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_7130998
_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         'C30 H38 K P2 U, C6 H6'
_chemical_formula_sum            'C36 H44 K P2 U'
_chemical_formula_weight         815.78
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-08-11
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-08-22 deposited with the CCDC.	2022-10-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.4180(6)
_cell_length_b                   15.1866(5)
_cell_length_c                   9.8667(2)
_cell_measurement_reflns_used    15614
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      33.2050
_cell_measurement_theta_min      1.7570
_cell_volume                     3508.99(16)
_computing_cell_refinement       'CrysAlisPro 1.171.42.64a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.64a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.64a (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_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -66.02 136.98   0.50    3.00    --  -28.53  73.75  -6.13  406
  2  \w    -66.02 136.98   0.50    3.00    --  -28.53  73.75 -62.52  406
  3  \w     86.98 136.98   0.50    3.00    --  -28.53  73.75-143.02  100
;
_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      -0.0096597000
_diffrn_orient_matrix_UB_12      -0.0266521000
_diffrn_orient_matrix_UB_13      0.0543470000
_diffrn_orient_matrix_UB_21      -0.0106060000
_diffrn_orient_matrix_UB_22      -0.0313254000
_diffrn_orient_matrix_UB_23      -0.0470255000
_diffrn_orient_matrix_UB_31      0.0266642000
_diffrn_orient_matrix_UB_32      -0.0221833000
_diffrn_orient_matrix_UB_33      0.0010198000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            29124
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.680
_diffrn_reflns_theta_min         2.240
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.857
_exptl_absorpt_correction_T_max  0.19548
_exptl_absorpt_correction_T_min  0.15921
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.64a (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 brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_description       block
_exptl_crystal_F_000             1604
_exptl_crystal_preparation       'By CAPG.'
_exptl_crystal_recrystallization_method 'From C6H6.'
_exptl_crystal_size_max          0.125
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.122
_exptl_crystal_size_rad          0.400
_refine_diff_density_max         1.757
_refine_diff_density_min         -0.819
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         3456
_refine_ls_number_restraints     409
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0245
_refine_ls_R_factor_gt           0.0231
_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^)+(0.0320P)^2^+0.7285P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0552
_refine_ls_wR_factor_ref         0.0561
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3300
_reflns_number_total             3456
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04803e2.cif
_cod_data_source_block           ms0702
_cod_original_cell_volume        3508.99(17)
_cod_database_code               7130998
_manchester_internal_validation_user GFSW
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         U(PC8H12)2(C7H7)2(C7H8)K
_shelx_estimated_absorpt_t_max   0.589
_shelx_estimated_absorpt_t_min   0.582
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C17-C18 \\sim C18-C19 \\sim C19-C20 \\sim C20-C21 \\sim C21-C22 \\sim C17-C22
\\sim C10-C11 \\sim C12-C11
 \\sim C13-C12 \\sim C14-C13 \\sim C15-C14 \\sim C10-C15
 with sigma of 0.02
 C17-C21 \\sim C18-C22 \\sim C20-C22 \\sim C19-C21 \\sim C18-C20 \\sim C17-C19
\\sim C10-C14 \\sim C15-C13
 \\sim C14-C12 \\sim C13-C11 \\sim C10-C12 \\sim C15-C11
 with sigma of 0.02
 C10-C9 \\sim C17-C16
 with sigma of 0.02
 C27-C23 \\sim C28-C24 \\sim C25-C23 \\sim C24-C26 \\sim C25-C27 \\sim C28-C26
 with sigma of 0.02
 C28-C23 \\sim C24-C23 \\sim C25-C24 \\sim C25-C26 \\sim C27-C26 \\sim C28-C27
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C23 \\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim C28: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim
C17 \\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 C23, C24, C25, C26, C27, C28
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C9, C10, C11, C12, C13, C14, C15, C16, C17, C18, C19, C20, C21, C22
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C9(0.5) H9A(0.5) H9B(0.5) C10(0.5) C11(0.5) H11(0.5) C12(0.5)
 H12(0.5) C13(0.5) H13(0.5) C14(0.5) H14(0.5) C15(0.5) H15(0.5) C16(0.5)
 H16A(0.5) H16B(0.5) C17(0.5) C18(0.5) H18(0.5) C19(0.5) H19(0.5) C20(0.5)
 H20(0.5) C21(0.5) H21(0.5) C22(0.5) H22(0.5) C23(0.5) H23(0.5) C24(0.5)
 H24(0.5) C25(0.5) H25(0.5) C26(0.5) H26(0.5) C27(0.5) H27(0.5) C28(0.5)
 H28(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C16(H16A,H16B)
6.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C18(H18), C19(H19),
 C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27),
  C28(H28)
6.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              65679
_shelx_hkl_checksum              5919
_olex2_date_sample_completion    2021-07-10
_olex2_date_sample_data_collection 2021-07-10
_olex2_date_sample_submission    2021-07-10
_olex2_exptl_crystal_mounting_method
'From a glass microfibre into a quartz capillary, then sealed at both ends using capillary wax. The outside was then coated with Hard As Nails(TM) clear polish to provide shatter resistance.'
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.320
_oxdiff_exptl_absorpt_empirical_full_min 0.474