#------------------------------------------------------------------------------ #$Date: 2021-10-02 02:04:16 +0300 (Sat, 02 Oct 2021) $ #$Revision: 269445 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/85/7708503.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_7708503 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 N2 O10 P2 U' _chemical_formula_sum 'C36 H66 N2 O10 P2 U' _chemical_formula_weight 986.87 _chemical_name_common 'uranyldinitrate bis(tricyclohexylphosphine oxide)' _chemical_name_systematic 'uraniumdioxodinitrato bis(tricyclohexylphosphine oxide)' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2020-01-06 _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 90 _cell_angle_beta 103.075(6) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 8.5735(6) _cell_length_b 16.4438(10) _cell_length_c 14.6892(9) _cell_measurement_reflns_used 5571 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 30.2290 _cell_measurement_theta_min 2.4320 _cell_volume 2017.2(2) _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)' _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 0.993 _diffrn_measured_fraction_theta_max 0.993 _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 2.27 185.07 0.40 20.00 -- 28.00 73.71 -25.73 457 2 \w 2.27 185.07 0.40 20.00 -- 28.00 73.71 64.28 457 3 \w 2.27 185.07 0.40 20.00 -- 28.00 73.71 154.28 457 4 \w 2.27 171.07 0.40 20.00 -- 28.00 73.71-115.72 422 ; _diffrn_measurement_device 'abstract diffractometer' _diffrn_measurement_device_type 'Saxi-CrysAlisPro-abstract goniometer imported SAXI images' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0093099000 _diffrn_orient_matrix_UB_12 0.0423017000 _diffrn_orient_matrix_UB_13 0.0090583000 _diffrn_orient_matrix_UB_21 -0.0251954000 _diffrn_orient_matrix_UB_22 0.0080910000 _diffrn_orient_matrix_UB_23 -0.0485243000 _diffrn_orient_matrix_UB_31 -0.0806155000 _diffrn_orient_matrix_UB_32 0.0023277000 _diffrn_orient_matrix_UB_33 0.0043825000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1389 _diffrn_reflns_av_unetI/netI 0.0796 _diffrn_reflns_Laue_measured_fraction_full 0.993 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 24252 _diffrn_reflns_point_group_measured_fraction_full 0.993 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.682 _diffrn_reflns_theta_min 1.887 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 4.158 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.29371 _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 1.625 _exptl_crystal_description needle _exptl_crystal_F_000 996 _exptl_crystal_preparation 'By CJW.' _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Acetone' _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.1 _refine_diff_density_max 1.770 _refine_diff_density_min -1.415 _refine_diff_density_rms 0.172 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.900 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 232 _refine_ls_number_reflns 3807 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.900 _refine_ls_R_factor_all 0.0557 _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^)+(0.0435P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0822 _refine_ls_wR_factor_ref 0.0851 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2562 _reflns_number_total 3807 _reflns_threshold_expression 'I > 2\s(I)' _twin_special_details ; Component 2 rotated by 179.9895\% around [-0.00 0.71 0.71] (reciprocal) or [0.30 0.58 0.76] (direct) ; _cod_data_source_file d1dt03041h2.cif _cod_data_source_block cjw91 _cod_original_sg_symbol_H-M P21/n _cod_database_code 7708503 _lanl_internal_la-ur LA-UR-19-30804 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula UO2(NO3)2(OPC18H51)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 0.681 _shelx_estimated_absorpt_t_min 0.350 _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) 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) ; _shelx_res_file ; TITL cjw91_twin1_hklf4_a.res in P2(1)/n cjw91.res created by SHELXL-2018/3 at 16:54:32 on 06-Jan-2020 REM Old TITL cjw91_twin1_hklf4 in P2(1)/n REM SHELXT solution in P2(1)/n: R1 0.100, Rweak 0.002, Alpha 0.048 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C34 N4 O10 P2 U CELL 0.71073 8.573451 16.443752 14.6892 90 103.0746 90 ZERR 2 0.000567 0.000971 0.000869 0 0.0061 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H N O P U UNIT 72 132 4 20 4 2 EQIV $1 1-X,1-Y,1-Z L.S. 10 0 0 PLAN 20 SIZE 0.1 0.14 0.32 TEMP -173(2) FREE U1 N1_$1 FREE U1 N1 BOND list 4 fmap 2 53 acta SHEL 100 0.82 OMIT 5 4 9 OMIT 1 3 0 OMIT 1 8 5 REM REM REM WGHT 0.043500 FVAR 0.79547 U1 6 0.500000 0.500000 0.500000 10.50000 0.01766 0.01936 = 0.01966 -0.00010 0.00711 0.00139 P1 5 0.304934 0.526594 0.709537 11.00000 0.02402 0.01858 = 0.02079 0.00031 0.01040 0.00002 O1 4 0.313896 0.504160 0.418181 11.00000 0.01297 0.03392 = 0.02074 -0.00005 -0.00617 0.00136 O2 4 0.374228 0.516369 0.624270 11.00000 0.02922 0.02440 = 0.02787 -0.00015 0.01149 0.00486 O3 4 0.407257 0.369207 0.563334 11.00000 0.04650 0.02254 = 0.03224 0.00071 0.02025 0.00539 O4 4 0.535055 0.352258 0.455264 11.00000 0.03652 0.02831 = 0.03109 -0.00211 0.01714 -0.00111 O5 4 0.441354 0.245729 0.516142 11.00000 0.05613 0.01967 = 0.04414 0.00004 0.01741 0.00118 N1 3 0.461739 0.318938 0.511720 11.00000 0.03346 0.02841 = 0.02501 0.00133 0.00718 0.00169 C1 1 0.462294 0.537991 0.814246 11.00000 0.02755 0.02086 = 0.02489 0.00233 0.01067 -0.00046 AFIX 13 H1 2 0.409797 0.543035 0.868240 11.00000 -1.20000 AFIX 0 C2 1 0.565615 0.614913 0.813457 11.00000 0.03001 0.02486 = 0.04121 0.00605 0.00733 -0.00487 AFIX 23 H2A 2 0.617674 0.612117 0.759862 11.00000 -1.20000 H2B 2 0.495744 0.663543 0.805113 11.00000 -1.20000 AFIX 0 C3 1 0.692973 0.623371 0.903202 11.00000 0.03404 0.03474 = 0.03814 0.00059 0.00158 -0.00497 AFIX 23 H3A 2 0.641122 0.631291 0.956311 11.00000 -1.20000 H3B 2 0.759706 0.671786 0.899149 11.00000 -1.20000 AFIX 0 C4 1 0.798605 0.548091 0.920288 11.00000 0.02731 0.05428 = 0.02842 -0.00001 0.00594 -0.00232 AFIX 23 H4A 2 0.860054 0.544193 0.870931 11.00000 -1.20000 H4B 2 0.876196 0.553631 0.981108 11.00000 -1.20000 AFIX 0 C5 1 0.702707 0.470615 0.920738 11.00000 0.03617 0.03383 = 0.02600 0.00312 0.00561 0.00773 AFIX 23 H5A 2 0.653357 0.470985 0.975499 11.00000 -1.20000 H5B 2 0.775556 0.423223 0.926846 11.00000 -1.20000 AFIX 0 C6 1 0.571754 0.461824 0.831735 11.00000 0.03484 0.02609 = 0.03635 0.00435 0.00820 0.00518 AFIX 23 H6A 2 0.506118 0.413250 0.836961 11.00000 -1.20000 H6B 2 0.621585 0.453685 0.777844 11.00000 -1.20000 AFIX 0 C7 1 0.196254 0.434720 0.725545 11.00000 0.03578 0.01269 = 0.03050 0.00043 0.01096 -0.00078 AFIX 13 H7 2 0.269798 0.388549 0.720597 11.00000 -1.20000 AFIX 0 C8 1 0.154396 0.425316 0.822152 11.00000 0.03859 0.02248 = 0.03388 0.00382 0.01572 -0.00614 AFIX 23 H8A 2 0.253435 0.429705 0.871940 11.00000 -1.20000 H8B 2 0.081583 0.469834 0.831115 11.00000 -1.20000 AFIX 0 C9 1 0.074328 0.343647 0.830356 11.00000 0.04590 0.02228 = 0.03879 0.00364 0.02141 -0.00106 AFIX 23 H9A 2 0.151749 0.299224 0.829093 11.00000 -1.20000 H9B 2 0.041949 0.340978 0.890846 11.00000 -1.20000 AFIX 0 C10 1 -0.071941 0.331901 0.751026 11.00000 0.03852 0.01848 = 0.05612 -0.00163 0.02741 -0.00480 AFIX 23 H10A 2 -0.153553 0.373177 0.756201 11.00000 -1.20000 H10B 2 -0.118476 0.277536 0.756658 11.00000 -1.20000 AFIX 0 C11 1 -0.031143 0.339276 0.655458 11.00000 0.03734 0.02296 = 0.04466 -0.00651 0.01549 -0.01442 AFIX 23 H11A 2 -0.129968 0.334205 0.605621 11.00000 -1.20000 H11B 2 0.042645 0.294931 0.647364 11.00000 -1.20000 AFIX 0 C12 1 0.047695 0.421600 0.647567 11.00000 0.02819 0.02785 = 0.03474 0.00193 0.00577 -0.00731 AFIX 23 H12A 2 0.077827 0.424952 0.586470 11.00000 -1.20000 H12B 2 -0.030428 0.465466 0.649829 11.00000 -1.20000 AFIX 0 C13 1 0.182701 0.618999 0.694344 11.00000 0.02184 0.02184 = 0.02742 0.00104 0.00849 0.00154 AFIX 13 H13 2 0.260084 0.665237 0.700096 11.00000 -1.20000 AFIX 0 C14 1 0.086160 0.634235 0.768782 11.00000 0.03233 0.02367 = 0.02451 -0.00200 0.00845 0.00418 AFIX 23 H14A 2 0.006661 0.590171 0.766431 11.00000 -1.20000 H14B 2 0.159036 0.633683 0.831557 11.00000 -1.20000 AFIX 0 C15 1 -0.000241 0.716191 0.752628 11.00000 0.04688 0.02929 = 0.03946 -0.00723 0.01721 0.01009 AFIX 23 H15A 2 -0.067525 0.723149 0.798684 11.00000 -1.20000 H15B 2 0.079755 0.760614 0.762233 11.00000 -1.20000 AFIX 0 C16 1 -0.105439 0.721726 0.653797 11.00000 0.02642 0.02252 = 0.03603 0.00292 0.00798 0.00568 AFIX 23 H16A 2 -0.191717 0.680588 0.646338 11.00000 -1.20000 H16B 2 -0.156147 0.776099 0.644596 11.00000 -1.20000 AFIX 0 C17 1 -0.009967 0.707923 0.580288 11.00000 0.02977 0.02442 = 0.03521 0.00345 0.00520 0.00322 AFIX 23 H17A 2 0.070141 0.751845 0.583751 11.00000 -1.20000 H17B 2 -0.082471 0.709483 0.517422 11.00000 -1.20000 AFIX 0 C18 1 0.075269 0.625529 0.595213 11.00000 0.03554 0.02363 = 0.03284 0.00054 0.01674 0.00790 AFIX 23 H18A 2 0.141468 0.618615 0.548583 11.00000 -1.20000 H18B 2 -0.005417 0.581431 0.585651 11.00000 -1.20000 AFIX 0 HKLF 4 REM cjw91_twin1_hklf4_a.res in P2(1)/n REM wR2 = 0.0851, GooF = S = 0.900, Restrained GooF = 0.900 for all data REM R1 = 0.0399 for 2562 Fo > 4sig(Fo) and 0.0557 for all 3807 data REM 232 parameters refined using 0 restraints END WGHT 0.0436 0.0000 REM Highest difference peak 1.770, deepest hole -1.415, 1-sigma level 0.172 Q1 1 0.4819 0.5346 0.5426 11.00000 0.05 1.77 Q2 1 0.5155 0.5340 0.4575 11.00000 0.05 1.72 Q3 1 0.4426 0.4770 0.5361 11.00000 0.05 1.59 Q4 1 0.5578 0.4757 0.4639 11.00000 0.05 1.57 Q5 1 0.3220 0.5000 0.4714 11.00000 0.05 1.09 Q6 1 -0.0547 0.6428 0.6354 11.00000 0.05 0.97 Q7 1 0.4149 0.5032 0.6756 11.00000 0.05 0.87 Q8 1 0.3954 0.4152 0.5166 11.00000 0.05 0.85 Q9 1 0.3687 0.4999 0.3987 11.00000 0.05 0.84 Q10 1 0.1240 0.7143 0.7392 11.00000 0.05 0.80 Q11 1 0.3186 0.4463 0.4007 11.00000 0.05 0.79 Q12 1 0.4371 0.5001 0.3910 11.00000 0.05 0.74 Q13 1 0.3202 0.5524 0.4025 11.00000 0.05 0.71 Q14 1 0.1281 0.2876 0.7389 11.00000 0.05 0.70 Q15 1 0.6068 0.4166 0.4835 11.00000 0.05 0.70 Q16 1 -0.0515 0.3572 0.6312 11.00000 0.05 0.69 Q17 1 0.2317 0.5000 0.4125 11.00000 0.05 0.60 Q18 1 0.4184 0.4967 0.6021 11.00000 0.05 0.60 Q19 1 0.3971 0.5416 0.6010 11.00000 0.05 0.59 Q20 1 0.4958 0.4101 0.4997 11.00000 0.05 0.56 ; _shelx_res_checksum 5924 _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 3.114 _oxdiff_exptl_absorpt_empirical_full_min 0.547 _oxdiff_twin_integration_method simultaneous _oxdiff_twin_items 2 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.500000 0.500000 0.500000 0.01843(10) Uani 1 2 d S T P . . P1 P 0.30493(17) 0.52659(8) 0.70954(9) 0.0203(3) Uani 1 1 d . . . . . O1 O 0.3139(4) 0.50416(19) 0.4182(2) 0.0241(8) Uani 1 1 d . . . . . O2 O 0.3742(4) 0.51637(19) 0.6243(2) 0.0264(9) Uani 1 1 d . . . . . O3 O 0.4073(5) 0.3692(2) 0.5633(2) 0.0320(10) Uani 1 1 d . . . . . O4 O 0.5351(4) 0.3523(2) 0.4553(2) 0.0305(9) Uani 1 1 d . . . . . O5 O 0.4414(5) 0.2457(2) 0.5161(2) 0.0390(10) Uani 1 1 d . . . . . N1 N 0.4617(6) 0.3189(3) 0.5117(3) 0.0289(11) Uani 1 1 d . . . . . C1 C 0.4623(6) 0.5380(3) 0.8142(3) 0.0237(12) Uani 1 1 d . . . . . H1 H 0.409797 0.543035 0.868240 0.028 Uiso 1 1 calc R . . . . C2 C 0.5656(6) 0.6149(3) 0.8135(4) 0.0321(14) Uani 1 1 d . . . . . H2A H 0.617674 0.612117 0.759862 0.039 Uiso 1 1 calc R . . . . H2B H 0.495744 0.663543 0.805113 0.039 Uiso 1 1 calc R . . . . C3 C 0.6930(7) 0.6234(3) 0.9032(4) 0.0367(14) Uani 1 1 d . . . . . H3A H 0.641122 0.631291 0.956311 0.044 Uiso 1 1 calc R . . . . H3B H 0.759706 0.671786 0.899149 0.044 Uiso 1 1 calc R . . . . C4 C 0.7986(7) 0.5481(4) 0.9203(4) 0.0367(15) Uani 1 1 d . . . . . H4A H 0.860054 0.544193 0.870931 0.044 Uiso 1 1 calc R . . . . H4B H 0.876196 0.553631 0.981108 0.044 Uiso 1 1 calc R . . . . C5 C 0.7027(7) 0.4706(4) 0.9207(4) 0.0322(14) Uani 1 1 d . . . . . H5A H 0.653357 0.470985 0.975499 0.039 Uiso 1 1 calc R . . . . H5B H 0.775556 0.423223 0.926846 0.039 Uiso 1 1 calc R . . . . C6 C 0.5718(7) 0.4618(4) 0.8317(4) 0.0324(13) Uani 1 1 d . . . . . H6A H 0.506118 0.413250 0.836961 0.039 Uiso 1 1 calc R . . . . H6B H 0.621585 0.453685 0.777844 0.039 Uiso 1 1 calc R . . . . C7 C 0.1963(6) 0.4347(3) 0.7255(3) 0.0258(12) Uani 1 1 d . . . . . H7 H 0.269798 0.388549 0.720597 0.031 Uiso 1 1 calc R . . . . C8 C 0.1544(7) 0.4253(3) 0.8222(4) 0.0305(13) Uani 1 1 d . . . . . H8A H 0.253435 0.429705 0.871940 0.037 Uiso 1 1 calc R . . . . H8B H 0.081583 0.469834 0.831115 0.037 Uiso 1 1 calc R . . . . C9 C 0.0743(7) 0.3436(3) 0.8304(4) 0.0338(14) Uani 1 1 d . . . . . H9A H 0.151749 0.299224 0.829093 0.041 Uiso 1 1 calc R . . . . H9B H 0.041949 0.340978 0.890846 0.041 Uiso 1 1 calc R . . . . C10 C -0.0719(7) 0.3319(3) 0.7510(4) 0.0351(15) Uani 1 1 d . . . . . H10A H -0.153553 0.373177 0.756201 0.042 Uiso 1 1 calc R . . . . H10B H -0.118476 0.277536 0.756658 0.042 Uiso 1 1 calc R . . . . C11 C -0.0311(7) 0.3393(3) 0.6555(4) 0.0340(14) Uani 1 1 d . . . . . H11A H -0.129968 0.334205 0.605621 0.041 Uiso 1 1 calc R . . . . H11B H 0.042645 0.294931 0.647364 0.041 Uiso 1 1 calc R . . . . C12 C 0.0477(6) 0.4216(3) 0.6476(4) 0.0305(13) Uani 1 1 d . . . . . H12A H 0.077827 0.424952 0.586470 0.037 Uiso 1 1 calc R . . . . H12B H -0.030428 0.465466 0.649829 0.037 Uiso 1 1 calc R . . . . C13 C 0.1827(6) 0.6190(3) 0.6943(3) 0.0232(12) Uani 1 1 d . . . . . H13 H 0.260084 0.665237 0.700096 0.028 Uiso 1 1 calc R . . . . C14 C 0.0862(6) 0.6342(3) 0.7688(3) 0.0265(13) Uani 1 1 d . . . . . H14A H 0.006661 0.590171 0.766431 0.032 Uiso 1 1 calc R . . . . H14B H 0.159036 0.633683 0.831557 0.032 Uiso 1 1 calc R . . . . C15 C -0.0002(7) 0.7162(3) 0.7526(4) 0.0374(15) Uani 1 1 d . . . . . H15A H -0.067525 0.723149 0.798684 0.045 Uiso 1 1 calc R . . . . H15B H 0.079755 0.760614 0.762233 0.045 Uiso 1 1 calc R . . . . C16 C -0.1054(6) 0.7217(3) 0.6538(3) 0.0282(13) Uani 1 1 d . . . . . H16A H -0.191717 0.680588 0.646338 0.034 Uiso 1 1 calc R . . . . H16B H -0.156147 0.776099 0.644596 0.034 Uiso 1 1 calc R . . . . C17 C -0.0100(6) 0.7079(3) 0.5803(4) 0.0301(13) Uani 1 1 d . . . . . H17A H 0.070141 0.751845 0.583751 0.036 Uiso 1 1 calc R . . . . H17B H -0.082471 0.709483 0.517422 0.036 Uiso 1 1 calc R . . . . C18 C 0.0753(6) 0.6255(3) 0.5952(3) 0.0292(13) Uani 1 1 d . . . . . H18A H 0.141468 0.618615 0.548583 0.035 Uiso 1 1 calc R . . . . H18B H -0.005417 0.581431 0.585651 0.035 Uiso 1 1 calc R . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.01766(14) 0.01936(15) 0.01966(14) -0.00010(13) 0.00711(10) 0.00139(14) P1 0.0240(7) 0.0186(7) 0.0208(7) 0.0003(5) 0.0104(6) 0.0000(6) O1 0.0130(16) 0.034(2) 0.0207(18) -0.0001(17) -0.0062(13) 0.0014(17) O2 0.029(2) 0.024(2) 0.028(2) -0.0002(15) 0.0115(16) 0.0049(15) O3 0.047(3) 0.023(2) 0.032(2) 0.0007(17) 0.0202(19) 0.0054(18) O4 0.037(2) 0.028(2) 0.031(2) -0.0021(18) 0.0171(19) -0.0011(19) O5 0.056(3) 0.020(2) 0.044(2) 0.0000(19) 0.017(2) 0.001(2) N1 0.033(3) 0.028(3) 0.025(3) 0.001(2) 0.007(2) 0.002(2) C1 0.028(3) 0.021(3) 0.025(3) 0.002(2) 0.011(2) 0.000(3) C2 0.030(3) 0.025(3) 0.041(3) 0.006(3) 0.007(3) -0.005(3) C3 0.034(4) 0.035(4) 0.038(3) 0.001(3) 0.002(3) -0.005(3) C4 0.027(3) 0.054(4) 0.028(3) 0.000(3) 0.006(3) -0.002(3) C5 0.036(3) 0.034(3) 0.026(3) 0.003(2) 0.006(3) 0.008(3) C6 0.035(4) 0.026(3) 0.036(3) 0.004(3) 0.008(3) 0.005(3) C7 0.036(3) 0.013(3) 0.030(3) 0.000(2) 0.011(3) -0.001(2) C8 0.039(4) 0.022(3) 0.034(3) 0.004(2) 0.016(3) -0.006(3) C9 0.046(4) 0.022(3) 0.039(3) 0.004(3) 0.021(3) -0.001(3) C10 0.039(4) 0.018(3) 0.056(4) -0.002(3) 0.027(3) -0.005(3) C11 0.037(4) 0.023(3) 0.045(4) -0.007(3) 0.015(3) -0.014(3) C12 0.028(3) 0.028(3) 0.035(3) 0.002(3) 0.006(3) -0.007(3) C13 0.022(3) 0.022(3) 0.027(3) 0.001(2) 0.008(2) 0.002(2) C14 0.032(3) 0.024(3) 0.025(3) -0.002(2) 0.008(2) 0.004(3) C15 0.047(4) 0.029(4) 0.039(3) -0.007(3) 0.017(3) 0.010(3) C16 0.026(3) 0.023(3) 0.036(3) 0.003(2) 0.008(2) 0.006(2) C17 0.030(3) 0.024(3) 0.035(3) 0.003(3) 0.005(3) 0.003(3) C18 0.036(3) 0.024(3) 0.033(3) 0.001(2) 0.017(3) 0.008(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' N N 0.0061 0.0033 '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 O1 U1 O1 180.0 3_666 . ? O1 U1 O2 88.76(15) . 3_666 ? O1 U1 O2 91.24(15) . . ? O1 U1 O2 91.24(15) 3_666 3_666 ? O1 U1 O2 88.76(15) 3_666 . ? O1 U1 O3 91.57(14) 3_666 . ? O1 U1 O3 91.57(14) . 3_666 ? O1 U1 O3 88.43(14) . . ? O1 U1 O3 88.43(14) 3_666 3_666 ? O1 U1 O4 89.86(13) 3_666 . ? O1 U1 O4 89.85(13) . 3_666 ? O1 U1 O4 90.14(13) 3_666 3_666 ? O1 U1 O4 90.15(13) . . ? O2 U1 O2 180.0 3_666 . ? O2 U1 O3 115.24(11) 3_666 . ? O2 U1 O3 115.24(11) . 3_666 ? O2 U1 O3 64.76(11) . . ? O2 U1 O3 64.76(11) 3_666 3_666 ? O2 U1 O4 65.61(11) . 3_666 ? O2 U1 O4 114.39(11) 3_666 3_666 ? O2 U1 O4 65.61(11) 3_666 . ? O2 U1 O4 114.39(11) . . ? O3 U1 O3 180.00(9) . 3_666 ? O3 U1 O4 130.28(12) 3_666 . ? O3 U1 O4 49.72(12) . . ? O3 U1 O4 130.28(12) . 3_666 ? O3 U1 O4 49.72(12) 3_666 3_666 ? O4 U1 O4 180.0 . 3_666 ? O2 P1 C1 111.0(2) . . ? O2 P1 C7 108.9(2) . . ? O2 P1 C13 108.2(2) . . ? C1 P1 C7 106.3(2) . . ? C1 P1 C13 108.3(2) . . ? C7 P1 C13 114.2(3) . . ? P1 O2 U1 175.8(2) . . ? N1 O3 U1 98.2(3) . . ? N1 O4 U1 97.9(3) . . ? O4 N1 O3 114.1(5) . . ? O5 N1 O3 122.0(5) . . ? O5 N1 O4 123.9(5) . . ? C2 C1 P1 113.3(4) . . ? C2 C1 C6 109.6(5) . . ? C6 C1 P1 111.3(4) . . ? C3 C2 C1 111.7(4) . . ? C2 C3 C4 110.7(5) . . ? C5 C4 C3 112.4(5) . . ? C4 C5 C6 111.7(5) . . ? C5 C6 C1 111.5(5) . . ? C8 C7 P1 115.7(4) . . ? C12 C7 P1 112.7(4) . . ? C12 C7 C8 110.3(5) . . ? C9 C8 C7 111.2(4) . . ? C10 C9 C8 111.1(5) . . ? C9 C10 C11 112.0(5) . . ? C10 C11 C12 109.7(4) . . ? C7 C12 C11 112.2(5) . . ? C14 C13 P1 115.8(4) . . ? C14 C13 C18 111.0(4) . . ? C18 C13 P1 112.1(3) . . ? C15 C14 C13 110.7(4) . . ? C16 C15 C14 111.1(4) . . ? C17 C16 C15 111.8(4) . . ? C16 C17 C18 110.4(4) . . ? C17 C18 C13 111.2(4) . . ? 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 O1 1.768(3) 3_666 ? U1 O1 1.768(3) . ? U1 O2 2.336(4) 3_666 ? U1 O2 2.336(4) . ? U1 O3 2.541(4) . ? U1 O3 2.541(4) 3_666 ? U1 O4 2.552(4) . ? U1 O4 2.552(4) 3_666 ? P1 O2 1.512(4) . ? P1 C1 1.812(5) . ? P1 C7 1.818(5) . ? P1 C13 1.831(5) . ? O3 N1 1.279(5) . ? O4 N1 1.272(6) . ? O5 N1 1.220(6) . ? C1 C2 1.546(7) . ? C1 C6 1.551(8) . ? C2 C3 1.516(7) . ? C3 C4 1.521(8) . ? C4 C5 1.517(9) . ? C5 C6 1.525(7) . ? C7 C8 1.548(6) . ? C7 C12 1.523(7) . ? C8 C9 1.525(7) . ? C9 C10 1.519(8) . ? C10 C11 1.526(7) . ? C11 C12 1.529(7) . ? C13 C14 1.534(6) . ? C13 C18 1.541(7) . ? C14 C15 1.530(7) . ? C15 C16 1.529(7) . ? C16 C17 1.512(7) . ? C17 C18 1.531(7) . ? 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 0.5063 16612 11874 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 2 0.4937 0 11874 nmt -0.9991 0.0001 0.0002 0.4414 -0.1400 1.1389 0.4419 0.8618 0.1395