Synthesis, characterization, and theoretical analysis of a plutonyl phosphine oxide complex
Windorff, Cory James; Beltrán Leiva, María Joaquina; Albrecht-Schmitt, Thomas E.; Bai, Zhuanling; Celis-Barros, Cristian; Goodwin, Conrad Alexander Phillip; Huffman, Zachary; McKinnon, Noah C.; Sperling, Joseph M.; Dalton Transactions  (2021) –; doi:10.1039/D1DT03041H

data_7708505
_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_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_checksum              17983
_olex2_exptl_crystal_mounting_method 'nylon loop'
_olex2_submission_original_sample_id cjw95
_olex2_submission_special_instructions 'No special instructions were received'