#------------------------------------------------------------------------------ #$Date: 2020-02-06 04:02:28 +0200 (Thu, 06 Feb 2020) $ #$Revision: 247904 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/72/1557254.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_1557254 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 Br3 Nd O3 P3' _chemical_formula_sum 'C54 H99 Br3 Nd O3 P3' _chemical_formula_weight 1273.21 _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 28.7058(10) _cell_length_b 11.4228(4) _cell_length_c 18.1359(7) _cell_measurement_reflns_used 9820 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 27.514 _cell_measurement_theta_min 2.22 _cell_volume 5946.8(4) _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 0.998 _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 0.0874 _diffrn_reflns_av_unetI/netI 0.0487 _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 106339 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.557 _diffrn_reflns_theta_min 2.223 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 3.007 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.6784 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0796 before and 0.0665 after correction. The Ratio of minimum to maximum transmission is 0.9099. The \l/2 correction factor is Not present.' _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.422 _exptl_crystal_description block _exptl_crystal_F_000 2628 _exptl_crystal_preparation 'combining reagents in iPrOH' _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: iPrOH' _exptl_crystal_size_max 0.224 _exptl_crystal_size_mid 0.202 _exptl_crystal_size_min 0.17 _refine_diff_density_max 1.021 _refine_diff_density_min -1.569 _refine_diff_density_rms 0.110 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack -0.006(12) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 578 _refine_ls_number_reflns 13649 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.037 _refine_ls_R_factor_all 0.0608 _refine_ls_R_factor_gt 0.0405 _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^)+(0.0083P)^2^+23.4074P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0680 _refine_ls_wR_factor_ref 0.0777 _reflns_Friedel_coverage 0.938 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 0.999 _reflns_number_gt 11307 _reflns_number_total 13649 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9sc05268b2.cif _cod_data_source_block 'save_b' _cod_database_code 1557254 _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 0.629 _shelx_estimated_absorpt_t_min 0.552 _olex2_refinement_description ; 1. Twinned data refinement Scales: 1.006(12) -0.006(12) 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_b.res in Pca2(1) save_b.res created by SHELXL-2016/6 at 13:28:04 on 24-Jun-2019 REM Old TITL save in Pca2(1) REM SHELXT solution in Pca2(1) REM R1 0.103, Rweak 0.010, Alpha 0.024, Orientation as input REM Flack x = -0.586 ( 0.020 ) from Parsons' quotients REM Formula found by SHELXT: C51 O6 P3 Br3 Nd CELL 0.71073 28.7058 11.4228 18.1359 90 90 90 ZERR 4 0.001 0.0004 0.0007 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 Nd UNIT 216 396 12 12 12 4 L.S. 20 PLAN 10 SIZE 0.17 0.202 0.224 TEMP -153(2) BOND $H LIST 6 fmap 2 ACTA TWIN -1 0 0 0 -1 0 0 0 -1 2 OMIT 4 0 0 OMIT 30 3 10 REM REM REM WGHT 0.008300 23.407400 BASF -0.00554 FVAR 0.15499 ND1 6 0.626351 0.412993 0.515951 11.00000 0.01335 0.01476 = 0.00981 0.00028 0.00076 0.00080 BR1 5 0.566557 0.409284 0.388481 11.00000 0.02901 0.03132 = 0.01793 -0.00069 -0.01037 0.00536 BR2 5 0.684173 0.387089 0.645427 11.00000 0.02628 0.03407 = 0.01693 -0.00008 -0.00836 0.00181 BR3 5 0.626934 0.668327 0.517128 11.00000 0.02931 0.01448 = 0.04584 0.00004 0.00856 0.00055 P1 4 0.733853 0.454452 0.398581 11.00000 0.01717 0.01960 = 0.01234 0.00138 0.00309 0.00139 P2 4 0.522185 0.464170 0.637505 11.00000 0.01757 0.02064 = 0.01940 0.00425 0.00720 0.00234 P3 4 0.612512 0.078946 0.511316 11.00000 0.02178 0.01353 = 0.01981 -0.00104 -0.00131 0.00000 O1 3 0.691407 0.417874 0.442316 11.00000 0.01981 0.02091 = 0.01647 0.00125 0.00467 0.00106 O2 3 0.561604 0.415654 0.591485 11.00000 0.02037 0.02103 = 0.02358 0.00043 0.00545 0.00209 O3 3 0.622640 0.208902 0.510857 11.00000 0.01985 0.02024 = 0.01831 -0.00195 -0.00087 -0.00146 C1 1 0.719750 0.452832 0.300854 11.00000 0.01798 0.02587 = 0.01402 0.00257 0.00384 0.00063 AFIX 13 H1 2 0.749370 0.458866 0.272082 11.00000 -1.20000 AFIX 0 C2 1 0.687976 0.556223 0.279428 11.00000 0.03202 0.03299 = 0.02222 0.00517 0.00072 0.00590 AFIX 23 H2A 2 0.658993 0.553587 0.308968 11.00000 -1.20000 H2B 2 0.704022 0.631076 0.290013 11.00000 -1.20000 AFIX 0 C3 1 0.675998 0.549242 0.196823 11.00000 0.04048 0.04708 = 0.02230 0.01045 -0.00364 0.00634 AFIX 23 H3A 2 0.654424 0.613792 0.184142 11.00000 -1.20000 H3B 2 0.704827 0.559979 0.167635 11.00000 -1.20000 AFIX 0 C4 1 0.653799 0.433999 0.176046 11.00000 0.03305 0.05765 = 0.02292 0.00720 -0.00963 0.00091 AFIX 23 H4A 2 0.648573 0.431859 0.122105 11.00000 -1.20000 H4B 2 0.623144 0.427085 0.200674 11.00000 -1.20000 AFIX 0 C5 1 0.684485 0.331111 0.198447 11.00000 0.02801 0.04414 = 0.02161 -0.00372 -0.00409 -0.00680 AFIX 23 H5A 2 0.713789 0.332847 0.169684 11.00000 -1.20000 H5B 2 0.668222 0.256731 0.187378 11.00000 -1.20000 AFIX 0 C6 1 0.695686 0.337060 0.280859 11.00000 0.02219 0.03130 = 0.02267 -0.00247 -0.00475 -0.00549 AFIX 23 H6A 2 0.716255 0.270841 0.294287 11.00000 -1.20000 H6B 2 0.666499 0.329512 0.309548 11.00000 -1.20000 AFIX 0 C7 1 0.750631 0.600933 0.425946 11.00000 0.01840 0.02526 = 0.01713 0.00055 0.00367 -0.00356 AFIX 13 H7 2 0.723338 0.652773 0.415553 11.00000 -1.20000 AFIX 0 C8 1 0.792149 0.651702 0.382662 11.00000 0.02559 0.02905 = 0.02462 0.00074 0.00551 -0.00133 AFIX 23 H8A 2 0.820269 0.603746 0.391968 11.00000 -1.20000 H8B 2 0.785352 0.649118 0.329170 11.00000 -1.20000 AFIX 0 C9 1 0.801302 0.778681 0.406307 11.00000 0.03495 0.02213 = 0.04428 0.00427 0.00490 -0.00325 AFIX 23 H9A 2 0.829479 0.807976 0.380806 11.00000 -1.20000 H9B 2 0.774673 0.828126 0.391027 11.00000 -1.20000 AFIX 0 C10 1 0.808114 0.789698 0.489204 11.00000 0.03347 0.02254 = 0.05259 -0.01107 -0.00262 -0.00079 AFIX 23 H10A 2 0.837636 0.750892 0.503304 11.00000 -1.20000 H10B 2 0.810687 0.873554 0.502384 11.00000 -1.20000 AFIX 0 C11 1 0.768376 0.735376 0.532207 11.00000 0.03475 0.02444 = 0.02945 -0.00888 -0.00065 0.00358 AFIX 23 H11A 2 0.739641 0.781322 0.523621 11.00000 -1.20000 H11B 2 0.775602 0.738755 0.585541 11.00000 -1.20000 AFIX 0 C12 1 0.759883 0.608399 0.509936 11.00000 0.02919 0.01924 = 0.02158 -0.00723 0.00380 0.00145 AFIX 23 H12A 2 0.732735 0.577100 0.537226 11.00000 -1.20000 H12B 2 0.787442 0.560407 0.522716 11.00000 -1.20000 AFIX 0 C13 1 0.782540 0.355345 0.417568 11.00000 0.02804 0.01958 = 0.01733 -0.00193 -0.00151 -0.00076 AFIX 13 H13 2 0.804458 0.399292 0.450289 11.00000 -1.20000 AFIX 0 C14 1 0.765778 0.248815 0.462218 11.00000 0.03904 0.02979 = 0.02863 0.01121 0.01670 0.01506 AFIX 23 H14A 2 0.751077 0.276113 0.508509 11.00000 -1.20000 H14B 2 0.741953 0.205891 0.433462 11.00000 -1.20000 AFIX 0 C15 1 0.805456 0.167074 0.480474 11.00000 0.04160 0.03237 = 0.02925 0.00962 0.00440 0.01423 AFIX 23 H15A 2 0.793133 0.098123 0.507182 11.00000 -1.20000 H15B 2 0.827717 0.207652 0.513415 11.00000 -1.20000 AFIX 0 C16 1 0.830836 0.126333 0.411667 11.00000 0.02564 0.02372 = 0.04114 0.00075 -0.00089 0.00566 AFIX 23 H16A 2 0.809275 0.081137 0.379968 11.00000 -1.20000 H16B 2 0.857039 0.074543 0.425656 11.00000 -1.20000 AFIX 0 C17 1 0.849370 0.232138 0.369183 11.00000 0.02010 0.02909 = 0.03406 -0.00759 0.00134 0.00386 AFIX 23 H17A 2 0.864562 0.204888 0.323280 11.00000 -1.20000 H17B 2 0.873208 0.272380 0.399410 11.00000 -1.20000 AFIX 0 C18 1 0.810702 0.319017 0.349631 11.00000 0.01811 0.02415 = 0.02482 -0.00004 0.00396 0.00199 AFIX 23 H18A 2 0.789566 0.282880 0.312990 11.00000 -1.20000 H18B 2 0.824697 0.389496 0.326858 11.00000 -1.20000 AFIX 0 C19 1 0.540867 0.598246 0.682656 11.00000 0.02276 0.02991 = 0.01525 -0.00608 -0.00185 0.00005 AFIX 13 H19 2 0.552878 0.650142 0.642524 11.00000 -1.20000 AFIX 0 C20 1 0.581248 0.578417 0.733878 11.00000 0.05634 0.06447 = 0.05714 -0.03865 -0.03210 0.02988 AFIX 23 H20A 2 0.606258 0.536029 0.707420 11.00000 -1.20000 H20B 2 0.571071 0.529335 0.775886 11.00000 -1.20000 AFIX 0 C21 1 0.599908 0.693050 0.762350 11.00000 0.04797 0.07061 = 0.07104 -0.04454 -0.04215 0.01932 AFIX 23 H21A 2 0.612934 0.738344 0.720626 11.00000 -1.20000 H21B 2 0.625554 0.677261 0.797467 11.00000 -1.20000 AFIX 0 C22 1 0.563079 0.765630 0.800392 11.00000 0.08306 0.04016 = 0.03265 -0.01556 -0.01678 0.01047 AFIX 23 H22A 2 0.553318 0.725915 0.846386 11.00000 -1.20000 H22B 2 0.576351 0.842719 0.813847 11.00000 -1.20000 AFIX 0 C23 1 0.521393 0.783402 0.751773 11.00000 0.05042 0.02159 = 0.03924 -0.00639 0.00652 -0.00158 AFIX 23 H23A 2 0.530070 0.835283 0.710259 11.00000 -1.20000 H23B 2 0.496591 0.822940 0.780384 11.00000 -1.20000 AFIX 0 C24 1 0.502272 0.667399 0.720804 11.00000 0.03554 0.01977 = 0.03472 -0.00112 0.01065 0.00084 AFIX 23 H24A 2 0.489027 0.620139 0.761477 11.00000 -1.20000 H24B 2 0.477025 0.684018 0.685120 11.00000 -1.20000 AFIX 0 C25 1 0.503338 0.349296 0.699919 11.00000 0.03968 0.04073 = 0.06432 0.03284 0.03154 0.01615 AFIX 13 H25 2 0.489916 0.293081 0.663376 11.00000 -1.20000 AFIX 0 C26 1 0.460677 0.374731 0.744239 11.00000 0.02891 0.02803 = 0.03662 0.00688 0.01933 -0.00070 AFIX 23 H26A 2 0.435035 0.396131 0.710316 11.00000 -1.20000 H26B 2 0.466854 0.443064 0.776362 11.00000 -1.20000 AFIX 0 C27 1 0.445213 0.273820 0.791351 11.00000 0.06590 0.06540 = 0.12143 0.05982 0.06492 0.01926 AFIX 23 H27A 2 0.427522 0.306535 0.833437 11.00000 -1.20000 H27B 2 0.423064 0.226648 0.761889 11.00000 -1.20000 AFIX 0 C28 1 0.478761 0.196817 0.820222 11.00000 0.05623 0.06595 = 0.07372 0.03865 0.01522 -0.00941 AFIX 23 H28A 2 0.463288 0.120722 0.829331 11.00000 -1.20000 H28B 2 0.488658 0.227772 0.868743 11.00000 -1.20000 AFIX 0 C29 1 0.521489 0.173775 0.776144 11.00000 0.03537 0.02978 = 0.04604 0.01638 -0.00139 0.00131 AFIX 23 H29A 2 0.515287 0.107718 0.742197 11.00000 -1.20000 H29B 2 0.546755 0.149396 0.809977 11.00000 -1.20000 AFIX 0 C30 1 0.538027 0.276836 0.731768 11.00000 0.04243 0.06096 = 0.11271 0.05984 0.03748 0.01775 AFIX 23 H30A 2 0.557740 0.326168 0.764030 11.00000 -1.20000 H30B 2 0.558145 0.247114 0.691575 11.00000 -1.20000 AFIX 0 C31 1 0.473272 0.501902 0.579789 11.00000 0.01434 0.02282 = 0.02839 -0.00401 0.00350 0.00178 AFIX 13 H31 2 0.447891 0.533168 0.612018 11.00000 -1.20000 AFIX 0 C32 1 0.454184 0.395554 0.537651 11.00000 0.03504 0.02282 = 0.03428 -0.00774 0.00992 -0.01018 AFIX 23 H32A 2 0.479708 0.359593 0.508761 11.00000 -1.20000 H32B 2 0.442944 0.336607 0.573496 11.00000 -1.20000 AFIX 0 C33 1 0.414806 0.427746 0.486160 11.00000 0.02585 0.04979 = 0.05003 -0.03117 -0.00003 -0.00450 AFIX 23 H33A 2 0.387624 0.453901 0.515442 11.00000 -1.20000 H33B 2 0.405377 0.357798 0.457592 11.00000 -1.20000 AFIX 0 C34 1 0.429148 0.524838 0.433202 11.00000 0.03575 0.04801 = 0.03999 -0.02073 -0.01862 0.01703 AFIX 23 H34A 2 0.454434 0.496576 0.400626 11.00000 -1.20000 H34B 2 0.402298 0.546978 0.401910 11.00000 -1.20000 AFIX 0 C35 1 0.445732 0.630404 0.476215 11.00000 0.04210 0.03266 = 0.03982 -0.00417 -0.01467 0.01576 AFIX 23 H35A 2 0.420032 0.660502 0.507292 11.00000 -1.20000 H35B 2 0.455086 0.693183 0.441616 11.00000 -1.20000 AFIX 0 C36 1 0.486889 0.597342 0.524723 11.00000 0.02934 0.01545 = 0.03118 0.00080 -0.01134 0.00111 AFIX 23 H36A 2 0.497850 0.667370 0.551804 11.00000 -1.20000 H36B 2 0.512799 0.568998 0.493429 11.00000 -1.20000 AFIX 0 C37 1 0.550989 0.055240 0.531651 11.00000 0.02332 0.01670 = 0.02476 -0.00079 0.00057 -0.00241 AFIX 13 H37 2 0.544596 0.099473 0.578146 11.00000 -1.20000 AFIX 0 C38 1 0.518428 0.107019 0.473628 11.00000 0.02608 0.02050 = 0.02929 0.00381 -0.00355 0.00007 AFIX 23 H38A 2 0.522739 0.065067 0.426351 11.00000 -1.20000 H38B 2 0.526370 0.190392 0.465612 11.00000 -1.20000 AFIX 0 C39 1 0.467540 0.097164 0.497897 11.00000 0.02209 0.03114 = 0.04414 0.00482 -0.00537 0.00127 AFIX 23 H39A 2 0.462581 0.146619 0.542033 11.00000 -1.20000 H39B 2 0.447197 0.127231 0.458093 11.00000 -1.20000 AFIX 0 C40 1 0.453794 -0.027584 0.515639 11.00000 0.02497 0.03035 = 0.04412 -0.00098 0.00102 -0.00773 AFIX 23 H40A 2 0.455113 -0.075838 0.470343 11.00000 -1.20000 H40B 2 0.421463 -0.029383 0.534606 11.00000 -1.20000 AFIX 0 C41 1 0.486728 -0.077245 0.573084 11.00000 0.03084 0.01978 = 0.04447 0.00533 0.00557 -0.00151 AFIX 23 H41A 2 0.478107 -0.159558 0.583367 11.00000 -1.20000 H41B 2 0.483342 -0.032357 0.619471 11.00000 -1.20000 AFIX 0 C42 1 0.537693 -0.072422 0.547826 11.00000 0.02482 0.01662 = 0.03368 0.00190 0.00139 0.00225 AFIX 23 H42A 2 0.541797 -0.120471 0.502862 11.00000 -1.20000 H42B 2 0.558171 -0.104415 0.586855 11.00000 -1.20000 AFIX 0 C43 1 0.646240 0.010080 0.584059 11.00000 0.03184 0.01100 = 0.02177 0.00036 -0.00669 0.00375 AFIX 13 H43 2 0.644737 -0.076783 0.577622 11.00000 -1.20000 AFIX 0 C44 1 0.626900 0.041479 0.660239 11.00000 0.02884 0.02557 = 0.02528 -0.00179 -0.00153 0.00332 AFIX 23 H44A 2 0.594623 0.011755 0.664619 11.00000 -1.20000 H44B 2 0.625997 0.127696 0.665616 11.00000 -1.20000 AFIX 0 C45 1 0.656788 -0.010937 0.721987 11.00000 0.04410 0.03471 = 0.02294 0.00307 -0.00054 0.00648 AFIX 23 H45A 2 0.643834 0.012794 0.770319 11.00000 -1.20000 H45B 2 0.655536 -0.097420 0.719013 11.00000 -1.20000 AFIX 0 C46 1 0.706948 0.028657 0.716909 11.00000 0.03927 0.03943 = 0.02402 -0.00360 -0.00956 0.01070 AFIX 23 H46A 2 0.725480 -0.009844 0.756041 11.00000 -1.20000 H46B 2 0.708687 0.114348 0.724608 11.00000 -1.20000 AFIX 0 C47 1 0.727028 -0.001942 0.642072 11.00000 0.03101 0.03784 = 0.02663 -0.00023 -0.00559 0.01430 AFIX 23 H47A 2 0.728499 -0.088139 0.636882 11.00000 -1.20000 H47B 2 0.759173 0.028942 0.638510 11.00000 -1.20000 AFIX 0 C48 1 0.697487 0.049137 0.579210 11.00000 0.02545 0.02669 = 0.02545 0.00120 -0.00418 0.00575 AFIX 23 H48A 2 0.710624 0.023698 0.531349 11.00000 -1.20000 H48B 2 0.698992 0.135669 0.581138 11.00000 -1.20000 AFIX 0 C49 1 0.623308 0.012432 0.420859 11.00000 0.02894 0.02159 = 0.02146 -0.00408 -0.00086 -0.00156 AFIX 13 H49 2 0.598899 -0.049141 0.414254 11.00000 -1.20000 AFIX 0 C50 1 0.614893 0.102839 0.360660 11.00000 0.03031 0.02944 = 0.02384 -0.00006 -0.00176 -0.00026 AFIX 23 H50A 2 0.583925 0.139048 0.368212 11.00000 -1.20000 H50B 2 0.638627 0.165384 0.364745 11.00000 -1.20000 AFIX 0 C51 1 0.616944 0.050482 0.283932 11.00000 0.04767 0.04500 = 0.02677 -0.00095 0.00416 0.00593 AFIX 23 H51A 2 0.613891 0.113663 0.246879 11.00000 -1.20000 H51B 2 0.590537 -0.004239 0.277232 11.00000 -1.20000 AFIX 0 C52 1 0.662591 -0.014661 0.271541 11.00000 0.04207 0.05076 = 0.02534 -0.00572 0.00779 -0.00124 AFIX 23 H52A 2 0.661330 -0.055769 0.223526 11.00000 -1.20000 H52B 2 0.688508 0.042432 0.269557 11.00000 -1.20000 AFIX 0 C53 1 0.672053 -0.103218 0.332493 11.00000 0.02988 0.03284 = 0.03504 -0.01248 0.00479 -0.00042 AFIX 23 H53A 2 0.703203 -0.138325 0.324753 11.00000 -1.20000 H53B 2 0.648706 -0.166832 0.329517 11.00000 -1.20000 AFIX 0 C54 1 0.670187 -0.048423 0.409083 11.00000 0.02822 0.02778 = 0.03206 -0.00450 0.00203 0.00023 AFIX 23 H54A 2 0.695730 0.009191 0.414412 11.00000 -1.20000 H54B 2 0.674504 -0.109935 0.446927 11.00000 -1.20000 AFIX 0 HKLF 4 REM save_b.res in Pca2(1) REM R1 = 0.0405 for 11307 Fo > 4sig(Fo) and 0.0608 for all 13649 data REM 578 parameters refined using 1 restraints END WGHT 0.0083 23.4068 REM Highest difference peak 1.021, deepest hole -1.569, 1-sigma level 0.110 Q1 1 0.5894 0.4788 0.5118 11.00000 0.05 1.02 Q2 1 0.5900 0.3450 0.5205 11.00000 0.05 0.98 Q3 1 0.6630 0.4827 0.5150 11.00000 0.05 0.92 Q4 1 0.6619 0.3422 0.5151 11.00000 0.05 0.87 Q5 1 0.6211 0.5782 0.5172 11.00000 0.05 0.78 Q6 1 0.6697 0.4177 0.5966 11.00000 0.05 0.77 Q7 1 0.6093 0.3994 0.3920 11.00000 0.05 0.71 Q8 1 0.6286 0.4691 0.5387 11.00000 0.05 0.71 Q9 1 0.6234 0.1452 0.5207 11.00000 0.05 0.69 Q10 1 0.7983 0.6649 0.1811 11.00000 0.05 0.69 ; _shelx_res_checksum 92554 _olex2_exptl_crystal_mounting_method 'nylon loop' _olex2_submission_original_sample_id cjw93 _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 Nd1 Nd 0.62635(2) 0.41299(3) 0.51595(3) 0.01264(7) Uani 1 1 d . Br1 Br 0.56656(3) 0.40928(7) 0.38848(4) 0.02609(17) Uani 1 1 d . Br2 Br 0.68417(3) 0.38709(7) 0.64543(4) 0.02576(17) Uani 1 1 d . Br3 Br 0.62693(3) 0.66833(5) 0.51713(8) 0.02987(15) Uani 1 1 d . P1 P 0.73385(6) 0.45445(16) 0.39858(10) 0.0164(4) Uani 1 1 d . P2 P 0.52218(6) 0.46417(16) 0.63751(11) 0.0192(4) Uani 1 1 d . P3 P 0.61251(5) 0.07895(14) 0.51132(13) 0.0184(3) Uani 1 1 d . O1 O 0.69141(17) 0.4179(4) 0.4423(3) 0.0191(11) Uani 1 1 d . O2 O 0.56160(17) 0.4157(4) 0.5915(3) 0.0217(11) Uani 1 1 d . O3 O 0.62264(16) 0.2089(3) 0.5109(4) 0.0195(9) Uani 1 1 d . C1 C 0.7197(2) 0.4528(6) 0.3009(4) 0.0193(15) Uani 1 1 d . H1 H 0.749370 0.458866 0.272082 0.023 Uiso 1 1 calc R C2 C 0.6880(3) 0.5562(7) 0.2794(4) 0.0291(18) Uani 1 1 d . H2A H 0.658993 0.553587 0.308968 0.035 Uiso 1 1 calc R H2B H 0.704022 0.631076 0.290013 0.035 Uiso 1 1 calc R C3 C 0.6760(3) 0.5492(8) 0.1968(4) 0.037(2) Uani 1 1 d . H3A H 0.654424 0.613792 0.184142 0.044 Uiso 1 1 calc R H3B H 0.704827 0.559979 0.167635 0.044 Uiso 1 1 calc R C4 C 0.6538(3) 0.4340(8) 0.1760(5) 0.038(2) Uani 1 1 d . H4A H 0.648573 0.431859 0.122105 0.045 Uiso 1 1 calc R H4B H 0.623144 0.427085 0.200674 0.045 Uiso 1 1 calc R C5 C 0.6845(3) 0.3311(8) 0.1984(4) 0.031(2) Uani 1 1 d . H5A H 0.713789 0.332847 0.169684 0.038 Uiso 1 1 calc R H5B H 0.668222 0.256731 0.187378 0.038 Uiso 1 1 calc R C6 C 0.6957(3) 0.3371(7) 0.2809(4) 0.0254(17) Uani 1 1 d . H6A H 0.716255 0.270841 0.294287 0.030 Uiso 1 1 calc R H6B H 0.666499 0.329512 0.309548 0.030 Uiso 1 1 calc R C7 C 0.7506(2) 0.6009(6) 0.4259(4) 0.0203(15) Uani 1 1 d . H7 H 0.723338 0.652773 0.415553 0.024 Uiso 1 1 calc R C8 C 0.7921(3) 0.6517(6) 0.3827(4) 0.0264(16) Uani 1 1 d . H8A H 0.820269 0.603746 0.391968 0.032 Uiso 1 1 calc R H8B H 0.785352 0.649118 0.329170 0.032 Uiso 1 1 calc R C9 C 0.8013(3) 0.7787(7) 0.4063(5) 0.034(2) Uani 1 1 d . H9A H 0.829479 0.807976 0.380806 0.041 Uiso 1 1 calc R H9B H 0.774673 0.828126 0.391027 0.041 Uiso 1 1 calc R C10 C 0.8081(3) 0.7897(7) 0.4892(5) 0.036(2) Uani 1 1 d . H10A H 0.837636 0.750892 0.503304 0.043 Uiso 1 1 calc R H10B H 0.810687 0.873554 0.502384 0.043 Uiso 1 1 calc R C11 C 0.7684(3) 0.7354(6) 0.5322(4) 0.0295(19) Uani 1 1 d . H11A H 0.739641 0.781322 0.523621 0.035 Uiso 1 1 calc R H11B H 0.775602 0.738755 0.585541 0.035 Uiso 1 1 calc R C12 C 0.7599(3) 0.6084(5) 0.5099(5) 0.0233(15) Uani 1 1 d . H12A H 0.732735 0.577100 0.537226 0.028 Uiso 1 1 calc R H12B H 0.787442 0.560407 0.522716 0.028 Uiso 1 1 calc R C13 C 0.7825(3) 0.3553(6) 0.4176(4) 0.0216(15) Uani 1 1 d . H13 H 0.804458 0.399292 0.450289 0.026 Uiso 1 1 calc R C14 C 0.7658(3) 0.2488(7) 0.4622(5) 0.032(2) Uani 1 1 d . H14A H 0.751077 0.276113 0.508509 0.039 Uiso 1 1 calc R H14B H 0.741953 0.205891 0.433462 0.039 Uiso 1 1 calc R C15 C 0.8055(3) 0.1671(7) 0.4805(5) 0.034(2) Uani 1 1 d . H15A H 0.793133 0.098123 0.507182 0.041 Uiso 1 1 calc R H15B H 0.827717 0.207652 0.513415 0.041 Uiso 1 1 calc R C16 C 0.8308(3) 0.1263(7) 0.4117(5) 0.0302(18) Uani 1 1 d . H16A H 0.809275 0.081137 0.379968 0.036 Uiso 1 1 calc R H16B H 0.857039 0.074543 0.425656 0.036 Uiso 1 1 calc R C17 C 0.8494(3) 0.2321(7) 0.3692(5) 0.0278(18) Uani 1 1 d . H17A H 0.864562 0.204888 0.323280 0.033 Uiso 1 1 calc R H17B H 0.873208 0.272380 0.399410 0.033 Uiso 1 1 calc R C18 C 0.8107(3) 0.3190(7) 0.3496(4) 0.0224(17) Uani 1 1 d . H18A H 0.789566 0.282880 0.312990 0.027 Uiso 1 1 calc R H18B H 0.824697 0.389496 0.326858 0.027 Uiso 1 1 calc R C19 C 0.5409(2) 0.5982(7) 0.6827(4) 0.0226(16) Uani 1 1 d . H19 H 0.552878 0.650142 0.642524 0.027 Uiso 1 1 calc R C20 C 0.5812(4) 0.5784(10) 0.7339(6) 0.059(3) Uani 1 1 d . H20A H 0.606258 0.536029 0.707420 0.071 Uiso 1 1 calc R H20B H 0.571071 0.529335 0.775886 0.071 Uiso 1 1 calc R C21 C 0.5999(4) 0.6930(10) 0.7624(7) 0.063(4) Uani 1 1 d . H21A H 0.612934 0.738344 0.720626 0.076 Uiso 1 1 calc R H21B H 0.625554 0.677261 0.797467 0.076 Uiso 1 1 calc R C22 C 0.5631(4) 0.7656(9) 0.8004(5) 0.052(3) Uani 1 1 d . H22A H 0.553318 0.725915 0.846386 0.062 Uiso 1 1 calc R H22B H 0.576351 0.842719 0.813847 0.062 Uiso 1 1 calc R C23 C 0.5214(3) 0.7834(7) 0.7518(5) 0.037(2) Uani 1 1 d . H23A H 0.530070 0.835283 0.710259 0.045 Uiso 1 1 calc R H23B H 0.496591 0.822940 0.780384 0.045 Uiso 1 1 calc R C24 C 0.5023(3) 0.6674(7) 0.7208(5) 0.0300(18) Uani 1 1 d . H24A H 0.489027 0.620139 0.761477 0.036 Uiso 1 1 calc R H24B H 0.477025 0.684018 0.685120 0.036 Uiso 1 1 calc R C25 C 0.5033(3) 0.3493(8) 0.6999(6) 0.048(3) Uani 1 1 d . H25 H 0.489916 0.293081 0.663376 0.058 Uiso 1 1 calc R C26 C 0.4607(3) 0.3747(7) 0.7442(5) 0.0312(19) Uani 1 1 d . H26A H 0.435035 0.396131 0.710316 0.037 Uiso 1 1 calc R H26B H 0.466854 0.443064 0.776362 0.037 Uiso 1 1 calc R C27 C 0.4452(4) 0.2738(11) 0.7914(8) 0.084(5) Uani 1 1 d . H27A H 0.427522 0.306535 0.833437 0.101 Uiso 1 1 calc R H27B H 0.423064 0.226648 0.761889 0.101 Uiso 1 1 calc R C28 C 0.4788(4) 0.1968(11) 0.8202(7) 0.065(3) Uani 1 1 d . H28A H 0.463288 0.120722 0.829331 0.078 Uiso 1 1 calc R H28B H 0.488658 0.227772 0.868743 0.078 Uiso 1 1 calc R C29 C 0.5215(3) 0.1738(7) 0.7761(5) 0.037(2) Uani 1 1 d . H29A H 0.515287 0.107718 0.742197 0.044 Uiso 1 1 calc R H29B H 0.546755 0.149396 0.809977 0.044 Uiso 1 1 calc R C30 C 0.5380(4) 0.2768(10) 0.7318(8) 0.072(4) Uani 1 1 d . H30A H 0.557740 0.326168 0.764030 0.086 Uiso 1 1 calc R H30B H 0.558145 0.247114 0.691575 0.086 Uiso 1 1 calc R C31 C 0.4733(2) 0.5019(6) 0.5798(4) 0.0218(16) Uani 1 1 d . H31 H 0.447891 0.533168 0.612018 0.026 Uiso 1 1 calc R C32 C 0.4542(3) 0.3956(7) 0.5377(4) 0.0307(19) Uani 1 1 d . H32A H 0.479708 0.359593 0.508761 0.037 Uiso 1 1 calc R H32B H 0.442944 0.336607 0.573496 0.037 Uiso 1 1 calc R C33 C 0.4148(3) 0.4277(8) 0.4862(5) 0.042(2) Uani 1 1 d . H33A H 0.387624 0.453901 0.515442 0.050 Uiso 1 1 calc R H33B H 0.405377 0.357798 0.457592 0.050 Uiso 1 1 calc R C34 C 0.4291(3) 0.5248(8) 0.4332(5) 0.041(2) Uani 1 1 d . H34A H 0.454434 0.496576 0.400626 0.050 Uiso 1 1 calc R H34B H 0.402298 0.546978 0.401910 0.050 Uiso 1 1 calc R C35 C 0.4457(3) 0.6304(8) 0.4762(5) 0.038(2) Uani 1 1 d . H35A H 0.420032 0.660502 0.507292 0.046 Uiso 1 1 calc R H35B H 0.455086 0.693183 0.441616 0.046 Uiso 1 1 calc R C36 C 0.4869(3) 0.5973(6) 0.5247(5) 0.0253(18) Uani 1 1 d . H36A H 0.497850 0.667370 0.551804 0.030 Uiso 1 1 calc R H36B H 0.512799 0.568998 0.493429 0.030 Uiso 1 1 calc R C37 C 0.5510(2) 0.0552(6) 0.5317(4) 0.0216(17) Uani 1 1 d . H37 H 0.544596 0.099473 0.578146 0.026 Uiso 1 1 calc R C38 C 0.5184(3) 0.1070(6) 0.4736(4) 0.0253(17) Uani 1 1 d . H38A H 0.522739 0.065067 0.426351 0.030 Uiso 1 1 calc R H38B H 0.526370 0.190392 0.465612 0.030 Uiso 1 1 calc R C39 C 0.4675(3) 0.0972(7) 0.4979(5) 0.032(2) Uani 1 1 d . H39A H 0.462581 0.146619 0.542033 0.039 Uiso 1 1 calc R H39B H 0.447197 0.127231 0.458093 0.039 Uiso 1 1 calc R C40 C 0.4538(2) -0.0276(6) 0.5156(6) 0.0331(16) Uani 1 1 d . H40A H 0.455113 -0.075838 0.470343 0.040 Uiso 1 1 calc R H40B H 0.421463 -0.029383 0.534606 0.040 Uiso 1 1 calc R C41 C 0.4867(3) -0.0772(7) 0.5731(5) 0.0317(19) Uani 1 1 d . H41A H 0.478107 -0.159558 0.583367 0.038 Uiso 1 1 calc R H41B H 0.483342 -0.032357 0.619471 0.038 Uiso 1 1 calc R C42 C 0.5377(3) -0.0724(6) 0.5478(4) 0.0250(16) Uani 1 1 d . H42A H 0.541797 -0.120471 0.502862 0.030 Uiso 1 1 calc R H42B H 0.558171 -0.104415 0.586855 0.030 Uiso 1 1 calc R C43 C 0.6462(3) 0.0101(6) 0.5841(4) 0.0215(16) Uani 1 1 d . H43 H 0.644737 -0.076783 0.577622 0.026 Uiso 1 1 calc R C44 C 0.6269(3) 0.0415(7) 0.6602(4) 0.0266(17) Uani 1 1 d . H44A H 0.594623 0.011755 0.664619 0.032 Uiso 1 1 calc R H44B H 0.625997 0.127696 0.665616 0.032 Uiso 1 1 calc R C45 C 0.6568(3) -0.0109(8) 0.7220(5) 0.034(2) Uani 1 1 d . H45A H 0.643834 0.012794 0.770319 0.041 Uiso 1 1 calc R H45B H 0.655536 -0.097420 0.719013 0.041 Uiso 1 1 calc R C46 C 0.7069(3) 0.0287(8) 0.7169(4) 0.034(2) Uani 1 1 d . H46A H 0.725480 -0.009844 0.756041 0.041 Uiso 1 1 calc R H46B H 0.708687 0.114348 0.724608 0.041 Uiso 1 1 calc R C47 C 0.7270(3) -0.0019(7) 0.6421(5) 0.0318(18) Uani 1 1 d . H47A H 0.728499 -0.088139 0.636882 0.038 Uiso 1 1 calc R H47B H 0.759173 0.028942 0.638510 0.038 Uiso 1 1 calc R C48 C 0.6975(3) 0.0491(7) 0.5792(4) 0.0259(17) Uani 1 1 d . H48A H 0.710624 0.023698 0.531349 0.031 Uiso 1 1 calc R H48B H 0.698992 0.135669 0.581138 0.031 Uiso 1 1 calc R C49 C 0.6233(3) 0.0124(7) 0.4209(4) 0.0240(17) Uani 1 1 d . H49 H 0.598899 -0.049141 0.414254 0.029 Uiso 1 1 calc R C50 C 0.6149(3) 0.1028(7) 0.3607(4) 0.0279(18) Uani 1 1 d . H50A H 0.583925 0.139048 0.368212 0.033 Uiso 1 1 calc R H50B H 0.638627 0.165384 0.364745 0.033 Uiso 1 1 calc R C51 C 0.6169(3) 0.0505(8) 0.2839(5) 0.040(2) Uani 1 1 d . H51A H 0.613891 0.113663 0.246879 0.048 Uiso 1 1 calc R H51B H 0.590537 -0.004239 0.277232 0.048 Uiso 1 1 calc R C52 C 0.6626(3) -0.0147(9) 0.2715(5) 0.039(2) Uani 1 1 d . H52A H 0.661330 -0.055769 0.223526 0.047 Uiso 1 1 calc R H52B H 0.688508 0.042432 0.269557 0.047 Uiso 1 1 calc R C53 C 0.6721(3) -0.1032(7) 0.3325(5) 0.0326(19) Uani 1 1 d . H53A H 0.703203 -0.138325 0.324753 0.039 Uiso 1 1 calc R H53B H 0.648706 -0.166832 0.329517 0.039 Uiso 1 1 calc R C54 C 0.6702(3) -0.0484(7) 0.4091(5) 0.0294(18) Uani 1 1 d . H54A H 0.695730 0.009191 0.414412 0.035 Uiso 1 1 calc R H54B H 0.674504 -0.109935 0.446927 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 Nd1 0.01335(14) 0.01476(14) 0.00981(13) 0.0003(2) 0.00076(14) 0.00080(13) Br1 0.0290(4) 0.0313(4) 0.0179(4) -0.0007(3) -0.0104(3) 0.0054(3) Br2 0.0263(4) 0.0341(4) 0.0169(4) -0.0001(3) -0.0084(3) 0.0018(3) Br3 0.0293(3) 0.0145(3) 0.0458(4) 0.0000(5) 0.0086(4) 0.0006(3) P1 0.0172(9) 0.0196(9) 0.0123(9) 0.0014(8) 0.0031(7) 0.0014(7) P2 0.0176(9) 0.0206(9) 0.0194(10) 0.0043(8) 0.0072(8) 0.0023(7) P3 0.0218(8) 0.0135(7) 0.0198(8) -0.0010(9) -0.0013(10) 0.0000(6) O1 0.020(3) 0.021(3) 0.016(3) 0.001(2) 0.005(2) 0.001(2) O2 0.020(3) 0.021(3) 0.024(3) 0.000(2) 0.005(2) 0.002(2) O3 0.020(2) 0.020(2) 0.018(2) -0.002(3) -0.001(2) -0.0015(19) C1 0.018(3) 0.026(4) 0.014(3) 0.003(3) 0.004(3) 0.001(3) C2 0.032(4) 0.033(4) 0.022(4) 0.005(3) 0.001(3) 0.006(4) C3 0.040(5) 0.047(5) 0.022(4) 0.010(4) -0.004(4) 0.006(4) C4 0.033(5) 0.058(6) 0.023(4) 0.007(4) -0.010(4) 0.001(4) C5 0.028(4) 0.044(5) 0.022(4) -0.004(4) -0.004(3) -0.007(4) C6 0.022(4) 0.031(4) 0.023(4) -0.002(3) -0.005(3) -0.005(3) C7 0.018(3) 0.025(4) 0.017(3) 0.001(3) 0.004(3) -0.004(3) C8 0.026(4) 0.029(4) 0.025(4) 0.001(3) 0.006(3) -0.001(3) C9 0.035(5) 0.022(4) 0.044(5) 0.004(4) 0.005(4) -0.003(3) C10 0.033(5) 0.023(4) 0.053(6) -0.011(4) -0.003(4) -0.001(4) C11 0.035(4) 0.024(4) 0.029(5) -0.009(3) -0.001(3) 0.004(3) C12 0.029(4) 0.019(3) 0.022(4) -0.007(4) 0.004(4) 0.001(3) C13 0.028(4) 0.020(4) 0.017(4) -0.002(3) -0.002(3) -0.001(3) C14 0.039(5) 0.030(4) 0.029(4) 0.011(4) 0.017(4) 0.015(4) C15 0.042(5) 0.032(5) 0.029(4) 0.010(4) 0.004(4) 0.014(4) C16 0.026(4) 0.024(4) 0.041(5) 0.001(3) -0.001(4) 0.006(3) C17 0.020(4) 0.029(4) 0.034(5) -0.008(3) 0.001(3) 0.004(3) C18 0.018(4) 0.024(4) 0.025(4) 0.000(3) 0.004(3) 0.002(3) C19 0.023(4) 0.030(4) 0.015(3) -0.006(3) -0.002(3) 0.000(3) C20 0.056(7) 0.064(7) 0.057(7) -0.039(6) -0.032(5) 0.030(6) C21 0.048(6) 0.071(7) 0.071(8) -0.045(6) -0.042(6) 0.019(5) C22 0.083(8) 0.040(5) 0.033(5) -0.016(4) -0.017(5) 0.010(5) C23 0.050(6) 0.022(4) 0.039(5) -0.006(4) 0.007(4) -0.002(4) C24 0.036(5) 0.020(4) 0.035(5) -0.001(3) 0.011(4) 0.001(3) C25 0.040(5) 0.041(5) 0.064(7) 0.033(5) 0.032(5) 0.016(4) C26 0.029(4) 0.028(4) 0.037(5) 0.007(4) 0.019(4) -0.001(3) C27 0.066(8) 0.065(8) 0.121(12) 0.060(8) 0.065(8) 0.019(6) C28 0.056(7) 0.066(8) 0.074(9) 0.039(7) 0.015(6) -0.009(6) C29 0.035(5) 0.030(5) 0.046(5) 0.016(4) -0.001(4) 0.001(4) C30 0.042(6) 0.061(7) 0.113(11) 0.060(7) 0.037(7) 0.018(5) C31 0.014(4) 0.023(4) 0.028(4) -0.004(3) 0.004(3) 0.002(3) C32 0.035(4) 0.023(4) 0.034(5) -0.008(3) 0.010(3) -0.010(3) C33 0.026(4) 0.050(6) 0.050(5) -0.031(4) 0.000(4) -0.005(4) C34 0.036(5) 0.048(6) 0.040(5) -0.021(4) -0.019(4) 0.017(4) C35 0.042(5) 0.033(5) 0.040(5) -0.004(4) -0.015(4) 0.016(4) C36 0.029(4) 0.015(3) 0.031(5) 0.001(4) -0.011(4) 0.001(3) C37 0.023(3) 0.017(3) 0.025(5) -0.001(3) 0.001(3) -0.002(3) C38 0.026(4) 0.021(4) 0.029(4) 0.004(3) -0.004(3) 0.000(3) C39 0.022(4) 0.031(4) 0.044(6) 0.005(4) -0.005(3) 0.001(3) C40 0.025(4) 0.030(4) 0.044(4) -0.001(5) 0.001(5) -0.008(3) C41 0.031(4) 0.020(4) 0.044(5) 0.005(4) 0.006(4) -0.002(3) C42 0.025(4) 0.017(4) 0.034(4) 0.002(3) 0.001(3) 0.002(3) C43 0.032(5) 0.011(3) 0.022(4) 0.000(3) -0.007(3) 0.004(3) C44 0.029(4) 0.026(4) 0.025(4) -0.002(3) -0.002(3) 0.003(3) C45 0.044(5) 0.035(5) 0.023(4) 0.003(4) -0.001(4) 0.006(4) C46 0.039(5) 0.039(5) 0.024(4) -0.004(4) -0.010(4) 0.011(4) C47 0.031(4) 0.038(4) 0.027(4) 0.000(4) -0.006(4) 0.014(4) C48 0.025(4) 0.027(4) 0.025(4) 0.001(3) -0.004(3) 0.006(3) C49 0.029(4) 0.022(4) 0.021(4) -0.004(3) -0.001(3) -0.002(3) C50 0.030(4) 0.029(4) 0.024(4) 0.000(3) -0.002(3) 0.000(4) C51 0.048(5) 0.045(5) 0.027(5) -0.001(4) 0.004(4) 0.006(4) C52 0.042(5) 0.051(6) 0.025(5) -0.006(4) 0.008(4) -0.001(4) C53 0.030(4) 0.033(5) 0.035(5) -0.012(4) 0.005(4) 0.000(4) C54 0.028(4) 0.028(4) 0.032(5) -0.005(3) 0.002(3) 0.000(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' Nd Nd -0.1943 3.0179 '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 Nd1 Br2 173.15(3) Br1 Nd1 Br3 91.38(3) Br2 Nd1 Br3 95.34(3) O1 Nd1 Br1 91.04(13) O1 Nd1 Br2 90.45(13) O1 Nd1 Br3 88.59(12) O1 Nd1 O2 177.70(16) O1 Nd1 O3 92.20(19) O2 Nd1 Br1 89.81(14) O2 Nd1 Br2 88.95(13) O2 Nd1 Br3 89.26(13) O2 Nd1 O3 89.99(19) O3 Nd1 Br1 85.78(15) O3 Nd1 Br2 87.49(15) O3 Nd1 Br3 177.06(14) O1 P1 C1 109.2(3) O1 P1 C7 109.0(3) O1 P1 C13 110.2(3) C1 P1 C13 110.3(3) C7 P1 C1 109.6(3) C7 P1 C13 108.5(3) O2 P2 C19 109.7(3) O2 P2 C25 107.6(4) O2 P2 C31 110.5(3) C25 P2 C19 114.6(5) C31 P2 C19 106.8(3) C31 P2 C25 107.6(4) O3 P3 C37 109.4(3) O3 P3 C43 109.1(3) O3 P3 C49 111.7(4) C37 P3 C49 106.4(3) C43 P3 C37 107.8(4) C43 P3 C49 112.4(4) P1 O1 Nd1 165.2(3) P2 O2 Nd1 159.2(3) P3 O3 Nd1 171.2(3) P1 C1 H1 108.6 C2 C1 P1 111.7(5) C2 C1 H1 108.6 C6 C1 P1 109.8(5) C6 C1 H1 108.6 C6 C1 C2 109.5(6) C1 C2 H2A 109.7 C1 C2 H2B 109.7 H2A C2 H2B 108.2 C3 C2 C1 109.7(7) C3 C2 H2A 109.7 C3 C2 H2B 109.7 C2 C3 H3A 109.1 C2 C3 H3B 109.1 H3A C3 H3B 107.8 C4 C3 C2 112.5(7) C4 C3 H3A 109.1 C4 C3 H3B 109.1 C3 C4 H4A 109.4 C3 C4 H4B 109.4 C3 C4 C5 111.2(7) H4A C4 H4B 108.0 C5 C4 H4A 109.4 C5 C4 H4B 109.4 C4 C5 H5A 109.6 C4 C5 H5B 109.6 C4 C5 C6 110.3(7) H5A C5 H5B 108.1 C6 C5 H5A 109.6 C6 C5 H5B 109.6 C1 C6 H6A 109.4 C1 C6 H6B 109.4 C5 C6 C1 111.3(6) C5 C6 H6A 109.4 C5 C6 H6B 109.4 H6A C6 H6B 108.0 P1 C7 H7 106.7 C8 C7 P1 114.5(5) C8 C7 H7 106.7 C8 C7 C12 110.4(6) C12 C7 P1 111.5(5) C12 C7 H7 106.7 C7 C8 H8A 109.6 C7 C8 H8B 109.6 H8A C8 H8B 108.1 C9 C8 C7 110.2(6) C9 C8 H8A 109.6 C9 C8 H8B 109.6 C8 C9 H9A 109.2 C8 C9 H9B 109.2 H9A C9 H9B 107.9 C10 C9 C8 112.1(7) C10 C9 H9A 109.2 C10 C9 H9B 109.2 C9 C10 H10A 109.2 C9 C10 H10B 109.2 H10A C10 H10B 107.9 C11 C10 C9 112.2(7) C11 C10 H10A 109.2 C11 C10 H10B 109.2 C10 C11 H11A 109.2 C10 C11 H11B 109.2 C10 C11 C12 111.9(6) H11A C11 H11B 107.9 C12 C11 H11A 109.2 C12 C11 H11B 109.2 C7 C12 H12A 109.7 C7 C12 H12B 109.7 C11 C12 C7 109.9(6) C11 C12 H12A 109.7 C11 C12 H12B 109.7 H12A C12 H12B 108.2 P1 C13 H13 106.3 C14 C13 P1 110.4(5) C14 C13 H13 106.3 C18 C13 P1 114.8(5) C18 C13 H13 106.3 C18 C13 C14 112.0(6) C13 C14 H14A 109.3 C13 C14 H14B 109.3 H14A C14 H14B 108.0 C15 C14 C13 111.6(7) C15 C14 H14A 109.3 C15 C14 H14B 109.3 C14 C15 H15A 109.3 C14 C15 H15B 109.3 C14 C15 C16 111.8(7) H15A C15 H15B 107.9 C16 C15 H15A 109.3 C16 C15 H15B 109.3 C15 C16 H16A 109.7 C15 C16 H16B 109.7 C15 C16 C17 109.8(6) H16A C16 H16B 108.2 C17 C16 H16A 109.7 C17 C16 H16B 109.7 C16 C17 H17A 109.2 C16 C17 H17B 109.2 C16 C17 C18 112.1(6) H17A C17 H17B 107.9 C18 C17 H17A 109.2 C18 C17 H17B 109.2 C13 C18 H18A 109.2 C13 C18 H18B 109.2 C17 C18 C13 111.9(6) C17 C18 H18A 109.2 C17 C18 H18B 109.2 H18A C18 H18B 107.9 P2 C19 H19 105.9 C20 C19 P2 112.3(6) C20 C19 H19 105.9 C20 C19 C24 111.0(7) C24 C19 P2 115.2(5) C24 C19 H19 105.9 C19 C20 H20A 109.5 C19 C20 H20B 109.5 C19 C20 C21 110.8(8) H20A C20 H20B 108.1 C21 C20 H20A 109.5 C21 C20 H20B 109.5 C20 C21 H21A 109.1 C20 C21 H21B 109.1 C20 C21 C22 112.6(9) H21A C21 H21B 107.8 C22 C21 H21A 109.1 C22 C21 H21B 109.1 C21 C22 H22A 109.4 C21 C22 H22B 109.4 H22A C22 H22B 108.0 C23 C22 C21 111.4(8) C23 C22 H22A 109.4 C23 C22 H22B 109.4 C22 C23 H23A 109.1 C22 C23 H23B 109.1 C22 C23 C24 112.5(7) H23A C23 H23B 107.8 C24 C23 H23A 109.1 C24 C23 H23B 109.1 C19 C24 C23 110.6(7) C19 C24 H24A 109.5 C19 C24 H24B 109.5 C23 C24 H24A 109.5 C23 C24 H24B 109.5 H24A C24 H24B 108.1 P2 C25 H25 99.5 C26 C25 P2 116.1(6) C26 C25 H25 99.5 C30 C25 P2 117.8(7) C30 C25 H25 99.5 C30 C25 C26 118.1(8) C25 C26 H26A 108.9 C25 C26 H26B 108.9 C25 C26 C27 113.5(8) H26A C26 H26B 107.7 C27 C26 H26A 108.9 C27 C26 H26B 108.9 C26 C27 H27A 107.5 C26 C27 H27B 107.5 H27A C27 H27B 107.0 C28 C27 C26 119.3(9) C28 C27 H27A 107.5 C28 C27 H27B 107.5 C27 C28 H28A 107.7 C27 C28 H28B 107.7 C27 C28 C29 118.4(9) H28A C28 H28B 107.1 C29 C28 H28A 107.7 C29 C28 H28B 107.7 C28 C29 H29A 108.7 C28 C29 H29B 108.7 C28 C29 C30 114.2(8) H29A C29 H29B 107.6 C30 C29 H29A 108.7 C30 C29 H29B 108.7 C25 C30 C29 117.0(9) C25 C30 H30A 108.1 C25 C30 H30B 108.1 C29 C30 H30A 108.1 C29 C30 H30B 108.1 H30A C30 H30B 107.3 P2 C31 H31 108.3 C32 C31 P2 112.2(5) C32 C31 H31 108.3 C36 C31 P2 110.5(5) C36 C31 H31 108.3 C36 C31 C32 109.3(6) C31 C32 H32A 109.1 C31 C32 H32B 109.1 H32A C32 H32B 107.8 C33 C32 C31 112.4(7) C33 C32 H32A 109.1 C33 C32 H32B 109.1 C32 C33 H33A 109.4 C32 C33 H33B 109.4 C32 C33 C34 111.4(7) H33A C33 H33B 108.0 C34 C33 H33A 109.4 C34 C33 H33B 109.4 C33 C34 H34A 109.7 C33 C34 H34B 109.7 H34A C34 H34B 108.2 C35 C34 C33 109.9(7) C35 C34 H34A 109.7 C35 C34 H34B 109.7 C34 C35 H35A 109.6 C34 C35 H35B 109.6 C34 C35 C36 110.2(7) H35A C35 H35B 108.1 C36 C35 H35A 109.6 C36 C35 H35B 109.6 C31 C36 H36A 109.5 C31 C36 H36B 109.5 C35 C36 C31 110.9(7) C35 C36 H36A 109.5 C35 C36 H36B 109.5 H36A C36 H36B 108.1 P3 C37 H37 105.8 C38 C37 P3 113.3(5) C38 C37 H37 105.8 C38 C37 C42 110.3(6) C42 C37 P3 114.8(5) C42 C37 H37 105.8 C37 C38 H38A 109.4 C37 C38 H38B 109.4 C37 C38 C39 111.0(6) H38A C38 H38B 108.0 C39 C38 H38A 109.4 C39 C38 H38B 109.4 C38 C39 H39A 109.1 C38 C39 H39B 109.1 H39A C39 H39B 107.9 C40 C39 C38 112.3(6) C40 C39 H39A 109.1 C40 C39 H39B 109.1 C39 C40 H40A 109.7 C39 C40 H40B 109.7 C39 C40 C41 109.6(6) H40A C40 H40B 108.2 C41 C40 H40A 109.7 C41 C40 H40B 109.7 C40 C41 H41A 109.2 C40 C41 H41B 109.2 C40 C41 C42 112.1(7) H41A C41 H41B 107.9 C42 C41 H41A 109.2 C42 C41 H41B 109.2 C37 C42 H42A 109.8 C37 C42 H42B 109.8 C41 C42 C37 109.2(6) C41 C42 H42A 109.8 C41 C42 H42B 109.8 H42A C42 H42B 108.3 P3 C43 H43 108.8 C44 C43 P3 111.1(5) C44 C43 H43 108.8 C44 C43 C48 109.3(6) C48 C43 P3 110.0(5) C48 C43 H43 108.8 C43 C44 H44A 109.3 C43 C44 H44B 109.3 C43 C44 C45 111.4(6) H44A C44 H44B 108.0 C45 C44 H44A 109.3 C45 C44 H44B 109.3 C44 C45 H45A 109.3 C44 C45 H45B 109.3 H45A C45 H45B 107.9 C46 C45 C44 111.8(7) C46 C45 H45A 109.3 C46 C45 H45B 109.3 C45 C46 H46A 109.6 C45 C46 H46B 109.6 C45 C46 C47 110.4(7) H46A C46 H46B 108.1 C47 C46 H46A 109.6 C47 C46 H46B 109.6 C46 C47 H47A 109.3 C46 C47 H47B 109.3 C46 C47 C48 111.5(6) H47A C47 H47B 108.0 C48 C47 H47A 109.3 C48 C47 H47B 109.3 C43 C48 H48A 109.2 C43 C48 H48B 109.2 C47 C48 C43 112.0(6) C47 C48 H48A 109.2 C47 C48 H48B 109.2 H48A C48 H48B 107.9 P3 C49 H49 106.3 C50 C49 P3 109.5(5) C50 C49 H49 106.3 C50 C49 C54 110.4(7) C54 C49 P3 117.5(6) C54 C49 H49 106.3 C49 C50 H50A 109.1 C49 C50 H50B 109.1 H50A C50 H50B 107.8 C51 C50 C49 112.6(7) C51 C50 H50A 109.1 C51 C50 H50B 109.1 C50 C51 H51A 109.4 C50 C51 H51B 109.4 C50 C51 C52 111.2(8) H51A C51 H51B 108.0 C52 C51 H51A 109.4 C52 C51 H51B 109.4 C51 C52 H52A 109.3 C51 C52 H52B 109.3 H52A C52 H52B 107.9 C53 C52 C51 111.8(7) C53 C52 H52A 109.3 C53 C52 H52B 109.3 C52 C53 H53A 109.1 C52 C53 H53B 109.1 C52 C53 C54 112.5(7) H53A C53 H53B 107.8 C54 C53 H53A 109.1 C54 C53 H53B 109.1 C49 C54 H54A 109.6 C49 C54 H54B 109.6 C53 C54 C49 110.2(7) C53 C54 H54A 109.6 C53 C54 H54B 109.6 H54A C54 H54B 108.1 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Nd1 Br1 2.8796(8) Nd1 Br2 2.8908(9) Nd1 Br3 2.9168(6) Nd1 O1 2.297(5) Nd1 O2 2.309(5) Nd1 O3 2.336(4) P1 O1 1.513(5) P1 C1 1.818(7) P1 C7 1.810(7) P1 C13 1.831(7) P2 O2 1.511(5) P2 C19 1.818(8) P2 C25 1.815(8) P2 C31 1.804(8) P3 O3 1.513(4) P3 C37 1.824(7) P3 C43 1.816(8) P3 C49 1.834(8) C1 H1 1.0000 C1 C2 1.542(10) C1 C6 1.535(10) C2 H2A 0.9900 C2 H2B 0.9900 C2 C3 1.539(11) C3 H3A 0.9900 C3 H3B 0.9900 C3 C4 1.510(12) C4 H4A 0.9900 C4 H4B 0.9900 C4 C5 1.524(12) C5 H5A 0.9900 C5 H5B 0.9900 C5 C6 1.530(10) C6 H6A 0.9900 C6 H6B 0.9900 C7 H7 1.0000 C7 C8 1.540(10) C7 C12 1.549(11) C8 H8A 0.9900 C8 H8B 0.9900 C8 C9 1.535(11) C9 H9A 0.9900 C9 H9B 0.9900 C9 C10 1.521(12) C10 H10A 0.9900 C10 H10B 0.9900 C10 C11 1.515(11) C11 H11A 0.9900 C11 H11B 0.9900 C11 C12 1.525(9) C12 H12A 0.9900 C12 H12B 0.9900 C13 H13 1.0000 C13 C14 1.539(10) C13 C18 1.531(10) C14 H14A 0.9900 C14 H14B 0.9900 C14 C15 1.510(11) C15 H15A 0.9900 C15 H15B 0.9900 C15 C16 1.518(11) C16 H16A 0.9900 C16 H16B 0.9900 C16 C17 1.529(11) C17 H17A 0.9900 C17 H17B 0.9900 C17 C18 1.531(10) C18 H18A 0.9900 C18 H18B 0.9900 C19 H19 1.0000 C19 C20 1.503(11) C19 C24 1.526(10) C20 H20A 0.9900 C20 H20B 0.9900 C20 C21 1.506(14) C21 H21A 0.9900 C21 H21B 0.9900 C21 C22 1.510(14) C22 H22A 0.9900 C22 H22B 0.9900 C22 C23 1.500(13) C23 H23A 0.9900 C23 H23B 0.9900 C23 C24 1.540(11) C24 H24A 0.9900 C24 H24B 0.9900 C25 H25 1.0000 C25 C26 1.493(11) C25 C30 1.418(13) C26 H26A 0.9900 C26 H26B 0.9900 C26 C27 1.502(12) C27 H27A 0.9900 C27 H27B 0.9900 C27 C28 1.405(15) C28 H28A 0.9900 C28 H28B 0.9900 C28 C29 1.488(14) C29 H29A 0.9900 C29 H29B 0.9900 C29 C30 1.503(12) C30 H30A 0.9900 C30 H30B 0.9900 C31 H31 1.0000 C31 C32 1.536(10) C31 C36 1.529(11) C32 H32A 0.9900 C32 H32B 0.9900 C32 C33 1.512(12) C33 H33A 0.9900 C33 H33B 0.9900 C33 C34 1.524(14) C34 H34A 0.9900 C34 H34B 0.9900 C34 C35 1.513(12) C35 H35A 0.9900 C35 H35B 0.9900 C35 C36 1.521(11) C36 H36A 0.9900 C36 H36B 0.9900 C37 H37 1.0000 C37 C38 1.527(10) C37 C42 1.536(9) C38 H38A 0.9900 C38 H38B 0.9900 C38 C39 1.530(10) C39 H39A 0.9900 C39 H39B 0.9900 C39 C40 1.513(10) C40 H40A 0.9900 C40 H40B 0.9900 C40 C41 1.517(12) C41 H41A 0.9900 C41 H41B 0.9900 C41 C42 1.534(10) C42 H42A 0.9900 C42 H42B 0.9900 C43 H43 1.0000 C43 C44 1.532(11) C43 C48 1.540(11) C44 H44A 0.9900 C44 H44B 0.9900 C44 C45 1.533(11) C45 H45A 0.9900 C45 H45B 0.9900 C45 C46 1.512(12) C46 H46A 0.9900 C46 H46B 0.9900 C46 C47 1.515(12) C47 H47A 0.9900 C47 H47B 0.9900 C47 C48 1.536(10) C48 H48A 0.9900 C48 H48B 0.9900 C49 H49 1.0000 C49 C50 1.522(11) C49 C54 1.530(11) C50 H50A 0.9900 C50 H50B 0.9900 C50 C51 1.516(11) C51 H51A 0.9900 C51 H51B 0.9900 C51 C52 1.524(12) C52 H52A 0.9900 C52 H52B 0.9900 C52 C53 1.523(13) C53 H53A 0.9900 C53 H53B 0.9900 C53 C54 1.524(11) C54 H54A 0.9900 C54 H54B 0.9900 loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 1.006(12) 2 -0.006(12)