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_7708502
_publ_section_title
;
 Synthesis, characterization, and theoretical analysis of a plutonyl
 phosphine oxide complex
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03041H
_journal_year                    2021
_chemical_formula_moiety         'C36 H66 Cl2 O4 P2 Pu'
_chemical_formula_sum            'C36 H66 Cl2 O4 P2 Pu'
_chemical_formula_weight         934.82
_chemical_name_common
'plutonyldichloride bis(tricyclohexylphosphine oxide)'
_chemical_name_systematic
'plutoniumdioxodicholoro bis(tricyclyhexylphosphine oxide)'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-10-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2021-08-04 deposited with the CCDC.	2021-10-01 downloaded from the CCDC.
;
_cell_angle_alpha                69.306(4)
_cell_angle_beta                 89.512(4)
_cell_angle_gamma                76.786(4)
_cell_formula_units_Z            2
_cell_length_a                   8.7416(4)
_cell_length_b                   14.1281(7)
_cell_length_c                   17.1398(8)
_cell_measurement_reflns_used    16651
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.8970
_cell_measurement_theta_min      2.4580
_cell_volume                     1921.72(17)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CMOS
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS detector'
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f    -25.73 334.27   2.00   45.00 138.83 -19.51  73.71    --   180
  2  \f    -25.73 334.27   2.00   45.00 -49.29 -19.51  73.71    --   180
  3  \w    -49.29 136.71   2.00   45.00    --  -19.51  73.71 -25.73   93
  4  \w    -49.29 136.71   2.00   45.00    --  -19.51  73.71  25.27   93
  5  \w    -49.29 136.71   2.00   45.00    --  -19.51  73.71  76.28   93
  6  \w    -49.29 136.71   2.00   45.00    --  -19.51  73.71 127.28   93
  7  \w    -49.29 136.71   2.00   45.00    --  -19.51  73.71 178.27   93
  8  \w    -49.29 136.71   2.00   45.00    --  -19.51  73.71-130.72   93
  9  \w    -49.29 136.71   2.00   45.00    --  -19.51  73.71 -79.73   93
 10  \w    -48.41 139.59   2.00   45.00    --  -18.62  73.71 -52.33   94
 11  \w    -48.41 139.59   2.00   45.00    --  -18.62  73.71 102.98   94
 12  \w     41.59 139.59   2.00   45.00    --  -18.62  73.71-151.57   49
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0221200000
_diffrn_orient_matrix_UB_12      -0.0236819000
_diffrn_orient_matrix_UB_13      -0.0269540000
_diffrn_orient_matrix_UB_21      0.0586159000
_diffrn_orient_matrix_UB_22      -0.0461232000
_diffrn_orient_matrix_UB_23      0.0213500000
_diffrn_orient_matrix_UB_31      -0.0553691000
_diffrn_orient_matrix_UB_32      -0.0192304000
_diffrn_orient_matrix_UB_33      0.0280532000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1237
_diffrn_reflns_av_unetI/netI     0.1075
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            87287
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         1.588
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.973
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71991
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_description       irregular
_exptl_crystal_F_000             944
_exptl_crystal_preparation       'By CJW.'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Methanol/Ethanol'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.231
_refine_diff_density_min         -1.398
_refine_diff_density_rms         0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.877
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         7198
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.877
_refine_ls_R_factor_all          0.0832
_refine_ls_R_factor_gt           0.0399
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0408P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0782
_refine_ls_wR_factor_ref         0.0829
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4109
_reflns_number_total             7198
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 5.7706\% 
 around [0.01 0.31 0.95] (reciprocal) or [-0.01 0.06 1.00] (direct)
Component 3 rotated by 179.0377\% 
 around [0.91 0.40 0.01] (reciprocal) or [1.00 0.04 -0.01] (direct)
;
_cod_data_source_file            d1dt03041h2.cif
_cod_data_source_block           cjw103
_cod_database_code               7708502
_lanl_internal_la-ur             LA-UR-19-30804
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         PuO2Cl2(OPC18H33)2
_shelx_estimated_absorpt_t_max   0.827
_shelx_estimated_absorpt_t_min   0.827
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1), C7(H7), C13(H13), C19(H19), C25(H25), C31(H31)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C8(H8A,H8B),
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C14(H14A,H14B),
 C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C20(H20A,H20B),
  C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C26(H26A,
 H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B),
 C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B)
;
_shelx_res_checksum              21117
_olex2_exptl_crystal_mounting_method
'From paratone on a microscope slide, onto a micromount.'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.349
_oxdiff_exptl_absorpt_empirical_full_min 0.798
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               3