#------------------------------------------------------------------------------ #$Date: 2021-10-02 02:04:16 +0300 (Sat, 02 Oct 2021) $ #$Revision: 269445 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/85/7708505.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_7708505 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 H30 Cl2 O4 P2 U' _chemical_formula_sum 'C36 H30 Cl2 O4 P2 U' _chemical_formula_weight 897.47 _chemical_name_common 'uranyldichloride bis(triphenylphosphine oxide)' _chemical_name_systematic 'uraniumdioxodicholoro bis(triphenylphosphine oxide)' _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _atom_sites_solution_hydrogens geom _audit_creation_date 2019-10-18 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2021-08-04 deposited with the CCDC. 2021-10-01 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 117.802(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 10.0387(6) _cell_length_b 18.6540(11) _cell_length_c 10.7043(6) _cell_measurement_reflns_used 9807 _cell_measurement_temperature 170(2) _cell_measurement_theta_max 27.556 _cell_measurement_theta_min 2.293 _cell_volume 1773.12(18) _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 170(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _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 0.0420 _diffrn_reflns_av_unetI/netI 0.0520 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 28492 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.607 _diffrn_reflns_theta_min 2.151 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 4.855 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.4809 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1281 before and 0.0782 after correction. The Ratio of minimum to maximum transmission is 0.6450. The \l/2 correction factor is Not present.' _exptl_crystal_colour 'clear yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.681 _exptl_crystal_description plate _exptl_crystal_F_000 868 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Ethanol' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _refine_diff_density_max 1.791 _refine_diff_density_min -0.694 _refine_diff_density_rms 0.104 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.055(7) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 407 _refine_ls_number_reflns 8125 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.033 _refine_ls_R_factor_all 0.0317 _refine_ls_R_factor_gt 0.0278 _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^)+(0.0238P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0635 _refine_ls_wR_factor_ref 0.0651 _reflns_Friedel_coverage 0.941 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 1.000 _reflns_number_gt 7547 _reflns_number_total 8125 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt03041h2.cif _cod_data_source_block 'save_c' _cod_original_sg_symbol_H-M P21 _cod_database_code 7708505 _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 0.793 _shelx_estimated_absorpt_t_min 0.444 _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.945(7) 0.055(7) 2. Fixed Uiso At 1.2 times of: All C(H) groups 3.a Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36) ; _shelx_res_file ; TITL save_c.res in P2(1) save_c.res created by SHELXL-2016/6 at 18:33:28 on 18-Oct-2019 REM Old TITL save in P2(1) REM SHELXT solution in P2(1) REM R1 0.079, Rweak 0.024, Alpha 0.144, Orientation as input REM Flack x = 0.126 ( 0.005 ) from Parsons' quotients REM Formula found by SHELXT: C34 O11 P3 Cl3 U CELL 0.71073 10.0387 18.654 10.7043 90 117.802 90 ZERR 2 0.0006 0.0011 0.0006 0 0.002 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H O P Cl U UNIT 72 60 8 4 4 2 L.S. 20 PLAN 5 SIZE 0.05 0.1 0.2 TEMP -103(2) BOND $H LIST 6 fmap 2 ACTA TWIN -1 0 0 0 -1 0 0 0 -1 2 REM REM REM WGHT 0.023800 BASF 0.05463 FVAR 0.37165 U1 6 0.617741 0.305090 0.265952 11.00000 0.02369 0.01761 = 0.02430 0.00163 0.00885 0.00223 CL1 5 0.445295 0.260531 0.002662 11.00000 0.04299 0.03807 = 0.02913 -0.00673 0.00774 0.00111 CL2 5 0.798045 0.342013 0.530097 11.00000 0.04051 0.07062 = 0.03027 -0.01653 0.00401 0.01038 P1 4 0.847985 0.138729 0.304133 11.00000 0.02455 0.01869 = 0.02891 -0.00070 0.01316 -0.00008 P2 4 0.338988 0.434489 0.267758 11.00000 0.02645 0.01891 = 0.02664 -0.00105 0.01147 0.00220 O1 3 0.774252 0.208686 0.306836 11.00000 0.02875 0.02643 = 0.03107 0.00021 0.00986 0.00767 O2 3 0.462735 0.400260 0.245105 11.00000 0.03258 0.02336 = 0.02853 0.00112 0.01114 0.00489 O3 3 0.723325 0.357747 0.206776 11.00000 0.03603 0.02230 = 0.04426 0.00266 0.02205 -0.00204 O4 3 0.508906 0.252630 0.322668 11.00000 0.03430 0.03496 = 0.04399 0.00916 0.02462 0.00170 C1 1 0.967874 0.109673 0.479863 11.00000 0.01985 0.03105 = 0.03662 0.01003 0.01172 0.00156 C2 1 1.013069 0.038365 0.511503 11.00000 0.03877 0.03356 = 0.06135 0.01233 0.01662 0.00687 AFIX 43 H2 2 0.977639 0.003231 0.438875 11.00000 -1.20000 AFIX 0 C3 1 1.109231 0.019342 0.648538 11.00000 0.04911 0.06723 = 0.08749 0.05391 0.02496 0.02859 AFIX 43 H3 2 1.138849 -0.029284 0.671078 11.00000 -1.20000 AFIX 0 C4 1 1.163143 0.070889 0.753973 11.00000 0.04270 0.11959 = 0.04570 0.04396 0.01405 0.01700 AFIX 43 H4 2 1.230732 0.057564 0.848294 11.00000 -1.20000 AFIX 0 C5 1 1.119872 0.140159 0.723093 11.00000 0.04433 0.09832 = 0.03340 0.00488 0.00897 -0.00269 AFIX 43 H5 2 1.158789 0.175224 0.795796 11.00000 -1.20000 AFIX 0 C6 1 1.020890 0.160167 0.588567 11.00000 0.03204 0.04499 = 0.03234 0.00421 0.01143 -0.00199 AFIX 43 H6 2 0.988084 0.208548 0.568979 11.00000 -1.20000 AFIX 0 C7 1 0.706997 0.072273 0.214773 11.00000 0.03141 0.02563 = 0.02976 -0.00338 0.01268 -0.00291 C8 1 0.732664 0.012238 0.151112 11.00000 0.07145 0.04167 = 0.06128 -0.02469 0.05348 -0.02495 AFIX 43 H8 2 0.826066 0.006773 0.149752 11.00000 -1.20000 AFIX 0 C9 1 0.620800 -0.039643 0.089571 11.00000 0.09612 0.05105 = 0.05886 -0.02748 0.05814 -0.03643 AFIX 43 H9 2 0.638711 -0.081131 0.048128 11.00000 -1.20000 AFIX 0 C10 1 0.485012 -0.030793 0.088858 11.00000 0.05784 0.04236 = 0.04611 0.00177 0.00524 -0.02551 AFIX 43 H10 2 0.407482 -0.065418 0.044990 11.00000 -1.20000 AFIX 0 C11 1 0.462247 0.027875 0.151375 11.00000 0.03271 0.05449 = 0.08636 -0.00361 0.01767 -0.00795 AFIX 43 H11 2 0.368692 0.033265 0.152464 11.00000 -1.20000 AFIX 0 C12 1 0.570473 0.079548 0.212964 11.00000 0.03022 0.02920 = 0.08041 -0.00220 0.02233 -0.00355 AFIX 43 H12 2 0.550727 0.120496 0.254486 11.00000 -1.20000 AFIX 0 C13 1 0.960488 0.150121 0.216177 11.00000 0.04491 0.02784 = 0.04505 -0.00388 0.03504 -0.00830 C14 1 0.891546 0.165039 0.073594 11.00000 0.07916 0.04142 = 0.04969 0.00174 0.04171 -0.01108 AFIX 43 H14 2 0.784785 0.164773 0.021194 11.00000 -1.20000 AFIX 0 C15 1 0.978079 0.180541 0.005899 11.00000 0.12589 0.05652 = 0.07039 0.00211 0.07568 -0.01477 AFIX 43 H15 2 0.930590 0.190042 -0.092657 11.00000 -1.20000 AFIX 0 C16 1 1.134923 0.181981 0.084092 11.00000 0.10985 0.05482 = 0.10785 -0.02675 0.09535 -0.04107 AFIX 43 H16 2 1.194675 0.193485 0.039394 11.00000 -1.20000 AFIX 0 C17 1 1.200250 0.167146 0.221599 11.00000 0.06264 0.06719 = 0.10504 -0.03651 0.06344 -0.03057 AFIX 43 H17 2 1.307074 0.167824 0.273022 11.00000 -1.20000 AFIX 0 C18 1 1.117721 0.150486 0.294106 11.00000 0.04147 0.04560 = 0.05746 -0.01619 0.03500 -0.01329 AFIX 43 H18 2 1.166966 0.139895 0.392243 11.00000 -1.20000 AFIX 0 C19 1 0.308096 0.390854 0.401462 11.00000 0.04034 0.01995 = 0.02702 -0.00009 0.01554 0.00034 C20 1 0.166245 0.370522 0.377144 11.00000 0.03996 0.05539 = 0.04442 0.01382 0.02138 -0.00237 AFIX 43 H20 2 0.082241 0.378269 0.287126 11.00000 -1.20000 AFIX 0 C21 1 0.145982 0.338559 0.484711 11.00000 0.06055 0.07504 = 0.05908 0.01721 0.03624 -0.00046 AFIX 43 H21 2 0.048202 0.324095 0.467661 11.00000 -1.20000 AFIX 0 C22 1 0.264131 0.328168 0.612204 11.00000 0.08200 0.05006 = 0.05364 0.01123 0.04557 0.00622 AFIX 43 H22 2 0.249158 0.307170 0.685549 11.00000 -1.20000 AFIX 0 C23 1 0.406795 0.347604 0.637872 11.00000 0.07217 0.04145 = 0.02799 0.00162 0.02104 0.01021 AFIX 43 H23 2 0.489944 0.339825 0.728416 11.00000 -1.20000 AFIX 0 C24 1 0.429114 0.378741 0.530743 11.00000 0.04700 0.03532 = 0.03064 0.00017 0.01791 0.00166 AFIX 43 H24 2 0.527646 0.391473 0.547327 11.00000 -1.20000 AFIX 0 C25 1 0.384561 0.526550 0.317913 11.00000 0.02941 0.02223 = 0.03030 -0.00479 0.01351 -0.00292 C26 1 0.472381 0.562909 0.269799 11.00000 0.05092 0.03336 = 0.06288 -0.01286 0.04016 -0.00736 AFIX 43 H26 2 0.511858 0.538723 0.216162 11.00000 -1.20000 AFIX 0 C27 1 0.501537 0.635152 0.301347 11.00000 0.07486 0.03834 = 0.08141 -0.00902 0.05517 -0.01783 AFIX 43 H27 2 0.564376 0.660361 0.272008 11.00000 -1.20000 AFIX 0 C28 1 0.440379 0.670179 0.374327 11.00000 0.07000 0.02518 = 0.07602 -0.01294 0.04525 -0.01565 AFIX 43 H28 2 0.459239 0.719924 0.393380 11.00000 -1.20000 AFIX 0 C29 1 0.352529 0.634787 0.420331 11.00000 0.05820 0.02905 = 0.05955 -0.01663 0.03872 -0.00763 AFIX 43 H29 2 0.310831 0.659660 0.471381 11.00000 -1.20000 AFIX 0 C30 1 0.324602 0.562365 0.392070 11.00000 0.04502 0.03114 = 0.04985 -0.01486 0.02985 -0.01049 AFIX 43 H30 2 0.263782 0.537382 0.424077 11.00000 -1.20000 AFIX 0 C31 1 0.164846 0.433028 0.108140 11.00000 0.02581 0.02541 = 0.02646 -0.00404 0.00736 -0.00103 C32 1 0.133116 0.373441 0.020951 11.00000 0.04262 0.03640 = 0.03897 -0.01231 -0.00163 0.01197 AFIX 43 H32 2 0.201683 0.334384 0.048063 11.00000 -1.20000 AFIX 0 C33 1 0.001785 0.371215 -0.105022 11.00000 0.05591 0.05491 = 0.05122 -0.02524 -0.00152 0.00461 AFIX 43 H33 2 -0.020215 0.330548 -0.164854 11.00000 -1.20000 AFIX 0 C34 1 -0.097393 0.427723 -0.144222 11.00000 0.04076 0.06440 = 0.03680 -0.00187 -0.00053 0.01398 AFIX 43 H34 2 -0.189798 0.425126 -0.229137 11.00000 -1.20000 AFIX 0 C35 1 -0.063883 0.487138 -0.062210 11.00000 0.03284 0.04941 = 0.05268 0.00769 0.01542 0.01306 AFIX 43 H35 2 -0.130700 0.526909 -0.092110 11.00000 -1.20000 AFIX 0 C36 1 0.067322 0.490165 0.065010 11.00000 0.03262 0.03142 = 0.04175 -0.00235 0.01600 0.00593 AFIX 43 H36 2 0.089844 0.531794 0.122450 11.00000 -1.20000 AFIX 0 HKLF 4 REM save_c.res in P2(1) REM R1 = 0.0278 for 7547 Fo > 4sig(Fo) and 0.0317 for all 8125 data REM 407 parameters refined using 1 restraints END WGHT 0.0225 0.0000 REM Highest difference peak 1.791, deepest hole -0.694, 1-sigma level 0.104 Q1 1 0.7050 0.3070 0.3363 11.00000 0.05 1.79 Q2 1 0.5195 0.3063 0.2042 11.00000 0.05 1.57 Q3 1 0.5607 0.3064 0.2982 11.00000 0.05 1.52 Q4 1 0.6449 0.2691 0.3164 11.00000 0.05 0.76 Q5 1 0.4446 0.3059 0.2579 11.00000 0.05 0.74 ; _shelx_res_checksum 17983 _olex2_exptl_crystal_mounting_method 'nylon loop' _olex2_submission_original_sample_id cjw95 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -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 U1 U 0.61774(2) 0.30509(2) 0.26595(2) 0.02280(7) Uani 1 1 d . . . . . Cl1 Cl 0.4453(2) 0.26053(10) 0.00266(18) 0.0403(4) Uani 1 1 d . . . . . Cl2 Cl 0.7980(2) 0.34201(13) 0.5301(2) 0.0521(5) Uani 1 1 d . . . . . P1 P 0.84798(18) 0.13873(9) 0.30413(18) 0.0238(3) Uani 1 1 d . . . . . P2 P 0.33899(18) 0.43449(9) 0.26776(17) 0.0244(3) Uani 1 1 d . . . . . O1 O 0.7743(5) 0.2087(3) 0.3068(5) 0.0304(10) Uani 1 1 d . . . . . O2 O 0.4627(5) 0.4003(2) 0.2451(5) 0.0294(10) Uani 1 1 d . . . . . O3 O 0.7233(5) 0.3577(3) 0.2068(5) 0.0329(11) Uani 1 1 d . . . . . O4 O 0.5089(5) 0.2526(3) 0.3227(5) 0.0352(11) Uani 1 1 d . . . . . C1 C 0.9679(7) 0.1097(4) 0.4799(8) 0.0297(16) Uani 1 1 d . . . . . C2 C 1.0131(10) 0.0384(4) 0.5115(10) 0.047(2) Uani 1 1 d . . . . . H2 H 0.977639 0.003231 0.438875 0.057 Uiso 1 1 calc R . . . . C3 C 1.1092(11) 0.0193(6) 0.6485(13) 0.071(3) Uani 1 1 d . . . . . H3 H 1.138849 -0.029284 0.671078 0.085 Uiso 1 1 calc R . . . . C4 C 1.1631(11) 0.0709(8) 0.7540(11) 0.072(4) Uani 1 1 d . . . . . H4 H 1.230732 0.057564 0.848294 0.086 Uiso 1 1 calc R . . . . C5 C 1.1199(10) 0.1402(7) 0.7231(10) 0.062(3) Uani 1 1 d . . . . . H5 H 1.158789 0.175224 0.795796 0.075 Uiso 1 1 calc R . . . . C6 C 1.0209(8) 0.1602(4) 0.5886(8) 0.0379(17) Uani 1 1 d . . . . . H6 H 0.988084 0.208548 0.568979 0.045 Uiso 1 1 calc R . . . . C7 C 0.7070(8) 0.0723(4) 0.2148(7) 0.0296(14) Uani 1 1 d . . . . . C8 C 0.7327(10) 0.0122(5) 0.1511(9) 0.049(2) Uani 1 1 d . . . . . H8 H 0.826066 0.006773 0.149752 0.059 Uiso 1 1 calc R . . . . C9 C 0.6208(12) -0.0396(5) 0.0896(10) 0.060(3) Uani 1 1 d . . . . . H9 H 0.638711 -0.081131 0.048128 0.072 Uiso 1 1 calc R . . . . C10 C 0.4850(10) -0.0308(5) 0.0889(9) 0.056(2) Uani 1 1 d . . . . . H10 H 0.407482 -0.065418 0.044990 0.068 Uiso 1 1 calc R . . . . C11 C 0.4622(10) 0.0279(5) 0.1514(11) 0.062(3) Uani 1 1 d . . . . . H11 H 0.368692 0.033265 0.152464 0.074 Uiso 1 1 calc R . . . . C12 C 0.5705(9) 0.0795(4) 0.2130(11) 0.048(2) Uani 1 1 d . . . . . H12 H 0.550727 0.120496 0.254486 0.058 Uiso 1 1 calc R . . . . C13 C 0.9605(9) 0.1501(4) 0.2162(8) 0.0337(16) Uani 1 1 d . . . . . C14 C 0.8915(12) 0.1650(5) 0.0736(10) 0.052(2) Uani 1 1 d . . . . . H14 H 0.784785 0.164773 0.021194 0.063 Uiso 1 1 calc R . . . . C15 C 0.9781(16) 0.1805(6) 0.0059(12) 0.072(3) Uani 1 1 d . . . . . H15 H 0.930590 0.190042 -0.092657 0.087 Uiso 1 1 calc R . . . . C16 C 1.1349(16) 0.1820(6) 0.0841(15) 0.073(4) Uani 1 1 d . . . . . H16 H 1.194675 0.193485 0.039394 0.088 Uiso 1 1 calc R . . . . C17 C 1.2003(12) 0.1671(6) 0.2216(14) 0.069(3) Uani 1 1 d . . . . . H17 H 1.307074 0.167824 0.273022 0.082 Uiso 1 1 calc R . . . . C18 C 1.1177(8) 0.1505(5) 0.2941(9) 0.043(2) Uani 1 1 d . . . . . H18 H 1.166966 0.139895 0.392243 0.052 Uiso 1 1 calc R . . . . C19 C 0.3081(8) 0.3909(4) 0.4015(7) 0.0292(14) Uani 1 1 d . . . . . C20 C 0.1662(9) 0.3705(5) 0.3771(9) 0.046(2) Uani 1 1 d . . . . . H20 H 0.082241 0.378269 0.287126 0.055 Uiso 1 1 calc R . . . . C21 C 0.1460(11) 0.3386(6) 0.4847(10) 0.062(3) Uani 1 1 d . . . . . H21 H 0.048202 0.324095 0.467661 0.074 Uiso 1 1 calc R . . . . C22 C 0.2641(11) 0.3282(5) 0.6122(10) 0.056(2) Uani 1 1 d . . . . . H22 H 0.249158 0.307170 0.685549 0.068 Uiso 1 1 calc R . . . . C23 C 0.4068(11) 0.3476(4) 0.6379(8) 0.048(2) Uani 1 1 d . . . . . H23 H 0.489944 0.339825 0.728416 0.058 Uiso 1 1 calc R . . . . C24 C 0.4291(9) 0.3787(4) 0.5307(8) 0.0377(17) Uani 1 1 d . . . . . H24 H 0.527646 0.391473 0.547327 0.045 Uiso 1 1 calc R . . . . C25 C 0.3846(7) 0.5266(4) 0.3179(7) 0.0275(14) Uani 1 1 d . . . . . C26 C 0.4724(9) 0.5629(4) 0.2698(9) 0.0436(19) Uani 1 1 d . . . . . H26 H 0.511858 0.538723 0.216162 0.052 Uiso 1 1 calc R . . . . C27 C 0.5015(11) 0.6352(5) 0.3013(11) 0.057(2) Uani 1 1 d . . . . . H27 H 0.564376 0.660361 0.272008 0.069 Uiso 1 1 calc R . . . . C28 C 0.4404(10) 0.6702(4) 0.3743(10) 0.053(2) Uani 1 1 d . . . . . H28 H 0.459239 0.719924 0.393380 0.063 Uiso 1 1 calc R . . . . C29 C 0.3525(10) 0.6348(4) 0.4203(9) 0.0445(19) Uani 1 1 d . . . . . H29 H 0.310831 0.659660 0.471381 0.053 Uiso 1 1 calc R . . . . C30 C 0.3246(9) 0.5624(4) 0.3921(9) 0.0389(17) Uani 1 1 d . . . . . H30 H 0.263782 0.537382 0.424077 0.047 Uiso 1 1 calc R . . . . C31 C 0.1648(8) 0.4330(4) 0.1081(8) 0.0278(17) Uani 1 1 d . . . . . C32 C 0.1331(9) 0.3734(4) 0.0210(8) 0.048(2) Uani 1 1 d . . . . . H32 H 0.201683 0.334384 0.048063 0.057 Uiso 1 1 calc R . . . . C33 C 0.0018(11) 0.3712(6) -0.1050(10) 0.065(3) Uani 1 1 d . . . . . H33 H -0.020215 0.330548 -0.164854 0.077 Uiso 1 1 calc R . . . . C34 C -0.0974(9) 0.4277(5) -0.1442(9) 0.055(2) Uani 1 1 d . . . . . H34 H -0.189798 0.425126 -0.229137 0.066 Uiso 1 1 calc R . . . . C35 C -0.0639(9) 0.4871(5) -0.0622(9) 0.047(2) Uani 1 1 d . . . . . H35 H -0.130700 0.526909 -0.092110 0.056 Uiso 1 1 calc R . . . . C36 C 0.0673(8) 0.4902(4) 0.0650(8) 0.0358(16) Uani 1 1 d . . . . . H36 H 0.089844 0.531794 0.122450 0.043 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 U1 0.02369(10) 0.01761(10) 0.02430(11) 0.00163(13) 0.00885(8) 0.00223(13) Cl1 0.0430(10) 0.0381(10) 0.0291(9) -0.0067(7) 0.0077(8) 0.0011(8) Cl2 0.0405(10) 0.0706(14) 0.0303(9) -0.0165(9) 0.0040(8) 0.0104(9) P1 0.0246(8) 0.0187(8) 0.0289(9) -0.0007(7) 0.0132(7) -0.0001(7) P2 0.0264(8) 0.0189(8) 0.0266(9) -0.0011(6) 0.0115(7) 0.0022(6) O1 0.029(2) 0.026(3) 0.031(3) 0.000(2) 0.010(2) 0.008(2) O2 0.033(3) 0.023(2) 0.029(3) 0.0011(19) 0.011(2) 0.005(2) O3 0.036(3) 0.022(2) 0.044(3) 0.003(2) 0.022(2) -0.002(2) O4 0.034(3) 0.035(3) 0.044(3) 0.009(2) 0.025(2) 0.002(2) C1 0.020(3) 0.031(4) 0.037(4) 0.010(3) 0.012(3) 0.002(3) C2 0.039(4) 0.034(6) 0.061(6) 0.012(5) 0.017(4) 0.007(5) C3 0.049(5) 0.067(7) 0.087(8) 0.054(7) 0.025(6) 0.029(5) C4 0.043(5) 0.120(11) 0.046(6) 0.044(7) 0.014(5) 0.017(6) C5 0.044(5) 0.098(9) 0.033(5) 0.005(5) 0.009(4) -0.003(5) C6 0.032(4) 0.045(5) 0.032(4) 0.004(3) 0.011(3) -0.002(3) C7 0.031(3) 0.026(3) 0.030(4) -0.003(3) 0.013(3) -0.003(3) C8 0.071(6) 0.042(5) 0.061(5) -0.025(4) 0.053(5) -0.025(4) C9 0.096(7) 0.051(6) 0.059(6) -0.027(4) 0.058(6) -0.036(5) C10 0.058(5) 0.042(5) 0.046(5) 0.002(4) 0.005(4) -0.026(4) C11 0.033(4) 0.054(6) 0.086(7) -0.004(5) 0.018(5) -0.008(4) C12 0.030(4) 0.029(4) 0.080(6) -0.002(4) 0.022(4) -0.004(3) C13 0.045(4) 0.028(4) 0.045(4) -0.004(3) 0.035(4) -0.008(3) C14 0.079(6) 0.041(5) 0.050(5) 0.002(4) 0.042(5) -0.011(4) C15 0.126(10) 0.057(6) 0.070(7) 0.002(5) 0.076(7) -0.015(6) C16 0.110(10) 0.055(7) 0.108(10) -0.027(7) 0.095(9) -0.041(7) C17 0.063(6) 0.067(7) 0.105(9) -0.037(6) 0.063(7) -0.031(5) C18 0.041(4) 0.046(5) 0.057(5) -0.016(4) 0.035(4) -0.013(3) C19 0.040(4) 0.020(3) 0.027(3) 0.000(3) 0.016(3) 0.000(3) C20 0.040(4) 0.055(5) 0.044(5) 0.014(4) 0.021(4) -0.002(4) C21 0.061(6) 0.075(7) 0.059(6) 0.017(5) 0.036(5) 0.000(5) C22 0.082(7) 0.050(6) 0.054(5) 0.011(4) 0.046(5) 0.006(4) C23 0.072(6) 0.041(5) 0.028(4) 0.002(3) 0.021(4) 0.010(4) C24 0.047(4) 0.035(4) 0.031(4) 0.000(3) 0.018(3) 0.002(3) C25 0.029(3) 0.022(3) 0.030(4) -0.005(3) 0.014(3) -0.003(3) C26 0.051(5) 0.033(4) 0.063(5) -0.013(4) 0.040(4) -0.007(4) C27 0.075(6) 0.038(5) 0.081(7) -0.009(4) 0.055(6) -0.018(5) C28 0.070(6) 0.025(4) 0.076(6) -0.013(4) 0.045(5) -0.016(4) C29 0.058(5) 0.029(4) 0.060(5) -0.017(4) 0.039(4) -0.008(4) C30 0.045(4) 0.031(4) 0.050(5) -0.015(3) 0.030(4) -0.010(3) C31 0.026(3) 0.025(4) 0.026(4) -0.004(3) 0.007(3) -0.001(3) C32 0.043(4) 0.036(4) 0.039(4) -0.012(3) -0.002(3) 0.012(3) C33 0.056(5) 0.055(6) 0.051(6) -0.025(5) -0.002(4) 0.005(5) C34 0.041(4) 0.064(6) 0.037(5) -0.002(4) -0.001(4) 0.014(4) C35 0.033(4) 0.049(5) 0.053(5) 0.008(4) 0.015(4) 0.013(4) C36 0.033(4) 0.031(4) 0.042(4) -0.002(3) 0.016(3) 0.006(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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 '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 Cl2 U1 Cl1 176.55(7) . . ? O1 U1 Cl1 90.37(12) . . ? O1 U1 Cl2 86.20(12) . . ? O1 U1 O2 174.79(17) . . ? O2 U1 Cl1 93.54(12) . . ? O2 U1 Cl2 89.85(12) . . ? O3 U1 Cl1 89.81(17) . . ? O3 U1 Cl2 90.73(17) . . ? O3 U1 O1 91.8(2) . . ? O3 U1 O2 91.6(2) . . ? O3 U1 O4 179.0(2) . . ? O4 U1 Cl1 89.42(18) . . ? O4 U1 Cl2 90.08(18) . . ? O4 U1 O1 88.8(2) . . ? O4 U1 O2 87.8(2) . . ? O1 P1 C1 109.8(3) . . ? O1 P1 C7 109.7(3) . . ? O1 P1 C13 110.1(3) . . ? C1 P1 C7 109.3(3) . . ? C1 P1 C13 108.1(4) . . ? C7 P1 C13 109.7(3) . . ? O2 P2 C19 113.4(3) . . ? O2 P2 C25 109.8(3) . . ? O2 P2 C31 110.5(3) . . ? C25 P2 C19 108.1(3) . . ? C31 P2 C19 107.4(4) . . ? C31 P2 C25 107.5(3) . . ? P1 O1 U1 167.1(3) . . ? P2 O2 U1 151.4(3) . . ? C2 C1 P1 122.0(6) . . ? C6 C1 P1 118.9(6) . . ? C6 C1 C2 119.1(7) . . ? C1 C2 H2 120.3 . . ? C3 C2 C1 119.5(9) . . ? C3 C2 H2 120.3 . . ? C2 C3 H3 119.9 . . ? C2 C3 C4 120.2(10) . . ? C4 C3 H3 119.9 . . ? C3 C4 H4 119.9 . . ? C5 C4 C3 120.3(9) . . ? C5 C4 H4 119.9 . . ? C4 C5 H5 119.6 . . ? C4 C5 C6 120.7(11) . . ? C6 C5 H5 119.6 . . ? C1 C6 H6 119.9 . . ? C5 C6 C1 120.1(9) . . ? C5 C6 H6 119.9 . . ? C8 C7 P1 122.5(6) . . ? C12 C7 P1 118.5(6) . . ? C12 C7 C8 119.0(7) . . ? C7 C8 H8 120.1 . . ? C9 C8 C7 119.8(8) . . ? C9 C8 H8 120.1 . . ? C8 C9 H9 120.0 . . ? C10 C9 C8 120.0(9) . . ? C10 C9 H9 120.0 . . ? C9 C10 H10 120.3 . . ? C11 C10 C9 119.4(8) . . ? C11 C10 H10 120.3 . . ? C10 C11 H11 119.1 . . ? C10 C11 C12 121.8(9) . . ? C12 C11 H11 119.1 . . ? C7 C12 C11 120.1(9) . . ? C7 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C14 C13 P1 119.5(6) . . ? C14 C13 C18 120.2(7) . . ? C18 C13 P1 120.0(6) . . ? C13 C14 H14 119.9 . . ? C13 C14 C15 120.2(10) . . ? C15 C14 H14 119.9 . . ? C14 C15 H15 120.2 . . ? C16 C15 C14 119.5(11) . . ? C16 C15 H15 120.2 . . ? C15 C16 H16 120.2 . . ? C17 C16 C15 119.7(9) . . ? C17 C16 H16 120.2 . . ? C16 C17 H17 118.6 . . ? C16 C17 C18 122.8(10) . . ? C18 C17 H17 118.6 . . ? C13 C18 C17 117.5(9) . . ? C13 C18 H18 121.2 . . ? C17 C18 H18 121.2 . . ? C20 C19 P2 121.5(6) . . ? C24 C19 P2 118.6(6) . . ? C24 C19 C20 119.9(7) . . ? C19 C20 H20 120.0 . . ? C19 C20 C21 119.9(8) . . ? C21 C20 H20 120.0 . . ? C20 C21 H21 119.9 . . ? C22 C21 C20 120.2(9) . . ? C22 C21 H21 119.9 . . ? C21 C22 H22 119.7 . . ? C21 C22 C23 120.7(8) . . ? C23 C22 H22 119.7 . . ? C22 C23 H23 120.1 . . ? C22 C23 C24 119.8(8) . . ? C24 C23 H23 120.1 . . ? C19 C24 C23 119.5(8) . . ? C19 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? C26 C25 P2 118.3(5) . . ? C30 C25 P2 121.3(5) . . ? C30 C25 C26 120.2(6) . . ? C25 C26 H26 120.6 . . ? C27 C26 C25 118.9(7) . . ? C27 C26 H26 120.6 . . ? C26 C27 H27 119.9 . . ? C28 C27 C26 120.3(8) . . ? C28 C27 H27 119.9 . . ? C27 C28 H28 119.5 . . ? C27 C28 C29 120.9(8) . . ? C29 C28 H28 119.5 . . ? C28 C29 H29 120.2 . . ? C28 C29 C30 119.5(7) . . ? C30 C29 H29 120.2 . . ? C25 C30 C29 120.2(7) . . ? C25 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C32 C31 P2 118.0(6) . . ? C36 C31 P2 122.4(6) . . ? C36 C31 C32 119.4(7) . . ? C31 C32 H32 120.1 . . ? C33 C32 C31 119.8(8) . . ? C33 C32 H32 120.1 . . ? C32 C33 H33 119.9 . . ? C34 C33 C32 120.1(8) . . ? C34 C33 H33 119.9 . . ? C33 C34 H34 119.9 . . ? C35 C34 C33 120.3(8) . . ? C35 C34 H34 119.9 . . ? C34 C35 H35 119.8 . . ? C34 C35 C36 120.3(8) . . ? C36 C35 H35 119.8 . . ? C31 C36 C35 120.0(7) . . ? C31 C36 H36 120.0 . . ? C35 C36 H36 120.0 . . ? 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 U1 Cl1 2.6607(17) . ? U1 Cl2 2.6403(18) . ? U1 O1 2.292(5) . ? U1 O2 2.302(5) . ? U1 O3 1.765(5) . ? U1 O4 1.772(5) . ? P1 O1 1.507(5) . ? P1 C1 1.780(7) . ? P1 C7 1.787(7) . ? P1 C13 1.789(7) . ? P2 O2 1.513(5) . ? P2 C19 1.795(7) . ? P2 C25 1.794(7) . ? P2 C31 1.786(7) . ? C1 C2 1.395(12) . ? C1 C6 1.395(11) . ? C2 H2 0.9500 . ? C2 C3 1.374(13) . ? C3 H3 0.9500 . ? C3 C4 1.386(17) . ? C4 H4 0.9500 . ? C4 C5 1.354(17) . ? C5 H5 0.9500 . ? C5 C6 1.366(11) . ? C6 H6 0.9500 . ? C7 C8 1.396(10) . ? C7 C12 1.368(10) . ? C8 H8 0.9500 . ? C8 C9 1.393(11) . ? C9 H9 0.9500 . ? C9 C10 1.370(13) . ? C10 H10 0.9500 . ? C10 C11 1.357(14) . ? C11 H11 0.9500 . ? C11 C12 1.370(12) . ? C12 H12 0.9500 . ? C13 C14 1.379(11) . ? C13 C18 1.400(10) . ? C14 H14 0.9500 . ? C14 C15 1.397(13) . ? C15 H15 0.9500 . ? C15 C16 1.397(18) . ? C16 H16 0.9500 . ? C16 C17 1.331(17) . ? C17 H17 0.9500 . ? C17 C18 1.409(11) . ? C18 H18 0.9500 . ? C19 C20 1.376(10) . ? C19 C24 1.369(10) . ? C20 H20 0.9500 . ? C20 C21 1.393(11) . ? C21 H21 0.9500 . ? C21 C22 1.340(13) . ? C22 H22 0.9500 . ? C22 C23 1.375(12) . ? C23 H23 0.9500 . ? C23 C24 1.394(11) . ? C24 H24 0.9500 . ? C25 C26 1.388(10) . ? C25 C30 1.373(10) . ? C26 H26 0.9500 . ? C26 C27 1.387(11) . ? C27 H27 0.9500 . ? C27 C28 1.364(12) . ? C28 H28 0.9500 . ? C28 C29 1.364(11) . ? C29 H29 0.9500 . ? C29 C30 1.384(10) . ? C30 H30 0.9500 . ? C31 C32 1.389(10) . ? C31 C36 1.373(10) . ? C32 H32 0.9500 . ? C32 C33 1.378(11) . ? C33 H33 0.9500 . ? C33 C34 1.374(12) . ? C34 H34 0.9500 . ? C34 C35 1.355(12) . ? C35 H35 0.9500 . ? C35 C36 1.385(10) . ? C36 H36 0.9500 . ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.945(7) 2 0.055(7)