Isostructural σ-hydrocarbyl phospholide complexes of uranium, neptunium, and plutonium
Černá, Michaela; Seed, John A.; Garrido Fernandez, Sara; Janicke, Michael T.; Scott, Brian L.; Whitehead, George F. S.; Gaunt, Andrew J.; Goodwin, Conrad A. P.; Chemical Communications  (2022) –; doi:10.1039/D2CC04803E

data_7130989
_publ_section_title
;
 Isostructural \s-hydrocarbyl phospholide complexes of uranium, neptunium,
 and plutonium
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC04803E
_journal_year                    2022
_chemical_formula_moiety         'C20 H32 I O P2 U'
_chemical_formula_sum            'C20 H32 I O P2 U'
_chemical_formula_weight         715.32
_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             2022-07-25
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-07-28 deposited with the CCDC.	2022-10-28 downloaded from the CCDC.
;
_cell_angle_alpha                99.655(7)
_cell_angle_beta                 96.384(6)
_cell_angle_gamma                99.298(6)
_cell_formula_units_Z            4
_cell_length_a                   11.6875(8)
_cell_length_b                   13.1727(11)
_cell_length_c                   15.8575(14)
_cell_measurement_reflns_used    7994
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      29.8820
_cell_measurement_theta_min      2.1220
_cell_volume                     2351.0(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.54a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.54a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.54a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.981
_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      2.24 185.24   0.50   10.00    --   28.00  73.78 -25.76  366
  2  \w      2.24 185.24   0.50   10.00    --   28.00  73.78  64.24  366
  3  \w      2.24 185.24   0.50   10.00    --   28.00  73.78 154.24  366
  4  \w      2.24 185.24   0.50   10.00    --   28.00  73.78-115.76  366
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_unetI/netI     0.0567
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            29950
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         2.163
_exptl_absorpt_coefficient_mu    8.359
_exptl_absorpt_correction_T_max  0.32605
_exptl_absorpt_correction_T_min  0.30182
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.54a (Rigaku Oxford Diffraction, 2022)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.021
_exptl_crystal_description       block
_exptl_crystal_F_000             1340
_exptl_crystal_preparation       'By CAPG.'
_exptl_crystal_recrystallization_method 'From THF.'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_exptl_crystal_size_rad          0.400
_refine_diff_density_max         1.452
_refine_diff_density_min         -0.748
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     486
_refine_ls_number_reflns         9440
_refine_ls_number_restraints     111
_refine_ls_restrained_S_all      0.958
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0264
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0126P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0540
_refine_ls_wR_factor_ref         0.0576
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7936
_reflns_number_total             9440
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04803e2.cif
_cod_data_source_block           dq0844
_cod_database_code               7130989
_manchester_internal_validation_user GFSW
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.489
_shelx_estimated_absorpt_t_min   0.315
_olex2_refinement_description
;
1. Restrained distances
 C39A-C37 \\sim C39B-C37 \\sim C38A-C40 \\sim C38B-C40
 with sigma of 0.02
 C39A-C40 \\sim C39B-C40 \\sim C38B-C39B \\sim C39A-C38A \\sim C38A-C37 \\sim
C38B-C37
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
C37 \\sim C40 \\sim C38A \\sim C39A: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C37 \\sim C40 \\sim C38A \\sim C39A \\sim C38B \\sim C39B: within 2A with sigma
of 0.02 and sigma for terminal atoms of 0.04 within 2A
3. Rigid body (RIGU) restrains
 C37, C40, C38A, C39A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C37, C40, C38A, C39A, C38B, C39B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Others
 Sof(H37C)=Sof(H37D)=Sof(H40C)=Sof(H40D)=Sof(C38B)=Sof(H38C)=Sof(H38D)=
 Sof(C39B)=Sof(H39C)=Sof(H39D)=1-FVAR(1)
 Sof(H37A)=Sof(H37B)=Sof(H40A)=Sof(H40B)=Sof(C38A)=Sof(H38A)=Sof(H38B)=
 Sof(C39A)=Sof(H39A)=Sof(H39B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C37(H37A,
 H37B), C37(H37C,H37D), C40(H40A,H40B), C40(H40C,H40D), C38A(H38A,H38B),
 C39A(H39A,H39B), C38B(H38C,H38D), C39B(H39C,H39D)
5.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C13(H13A,
 H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C),
 C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,
 H28C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,
 H36B,H36C)
;
_shelx_res_checksum              13124
_shelx_hkl_checksum              69345
_olex2_exptl_crystal_mounting_method
'From Paratone-N on a microscope slide, on to 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
;