#------------------------------------------------------------------------------ #$Date: 2020-02-06 04:02:28 +0200 (Thu, 06 Feb 2020) $ #$Revision: 247904 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/72/1557253.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_1557253 loop_ _publ_author_name 'Windorff, Cory J.' 'Celis-Barros, Cristian' 'Sperling, Joseph M.' 'McKinnon, Noah C.' 'Albrecht-Schmitt, Thomas' _publ_section_title ; Probing a variation of the inverse-trans-influence in americium and lanthanide tribromide tris(tricyclohexylphosphine oxide) complexes ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/C9SC05268B _journal_year 2020 _chemical_formula_moiety 'C54 H99 Am Br3 O3 P3' _chemical_formula_sum 'C54 H99 Am Br3 O3 P3' _chemical_formula_weight 1371.97 _space_group_crystal_system orthorhombic _space_group_IT_number 29 _space_group_name_Hall 'P 2c -2ac' _space_group_name_H-M_alt 'P c a 21' _atom_sites_solution_hydrogens geom _audit_creation_date 2019-05-29 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2019-10-16 deposited with the CCDC. 2020-02-05 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 28.768(9) _cell_length_b 11.456(4) _cell_length_c 18.185(6) _cell_measurement_reflns_used 9657 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 27.47 _cell_measurement_theta_min 2.22 _cell_volume 5993(3) _computing_cell_refinement 'SAINT V8.38A (?, 2016)' _computing_data_reduction 'SAINT V8.38A (?, 2016)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 120(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type 'Bruker APEX-III CMOS' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0751 _diffrn_reflns_av_unetI/netI 0.0558 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 70455 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.521 _diffrn_reflns_theta_min 2.217 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 3.398 _exptl_absorpt_correction_T_max 0.0949 _exptl_absorpt_correction_T_min 0.0640 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1084 before and 0.0837 after correction. The Ratio of minimum to maximum transmission is 0.6744. The \l/2 correction factor is Not present.' _exptl_crystal_colour 'clear yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.521 _exptl_crystal_description block _exptl_crystal_F_000 2768 _exptl_crystal_preparation 'combining reagents isopropanol' _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: iPrOH' _exptl_crystal_size_max 0.196 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _refine_diff_density_max 2.033 _refine_diff_density_min -2.008 _refine_diff_density_rms 0.170 _refine_ls_abs_structure_details ; Flack x determined using 3383 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.004(7) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 578 _refine_ls_number_reflns 12088 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.081 _refine_ls_R_factor_all 0.0606 _refine_ls_R_factor_gt 0.0399 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0026P)^2^+27.6607P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0787 _refine_ls_wR_factor_ref 0.0858 _reflns_Friedel_coverage 0.938 _reflns_Friedel_fraction_full 0.999 _reflns_Friedel_fraction_max 0.995 _reflns_number_gt 9606 _reflns_number_total 12088 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9sc05268b2.cif _cod_data_source_block save4_b _cod_database_code 1557253 _shelx_shelxl_version_number 2016/6 _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 0.822 _shelx_estimated_absorpt_t_min 0.556 _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.970(17) 0.030(17) 2. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups 3.a Ternary CH refined with riding coordinates: C1(H1), C7(H7), C13(H13), C19(H19), C25(H25), C31(H31), C37(H37), C43(H43), C49(H49) 3.b Secondary CH2 refined with riding coordinates: C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C26(H26A, H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A, H42B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B) ; _shelx_res_file ; TITL save4_b.res in Pca2(1) save4_b.res created by SHELXL-2016/6 at 10:20:13 on 29-May-2019 REM Old TITL save4 in Pbcm REM SHELXT solution in Pca2(1) REM R1 0.107, Rweak 0.008, Alpha 0.016, Orientation a'=b, b'=a, c'=-c REM Flack x = 0.200 ( 0.007 ) from Parsons' quotients REM Formula found by SHELXT: C60 O13 P3 Br3 Pu CELL 0.71073 28.7681 11.4556 18.1848 90 90 90 ZERR 4 0.0089 0.0038 0.0062 0 0 0 LATT -1 SYMM -X,-Y,0.5+Z SYMM 0.5+X,-Y,+Z SYMM 0.5-X,+Y,0.5+Z SFAC C H O P Br SFAC Am 36.671 0.484 24.099 3.206 17.342 14.314 3.493 102.273 13.359 = -7.899 4.513 18900 3 243 UNIT 216 396 12 12 12 4 L.S. 15 PLAN 10 SIZE 0.06 0.12 0.196 TEMP -153(2) BOND $H LIST 6 fmap 2 ACTA TWIN -1 0 0 0 1 0 0 0 -1 2 OMIT 1 7 -16 OMIT 0 6 -16 OMIT 6 1 -21 OMIT 1 7 -15 REM REM REM WGHT 0.002600 27.660700 BASF 0.02978 FVAR 0.13859 AM1 6 0.626423 0.585859 0.471170 11.00000 0.01899 0.02438 = 0.02301 -0.00017 0.00089 -0.00115 BR1 5 0.683922 0.612734 0.599845 11.00000 0.03171 0.04373 = 0.02957 0.00068 -0.00817 -0.00289 BR2 5 0.567001 0.590274 0.344396 11.00000 0.03423 0.04202 = 0.03029 0.00192 -0.01021 -0.00634 BR3 5 0.627075 0.331704 0.472253 11.00000 0.03668 0.02304 = 0.05781 -0.00056 0.00953 -0.00112 P1 4 0.522204 0.535590 0.593073 11.00000 0.02557 0.02984 = 0.03096 -0.00489 0.00702 -0.00191 P2 4 0.733943 0.544915 0.353179 11.00000 0.02162 0.02741 = 0.02869 0.00026 0.00346 -0.00078 P3 4 0.612731 0.920498 0.466348 11.00000 0.02808 0.02576 = 0.03197 -0.00027 -0.00229 0.00051 O1 3 0.561630 0.583646 0.546408 11.00000 0.02677 0.03285 = 0.02324 -0.00227 -0.00140 -0.00261 O2 3 0.691503 0.581959 0.397526 11.00000 0.02926 0.03456 = 0.01742 0.00237 0.00492 -0.00259 O3 3 0.622760 0.790466 0.464849 11.00000 0.02353 0.03425 = 0.03071 0.00108 -0.00562 0.00361 C1 1 0.751010 0.399325 0.380747 11.00000 0.02362 0.03204 = 0.02798 0.00224 0.00529 -0.00467 AFIX 13 H1 2 0.723690 0.347861 0.370496 11.00000 -1.20000 AFIX 0 C2 1 0.792229 0.346479 0.337866 11.00000 0.02589 0.03640 = 0.03124 0.00113 0.00184 0.00119 AFIX 23 H2A 2 0.785400 0.348722 0.284526 11.00000 -1.20000 H2B 2 0.820458 0.393824 0.346805 11.00000 -1.20000 AFIX 0 C3 1 0.801236 0.220530 0.361372 11.00000 0.04313 0.03166 = 0.05956 -0.00397 0.01099 0.00731 AFIX 23 H3A 2 0.774519 0.171423 0.346528 11.00000 -1.20000 H3B 2 0.829187 0.190962 0.335648 11.00000 -1.20000 AFIX 0 C4 1 0.808373 0.209896 0.443552 11.00000 0.04166 0.02765 = 0.07490 0.00617 -0.00191 -0.00143 AFIX 23 H4A 2 0.837824 0.248948 0.457261 11.00000 -1.20000 H4B 2 0.811135 0.126347 0.456766 11.00000 -1.20000 AFIX 0 C5 1 0.768505 0.264186 0.487079 11.00000 0.03749 0.03223 = 0.04299 0.00470 -0.00156 -0.00995 AFIX 23 H5A 2 0.775883 0.261114 0.540220 11.00000 -1.20000 H5B 2 0.739830 0.218256 0.478789 11.00000 -1.20000 AFIX 0 C6 1 0.760015 0.390957 0.464451 11.00000 0.02778 0.03093 = 0.04063 0.00934 0.00852 -0.00122 AFIX 23 H6A 2 0.787453 0.438848 0.477477 11.00000 -1.20000 H6B 2 0.732853 0.422102 0.491514 11.00000 -1.20000 AFIX 0 C7 1 0.782719 0.646005 0.371831 11.00000 0.02667 0.03013 = 0.02226 0.00292 -0.00390 -0.00418 AFIX 13 H7 2 0.804641 0.602631 0.404614 11.00000 -1.20000 AFIX 0 C8 1 0.810762 0.680638 0.304250 11.00000 0.02610 0.02927 = 0.03674 -0.00694 0.00453 -0.00203 AFIX 23 H8A 2 0.789791 0.715931 0.267251 11.00000 -1.20000 H8B 2 0.824927 0.610074 0.282211 11.00000 -1.20000 AFIX 0 C9 1 0.849056 0.767848 0.324056 11.00000 0.03012 0.04462 = 0.03056 0.00588 0.00389 -0.00458 AFIX 23 H9A 2 0.873039 0.727437 0.353658 11.00000 -1.20000 H9B 2 0.864011 0.795593 0.278245 11.00000 -1.20000 AFIX 0 C10 1 0.831360 0.872251 0.366802 11.00000 0.03631 0.03256 = 0.05507 0.00203 -0.00358 -0.00797 AFIX 23 H10A 2 0.857839 0.922594 0.381065 11.00000 -1.20000 H10B 2 0.810174 0.918718 0.335439 11.00000 -1.20000 AFIX 0 C11 1 0.805886 0.832369 0.434747 11.00000 0.04504 0.04405 = 0.04773 -0.01999 0.01094 -0.01382 AFIX 23 H11A 2 0.793649 0.901344 0.461225 11.00000 -1.20000 H11B 2 0.827902 0.791684 0.467821 11.00000 -1.20000 AFIX 0 C12 1 0.765841 0.750666 0.416155 11.00000 0.04363 0.04327 = 0.04618 -0.01561 0.01057 -0.00948 AFIX 23 H12A 2 0.742131 0.793679 0.387473 11.00000 -1.20000 H12B 2 0.751110 0.723081 0.462185 11.00000 -1.20000 AFIX 0 C13 1 0.719839 0.546848 0.255865 11.00000 0.02501 0.03997 = 0.02406 -0.00585 0.00261 0.00110 AFIX 13 H13 2 0.749443 0.540907 0.227289 11.00000 -1.20000 AFIX 0 C14 1 0.687811 0.441896 0.233774 11.00000 0.03223 0.03049 = 0.03503 -0.01393 -0.00392 -0.00706 AFIX 23 H14A 2 0.703987 0.367387 0.244064 11.00000 -1.20000 H14B 2 0.658923 0.443893 0.263332 11.00000 -1.20000 AFIX 0 C15 1 0.675729 0.449103 0.151696 11.00000 0.04518 0.05774 = 0.03030 -0.01152 -0.00963 -0.00550 AFIX 23 H15A 2 0.704361 0.437856 0.122337 11.00000 -1.20000 H15B 2 0.653885 0.385385 0.139104 11.00000 -1.20000 AFIX 0 C16 1 0.653802 0.565901 0.131552 11.00000 0.03458 0.07776 = 0.03142 -0.00140 -0.00626 0.00742 AFIX 23 H16A 2 0.648320 0.568412 0.077830 11.00000 -1.20000 H16B 2 0.623317 0.572963 0.156417 11.00000 -1.20000 AFIX 0 C17 1 0.684398 0.668708 0.153551 11.00000 0.02936 0.05949 = 0.03746 0.00348 -0.00109 0.00862 AFIX 23 H17A 2 0.668005 0.742803 0.142941 11.00000 -1.20000 H17B 2 0.713489 0.667390 0.124480 11.00000 -1.20000 AFIX 0 C18 1 0.695937 0.662020 0.235543 11.00000 0.02714 0.03867 = 0.04009 0.00906 0.00260 -0.00377 AFIX 23 H18A 2 0.666918 0.669885 0.264383 11.00000 -1.20000 H18B 2 0.716566 0.727925 0.248775 11.00000 -1.20000 AFIX 0 C19 1 0.623913 0.986732 0.377195 11.00000 0.03813 0.04409 = 0.02896 0.00502 -0.00382 0.00243 AFIX 13 H19 2 0.599460 1.047951 0.370854 11.00000 -1.20000 AFIX 0 C20 1 0.615252 0.896826 0.315582 11.00000 0.04368 0.03481 = 0.03303 -0.00267 -0.00256 -0.00160 AFIX 23 H20A 2 0.638850 0.834216 0.319395 11.00000 -1.20000 H20B 2 0.584352 0.860758 0.323197 11.00000 -1.20000 AFIX 0 C21 1 0.617067 0.947782 0.239518 11.00000 0.05560 0.05651 = 0.04145 0.00041 -0.00167 -0.00603 AFIX 23 H21A 2 0.590218 1.000633 0.232365 11.00000 -1.20000 H21B 2 0.614732 0.884154 0.202863 11.00000 -1.20000 AFIX 0 C22 1 0.662397 1.015980 0.226935 11.00000 0.04609 0.06398 = 0.04822 0.00711 0.00934 0.00076 AFIX 23 H22A 2 0.688620 0.960246 0.223744 11.00000 -1.20000 H22B 2 0.660396 1.057962 0.179455 11.00000 -1.20000 AFIX 0 C23 1 0.672121 1.103477 0.288035 11.00000 0.03701 0.04607 = 0.04734 0.01380 0.00446 0.00015 AFIX 23 H23A 2 0.648976 1.167287 0.285336 11.00000 -1.20000 H23B 2 0.703270 1.138099 0.280298 11.00000 -1.20000 AFIX 0 C24 1 0.670268 1.048588 0.364272 11.00000 0.03689 0.03533 = 0.04255 0.00245 -0.00434 -0.00488 AFIX 23 H24A 2 0.674556 1.110035 0.401947 11.00000 -1.20000 H24B 2 0.695971 0.991713 0.369443 11.00000 -1.20000 AFIX 0 C25 1 0.646897 0.988543 0.539417 11.00000 0.03000 0.01729 = 0.04079 0.00643 0.00296 -0.00335 AFIX 13 H25 2 0.645513 1.075143 0.532857 11.00000 -1.20000 AFIX 0 C26 1 0.697974 0.950158 0.534449 11.00000 0.03165 0.03214 = 0.04488 -0.00410 -0.01245 -0.00731 AFIX 23 H26A 2 0.699644 0.863902 0.536525 11.00000 -1.20000 H26B 2 0.711005 0.975508 0.486659 11.00000 -1.20000 AFIX 0 C27 1 0.727110 1.001511 0.596674 11.00000 0.03873 0.04839 = 0.04324 0.00921 -0.00360 -0.00343 AFIX 23 H27A 2 0.759252 0.971147 0.593148 11.00000 -1.20000 H27B 2 0.728404 1.087434 0.591214 11.00000 -1.20000 AFIX 0 C28 1 0.707255 0.971441 0.671787 11.00000 0.04942 0.04727 = 0.04113 0.01007 -0.01154 -0.01570 AFIX 23 H28A 2 0.725924 1.009999 0.710537 11.00000 -1.20000 H28B 2 0.708998 0.886038 0.679646 11.00000 -1.20000 AFIX 0 C29 1 0.656896 1.011261 0.677430 11.00000 0.06054 0.05484 = 0.02934 -0.00512 -0.00416 -0.01010 AFIX 23 H29A 2 0.655580 1.097536 0.675055 11.00000 -1.20000 H29B 2 0.643918 0.986547 0.725387 11.00000 -1.20000 AFIX 0 C30 1 0.627126 0.958861 0.614312 11.00000 0.03592 0.03411 = 0.04654 0.00462 0.00173 -0.00099 AFIX 23 H30A 2 0.625785 0.872962 0.619893 11.00000 -1.20000 H30B 2 0.595008 0.989380 0.617868 11.00000 -1.20000 AFIX 0 C31 1 0.551512 0.944531 0.486498 11.00000 0.03169 0.03487 = 0.03131 0.00292 0.00233 0.00066 AFIX 13 H31 2 0.545172 0.900425 0.532882 11.00000 -1.20000 AFIX 0 C32 1 0.518568 0.892691 0.428648 11.00000 0.03360 0.04069 = 0.05217 -0.00350 -0.00637 0.00038 AFIX 23 H32A 2 0.522923 0.934177 0.381390 11.00000 -1.20000 H32B 2 0.526387 0.809457 0.420806 11.00000 -1.20000 AFIX 0 C33 1 0.467654 0.902819 0.452561 11.00000 0.02792 0.04286 = 0.05063 -0.00999 -0.01185 0.00162 AFIX 23 H33A 2 0.447437 0.872840 0.412759 11.00000 -1.20000 H33B 2 0.462562 0.853613 0.496585 11.00000 -1.20000 AFIX 0 C34 1 0.453975 1.027186 0.470059 11.00000 0.03158 0.04217 = 0.05650 -0.00025 -0.00172 0.00458 AFIX 23 H34A 2 0.421643 1.029112 0.488662 11.00000 -1.20000 H34B 2 0.455478 1.075202 0.424856 11.00000 -1.20000 AFIX 0 C35 1 0.486880 1.077258 0.528080 11.00000 0.04265 0.02314 = 0.06275 0.00593 0.00957 0.00343 AFIX 23 H35A 2 0.483458 1.032527 0.574346 11.00000 -1.20000 H35B 2 0.478289 1.159373 0.538241 11.00000 -1.20000 AFIX 0 C36 1 0.537611 1.072107 0.502722 11.00000 0.04127 0.02735 = 0.05071 -0.00295 -0.00328 0.00006 AFIX 23 H36A 2 0.558039 1.104453 0.541506 11.00000 -1.20000 H36B 2 0.541575 1.119956 0.457823 11.00000 -1.20000 AFIX 0 C37 1 0.473052 0.497260 0.535127 11.00000 0.02772 0.02900 = 0.03952 0.00987 0.00624 -0.00386 AFIX 13 H37 2 0.447586 0.466517 0.567158 11.00000 -1.20000 AFIX 0 C38 1 0.454483 0.605079 0.492798 11.00000 0.03979 0.03321 = 0.04154 0.00895 0.01202 0.00575 AFIX 23 H38A 2 0.443082 0.663844 0.528408 11.00000 -1.20000 H38B 2 0.480156 0.640725 0.464337 11.00000 -1.20000 AFIX 0 C39 1 0.415625 0.572218 0.441229 11.00000 0.03057 0.06417 = 0.06523 0.03562 -0.00337 0.00454 AFIX 23 H39A 2 0.406245 0.641850 0.412603 11.00000 -1.20000 H39B 2 0.388431 0.546357 0.470345 11.00000 -1.20000 AFIX 0 C40 1 0.429521 0.476004 0.388814 11.00000 0.04444 0.05919 = 0.05811 0.02231 -0.02843 -0.02071 AFIX 23 H40A 2 0.454761 0.503982 0.356274 11.00000 -1.20000 H40B 2 0.402627 0.454638 0.357628 11.00000 -1.20000 AFIX 0 C41 1 0.446021 0.369000 0.431327 11.00000 0.05072 0.04363 = 0.04875 0.01201 -0.02061 -0.02282 AFIX 23 H41A 2 0.455596 0.307175 0.396434 11.00000 -1.20000 H41B 2 0.420258 0.338223 0.461771 11.00000 -1.20000 AFIX 0 C42 1 0.487016 0.401675 0.480654 11.00000 0.04364 0.02655 = 0.03454 0.00129 -0.01515 -0.00253 AFIX 23 H42A 2 0.513166 0.429546 0.449926 11.00000 -1.20000 H42B 2 0.497600 0.331824 0.507989 11.00000 -1.20000 AFIX 0 C43 1 0.503133 0.648839 0.657434 11.00000 0.04119 0.05180 = 0.08620 -0.04017 0.03413 -0.02238 AFIX 13 H43 2 0.489269 0.703624 0.620667 11.00000 -1.20000 AFIX 0 C44 1 0.537785 0.725243 0.685933 11.00000 0.05514 0.06697 = 0.11466 -0.05129 0.03977 -0.01276 AFIX 23 H44A 2 0.555993 0.756234 0.644065 11.00000 -1.20000 H44B 2 0.559272 0.678607 0.716677 11.00000 -1.20000 AFIX 0 C45 1 0.520960 0.827246 0.731109 11.00000 0.05611 0.03474 = 0.04961 -0.00830 0.00084 0.00652 AFIX 23 H45A 2 0.546283 0.851512 0.764653 11.00000 -1.20000 H45B 2 0.514594 0.893415 0.697569 11.00000 -1.20000 AFIX 0 C46 1 0.478433 0.804592 0.775768 11.00000 0.06566 0.10032 = 0.08243 -0.04148 0.02042 0.00490 AFIX 23 H46A 2 0.488495 0.775213 0.824429 11.00000 -1.20000 H46B 2 0.462691 0.880297 0.784088 11.00000 -1.20000 AFIX 0 C47 1 0.445103 0.725544 0.747410 11.00000 0.07366 0.07824 = 0.13578 -0.06129 0.06323 -0.02303 AFIX 23 H47A 2 0.422384 0.771566 0.718573 11.00000 -1.20000 H47B 2 0.428073 0.692084 0.789762 11.00000 -1.20000 AFIX 0 C48 1 0.460833 0.624851 0.699649 11.00000 0.03458 0.03787 = 0.05186 -0.00979 0.01433 -0.00022 AFIX 23 H48A 2 0.466341 0.555949 0.731334 11.00000 -1.20000 H48B 2 0.435503 0.604825 0.665022 11.00000 -1.20000 AFIX 0 C49 1 0.540235 0.402428 0.639153 11.00000 0.03130 0.04567 = 0.03040 0.01236 0.00641 -0.00268 AFIX 13 H49 2 0.551853 0.351066 0.598665 11.00000 -1.20000 AFIX 0 C50 1 0.501951 0.331040 0.676118 11.00000 0.04137 0.03619 = 0.04675 0.00349 0.01410 -0.00192 AFIX 23 H50A 2 0.477141 0.314106 0.639930 11.00000 -1.20000 H50B 2 0.488109 0.377108 0.716641 11.00000 -1.20000 AFIX 0 C51 1 0.521286 0.214860 0.707065 11.00000 0.05604 0.03471 = 0.04673 0.00707 0.00645 -0.00106 AFIX 23 H51A 2 0.496639 0.175287 0.735737 11.00000 -1.20000 H51B 2 0.529925 0.163167 0.665633 11.00000 -1.20000 AFIX 0 C52 1 0.562589 0.232887 0.754908 11.00000 0.10061 0.04717 = 0.04383 0.00077 -0.01983 -0.00144 AFIX 23 H52A 2 0.575833 0.156097 0.768499 11.00000 -1.20000 H52B 2 0.552855 0.272691 0.800711 11.00000 -1.20000 AFIX 0 C53 1 0.599288 0.304777 0.717165 11.00000 0.05917 0.08437 = 0.08200 0.04491 -0.04592 -0.02033 AFIX 23 H53A 2 0.612097 0.259088 0.675635 11.00000 -1.20000 H53B 2 0.624954 0.319108 0.752290 11.00000 -1.20000 AFIX 0 C54 1 0.582240 0.421364 0.688096 11.00000 0.06880 0.09035 = 0.06660 0.03628 -0.03728 -0.03345 AFIX 23 H54A 2 0.573773 0.472875 0.729706 11.00000 -1.20000 H54B 2 0.607297 0.459809 0.659706 11.00000 -1.20000 AFIX 0 HKLF 4 REM save4_b.res in Pca2(1) REM R1 = 0.0399 for 9606 Fo > 4sig(Fo) and 0.0606 for all 12088 data REM 578 parameters refined using 1 restraints END WGHT 0.0027 27.6447 REM Highest difference peak 2.033, deepest hole -2.008, 1-sigma level 0.170 Q1 1 0.6506 0.5836 0.5004 11.00000 0.05 2.03 Q2 1 0.6015 0.5898 0.5008 11.00000 0.05 1.81 Q3 1 0.6014 0.5834 0.4423 11.00000 0.05 1.76 Q4 1 0.6519 0.5834 0.4426 11.00000 0.05 1.74 Q5 1 0.6183 0.4167 0.4725 11.00000 0.05 1.54 Q6 1 0.6299 0.5140 0.4705 11.00000 0.05 1.19 Q7 1 0.5968 0.6430 0.4670 11.00000 0.05 1.18 Q8 1 0.6192 0.6346 0.4058 11.00000 0.05 1.16 Q9 1 0.6275 0.2436 0.4715 11.00000 0.05 1.11 Q10 1 0.6554 0.6445 0.4695 11.00000 0.05 1.08 ; _shelx_res_checksum 42237 _olex2_exptl_crystal_mounting_method 'nyloon loop' _olex2_submission_original_sample_id cjw84 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn Am1 Am 0.62642(2) 0.58586(2) 0.47117(3) 0.02212(8) Uani 1 1 d . Br1 Br 0.68392(4) 0.61273(10) 0.59985(7) 0.0350(3) Uani 1 1 d . Br2 Br 0.56700(4) 0.59027(10) 0.34440(7) 0.0355(3) Uani 1 1 d . Br3 Br 0.62707(4) 0.33170(7) 0.47225(14) 0.0392(2) Uani 1 1 d . P1 P 0.52220(9) 0.5356(3) 0.59307(17) 0.0288(6) Uani 1 1 d . P2 P 0.73394(9) 0.5449(2) 0.35318(16) 0.0259(6) Uani 1 1 d . P3 P 0.61273(8) 0.9205(2) 0.4663(2) 0.0286(5) Uani 1 1 d . O1 O 0.5616(2) 0.5836(6) 0.5464(4) 0.0276(16) Uani 1 1 d . O2 O 0.6915(2) 0.5820(6) 0.3975(4) 0.0271(16) Uani 1 1 d . O3 O 0.6228(2) 0.7905(5) 0.4648(7) 0.0295(15) Uani 1 1 d . C1 C 0.7510(3) 0.3993(9) 0.3807(6) 0.028(2) Uani 1 1 d . H1 H 0.723690 0.347861 0.370496 0.033 Uiso 1 1 calc R C2 C 0.7922(3) 0.3465(9) 0.3379(6) 0.031(2) Uani 1 1 d . H2A H 0.785400 0.348722 0.284526 0.037 Uiso 1 1 calc R H2B H 0.820458 0.393824 0.346805 0.037 Uiso 1 1 calc R C3 C 0.8012(4) 0.2205(10) 0.3614(7) 0.045(3) Uani 1 1 d . H3A H 0.774519 0.171423 0.346528 0.054 Uiso 1 1 calc R H3B H 0.829187 0.190962 0.335648 0.054 Uiso 1 1 calc R C4 C 0.8084(4) 0.2099(10) 0.4436(7) 0.048(4) Uani 1 1 d . H4A H 0.837824 0.248948 0.457261 0.058 Uiso 1 1 calc R H4B H 0.811135 0.126347 0.456766 0.058 Uiso 1 1 calc R C5 C 0.7685(4) 0.2642(9) 0.4871(6) 0.038(3) Uani 1 1 d . H5A H 0.775883 0.261114 0.540220 0.045 Uiso 1 1 calc R H5B H 0.739830 0.218256 0.478789 0.045 Uiso 1 1 calc R C6 C 0.7600(3) 0.3910(8) 0.4645(9) 0.033(3) Uani 1 1 d . H6A H 0.787453 0.438848 0.477477 0.040 Uiso 1 1 calc R H6B H 0.732853 0.422102 0.491514 0.040 Uiso 1 1 calc R C7 C 0.7827(3) 0.6460(9) 0.3718(5) 0.026(2) Uani 1 1 d . H7 H 0.804641 0.602631 0.404614 0.032 Uiso 1 1 calc R C8 C 0.8108(4) 0.6806(10) 0.3042(6) 0.031(3) Uani 1 1 d . H8A H 0.789791 0.715931 0.267251 0.037 Uiso 1 1 calc R H8B H 0.824927 0.610074 0.282211 0.037 Uiso 1 1 calc R C9 C 0.8491(4) 0.7678(10) 0.3241(6) 0.035(3) Uani 1 1 d . H9A H 0.873039 0.727437 0.353658 0.042 Uiso 1 1 calc R H9B H 0.864011 0.795593 0.278245 0.042 Uiso 1 1 calc R C10 C 0.8314(4) 0.8723(10) 0.3668(7) 0.041(3) Uani 1 1 d . H10A H 0.857839 0.922594 0.381065 0.050 Uiso 1 1 calc R H10B H 0.810174 0.918718 0.335439 0.050 Uiso 1 1 calc R C11 C 0.8059(4) 0.8324(11) 0.4347(7) 0.046(3) Uani 1 1 d . H11A H 0.793649 0.901344 0.461225 0.055 Uiso 1 1 calc R H11B H 0.827902 0.791684 0.467821 0.055 Uiso 1 1 calc R C12 C 0.7658(4) 0.7507(10) 0.4162(7) 0.044(3) Uani 1 1 d . H12A H 0.742131 0.793679 0.387473 0.053 Uiso 1 1 calc R H12B H 0.751110 0.723081 0.462185 0.053 Uiso 1 1 calc R C13 C 0.7198(3) 0.5468(9) 0.2559(6) 0.030(2) Uani 1 1 d . H13 H 0.749443 0.540907 0.227289 0.036 Uiso 1 1 calc R C14 C 0.6878(4) 0.4419(9) 0.2338(6) 0.033(3) Uani 1 1 d . H14A H 0.703987 0.367387 0.244064 0.039 Uiso 1 1 calc R H14B H 0.658923 0.443893 0.263332 0.039 Uiso 1 1 calc R C15 C 0.6757(4) 0.4491(11) 0.1517(6) 0.044(3) Uani 1 1 d . H15A H 0.704361 0.437856 0.122337 0.053 Uiso 1 1 calc R H15B H 0.653885 0.385385 0.139104 0.053 Uiso 1 1 calc R C16 C 0.6538(4) 0.5659(12) 0.1316(7) 0.048(3) Uani 1 1 d . H16A H 0.648320 0.568412 0.077830 0.058 Uiso 1 1 calc R H16B H 0.623317 0.572963 0.156417 0.058 Uiso 1 1 calc R C17 C 0.6844(4) 0.6687(12) 0.1536(7) 0.042(3) Uani 1 1 d . H17A H 0.668005 0.742803 0.142941 0.051 Uiso 1 1 calc R H17B H 0.713489 0.667390 0.124480 0.051 Uiso 1 1 calc R C18 C 0.6959(4) 0.6620(10) 0.2355(6) 0.035(3) Uani 1 1 d . H18A H 0.666918 0.669885 0.264383 0.042 Uiso 1 1 calc R H18B H 0.716566 0.727925 0.248775 0.042 Uiso 1 1 calc R C19 C 0.6239(4) 0.9867(11) 0.3772(7) 0.037(3) Uani 1 1 d . H19 H 0.599460 1.047951 0.370854 0.044 Uiso 1 1 calc R C20 C 0.6153(4) 0.8968(10) 0.3156(6) 0.037(3) Uani 1 1 d . H20A H 0.638850 0.834216 0.319395 0.045 Uiso 1 1 calc R H20B H 0.584352 0.860758 0.323197 0.045 Uiso 1 1 calc R C21 C 0.6171(5) 0.9478(12) 0.2395(7) 0.051(3) Uani 1 1 d . H21A H 0.590218 1.000633 0.232365 0.061 Uiso 1 1 calc R H21B H 0.614732 0.884154 0.202863 0.061 Uiso 1 1 calc R C22 C 0.6624(5) 1.0160(13) 0.2269(8) 0.053(4) Uani 1 1 d . H22A H 0.688620 0.960246 0.223744 0.063 Uiso 1 1 calc R H22B H 0.660396 1.057962 0.179455 0.063 Uiso 1 1 calc R C23 C 0.6721(4) 1.1035(11) 0.2880(7) 0.043(3) Uani 1 1 d . H23A H 0.648976 1.167287 0.285336 0.052 Uiso 1 1 calc R H23B H 0.703270 1.138099 0.280298 0.052 Uiso 1 1 calc R C24 C 0.6703(4) 1.0486(10) 0.3643(6) 0.038(3) Uani 1 1 d . H24A H 0.674556 1.110035 0.401947 0.046 Uiso 1 1 calc R H24B H 0.695971 0.991713 0.369443 0.046 Uiso 1 1 calc R C25 C 0.6469(4) 0.9885(9) 0.5394(7) 0.029(3) Uani 1 1 d . H25 H 0.645513 1.075143 0.532857 0.035 Uiso 1 1 calc R C26 C 0.6980(4) 0.9502(10) 0.5344(7) 0.036(3) Uani 1 1 d . H26A H 0.699644 0.863902 0.536525 0.043 Uiso 1 1 calc R H26B H 0.711005 0.975508 0.486659 0.043 Uiso 1 1 calc R C27 C 0.7271(4) 1.0015(10) 0.5967(7) 0.043(3) Uani 1 1 d . H27A H 0.759252 0.971147 0.593148 0.052 Uiso 1 1 calc R H27B H 0.728404 1.087434 0.591214 0.052 Uiso 1 1 calc R C28 C 0.7073(4) 0.9714(11) 0.6718(7) 0.046(3) Uani 1 1 d . H28A H 0.725924 1.009999 0.710537 0.055 Uiso 1 1 calc R H28B H 0.708998 0.886038 0.679646 0.055 Uiso 1 1 calc R C29 C 0.6569(5) 1.0113(13) 0.6774(7) 0.048(3) Uani 1 1 d . H29A H 0.655580 1.097536 0.675055 0.058 Uiso 1 1 calc R H29B H 0.643918 0.986547 0.725387 0.058 Uiso 1 1 calc R C30 C 0.6271(4) 0.9589(11) 0.6143(7) 0.039(3) Uani 1 1 d . H30A H 0.625785 0.872962 0.619893 0.047 Uiso 1 1 calc R H30B H 0.595008 0.989380 0.617868 0.047 Uiso 1 1 calc R C31 C 0.5515(3) 0.9445(9) 0.4865(6) 0.033(3) Uani 1 1 d . H31 H 0.545172 0.900425 0.532882 0.039 Uiso 1 1 calc R C32 C 0.5186(4) 0.8927(10) 0.4286(7) 0.042(3) Uani 1 1 d . H32A H 0.522923 0.934177 0.381390 0.051 Uiso 1 1 calc R H32B H 0.526387 0.809457 0.420806 0.051 Uiso 1 1 calc R C33 C 0.4677(3) 0.9028(10) 0.4526(7) 0.040(3) Uani 1 1 d . H33A H 0.447437 0.872840 0.412759 0.049 Uiso 1 1 calc R H33B H 0.462562 0.853613 0.496585 0.049 Uiso 1 1 calc R C34 C 0.4540(3) 1.0272(9) 0.4701(10) 0.043(2) Uani 1 1 d . H34A H 0.421643 1.029112 0.488662 0.052 Uiso 1 1 calc R H34B H 0.455478 1.075202 0.424856 0.052 Uiso 1 1 calc R C35 C 0.4869(4) 1.0773(10) 0.5281(7) 0.043(3) Uani 1 1 d . H35A H 0.483458 1.032527 0.574346 0.051 Uiso 1 1 calc R H35B H 0.478289 1.159373 0.538241 0.051 Uiso 1 1 calc R C36 C 0.5376(4) 1.0721(9) 0.5027(7) 0.040(3) Uani 1 1 d . H36A H 0.558039 1.104453 0.541506 0.048 Uiso 1 1 calc R H36B H 0.541575 1.119956 0.457823 0.048 Uiso 1 1 calc R C37 C 0.4731(4) 0.4973(9) 0.5351(6) 0.032(3) Uani 1 1 d . H37 H 0.447586 0.466517 0.567158 0.038 Uiso 1 1 calc R C38 C 0.4545(4) 0.6051(9) 0.4928(6) 0.038(3) Uani 1 1 d . H38A H 0.443082 0.663844 0.528408 0.046 Uiso 1 1 calc R H38B H 0.480156 0.640725 0.464337 0.046 Uiso 1 1 calc R C39 C 0.4156(4) 0.5722(12) 0.4412(7) 0.053(4) Uani 1 1 d . H39A H 0.406245 0.641850 0.412603 0.064 Uiso 1 1 calc R H39B H 0.388431 0.546357 0.470345 0.064 Uiso 1 1 calc R C40 C 0.4295(5) 0.4760(12) 0.3888(8) 0.054(4) Uani 1 1 d . H40A H 0.454761 0.503982 0.356274 0.065 Uiso 1 1 calc R H40B H 0.402627 0.454638 0.357628 0.065 Uiso 1 1 calc R C41 C 0.4460(4) 0.3690(11) 0.4313(7) 0.048(3) Uani 1 1 d . H41A H 0.455596 0.307175 0.396434 0.057 Uiso 1 1 calc R H41B H 0.420258 0.338223 0.461771 0.057 Uiso 1 1 calc R C42 C 0.4870(4) 0.4017(8) 0.4807(8) 0.035(3) Uani 1 1 d . H42A H 0.513166 0.429546 0.449926 0.042 Uiso 1 1 calc R H42B H 0.497600 0.331824 0.507989 0.042 Uiso 1 1 calc R C43 C 0.5031(4) 0.6488(12) 0.6574(9) 0.060(4) Uani 1 1 d . H43 H 0.489269 0.703624 0.620667 0.072 Uiso 1 1 calc R C44 C 0.5378(5) 0.7252(14) 0.6859(10) 0.079(6) Uani 1 1 d . H44A H 0.555993 0.756234 0.644065 0.095 Uiso 1 1 calc R H44B H 0.559272 0.678607 0.716677 0.095 Uiso 1 1 calc R C45 C 0.5210(5) 0.8272(10) 0.7311(7) 0.047(3) Uani 1 1 d . H45A H 0.546283 0.851512 0.764653 0.056 Uiso 1 1 calc R H45B H 0.514594 0.893415 0.697569 0.056 Uiso 1 1 calc R C46 C 0.4784(6) 0.8046(17) 0.7758(10) 0.083(6) Uani 1 1 d . H46A H 0.488495 0.775213 0.824429 0.099 Uiso 1 1 calc R H46B H 0.462691 0.880297 0.784088 0.099 Uiso 1 1 calc R C47 C 0.4451(6) 0.7255(15) 0.7474(12) 0.096(7) Uani 1 1 d . H47A H 0.422384 0.771566 0.718573 0.115 Uiso 1 1 calc R H47B H 0.428073 0.692084 0.789762 0.115 Uiso 1 1 calc R C48 C 0.4608(4) 0.6249(10) 0.6996(7) 0.041(3) Uani 1 1 d . H48A H 0.466341 0.555949 0.731334 0.050 Uiso 1 1 calc R H48B H 0.435503 0.604825 0.665022 0.050 Uiso 1 1 calc R C49 C 0.5402(4) 0.4024(10) 0.6392(6) 0.036(3) Uani 1 1 d . H49 H 0.551853 0.351066 0.598665 0.043 Uiso 1 1 calc R C50 C 0.5020(4) 0.3310(10) 0.6761(7) 0.041(3) Uani 1 1 d . H50A H 0.477141 0.314106 0.639930 0.050 Uiso 1 1 calc R H50B H 0.488109 0.377108 0.716641 0.050 Uiso 1 1 calc R C51 C 0.5213(5) 0.2149(11) 0.7071(7) 0.046(3) Uani 1 1 d . H51A H 0.496639 0.175287 0.735737 0.055 Uiso 1 1 calc R H51B H 0.529925 0.163167 0.665633 0.055 Uiso 1 1 calc R C52 C 0.5626(6) 0.2329(12) 0.7549(8) 0.064(4) Uani 1 1 d . H52A H 0.575833 0.156097 0.768499 0.077 Uiso 1 1 calc R H52B H 0.552855 0.272691 0.800711 0.077 Uiso 1 1 calc R C53 C 0.5993(5) 0.3048(14) 0.7172(9) 0.075(5) Uani 1 1 d . H53A H 0.612097 0.259088 0.675635 0.090 Uiso 1 1 calc R H53B H 0.624954 0.319108 0.752290 0.090 Uiso 1 1 calc R C54 C 0.5822(5) 0.4214(14) 0.6881(9) 0.075(5) Uani 1 1 d . H54A H 0.573773 0.472875 0.729706 0.090 Uiso 1 1 calc R H54B H 0.607297 0.459809 0.659706 0.090 Uiso 1 1 calc R 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 Am1 0.01899(12) 0.02438(14) 0.02301(14) -0.0002(3) 0.00089(17) -0.00115(14) Br1 0.0317(5) 0.0437(6) 0.0296(6) 0.0007(5) -0.0082(5) -0.0029(5) Br2 0.0342(6) 0.0420(6) 0.0303(6) 0.0019(6) -0.0102(5) -0.0063(5) Br3 0.0367(5) 0.0230(4) 0.0578(6) -0.0006(11) 0.0095(7) -0.0011(4) P1 0.0256(13) 0.0298(14) 0.0310(16) -0.0049(15) 0.0070(13) -0.0019(12) P2 0.0216(12) 0.0274(14) 0.0287(15) 0.0003(14) 0.0035(12) -0.0008(11) P3 0.0281(11) 0.0258(10) 0.0320(14) -0.0003(18) -0.0023(19) 0.0005(9) O1 0.027(4) 0.033(4) 0.023(4) -0.002(3) -0.001(3) -0.003(3) O2 0.029(4) 0.035(4) 0.017(4) 0.002(3) 0.005(3) -0.003(3) O3 0.024(3) 0.034(3) 0.031(4) 0.001(5) -0.006(4) 0.004(3) C1 0.024(5) 0.032(6) 0.028(6) 0.002(5) 0.005(4) -0.005(4) C2 0.026(5) 0.036(6) 0.031(6) 0.001(5) 0.002(5) 0.001(4) C3 0.043(7) 0.032(6) 0.060(9) -0.004(6) 0.011(6) 0.007(5) C4 0.042(7) 0.028(6) 0.075(10) 0.006(6) -0.002(6) -0.001(5) C5 0.037(6) 0.032(5) 0.043(9) 0.005(5) -0.002(5) -0.010(5) C6 0.028(5) 0.031(5) 0.041(7) 0.009(7) 0.009(7) -0.001(4) C7 0.027(5) 0.030(6) 0.022(5) 0.003(4) -0.004(4) -0.004(4) C8 0.026(6) 0.029(6) 0.037(7) -0.007(5) 0.005(5) -0.002(5) C9 0.030(6) 0.045(7) 0.031(6) 0.006(5) 0.004(5) -0.005(5) C10 0.036(6) 0.033(6) 0.055(8) 0.002(6) -0.004(6) -0.008(5) C11 0.045(7) 0.044(7) 0.048(7) -0.020(6) 0.011(6) -0.014(6) C12 0.044(7) 0.043(7) 0.046(8) -0.016(6) 0.011(6) -0.009(6) C13 0.025(5) 0.040(6) 0.024(5) -0.006(5) 0.003(4) 0.001(5) C14 0.032(6) 0.030(6) 0.035(6) -0.014(5) -0.004(5) -0.007(5) C15 0.045(7) 0.058(8) 0.030(6) -0.012(6) -0.010(6) -0.005(6) C16 0.035(6) 0.078(10) 0.031(7) -0.001(7) -0.006(5) 0.007(6) C17 0.029(6) 0.059(9) 0.037(7) 0.003(6) -0.001(6) 0.009(6) C18 0.027(5) 0.039(6) 0.040(7) 0.009(5) 0.003(5) -0.004(5) C19 0.038(7) 0.044(7) 0.029(7) 0.005(6) -0.004(5) 0.002(6) C20 0.044(7) 0.035(7) 0.033(7) -0.003(5) -0.003(5) -0.002(5) C21 0.056(8) 0.057(8) 0.041(8) 0.000(6) -0.002(6) -0.006(7) C22 0.046(8) 0.064(9) 0.048(8) 0.007(8) 0.009(7) 0.001(7) C23 0.037(6) 0.046(8) 0.047(8) 0.014(6) 0.004(6) 0.000(6) C24 0.037(6) 0.035(6) 0.043(7) 0.002(5) -0.004(5) -0.005(5) C25 0.030(7) 0.017(5) 0.041(7) 0.006(5) 0.003(6) -0.003(5) C26 0.032(6) 0.032(6) 0.045(7) -0.004(5) -0.012(5) -0.007(5) C27 0.039(6) 0.048(7) 0.043(7) 0.009(6) -0.004(6) -0.003(5) C28 0.049(8) 0.047(7) 0.041(7) 0.010(6) -0.012(6) -0.016(6) C29 0.061(9) 0.055(9) 0.029(7) -0.005(6) -0.004(7) -0.010(7) C30 0.036(6) 0.034(6) 0.047(8) 0.005(6) 0.002(6) -0.001(5) C31 0.032(5) 0.035(6) 0.031(8) 0.003(5) 0.002(5) 0.001(4) C32 0.034(6) 0.041(7) 0.052(8) -0.004(6) -0.006(6) 0.000(5) C33 0.028(5) 0.043(6) 0.051(9) -0.010(6) -0.012(5) 0.002(5) C34 0.032(5) 0.042(6) 0.057(7) 0.000(9) -0.002(8) 0.005(4) C35 0.043(7) 0.023(6) 0.063(8) 0.006(6) 0.010(6) 0.003(5) C36 0.041(6) 0.027(6) 0.051(7) -0.003(5) -0.003(5) 0.000(5) C37 0.028(6) 0.029(6) 0.040(7) 0.010(5) 0.006(5) -0.004(4) C38 0.040(6) 0.033(6) 0.042(7) 0.009(5) 0.012(5) 0.006(5) C39 0.031(6) 0.064(9) 0.065(9) 0.036(7) -0.003(6) 0.005(6) C40 0.044(7) 0.059(9) 0.058(9) 0.022(7) -0.028(7) -0.021(7) C41 0.051(7) 0.044(7) 0.049(8) 0.012(6) -0.021(6) -0.023(6) C42 0.044(5) 0.027(5) 0.035(8) 0.001(6) -0.015(6) -0.003(4) C43 0.041(7) 0.052(8) 0.086(11) -0.040(8) 0.034(7) -0.022(6) C44 0.055(9) 0.067(10) 0.115(14) -0.051(10) 0.040(10) -0.013(8) C45 0.056(8) 0.035(7) 0.050(8) -0.008(6) 0.001(7) 0.007(6) C46 0.066(10) 0.100(14) 0.082(13) -0.041(11) 0.020(10) 0.005(10) C47 0.074(11) 0.078(12) 0.136(17) -0.061(12) 0.063(12) -0.023(9) C48 0.035(6) 0.038(7) 0.052(8) -0.010(6) 0.014(6) 0.000(5) C49 0.031(6) 0.046(7) 0.030(6) 0.012(5) 0.006(5) -0.003(5) C50 0.041(7) 0.036(7) 0.047(7) 0.003(6) 0.014(6) -0.002(5) C51 0.056(8) 0.035(7) 0.047(8) 0.007(6) 0.006(7) -0.001(6) C52 0.101(13) 0.047(8) 0.044(8) 0.001(7) -0.020(8) -0.001(8) C53 0.059(9) 0.084(11) 0.082(11) 0.045(9) -0.046(9) -0.020(8) C54 0.069(10) 0.090(12) 0.067(10) 0.036(9) -0.037(9) -0.033(9) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Am Am -7.8990 4.5130 '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 Br1 Am1 Br3 95.60(5) Br1 Am1 P1 89.73(6) Br1 Am1 P2 90.25(6) Br1 Am1 P3 88.33(6) Br2 Am1 Br1 172.74(3) Br2 Am1 Br3 91.54(5) Br2 Am1 P1 90.08(6) Br2 Am1 P2 91.92(6) Br2 Am1 P3 84.45(6) Br3 Am1 P1 81.29(6) Br3 Am1 P2 82.82(5) Br3 Am1 P3 174.43(4) P1 Am1 P2 164.03(5) P1 Am1 P3 94.82(7) P2 Am1 P3 101.15(7) O1 Am1 Br1 89.05(18) O1 Am1 Br2 89.73(19) O1 Am1 Br3 89.44(18) O1 Am1 P1 8.15(18) O1 Am1 P2 172.12(18) O1 Am1 P3 86.67(19) O1 Am1 O3 90.2(3) O2 Am1 Br1 90.44(18) O2 Am1 Br2 91.00(18) O2 Am1 Br3 88.81(18) O2 Am1 P1 170.07(19) O2 Am1 P2 6.05(18) O2 Am1 P3 95.12(19) O2 Am1 O1 178.1(2) O2 Am1 O3 91.6(3) O3 Am1 Br1 87.6(2) O3 Am1 Br2 85.2(2) O3 Am1 Br3 176.7(2) O3 Am1 P1 98.4(2) O3 Am1 P2 97.6(2) O3 Am1 P3 3.6(2) O1 P1 Am1 12.5(3) O1 P1 C37 110.1(5) O1 P1 C43 108.9(5) O1 P1 C49 110.4(5) C37 P1 Am1 108.3(4) C37 P1 C43 108.0(6) C43 P1 Am1 120.4(4) C49 P1 Am1 99.9(3) C49 P1 C37 106.7(5) C49 P1 C43 112.7(7) O2 P2 Am1 9.2(3) O2 P2 C1 109.1(4) O2 P2 C7 109.7(4) O2 P2 C13 109.5(4) C1 P2 Am1 100.3(3) C1 P2 C7 108.7(5) C1 P2 C13 110.0(5) C7 P2 Am1 115.9(3) C13 P2 Am1 111.6(3) C13 P2 C7 109.9(5) O3 P3 Am1 5.6(3) O3 P3 C19 111.1(7) O3 P3 C25 109.2(5) O3 P3 C31 109.6(4) C19 P3 Am1 114.7(4) C19 P3 C25 112.0(5) C19 P3 C31 106.7(5) C25 P3 Am1 110.7(3) C31 P3 Am1 104.2(3) C31 P3 C25 108.0(5) P1 O1 Am1 159.4(5) P2 O2 Am1 164.8(5) P3 O3 Am1 170.8(5) P2 C1 H1 106.2 C2 C1 P2 115.5(7) C2 C1 H1 106.2 C2 C1 C6 110.1(8) C6 C1 P2 112.0(7) C6 C1 H1 106.2 C1 C2 H2A 109.4 C1 C2 H2B 109.4 H2A C2 H2B 108.0 C3 C2 C1 111.1(9) C3 C2 H2A 109.4 C3 C2 H2B 109.4 C2 C3 H3A 109.2 C2 C3 H3B 109.2 H3A C3 H3B 107.9 C4 C3 C2 112.1(10) C4 C3 H3A 109.2 C4 C3 H3B 109.2 C3 C4 H4A 109.2 C3 C4 H4B 109.2 C3 C4 C5 112.2(10) H4A C4 H4B 107.9 C5 C4 H4A 109.2 C5 C4 H4B 109.2 C4 C5 H5A 109.3 C4 C5 H5B 109.3 C4 C5 C6 111.6(9) H5A C5 H5B 108.0 C6 C5 H5A 109.3 C6 C5 H5B 109.3 C1 C6 H6A 109.5 C1 C6 H6B 109.5 C5 C6 C1 110.5(10) C5 C6 H6A 109.5 C5 C6 H6B 109.5 H6A C6 H6B 108.1 P2 C7 H7 106.1 C8 C7 P2 114.6(7) C8 C7 H7 106.1 C8 C7 C12 113.0(9) C12 C7 P2 110.3(7) C12 C7 H7 106.1 C7 C8 H8A 109.4 C7 C8 H8B 109.4 C7 C8 C9 111.2(9) H8A C8 H8B 108.0 C9 C8 H8A 109.4 C9 C8 H8B 109.4 C8 C9 H9A 108.9 C8 C9 H9B 108.9 H9A C9 H9B 107.7 C10 C9 C8 113.2(9) C10 C9 H9A 108.9 C10 C9 H9B 108.9 C9 C10 H10A 109.6 C9 C10 H10B 109.6 H10A C10 H10B 108.1 C11 C10 C9 110.2(9) C11 C10 H10A 109.6 C11 C10 H10B 109.6 C10 C11 H11A 109.2 C10 C11 H11B 109.2 C10 C11 C12 111.9(10) H11A C11 H11B 107.9 C12 C11 H11A 109.2 C12 C11 H11B 109.2 C7 C12 H12A 109.4 C7 C12 H12B 109.4 C11 C12 C7 111.1(9) C11 C12 H12A 109.4 C11 C12 H12B 109.4 H12A C12 H12B 108.0 P2 C13 H13 108.4 C14 C13 P2 111.8(7) C14 C13 H13 108.4 C18 C13 P2 110.2(7) C18 C13 H13 108.4 C18 C13 C14 109.6(9) C13 C14 H14A 109.7 C13 C14 H14B 109.7 H14A C14 H14B 108.2 C15 C14 C13 109.9(9) C15 C14 H14A 109.7 C15 C14 H14B 109.7 C14 C15 H15A 109.2 C14 C15 H15B 109.2 H15A C15 H15B 107.9 C16 C15 C14 112.0(10) C16 C15 H15A 109.2 C16 C15 H15B 109.2 C15 C16 H16A 109.2 C15 C16 H16B 109.2 H16A C16 H16B 107.9 C17 C16 C15 112.1(10) C17 C16 H16A 109.2 C17 C16 H16B 109.2 C16 C17 H17A 109.7 C16 C17 H17B 109.7 C16 C17 C18 110.0(10) H17A C17 H17B 108.2 C18 C17 H17A 109.7 C18 C17 H17B 109.7 C13 C18 H18A 109.2 C13 C18 H18B 109.2 C17 C18 C13 112.1(10) C17 C18 H18A 109.2 C17 C18 H18B 109.2 H18A C18 H18B 107.9 P3 C19 H19 105.7 C20 C19 P3 109.9(8) C20 C19 H19 105.7 C24 C19 P3 119.0(9) C24 C19 H19 105.7 C24 C19 C20 109.8(10) C19 C20 H20A 108.8 C19 C20 H20B 108.8 H20A C20 H20B 107.7 C21 C20 C19 113.8(10) C21 C20 H20A 108.8 C21 C20 H20B 108.8 C20 C21 H21A 109.4 C20 C21 H21B 109.4 C20 C21 C22 111.3(11) H21A C21 H21B 108.0 C22 C21 H21A 109.4 C22 C21 H21B 109.4 C21 C22 H22A 109.1 C21 C22 H22B 109.1 H22A C22 H22B 107.8 C23 C22 C21 112.4(11) C23 C22 H22A 109.1 C23 C22 H22B 109.1 C22 C23 H23A 109.0 C22 C23 H23B 109.0 C22 C23 C24 112.7(10) H23A C23 H23B 107.8 C24 C23 H23A 109.0 C24 C23 H23B 109.0 C19 C24 H24A 109.4 C19 C24 H24B 109.4 C23 C24 C19 111.2(10) C23 C24 H24A 109.4 C23 C24 H24B 109.4 H24A C24 H24B 108.0 P3 C25 H25 108.4 C26 C25 P3 110.5(8) C26 C25 H25 108.4 C30 C25 P3 110.9(7) C30 C25 H25 108.4 C30 C25 C26 110.4(9) C25 C26 H26A 109.3 C25 C26 H26B 109.3 H26A C26 H26B 107.9 C27 C26 C25 111.8(10) C27 C26 H26A 109.3 C27 C26 H26B 109.3 C26 C27 H27A 109.2 C26 C27 H27B 109.2 H27A C27 H27B 107.9 C28 C27 C26 111.9(10) C28 C27 H27A 109.2 C28 C27 H27B 109.2 C27 C28 H28A 109.5 C27 C28 H28B 109.5 C27 C28 C29 110.5(10) H28A C28 H28B 108.1 C29 C28 H28A 109.5 C29 C28 H28B 109.5 C28 C29 H29A 109.4 C28 C29 H29B 109.4 C28 C29 C30 111.1(11) H29A C29 H29B 108.0 C30 C29 H29A 109.4 C30 C29 H29B 109.4 C25 C30 C29 111.8(10) C25 C30 H30A 109.3 C25 C30 H30B 109.3 C29 C30 H30A 109.3 C29 C30 H30B 109.3 H30A C30 H30B 107.9 P3 C31 H31 105.7 C32 C31 P3 113.6(8) C32 C31 H31 105.7 C32 C31 C36 109.7(9) C36 C31 P3 115.6(7) C36 C31 H31 105.7 C31 C32 H32A 109.3 C31 C32 H32B 109.3 H32A C32 H32B 108.0 C33 C32 C31 111.5(10) C33 C32 H32A 109.3 C33 C32 H32B 109.3 C32 C33 H33A 109.1 C32 C33 H33B 109.1 H33A C33 H33B 107.9 C34 C33 C32 112.3(9) C34 C33 H33A 109.1 C34 C33 H33B 109.1 C33 C34 H34A 109.7 C33 C34 H34B 109.7 C33 C34 C35 109.7(9) H34A C34 H34B 108.2 C35 C34 H34A 109.7 C35 C34 H34B 109.7 C34 C35 H35A 109.3 C34 C35 H35B 109.3 C34 C35 C36 111.6(10) H35A C35 H35B 108.0 C36 C35 H35A 109.3 C36 C35 H35B 109.3 C31 C36 H36A 109.7 C31 C36 H36B 109.7 C35 C36 C31 109.9(9) C35 C36 H36A 109.7 C35 C36 H36B 109.7 H36A C36 H36B 108.2 P1 C37 H37 108.5 C38 C37 P1 111.3(7) C38 C37 H37 108.5 C42 C37 P1 110.1(7) C42 C37 H37 108.5 C42 C37 C38 109.8(9) C37 C38 H38A 109.3 C37 C38 H38B 109.3 H38A C38 H38B 108.0 C39 C38 C37 111.4(9) C39 C38 H38A 109.3 C39 C38 H38B 109.3 C38 C39 H39A 109.2 C38 C39 H39B 109.2 C38 C39 C40 112.2(10) H39A C39 H39B 107.9 C40 C39 H39A 109.2 C40 C39 H39B 109.2 C39 C40 H40A 109.6 C39 C40 H40B 109.6 C39 C40 C41 110.4(11) H40A C40 H40B 108.1 C41 C40 H40A 109.6 C41 C40 H40B 109.6 C40 C41 H41A 109.7 C40 C41 H41B 109.7 C40 C41 C42 109.9(9) H41A C41 H41B 108.2 C42 C41 H41A 109.7 C42 C41 H41B 109.7 C37 C42 H42A 109.5 C37 C42 H42B 109.5 C41 C42 C37 110.6(9) C41 C42 H42A 109.5 C41 C42 H42B 109.5 H42A C42 H42B 108.1 P1 C43 H43 97.9 C44 C43 P1 117.3(9) C44 C43 H43 97.9 C44 C43 C48 120.4(12) C48 C43 P1 116.8(8) C48 C43 H43 97.9 C43 C44 H44A 108.1 C43 C44 H44B 108.1 C43 C44 C45 116.7(12) H44A C44 H44B 107.3 C45 C44 H44A 108.1 C45 C44 H44B 108.1 C44 C45 H45A 108.5 C44 C45 H45B 108.5 H45A C45 H45B 107.5 C46 C45 C44 115.2(12) C46 C45 H45A 108.5 C46 C45 H45B 108.5 C45 C46 H46A 107.8 C45 C46 H46B 107.8 H46A C46 H46B 107.2 C47 C46 C45 117.9(14) C47 C46 H46A 107.8 C47 C46 H46B 107.8 C46 C47 H47A 107.4 C46 C47 H47B 107.4 C46 C47 C48 119.6(14) H47A C47 H47B 107.0 C48 C47 H47A 107.4 C48 C47 H47B 107.4 C43 C48 C47 114.0(11) C43 C48 H48A 108.8 C43 C48 H48B 108.8 C47 C48 H48A 108.8 C47 C48 H48B 108.8 H48A C48 H48B 107.7 P1 C49 H49 104.5 C50 C49 P1 116.5(8) C50 C49 H49 104.5 C54 C49 P1 112.2(9) C54 C49 H49 104.5 C54 C49 C50 113.1(10) C49 C50 H50A 109.4 C49 C50 H50B 109.4 C49 C50 C51 111.2(10) H50A C50 H50B 108.0 C51 C50 H50A 109.4 C51 C50 H50B 109.4 C50 C51 H51A 109.1 C50 C51 H51B 109.1 H51A C51 H51B 107.9 C52 C51 C50 112.4(11) C52 C51 H51A 109.1 C52 C51 H51B 109.1 C51 C52 H52A 109.3 C51 C52 H52B 109.3 C51 C52 C53 111.7(11) H52A C52 H52B 107.9 C53 C52 H52A 109.3 C53 C52 H52B 109.3 C52 C53 H53A 108.7 C52 C53 H53B 108.7 C52 C53 C54 114.4(13) H53A C53 H53B 107.6 C54 C53 H53A 108.7 C54 C53 H53B 108.7 C49 C54 C53 109.6(12) C49 C54 H54A 109.7 C49 C54 H54B 109.7 C53 C54 H54A 109.7 C53 C54 H54B 109.7 H54A C54 H54B 108.2 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Am1 Br1 2.8821(14) Am1 Br2 2.8704(14) Am1 Br3 2.9116(13) Am1 P1 3.773(3) Am1 P2 3.794(3) Am1 P3 3.855(3) Am1 O1 2.312(7) Am1 O2 2.302(7) Am1 O3 2.349(6) P1 O1 1.520(8) P1 C37 1.817(11) P1 C43 1.831(12) P1 C49 1.816(11) P2 O2 1.523(7) P2 C1 1.809(11) P2 C7 1.851(10) P2 C13 1.816(11) P3 O3 1.518(6) P3 C19 1.819(13) P3 C25 1.827(12) P3 C31 1.820(10) C1 H1 1.0000 C1 C2 1.543(14) C1 C6 1.547(18) C2 H2A 0.9900 C2 H2B 0.9900 C2 C3 1.527(15) C3 H3A 0.9900 C3 H3B 0.9900 C3 C4 1.513(17) C4 H4A 0.9900 C4 H4B 0.9900 C4 C5 1.526(15) C5 H5A 0.9900 C5 H5B 0.9900 C5 C6 1.529(13) C6 H6A 0.9900 C6 H6B 0.9900 C7 H7 1.0000 C7 C8 1.523(14) C7 C12 1.524(15) C8 H8A 0.9900 C8 H8B 0.9900 C8 C9 1.530(15) C9 H9A 0.9900 C9 H9B 0.9900 C9 C10 1.515(15) C10 H10A 0.9900 C10 H10B 0.9900 C10 C11 1.507(16) C11 H11A 0.9900 C11 H11B 0.9900 C11 C12 1.522(15) C12 H12A 0.9900 C12 H12B 0.9900 C13 H13 1.0000 C13 C14 1.567(14) C13 C18 1.533(15) C14 H14A 0.9900 C14 H14B 0.9900 C14 C15 1.535(15) C15 H15A 0.9900 C15 H15B 0.9900 C15 C16 1.524(17) C16 H16A 0.9900 C16 H16B 0.9900 C16 C17 1.524(18) C17 H17A 0.9900 C17 H17B 0.9900 C17 C18 1.529(16) C18 H18A 0.9900 C18 H18B 0.9900 C19 H19 1.0000 C19 C20 1.542(17) C19 C24 1.528(15) C20 H20A 0.9900 C20 H20B 0.9900 C20 C21 1.502(17) C21 H21A 0.9900 C21 H21B 0.9900 C21 C22 1.537(17) C22 H22A 0.9900 C22 H22B 0.9900 C22 C23 1.522(19) C23 H23A 0.9900 C23 H23B 0.9900 C23 C24 1.523(16) C24 H24A 0.9900 C24 H24B 0.9900 C25 H25 1.0000 C25 C26 1.536(15) C25 C30 1.515(16) C26 H26A 0.9900 C26 H26B 0.9900 C26 C27 1.526(16) C27 H27A 0.9900 C27 H27B 0.9900 C27 C28 1.520(17) C28 H28A 0.9900 C28 H28B 0.9900 C28 C29 1.522(18) C29 H29A 0.9900 C29 H29B 0.9900 C29 C30 1.553(17) C30 H30A 0.9900 C30 H30B 0.9900 C31 H31 1.0000 C31 C32 1.535(15) C31 C36 1.544(14) C32 H32A 0.9900 C32 H32B 0.9900 C32 C33 1.532(14) C33 H33A 0.9900 C33 H33B 0.9900 C33 C34 1.512(14) C34 H34A 0.9900 C34 H34B 0.9900 C34 C35 1.529(18) C35 H35A 0.9900 C35 H35B 0.9900 C35 C36 1.532(15) C36 H36A 0.9900 C36 H36B 0.9900 C37 H37 1.0000 C37 C38 1.550(14) C37 C42 1.530(16) C38 H38A 0.9900 C38 H38B 0.9900 C38 C39 1.507(17) C39 H39A 0.9900 C39 H39B 0.9900 C39 C40 1.511(19) C40 H40A 0.9900 C40 H40B 0.9900 C40 C41 1.525(17) C41 H41A 0.9900 C41 H41B 0.9900 C41 C42 1.528(15) C42 H42A 0.9900 C42 H42B 0.9900 C43 H43 1.0000 C43 C44 1.424(18) C43 C48 1.465(16) C44 H44A 0.9900 C44 H44B 0.9900 C44 C45 1.508(17) C45 H45A 0.9900 C45 H45B 0.9900 C45 C46 1.491(19) C46 H46A 0.9900 C46 H46B 0.9900 C46 C47 1.42(2) C47 H47A 0.9900 C47 H47B 0.9900 C47 C48 1.513(17) C48 H48A 0.9900 C48 H48B 0.9900 C49 H49 1.0000 C49 C50 1.528(15) C49 C54 1.516(17) C50 H50A 0.9900 C50 H50B 0.9900 C50 C51 1.548(16) C51 H51A 0.9900 C51 H51B 0.9900 C51 C52 1.487(19) C52 H52A 0.9900 C52 H52B 0.9900 C52 C53 1.50(2) C53 H53A 0.9900 C53 H53B 0.9900 C53 C54 1.52(2) C54 H54A 0.9900 C54 H54B 0.9900 loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.970(17) 2 0.030(17)