#------------------------------------------------------------------------------ #$Date: 2020-04-05 13:25:03 +0300 (Sun, 05 Apr 2020) $ #$Revision: 250212 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/72/1557257.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_1557257 loop_ _publ_author_name 'Windorff, Cory J.' 'Celis-Barros, Cristian' 'Sperling, Joseph M.' 'McKinnon, Noah C.' 'Albrecht-Schmitt, Thomas E.' _publ_section_title ; Probing a variation of the inverse-trans-influence in americium and lanthanide tribromide tris(tricyclohexylphosphine oxide) complexes ; _journal_issue 10 _journal_name_full 'Chemical Science' _journal_page_first 2770 _journal_paper_doi 10.1039/C9SC05268B _journal_volume 11 _journal_year 2020 _chemical_absolute_configuration ad _chemical_formula_moiety 'C54 H99 Br3 O3 P3 Pr' _chemical_formula_sum 'C54 H99 Br3 O3 P3 Pr' _chemical_formula_weight 1269.88 _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 2019-06-24 _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 28.7155(12) _cell_length_b 11.4126(4) _cell_length_c 18.1299(8) _cell_measurement_reflns_used 9919 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 27.53 _cell_measurement_theta_min 2.22 _cell_volume 5941.5(4) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _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 0.998 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0613 _diffrn_reflns_av_unetI/netI 0.0404 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 106432 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.500 _diffrn_reflns_theta_max 27.551 _diffrn_reflns_theta_min 2.225 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.956 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.6775 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.420 _exptl_crystal_description block _exptl_crystal_F_000 2624 _exptl_crystal_preparation 'combining reagents in iPrOH' _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: iPrOH' _exptl_crystal_size_max 0.315 _exptl_crystal_size_mid 0.205 _exptl_crystal_size_min 0.188 _refine_diff_density_max 0.990 _refine_diff_density_min -0.720 _refine_diff_density_rms 0.101 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.009(9) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 578 _refine_ls_number_reflns 13677 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.055 _refine_ls_R_factor_all 0.0481 _refine_ls_R_factor_gt 0.0317 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0056P)^2^+11.3971P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0556 _refine_ls_wR_factor_ref 0.0617 _reflns_Friedel_coverage 0.938 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 0.999 _reflns_number_gt 11537 _reflns_number_total 13677 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9sc05268b2.cif _cod_data_source_block 'save_a_CCDC1' _cod_depositor_comments 'Adding full bibliography for 1557253--1557257.cif.' _cod_database_code 1557257 _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 0.606 _shelx_estimated_absorpt_t_min 0.456 _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.991(9) 0.009(9) 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 save_a.res in Pca2(1) save_a.res created by SHELXL-2016/6 at 14:10:11 on 24-Jun-2019 REM Old TITL save in Pca2(1) REM SHELXT solution in Pca2(1) REM R1 0.084, Rweak 0.009, Alpha 0.030, Orientation as input REM Flack x = 0.035 ( 0.004 ) from Parsons' quotients REM Formula found by SHELXT: C53 O4 P3 Br3 Pr CELL 0.71073 28.7155 11.4126 18.1299 90 90 90 ZERR 4 0.0012 0.0004 0.0008 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 Pr UNIT 216 396 12 12 12 4 L.S. 20 PLAN 10 SIZE 0.188 0.205 0.315 TEMP -153(2) BOND $H LIST 6 fmap 2 acta 51 TWIN -1 0 0 0 -1 0 0 0 -1 2 OMIT 2 0 2 OMIT 21 1 0 REM REM REM WGHT 0.005600 11.397100 BASF 0.00891 FVAR 0.15502 PR1 6 0.373643 0.413099 0.518571 11.00000 0.01124 0.01453 = 0.00968 0.00015 -0.00072 -0.00092 BR1 5 0.433401 0.409489 0.391147 11.00000 0.02859 0.03270 = 0.01848 -0.00086 0.01024 -0.00580 BR2 5 0.315816 0.387196 0.647972 11.00000 0.02498 0.03560 = 0.01790 -0.00005 0.00833 -0.00218 BR3 5 0.373068 0.668466 0.519817 11.00000 0.02905 0.01574 = 0.04626 0.00010 -0.00886 -0.00081 P1 4 0.266168 0.454320 0.401147 11.00000 0.01651 0.01965 = 0.01458 0.00059 -0.00365 -0.00139 P2 4 0.477798 0.464297 0.640014 11.00000 0.01742 0.02115 = 0.01898 0.00275 -0.00652 -0.00183 P3 4 0.387495 0.079008 0.513903 11.00000 0.02198 0.01484 = 0.02081 -0.00067 0.00176 -0.00024 O1 3 0.308761 0.418162 0.444793 11.00000 0.01484 0.02439 = 0.01611 -0.00054 -0.00632 0.00059 O2 3 0.438319 0.416165 0.593560 11.00000 0.01477 0.02186 = 0.02115 0.00229 -0.00543 -0.00234 O3 3 0.377332 0.208838 0.513239 11.00000 0.02147 0.02028 = 0.01955 -0.00366 0.00126 0.00238 C1 1 0.217522 0.354653 0.420204 11.00000 0.02178 0.02071 = 0.01738 -0.00227 -0.00137 0.00012 AFIX 13 H1 2 0.195568 0.398294 0.453046 11.00000 -1.20000 AFIX 0 C2 1 0.234664 0.249241 0.464375 11.00000 0.03792 0.03209 = 0.02734 0.01089 -0.01335 -0.00964 AFIX 23 H2A 2 0.258377 0.206333 0.435365 11.00000 -1.20000 H2B 2 0.249499 0.276687 0.510539 11.00000 -1.20000 AFIX 0 C3 1 0.194626 0.167130 0.482964 11.00000 0.04044 0.03634 = 0.03088 0.01205 -0.00519 -0.01197 AFIX 23 H3A 2 0.206897 0.097994 0.509611 11.00000 -1.20000 H3B 2 0.172474 0.207909 0.516007 11.00000 -1.20000 AFIX 0 C4 1 0.169081 0.126601 0.414061 11.00000 0.02800 0.02492 = 0.03936 -0.00025 -0.00119 -0.01107 AFIX 23 H4A 2 0.190580 0.081371 0.382254 11.00000 -1.20000 H4B 2 0.142913 0.074735 0.428133 11.00000 -1.20000 AFIX 0 C5 1 0.150573 0.231637 0.371840 11.00000 0.01899 0.03073 = 0.03641 -0.00466 -0.00278 -0.00374 AFIX 23 H5A 2 0.126813 0.272071 0.402135 11.00000 -1.20000 H5B 2 0.135319 0.204317 0.325989 11.00000 -1.20000 AFIX 0 C6 1 0.189543 0.318667 0.352074 11.00000 0.02063 0.02772 = 0.02378 -0.00083 -0.00385 -0.00393 AFIX 23 H6A 2 0.210689 0.282233 0.315549 11.00000 -1.20000 H6B 2 0.175682 0.389297 0.329204 11.00000 -1.20000 AFIX 0 C7 1 0.280332 0.452558 0.303155 11.00000 0.01985 0.02972 = 0.01502 0.00160 -0.00245 0.00188 AFIX 13 H7 2 0.250740 0.458605 0.274327 11.00000 -1.20000 AFIX 0 C8 1 0.304221 0.336854 0.283533 11.00000 0.02086 0.03080 = 0.02455 0.00079 0.00257 0.00119 AFIX 23 H8A 2 0.283565 0.270690 0.296826 11.00000 -1.20000 H8B 2 0.333348 0.329123 0.312340 11.00000 -1.20000 AFIX 0 C9 1 0.315492 0.331354 0.201012 11.00000 0.02609 0.04427 = 0.02761 -0.00528 0.00143 0.00634 AFIX 23 H9A 2 0.331689 0.256874 0.189811 11.00000 -1.20000 H9B 2 0.286213 0.333372 0.172209 11.00000 -1.20000 AFIX 0 C10 1 0.346270 0.434255 0.178739 11.00000 0.03295 0.06042 = 0.02201 0.00602 0.00796 0.00375 AFIX 23 H10A 2 0.376829 0.427438 0.203651 11.00000 -1.20000 H10B 2 0.351672 0.432018 0.124827 11.00000 -1.20000 AFIX 0 C11 1 0.323888 0.549693 0.199318 11.00000 0.04044 0.04930 = 0.02495 0.01373 0.00553 -0.00283 AFIX 23 H11A 2 0.295010 0.560049 0.170210 11.00000 -1.20000 H11B 2 0.345339 0.614489 0.186521 11.00000 -1.20000 AFIX 0 C12 1 0.312050 0.556414 0.282061 11.00000 0.03106 0.03071 = 0.02548 0.00608 -0.00292 -0.00572 AFIX 23 H12A 2 0.295981 0.631222 0.292855 11.00000 -1.20000 H12B 2 0.341054 0.553649 0.311529 11.00000 -1.20000 AFIX 0 C13 1 0.249351 0.600637 0.428471 11.00000 0.02166 0.02248 = 0.02144 0.00349 -0.00478 -0.00052 AFIX 13 H13 2 0.276639 0.652531 0.418120 11.00000 -1.20000 AFIX 0 C14 1 0.207880 0.651854 0.385463 11.00000 0.02333 0.02760 = 0.02845 0.00031 -0.00491 0.00157 AFIX 23 H14A 2 0.214610 0.649175 0.331934 11.00000 -1.20000 H14B 2 0.179772 0.603880 0.394833 11.00000 -1.20000 AFIX 0 C15 1 0.198632 0.778665 0.408799 11.00000 0.03026 0.02459 = 0.04709 0.00475 -0.00758 0.00350 AFIX 23 H15A 2 0.225212 0.828283 0.393504 11.00000 -1.20000 H15B 2 0.170436 0.807750 0.383262 11.00000 -1.20000 AFIX 0 C16 1 0.191833 0.789480 0.491437 11.00000 0.03523 0.02199 = 0.05074 -0.00989 0.00256 0.00230 AFIX 23 H16A 2 0.189159 0.873369 0.504675 11.00000 -1.20000 H16B 2 0.162369 0.750386 0.505522 11.00000 -1.20000 AFIX 0 C17 1 0.231610 0.735372 0.534376 11.00000 0.03385 0.02526 = 0.03011 -0.00773 0.00220 -0.00533 AFIX 23 H17A 2 0.224464 0.738834 0.587752 11.00000 -1.20000 H17B 2 0.260325 0.781327 0.525634 11.00000 -1.20000 AFIX 0 C18 1 0.239969 0.608602 0.512120 11.00000 0.02529 0.02308 = 0.02157 -0.00316 -0.00351 0.00076 AFIX 23 H18A 2 0.212338 0.560804 0.524814 11.00000 -1.20000 H18B 2 0.267008 0.577085 0.539581 11.00000 -1.20000 AFIX 0 C19 1 0.526740 0.502111 0.582494 11.00000 0.01761 0.02012 = 0.03041 -0.00583 -0.00517 -0.00483 AFIX 13 H19 2 0.552102 0.533436 0.614742 11.00000 -1.20000 AFIX 0 C20 1 0.513059 0.597232 0.527524 11.00000 0.03189 0.01703 = 0.03204 0.00152 0.01153 0.00330 AFIX 23 H20A 2 0.502022 0.667233 0.554626 11.00000 -1.20000 H20B 2 0.487163 0.568632 0.496293 11.00000 -1.20000 AFIX 0 C21 1 0.554213 0.630954 0.478639 11.00000 0.04010 0.03494 = 0.03882 -0.00426 0.01515 -0.01308 AFIX 23 H21A 2 0.544669 0.693246 0.443772 11.00000 -1.20000 H21B 2 0.579880 0.661737 0.509520 11.00000 -1.20000 AFIX 0 C22 1 0.570844 0.524576 0.436093 11.00000 0.03743 0.04979 = 0.04042 -0.01929 0.01797 -0.02046 AFIX 23 H22A 2 0.545550 0.496086 0.403610 11.00000 -1.20000 H22B 2 0.597630 0.546601 0.404635 11.00000 -1.20000 AFIX 0 C23 1 0.585193 0.428247 0.488356 11.00000 0.02268 0.05267 = 0.04912 -0.02987 0.00121 0.00239 AFIX 23 H23A 2 0.612417 0.454381 0.517542 11.00000 -1.20000 H23B 2 0.594565 0.358306 0.459668 11.00000 -1.20000 AFIX 0 C24 1 0.545788 0.395886 0.540135 11.00000 0.03614 0.02032 = 0.03626 -0.00314 -0.00843 0.00858 AFIX 23 H24A 2 0.557074 0.336782 0.575885 11.00000 -1.20000 H24B 2 0.520233 0.359960 0.511290 11.00000 -1.20000 AFIX 0 C25 1 0.459158 0.597961 0.684970 11.00000 0.02305 0.03185 = 0.01838 -0.00610 0.00127 -0.00346 AFIX 13 H25 2 0.447073 0.649894 0.644879 11.00000 -1.20000 AFIX 0 C26 1 0.497918 0.667649 0.723449 11.00000 0.03605 0.02146 = 0.03746 0.00112 -0.01552 -0.00267 AFIX 23 H26A 2 0.511026 0.620610 0.764364 11.00000 -1.20000 H26B 2 0.523261 0.684075 0.687901 11.00000 -1.20000 AFIX 0 C27 1 0.478708 0.783254 0.753759 11.00000 0.05134 0.02237 = 0.03963 -0.00391 -0.00653 -0.00213 AFIX 23 H27A 2 0.503486 0.823700 0.781925 11.00000 -1.20000 H27B 2 0.469712 0.834417 0.712028 11.00000 -1.20000 AFIX 0 C28 1 0.437201 0.765167 0.802974 11.00000 0.08765 0.04542 = 0.02969 -0.01538 0.01413 -0.01072 AFIX 23 H28A 2 0.424199 0.842222 0.817290 11.00000 -1.20000 H28B 2 0.447067 0.724142 0.848479 11.00000 -1.20000 AFIX 0 C29 1 0.399976 0.693778 0.764345 11.00000 0.05143 0.07426 = 0.07633 -0.04360 0.04605 -0.02141 AFIX 23 H29A 2 0.387568 0.739200 0.722178 11.00000 -1.20000 H29B 2 0.373987 0.679109 0.799015 11.00000 -1.20000 AFIX 0 C30 1 0.418660 0.577501 0.736596 11.00000 0.05640 0.07213 = 0.05079 -0.03515 0.03216 -0.03169 AFIX 23 H30A 2 0.428947 0.529129 0.778894 11.00000 -1.20000 H30B 2 0.393699 0.534536 0.710379 11.00000 -1.20000 AFIX 0 C31 1 0.496754 0.349042 0.702309 11.00000 0.03773 0.04816 = 0.06431 0.03484 -0.03046 -0.02037 AFIX 13 H31 2 0.510115 0.292608 0.665805 11.00000 -1.20000 AFIX 0 C32 1 0.539357 0.374258 0.747164 11.00000 0.02942 0.03217 = 0.03518 0.00760 -0.01758 0.00122 AFIX 23 H32A 2 0.564916 0.397125 0.713463 11.00000 -1.20000 H32B 2 0.532882 0.441835 0.779830 11.00000 -1.20000 AFIX 0 C33 1 0.555288 0.273817 0.793267 11.00000 0.06150 0.05886 = 0.12001 0.05332 -0.06094 -0.02096 AFIX 23 H33A 2 0.577072 0.226504 0.763196 11.00000 -1.20000 H33B 2 0.573337 0.306074 0.835127 11.00000 -1.20000 AFIX 0 C34 1 0.521049 0.196529 0.822685 11.00000 0.04949 0.07247 = 0.07990 0.04452 -0.02120 0.00608 AFIX 23 H34A 2 0.510999 0.228364 0.870922 11.00000 -1.20000 H34B 2 0.536332 0.120324 0.832414 11.00000 -1.20000 AFIX 0 C35 1 0.478460 0.173361 0.778154 11.00000 0.03933 0.02818 = 0.04572 0.01507 -0.00044 0.00161 AFIX 23 H35A 2 0.453308 0.147320 0.811711 11.00000 -1.20000 H35B 2 0.485037 0.108194 0.743651 11.00000 -1.20000 AFIX 0 C36 1 0.461315 0.276369 0.734637 11.00000 0.04127 0.06766 = 0.10380 0.05578 -0.03643 -0.01948 AFIX 23 H36A 2 0.440936 0.247063 0.694641 11.00000 -1.20000 H36B 2 0.441929 0.325700 0.767420 11.00000 -1.20000 AFIX 0 C37 1 0.448945 0.055067 0.534486 11.00000 0.02415 0.01821 = 0.02611 -0.00327 0.00155 0.00318 AFIX 13 H37 2 0.455328 0.099488 0.580944 11.00000 -1.20000 AFIX 0 C38 1 0.481700 0.106899 0.476044 11.00000 0.02458 0.02529 = 0.03259 0.00362 0.00255 -0.00259 AFIX 23 H38A 2 0.477332 0.064718 0.428833 11.00000 -1.20000 H38B 2 0.473721 0.190290 0.467886 11.00000 -1.20000 AFIX 0 C39 1 0.532683 0.097406 0.499967 11.00000 0.02331 0.03196 = 0.04284 0.00671 0.00436 -0.00136 AFIX 23 H39A 2 0.552938 0.127116 0.459932 11.00000 -1.20000 H39B 2 0.537801 0.147066 0.544000 11.00000 -1.20000 AFIX 0 C40 1 0.546152 -0.028055 0.517848 11.00000 0.02557 0.02882 = 0.04857 -0.00411 -0.00245 0.00617 AFIX 23 H40A 2 0.578578 -0.030313 0.536342 11.00000 -1.20000 H40B 2 0.544480 -0.076416 0.472594 11.00000 -1.20000 AFIX 0 C41 1 0.513404 -0.077762 0.576036 11.00000 0.02945 0.02021 = 0.04602 -0.00061 -0.00183 -0.00010 AFIX 23 H41A 2 0.516954 -0.032839 0.622410 11.00000 -1.20000 H41B 2 0.521873 -0.160281 0.586215 11.00000 -1.20000 AFIX 0 C42 1 0.462557 -0.071889 0.550504 11.00000 0.02439 0.02017 = 0.03361 0.00068 -0.00157 -0.00176 AFIX 23 H42A 2 0.458530 -0.119764 0.505417 11.00000 -1.20000 H42B 2 0.442015 -0.104252 0.589340 11.00000 -1.20000 AFIX 0 C43 1 0.353327 0.010891 0.586545 11.00000 0.02559 0.01836 = 0.01997 -0.00043 0.00128 -0.00416 AFIX 13 H43 2 0.354710 -0.076052 0.580047 11.00000 -1.20000 AFIX 0 C44 1 0.373108 0.041589 0.662872 11.00000 0.03170 0.02327 = 0.02360 -0.00519 -0.00080 -0.00266 AFIX 23 H44A 2 0.405345 0.011470 0.666798 11.00000 -1.20000 H44B 2 0.374179 0.127829 0.668516 11.00000 -1.20000 AFIX 0 C45 1 0.343605 -0.010734 0.724436 11.00000 0.04298 0.03811 = 0.02341 0.00190 0.00275 -0.00310 AFIX 23 H45A 2 0.345073 -0.097284 0.721596 11.00000 -1.20000 H45B 2 0.356571 0.013406 0.772697 11.00000 -1.20000 AFIX 0 C46 1 0.293226 0.028097 0.719543 11.00000 0.03908 0.03896 = 0.02561 -0.00400 0.01160 -0.01360 AFIX 23 H46A 2 0.291255 0.113792 0.727422 11.00000 -1.20000 H46B 2 0.274858 -0.010955 0.758672 11.00000 -1.20000 AFIX 0 C47 1 0.273032 -0.002626 0.644363 11.00000 0.03018 0.03970 = 0.02815 -0.00340 0.00675 -0.01181 AFIX 23 H47A 2 0.240796 0.027643 0.640934 11.00000 -1.20000 H47B 2 0.271873 -0.088881 0.638862 11.00000 -1.20000 AFIX 0 C48 1 0.302291 0.049567 0.582196 11.00000 0.02403 0.03168 = 0.02427 0.00249 0.00443 -0.00536 AFIX 23 H48A 2 0.300710 0.136123 0.584805 11.00000 -1.20000 H48B 2 0.289128 0.024986 0.534157 11.00000 -1.20000 AFIX 0 C49 1 0.376581 0.011986 0.423911 11.00000 0.02633 0.02156 = 0.02259 -0.00346 0.00112 -0.00183 AFIX 13 H49 2 0.400935 -0.049751 0.417272 11.00000 -1.20000 AFIX 0 C50 1 0.329688 -0.048176 0.411639 11.00000 0.02696 0.03078 = 0.03062 -0.00340 -0.00185 -0.00196 AFIX 23 H50A 2 0.325051 -0.109380 0.449632 11.00000 -1.20000 H50B 2 0.304305 0.009988 0.416628 11.00000 -1.20000 AFIX 0 C51 1 0.327721 -0.103609 0.335295 11.00000 0.03130 0.03070 = 0.03904 -0.01016 -0.00565 0.00148 AFIX 23 H51A 2 0.296559 -0.138679 0.327654 11.00000 -1.20000 H51B 2 0.351049 -0.167312 0.332370 11.00000 -1.20000 AFIX 0 C52 1 0.337217 -0.014599 0.274180 11.00000 0.04005 0.05320 = 0.02786 -0.00729 -0.00979 -0.00027 AFIX 23 H52A 2 0.338446 -0.055673 0.226123 11.00000 -1.20000 H52B 2 0.311320 0.042582 0.272256 11.00000 -1.20000 AFIX 0 C53 1 0.382680 0.050282 0.286485 11.00000 0.04985 0.04607 = 0.02421 -0.00221 -0.00323 -0.00510 AFIX 23 H53A 2 0.385740 0.113354 0.249311 11.00000 -1.20000 H53B 2 0.409041 -0.004601 0.279785 11.00000 -1.20000 AFIX 0 C54 1 0.384956 0.103171 0.363240 11.00000 0.03169 0.03284 = 0.02323 0.00306 -0.00026 0.00090 AFIX 23 H54A 2 0.361256 0.165822 0.367413 11.00000 -1.20000 H54B 2 0.415949 0.139336 0.370577 11.00000 -1.20000 AFIX 0 HKLF 4 REM save_a.res in Pca2(1) REM R1 = 0.0317 for 11537 Fo > 4sig(Fo) and 0.0481 for all 13677 data REM 578 parameters refined using 1 restraints END WGHT 0.0056 11.3965 REM Highest difference peak 0.990, deepest hole -0.720, 1-sigma level 0.101 Q1 1 0.3725 0.2988 0.5159 11.00000 0.05 0.99 Q2 1 0.3724 0.1545 0.5206 11.00000 0.05 0.92 Q3 1 0.3636 0.4544 0.5376 11.00000 0.05 0.80 Q4 1 0.3792 0.5566 0.5197 11.00000 0.05 0.76 Q5 1 0.4326 0.4147 0.6451 11.00000 0.05 0.73 Q6 1 0.3172 0.6475 0.6499 11.00000 0.05 0.69 Q7 1 0.2025 0.6772 0.1881 11.00000 0.05 0.68 Q8 1 0.3147 0.4119 0.3907 11.00000 0.05 0.66 Q9 1 0.4819 0.3817 0.7341 11.00000 0.05 0.65 Q10 1 0.3644 0.3894 0.5032 11.00000 0.05 0.65 ; _shelx_res_checksum 12027 _olex2_exptl_crystal_mounting_method 'nylon loop' _olex2_submission_original_sample_id cjw94 _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 Pr1 Pr 0.37364(2) 0.41310(2) 0.51857(2) 0.01182(6) Uani 1 1 d . Br1 Br 0.43340(2) 0.40949(6) 0.39115(3) 0.02659(14) Uani 1 1 d . Br2 Br 0.31582(2) 0.38720(5) 0.64797(3) 0.02616(14) Uani 1 1 d . Br3 Br 0.37307(2) 0.66847(4) 0.51982(6) 0.03035(12) Uani 1 1 d . P1 P 0.26617(5) 0.45432(13) 0.40115(8) 0.0169(3) Uani 1 1 d . P2 P 0.47780(5) 0.46430(14) 0.64001(9) 0.0192(3) Uani 1 1 d . P3 P 0.38750(4) 0.07901(11) 0.51390(11) 0.0192(3) Uani 1 1 d . O1 O 0.30876(13) 0.4182(4) 0.4448(2) 0.0184(8) Uani 1 1 d . O2 O 0.43832(13) 0.4162(3) 0.5936(2) 0.0193(8) Uani 1 1 d . O3 O 0.37733(13) 0.2088(3) 0.5132(3) 0.0204(8) Uani 1 1 d . C1 C 0.2175(2) 0.3547(5) 0.4202(3) 0.0200(12) Uani 1 1 d . H1 H 0.195568 0.398294 0.453046 0.024 Uiso 1 1 calc R C2 C 0.2347(2) 0.2492(6) 0.4644(4) 0.0324(16) Uani 1 1 d . H2A H 0.258377 0.206333 0.435365 0.039 Uiso 1 1 calc R H2B H 0.249499 0.276687 0.510539 0.039 Uiso 1 1 calc R C3 C 0.1946(2) 0.1671(6) 0.4830(4) 0.0359(16) Uani 1 1 d . H3A H 0.206897 0.097994 0.509611 0.043 Uiso 1 1 calc R H3B H 0.172474 0.207909 0.516007 0.043 Uiso 1 1 calc R C4 C 0.1691(2) 0.1266(6) 0.4141(4) 0.0308(15) Uani 1 1 d . H4A H 0.190580 0.081371 0.382254 0.037 Uiso 1 1 calc R H4B H 0.142913 0.074735 0.428133 0.037 Uiso 1 1 calc R C5 C 0.1506(2) 0.2316(6) 0.3718(4) 0.0287(15) Uani 1 1 d . H5A H 0.126813 0.272071 0.402135 0.034 Uiso 1 1 calc R H5B H 0.135319 0.204317 0.325989 0.034 Uiso 1 1 calc R C6 C 0.1895(2) 0.3187(6) 0.3521(3) 0.0240(14) Uani 1 1 d . H6A H 0.210689 0.282233 0.315549 0.029 Uiso 1 1 calc R H6B H 0.175682 0.389297 0.329204 0.029 Uiso 1 1 calc R C7 C 0.2803(2) 0.4526(5) 0.3032(3) 0.0215(12) Uani 1 1 d . H7 H 0.250740 0.458605 0.274327 0.026 Uiso 1 1 calc R C8 C 0.3042(2) 0.3369(5) 0.2835(3) 0.0254(13) Uani 1 1 d . H8A H 0.283565 0.270690 0.296826 0.030 Uiso 1 1 calc R H8B H 0.333348 0.329123 0.312340 0.030 Uiso 1 1 calc R C9 C 0.3155(2) 0.3314(7) 0.2010(4) 0.0327(16) Uani 1 1 d . H9A H 0.331689 0.256874 0.189811 0.039 Uiso 1 1 calc R H9B H 0.286213 0.333372 0.172209 0.039 Uiso 1 1 calc R C10 C 0.3463(2) 0.4343(7) 0.1787(4) 0.0385(18) Uani 1 1 d . H10A H 0.376829 0.427438 0.203651 0.046 Uiso 1 1 calc R H10B H 0.351672 0.432018 0.124827 0.046 Uiso 1 1 calc R C11 C 0.3239(3) 0.5497(6) 0.1993(4) 0.0382(17) Uani 1 1 d . H11A H 0.295010 0.560049 0.170210 0.046 Uiso 1 1 calc R H11B H 0.345339 0.614489 0.186521 0.046 Uiso 1 1 calc R C12 C 0.3120(2) 0.5564(6) 0.2821(3) 0.0291(14) Uani 1 1 d . H12A H 0.295981 0.631222 0.292855 0.035 Uiso 1 1 calc R H12B H 0.341054 0.553649 0.311529 0.035 Uiso 1 1 calc R C13 C 0.2494(2) 0.6006(5) 0.4285(3) 0.0219(12) Uani 1 1 d . H13 H 0.276639 0.652531 0.418120 0.026 Uiso 1 1 calc R C14 C 0.2079(2) 0.6519(5) 0.3855(4) 0.0265(13) Uani 1 1 d . H14A H 0.214610 0.649175 0.331934 0.032 Uiso 1 1 calc R H14B H 0.179772 0.603880 0.394833 0.032 Uiso 1 1 calc R C15 C 0.1986(2) 0.7787(5) 0.4088(4) 0.0340(16) Uani 1 1 d . H15A H 0.225212 0.828283 0.393504 0.041 Uiso 1 1 calc R H15B H 0.170436 0.807750 0.383262 0.041 Uiso 1 1 calc R C16 C 0.1918(2) 0.7895(6) 0.4914(4) 0.0360(17) Uani 1 1 d . H16A H 0.189159 0.873369 0.504675 0.043 Uiso 1 1 calc R H16B H 0.162369 0.750386 0.505522 0.043 Uiso 1 1 calc R C17 C 0.2316(2) 0.7354(5) 0.5344(3) 0.0297(15) Uani 1 1 d . H17A H 0.224464 0.738834 0.587752 0.036 Uiso 1 1 calc R H17B H 0.260325 0.781327 0.525634 0.036 Uiso 1 1 calc R C18 C 0.2400(2) 0.6086(4) 0.5121(4) 0.0233(12) Uani 1 1 d . H18A H 0.212338 0.560804 0.524814 0.028 Uiso 1 1 calc R H18B H 0.267008 0.577085 0.539581 0.028 Uiso 1 1 calc R C19 C 0.5267(2) 0.5021(5) 0.5825(3) 0.0227(13) Uani 1 1 d . H19 H 0.552102 0.533436 0.614742 0.027 Uiso 1 1 calc R C20 C 0.5131(2) 0.5972(5) 0.5275(4) 0.0270(14) Uani 1 1 d . H20A H 0.502022 0.667233 0.554626 0.032 Uiso 1 1 calc R H20B H 0.487163 0.568632 0.496293 0.032 Uiso 1 1 calc R C21 C 0.5542(2) 0.6310(6) 0.4786(4) 0.0380(17) Uani 1 1 d . H21A H 0.544669 0.693246 0.443772 0.046 Uiso 1 1 calc R H21B H 0.579880 0.661737 0.509520 0.046 Uiso 1 1 calc R C22 C 0.5708(3) 0.5246(7) 0.4361(4) 0.0425(19) Uani 1 1 d . H22A H 0.545550 0.496086 0.403610 0.051 Uiso 1 1 calc R H22B H 0.597630 0.546601 0.404635 0.051 Uiso 1 1 calc R C23 C 0.5852(2) 0.4282(7) 0.4884(4) 0.0415(19) Uani 1 1 d . H23A H 0.612417 0.454381 0.517542 0.050 Uiso 1 1 calc R H23B H 0.594565 0.358306 0.459668 0.050 Uiso 1 1 calc R C24 C 0.5458(2) 0.3959(5) 0.5401(4) 0.0309(15) Uani 1 1 d . H24A H 0.557074 0.336782 0.575885 0.037 Uiso 1 1 calc R H24B H 0.520233 0.359960 0.511290 0.037 Uiso 1 1 calc R C25 C 0.4592(2) 0.5980(6) 0.6850(3) 0.0244(13) Uani 1 1 d . H25 H 0.447073 0.649894 0.644879 0.029 Uiso 1 1 calc R C26 C 0.4979(2) 0.6676(5) 0.7234(4) 0.0317(15) Uani 1 1 d . H26A H 0.511026 0.620610 0.764364 0.038 Uiso 1 1 calc R H26B H 0.523261 0.684075 0.687901 0.038 Uiso 1 1 calc R C27 C 0.4787(3) 0.7833(6) 0.7538(4) 0.0378(17) Uani 1 1 d . H27A H 0.503486 0.823700 0.781925 0.045 Uiso 1 1 calc R H27B H 0.469712 0.834417 0.712028 0.045 Uiso 1 1 calc R C28 C 0.4372(3) 0.7652(7) 0.8030(4) 0.054(2) Uani 1 1 d . H28A H 0.424199 0.842222 0.817290 0.065 Uiso 1 1 calc R H28B H 0.447067 0.724142 0.848479 0.065 Uiso 1 1 calc R C29 C 0.4000(3) 0.6938(8) 0.7643(5) 0.067(3) Uani 1 1 d . H29A H 0.387568 0.739200 0.722178 0.081 Uiso 1 1 calc R H29B H 0.373987 0.679109 0.799015 0.081 Uiso 1 1 calc R C30 C 0.4187(3) 0.5775(8) 0.7366(5) 0.060(3) Uani 1 1 d . H30A H 0.428947 0.529129 0.778894 0.072 Uiso 1 1 calc R H30B H 0.393699 0.534536 0.710379 0.072 Uiso 1 1 calc R C31 C 0.4968(3) 0.3490(7) 0.7023(5) 0.050(2) Uani 1 1 d . H31 H 0.510115 0.292608 0.665805 0.060 Uiso 1 1 calc R C32 C 0.5394(2) 0.3743(6) 0.7472(4) 0.0323(16) Uani 1 1 d . H32A H 0.564916 0.397125 0.713463 0.039 Uiso 1 1 calc R H32B H 0.532882 0.441835 0.779830 0.039 Uiso 1 1 calc R C33 C 0.5553(3) 0.2738(8) 0.7933(6) 0.080(4) Uani 1 1 d . H33A H 0.577072 0.226504 0.763196 0.096 Uiso 1 1 calc R H33B H 0.573337 0.306074 0.835127 0.096 Uiso 1 1 calc R C34 C 0.5210(3) 0.1965(9) 0.8227(6) 0.067(3) Uani 1 1 d . H34A H 0.510999 0.228364 0.870922 0.081 Uiso 1 1 calc R H34B H 0.536332 0.120324 0.832414 0.081 Uiso 1 1 calc R C35 C 0.4785(2) 0.1734(6) 0.7782(4) 0.0377(17) Uani 1 1 d . H35A H 0.453308 0.147320 0.811711 0.045 Uiso 1 1 calc R H35B H 0.485037 0.108194 0.743651 0.045 Uiso 1 1 calc R C36 C 0.4613(3) 0.2764(8) 0.7346(6) 0.071(3) Uani 1 1 d . H36A H 0.440936 0.247063 0.694641 0.085 Uiso 1 1 calc R H36B H 0.441929 0.325700 0.767420 0.085 Uiso 1 1 calc R C37 C 0.44895(19) 0.0551(5) 0.5345(3) 0.0228(14) Uani 1 1 d . H37 H 0.455328 0.099488 0.580944 0.027 Uiso 1 1 calc R C38 C 0.4817(2) 0.1069(5) 0.4760(3) 0.0275(14) Uani 1 1 d . H38A H 0.477332 0.064718 0.428833 0.033 Uiso 1 1 calc R H38B H 0.473721 0.190290 0.467886 0.033 Uiso 1 1 calc R C39 C 0.5327(2) 0.0974(6) 0.5000(4) 0.0327(16) Uani 1 1 d . H39A H 0.552938 0.127116 0.459932 0.039 Uiso 1 1 calc R H39B H 0.537801 0.147066 0.544000 0.039 Uiso 1 1 calc R C40 C 0.5462(2) -0.0281(5) 0.5178(5) 0.0343(13) Uani 1 1 d . H40A H 0.578578 -0.030313 0.536342 0.041 Uiso 1 1 calc R H40B H 0.544480 -0.076416 0.472594 0.041 Uiso 1 1 calc R C41 C 0.5134(2) -0.0778(6) 0.5760(4) 0.0319(15) Uani 1 1 d . H41A H 0.516954 -0.032839 0.622410 0.038 Uiso 1 1 calc R H41B H 0.521873 -0.160281 0.586215 0.038 Uiso 1 1 calc R C42 C 0.4626(2) -0.0719(5) 0.5505(4) 0.0261(13) Uani 1 1 d . H42A H 0.458530 -0.119764 0.505417 0.031 Uiso 1 1 calc R H42B H 0.442015 -0.104252 0.589340 0.031 Uiso 1 1 calc R C43 C 0.3533(2) 0.0109(5) 0.5865(3) 0.0213(13) Uani 1 1 d . H43 H 0.354710 -0.076052 0.580047 0.026 Uiso 1 1 calc R C44 C 0.3731(2) 0.0416(6) 0.6629(3) 0.0262(13) Uani 1 1 d . H44A H 0.405345 0.011470 0.666798 0.031 Uiso 1 1 calc R H44B H 0.374179 0.127829 0.668516 0.031 Uiso 1 1 calc R C45 C 0.3436(3) -0.0107(6) 0.7244(4) 0.0348(16) Uani 1 1 d . H45A H 0.345073 -0.097284 0.721596 0.042 Uiso 1 1 calc R H45B H 0.356571 0.013406 0.772697 0.042 Uiso 1 1 calc R C46 C 0.2932(2) 0.0281(6) 0.7195(4) 0.0345(16) Uani 1 1 d . H46A H 0.291255 0.113792 0.727422 0.041 Uiso 1 1 calc R H46B H 0.274858 -0.010955 0.758672 0.041 Uiso 1 1 calc R C47 C 0.2730(2) -0.0026(6) 0.6444(4) 0.0327(15) Uani 1 1 d . H47A H 0.240796 0.027643 0.640934 0.039 Uiso 1 1 calc R H47B H 0.271873 -0.088881 0.638862 0.039 Uiso 1 1 calc R C48 C 0.3023(2) 0.0496(6) 0.5822(3) 0.0267(14) Uani 1 1 d . H48A H 0.300710 0.136123 0.584805 0.032 Uiso 1 1 calc R H48B H 0.289128 0.024986 0.534157 0.032 Uiso 1 1 calc R C49 C 0.3766(2) 0.0120(5) 0.4239(3) 0.0235(13) Uani 1 1 d . H49 H 0.400935 -0.049751 0.417272 0.028 Uiso 1 1 calc R C50 C 0.3297(2) -0.0482(6) 0.4116(3) 0.0295(14) Uani 1 1 d . H50A H 0.325051 -0.109380 0.449632 0.035 Uiso 1 1 calc R H50B H 0.304305 0.009988 0.416628 0.035 Uiso 1 1 calc R C51 C 0.3277(2) -0.1036(6) 0.3353(4) 0.0337(15) Uani 1 1 d . H51A H 0.296559 -0.138679 0.327654 0.040 Uiso 1 1 calc R H51B H 0.351049 -0.167312 0.332370 0.040 Uiso 1 1 calc R C52 C 0.3372(3) -0.0146(7) 0.2742(4) 0.0404(18) Uani 1 1 d . H52A H 0.338446 -0.055673 0.226123 0.048 Uiso 1 1 calc R H52B H 0.311320 0.042582 0.272256 0.048 Uiso 1 1 calc R C53 C 0.3827(3) 0.0503(7) 0.2865(4) 0.0400(17) Uani 1 1 d . H53A H 0.385740 0.113354 0.249311 0.048 Uiso 1 1 calc R H53B H 0.409041 -0.004601 0.279785 0.048 Uiso 1 1 calc R C54 C 0.3850(2) 0.1032(6) 0.3632(3) 0.0293(15) Uani 1 1 d . H54A H 0.361256 0.165822 0.367413 0.035 Uiso 1 1 calc R H54B H 0.415949 0.139336 0.370577 0.035 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 Pr1 0.01124(10) 0.01453(11) 0.00968(10) 0.00015(19) -0.00072(11) -0.00092(11) Br1 0.0286(3) 0.0327(3) 0.0185(3) -0.0009(3) 0.0102(3) -0.0058(3) Br2 0.0250(3) 0.0356(3) 0.0179(3) -0.0001(3) 0.0083(3) -0.0022(3) Br3 0.0290(3) 0.0157(2) 0.0463(3) 0.0001(4) -0.0089(3) -0.0008(2) P1 0.0165(7) 0.0196(7) 0.0146(7) 0.0006(6) -0.0037(6) -0.0014(6) P2 0.0174(7) 0.0211(7) 0.0190(8) 0.0028(7) -0.0065(6) -0.0018(6) P3 0.0220(6) 0.0148(6) 0.0208(7) -0.0007(8) 0.0018(8) -0.0002(5) O1 0.0148(19) 0.024(2) 0.016(2) -0.0005(17) -0.0063(15) 0.0006(17) O2 0.0148(19) 0.022(2) 0.021(2) 0.0023(18) -0.0054(16) -0.0023(17) O3 0.0215(17) 0.0203(17) 0.0196(19) -0.004(2) 0.0013(18) 0.0024(15) C1 0.022(3) 0.021(3) 0.017(3) -0.002(2) -0.001(2) 0.000(2) C2 0.038(4) 0.032(4) 0.027(3) 0.011(3) -0.013(3) -0.010(3) C3 0.040(4) 0.036(4) 0.031(4) 0.012(3) -0.005(3) -0.012(3) C4 0.028(3) 0.025(3) 0.039(4) 0.000(3) -0.001(3) -0.011(3) C5 0.019(3) 0.031(4) 0.036(4) -0.005(3) -0.003(3) -0.004(3) C6 0.021(3) 0.028(3) 0.024(3) -0.001(3) -0.004(3) -0.004(3) C7 0.020(3) 0.030(3) 0.015(3) 0.002(2) -0.002(2) 0.002(3) C8 0.021(3) 0.031(4) 0.025(3) 0.001(3) 0.003(2) 0.001(3) C9 0.026(4) 0.044(4) 0.028(3) -0.005(3) 0.001(3) 0.006(3) C10 0.033(4) 0.060(5) 0.022(3) 0.006(3) 0.008(3) 0.004(3) C11 0.040(4) 0.049(5) 0.025(3) 0.014(3) 0.006(3) -0.003(3) C12 0.031(3) 0.031(4) 0.025(3) 0.006(3) -0.003(3) -0.006(3) C13 0.022(3) 0.022(3) 0.021(3) 0.003(2) -0.005(2) -0.001(3) C14 0.023(3) 0.028(3) 0.028(3) 0.000(3) -0.005(3) 0.002(3) C15 0.030(4) 0.025(3) 0.047(4) 0.005(3) -0.008(3) 0.004(3) C16 0.035(4) 0.022(3) 0.051(4) -0.010(3) 0.003(3) 0.002(3) C17 0.034(3) 0.025(3) 0.030(4) -0.008(3) 0.002(3) -0.005(3) C18 0.025(3) 0.023(3) 0.022(3) -0.003(3) -0.004(3) 0.001(2) C19 0.018(3) 0.020(3) 0.030(3) -0.006(2) -0.005(3) -0.005(2) C20 0.032(3) 0.017(3) 0.032(4) 0.002(3) 0.012(3) 0.003(2) C21 0.040(4) 0.035(4) 0.039(4) -0.004(3) 0.015(3) -0.013(3) C22 0.037(4) 0.050(5) 0.040(4) -0.019(4) 0.018(3) -0.020(4) C23 0.023(3) 0.053(5) 0.049(4) -0.030(4) 0.001(3) 0.002(3) C24 0.036(4) 0.020(3) 0.036(4) -0.003(3) -0.008(3) 0.009(3) C25 0.023(3) 0.032(3) 0.018(3) -0.006(3) 0.001(2) -0.003(3) C26 0.036(4) 0.021(3) 0.037(4) 0.001(3) -0.016(3) -0.003(3) C27 0.051(5) 0.022(4) 0.040(4) -0.004(3) -0.007(4) -0.002(3) C28 0.088(7) 0.045(5) 0.030(4) -0.015(4) 0.014(4) -0.011(5) C29 0.051(5) 0.074(6) 0.076(6) -0.044(5) 0.046(5) -0.021(5) C30 0.056(5) 0.072(6) 0.051(5) -0.035(5) 0.032(4) -0.032(5) C31 0.038(4) 0.048(5) 0.064(5) 0.035(4) -0.030(4) -0.020(4) C32 0.029(3) 0.032(4) 0.035(4) 0.008(3) -0.018(3) 0.001(3) C33 0.062(6) 0.059(6) 0.120(9) 0.053(6) -0.061(6) -0.021(5) C34 0.049(5) 0.072(7) 0.080(7) 0.045(6) -0.021(5) 0.006(5) C35 0.039(4) 0.028(4) 0.046(4) 0.015(3) 0.000(3) 0.002(3) C36 0.041(5) 0.068(6) 0.104(8) 0.056(6) -0.036(5) -0.019(4) C37 0.024(3) 0.018(3) 0.026(4) -0.003(2) 0.002(2) 0.003(2) C38 0.025(3) 0.025(3) 0.033(3) 0.004(3) 0.003(3) -0.003(3) C39 0.023(3) 0.032(4) 0.043(4) 0.007(3) 0.004(3) -0.001(3) C40 0.026(3) 0.029(3) 0.049(4) -0.004(4) -0.002(4) 0.006(2) C41 0.029(3) 0.020(3) 0.046(4) -0.001(3) -0.002(3) 0.000(3) C42 0.024(3) 0.020(3) 0.034(3) 0.001(3) -0.002(3) -0.002(3) C43 0.026(4) 0.018(3) 0.020(3) 0.000(2) 0.001(3) -0.004(3) C44 0.032(3) 0.023(3) 0.024(3) -0.005(3) -0.001(3) -0.003(3) C45 0.043(4) 0.038(4) 0.023(4) 0.002(3) 0.003(3) -0.003(3) C46 0.039(4) 0.039(4) 0.026(3) -0.004(3) 0.012(3) -0.014(3) C47 0.030(3) 0.040(4) 0.028(3) -0.003(3) 0.007(3) -0.012(3) C48 0.024(3) 0.032(4) 0.024(3) 0.002(3) 0.004(2) -0.005(3) C49 0.026(3) 0.022(3) 0.023(3) -0.003(3) 0.001(3) -0.002(3) C50 0.027(3) 0.031(4) 0.031(3) -0.003(3) -0.002(3) -0.002(3) C51 0.031(4) 0.031(4) 0.039(4) -0.010(3) -0.006(3) 0.001(3) C52 0.040(4) 0.053(5) 0.028(4) -0.007(3) -0.010(3) 0.000(4) C53 0.050(5) 0.046(4) 0.024(3) -0.002(3) -0.003(3) -0.005(4) C54 0.032(3) 0.033(4) 0.023(3) 0.003(3) 0.000(3) 0.001(3) 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' Pr Pr -0.2180 2.8214 '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 Pr1 Br2 173.18(2) Br1 Pr1 Br3 91.37(3) Br2 Pr1 Br3 95.32(2) O1 Pr1 Br1 90.95(10) O1 Pr1 Br2 90.53(10) O1 Pr1 Br3 88.55(10) O1 Pr1 O2 177.63(13) O1 Pr1 O3 92.17(15) O2 Pr1 Br1 89.61(10) O2 Pr1 Br2 89.18(10) O2 Pr1 Br3 89.13(10) O2 Pr1 O3 90.17(15) O3 Pr1 Br1 85.72(12) O3 Pr1 Br2 87.57(12) O3 Pr1 Br3 177.02(11) O1 P1 C1 110.3(2) O1 P1 C7 109.0(2) O1 P1 C13 108.9(2) C7 P1 C1 110.3(3) C13 P1 C1 108.5(3) C13 P1 C7 109.7(3) O2 P2 C19 110.4(3) O2 P2 C25 109.5(3) O2 P2 C31 107.9(3) C19 P2 C25 106.8(3) C19 P2 C31 107.4(3) C25 P2 C31 114.8(4) O3 P3 C37 109.6(2) O3 P3 C43 108.7(3) O3 P3 C49 111.7(3) C37 P3 C49 106.6(3) C43 P3 C37 108.1(3) C43 P3 C49 112.0(3) P1 O1 Pr1 165.4(3) P2 O2 Pr1 159.6(3) P3 O3 Pr1 171.0(3) P1 C1 H1 106.5 C2 C1 P1 110.0(4) C2 C1 H1 106.5 C2 C1 C6 112.4(5) C6 C1 P1 114.5(4) C6 C1 H1 106.5 C1 C2 H2A 109.4 C1 C2 H2B 109.4 H2A C2 H2B 108.0 C3 C2 C1 111.0(5) C3 C2 H2A 109.4 C3 C2 H2B 109.4 C2 C3 H3A 109.3 C2 C3 H3B 109.3 H3A C3 H3B 107.9 C4 C3 C2 111.7(5) C4 C3 H3A 109.3 C4 C3 H3B 109.3 C3 C4 H4A 109.7 C3 C4 H4B 109.7 H4A C4 H4B 108.2 C5 C4 C3 110.1(5) C5 C4 H4A 109.7 C5 C4 H4B 109.7 C4 C5 H5A 109.2 C4 C5 H5B 109.2 C4 C5 C6 111.9(5) H5A C5 H5B 107.9 C6 C5 H5A 109.2 C6 C5 H5B 109.2 C1 C6 C5 111.5(5) C1 C6 H6A 109.3 C1 C6 H6B 109.3 C5 C6 H6A 109.3 C5 C6 H6B 109.3 H6A C6 H6B 108.0 P1 C7 H7 108.6 C8 C7 P1 109.6(4) C8 C7 H7 108.6 C8 C7 C12 109.9(5) C12 C7 P1 111.4(4) C12 C7 H7 108.6 C7 C8 H8A 109.5 C7 C8 H8B 109.5 C7 C8 C9 110.9(5) H8A C8 H8B 108.0 C9 C8 H8A 109.5 C9 C8 H8B 109.5 C8 C9 H9A 109.6 C8 C9 H9B 109.6 H9A C9 H9B 108.1 C10 C9 C8 110.5(6) C10 C9 H9A 109.6 C10 C9 H9B 109.6 C9 C10 H10A 109.4 C9 C10 H10B 109.4 H10A C10 H10B 108.0 C11 C10 C9 111.1(6) C11 C10 H10A 109.4 C11 C10 H10B 109.4 C10 C11 H11A 109.2 C10 C11 H11B 109.2 C10 C11 C12 112.2(5) H11A C11 H11B 107.9 C12 C11 H11A 109.2 C12 C11 H11B 109.2 C7 C12 H12A 109.8 C7 C12 H12B 109.8 C11 C12 C7 109.5(5) C11 C12 H12A 109.8 C11 C12 H12B 109.8 H12A C12 H12B 108.2 P1 C13 H13 106.6 C14 C13 P1 114.8(4) C14 C13 H13 106.6 C14 C13 C18 109.9(5) C18 C13 P1 111.7(4) C18 C13 H13 106.6 C13 C14 H14A 109.5 C13 C14 H14B 109.5 H14A C14 H14B 108.1 C15 C14 C13 110.7(5) C15 C14 H14A 109.5 C15 C14 H14B 109.5 C14 C15 H15A 109.2 C14 C15 H15B 109.2 H15A C15 H15B 107.9 C16 C15 C14 111.9(5) 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 112.2(5) C17 C16 H16A 109.2 C17 C16 H16B 109.2 C16 C17 H17A 109.3 C16 C17 H17B 109.3 C16 C17 C18 111.8(5) H17A C17 H17B 107.9 C18 C17 H17A 109.3 C18 C17 H17B 109.3 C13 C18 H18A 109.6 C13 C18 H18B 109.6 C17 C18 C13 110.1(5) C17 C18 H18A 109.6 C17 C18 H18B 109.6 H18A C18 H18B 108.1 P2 C19 H19 108.4 C20 C19 P2 110.3(4) C20 C19 H19 108.4 C20 C19 C24 109.1(5) C24 C19 P2 112.2(4) C24 C19 H19 108.4 C19 C20 H20A 109.4 C19 C20 H20B 109.4 C19 C20 C21 111.1(5) H20A C20 H20B 108.0 C21 C20 H20A 109.4 C21 C20 H20B 109.4 C20 C21 H21A 109.7 C20 C21 H21B 109.7 H21A C21 H21B 108.2 C22 C21 C20 109.7(5) C22 C21 H21A 109.7 C22 C21 H21B 109.7 C21 C22 H22A 109.6 C21 C22 H22B 109.6 H22A C22 H22B 108.1 C23 C22 C21 110.5(6) C23 C22 H22A 109.6 C23 C22 H22B 109.6 C22 C23 H23A 109.4 C22 C23 H23B 109.4 C22 C23 C24 111.3(6) H23A C23 H23B 108.0 C24 C23 H23A 109.4 C24 C23 H23B 109.4 C19 C24 H24A 109.1 C19 C24 H24B 109.1 C23 C24 C19 112.5(5) C23 C24 H24A 109.1 C23 C24 H24B 109.1 H24A C24 H24B 107.8 P2 C25 H25 105.9 C26 C25 P2 115.3(4) C26 C25 H25 105.9 C30 C25 P2 112.1(5) C30 C25 H25 105.9 C30 C25 C26 110.9(5) C25 C26 H26A 109.6 C25 C26 H26B 109.6 H26A C26 H26B 108.1 C27 C26 C25 110.4(6) C27 C26 H26A 109.6 C27 C26 H26B 109.6 C26 C27 H27A 109.1 C26 C27 H27B 109.1 H27A C27 H27B 107.9 C28 C27 C26 112.3(6) C28 C27 H27A 109.1 C28 C27 H27B 109.1 C27 C28 H28A 109.4 C27 C28 H28B 109.4 C27 C28 C29 111.0(6) H28A C28 H28B 108.0 C29 C28 H28A 109.4 C29 C28 H28B 109.4 C28 C29 H29A 109.2 C28 C29 H29B 109.2 C28 C29 C30 112.0(8) H29A C29 H29B 107.9 C30 C29 H29A 109.2 C30 C29 H29B 109.2 C25 C30 C29 110.0(7) C25 C30 H30A 109.7 C25 C30 H30B 109.7 C29 C30 H30A 109.7 C29 C30 H30B 109.7 H30A C30 H30B 108.2 P2 C31 H31 99.8 C32 C31 P2 116.3(5) C32 C31 H31 99.8 C36 C31 P2 117.3(5) C36 C31 H31 99.8 C36 C31 C32 117.9(7) C31 C32 H32A 108.7 C31 C32 H32B 108.7 H32A C32 H32B 107.6 C33 C32 C31 114.1(6) C33 C32 H32A 108.7 C33 C32 H32B 108.7 C32 C33 H33A 107.7 C32 C33 H33B 107.7 H33A C33 H33B 107.1 C34 C33 C32 118.3(7) C34 C33 H33A 107.7 C34 C33 H33B 107.7 C33 C34 H34A 107.7 C33 C34 H34B 107.7 C33 C34 C35 118.3(7) H34A C34 H34B 107.1 C35 C34 H34A 107.7 C35 C34 H34B 107.7 C34 C35 H35A 108.6 C34 C35 H35B 108.6 C34 C35 C36 114.6(7) H35A C35 H35B 107.6 C36 C35 H35A 108.6 C36 C35 H35B 108.6 C31 C36 C35 115.8(7) C31 C36 H36A 108.3 C31 C36 H36B 108.3 C35 C36 H36A 108.3 C35 C36 H36B 108.3 H36A C36 H36B 107.4 P3 C37 H37 105.9 C38 C37 P3 113.2(4) C38 C37 H37 105.9 C42 C37 P3 115.4(4) C42 C37 H37 105.9 C42 C37 C38 109.9(5) C37 C38 H38A 109.4 C37 C38 H38B 109.4 H38A C38 H38B 108.0 C39 C38 C37 111.3(5) C39 C38 H38A 109.4 C39 C38 H38B 109.4 C38 C39 H39A 109.3 C38 C39 H39B 109.3 H39A C39 H39B 107.9 C40 C39 C38 111.8(5) C40 C39 H39A 109.3 C40 C39 H39B 109.3 C39 C40 H40A 109.7 C39 C40 H40B 109.7 C39 C40 C41 110.0(5) H40A C40 H40B 108.2 C41 C40 H40A 109.7 C41 C40 H40B 109.7 C40 C41 H41A 109.4 C40 C41 H41B 109.4 C40 C41 C42 111.3(5) H41A C41 H41B 108.0 C42 C41 H41A 109.4 C42 C41 H41B 109.4 C37 C42 C41 110.0(5) C37 C42 H42A 109.7 C37 C42 H42B 109.7 C41 C42 H42A 109.7 C41 C42 H42B 109.7 H42A C42 H42B 108.2 P3 C43 H43 108.5 C44 C43 P3 110.8(4) C44 C43 H43 108.5 C48 C43 P3 110.8(4) C48 C43 H43 108.5 C48 C43 C44 109.5(5) C43 C44 H44A 109.3 C43 C44 H44B 109.3 H44A C44 H44B 108.0 C45 C44 C43 111.4(5) C45 C44 H44A 109.3 C45 C44 H44B 109.3 C44 C45 H45A 109.2 C44 C45 H45B 109.2 H45A C45 H45B 107.9 C46 C45 C44 111.9(6) C46 C45 H45A 109.2 C46 C45 H45B 109.2 C45 C46 H46A 109.6 C45 C46 H46B 109.6 C45 C46 C47 110.4(6) H46A C46 H46B 108.1 C47 C46 H46A 109.6 C47 C46 H46B 109.6 C46 C47 H47A 109.4 C46 C47 H47B 109.4 C46 C47 C48 111.2(5) H47A C47 H47B 108.0 C48 C47 H47A 109.4 C48 C47 H47B 109.4 C43 C48 H48A 109.2 C43 C48 H48B 109.2 C47 C48 C43 112.1(5) C47 C48 H48A 109.2 C47 C48 H48B 109.2 H48A C48 H48B 107.9 P3 C49 H49 106.4 C50 C49 P3 118.0(4) C50 C49 H49 106.4 C50 C49 C54 109.8(5) C54 C49 P3 109.2(4) C54 C49 H49 106.4 C49 C50 H50A 109.5 C49 C50 H50B 109.5 H50A C50 H50B 108.1 C51 C50 C49 110.6(5) C51 C50 H50A 109.5 C51 C50 H50B 109.5 C50 C51 H51A 109.2 C50 C51 H51B 109.2 C50 C51 C52 112.1(6) H51A C51 H51B 107.9 C52 C51 H51A 109.2 C52 C51 H51B 109.2 C51 C52 H52A 109.3 C51 C52 H52B 109.3 H52A C52 H52B 107.9 C53 C52 C51 111.8(6) C53 C52 H52A 109.3 C53 C52 H52B 109.3 C52 C53 H53A 109.3 C52 C53 H53B 109.3 C52 C53 C54 111.5(6) H53A C53 H53B 108.0 C54 C53 H53A 109.3 C54 C53 H53B 109.3 C49 C54 H54A 109.1 C49 C54 H54B 109.1 C53 C54 C49 112.4(6) C53 C54 H54A 109.1 C53 C54 H54B 109.1 H54A C54 H54B 107.9 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Pr1 Br1 2.8781(7) Pr1 Br2 2.8894(7) Pr1 Br3 2.9145(5) Pr1 O1 2.294(4) Pr1 O2 2.302(4) Pr1 O3 2.336(3) P1 O1 1.514(4) P1 C1 1.834(6) P1 C7 1.823(6) P1 C13 1.807(6) P2 O2 1.515(4) P2 C19 1.802(6) P2 C25 1.810(6) P2 C31 1.817(7) P3 O3 1.510(3) P3 C37 1.824(6) P3 C43 1.817(6) P3 C49 1.829(6) C1 H1 1.0000 C1 C2 1.527(8) C1 C6 1.530(8) C2 H2A 0.9900 C2 H2B 0.9900 C2 C3 1.521(9) C3 H3A 0.9900 C3 H3B 0.9900 C3 C4 1.521(9) C4 H4A 0.9900 C4 H4B 0.9900 C4 C5 1.518(9) C5 H5A 0.9900 C5 H5B 0.9900 C5 C6 1.539(8) C6 H6A 0.9900 C6 H6B 0.9900 C7 H7 1.0000 C7 C8 1.530(8) C7 C12 1.543(8) C8 H8A 0.9900 C8 H8B 0.9900 C8 C9 1.532(8) C9 H9A 0.9900 C9 H9B 0.9900 C9 C10 1.524(10) C10 H10A 0.9900 C10 H10B 0.9900 C10 C11 1.513(10) C11 H11A 0.9900 C11 H11B 0.9900 C11 C12 1.540(9) C12 H12A 0.9900 C12 H12B 0.9900 C13 H13 1.0000 C13 C14 1.539(8) C13 C18 1.543(9) C14 H14A 0.9900 C14 H14B 0.9900 C14 C15 1.531(9) C15 H15A 0.9900 C15 H15B 0.9900 C15 C16 1.516(10) C16 H16A 0.9900 C16 H16B 0.9900 C16 C17 1.514(9) C17 H17A 0.9900 C17 H17B 0.9900 C17 C18 1.521(8) C18 H18A 0.9900 C18 H18B 0.9900 C19 H19 1.0000 C19 C20 1.525(9) C19 C24 1.536(8) C20 H20A 0.9900 C20 H20B 0.9900 C20 C21 1.526(9) C21 H21A 0.9900 C21 H21B 0.9900 C21 C22 1.516(9) C22 H22A 0.9900 C22 H22B 0.9900 C22 C23 1.509(11) C23 H23A 0.9900 C23 H23B 0.9900 C23 C24 1.516(9) C24 H24A 0.9900 C24 H24B 0.9900 C25 H25 1.0000 C25 C26 1.536(8) C25 C30 1.511(9) C26 H26A 0.9900 C26 H26B 0.9900 C26 C27 1.532(9) C27 H27A 0.9900 C27 H27B 0.9900 C27 C28 1.503(11) C28 H28A 0.9900 C28 H28B 0.9900 C28 C29 1.516(12) C29 H29A 0.9900 C29 H29B 0.9900 C29 C30 1.517(11) C30 H30A 0.9900 C30 H30B 0.9900 C31 H31 1.0000 C31 C32 1.497(9) C31 C36 1.438(11) C32 H32A 0.9900 C32 H32B 0.9900 C32 C33 1.491(9) C33 H33A 0.9900 C33 H33B 0.9900 C33 C34 1.424(12) C34 H34A 0.9900 C34 H34B 0.9900 C34 C35 1.489(11) C35 H35A 0.9900 C35 H35B 0.9900 C35 C36 1.499(10) C36 H36A 0.9900 C36 H36B 0.9900 C37 H37 1.0000 C37 C38 1.535(8) C37 C42 1.529(8) C38 H38A 0.9900 C38 H38B 0.9900 C38 C39 1.531(8) C39 H39A 0.9900 C39 H39B 0.9900 C39 C40 1.518(8) C40 H40A 0.9900 C40 H40B 0.9900 C40 C41 1.523(10) C41 H41A 0.9900 C41 H41B 0.9900 C41 C42 1.533(8) C42 H42A 0.9900 C42 H42B 0.9900 C43 H43 1.0000 C43 C44 1.536(8) C43 C48 1.533(8) C44 H44A 0.9900 C44 H44B 0.9900 C44 C45 1.523(9) C45 H45A 0.9900 C45 H45B 0.9900 C45 C46 1.516(10) C46 H46A 0.9900 C46 H46B 0.9900 C46 C47 1.522(9) C47 H47A 0.9900 C47 H47B 0.9900 C47 C48 1.527(8) C48 H48A 0.9900 C48 H48B 0.9900 C49 H49 1.0000 C49 C50 1.528(8) C49 C54 1.533(9) C50 H50A 0.9900 C50 H50B 0.9900 C50 C51 1.523(9) C51 H51A 0.9900 C51 H51B 0.9900 C51 C52 1.528(10) C52 H52A 0.9900 C52 H52B 0.9900 C52 C53 1.517(10) C53 H53A 0.9900 C53 H53B 0.9900 C53 C54 1.518(9) C54 H54A 0.9900 C54 H54B 0.9900 loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.991(9) 2 0.009(9)