#------------------------------------------------------------------------------ #$Date: 2021-10-02 02:04:16 +0300 (Sat, 02 Oct 2021) $ #$Revision: 269445 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/85/7708502.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_7708502 loop_ _publ_author_name 'Windorff, Cory James' 'Beltr\'an Leiva, Mar\'ia Joaquina' 'Albrecht-Schmitt, Thomas E.' 'Bai, Zhuanling' 'Celis-Barros, Cristian' 'Goodwin, Conrad Alexander Phillip' 'Huffman, Zachary' 'McKinnon, Noah C.' 'Sperling, Joseph M.' _publ_section_title ; Synthesis, characterization, and theoretical analysis of a plutonyl phosphine oxide complex ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D1DT03041H _journal_year 2021 _chemical_formula_moiety 'C36 H66 Cl2 O4 P2 Pu' _chemical_formula_sum 'C36 H66 Cl2 O4 P2 Pu' _chemical_formula_weight 934.82 _chemical_name_common 'plutonyldichloride bis(tricyclohexylphosphine oxide)' _chemical_name_systematic 'plutoniumdioxodicholoro bis(tricyclyhexylphosphine oxide)' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2019-10-25 _audit_creation_method ; Olex2 1.2 (compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492) ; _audit_update_record ; 2021-08-04 deposited with the CCDC. 2021-10-01 downloaded from the CCDC. ; _cell_angle_alpha 69.306(4) _cell_angle_beta 89.512(4) _cell_angle_gamma 76.786(4) _cell_formula_units_Z 2 _cell_length_a 8.7416(4) _cell_length_b 14.1281(7) _cell_length_c 17.1398(8) _cell_measurement_reflns_used 16651 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 27.8970 _cell_measurement_theta_min 2.4580 _cell_volume 1921.72(17) _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 100(2) _diffrn_detector CMOS _diffrn_detector_area_resol_mean 7.9 _diffrn_detector_type 'CMOS detector' _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.984 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \f -25.73 334.27 2.00 45.00 138.83 -19.51 73.71 -- 180 2 \f -25.73 334.27 2.00 45.00 -49.29 -19.51 73.71 -- 180 3 \w -49.29 136.71 2.00 45.00 -- -19.51 73.71 -25.73 93 4 \w -49.29 136.71 2.00 45.00 -- -19.51 73.71 25.27 93 5 \w -49.29 136.71 2.00 45.00 -- -19.51 73.71 76.28 93 6 \w -49.29 136.71 2.00 45.00 -- -19.51 73.71 127.28 93 7 \w -49.29 136.71 2.00 45.00 -- -19.51 73.71 178.27 93 8 \w -49.29 136.71 2.00 45.00 -- -19.51 73.71-130.72 93 9 \w -49.29 136.71 2.00 45.00 -- -19.51 73.71 -79.73 93 10 \w -48.41 139.59 2.00 45.00 -- -18.62 73.71 -52.33 94 11 \w -48.41 139.59 2.00 45.00 -- -18.62 73.71 102.98 94 12 \w 41.59 139.59 2.00 45.00 -- -18.62 73.71-151.57 49 ; _diffrn_measurement_device 'abstract diffractometer' _diffrn_measurement_device_type 'Saxi-CrysAlisPro-abstract goniometer imported SAXI images' _diffrn_measurement_method '\w and \f scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0221200000 _diffrn_orient_matrix_UB_12 -0.0236819000 _diffrn_orient_matrix_UB_13 -0.0269540000 _diffrn_orient_matrix_UB_21 0.0586159000 _diffrn_orient_matrix_UB_22 -0.0461232000 _diffrn_orient_matrix_UB_23 0.0213500000 _diffrn_orient_matrix_UB_31 -0.0553691000 _diffrn_orient_matrix_UB_32 -0.0192304000 _diffrn_orient_matrix_UB_33 0.0280532000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1237 _diffrn_reflns_av_unetI/netI 0.1075 _diffrn_reflns_Laue_measured_fraction_full 0.985 _diffrn_reflns_Laue_measured_fraction_max 0.984 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 87287 _diffrn_reflns_point_group_measured_fraction_full 0.985 _diffrn_reflns_point_group_measured_fraction_max 0.984 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.681 _diffrn_reflns_theta_min 1.588 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 1.973 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.71991 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear brown' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.621 _exptl_crystal_description irregular _exptl_crystal_F_000 944 _exptl_crystal_preparation 'By CJW.' _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Methanol/Ethanol' _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _refine_diff_density_max 2.231 _refine_diff_density_min -1.398 _refine_diff_density_rms 0.190 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.877 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 409 _refine_ls_number_reflns 7198 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.877 _refine_ls_R_factor_all 0.0832 _refine_ls_R_factor_gt 0.0399 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0408P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0782 _refine_ls_wR_factor_ref 0.0829 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4109 _reflns_number_total 7198 _reflns_threshold_expression 'I > 2\s(I)' _twin_special_details ; Component 2 rotated by 5.7706\% around [0.01 0.31 0.95] (reciprocal) or [-0.01 0.06 1.00] (direct) Component 3 rotated by 179.0377\% around [0.91 0.40 0.01] (reciprocal) or [1.00 0.04 -0.01] (direct) ; _cod_data_source_file d1dt03041h2.cif _cod_data_source_block cjw103 _cod_database_code 7708502 _lanl_internal_la-ur LA-UR-19-30804 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula PuO2Cl2(OPC18H33)2 _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 0.827 _shelx_estimated_absorpt_t_min 0.827 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups 2.a Ternary CH refined with riding coordinates: C1(H1), C7(H7), C13(H13), C19(H19), C25(H25), C31(H31) 2.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) ; _shelx_res_file ; TITL cjw103_twin1_hklf4_a.res in P-1 cjw103.res created by SHELXL-2018/3 at 13:30:13 on 25-Oct-2019 REM Old TITL cjw103_twin1_hklf4 in P-1 REM SHELXT solution in P-1: R1 0.125, Rweak 0.006, Alpha 0.079 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C32 O8 P3 Cl2 Pu CELL 0.71073 8.7416 14.1281 17.1398 69.306 89.512 76.786 ZERR 2 0.0004 0.0007 0.0008 0.004 0.004 0.004 LATT 1 SFAC C H O P Cl Pu UNIT 72 132 8 4 4 2 L.S. 10 0 0 PLAN 20 SIZE 0.1 0.1 0.1 TEMP -173(2) BOND list 4 BOND $H fmap 2 53 acta SHEL 100 0.82 OMIT 0 2 8 OMIT 0 3 8 OMIT 1 4 9 OMIT 2 5 12 OMIT 1 3 7 REM REM REM WGHT 0.040800 FVAR 0.19411 PU1 6 0.000000 0.500000 0.500000 10.50000 0.02515 0.02270 = 0.01381 -0.00567 0.00110 -0.00699 CL1 5 0.258101 0.353860 0.568455 11.00000 0.02788 0.02703 = 0.03573 -0.00712 -0.00421 -0.00249 P1 4 0.199455 0.714439 0.491835 11.00000 0.01854 0.01613 = 0.01857 -0.00633 0.00476 -0.00493 O1 3 0.057127 0.496916 0.401943 11.00000 0.04217 0.04104 = 0.01672 -0.01744 0.01376 -0.01674 O3 3 0.137529 0.624550 0.488145 11.00000 0.02002 0.01597 = 0.03086 -0.00588 0.00588 -0.00894 C1 1 0.325955 0.753633 0.407489 11.00000 0.01659 0.02494 = 0.01515 -0.00734 0.00285 -0.00127 AFIX 13 H1 2 0.434492 0.709809 0.429789 11.00000 -1.20000 AFIX 0 C2 1 0.338784 0.867788 0.378836 11.00000 0.02424 0.01642 = 0.01602 -0.00737 -0.00007 -0.00366 AFIX 23 H2A 2 0.233203 0.914883 0.357756 11.00000 -1.20000 H2B 2 0.376426 0.881460 0.427216 11.00000 -1.20000 AFIX 0 C3 1 0.452018 0.890948 0.310060 11.00000 0.03404 0.02107 = 0.02142 -0.00826 0.00390 -0.00693 AFIX 23 H3A 2 0.452092 0.965794 0.290337 11.00000 -1.20000 H3B 2 0.560209 0.849935 0.333074 11.00000 -1.20000 AFIX 0 C4 1 0.404944 0.864076 0.236786 11.00000 0.03192 0.03212 = 0.02143 -0.00417 0.00809 -0.01028 AFIX 23 H4A 2 0.300881 0.909813 0.210555 11.00000 -1.20000 H4B 2 0.482728 0.877278 0.194339 11.00000 -1.20000 AFIX 0 C5 1 0.396369 0.750910 0.264107 11.00000 0.03027 0.02768 = 0.01936 -0.01202 -0.00201 -0.00565 AFIX 23 H5A 2 0.502642 0.704893 0.285242 11.00000 -1.20000 H5B 2 0.360208 0.737091 0.215490 11.00000 -1.20000 AFIX 0 C6 1 0.282982 0.726544 0.332640 11.00000 0.02271 0.02528 = 0.02795 -0.01063 0.00825 -0.01044 AFIX 23 H6A 2 0.284652 0.651449 0.352017 11.00000 -1.20000 H6B 2 0.174574 0.766556 0.309198 11.00000 -1.20000 AFIX 0 C7 1 0.312325 0.675114 0.591688 11.00000 0.01999 0.02103 = 0.01434 -0.00616 0.00139 0.00012 AFIX 13 H7 2 0.236556 0.662317 0.636112 11.00000 -1.20000 AFIX 0 C8 1 0.437819 0.571193 0.610259 11.00000 0.03414 0.02481 = 0.02184 -0.00967 0.00040 -0.00550 AFIX 23 H8A 2 0.386526 0.516595 0.607724 11.00000 -1.20000 H8B 2 0.515736 0.580303 0.567604 11.00000 -1.20000 AFIX 0 C9 1 0.521047 0.537754 0.696938 11.00000 0.04216 0.02809 = 0.02352 -0.00971 -0.00665 -0.00190 AFIX 23 H9A 2 0.601809 0.471746 0.708060 11.00000 -1.20000 H9B 2 0.443369 0.524484 0.739437 11.00000 -1.20000 AFIX 0 C10 1 0.600485 0.620498 0.705605 11.00000 0.02806 0.04377 = 0.01930 -0.01035 -0.00491 -0.00933 AFIX 23 H10A 2 0.650124 0.596887 0.763121 11.00000 -1.20000 H10B 2 0.683758 0.630775 0.666090 11.00000 -1.20000 AFIX 0 C11 1 0.476046 0.723426 0.686666 11.00000 0.02991 0.03946 = 0.01993 -0.01783 -0.00034 -0.01022 AFIX 23 H11A 2 0.398374 0.714151 0.729445 11.00000 -1.20000 H11B 2 0.527628 0.777703 0.689647 11.00000 -1.20000 AFIX 0 C12 1 0.391121 0.759109 0.600353 11.00000 0.03788 0.01585 = 0.02524 -0.00652 0.00121 -0.00571 AFIX 23 H12A 2 0.467441 0.773868 0.557277 11.00000 -1.20000 H12B 2 0.309630 0.824446 0.590650 11.00000 -1.20000 AFIX 0 C13 1 0.036798 0.823868 0.483490 11.00000 0.01843 0.02352 = 0.02655 -0.01438 0.00655 -0.00568 AFIX 13 H13 2 0.081901 0.881316 0.487081 11.00000 -1.20000 AFIX 0 C14 1 -0.071022 0.797699 0.553949 11.00000 0.02232 0.02773 = 0.01978 -0.00973 0.00249 -0.00271 AFIX 23 H14A 2 -0.008467 0.773838 0.608199 11.00000 -1.20000 H14B 2 -0.114843 0.739610 0.552414 11.00000 -1.20000 AFIX 0 C15 1 -0.206529 0.890370 0.548206 11.00000 0.02361 0.03433 = 0.02874 -0.01816 0.01096 -0.01132 AFIX 23 H15A 2 -0.277133 0.868178 0.593051 11.00000 -1.20000 H15B 2 -0.163983 0.945638 0.556484 11.00000 -1.20000 AFIX 0 C16 1 -0.298739 0.933023 0.464483 11.00000 0.02248 0.03249 = 0.02945 -0.01618 0.00831 -0.00393 AFIX 23 H16A 2 -0.379984 0.996604 0.460299 11.00000 -1.20000 H16B 2 -0.353246 0.880920 0.459633 11.00000 -1.20000 AFIX 0 C17 1 -0.192246 0.959470 0.392667 11.00000 0.02237 0.02828 = 0.02157 -0.00764 0.00398 -0.00433 AFIX 23 H17A 2 -0.255822 0.984248 0.338623 11.00000 -1.20000 H17B 2 -0.145350 1.016326 0.394242 11.00000 -1.20000 AFIX 0 C18 1 -0.062751 0.865471 0.399053 11.00000 0.01956 0.02226 = 0.02211 -0.00603 0.00356 -0.00638 AFIX 23 H18A 2 0.005867 0.884567 0.352618 11.00000 -1.20000 H18B 2 -0.109409 0.810140 0.393925 11.00000 -1.20000 AFIX 0 PU2 6 0.500000 0.500000 1.000000 10.50000 0.01877 0.01708 = 0.01143 -0.00396 0.00022 -0.00512 CL2 5 0.738491 0.407577 0.935053 11.00000 0.02993 0.03581 = 0.03921 -0.02143 0.01400 -0.01008 P2 4 0.691824 0.721949 0.974471 11.00000 0.02036 0.01761 = 0.01553 -0.00792 0.00340 -0.00654 O2 3 0.594752 0.428569 1.099433 11.00000 0.03626 0.02637 = 0.01711 -0.00841 -0.00072 -0.00868 O4 3 0.628270 0.627546 0.987920 11.00000 0.02464 0.02613 = 0.01445 -0.00910 0.00194 -0.00408 C19 1 0.821259 0.698396 1.063663 11.00000 0.02357 0.01731 = 0.01664 -0.00732 0.00563 -0.00426 AFIX 13 H19 2 0.926731 0.660771 1.053633 11.00000 -1.20000 AFIX 0 C20 1 0.773191 0.624070 1.144267 11.00000 0.04322 0.03134 = 0.01792 -0.00778 -0.00253 -0.01035 AFIX 23 H20A 2 0.667906 0.657055 1.156675 11.00000 -1.20000 H20B 2 0.765937 0.559194 1.136165 11.00000 -1.20000 AFIX 0 C21 1 0.891474 0.597547 1.217645 11.00000 0.04751 0.03133 = 0.02237 -0.00416 -0.00141 -0.02180 AFIX 23 H21A 2 0.994567 0.558609 1.207762 11.00000 -1.20000 H21B 2 0.855022 0.552508 1.269304 11.00000 -1.20000 AFIX 0 C22 1 0.910647 0.698110 1.228881 11.00000 0.04675 0.04147 = 0.02154 -0.01166 -0.00308 -0.01575 AFIX 23 H22A 2 0.808999 0.734704 1.242287 11.00000 -1.20000 H22B 2 0.989578 0.679816 1.276184 11.00000 -1.20000 AFIX 0 C23 1 0.962264 0.768491 1.151238 11.00000 0.03540 0.03393 = 0.01773 -0.01251 -0.00740 -0.00690 AFIX 23 H23A 2 1.067549 0.733663 1.140253 11.00000 -1.20000 H23B 2 0.971370 0.833024 1.159363 11.00000 -1.20000 AFIX 0 C24 1 0.847579 0.796255 1.076986 11.00000 0.02579 0.02922 = 0.01856 -0.01268 0.00307 -0.01036 AFIX 23 H24A 2 0.888147 0.839927 1.026166 11.00000 -1.20000 H24B 2 0.745461 0.837739 1.085450 11.00000 -1.20000 AFIX 0 C25 1 0.798134 0.746435 0.880002 11.00000 0.01424 0.02103 = 0.01279 -0.00620 0.00038 0.00053 AFIX 13 H25 2 0.720860 0.755310 0.833774 11.00000 -1.20000 AFIX 0 C26 1 0.853546 0.848305 0.854103 11.00000 0.02168 0.02486 = 0.02504 -0.00862 0.00521 -0.01204 AFIX 23 H26A 2 0.762177 0.907400 0.847892 11.00000 -1.20000 H26B 2 0.929769 0.844116 0.898296 11.00000 -1.20000 AFIX 0 C27 1 0.930801 0.867201 0.772014 11.00000 0.02374 0.02561 = 0.02958 -0.00478 0.00988 -0.01007 AFIX 23 H27A 2 0.971525 0.930615 0.758268 11.00000 -1.20000 H27B 2 0.851069 0.879261 0.726674 11.00000 -1.20000 AFIX 0 C28 1 1.065629 0.775033 0.776743 11.00000 0.03053 0.04085 = 0.02168 -0.01208 0.01090 -0.01485 AFIX 23 H28A 2 1.109973 0.788241 0.721615 11.00000 -1.20000 H28B 2 1.150249 0.767031 0.818256 11.00000 -1.20000 AFIX 0 C29 1 1.008702 0.675451 0.801654 11.00000 0.03416 0.02989 = 0.02185 -0.01332 0.01354 -0.01389 AFIX 23 H29A 2 1.099014 0.616301 0.806339 11.00000 -1.20000 H29B 2 0.931047 0.681407 0.757426 11.00000 -1.20000 AFIX 0 C30 1 0.932846 0.653316 0.884751 11.00000 0.03136 0.03453 = 0.01718 -0.01147 0.00675 -0.00917 AFIX 23 H30A 2 1.012800 0.640212 0.930294 11.00000 -1.20000 H30B 2 0.891658 0.590220 0.897400 11.00000 -1.20000 AFIX 0 C31 1 0.528613 0.834844 0.958480 11.00000 0.01615 0.01637 = 0.01361 -0.00714 -0.00136 -0.00518 AFIX 13 H31 2 0.573324 0.896583 0.950001 11.00000 -1.20000 AFIX 0 C32 1 0.433719 0.818882 1.035345 11.00000 0.02771 0.02696 = 0.01747 -0.01197 0.00387 -0.01027 AFIX 23 H32A 2 0.400139 0.752871 1.049091 11.00000 -1.20000 H32B 2 0.501590 0.812886 1.083636 11.00000 -1.20000 AFIX 0 C33 1 0.289570 0.907997 1.021195 11.00000 0.02233 0.02610 = 0.02462 -0.01426 0.00562 -0.00466 AFIX 23 H33A 2 0.228014 0.892662 1.071005 11.00000 -1.20000 H33B 2 0.323452 0.972635 1.013967 11.00000 -1.20000 AFIX 0 C34 1 0.186652 0.924823 0.945243 11.00000 0.01759 0.02385 = 0.02492 -0.00765 -0.00406 0.00121 AFIX 23 H34A 2 0.095589 0.984817 0.936851 11.00000 -1.20000 H34B 2 0.145589 0.862310 0.954294 11.00000 -1.20000 AFIX 0 C35 1 0.278722 0.945707 0.866940 11.00000 0.02674 0.03185 = 0.01674 -0.00482 -0.00305 -0.00240 AFIX 23 H35A 2 0.209652 0.953832 0.818370 11.00000 -1.20000 H35B 2 0.312099 1.011505 0.855093 11.00000 -1.20000 AFIX 0 C36 1 0.421276 0.857848 0.878724 11.00000 0.02241 0.02443 = 0.02425 -0.00452 0.00322 -0.00483 AFIX 23 H36A 2 0.482905 0.875738 0.829099 11.00000 -1.20000 H36B 2 0.386802 0.794257 0.883014 11.00000 -1.20000 AFIX 0 HKLF 4 REM cjw103_twin1_hklf4_a.res in P-1 REM wR2 = 0.0829, GooF = S = 0.877, Restrained GooF = 0.877 for all data REM R1 = 0.0399 for 4109 Fo > 4sig(Fo) and 0.0832 for all 7198 data REM 409 parameters refined using 0 restraints END WGHT 0.0408 0.0000 REM Highest difference peak 2.231, deepest hole -1.398, 1-sigma level 0.190 Q1 1 0.4496 0.5777 0.9844 11.00000 0.05 2.23 Q2 1 0.0534 0.4201 0.5153 11.00000 0.05 1.81 Q3 1 0.5007 0.4926 1.0330 11.00000 0.05 1.33 Q4 1 0.3880 0.5213 1.0161 11.00000 0.05 1.31 Q5 1 0.5735 0.5245 1.0070 11.00000 0.05 1.20 Q6 1 0.1361 0.4194 0.5559 11.00000 0.05 1.20 Q7 1 0.0487 0.6229 0.4781 11.00000 0.05 1.18 Q8 1 0.5525 0.6169 0.9723 11.00000 0.05 1.17 Q9 1 0.6582 0.3966 0.9791 11.00000 0.05 1.03 Q10 1 0.5642 0.3631 1.0768 11.00000 0.05 1.02 Q11 1 0.6363 0.4181 1.0554 11.00000 0.05 1.01 Q12 1 0.0610 0.3635 0.5764 11.00000 0.05 1.01 Q13 1 0.1270 0.4808 0.4801 11.00000 0.05 1.00 Q14 1 0.2491 0.4045 0.4379 11.00000 0.05 0.99 Q15 1 0.7634 0.3562 1.0676 11.00000 0.05 0.98 Q16 1 0.3087 0.4871 0.5028 11.00000 0.05 0.97 Q17 1 0.6444 0.4173 0.9578 11.00000 0.05 0.95 Q18 1 0.1593 0.3983 0.4844 11.00000 0.05 0.92 Q19 1 0.6794 0.6174 0.9606 11.00000 0.05 0.82 Q20 1 0.6057 0.7657 0.9663 11.00000 0.05 0.81 ; _shelx_res_checksum 21117 _olex2_exptl_crystal_mounting_method 'From paratone on a microscope slide, onto a micromount.' _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.349 _oxdiff_exptl_absorpt_empirical_full_min 0.798 _oxdiff_twin_integration_method simultaneous _oxdiff_twin_items 3 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pu1 Pu 0.000000 0.500000 0.500000 0.02060(14) Uani 1 2 d S T P . . Cl1 Cl 0.2581(2) 0.35386(13) 0.56846(11) 0.0321(4) Uani 1 1 d . . . . . P1 P 0.1995(2) 0.71444(15) 0.49183(13) 0.0176(5) Uani 1 1 d . . . . . O1 O 0.0571(6) 0.4969(4) 0.4019(3) 0.0303(12) Uani 1 1 d . . . . . O3 O 0.1375(5) 0.6245(3) 0.4881(3) 0.0222(13) Uani 1 1 d . . . . . C1 C 0.3260(8) 0.7536(5) 0.4075(4) 0.0195(18) Uani 1 1 d . . . . . H1 H 0.434492 0.709809 0.429789 0.023 Uiso 1 1 calc R . . . . C2 C 0.3388(8) 0.8678(5) 0.3788(4) 0.0187(17) Uani 1 1 d . . . . . H2A H 0.233203 0.914883 0.357756 0.022 Uiso 1 1 calc R . . . . H2B H 0.376426 0.881460 0.427216 0.022 Uiso 1 1 calc R . . . . C3 C 0.4520(8) 0.8909(5) 0.3101(4) 0.0253(17) Uani 1 1 d . . . . . H3A H 0.452092 0.965794 0.290337 0.030 Uiso 1 1 calc R . . . . H3B H 0.560209 0.849935 0.333074 0.030 Uiso 1 1 calc R . . . . C4 C 0.4049(9) 0.8641(5) 0.2368(4) 0.030(2) Uani 1 1 d . . . . . H4A H 0.300881 0.909813 0.210555 0.036 Uiso 1 1 calc R . . . . H4B H 0.482728 0.877278 0.194339 0.036 Uiso 1 1 calc R . . . . C5 C 0.3964(8) 0.7509(5) 0.2641(4) 0.0250(16) Uani 1 1 d . . . . . H5A H 0.502642 0.704893 0.285242 0.030 Uiso 1 1 calc R . . . . H5B H 0.360208 0.737091 0.215490 0.030 Uiso 1 1 calc R . . . . C6 C 0.2830(8) 0.7265(5) 0.3326(4) 0.0243(17) Uani 1 1 d . . . . . H6A H 0.284652 0.651449 0.352017 0.029 Uiso 1 1 calc R . . . . H6B H 0.174574 0.766556 0.309198 0.029 Uiso 1 1 calc R . . . . C7 C 0.3123(8) 0.6751(5) 0.5917(4) 0.0194(18) Uani 1 1 d . . . . . H7 H 0.236556 0.662317 0.636112 0.023 Uiso 1 1 calc R . . . . C8 C 0.4378(8) 0.5712(5) 0.6103(4) 0.0269(17) Uani 1 1 d . . . . . H8A H 0.386526 0.516595 0.607724 0.032 Uiso 1 1 calc R . . . . H8B H 0.515736 0.580303 0.567604 0.032 Uiso 1 1 calc R . . . . C9 C 0.5210(8) 0.5378(5) 0.6969(4) 0.0322(18) Uani 1 1 d . . . . . H9A H 0.601809 0.471746 0.708060 0.039 Uiso 1 1 calc R . . . . H9B H 0.443369 0.524484 0.739437 0.039 Uiso 1 1 calc R . . . . C10 C 0.6005(8) 0.6205(5) 0.7056(4) 0.0305(18) Uani 1 1 d . . . . . H10A H 0.650124 0.596887 0.763121 0.037 Uiso 1 1 calc R . . . . H10B H 0.683758 0.630775 0.666090 0.037 Uiso 1 1 calc R . . . . C11 C 0.4760(8) 0.7234(6) 0.6867(5) 0.0275(19) Uani 1 1 d . . . . . H11A H 0.398374 0.714151 0.729445 0.033 Uiso 1 1 calc R . . . . H11B H 0.527628 0.777703 0.689647 0.033 Uiso 1 1 calc R . . . . C12 C 0.3911(9) 0.7591(5) 0.6004(4) 0.027(2) Uani 1 1 d . . . . . H12A H 0.467441 0.773868 0.557277 0.032 Uiso 1 1 calc R . . . . H12B H 0.309630 0.824446 0.590650 0.032 Uiso 1 1 calc R . . . . C13 C 0.0368(8) 0.8239(6) 0.4835(5) 0.0213(19) Uani 1 1 d . . . . . H13 H 0.081901 0.881316 0.487081 0.026 Uiso 1 1 calc R . . . . C14 C -0.0710(8) 0.7977(6) 0.5539(4) 0.0235(19) Uani 1 1 d . . . . . H14A H -0.008467 0.773838 0.608199 0.028 Uiso 1 1 calc R . . . . H14B H -0.114843 0.739610 0.552414 0.028 Uiso 1 1 calc R . . . . C15 C -0.2065(9) 0.8904(6) 0.5482(5) 0.026(2) Uani 1 1 d . . . . . H15A H -0.277133 0.868178 0.593051 0.032 Uiso 1 1 calc R . . . . H15B H -0.163983 0.945638 0.556484 0.032 Uiso 1 1 calc R . . . . C16 C -0.2987(8) 0.9330(6) 0.4645(5) 0.027(2) Uani 1 1 d . . . . . H16A H -0.379984 0.996604 0.460299 0.033 Uiso 1 1 calc R . . . . H16B H -0.353246 0.880920 0.459633 0.033 Uiso 1 1 calc R . . . . C17 C -0.1922(8) 0.9595(5) 0.3927(4) 0.0248(19) Uani 1 1 d . . . . . H17A H -0.255822 0.984248 0.338623 0.030 Uiso 1 1 calc R . . . . H17B H -0.145350 1.016326 0.394242 0.030 Uiso 1 1 calc R . . . . C18 C -0.0628(8) 0.8655(5) 0.3991(4) 0.0216(19) Uani 1 1 d . . . . . H18A H 0.005867 0.884567 0.352618 0.026 Uiso 1 1 calc R . . . . H18B H -0.109409 0.810140 0.393925 0.026 Uiso 1 1 calc R . . . . Pu2 Pu 0.500000 0.500000 1.000000 0.01594(13) Uani 1 2 d S T P . . Cl2 Cl 0.7385(2) 0.40758(14) 0.93505(12) 0.0325(4) Uani 1 1 d . . . . . P2 P 0.6918(2) 0.72195(16) 0.97447(13) 0.0170(5) Uani 1 1 d . . . . . O2 O 0.5948(5) 0.4286(3) 1.0994(3) 0.0262(11) Uani 1 1 d . . . . . O4 O 0.6283(5) 0.6275(3) 0.9879(3) 0.0216(13) Uani 1 1 d . . . . . C19 C 0.8213(8) 0.6984(5) 1.0637(4) 0.0190(18) Uani 1 1 d . . . . . H19 H 0.926731 0.660771 1.053633 0.023 Uiso 1 1 calc R . . . . C20 C 0.7732(8) 0.6241(5) 1.1443(4) 0.0309(18) Uani 1 1 d . . . . . H20A H 0.667906 0.657055 1.156675 0.037 Uiso 1 1 calc R . . . . H20B H 0.765937 0.559194 1.136165 0.037 Uiso 1 1 calc R . . . . C21 C 0.8915(9) 0.5975(5) 1.2176(4) 0.0331(19) Uani 1 1 d . . . . . H21A H 0.994567 0.558609 1.207762 0.040 Uiso 1 1 calc R . . . . H21B H 0.855022 0.552508 1.269304 0.040 Uiso 1 1 calc R . . . . C22 C 0.9106(9) 0.6981(5) 1.2289(4) 0.0356(19) Uani 1 1 d . . . . . H22A H 0.808999 0.734704 1.242287 0.043 Uiso 1 1 calc R . . . . H22B H 0.989578 0.679816 1.276184 0.043 Uiso 1 1 calc R . . . . C23 C 0.9623(8) 0.7685(6) 1.1512(4) 0.0283(19) Uani 1 1 d . . . . . H23A H 1.067549 0.733663 1.140253 0.034 Uiso 1 1 calc R . . . . H23B H 0.971370 0.833024 1.159363 0.034 Uiso 1 1 calc R . . . . C24 C 0.8476(8) 0.7963(5) 1.0770(4) 0.0228(18) Uani 1 1 d . . . . . H24A H 0.888147 0.839927 1.026166 0.027 Uiso 1 1 calc R . . . . H24B H 0.745461 0.837739 1.085450 0.027 Uiso 1 1 calc R . . . . C25 C 0.7981(8) 0.7464(5) 0.8800(4) 0.0168(17) Uani 1 1 d . . . . . H25 H 0.720860 0.755310 0.833774 0.020 Uiso 1 1 calc R . . . . C26 C 0.8535(8) 0.8483(5) 0.8541(4) 0.0229(19) Uani 1 1 d . . . . . H26A H 0.762177 0.907400 0.847892 0.027 Uiso 1 1 calc R . . . . H26B H 0.929769 0.844116 0.898296 0.027 Uiso 1 1 calc R . . . . C27 C 0.9308(8) 0.8672(5) 0.7720(5) 0.027(2) Uani 1 1 d . . . . . H27A H 0.971525 0.930615 0.758268 0.033 Uiso 1 1 calc R . . . . H27B H 0.851069 0.879261 0.726674 0.033 Uiso 1 1 calc R . . . . C28 C 1.0656(8) 0.7750(5) 0.7767(4) 0.0298(18) Uani 1 1 d . . . . . H28A H 1.109973 0.788241 0.721615 0.036 Uiso 1 1 calc R . . . . H28B H 1.150249 0.767031 0.818256 0.036 Uiso 1 1 calc R . . . . C29 C 1.0087(8) 0.6755(5) 0.8017(4) 0.0265(17) Uani 1 1 d . . . . . H29A H 1.099014 0.616301 0.806339 0.032 Uiso 1 1 calc R . . . . H29B H 0.931047 0.681407 0.757426 0.032 Uiso 1 1 calc R . . . . C30 C 0.9328(8) 0.6533(5) 0.8848(4) 0.0269(17) Uani 1 1 d . . . . . H30A H 1.012800 0.640212 0.930294 0.032 Uiso 1 1 calc R . . . . H30B H 0.891658 0.590220 0.897400 0.032 Uiso 1 1 calc R . . . . C31 C 0.5286(8) 0.8348(5) 0.9585(4) 0.0147(18) Uani 1 1 d . . . . . H31 H 0.573324 0.896583 0.950001 0.018 Uiso 1 1 calc R . . . . C32 C 0.4337(9) 0.8189(6) 1.0353(4) 0.022(2) Uani 1 1 d . . . . . H32A H 0.400139 0.752871 1.049091 0.027 Uiso 1 1 calc R . . . . H32B H 0.501590 0.812886 1.083636 0.027 Uiso 1 1 calc R . . . . C33 C 0.2896(8) 0.9080(6) 1.0212(5) 0.023(2) Uani 1 1 d . . . . . H33A H 0.228014 0.892662 1.071005 0.028 Uiso 1 1 calc R . . . . H33B H 0.323452 0.972635 1.013967 0.028 Uiso 1 1 calc R . . . . C34 C 0.1867(8) 0.9248(5) 0.9452(4) 0.023(2) Uani 1 1 d . . . . . H34A H 0.095589 0.984817 0.936851 0.028 Uiso 1 1 calc R . . . . H34B H 0.145589 0.862310 0.954294 0.028 Uiso 1 1 calc R . . . . C35 C 0.2787(8) 0.9457(6) 0.8669(4) 0.0270(19) Uani 1 1 d . . . . . H35A H 0.209652 0.953832 0.818370 0.032 Uiso 1 1 calc R . . . . H35B H 0.312099 1.011505 0.855093 0.032 Uiso 1 1 calc R . . . . C36 C 0.4213(8) 0.8578(5) 0.8787(5) 0.025(2) Uani 1 1 d . . . . . H36A H 0.482905 0.875738 0.829099 0.030 Uiso 1 1 calc R . . . . H36B H 0.386802 0.794257 0.883014 0.030 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 Pu1 0.0252(3) 0.0227(3) 0.0138(3) -0.0057(2) 0.0011(2) -0.0070(2) Cl1 0.0279(11) 0.0270(10) 0.0357(11) -0.0071(8) -0.0042(8) -0.0025(8) P1 0.0185(13) 0.0161(11) 0.0186(11) -0.0063(9) 0.0048(8) -0.0049(9) O1 0.042(3) 0.041(3) 0.017(3) -0.017(2) 0.014(2) -0.017(3) O3 0.020(3) 0.016(3) 0.031(3) -0.006(3) 0.006(2) -0.009(3) C1 0.017(4) 0.025(4) 0.015(4) -0.007(3) 0.003(3) -0.001(3) C2 0.024(4) 0.016(4) 0.016(4) -0.007(3) 0.000(3) -0.004(3) C3 0.034(5) 0.021(4) 0.021(4) -0.008(3) 0.004(3) -0.007(3) C4 0.032(5) 0.032(5) 0.021(4) -0.004(4) 0.008(4) -0.010(4) C5 0.030(4) 0.028(4) 0.019(4) -0.012(3) -0.002(3) -0.006(3) C6 0.023(4) 0.025(4) 0.028(4) -0.011(3) 0.008(3) -0.010(3) C7 0.020(4) 0.021(4) 0.014(4) -0.006(4) 0.001(3) 0.000(3) C8 0.034(5) 0.025(4) 0.022(4) -0.010(3) 0.000(3) -0.005(3) C9 0.042(5) 0.028(4) 0.024(4) -0.010(3) -0.007(3) -0.002(4) C10 0.028(4) 0.044(5) 0.019(4) -0.010(3) -0.005(3) -0.009(4) C11 0.030(5) 0.039(5) 0.020(4) -0.018(4) 0.000(4) -0.010(4) C12 0.038(5) 0.016(4) 0.025(5) -0.007(3) 0.001(4) -0.006(4) C13 0.018(4) 0.024(4) 0.027(5) -0.014(3) 0.007(3) -0.006(3) C14 0.022(5) 0.028(5) 0.020(4) -0.010(4) 0.002(3) -0.003(4) C15 0.024(5) 0.034(5) 0.029(5) -0.018(4) 0.011(3) -0.011(4) C16 0.022(5) 0.032(5) 0.029(5) -0.016(4) 0.008(4) -0.004(4) C17 0.022(4) 0.028(4) 0.022(4) -0.008(3) 0.004(3) -0.004(3) C18 0.020(5) 0.022(4) 0.022(4) -0.006(3) 0.004(3) -0.006(3) Pu2 0.0188(3) 0.0171(3) 0.0114(3) -0.0040(2) 0.0002(2) -0.0051(2) Cl2 0.0299(11) 0.0358(11) 0.0392(11) -0.0214(9) 0.0140(8) -0.0101(8) P2 0.0204(13) 0.0176(12) 0.0155(10) -0.0079(9) 0.0034(8) -0.0065(10) O2 0.036(3) 0.026(3) 0.017(3) -0.008(2) -0.001(2) -0.009(2) O4 0.025(4) 0.026(3) 0.014(3) -0.009(2) 0.002(2) -0.004(3) C19 0.024(4) 0.017(4) 0.017(4) -0.007(3) 0.006(3) -0.004(3) C20 0.043(5) 0.031(4) 0.018(4) -0.008(3) -0.003(3) -0.010(4) C21 0.048(5) 0.031(4) 0.022(4) -0.004(3) -0.001(3) -0.022(4) C22 0.047(5) 0.041(5) 0.022(4) -0.012(4) -0.003(4) -0.016(4) C23 0.035(5) 0.034(5) 0.018(4) -0.013(4) -0.007(4) -0.007(4) C24 0.026(4) 0.029(5) 0.019(4) -0.013(4) 0.003(3) -0.010(4) C25 0.014(4) 0.021(4) 0.013(4) -0.006(3) 0.000(3) 0.001(3) C26 0.022(4) 0.025(4) 0.025(4) -0.009(3) 0.005(3) -0.012(3) C27 0.024(5) 0.026(4) 0.030(5) -0.005(4) 0.010(4) -0.010(3) C28 0.031(5) 0.041(5) 0.022(4) -0.012(3) 0.011(3) -0.015(4) C29 0.034(5) 0.030(4) 0.022(4) -0.013(3) 0.014(3) -0.014(4) C30 0.031(5) 0.035(4) 0.017(4) -0.011(3) 0.007(3) -0.009(3) C31 0.016(4) 0.016(4) 0.014(4) -0.007(3) -0.001(3) -0.005(3) C32 0.028(5) 0.027(4) 0.017(4) -0.012(3) 0.004(3) -0.010(4) C33 0.022(5) 0.026(4) 0.025(5) -0.014(4) 0.006(4) -0.005(4) C34 0.018(4) 0.024(4) 0.025(4) -0.008(3) -0.004(3) 0.001(3) C35 0.027(5) 0.032(5) 0.017(4) -0.005(3) -0.003(3) -0.002(4) C36 0.022(5) 0.024(4) 0.024(4) -0.005(4) 0.003(3) -0.005(4) 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pu Pu -9.4100 4.3056 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Pu1 Cl1 180.0 . 2_566 ? O1 Pu1 Cl1 87.93(16) . . ? O1 Pu1 Cl1 87.93(16) 2_566 2_566 ? O1 Pu1 Cl1 92.07(16) . 2_566 ? O1 Pu1 Cl1 92.07(16) 2_566 . ? O1 Pu1 O1 180.0 . 2_566 ? O1 Pu1 O3 90.08(19) . . ? O1 Pu1 O3 89.92(19) . 2_566 ? O1 Pu1 O3 89.91(19) 2_566 . ? O1 Pu1 O3 90.09(19) 2_566 2_566 ? O3 Pu1 Cl1 89.37(12) 2_566 2_566 ? O3 Pu1 Cl1 89.37(12) . . ? O3 Pu1 Cl1 90.63(12) . 2_566 ? O3 Pu1 Cl1 90.63(12) 2_566 . ? O3 Pu1 O3 180.0 2_566 . ? O3 P1 C1 110.4(3) . . ? O3 P1 C7 109.5(3) . . ? O3 P1 C13 109.9(3) . . ? C1 P1 C7 109.1(3) . . ? C13 P1 C1 109.5(3) . . ? C13 P1 C7 108.3(3) . . ? P1 O3 Pu1 167.1(3) . . ? P1 C1 H1 106.0 . . ? C2 C1 P1 115.9(5) . . ? C2 C1 H1 106.0 . . ? C6 C1 P1 111.4(5) . . ? C6 C1 H1 106.0 . . ? C6 C1 C2 110.9(5) . . ? C1 C2 H2A 109.4 . . ? C1 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? C3 C2 C1 111.3(5) . . ? C3 C2 H2A 109.4 . . ? C3 C2 H2B 109.4 . . ? C2 C3 H3A 109.4 . . ? C2 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? C4 C3 C2 111.2(6) . . ? C4 C3 H3A 109.4 . . ? C4 C3 H3B 109.4 . . ? C3 C4 H4A 109.3 . . ? C3 C4 H4B 109.3 . . ? H4A C4 H4B 107.9 . . ? C5 C4 C3 111.7(6) . . ? C5 C4 H4A 109.3 . . ? C5 C4 H4B 109.3 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? C4 C5 C6 110.6(6) . . ? H5A C5 H5B 108.1 . . ? C6 C5 H5A 109.5 . . ? C6 C5 H5B 109.5 . . ? C1 C6 H6A 109.2 . . ? C1 C6 H6B 109.2 . . ? C5 C6 C1 112.1(6) . . ? C5 C6 H6A 109.2 . . ? C5 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? P1 C7 H7 107.0 . . ? C8 C7 P1 111.6(5) . . ? C8 C7 H7 107.0 . . ? C8 C7 C12 109.8(6) . . ? C12 C7 P1 114.1(5) . . ? C12 C7 H7 107.0 . . ? C7 C8 H8A 109.7 . . ? C7 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? C9 C8 C7 109.6(5) . . ? C9 C8 H8A 109.7 . . ? C9 C8 H8B 109.7 . . ? C8 C9 H9A 109.1 . . ? C8 C9 H9B 109.1 . . ? C8 C9 C10 112.3(5) . . ? H9A C9 H9B 107.9 . . ? C10 C9 H9A 109.1 . . ? C10 C9 H9B 109.1 . . ? C9 C10 H10A 109.8 . . ? C9 C10 H10B 109.8 . . ? H10A C10 H10B 108.3 . . ? C11 C10 C9 109.2(6) . . ? C11 C10 H10A 109.8 . . ? C11 C10 H10B 109.8 . . ? C10 C11 H11A 109.4 . . ? C10 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? C12 C11 C10 111.3(6) . . ? C12 C11 H11A 109.4 . . ? C12 C11 H11B 109.4 . . ? C7 C12 H12A 109.4 . . ? C7 C12 H12B 109.4 . . ? C11 C12 C7 111.3(5) . . ? C11 C12 H12A 109.4 . . ? C11 C12 H12B 109.4 . . ? H12A C12 H12B 108.0 . . ? P1 C13 H13 107.8 . . ? C14 C13 P1 112.4(5) . . ? C14 C13 H13 107.8 . . ? C14 C13 C18 108.8(6) . . ? C18 C13 P1 112.1(5) . . ? C18 C13 H13 107.8 . . ? C13 C14 H14A 109.1 . . ? C13 C14 H14B 109.1 . . ? C13 C14 C15 112.6(6) . . ? H14A C14 H14B 107.8 . . ? C15 C14 H14A 109.1 . . ? C15 C14 H14B 109.1 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 108.1 . . ? C16 C15 C14 110.7(6) . . ? C16 C15 H15A 109.5 . . ? C16 C15 H15B 109.5 . . ? C15 C16 H16A 109.3 . . ? C15 C16 H16B 109.3 . . ? C15 C16 C17 111.6(6) . . ? H16A C16 H16B 108.0 . . ? C17 C16 H16A 109.3 . . ? C17 C16 H16B 109.3 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 108.1 . . ? C18 C17 C16 110.8(6) . . ? C18 C17 H17A 109.5 . . ? C18 C17 H17B 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? C17 C18 C13 110.7(6) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 108.1 . . ? Cl2 Pu2 Cl2 180.0 2_667 . ? O2 Pu2 Cl2 89.35(15) 2_667 2_667 ? O2 Pu2 Cl2 89.35(15) . . ? O2 Pu2 Cl2 90.65(15) 2_667 . ? O2 Pu2 Cl2 90.65(15) . 2_667 ? O2 Pu2 O2 180.0(4) 2_667 . ? O2 Pu2 O4 89.80(18) 2_667 2_667 ? O2 Pu2 O4 90.20(18) 2_667 . ? O2 Pu2 O4 89.80(18) . . ? O2 Pu2 O4 90.20(18) . 2_667 ? O4 Pu2 Cl2 91.06(12) 2_667 . ? O4 Pu2 Cl2 91.06(12) . 2_667 ? O4 Pu2 Cl2 88.94(12) . . ? O4 Pu2 Cl2 88.94(12) 2_667 2_667 ? O4 Pu2 O4 180.00(12) . 2_667 ? O4 P2 C19 109.2(3) . . ? O4 P2 C25 108.7(3) . . ? O4 P2 C31 109.4(3) . . ? C19 P2 C25 110.5(4) . . ? C19 P2 C31 111.0(3) . . ? C31 P2 C25 108.1(3) . . ? P2 O4 Pu2 172.2(3) . . ? P2 C19 H19 105.9 . . ? C20 C19 P2 111.8(5) . . ? C20 C19 H19 105.9 . . ? C20 C19 C24 110.5(6) . . ? C24 C19 P2 116.0(5) . . ? C24 C19 H19 105.9 . . ? C19 C20 H20A 109.4 . . ? C19 C20 H20B 109.4 . . ? H20A C20 H20B 108.0 . . ? C21 C20 C19 111.2(6) . . ? C21 C20 H20A 109.4 . . ? C21 C20 H20B 109.4 . . ? C20 C21 H21A 109.6 . . ? C20 C21 H21B 109.6 . . ? C20 C21 C22 110.3(6) . . ? H21A C21 H21B 108.1 . . ? C22 C21 H21A 109.6 . . ? C22 C21 H21B 109.6 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 108.1 . . ? C23 C22 C21 110.7(6) . . ? C23 C22 H22A 109.5 . . ? C23 C22 H22B 109.5 . . ? C22 C23 H23A 109.4 . . ? C22 C23 H23B 109.4 . . ? C22 C23 C24 111.4(6) . . ? H23A C23 H23B 108.0 . . ? C24 C23 H23A 109.4 . . ? C24 C23 H23B 109.4 . . ? C19 C24 H24A 109.2 . . ? C19 C24 H24B 109.2 . . ? C23 C24 C19 112.0(6) . . ? C23 C24 H24A 109.2 . . ? C23 C24 H24B 109.2 . . ? H24A C24 H24B 107.9 . . ? P2 C25 H25 106.1 . . ? C26 C25 P2 113.6(5) . . ? C26 C25 H25 106.1 . . ? C30 C25 P2 112.5(4) . . ? C30 C25 H25 106.1 . . ? C30 C25 C26 111.8(6) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 108.1 . . ? C27 C26 C25 110.6(6) . . ? C27 C26 H26A 109.5 . . ? C27 C26 H26B 109.5 . . ? C26 C27 H27A 109.3 . . ? C26 C27 H27B 109.3 . . ? C26 C27 C28 111.5(6) . . ? H27A C27 H27B 108.0 . . ? C28 C27 H27A 109.3 . . ? C28 C27 H27B 109.3 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 108.1 . . ? C29 C28 C27 110.7(6) . . ? C29 C28 H28A 109.5 . . ? C29 C28 H28B 109.5 . . ? C28 C29 H29A 109.2 . . ? C28 C29 H29B 109.2 . . ? C28 C29 C30 111.9(6) . . ? H29A C29 H29B 107.9 . . ? C30 C29 H29A 109.2 . . ? C30 C29 H29B 109.2 . . ? C25 C30 H30A 109.7 . . ? C25 C30 H30B 109.7 . . ? C29 C30 C25 109.9(5) . . ? C29 C30 H30A 109.7 . . ? C29 C30 H30B 109.7 . . ? H30A C30 H30B 108.2 . . ? P2 C31 H31 108.1 . . ? C32 C31 P2 110.7(5) . . ? C32 C31 H31 108.1 . . ? C32 C31 C36 110.9(6) . . ? C36 C31 P2 110.7(5) . . ? C36 C31 H31 108.1 . . ? C31 C32 H32A 109.2 . . ? C31 C32 H32B 109.2 . . ? H32A C32 H32B 107.9 . . ? C33 C32 C31 111.8(6) . . ? C33 C32 H32A 109.2 . . ? C33 C32 H32B 109.2 . . ? C32 C33 H33A 109.3 . . ? C32 C33 H33B 109.3 . . ? H33A C33 H33B 108.0 . . ? C34 C33 C32 111.6(6) . . ? C34 C33 H33A 109.3 . . ? C34 C33 H33B 109.3 . . ? C33 C34 H34A 109.4 . . ? C33 C34 H34B 109.4 . . ? C33 C34 C35 111.1(6) . . ? H34A C34 H34B 108.0 . . ? C35 C34 H34A 109.4 . . ? C35 C34 H34B 109.4 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 108.1 . . ? C36 C35 C34 110.8(6) . . ? C36 C35 H35A 109.5 . . ? C36 C35 H35B 109.5 . . ? C31 C36 H36A 109.2 . . ? C31 C36 H36B 109.2 . . ? C35 C36 C31 112.2(6) . . ? C35 C36 H36A 109.2 . . ? C35 C36 H36B 109.2 . . ? H36A C36 H36B 107.9 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pu1 Cl1 2.6331(17) 2_566 ? Pu1 Cl1 2.6331(17) . ? Pu1 O1 1.762(4) 2_566 ? Pu1 O1 1.762(4) . ? Pu1 O3 2.301(4) 2_566 ? Pu1 O3 2.301(4) . ? P1 O3 1.510(5) . ? P1 C1 1.818(7) . ? P1 C7 1.821(7) . ? P1 C13 1.810(7) . ? C1 H1 1.0000 . ? C1 C2 1.542(8) . ? C1 C6 1.534(9) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C2 C3 1.527(8) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C3 C4 1.519(9) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C4 C5 1.519(9) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C5 C6 1.527(8) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7 1.0000 . ? C7 C8 1.549(8) . ? C7 C12 1.551(9) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C8 C9 1.525(9) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C9 C10 1.538(9) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C10 C11 1.534(9) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C11 C12 1.521(9) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13 1.0000 . ? C13 C14 1.519(9) . ? C13 C18 1.544(9) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C14 C15 1.526(9) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C15 C16 1.503(10) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C16 C17 1.528(9) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C17 C18 1.506(8) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? Pu2 Cl2 2.6521(17) . ? Pu2 Cl2 2.6521(17) 2_667 ? Pu2 O2 1.742(4) 2_667 ? Pu2 O2 1.742(4) . ? Pu2 O4 2.281(5) 2_667 ? Pu2 O4 2.281(5) . ? P2 O4 1.503(5) . ? P2 C19 1.796(7) . ? P2 C25 1.825(7) . ? P2 C31 1.820(7) . ? C19 H19 1.0000 . ? C19 C20 1.534(8) . ? C19 C24 1.545(9) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C20 C21 1.518(9) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C21 C22 1.545(9) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C22 C23 1.491(9) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C23 C24 1.506(9) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25 1.0000 . ? C25 C26 1.538(9) . ? C25 C30 1.530(8) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C26 C27 1.519(9) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C27 C28 1.522(9) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C28 C29 1.517(9) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C29 C30 1.526(8) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31 1.0000 . ? C31 C32 1.527(9) . ? C31 C36 1.557(9) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C32 C33 1.515(9) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C33 C34 1.505(9) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C34 C35 1.532(9) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C35 C36 1.501(8) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined _oxdiff_twin_reflns_isolated _oxdiff_twin_reflns_overlapped _twin_individual_twin_lattice_type _twin_individual_twin_matrix_11 _twin_individual_twin_matrix_12 _twin_individual_twin_matrix_13 _twin_individual_twin_matrix_21 _twin_individual_twin_matrix_22 _twin_individual_twin_matrix_23 _twin_individual_twin_matrix_31 _twin_individual_twin_matrix_32 _twin_individual_twin_matrix_33 1 0.4846 65162 70953 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 2 0.2800 0 64922 nmt 1.0200 -0.0682 0.0239 0.1537 0.9701 0.0101 -0.0096 0.0011 1.0008 3 0.2354 0 58478 nmt 0.9694 0.0696 -0.0219 0.8696 -0.9623 -0.0263 0.0089 0.0231 -1.0080