#------------------------------------------------------------------------------ #$Date: 2021-10-02 02:04:16 +0300 (Sat, 02 Oct 2021) $ #$Revision: 269445 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/85/7708504.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_7708504 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 U' _chemical_formula_sum 'C36 H66 Cl2 O4 P2 U' _chemical_formula_weight 933.75 _chemical_name_common 'uranyldichloride bis(tricyclyhexylphosphine oxide)' _chemical_name_systematic 'uraniumdioxodicholoro 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 69.441(3) _cell_angle_beta 89.371(2) _cell_angle_gamma 77.147(2) _cell_formula_units_Z 2 _cell_length_a 8.7605(2) _cell_length_b 14.1151(4) _cell_length_c 17.1633(5) _cell_measurement_reflns_used 20552 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 32.5090 _cell_measurement_theta_min 2.4520 _cell_volume 1932.13(10) _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 (Sheldrick, 2015)' _diffrn_ambient_temperature 120(2) _diffrn_detector CMOS _diffrn_detector_area_resol_mean 7.9 _diffrn_detector_type 'CMOS detector' _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -25.00 129.70 1.30 10.00 -- -10.78 73.71 -25.73 119 2 \w -25.00 129.70 1.30 10.00 -- -10.78 73.71 118.28 119 3 \w -25.00 129.70 1.30 10.00 -- -10.78 73.71 -97.73 119 4 \w -25.00 129.70 1.30 10.00 -- -10.78 73.71 46.27 119 5 \w -25.00 129.70 1.30 10.00 -- -10.78 73.71-169.72 119 6 \f -25.73 333.08 1.30 10.00 -25.00 -10.78 73.71 -- 276 7 \f -25.73 242.08 1.30 10.00 132.00 -10.78 73.71 -- 206 ; _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 -0.0036166000 _diffrn_orient_matrix_UB_12 -0.0117314000 _diffrn_orient_matrix_UB_13 -0.0367799000 _diffrn_orient_matrix_UB_21 -0.0185538000 _diffrn_orient_matrix_UB_22 0.0539147000 _diffrn_orient_matrix_UB_23 -0.0243118000 _diffrn_orient_matrix_UB_31 0.0810980000 _diffrn_orient_matrix_UB_32 -0.0014202000 _diffrn_orient_matrix_UB_33 -0.0038602000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0497 _diffrn_reflns_av_unetI/netI 0.0684 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 9 _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 35033 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.680 _diffrn_reflns_theta_min 1.639 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 4.457 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.48320 _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 yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.605 _exptl_crystal_description plank _exptl_crystal_F_000 940 _exptl_crystal_preparation 'By CJW.' _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Ethanol' _exptl_crystal_size_max 0.402 _exptl_crystal_size_mid 0.185 _exptl_crystal_size_min 0.156 _refine_diff_density_max 1.081 _refine_diff_density_min -0.953 _refine_diff_density_rms 0.133 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.911 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 409 _refine_ls_number_reflns 7307 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 0.910 _refine_ls_R_factor_all 0.0475 _refine_ls_R_factor_gt 0.0270 _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^)] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0471 _refine_ls_wR_factor_ref 0.0549 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5257 _reflns_number_total 7307 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt03041h2.cif _cod_data_source_block cjw92 _cod_database_code 7708504 _lanl_internal_la-ur LA-UR-19-30804 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula UO2Cl2(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 0.543 _shelx_estimated_absorpt_t_min 0.267 _reflns_odcompleteness_completeness 99.41 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups 2. Uiso/Uaniso restraints and constraints Uanis(C9) \\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.016 3.a Ternary CH refined with riding coordinates: C1(H1), C7(H7), C13(H13), C19(H19), C25(H25), C31(H31) 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) ; _shelx_res_file ; TITL cjw92_a.res in P-1 cjw92.res created by SHELXL-2018/3 at 13:33:52 on 25-Oct-2019 REM Old TITL cjw92 in P-1 REM SHELXT solution in P-1: R1 0.136, Rweak 0.002, Alpha 0.030 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C36 O4 P2 Cl2 U CELL 0.71073 8.7605 14.1151 17.1633 69.441 89.371 77.147 ZERR 2 0.0002 0.0004 0.0005 0.003 0.002 0.002 LATT 1 SFAC C H Cl O P U UNIT 72 132 4 8 4 2 ISOR 0.008 0.016 C9 L.S. 20 PLAN 20 SIZE 0.402 0.185 0.156 TEMP -153(2) BOND list 4 BOND $H fmap 2 53 acta SHEL 999 0.82 OMIT 3 16 13 OMIT 4 1 16 REM REM REM WGHT 0.000000 FVAR 1.23843 U1 6 0.500000 0.500000 1.000000 10.50000 0.01176 0.01185 = 0.01310 -0.00302 0.00051 -0.00382 CL1 3 0.241819 0.646818 0.930318 11.00000 0.01634 0.02058 = 0.03072 -0.00356 -0.00352 -0.00076 P1 5 0.700891 0.715324 0.991681 11.00000 0.01232 0.01018 = 0.01873 -0.00451 0.00308 -0.00409 O1 4 0.442847 0.502966 1.097875 11.00000 0.02236 0.02145 = 0.01800 -0.00625 0.00466 -0.00676 O3 4 0.636418 0.625359 0.988178 11.00000 0.01556 0.01180 = 0.01999 -0.00489 0.00044 -0.00411 C1 1 0.537700 0.824704 0.983909 11.00000 0.01387 0.01264 = 0.02205 -0.00813 0.00287 -0.00636 AFIX 13 H1 2 0.582423 0.882368 0.987712 11.00000 -1.20000 AFIX 0 C2 1 0.430696 0.796134 1.055880 11.00000 0.01700 0.02601 = 0.01962 -0.01208 0.00820 -0.00675 AFIX 23 H2A 2 0.387678 0.737471 1.054586 11.00000 -1.20000 H2B 2 0.493035 0.773289 1.109738 11.00000 -1.20000 AFIX 0 C3 1 0.295247 0.888970 1.049401 11.00000 0.01833 0.03125 = 0.02835 -0.01633 0.00538 -0.00607 AFIX 23 H3A 2 0.224342 0.866897 1.094138 11.00000 -1.20000 H3B 2 0.337850 0.944338 1.057742 11.00000 -1.20000 AFIX 0 C4 1 0.202538 0.932186 0.965354 11.00000 0.01831 0.02291 = 0.03135 -0.01103 0.00446 -0.00246 AFIX 23 H4A 2 0.147989 0.880094 0.960173 11.00000 -1.20000 H4B 2 0.121897 0.995383 0.961706 11.00000 -1.20000 AFIX 0 C5 1 0.308334 0.959056 0.894358 11.00000 0.01563 0.01836 = 0.02667 -0.00331 0.00210 -0.00367 AFIX 23 H5A 2 0.354199 1.016428 0.896094 11.00000 -1.20000 H5B 2 0.245293 0.983468 0.840534 11.00000 -1.20000 AFIX 0 C6 1 0.440315 0.865374 0.899722 11.00000 0.01072 0.02061 = 0.01667 -0.00466 0.00633 -0.00693 AFIX 23 H6A 2 0.508996 0.885734 0.853508 11.00000 -1.20000 H6B 2 0.395191 0.809547 0.894042 11.00000 -1.20000 AFIX 0 C7 1 0.813841 0.675833 1.090428 11.00000 0.01370 0.01869 = 0.01614 -0.00361 0.00151 -0.00395 AFIX 13 H7 2 0.738032 0.661953 1.134739 11.00000 -1.20000 AFIX 0 C8 1 0.890003 0.758806 1.101042 11.00000 0.02552 0.01878 = 0.02116 -0.00635 0.00425 -0.00924 AFIX 23 H8A 2 0.964938 0.776074 1.057555 11.00000 -1.20000 H8B 2 0.807811 0.822844 1.093091 11.00000 -1.20000 AFIX 0 C9 1 0.976169 0.722492 1.186634 11.00000 0.02608 0.02195 = 0.02463 -0.01138 0.00029 -0.00882 AFIX 23 H9A 2 1.028454 0.776615 1.189650 11.00000 -1.20000 H9B 2 0.899511 0.712720 1.229914 11.00000 -1.20000 AFIX 0 C10 1 1.098078 0.620986 1.204026 11.00000 0.02008 0.03142 = 0.02474 -0.00891 -0.00223 -0.00424 AFIX 23 H10A 2 1.181252 0.632380 1.164575 11.00000 -1.20000 H10B 2 1.147392 0.597054 1.261363 11.00000 -1.20000 AFIX 0 C11 1 1.022939 0.538718 1.194812 11.00000 0.02866 0.02261 = 0.02261 -0.00502 -0.00537 0.00214 AFIX 23 H11A 2 0.947154 0.522844 1.238041 11.00000 -1.20000 H11B 2 1.104947 0.474203 1.204141 11.00000 -1.20000 AFIX 0 C12 1 0.937604 0.572856 1.108577 11.00000 0.02380 0.02017 = 0.02080 -0.00713 -0.00384 -0.00435 AFIX 23 H12A 2 0.885725 0.518226 1.106306 11.00000 -1.20000 H12B 2 1.014569 0.582066 1.065440 11.00000 -1.20000 AFIX 0 C13 1 0.826671 0.753756 0.906757 11.00000 0.01138 0.01270 = 0.01686 -0.00492 -0.00062 0.00027 AFIX 13 H13 2 0.934649 0.710012 0.928256 11.00000 -1.20000 AFIX 0 C14 1 0.839667 0.868222 0.879433 11.00000 0.01507 0.01622 = 0.02314 -0.00579 0.00316 -0.00821 AFIX 23 H14A 2 0.734413 0.915036 0.859717 11.00000 -1.20000 H14B 2 0.878907 0.881009 0.927836 11.00000 -1.20000 AFIX 0 C15 1 0.950407 0.892385 0.809985 11.00000 0.02064 0.01914 = 0.02069 -0.00427 0.00640 -0.00843 AFIX 23 H15A 2 0.949934 0.967313 0.790514 11.00000 -1.20000 H15B 2 1.058527 0.852313 0.832128 11.00000 -1.20000 AFIX 0 C16 1 0.903609 0.865567 0.736802 11.00000 0.03001 0.02533 = 0.01755 -0.00419 0.00805 -0.01073 AFIX 23 H16A 2 0.981141 0.879096 0.694248 11.00000 -1.20000 H16B 2 0.799941 0.910688 0.710981 11.00000 -1.20000 AFIX 0 C17 1 0.895309 0.752186 0.764397 11.00000 0.02897 0.02329 = 0.01649 -0.01060 0.00520 -0.00726 AFIX 23 H17A 2 1.001078 0.706941 0.785666 11.00000 -1.20000 H17B 2 0.860478 0.737639 0.715948 11.00000 -1.20000 AFIX 0 C18 1 0.781291 0.727275 0.832626 11.00000 0.01793 0.01628 = 0.02168 -0.00676 0.00179 -0.00551 AFIX 23 H18A 2 0.673645 0.767606 0.809712 11.00000 -1.20000 H18B 2 0.781763 0.652379 0.851506 11.00000 -1.20000 AFIX 0 U2 6 0.000000 0.500000 0.500000 10.50000 0.01211 0.01175 = 0.01413 -0.00391 0.00029 -0.00432 CL2 3 0.236831 0.409093 0.431999 11.00000 0.02179 0.02791 = 0.03906 -0.01897 0.01120 -0.00782 P2 5 0.194833 0.722158 0.474833 11.00000 0.01188 0.01147 = 0.01549 -0.00531 0.00163 -0.00426 O2 4 0.095229 0.426425 0.600143 11.00000 0.02515 0.02013 = 0.02145 -0.00310 -0.00264 -0.00967 O4 4 0.129177 0.627206 0.488374 11.00000 0.01354 0.01361 = 0.01877 -0.00816 0.00317 -0.00537 C19 1 0.300082 0.744854 0.380684 11.00000 0.01207 0.01738 = 0.01257 -0.00341 0.00064 -0.00462 AFIX 13 H19 2 0.223750 0.751503 0.335103 11.00000 -1.20000 AFIX 0 C20 1 0.435978 0.653159 0.386481 11.00000 0.02200 0.01861 = 0.01683 -0.00386 0.00255 -0.00159 AFIX 23 H20A 2 0.396650 0.589014 0.400586 11.00000 -1.20000 H20B 2 0.514793 0.642753 0.431415 11.00000 -1.20000 AFIX 0 C21 1 0.513403 0.673448 0.302949 11.00000 0.02161 0.02113 = 0.02408 -0.01156 0.00703 0.00092 AFIX 23 H21A 2 0.604409 0.614953 0.308483 11.00000 -1.20000 H21B 2 0.437188 0.677257 0.259164 11.00000 -1.20000 AFIX 0 C22 1 0.567810 0.774302 0.277217 11.00000 0.02265 0.03624 = 0.01701 -0.01376 0.00363 -0.00857 AFIX 23 H22A 2 0.613690 0.786859 0.222544 11.00000 -1.20000 H22B 2 0.650376 0.768397 0.318709 11.00000 -1.20000 AFIX 0 C23 1 0.431787 0.865406 0.271001 11.00000 0.02514 0.02154 = 0.02269 -0.00396 0.00524 -0.00852 AFIX 23 H23A 2 0.353108 0.874718 0.226354 11.00000 -1.20000 H23B 2 0.470605 0.929842 0.255883 11.00000 -1.20000 AFIX 0 C24 1 0.354483 0.847539 0.353236 11.00000 0.02088 0.01749 = 0.02055 -0.00462 0.00690 -0.00715 AFIX 23 H24A 2 0.263085 0.906148 0.346688 11.00000 -1.20000 H24B 2 0.430101 0.845060 0.396753 11.00000 -1.20000 AFIX 0 C25 1 0.323750 0.699498 0.564396 11.00000 0.01291 0.01885 = 0.01983 -0.00952 0.00179 -0.00162 AFIX 13 H25 2 0.428657 0.661024 0.555151 11.00000 -1.20000 AFIX 0 C26 1 0.271568 0.627178 0.644139 11.00000 0.02365 0.01382 = 0.01979 -0.00410 -0.00275 -0.00802 AFIX 23 H26A 2 0.166840 0.661384 0.655670 11.00000 -1.20000 H26B 2 0.262561 0.562409 0.636220 11.00000 -1.20000 AFIX 0 C27 1 0.387815 0.600418 0.718128 11.00000 0.03903 0.02409 = 0.01458 0.00500 -0.00914 -0.01052 AFIX 23 H27A 2 0.489772 0.559831 0.709231 11.00000 -1.20000 H27B 2 0.348387 0.556893 0.769441 11.00000 -1.20000 AFIX 0 C28 1 0.411214 0.699474 0.729099 11.00000 0.03922 0.02871 = 0.01771 -0.00464 -0.00610 -0.01290 AFIX 23 H28A 2 0.311006 0.737032 0.742596 11.00000 -1.20000 H28B 2 0.489869 0.680449 0.776290 11.00000 -1.20000 AFIX 0 C29 1 0.465953 0.770039 0.650827 11.00000 0.02186 0.02163 = 0.02609 -0.01043 -0.00158 -0.00862 AFIX 23 H29A 2 0.570347 0.734610 0.639914 11.00000 -1.20000 H29B 2 0.476704 0.834307 0.659060 11.00000 -1.20000 AFIX 0 C30 1 0.350608 0.798448 0.575910 11.00000 0.02039 0.02085 = 0.01476 -0.00733 0.00300 -0.00902 AFIX 23 H30A 2 0.392223 0.841100 0.524997 11.00000 -1.20000 H30B 2 0.249332 0.840401 0.584145 11.00000 -1.20000 AFIX 0 C31 1 0.032923 0.834649 0.457595 11.00000 0.01152 0.01076 = 0.01995 -0.00721 0.00511 -0.00576 AFIX 13 H31 2 0.077363 0.896846 0.448283 11.00000 -1.20000 AFIX 0 C32 1 -0.062403 0.819034 0.535166 11.00000 0.01148 0.01740 = 0.01675 -0.00778 -0.00049 -0.00136 AFIX 23 H32A 2 0.005196 0.813967 0.582988 11.00000 -1.20000 H32B 2 -0.095945 0.752807 0.549407 11.00000 -1.20000 AFIX 0 C33 1 -0.208430 0.909168 0.520795 11.00000 0.01719 0.01941 = 0.02390 -0.01210 0.00549 -0.00561 AFIX 23 H33A 2 -0.270387 0.894283 0.570458 11.00000 -1.20000 H33B 2 -0.175095 0.974337 0.512778 11.00000 -1.20000 AFIX 0 C34 1 -0.309366 0.922897 0.444649 11.00000 0.01324 0.02233 = 0.02668 -0.00909 0.00229 -0.00018 AFIX 23 H34A 2 -0.401137 0.982043 0.435506 11.00000 -1.20000 H34B 2 -0.348750 0.859429 0.454486 11.00000 -1.20000 AFIX 0 C35 1 -0.216901 0.943084 0.367095 11.00000 0.01949 0.02432 = 0.02638 -0.00813 -0.00400 -0.00299 AFIX 23 H35A 2 -0.184184 1.009322 0.354793 11.00000 -1.20000 H35B 2 -0.284833 0.949925 0.318783 11.00000 -1.20000 AFIX 0 C36 1 -0.071998 0.854715 0.379510 11.00000 0.01869 0.01655 = 0.02156 -0.00403 0.00035 -0.00253 AFIX 23 H36A 2 -0.010455 0.872198 0.329824 11.00000 -1.20000 H36B 2 -0.105612 0.790405 0.384713 11.00000 -1.20000 AFIX 0 HKLF 4 REM cjw92_a.res in P-1 REM wR2 = 0.0549, GooF = S = 0.911, Restrained GooF = 0.910 for all data REM R1 = 0.0270 for 5257 Fo > 4sig(Fo) and 0.0475 for all 7307 data REM 409 parameters refined using 6 restraints END WGHT 0.0000 0.0000 REM Highest difference peak 1.081, deepest hole -0.953, 1-sigma level 0.133 Q1 1 0.2565 0.3586 0.5653 11.00000 0.05 1.08 Q2 1 0.2677 0.5833 1.0717 11.00000 0.05 0.90 Q3 1 -0.0048 0.4390 0.5785 11.00000 0.05 0.74 Q4 1 0.4425 0.4390 0.9968 11.00000 0.05 0.70 Q5 1 0.4474 0.5378 1.0523 11.00000 0.05 0.67 Q6 1 0.3517 0.4231 1.0983 11.00000 0.05 0.67 Q7 1 0.4015 0.5794 0.9723 11.00000 0.05 0.66 Q8 1 0.0854 0.4062 0.5456 11.00000 0.05 0.65 Q9 1 0.2664 0.6210 0.8862 11.00000 0.05 0.64 Q10 1 0.1887 0.4373 0.5613 11.00000 0.05 0.63 Q11 1 -0.0530 0.4434 0.4995 11.00000 0.05 0.62 Q12 1 0.1524 0.5788 0.4591 11.00000 0.05 0.62 Q13 1 0.4987 0.4362 1.0797 11.00000 0.05 0.60 Q14 1 0.0713 0.4866 0.5610 11.00000 0.05 0.58 Q15 1 0.2421 0.7249 0.4439 11.00000 0.05 0.56 Q16 1 0.1307 0.5146 0.3608 11.00000 0.05 0.56 Q17 1 0.1262 0.7782 0.4618 11.00000 0.05 0.55 Q18 1 0.0537 0.6411 0.4679 11.00000 0.05 0.53 Q19 1 0.2459 0.3785 0.6169 11.00000 0.05 0.53 Q20 1 0.1403 0.4181 0.4743 11.00000 0.05 0.52 ; _shelx_res_checksum 16734 _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 1.808 _oxdiff_exptl_absorpt_empirical_full_min 0.733 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 U1 U 0.500000 0.500000 1.000000 0.01245(6) Uani 1 2 d S T P . . Cl1 Cl 0.24182(13) 0.64682(9) 0.93032(7) 0.0246(3) Uani 1 1 d . . . . . P1 P 0.70089(13) 0.71532(9) 0.99168(7) 0.0137(2) Uani 1 1 d . . . . . O1 O 0.4428(4) 0.5030(2) 1.09787(17) 0.0206(7) Uani 1 1 d . . . . . O3 O 0.6364(3) 0.6254(2) 0.98818(17) 0.0158(7) Uani 1 1 d . . . . . C1 C 0.5377(5) 0.8247(3) 0.9839(3) 0.0151(10) Uani 1 1 d . . . . . H1 H 0.582423 0.882368 0.987712 0.018 Uiso 1 1 calc R . . . . C2 C 0.4307(5) 0.7961(3) 1.0559(3) 0.0196(11) Uani 1 1 d . . . . . H2A H 0.387678 0.737471 1.054586 0.023 Uiso 1 1 calc R . . . . H2B H 0.493035 0.773289 1.109738 0.023 Uiso 1 1 calc R . . . . C3 C 0.2952(5) 0.8890(4) 1.0494(3) 0.0244(11) Uani 1 1 d . . . . . H3A H 0.224342 0.866897 1.094138 0.029 Uiso 1 1 calc R . . . . H3B H 0.337850 0.944338 1.057742 0.029 Uiso 1 1 calc R . . . . C4 C 0.2025(5) 0.9322(4) 0.9654(3) 0.0242(11) Uani 1 1 d . . . . . H4A H 0.147989 0.880094 0.960173 0.029 Uiso 1 1 calc R . . . . H4B H 0.121897 0.995383 0.961706 0.029 Uiso 1 1 calc R . . . . C5 C 0.3083(5) 0.9591(3) 0.8944(3) 0.0216(11) Uani 1 1 d . . . . . H5A H 0.354199 1.016428 0.896094 0.026 Uiso 1 1 calc R . . . . H5B H 0.245293 0.983468 0.840534 0.026 Uiso 1 1 calc R . . . . C6 C 0.4403(5) 0.8654(3) 0.8997(2) 0.0160(10) Uani 1 1 d . . . . . H6A H 0.508996 0.885734 0.853508 0.019 Uiso 1 1 calc R . . . . H6B H 0.395191 0.809547 0.894042 0.019 Uiso 1 1 calc R . . . . C7 C 0.8138(5) 0.6758(3) 1.0904(3) 0.0169(10) Uani 1 1 d . . . . . H7 H 0.738032 0.661953 1.134739 0.020 Uiso 1 1 calc R . . . . C8 C 0.8900(6) 0.7588(3) 1.1010(3) 0.0214(11) Uani 1 1 d . . . . . H8A H 0.964938 0.776074 1.057555 0.026 Uiso 1 1 calc R . . . . H8B H 0.807811 0.822844 1.093091 0.026 Uiso 1 1 calc R . . . . C9 C 0.9762(6) 0.7225(3) 1.1866(3) 0.0228(11) Uani 1 1 d . U . . . H9A H 1.028454 0.776615 1.189650 0.027 Uiso 1 1 calc R . . . . H9B H 0.899511 0.712720 1.229914 0.027 Uiso 1 1 calc R . . . . C10 C 1.0981(6) 0.6210(4) 1.2040(3) 0.0260(11) Uani 1 1 d . . . . . H10A H 1.181252 0.632380 1.164575 0.031 Uiso 1 1 calc R . . . . H10B H 1.147392 0.597054 1.261363 0.031 Uiso 1 1 calc R . . . . C11 C 1.0229(6) 0.5387(4) 1.1948(3) 0.0268(12) Uani 1 1 d . . . . . H11A H 0.947154 0.522844 1.238041 0.032 Uiso 1 1 calc R . . . . H11B H 1.104947 0.474203 1.204141 0.032 Uiso 1 1 calc R . . . . C12 C 0.9376(5) 0.5729(3) 1.1086(3) 0.0217(11) Uani 1 1 d . . . . . H12A H 0.885725 0.518226 1.106306 0.026 Uiso 1 1 calc R . . . . H12B H 1.014569 0.582066 1.065440 0.026 Uiso 1 1 calc R . . . . C13 C 0.8267(5) 0.7538(3) 0.9068(2) 0.0143(10) Uani 1 1 d . . . . . H13 H 0.934649 0.710012 0.928256 0.017 Uiso 1 1 calc R . . . . C14 C 0.8397(5) 0.8682(3) 0.8794(3) 0.0177(10) Uani 1 1 d . . . . . H14A H 0.734413 0.915036 0.859717 0.021 Uiso 1 1 calc R . . . . H14B H 0.878907 0.881009 0.927836 0.021 Uiso 1 1 calc R . . . . C15 C 0.9504(5) 0.8924(3) 0.8100(3) 0.0203(11) Uani 1 1 d . . . . . H15A H 0.949934 0.967313 0.790514 0.024 Uiso 1 1 calc R . . . . H15B H 1.058527 0.852313 0.832128 0.024 Uiso 1 1 calc R . . . . C16 C 0.9036(6) 0.8656(4) 0.7368(3) 0.0246(11) Uani 1 1 d . . . . . H16A H 0.981141 0.879096 0.694248 0.030 Uiso 1 1 calc R . . . . H16B H 0.799941 0.910688 0.710981 0.030 Uiso 1 1 calc R . . . . C17 C 0.8953(6) 0.7522(3) 0.7644(3) 0.0218(11) Uani 1 1 d . . . . . H17A H 1.001078 0.706941 0.785666 0.026 Uiso 1 1 calc R . . . . H17B H 0.860478 0.737639 0.715948 0.026 Uiso 1 1 calc R . . . . C18 C 0.7813(5) 0.7273(3) 0.8326(3) 0.0184(10) Uani 1 1 d . . . . . H18A H 0.673645 0.767606 0.809712 0.022 Uiso 1 1 calc R . . . . H18B H 0.781763 0.652379 0.851506 0.022 Uiso 1 1 calc R . . . . U2 U 0.000000 0.500000 0.500000 0.01260(6) Uani 1 2 d S T P . . Cl2 Cl 0.23683(14) 0.40909(9) 0.43200(7) 0.0274(3) Uani 1 1 d . . . . . P2 P 0.19483(13) 0.72216(9) 0.47483(7) 0.0126(2) Uani 1 1 d . . . . . O2 O 0.0952(4) 0.4264(2) 0.60014(18) 0.0227(7) Uani 1 1 d . . . . . O4 O 0.1292(3) 0.6272(2) 0.48837(17) 0.0143(7) Uani 1 1 d . . . . . C19 C 0.3001(5) 0.7449(3) 0.3807(2) 0.0143(10) Uani 1 1 d . . . . . H19 H 0.223750 0.751503 0.335103 0.017 Uiso 1 1 calc R . . . . C20 C 0.4360(5) 0.6532(3) 0.3865(3) 0.0204(11) Uani 1 1 d . . . . . H20A H 0.396650 0.589014 0.400586 0.024 Uiso 1 1 calc R . . . . H20B H 0.514793 0.642753 0.431415 0.024 Uiso 1 1 calc R . . . . C21 C 0.5134(6) 0.6734(3) 0.3029(3) 0.0223(11) Uani 1 1 d . . . . . H21A H 0.604409 0.614953 0.308483 0.027 Uiso 1 1 calc R . . . . H21B H 0.437188 0.677257 0.259164 0.027 Uiso 1 1 calc R . . . . C22 C 0.5678(5) 0.7743(4) 0.2772(3) 0.0239(11) Uani 1 1 d . . . . . H22A H 0.613690 0.786859 0.222544 0.029 Uiso 1 1 calc R . . . . H22B H 0.650376 0.768397 0.318709 0.029 Uiso 1 1 calc R . . . . C23 C 0.4318(5) 0.8654(4) 0.2710(3) 0.0237(11) Uani 1 1 d . . . . . H23A H 0.353108 0.874718 0.226354 0.028 Uiso 1 1 calc R . . . . H23B H 0.470605 0.929842 0.255883 0.028 Uiso 1 1 calc R . . . . C24 C 0.3545(5) 0.8475(3) 0.3532(3) 0.0198(10) Uani 1 1 d . . . . . H24A H 0.263085 0.906148 0.346688 0.024 Uiso 1 1 calc R . . . . H24B H 0.430101 0.845060 0.396753 0.024 Uiso 1 1 calc R . . . . C25 C 0.3238(5) 0.6995(3) 0.5644(3) 0.0168(10) Uani 1 1 d . . . . . H25 H 0.428657 0.661024 0.555151 0.020 Uiso 1 1 calc R . . . . C26 C 0.2716(5) 0.6272(3) 0.6441(2) 0.0190(10) Uani 1 1 d . . . . . H26A H 0.166840 0.661384 0.655670 0.023 Uiso 1 1 calc R . . . . H26B H 0.262561 0.562409 0.636220 0.023 Uiso 1 1 calc R . . . . C27 C 0.3878(6) 0.6004(4) 0.7181(3) 0.0286(12) Uani 1 1 d . . . . . H27A H 0.489772 0.559831 0.709231 0.034 Uiso 1 1 calc R . . . . H27B H 0.348387 0.556893 0.769441 0.034 Uiso 1 1 calc R . . . . C28 C 0.4112(6) 0.6995(4) 0.7291(3) 0.0287(12) Uani 1 1 d . . . . . H28A H 0.311006 0.737032 0.742596 0.034 Uiso 1 1 calc R . . . . H28B H 0.489869 0.680449 0.776290 0.034 Uiso 1 1 calc R . . . . C29 C 0.4660(5) 0.7700(4) 0.6508(3) 0.0221(11) Uani 1 1 d . . . . . H29A H 0.570347 0.734610 0.639914 0.026 Uiso 1 1 calc R . . . . H29B H 0.476704 0.834307 0.659060 0.026 Uiso 1 1 calc R . . . . C30 C 0.3506(5) 0.7984(3) 0.5759(2) 0.0177(10) Uani 1 1 d . . . . . H30A H 0.392223 0.841100 0.524997 0.021 Uiso 1 1 calc R . . . . H30B H 0.249332 0.840401 0.584145 0.021 Uiso 1 1 calc R . . . . C31 C 0.0329(5) 0.8346(3) 0.4576(2) 0.0131(9) Uani 1 1 d . . . . . H31 H 0.077363 0.896846 0.448283 0.016 Uiso 1 1 calc R . . . . C32 C -0.0624(5) 0.8190(3) 0.5352(2) 0.0151(10) Uani 1 1 d . . . . . H32A H 0.005196 0.813967 0.582988 0.018 Uiso 1 1 calc R . . . . H32B H -0.095945 0.752807 0.549407 0.018 Uiso 1 1 calc R . . . . C33 C -0.2084(5) 0.9092(3) 0.5208(3) 0.0188(10) Uani 1 1 d . . . . . H33A H -0.270387 0.894283 0.570458 0.023 Uiso 1 1 calc R . . . . H33B H -0.175095 0.974337 0.512778 0.023 Uiso 1 1 calc R . . . . C34 C -0.3094(5) 0.9229(4) 0.4446(3) 0.0213(11) Uani 1 1 d . . . . . H34A H -0.401137 0.982043 0.435506 0.026 Uiso 1 1 calc R . . . . H34B H -0.348750 0.859429 0.454486 0.026 Uiso 1 1 calc R . . . . C35 C -0.2169(5) 0.9431(4) 0.3671(3) 0.0240(11) Uani 1 1 d . . . . . H35A H -0.184184 1.009322 0.354793 0.029 Uiso 1 1 calc R . . . . H35B H -0.284833 0.949925 0.318783 0.029 Uiso 1 1 calc R . . . . C36 C -0.0720(5) 0.8547(3) 0.3795(3) 0.0200(10) Uani 1 1 d . . . . . H36A H -0.010455 0.872198 0.329824 0.024 Uiso 1 1 calc R . . . . H36B H -0.105612 0.790405 0.384713 0.024 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 0.01176(13) 0.01185(13) 0.01310(12) -0.00302(10) 0.00051(10) -0.00382(10) Cl1 0.0163(6) 0.0206(6) 0.0307(7) -0.0036(5) -0.0035(5) -0.0008(5) P1 0.0123(6) 0.0102(6) 0.0187(6) -0.0045(5) 0.0031(5) -0.0041(5) O1 0.0224(18) 0.0214(18) 0.0180(16) -0.0062(14) 0.0047(14) -0.0068(15) O3 0.0156(17) 0.0118(16) 0.0200(16) -0.0049(13) 0.0004(13) -0.0041(13) C1 0.014(2) 0.013(2) 0.022(2) -0.008(2) 0.0029(19) -0.0064(19) C2 0.017(3) 0.026(3) 0.020(2) -0.012(2) 0.008(2) -0.007(2) C3 0.018(3) 0.031(3) 0.028(3) -0.016(2) 0.005(2) -0.006(2) C4 0.018(3) 0.023(3) 0.031(3) -0.011(2) 0.004(2) -0.002(2) C5 0.016(3) 0.018(3) 0.027(3) -0.003(2) 0.002(2) -0.004(2) C6 0.011(2) 0.021(3) 0.017(2) -0.005(2) 0.0063(19) -0.007(2) C7 0.014(2) 0.019(3) 0.016(2) -0.004(2) 0.0015(19) -0.004(2) C8 0.026(3) 0.019(3) 0.021(3) -0.006(2) 0.004(2) -0.009(2) C9 0.026(3) 0.022(3) 0.025(2) -0.011(2) 0.000(2) -0.009(2) C10 0.020(3) 0.031(3) 0.025(3) -0.009(2) -0.002(2) -0.004(2) C11 0.029(3) 0.023(3) 0.023(3) -0.005(2) -0.005(2) 0.002(2) C12 0.024(3) 0.020(3) 0.021(3) -0.007(2) -0.004(2) -0.004(2) C13 0.011(2) 0.013(2) 0.017(2) -0.0049(19) -0.0006(19) 0.0003(19) C14 0.015(2) 0.016(2) 0.023(2) -0.006(2) 0.003(2) -0.008(2) C15 0.021(3) 0.019(3) 0.021(2) -0.004(2) 0.006(2) -0.008(2) C16 0.030(3) 0.025(3) 0.018(2) -0.004(2) 0.008(2) -0.011(2) C17 0.029(3) 0.023(3) 0.016(2) -0.011(2) 0.005(2) -0.007(2) C18 0.018(3) 0.016(3) 0.022(2) -0.007(2) 0.002(2) -0.006(2) U2 0.01211(13) 0.01175(13) 0.01413(12) -0.00391(10) 0.00029(10) -0.00432(10) Cl2 0.0218(7) 0.0279(7) 0.0391(7) -0.0190(6) 0.0112(6) -0.0078(5) P2 0.0119(6) 0.0115(6) 0.0155(6) -0.0053(5) 0.0016(5) -0.0043(5) O2 0.0252(19) 0.0201(18) 0.0214(17) -0.0031(14) -0.0026(15) -0.0097(15) O4 0.0135(16) 0.0136(16) 0.0188(16) -0.0082(13) 0.0032(13) -0.0054(13) C19 0.012(2) 0.017(2) 0.013(2) -0.0034(19) 0.0006(18) -0.0046(19) C20 0.022(3) 0.019(3) 0.017(2) -0.004(2) 0.003(2) -0.002(2) C21 0.022(3) 0.021(3) 0.024(3) -0.012(2) 0.007(2) 0.001(2) C22 0.023(3) 0.036(3) 0.017(2) -0.014(2) 0.004(2) -0.009(2) C23 0.025(3) 0.022(3) 0.023(3) -0.004(2) 0.005(2) -0.009(2) C24 0.021(3) 0.017(3) 0.021(2) -0.005(2) 0.007(2) -0.007(2) C25 0.013(2) 0.019(3) 0.020(2) -0.010(2) 0.0018(19) -0.002(2) C26 0.024(3) 0.014(2) 0.020(2) -0.004(2) -0.003(2) -0.008(2) C27 0.039(3) 0.024(3) 0.015(2) 0.005(2) -0.009(2) -0.011(2) C28 0.039(3) 0.029(3) 0.018(3) -0.005(2) -0.006(2) -0.013(3) C29 0.022(3) 0.022(3) 0.026(3) -0.010(2) -0.002(2) -0.009(2) C30 0.020(3) 0.021(3) 0.015(2) -0.007(2) 0.003(2) -0.009(2) C31 0.012(2) 0.011(2) 0.020(2) -0.0072(19) 0.0051(19) -0.0058(18) C32 0.011(2) 0.017(2) 0.017(2) -0.008(2) -0.0005(19) -0.0014(19) C33 0.017(3) 0.019(3) 0.024(3) -0.012(2) 0.005(2) -0.006(2) C34 0.013(2) 0.022(3) 0.027(3) -0.009(2) 0.002(2) 0.000(2) C35 0.019(3) 0.024(3) 0.026(3) -0.008(2) -0.004(2) -0.003(2) C36 0.019(3) 0.017(3) 0.022(3) -0.004(2) 0.000(2) -0.003(2) 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' Cl Cl 0.1484 0.1585 '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' 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 Cl1 U1 Cl1 180.0 2_667 . ? O1 U1 Cl1 88.43(10) 2_667 2_667 ? O1 U1 Cl1 88.43(10) . . ? O1 U1 Cl1 91.57(10) 2_667 . ? O1 U1 Cl1 91.57(10) . 2_667 ? O1 U1 O1 180.0 2_667 . ? O1 U1 O3 90.18(12) 2_667 . ? O1 U1 O3 89.82(12) 2_667 2_667 ? O1 U1 O3 89.82(12) . . ? O1 U1 O3 90.18(12) . 2_667 ? O3 U1 Cl1 89.68(8) 2_667 . ? O3 U1 Cl1 89.68(8) . 2_667 ? O3 U1 Cl1 90.32(8) . . ? O3 U1 Cl1 90.32(8) 2_667 2_667 ? O3 U1 O3 180.0 2_667 . ? O3 P1 C1 109.11(19) . . ? O3 P1 C7 109.45(18) . . ? O3 P1 C13 110.24(18) . . ? C7 P1 C1 108.83(19) . . ? C7 P1 C13 109.2(2) . . ? C13 P1 C1 109.96(19) . . ? P1 O3 U1 167.99(18) . . ? P1 C1 H1 107.9 . . ? C2 C1 P1 111.6(3) . . ? C2 C1 H1 107.9 . . ? C2 C1 C6 109.8(4) . . ? C6 C1 P1 111.7(3) . . ? C6 C1 H1 107.9 . . ? C1 C2 H2A 109.4 . . ? C1 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? C3 C2 C1 111.1(4) . . ? C3 C2 H2A 109.4 . . ? C3 C2 H2B 109.4 . . ? C2 C3 H3A 109.3 . . ? C2 C3 H3B 109.3 . . ? H3A C3 H3B 107.9 . . ? C4 C3 C2 111.7(4) . . ? C4 C3 H3A 109.3 . . ? C4 C3 H3B 109.3 . . ? C3 C4 H4A 109.4 . . ? C3 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? C5 C4 C3 111.4(4) . . ? C5 C4 H4A 109.4 . . ? C5 C4 H4B 109.4 . . ? C4 C5 H5A 109.3 . . ? C4 C5 H5B 109.3 . . ? C4 C5 C6 111.5(4) . . ? H5A C5 H5B 108.0 . . ? C6 C5 H5A 109.3 . . ? C6 C5 H5B 109.3 . . ? C1 C6 H6A 109.6 . . ? C1 C6 H6B 109.6 . . ? C5 C6 C1 110.1(3) . . ? C5 C6 H6A 109.6 . . ? C5 C6 H6B 109.6 . . ? H6A C6 H6B 108.1 . . ? P1 C7 H7 106.4 . . ? C8 C7 P1 114.8(3) . . ? C8 C7 H7 106.4 . . ? C8 C7 C12 110.2(4) . . ? C12 C7 P1 112.2(3) . . ? C12 C7 H7 106.4 . . ? C7 C8 H8A 109.2 . . ? C7 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? C9 C8 C7 112.0(4) . . ? C9 C8 H8A 109.2 . . ? C9 C8 H8B 109.2 . . ? C8 C9 H9A 109.3 . . ? C8 C9 H9B 109.3 . . ? H9A C9 H9B 108.0 . . ? C10 C9 C8 111.4(4) . . ? C10 C9 H9A 109.3 . . ? C10 C9 H9B 109.3 . . ? C9 C10 H10A 109.6 . . ? C9 C10 H10B 109.6 . . ? H10A C10 H10B 108.1 . . ? C11 C10 C9 110.5(4) . . ? C11 C10 H10A 109.6 . . ? C11 C10 H10B 109.6 . . ? C10 C11 H11A 109.1 . . ? C10 C11 H11B 109.1 . . ? C10 C11 C12 112.3(4) . . ? H11A C11 H11B 107.9 . . ? C12 C11 H11A 109.1 . . ? C12 C11 H11B 109.1 . . ? C7 C12 H12A 109.6 . . ? C7 C12 H12B 109.6 . . ? C11 C12 C7 110.5(4) . . ? C11 C12 H12A 109.6 . . ? C11 C12 H12B 109.6 . . ? H12A C12 H12B 108.1 . . ? P1 C13 H13 106.2 . . ? C14 C13 P1 114.6(3) . . ? C14 C13 H13 106.2 . . ? C18 C13 P1 111.4(3) . . ? C18 C13 H13 106.2 . . ? C18 C13 C14 111.5(3) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? C15 C14 C13 110.9(3) . . ? C15 C14 H14A 109.5 . . ? C15 C14 H14B 109.5 . . ? C14 C15 H15A 109.3 . . ? C14 C15 H15B 109.3 . . ? H15A C15 H15B 107.9 . . ? C16 C15 C14 111.8(4) . . ? C16 C15 H15A 109.3 . . ? C16 C15 H15B 109.3 . . ? C15 C16 H16A 109.4 . . ? C15 C16 H16B 109.4 . . ? C15 C16 C17 111.2(4) . . ? H16A C16 H16B 108.0 . . ? C17 C16 H16A 109.4 . . ? C17 C16 H16B 109.4 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? C16 C17 C18 110.9(4) . . ? H17A C17 H17B 108.0 . . ? C18 C17 H17A 109.5 . . ? C18 C17 H17B 109.5 . . ? C13 C18 C17 111.0(4) . . ? C13 C18 H18A 109.4 . . ? C13 C18 H18B 109.4 . . ? C17 C18 H18A 109.4 . . ? C17 C18 H18B 109.4 . . ? H18A C18 H18B 108.0 . . ? Cl2 U2 Cl2 180.0 . 2_566 ? O2 U2 Cl2 89.76(10) 2_566 2_566 ? O2 U2 Cl2 89.76(10) . . ? O2 U2 Cl2 90.24(10) . 2_566 ? O2 U2 Cl2 90.24(10) 2_566 . ? O2 U2 O2 180.0 . 2_566 ? O2 U2 O4 89.78(12) 2_566 . ? O2 U2 O4 89.78(12) . 2_566 ? O2 U2 O4 90.22(12) 2_566 2_566 ? O2 U2 O4 90.22(12) . . ? O4 U2 Cl2 91.11(7) 2_566 . ? O4 U2 Cl2 88.89(7) . . ? O4 U2 Cl2 88.90(7) 2_566 2_566 ? O4 U2 Cl2 91.11(7) . 2_566 ? O4 U2 O4 180.0 . 2_566 ? O4 P2 C19 108.01(18) . . ? O4 P2 C25 109.49(18) . . ? O4 P2 C31 108.94(19) . . ? C25 P2 C19 111.1(2) . . ? C25 P2 C31 111.46(19) . . ? C31 P2 C19 107.81(19) . . ? P2 O4 U2 172.31(19) . . ? P2 C19 H19 106.4 . . ? C20 C19 P2 112.6(3) . . ? C20 C19 H19 106.4 . . ? C20 C19 C24 111.2(4) . . ? C24 C19 P2 113.3(3) . . ? C24 C19 H19 106.4 . . ? C19 C20 H20A 109.6 . . ? C19 C20 H20B 109.6 . . ? C19 C20 C21 110.4(4) . . ? H20A C20 H20B 108.1 . . ? C21 C20 H20A 109.6 . . ? C21 C20 H20B 109.6 . . ? C20 C21 H21A 109.4 . . ? C20 C21 H21B 109.4 . . ? H21A C21 H21B 108.0 . . ? C22 C21 C20 111.0(4) . . ? C22 C21 H21A 109.4 . . ? C22 C21 H21B 109.4 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? C21 C22 C23 110.9(4) . . ? H22A C22 H22B 108.1 . . ? C23 C22 H22A 109.5 . . ? C23 C22 H22B 109.5 . . ? C22 C23 H23A 109.4 . . ? C22 C23 H23B 109.4 . . ? C22 C23 C24 111.1(4) . . ? H23A C23 H23B 108.0 . . ? C24 C23 H23A 109.4 . . ? C24 C23 H23B 109.4 . . ? C19 C24 H24A 109.5 . . ? C19 C24 H24B 109.5 . . ? C23 C24 C19 110.6(4) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 108.1 . . ? P2 C25 H25 106.2 . . ? C26 C25 P2 111.1(3) . . ? C26 C25 H25 106.2 . . ? C26 C25 C30 111.2(3) . . ? C30 C25 P2 115.3(3) . . ? C30 C25 H25 106.2 . . ? C25 C26 H26A 109.4 . . ? C25 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? C27 C26 C25 111.1(4) . . ? C27 C26 H26A 109.4 . . ? C27 C26 H26B 109.4 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? C26 C27 C28 110.7(4) . . ? H27A C27 H27B 108.1 . . ? C28 C27 H27A 109.5 . . ? C28 C27 H27B 109.5 . . ? C27 C28 H28A 109.4 . . ? C27 C28 H28B 109.4 . . ? H28A C28 H28B 108.0 . . ? C29 C28 C27 111.2(4) . . ? C29 C28 H28A 109.4 . . ? C29 C28 H28B 109.4 . . ? C28 C29 H29A 109.4 . . ? C28 C29 H29B 109.4 . . ? C28 C29 C30 111.1(4) . . ? H29A C29 H29B 108.0 . . ? C30 C29 H29A 109.4 . . ? C30 C29 H29B 109.4 . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? C29 C30 C25 110.7(4) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 108.1 . . ? P2 C31 H31 108.3 . . ? C32 C31 P2 110.1(3) . . ? C32 C31 H31 108.3 . . ? C36 C31 P2 110.6(3) . . ? C36 C31 H31 108.3 . . ? C36 C31 C32 111.1(4) . . ? C31 C32 H32A 109.2 . . ? C31 C32 H32B 109.2 . . ? C31 C32 C33 111.8(3) . . ? H32A C32 H32B 107.9 . . ? C33 C32 H32A 109.2 . . ? C33 C32 H32B 109.2 . . ? C32 C33 H33A 109.6 . . ? C32 C33 H33B 109.6 . . ? H33A C33 H33B 108.1 . . ? C34 C33 C32 110.4(3) . . ? C34 C33 H33A 109.6 . . ? C34 C33 H33B 109.6 . . ? C33 C34 H34A 109.4 . . ? C33 C34 H34B 109.4 . . ? C33 C34 C35 111.3(4) . . ? H34A C34 H34B 108.0 . . ? C35 C34 H34A 109.4 . . ? C35 C34 H34B 109.4 . . ? C34 C35 H35A 109.4 . . ? C34 C35 H35B 109.4 . . ? C34 C35 C36 111.0(4) . . ? H35A C35 H35B 108.0 . . ? C36 C35 H35A 109.4 . . ? C36 C35 H35B 109.4 . . ? C31 C36 H36A 109.2 . . ? C31 C36 H36B 109.2 . . ? C35 C36 C31 112.1(4) . . ? 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 U1 Cl1 2.6597(11) . ? U1 Cl1 2.6597(11) 2_667 ? U1 O1 1.760(3) 2_667 ? U1 O1 1.760(3) . ? U1 O3 2.299(3) 2_667 ? U1 O3 2.299(3) . ? P1 O3 1.519(3) . ? P1 C1 1.823(4) . ? P1 C7 1.814(4) . ? P1 C13 1.819(4) . ? C1 H1 1.0000 . ? C1 C2 1.536(6) . ? C1 C6 1.540(6) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C2 C3 1.532(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C3 C4 1.517(6) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C4 C5 1.515(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C5 C6 1.527(6) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7 1.0000 . ? C7 C8 1.533(6) . ? C7 C12 1.541(6) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C8 C9 1.521(6) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C9 C10 1.519(6) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C10 C11 1.509(6) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C11 C12 1.531(6) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13 1.0000 . ? C13 C14 1.547(5) . ? C13 C18 1.526(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C14 C15 1.521(5) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C15 C16 1.518(6) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C16 C17 1.520(6) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C17 C18 1.528(6) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? U2 Cl2 2.6698(11) 2_566 ? U2 Cl2 2.6697(11) . ? U2 O2 1.767(3) . ? U2 O2 1.767(3) 2_566 ? U2 O4 2.279(3) 2_566 ? U2 O4 2.279(3) . ? P2 O4 1.517(3) . ? P2 C19 1.816(4) . ? P2 C25 1.809(4) . ? P2 C31 1.816(4) . ? C19 H19 1.0000 . ? C19 C20 1.526(6) . ? C19 C24 1.540(6) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C20 C21 1.541(5) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C21 C22 1.518(6) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C22 C23 1.520(6) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C23 C24 1.523(5) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25 1.0000 . ? C25 C26 1.529(6) . ? C25 C30 1.545(6) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C26 C27 1.521(6) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C27 C28 1.532(6) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C28 C29 1.512(6) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C29 C30 1.524(6) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31 1.0000 . ? C31 C32 1.539(5) . ? C31 C36 1.538(6) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C32 C33 1.542(6) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C33 C34 1.516(6) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C34 C35 1.524(6) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C35 C36 1.526(6) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ?