 0.048(3) Uani 0.565(14) 1 d . . P A 1 H49 H 0.922655 0.638358 0.058079 0.057 Uiso 0.565(14) 1 calc R U P A 1 C50 C 0.9143(13) 0.5074(11) -0.0555(10) 0.070(5) Uani 0.435(14) 1 d . . P A 2 H50 H 0.976695 0.515873 -0.064125 0.085 Uiso 0.435(14) 1 calc R U P A 2 C51 C 0.9172(10) 0.5368(10) 0.0264(8) 0.052(3) Uani 0.435(14) 1 d . . P A 2 H51 H 0.982197 0.574839 0.073565 0.063 Uiso 0.435(14) 1 calc R U P A 2 C52 C 0.6853(3) 0.5058(3) 0.1327(2) 0.0320(7) Uani 1 1 d . . . . . C53 C 0.6426(4) 0.5747(3) 0.1292(3) 0.0448(10) Uani 1 1 d . . . . . H53 H 0.686091 0.636994 0.135858 0.054 Uiso 1 1 calc R U . . . C54 C 0.5364(4) 0.5521(4) 0.1161(3) 0.0520(11) Uani 1 1 d . . . . . H54 H 0.508349 0.598395 0.111947 0.062 Uiso 1 1 calc R U . . . C55 C 0.4722(4) 0.4608(4) 0.1091(3) 0.0473(10) Uani 1 1 d . . . . . H55 H 0.401114 0.445965 0.101003 0.057 Uiso 1 1 calc R U . . . C56 C 0.5126(4) 0.3920(4) 0.1141(3) 0.0482(10) Uani 1 1 d . . . . . H56 H 0.469233 0.330813 0.109896 0.058 Uiso 1 1 calc R U . . . C57 C 0.6192(3) 0.4139(3) 0.1254(3) 0.0408(9) Uani 1 1 d . . . . . H57 H 0.646171 0.366767 0.128148 0.049 Uiso 1 1 calc R U . . . Br3 Br -0.47998(4) -0.18092(4) 0.15916(3) 0.05139(14) Uani 1 1 d . . . . . P3 P 0.31527(7) 0.11706(7) 0.14265(6) 0.0323(2) Uani 1 1 d . . . . . O3 O -0.0298(2) 0.1051(2) 0.13328(17) 0.0373(6) Uani 1 1 d . . . . . C59 C 0.4494(3) 0.1371(3) 0.1469(3) 0.0339(8) Uani 1 1 d . . . . . C60 C 0.4588(3) 0.1013(3) 0.0703(3) 0.0408(9) Uani 1 1 d . . . . . H60 H 0.397632 0.060395 0.020817 0.049 Uiso 1 1 calc R U . . . C61 C 0.5599(4) 0.1268(4) 0.0680(3) 0.0476(10) Uani 1 1 d . . . . . H61 H 0.565905 0.103267 0.016927 0.057 Uiso 1 1 calc R U . . . C62 C 0.6500(3) 0.1863(3) 0.1409(3) 0.0480(11) Uani 1 1 d . . . . . H62 H 0.717113 0.202568 0.139281 0.058 Uiso 1 1 calc R U . . . C63 C 0.6422(3) 0.2225(3) 0.2168(3) 0.0459(10) Uani 1 1 d . . . . . H63 H 0.703850 0.263135 0.265960 0.055 Uiso 1 1 calc R U . . . C64 C 0.5425(3) 0.1983(3) 0.2197(3) 0.0405(9) Uani 1 1 d . . . . . H64 H 0.537665 0.223400 0.270931 0.049 Uiso 1 1 calc R U . . . C65 C 0.3379(3) 0.1404(3) 0.2567(3) 0.0420(9) Uani 1 1 d . . . . . C66 C 0.3169(4) 0.2159(4) 0.2957(3) 0.0573(13) Uani 1 1 d . . . . . H66 H 0.294017 0.252813 0.263999 0.069 Uiso 1 1 calc R U . . . C67 C 0.3292(4) 0.2361(5) 0.3786(4) 0.0745(19) Uani 1 1 d . . . . . H67 H 0.312643 0.285223 0.403165 0.089 Uiso 1 1 calc R U . . . C68 C 0.3671(5) 0.1828(6) 0.4277(3) 0.084(2) Uani 1 1 d . . . . . H68 H 0.378582 0.198425 0.485546 0.101 Uiso 1 1 calc R U . . . C69 C 0.3875(5) 0.1071(5) 0.3903(3) 0.0695(16) Uani 1 1 d . . . . . H69 H 0.411485 0.070945 0.422402 0.083 Uiso 1 1 calc R U . . . C70 C 0.3717(4) 0.0858(4) 0.3048(3) 0.0585(13) Uani 1 1 d . . . . . H70 H 0.383900 0.034200 0.278955 0.070 Uiso 1 1 calc R U . . . C71 C 0.0712(3) 0.0066(3) 0.0541(2) 0.0293(7) Uani 1 1 d . . . . . H71 H 0.107227 0.065586 0.104432 0.035 Uiso 1 1 calc R U . . . C72 C -0.0515(3) -0.0347(3) 0.0307(2) 0.0294(7) Uani 1 1 d . . . . . H72 H -0.082453 -0.104630 0.018522 0.035 Uiso 1 1 calc R U . . . C73 C -0.0823(3) 0.0187(3) 0.0944(2) 0.0302(7) Uani 1 1 d . . . . . C74 C -0.1819(3) -0.0336(3) 0.1060(2) 0.0305(7) Uani 1 1 d . . . . . C75 C -0.2198(3) 0.0216(3) 0.1513(2) 0.0356(8) Uani 1 1 d . . . . . H75 H -0.184202 0.088496 0.172325 0.043 Uiso 1 1 calc R U . . . C76 C -0.3103(3) -0.0224(3) 0.1651(2) 0.0392(9) Uani 1 1 d . . . . . H76 H -0.337029 0.014370 0.193664 0.047 Uiso 1 1 calc R U . . . C77 C -0.3597(3) -0.1214(3) 0.1358(2) 0.0360(8) Uani 1 1 d . . . . . C78 C -0.3255(3) -0.1786(3) 0.0897(3) 0.0366(8) Uani 1 1 d . . . . . H78 H -0.361738 -0.245428 0.068842 0.044 Uiso 1 1 calc R U . . . C79 C -0.2355(3) -0.1337(3) 0.0755(2) 0.0345(8) Uani 1 1 d . . . . . H79 H -0.210725 -0.170928 0.045073 0.041 Uiso 1 1 calc R U . . . C80 C 0.1316(3) -0.0573(3) 0.0673(2) 0.0293(7) Uani 1 1 d . . . . . C81 C 0.2446(3) -0.0160(3) 0.1014(2) 0.0298(7) Uani 1 1 d . . . . . C82 C 0.3004(3) -0.0762(3) 0.1082(3) 0.0371(8) Uani 1 1 d . . . . . H82 H 0.374958 -0.049228 0.129507 0.045 Uiso 1 1 calc R U . . . C83 C 0.2455(3) -0.1753(3) 0.0833(3) 0.0392(9) Uani 1 1 d . . . . . H83 H 0.283022 -0.214608 0.086660 0.047 Uiso 1 1 calc R U . . . C84 C 0.1355(3) -0.2154(3) 0.0537(2) 0.0361(8) Uani 1 1 d . . . . . H84 H 0.098919 -0.281408 0.040267 0.043 Uiso 1 1 calc R U . . . C85 C 0.0792(3) -0.1574(3) 0.0438(2) 0.0337(8) Uani 1 1 d . . . . . H85 H 0.004591 -0.185754 0.020910 0.040 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.0636(3) 0.1070(5) 0.0555(3) 0.0428(3) 0.0428(3) 0.0412(3) Br2 0.0376(2) 0.0706(3) 0.0571(3) 0.0258(2) 0.0295(2) 0.0149(2) P1 0.0403(5) 0.0318(5) 0.0366(5) 0.0191(4) 0.0178(4) 0.0173(4) P2 0.0334(5) 0.0258(4) 0.0299(4) 0.0114(3) 0.0129(4) 0.0158(4) O1 0.0382(15) 0.0405(16) 0.0386(15) 0.0058(12) 0.0175(13) 0.0058(13) O2 0.0320(13) 0.0379(14) 0.0441(14) 0.0246(12) 0.0177(12) 0.0199(11) C2 0.0262(16) 0.0227(15) 0.0270(16) 0.0089(13) 0.0108(13) 0.0140(13) C3 0.0248(16) 0.0248(16) 0.0320(17) 0.0139(13) 0.0124(14) 0.0135(13) C4 0.0283(17) 0.0244(16) 0.0290(16) 0.0109(13) 0.0122(14) 0.0125(14) C5 0.0278(17) 0.0210(15) 0.0303(16) 0.0081(13) 0.0120(14) 0.0113(13) C6 0.0290(17) 0.0250(16) 0.0330(17) 0.0096(14) 0.0148(15) 0.0145(14) C7 0.0262(18) 0.039(2) 0.0297(17) 0.0095(15) 0.0093(15) 0.0123(15) C8 0.038(2) 0.055(3) 0.0341(19) 0.0173(18) 0.0185(17) 0.0174(19) C9 0.0331(19) 0.041(2) 0.043(2) 0.0124(17) 0.0241(17) 0.0161(17) C10 0.0290(19) 0.040(2) 0.052(2) 0.0183(18) 0.0182(17) 0.0184(16) C11 0.0316(19) 0.0332(18) 0.043(2) 0.0174(16) 0.0155(16) 0.0191(16) C12 0.0282(17) 0.0251(16) 0.0343(17) 0.0135(14) 0.0180(14) 0.0162(14) C13 0.0291(17) 0.0263(16) 0.0329(17) 0.0137(14) 0.0170(14) 0.0139(14) C14 0.0347(19) 0.0265(17) 0.0386(19) 0.0114(15) 0.0170(16) 0.0174(15) C15 0.0313(19) 0.0359(19) 0.044(2) 0.0181(16) 0.0172(16) 0.0216(16) C16 0.0286(18) 0.037(2) 0.0379(19) 0.0131(16) 0.0105(16) 0.0187(16) C17 0.0299(18) 0.0286(18) 0.0397(19) 0.0109(15) 0.0152(16) 0.0158(15) C18 0.0317(18) 0.0284(17) 0.0309(17) 0.0075(14) 0.0117(15) 0.0174(15) C19 0.038(2) 0.048(2) 0.0344(19) 0.0133(17) 0.0113(17) 0.0251(19) C20 0.037(2) 0.058(3) 0.040(2) 0.0114(19) 0.0099(18) 0.028(2) C21 0.035(2) 0.034(2) 0.053(2) 0.0071(17) 0.0197(18) 0.0149(17) C22 0.043(2) 0.0264(17) 0.043(2) 0.0109(15) 0.0205(18) 0.0181(16) C23 0.0307(18) 0.0262(17) 0.0333(18) 0.0096(14) 0.0110(15) 0.0147(14) C24 0.0325(18) 0.0313(18) 0.0280(17) 0.0123(14) 0.0119(15) 0.0166(15) C25 0.0364(19) 0.0324(18) 0.0289(17) 0.0140(14) 0.0122(15) 0.0186(16) C26 0.041(2) 0.0262(17) 0.0353(19) 0.0108(15) 0.0097(16) 0.0146(16) C27 0.051(2) 0.036(2) 0.036(2) 0.0091(16) 0.0130(18) 0.0266(19) C28 0.040(2) 0.051(2) 0.036(2) 0.0078(18) 0.0137(18) 0.026(2) C29 0.035(2) 0.041(2) 0.0356(19) 0.0116(16) 0.0129(17) 0.0166(17) C30 0.0287(18) 0.0266(17) 0.040(2) 0.0121(15) 0.0171(16) 0.0140(15) C31 0.0279(17) 0.0230(15) 0.0285(16) 0.0097(13) 0.0137(14) 0.0129(13) C32 0.0371(19) 0.0316(18) 0.0386(19) 0.0176(15) 0.0216(16) 0.0211(16) C33 0.033(2) 0.042(2) 0.038(2) 0.0135(17) 0.0185(17) 0.0137(17) C34 0.040(2) 0.062(3) 0.036(2) 0.0174(19) 0.0180(18) 0.020(2) C35 0.052(3) 0.057(3) 0.052(2) 0.033(2) 0.035(2) 0.033(2) C36 0.033(2) 0.049(2) 0.052(2) 0.0269(19) 0.0245(18) 0.0238(18) C37 0.0278(18) 0.038(2) 0.041(2) 0.0165(16) 0.0144(16) 0.0169(16) C38 0.0219(15) 0.0241(16) 0.0315(17) 0.0103(13) 0.0127(14) 0.0088(13) C39 0.0304(17) 0.0291(17) 0.0308(17) 0.0123(14) 0.0126(14) 0.0159(14) C40 0.0314(18) 0.0292(17) 0.0359(18) 0.0138(15) 0.0144(15) 0.0168(15) C41 0.037(2) 0.0345(19) 0.041(2) 0.0129(16) 0.0231(17) 0.0198(16) C42 0.0348(19) 0.0342(18) 0.0307(17) 0.0133(15) 0.0182(15) 0.0163(15) C43 0.0244(16) 0.0281(17) 0.0318(17) 0.0125(14) 0.0133(14) 0.0099(14) C44 0.045(2) 0.040(2) 0.038(2) 0.0200(17) 0.0205(18) 0.0140(18) C45 0.043(2) 0.046(2) 0.043(2) 0.0179(19) 0.0221(19) 0.0168(19) C46 0.058(3) 0.050(3) 0.036(2) 0.0150(19) 0.019(2) 0.025(2) C47 0.076(4) 0.103(5) 0.046(3) 0.022(3) 0.035(3) 0.012(4) C48 0.059(6) 0.069(7) 0.045(5) 0.026(4) 0.030(4) 0.000(5) C49 0.041(5) 0.049(5) 0.042(4) 0.016(4) 0.015(4) 0.004(4) C50 0.087(10) 0.074(9) 0.099(10) 0.051(8) 0.078(9) 0.040(8) C51 0.037(6) 0.066(8) 0.059(7) 0.033(6) 0.026(5) 0.012(6) C52 0.041(2) 0.0322(18) 0.0306(17) 0.0148(15) 0.0150(16) 0.0219(16) C53 0.049(2) 0.038(2) 0.048(2) 0.0153(18) 0.012(2) 0.0246(19) C54 0.054(3) 0.055(3) 0.052(3) 0.013(2) 0.014(2) 0.039(2) C55 0.041(2) 0.072(3) 0.042(2) 0.021(2) 0.0197(19) 0.034(2) C56 0.040(2) 0.054(3) 0.056(3) 0.029(2) 0.021(2) 0.019(2) C57 0.043(2) 0.040(2) 0.054(2) 0.0257(19) 0.0234(19) 0.0251(19) Br3 0.0392(2) 0.0658(3) 0.0690(3) 0.0351(3) 0.0368(2) 0.0230(2) P3 0.0263(4) 0.0328(5) 0.0398(5) 0.0140(4) 0.0130(4) 0.0141(4) O3 0.0345(14) 0.0374(15) 0.0433(15) 0.0150(12) 0.0187(12) 0.0148(12) C59 0.0266(18) 0.0362(19) 0.045(2) 0.0217(17) 0.0142(16) 0.0160(15) C60 0.036(2) 0.048(2) 0.048(2) 0.0227(19) 0.0194(18) 0.0227(19) C61 0.044(2) 0.057(3) 0.061(3) 0.034(2) 0.029(2) 0.028(2) C62 0.030(2) 0.043(2) 0.087(3) 0.037(2) 0.029(2) 0.0196(18) C63 0.031(2) 0.036(2) 0.067(3) 0.022(2) 0.013(2) 0.0125(17) C64 0.031(2) 0.035(2) 0.052(2) 0.0165(18) 0.0115(18) 0.0132(16) C65 0.034(2) 0.042(2) 0.042(2) 0.0098(18) 0.0168(18) 0.0070(17) C66 0.036(2) 0.057(3) 0.059(3) -0.002(2) 0.020(2) 0.009(2) C67 0.048(3) 0.088(4) 0.063(3) -0.009(3) 0.032(3) 0.010(3) C68 0.047(3) 0.121(6) 0.039(3) 0.002(3) 0.020(2) -0.010(3) C69 0.056(3) 0.084(4) 0.041(3) 0.021(3) 0.013(2) 0.003(3) C70 0.060(3) 0.061(3) 0.043(2) 0.019(2) 0.017(2) 0.013(2) C71 0.0236(16) 0.0329(18) 0.0360(18) 0.0149(15) 0.0137(15) 0.0135(14) C72 0.0253(17) 0.0333(18) 0.0358(18) 0.0150(15) 0.0148(15) 0.0151(14) C73 0.0265(17) 0.038(2) 0.0364(18) 0.0202(16) 0.0147(15) 0.0188(15) C74 0.0253(17) 0.042(2) 0.0310(17) 0.0172(15) 0.0123(14) 0.0179(16) C75 0.0303(19) 0.042(2) 0.0370(19) 0.0121(16) 0.0157(16) 0.0170(17) C76 0.034(2) 0.056(3) 0.036(2) 0.0157(18) 0.0190(17) 0.0235(19) C77 0.0256(18) 0.055(2) 0.042(2) 0.0254(18) 0.0220(16) 0.0204(17) C78 0.0326(19) 0.044(2) 0.046(2) 0.0248(18) 0.0215(17) 0.0197(17) C79 0.037(2) 0.040(2) 0.043(2) 0.0239(17) 0.0232(17) 0.0223(17) C80 0.0277(17) 0.0365(19) 0.0294(17) 0.0148(15) 0.0128(14) 0.0167(15) C81 0.0268(17) 0.0342(18) 0.0318(17) 0.0131(15) 0.0122(15) 0.0150(15) C82 0.0275(18) 0.039(2) 0.051(2) 0.0191(18) 0.0149(17) 0.0195(16) C83 0.038(2) 0.040(2) 0.048(2) 0.0177(18) 0.0162(18) 0.0253(18) C84 0.037(2) 0.0303(19) 0.041(2) 0.0121(16) 0.0162(17) 0.0139(16) C85 0.0276(18) 0.0342(19) 0.040(2) 0.0123(16) 0.0136(16) 0.0142(15) 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' Br Br -0.6763 1.2805 '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' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C44 P1 C43 103.24(17) . . ? C52 P1 C43 104.38(16) . . ? C52 P1 C44 101.87(18) . . ? C18 P2 C13 103.45(16) . . ? C18 P2 C24 102.05(16) . . ? C24 P2 C13 102.75(15) . . ? C3 C2 H2 112.0 . . ? C3 C2 C31 87.8(2) . . ? C12 C2 H2 112.0 . . ? C12 C2 C3 111.7(3) . . ? C12 C2 C31 119.2(3) . . ? C31 C2 H2 112.0 . . ? C2 C3 H3 114.0 . . ? C2 C3 C4 87.9(2) . . ? C4 C3 H3 114.0 . . ? C5 C3 C2 112.0(3) . . ? C5 C3 H3 114.0 . . ? C5 C3 C4 112.4(3) . . ? C3 C4 H4 107.4 . . ? C31 C4 C3 88.2(2) . . ? C31 C4 H4 107.4 . . ? C38 C4 C3 120.5(3) . . ? C38 C4 H4 107.4 . . ? C38 C4 C31 123.8(3) . . ? O2 C5 C3 120.4(3) . . ? O2 C5 C6 119.8(3) . . ? C6 C5 C3 119.8(3) . . ? C7 C6 C5 123.0(3) . . ? C7 C6 C11 119.4(3) . . ? C11 C6 C5 117.5(3) . . ? C6 C7 H7 119.9 . . ? C6 C7 C8 120.2(3) . . ? C8 C7 H7 119.9 . . ? C7 C8 H8 120.7 . . ? C9 C8 C7 118.5(4) . . ? C9 C8 H8 120.7 . . ? C8 C9 Br2 119.4(3) . . ? C8 C9 C10 122.5(4) . . ? C10 C9 Br2 118.1(3) . . ? C9 C10 H10 120.9 . . ? C11 C10 C9 118.1(4) . . ? C11 C10 H10 120.9 . . ? C6 C11 H11 119.4 . . ? C10 C11 C6 121.3(3) . . ? C10 C11 H11 119.4 . . ? C13 C12 C2 119.0(3) . . ? C17 C12 C2 121.9(3) . . ? C17 C12 C13 118.9(3) . . ? C12 C13 P2 119.6(2) . . ? C14 C13 P2 121.6(3) . . ? C14 C13 C12 118.5(3) . . ? C13 C14 H14 119.2 . . ? C15 C14 C13 121.5(3) . . ? C15 C14 H14 119.2 . . ? C14 C15 H15 120.0 . . ? C16 C15 C14 120.0(3) . . ? C16 C15 H15 120.0 . . ? C15 C16 H16 120.3 . . ? C15 C16 C17 119.5(3) . . ? C17 C16 H16 120.3 . . ? C12 C17 C16 121.4(3) . . ? C12 C17 H17 119.3 . . ? C16 C17 H17 119.3 . . ? C19 C18 P2 117.0(3) . . ? C23 C18 P2 124.7(3) . . ? C23 C18 C19 118.3(3) . . ? C18 C19 H19 119.6 . . ? C20 C19 C18 120.9(4) . . ? C20 C19 H19 119.6 . . ? C19 C20 H20 120.2 . . ? C21 C20 C19 119.7(4) . . ? C21 C20 H20 120.2 . . ? C20 C21 H21 119.8 . . ? C22 C21 C20 120.4(4) . . ? C22 C21 H21 119.8 . . ? C21 C22 H22 120.0 . . ? C21 C22 C23 120.0(4) . . ? C23 C22 H22 120.0 . . ? C18 C23 H23 119.7 . . ? C22 C23 C18 120.6(3) . . ? C22 C23 H23 119.7 . . ? C25 C24 P2 124.5(3) . . ? C25 C24 C29 118.5(3) . . ? C29 C24 P2 116.9(3) . . ? C24 C25 H25 119.6 . . ? C24 C25 C26 120.9(4) . . ? C26 C25 H25 119.6 . . ? C25 C26 H26 119.9 . . ? C27 C26 C25 120.2(4) . . ? C27 C26 H26 119.9 . . ? C26 C27 H27 120.0 . . ? C26 C27 C28 119.9(4) . . ? C28 C27 H27 120.0 . . ? C27 C28 H28 120.0 . . ? C27 C28 C29 120.0(4) . . ? C29 C28 H28 120.0 . . ? C24 C29 H29 119.8 . . ? C28 C29 C24 120.5(4) . . ? C28 C29 H29 119.8 . . ? O1 C30 C31 120.0(3) . . ? O1 C30 C32 120.5(3) . . ? C32 C30 C31 119.4(3) . . ? C2 C31 H31 108.2 . . ? C4 C31 C2 89.5(2) . . ? C4 C31 H31 108.2 . . ? C30 C31 C2 122.9(3) . . ? C30 C31 C4 118.2(3) . . ? C30 C31 H31 108.2 . . ? C33 C32 C30 122.5(3) . . ? C33 C32 C37 119.4(3) . . ? C37 C32 C30 118.1(3) . . ? C32 C33 H33 119.8 . . ? C32 C33 C34 120.4(4) . . ? C34 C33 H33 119.8 . . ? C33 C34 H34 120.5 . . ? C35 C34 C33 119.1(4) . . ? C35 C34 H34 120.5 . . ? C34 C35 Br1 120.3(4) . . ? C36 C35 Br1 118.6(3) . . ? C36 C35 C34 121.1(4) . . ? C35 C36 H36 120.2 . . ? C37 C36 C35 119.7(4) . . ? C37 C36 H36 120.2 . . ? C32 C37 H37 119.8 . . ? C36 C37 C32 120.4(4) . . ? C36 C37 H37 119.8 . . ? C39 C38 C4 121.8(3) . . ? C39 C38 C43 118.8(3) . . ? C43 C38 C4 119.4(3) . . ? C38 C39 H39 119.2 . . ? C38 C39 C40 121.5(3) . . ? C40 C39 H39 119.2 . . ? C39 C40 H40 120.1 . . ? C41 C40 C39 119.7(3) . . ? C41 C40 H40 120.1 . . ? C40 C41 H41 120.2 . . ? C40 C41 C42 119.6(3) . . ? C42 C41 H41 120.2 . . ? C41 C42 H42 119.1 . . ? C41 C42 C43 121.7(3) . . ? C43 C42 H42 119.1 . . ? C38 C43 P1 118.8(3) . . ? C42 C43 P1 122.3(3) . . ? C42 C43 C38 118.7(3) . . ? C45 C44 P1 125.7(3) . . ? C45 C44 C49 116.6(5) . . ? C45 C44 C51 114.0(6) . . ? C49 C44 P1 114.7(4) . . ? C51 C44 P1 116.3(5) . . ? C44 C45 H45 119.0 . . ? C44 C45 C46 122.1(4) . . ? C46 C45 H45 119.0 . . ? C45 C46 H46 119.9 . . ? C47 C46 C45 120.3(5) . . ? C47 C46 H46 119.9 . . ? C46 C47 H47 122.1 . . ? C46 C47 H47A 122.5 . . ? C46 C47 C48 115.9(5) . . ? C46 C47 C50 115.0(6) . . ? C48 C47 H47 122.1 . . ? C50 C47 H47A 122.5 . . ? C47 C48 H48 120.4 . . ? C49 C48 C47 119.2(7) . . ? C49 C48 H48 120.4 . . ? C44 C49 H49 119.9 . . ? C48 C49 C44 120.1(8) . . ? C48 C49 H49 119.9 . . ? C47 C50 H50 121.4 . . ? C51 C50 C47 117.1(10) . . ? C51 C50 H50 121.4 . . ? C44 C51 H51 120.5 . . ? C50 C51 C44 119.0(10) . . ? C50 C51 H51 120.5 . . ? C53 C52 P1 117.1(3) . . ? C53 C52 C57 118.1(4) . . ? C57 C52 P1 124.7(3) . . ? C52 C53 H53 119.5 . . ? C54 C53 C52 121.1(4) . . ? C54 C53 H53 119.5 . . ? C53 C54 H54 120.0 . . ? C55 C54 C53 120.0(4) . . ? C55 C54 H54 120.0 . . ? C54 C55 H55 119.9 . . ? C56 C55 C54 120.3(4) . . ? C56 C55 H55 119.9 . . ? C55 C56 H56 120.0 . . ? C55 C56 C57 120.0(4) . . ? C57 C56 H56 120.0 . . ? C52 C57 C56 120.6(4) . . ? C52 C57 H57 119.7 . . ? C56 C57 H57 119.7 . . ? C59 P3 C65 102.22(18) . . ? C59 P3 C81 103.13(17) . . ? C65 P3 C81 99.92(18) . . ? C60 C59 P3 118.3(3) . . ? C64 C59 P3 122.5(3) . . ? C64 C59 C60 118.4(4) . . ? C59 C60 H60 119.9 . . ? C61 C60 C59 120.2(4) . . ? C61 C60 H60 119.9 . . ? C60 C61 H61 120.0 . . ? C62 C61 C60 120.0(4) . . ? C62 C61 H61 120.0 . . ? C61 C62 H62 119.7 . . ? C61 C62 C63 120.7(4) . . ? C63 C62 H62 119.7 . . ? C62 C63 H63 120.0 . . ? C62 C63 C64 119.9(4) . . ? C64 C63 H63 120.0 . . ? C59 C64 H64 119.6 . . ? C63 C64 C59 120.9(4) . . ? C63 C64 H64 119.6 . . ? C66 C65 P3 117.5(4) . . ? C70 C65 P3 123.7(4) . . ? C70 C65 C66 118.8(5) . . ? C65 C66 H66 119.5 . . ? C67 C66 C65 121.0(6) . . ? C67 C66 H66 119.5 . . ? C66 C67 H67 120.1 . . ? C66 C67 C68 119.8(6) . . ? C68 C67 H67 120.1 . . ? C67 C68 H68 119.9 . . ? C69 C68 C67 120.2(5) . . ? C69 C68 H68 119.9 . . ? C68 C69 H69 120.4 . . ? C70 C69 C68 119.2(6) . . ? C70 C69 H69 120.4 . . ? C65 C70 H70 119.5 . . ? C69 C70 C65 120.9(6) . . ? C69 C70 H70 119.5 . . ? C72 C71 H71 109.2 2 . ? C72 C71 H71 109.2 . . ? C72 C71 C72 90.3(3) . 2 ? C80 C71 H71 109.2 . . ? C80 C71 C72 117.4(3) . 2 ? C80 C71 C72 120.0(3) . . ? C71 C72 C71 89.7(3) . 2 ? C71 C72 H72 112.6 2 . ? C71 C72 H72 112.6 . . ? C73 C72 C71 113.7(3) . . ? C73 C72 C71 113.9(3) . 2 ? C73 C72 H72 112.6 . . ? O3 C73 C72 120.3(3) . . ? O3 C73 C74 120.1(3) . . ? C74 C73 C72 119.6(3) . . ? C75 C74 C73 117.7(3) . . ? C79 C74 C73 123.1(3) . . ? C79 C74 C75 119.1(3) . . ? C74 C75 H75 119.8 . . ? C76 C75 C74 120.4(4) . . ? C76 C75 H75 119.8 . . ? C75 C76 H76 120.6 . . ? C77 C76 C75 118.8(4) . . ? C77 C76 H76 120.6 . . ? C76 C77 Br3 118.4(3) . . ? C76 C77 C78 122.4(3) . . ? C78 C77 Br3 119.2(3) . . ? C77 C78 H78 120.9 . . ? C77 C78 C79 118.2(4) . . ? C79 C78 H78 120.9 . . ? C74 C79 H79 119.5 . . ? C78 C79 C74 120.9(3) . . ? C78 C79 H79 119.5 . . ? C81 C80 C71 119.5(3) . . ? C85 C80 C71 122.3(3) . . ? C85 C80 C81 118.1(3) . . ? C80 C81 P3 118.5(3) . . ? C82 C81 P3 121.9(3) . . ? C82 C81 C80 119.5(3) . . ? C81 C82 H82 119.7 . . ? C83 C82 C81 120.7(4) . . ? C83 C82 H82 119.7 . . ? C82 C83 H83 120.0 . . ? C84 C83 C82 119.9(3) . . ? C84 C83 H83 120.0 . . ? C83 C84 H84 120.0 . . ? C83 C84 C85 120.0(4) . . ? C85 C84 H84 120.0 . . ? C80 C85 H85 119.2 . . ? C84 C85 C80 121.7(3) . . ? C84 C85 H85 119.2 . . ? 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 Br1 C35 1.895(4) . ? Br2 C9 1.912(4) . ? P1 C43 1.842(3) . ? P1 C44 1.837(4) . ? P1 C52 1.828(4) . ? P2 C13 1.841(4) . ? P2 C18 1.831(4) . ? P2 C24 1.838(4) . ? O1 C30 1.223(5) . ? O2 C5 1.223(4) . ? C2 H2 0.9800 . ? C2 C3 1.570(4) . ? C2 C12 1.507(4) . ? C2 C31 1.571(4) . ? C3 H3 0.9800 . ? C3 C4 1.586(5) . ? C3 C5 1.517(4) . ? C4 H4 0.9800 . ? C4 C31 1.540(4) . ? C4 C38 1.500(5) . ? C5 C6 1.494(5) . ? C6 C7 1.393(5) . ? C6 C11 1.395(5) . ? C7 H7 0.9300 . ? C7 C8 1.394(5) . ? C8 H8 0.9300 . ? C8 C9 1.379(6) . ? C9 C10 1.389(6) . ? C10 H10 0.9300 . ? C10 C11 1.374(5) . ? C11 H11 0.9300 . ? C12 C13 1.412(5) . ? C12 C17 1.398(5) . ? C13 C14 1.401(5) . ? C14 H14 0.9300 . ? C14 C15 1.390(5) . ? C15 H15 0.9300 . ? C15 C16 1.373(5) . ? C16 H16 0.9300 . ? C16 C17 1.398(5) . ? C17 H17 0.9300 . ? C18 C19 1.400(5) . ? C18 C23 1.393(5) . ? C19 H19 0.9300 . ? C19 C20 1.389(6) . ? C20 H20 0.9300 . ? C20 C21 1.381(6) . ? C21 H21 0.9300 . ? C21 C22 1.380(6) . ? C22 H22 0.9300 . ? C22 C23 1.391(5) . ? C23 H23 0.9300 . ? C24 C25 1.389(5) . ? C24 C29 1.404(5) . ? C25 H25 0.9300 . ? C25 C26 1.391(5) . ? C26 H26 0.9300 . ? C26 C27 1.380(6) . ? C27 H27 0.9300 . ? C27 C28 1.390(6) . ? C28 H28 0.9300 . ? C28 C29 1.392(6) . ? C29 H29 0.9300 . ? C30 C31 1.502(5) . ? C30 C32 1.501(5) . ? C31 H31 0.9800 . ? C32 C33 1.387(5) . ? C32 C37 1.399(5) . ? C33 H33 0.9300 . ? C33 C34 1.394(5) . ? C34 H34 0.9300 . ? C34 C35 1.385(6) . ? C35 C36 1.383(6) . ? C36 H36 0.9300 . ? C36 C37 1.377(5) . ? C37 H37 0.9300 . ? C38 C39 1.389(5) . ? C38 C43 1.422(5) . ? C39 H39 0.9300 . ? C39 C40 1.396(5) . ? C40 H40 0.9300 . ? C40 C41 1.382(5) . ? C41 H41 0.9300 . ? C41 C42 1.388(5) . ? C42 H42 0.9300 . ? C42 C43 1.396(5) . ? C44 C45 1.371(6) . ? C44 C49 1.387(9) . ? C44 C51 1.490(11) . ? C45 H45 0.9300 . ? C45 C46 1.387(6) . ? C46 H46 0.9300 . ? C46 C47 1.340(7) . ? C47 H47 0.9300 . ? C47 H47A 0.9300 . ? C47 C48 1.468(12) . ? C47 C50 1.476(18) . ? C48 H48 0.9300 . ? C48 C49 1.378(11) . ? C49 H49 0.9300 . ? C50 H50 0.9300 . ? C50 C51 1.386(17) . ? C51 H51 0.9300 . ? C52 C53 1.390(5) . ? C52 C57 1.396(6) . ? C53 H53 0.9300 . ? C53 C54 1.386(7) . ? C54 H54 0.9300 . ? C54 C55 1.381(7) . ? C55 H55 0.9300 . ? C55 C56 1.367(6) . ? C56 H56 0.9300 . ? C56 C57 1.400(6) . ? C57 H57 0.9300 . ? Br3 C77 1.897(4) . ? P3 C59 1.830(4) . ? P3 C65 1.839(4) . ? P3 C81 1.850(4) . ? O3 C73 1.222(5) . ? C59 C60 1.399(6) . ? C59 C64 1.391(6) . ? C60 H60 0.9300 . ? C60 C61 1.397(6) . ? C61 H61 0.9300 . ? C61 C62 1.368(7) . ? C62 H62 0.9300 . ? C62 C63 1.376(7) . ? C63 H63 0.9300 . ? C63 C64 1.383(6) . ? C64 H64 0.9300 . ? C65 C66 1.397(7) . ? C65 C70 1.387(7) . ? C66 H66 0.9300 . ? C66 C67 1.350(7) . ? C67 H67 0.9300 . ? C67 C68 1.404(11) . ? C68 H68 0.9300 . ? C68 C69 1.383(10) . ? C69 H69 0.9300 . ? C69 C70 1.381(7) . ? C70 H70 0.9300 . ? C71 H71 0.9800 . ? C71 C72 1.582(5) 2 ? C71 C72 1.555(5) . ? C71 C80 1.514(5) . ? C72 H72 0.9800 . ? C72 C73 1.509(5) . ? C73 C74 1.506(5) . ? C74 C75 1.394(5) . ? C74 C79 1.391(6) . ? C75 H75 0.9300 . ? C75 C76 1.386(5) . ? C76 H76 0.9300 . ? C76 C77 1.374(6) . ? C77 C78 1.380(5) . ? C78 H78 0.9300 . ? C78 C79 1.388(5) . ? C79 H79 0.9300 . ? C80 C81 1.408(5) . ? C80 C85 1.397(5) . ? C81 C82 1.408(5) . ? C82 H82 0.9300 . ? C82 C83 1.386(6) . ? C83 H83 0.9300 . ? C83 C84 1.375(6) . ? C84 H84 0.9300 . ? C84 C85 1.387(5) . ? C85 H85 0.9300 . ? 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 Br1 C35 C36 C37 177.5(3) . . . . ? Br2 C9 C10 C11 176.3(3) . . . . ? P1 C44 C45 C46 178.9(3) . . . . ? P1 C44 C49 C48 -179.1(8) . . . . ? P1 C44 C51 C50 177.2(10) . . . . ? P1 C52 C53 C54 179.3(3) . . . . ? P1 C52 C57 C56 179.1(3) . . . . ? P2 C13 C14 C15 -173.2(3) . . . . ? P2 C18 C19 C20 -174.8(3) . . . . ? P2 C18 C23 C22 176.0(3) . . . . ? P2 C24 C25 C26 -176.9(3) . . . . ? P2 C24 C29 C28 178.4(3) . . . . ? O1 C30 C31 C2 122.3(4) . . . . ? O1 C30 C31 C4 12.8(5) . . . . ? O1 C30 C32 C33 177.2(4) . . . . ? O1 C30 C32 C37 -0.2(5) . . . . ? O2 C5 C6 C7 172.4(3) . . . . ? O2 C5 C6 C11 -11.6(5) . . . . ? C2 C3 C4 C31 -19.4(2) . . . . ? C2 C3 C4 C38 -148.3(3) . . . . ? C2 C3 C5 O2 25.3(4) . . . . ? C2 C3 C5 C6 -153.6(3) . . . . ? C2 C12 C13 P2 -14.5(4) . . . . ? C2 C12 C13 C14 171.3(3) . . . . ? C2 C12 C17 C16 -171.7(3) . . . . ? C3 C2 C12 C13 -102.0(3) . . . . ? C3 C2 C12 C17 72.3(4) . . . . ? C3 C2 C31 C4 -19.6(2) . . . . ? C3 C2 C31 C30 -143.3(3) . . . . ? C3 C4 C31 C2 19.4(2) . . . . ? C3 C4 C31 C30 147.0(3) . . . . ? C3 C4 C38 C39 88.9(4) . . . . ? C3 C4 C38 C43 -90.8(4) . . . . ? C3 C5 C6 C7 -8.6(5) . . . . ? C3 C5 C6 C11 167.3(3) . . . . ? C4 C3 C5 O2 -71.8(4) . . . . ? C4 C3 C5 C6 109.2(3) . . . . ? C4 C38 C39 C40 -178.4(3) . . . . ? C4 C38 C43 P1 4.0(4) . . . . ? C4 C38 C43 C42 179.1(3) . . . . ? C5 C3 C4 C31 93.6(3) . . . . ? C5 C3 C4 C38 -35.4(4) . . . . ? C5 C6 C7 C8 174.5(3) . . . . ? C5 C6 C11 C10 -174.7(3) . . . . ? C6 C7 C8 C9 -0.6(6) . . . . ? C7 C6 C11 C10 1.3(6) . . . . ? C7 C8 C9 Br2 -176.3(3) . . . . ? C7 C8 C9 C10 2.8(6) . . . . ? C8 C9 C10 C11 -2.8(6) . . . . ? C9 C10 C11 C6 0.7(6) . . . . ? C11 C6 C7 C8 -1.4(6) . . . . ? C12 C2 C3 C4 -101.6(3) . . . . ? C12 C2 C3 C5 145.0(3) . . . . ? C12 C2 C31 C4 94.1(3) . . . . ? C12 C2 C31 C30 -29.7(4) . . . . ? C12 C13 C14 C15 0.8(5) . . . . ? C13 P2 C18 C19 -158.1(3) . . . . ? C13 P2 C18 C23 23.9(3) . . . . ? C13 P2 C24 C25 -106.0(3) . . . . ? C13 P2 C24 C29 77.2(3) . . . . ? C13 C12 C17 C16 2.7(5) . . . . ? C13 C14 C15 C16 2.3(6) . . . . ? C14 C15 C16 C17 -2.9(6) . . . . ? C15 C16 C17 C12 0.4(6) . . . . ? C17 C12 C13 P2 171.0(3) . . . . ? C17 C12 C13 C14 -3.2(5) . . . . ? C18 P2 C13 C12 80.0(3) . . . . ? C18 P2 C13 C14 -106.0(3) . . . . ? C18 P2 C24 C25 1.0(3) . . . . ? C18 P2 C24 C29 -175.8(3) . . . . ? C18 C19 C20 C21 -1.7(6) . . . . ? C19 C18 C23 C22 -1.9(5) . . . . ? C19 C20 C21 C22 -1.4(6) . . . . ? C20 C21 C22 C23 2.8(6) . . . . ? C21 C22 C23 C18 -1.1(5) . . . . ? C23 C18 C19 C20 3.3(6) . . . . ? C24 P2 C13 C12 -174.0(3) . . . . ? C24 P2 C13 C14 0.0(3) . . . . ? C24 P2 C18 C19 95.4(3) . . . . ? C24 P2 C18 C23 -82.6(3) . . . . ? C24 C25 C26 C27 -0.5(5) . . . . ? C25 C24 C29 C28 1.4(5) . . . . ? C25 C26 C27 C28 0.0(6) . . . . ? C26 C27 C28 C29 1.2(6) . . . . ? C27 C28 C29 C24 -1.9(6) . . . . ? C29 C24 C25 C26 -0.2(5) . . . . ? C30 C32 C33 C34 -179.3(4) . . . . ? C30 C32 C37 C36 179.3(3) . . . . ? C31 C2 C3 C4 19.0(2) . . . . ? C31 C2 C3 C5 -94.4(3) . . . . ? C31 C2 C12 C13 158.0(3) . . . . ? C31 C2 C12 C17 -27.7(5) . . . . ? C31 C4 C38 C39 -21.7(5) . . . . ? C31 C4 C38 C43 158.5(3) . . . . ? C31 C30 C32 C33 -1.9(5) . . . . ? C31 C30 C32 C37 -179.3(3) . . . . ? C32 C30 C31 C2 -58.7(4) . . . . ? C32 C30 C31 C4 -168.1(3) . . . . ? C32 C33 C34 C35 0.5(7) . . . . ? C33 C32 C37 C36 1.8(5) . . . . ? C33 C34 C35 Br1 -177.6(3) . . . . ? C33 C34 C35 C36 0.9(7) . . . . ? C34 C35 C36 C37 -1.0(6) . . . . ? C35 C36 C37 C32 -0.4(6) . . . . ? C37 C32 C33 C34 -1.9(6) . . . . ? C38 C4 C31 C2 145.6(3) . . . . ? C38 C4 C31 C30 -86.7(4) . . . . ? C38 C39 C40 C41 -1.2(6) . . . . ? C39 C38 C43 P1 -175.8(3) . . . . ? C39 C38 C43 C42 -0.6(5) . . . . ? C39 C40 C41 C42 0.4(6) . . . . ? C40 C41 C42 C43 0.3(6) . . . . ? C41 C42 C43 P1 174.8(3) . . . . ? C41 C42 C43 C38 -0.2(5) . . . . ? C43 P1 C44 C45 77.8(4) . . . . ? C43 P1 C44 C49 -122.4(6) . . . . ? C43 P1 C44 C51 -78.5(7) . . . . ? C43 P1 C52 C53 157.9(3) . . . . ? C43 P1 C52 C57 -20.5(4) . . . . ? C43 C38 C39 C40 1.3(5) . . . . ? C44 P1 C43 C38 179.6(3) . . . . ? C44 P1 C43 C42 4.6(3) . . . . ? C44 P1 C52 C53 -94.9(3) . . . . ? C44 P1 C52 C57 86.7(4) . . . . ? C44 C45 C46 C47 -0.3(8) . . . . ? C45 C44 C49 C48 -17.4(13) . . . . ? C45 C44 C51 C50 18.1(14) . . . . ? C45 C46 C47 C48 -19.3(10) . . . . ? C45 C46 C47 C50 30.4(11) . . . . ? C46 C47 C48 C49 20.7(14) . . . . ? C46 C47 C50 C51 -34.9(15) . . . . ? C47 C48 C49 C44 -2.1(16) . . . . ? C47 C50 C51 C44 10.4(18) . . . . ? C49 C44 C45 C46 19.4(8) . . . . ? C51 C44 C45 C46 -24.3(9) . . . . ? C52 P1 C43 C38 -74.3(3) . . . . ? C52 P1 C43 C42 110.7(3) . . . . ? C52 P1 C44 C45 -30.3(4) . . . . ? C52 P1 C44 C49 129.6(6) . . . . ? C52 P1 C44 C51 173.4(7) . . . . ? C52 C53 C54 C55 2.2(7) . . . . ? C53 C52 C57 C56 0.7(6) . . . . ? C53 C54 C55 C56 -0.8(7) . . . . ? C54 C55 C56 C57 -0.6(7) . . . . ? C55 C56 C57 C52 0.7(7) . . . . ? C57 C52 C53 C54 -2.1(6) . . . . ? Br3 C77 C78 C79 -178.2(3) . . . . ? P3 C59 C60 C61 170.6(3) . . . . ? P3 C59 C64 C63 -170.7(3) . . . . ? P3 C65 C66 C67 178.5(4) . . . . ? P3 C65 C70 C69 179.9(4) . . . . ? P3 C81 C82 C83 174.6(3) . . . . ? O3 C73 C74 C75 9.5(5) . . . . ? O3 C73 C74 C79 -169.1(3) . . . . ? C59 P3 C65 C66 118.8(3) . . . . ? C59 P3 C65 C70 -63.0(4) . . . . ? C59 P3 C81 C80 -162.5(3) . . . . ? C59 P3 C81 C82 21.5(3) . . . . ? C59 C60 C61 C62 0.5(6) . . . . ? C60 C59 C64 C63 -0.7(6) . . . . ? C60 C61 C62 C63 -0.7(6) . . . . ? C61 C62 C63 C64 0.2(6) . . . . ? C62 C63 C64 C59 0.5(6) . . . . ? C64 C59 C60 C61 0.3(6) . . . . ? C65 P3 C59 C60 163.1(3) . . . . ? C65 P3 C59 C64 -27.0(4) . . . . ? C65 P3 C81 C80 92.3(3) . . . . ? C65 P3 C81 C82 -83.7(3) . . . . ? C65 C66 C67 C68 2.1(8) . . . . ? C66 C65 C70 C69 -1.9(7) . . . . ? C66 C67 C68 C69 -2.7(9) . . . . ? C67 C68 C69 C70 1.0(8) . . . . ? C68 C69 C70 C65 1.3(8) . . . . ? C70 C65 C66 C67 0.2(7) . . . . ? C71 C72 C73 O3 31.2(4) . . . . ? C71 C72 C73 O3 -69.6(4) 2 . . . ? C71 C72 C73 C74 106.9(4) 2 . . . ? C71 C72 C73 C74 -152.2(3) . . . . ? C71 C80 C81 P3 8.2(4) . . . . ? C71 C80 C81 C82 -175.7(3) . . . . ? C71 C80 C85 C84 177.9(3) . . . . ? C72 C71 C72 C71 0.003(1) 2 . . 2 ? C72 C71 C72 C73 -116.1(3) 2 . . . ? C72 C71 C80 C81 82.1(4) 2 . . . ? C72 C71 C80 C81 -170.1(3) . . . . ? C72 C71 C80 C85 12.3(5) . . . . ? C72 C71 C80 C85 -95.5(4) 2 . . . ? C72 C73 C74 C75 -167.1(3) . . . . ? C72 C73 C74 C79 14.3(5) . . . . ? C73 C74 C75 C76 -179.2(3) . . . . ? C73 C74 C79 C78 178.4(3) . . . . ? C74 C75 C76 C77 2.0(6) . . . . ? C75 C74 C79 C78 -0.2(5) . . . . ? C75 C76 C77 Br3 177.5(3) . . . . ? C75 C76 C77 C78 -3.0(6) . . . . ? C76 C77 C78 C79 2.3(6) . . . . ? C77 C78 C79 C74 -0.6(6) . . . . ? C79 C74 C75 C76 -0.5(5) . . . . ? C80 C71 C72 C71 -122.3(4) . . . 2 ? C80 C71 C72 C73 121.6(3) . . . . ? C80 C81 C82 C83 -1.4(6) . . . . ? C81 P3 C59 C60 59.7(3) . . . . ? C81 P3 C59 C64 -130.4(3) . . . . ? C81 P3 C65 C66 -135.3(3) . . . . ? C81 P3 C65 C70 42.9(4) . . . . ? C81 C80 C85 C84 0.3(5) . . . . ? C81 C82 C83 C84 -1.6(6) . . . . ? C82 C83 C84 C85 3.9(6) . . . . ? C83 C84 C85 C80 -3.3(6) . . . . ? C85 C80 C81 P3 -174.1(3) . . . . ? C85 C80 C81 C82 2.0(5) . . . . ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 0.199 0.287 0.123 40.2 6.5 ? 2 0.801 0.713 0.877 40.2 6.7 ?