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_7130995
_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 Ce K P2, C7 H8'
_chemical_formula_sum            'C37 H46 Ce K P2'
_chemical_formula_weight         731.90
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.4368(2)
_cell_length_b                   10.04890(10)
_cell_length_c                   14.85740(10)
_cell_measurement_reflns_used    25897
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      75.5360
_cell_measurement_theta_min      2.9830
_cell_volume                     3499.13(5)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_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    -84.00 -57.00   0.50    1.00    --    5.00 -11.00-170.00   54
  2  \w    -64.00  18.00   0.50    1.00    --  -44.02 -11.00-170.00  164
  3  \w    -94.00 -62.00   0.50    2.00    -- -107.20  11.00   2.00   64
  4  \w    -53.00 -18.00   0.50    2.00    -- -107.20  11.00   2.00   70
  5  \w   -123.00 -97.00   0.50    2.00    -- -107.20  11.00   2.00   52
  6  \w    -26.00  44.00   0.50    1.00    --    5.00  57.00-180.00  140
  7  \w    -75.00  31.00   0.50    1.00    --  -44.02  57.00  60.00  212
  8  \w    -74.00  26.00   0.50    1.00    --  -44.02  57.00-180.00  200
  9  \w    -71.00 -46.00   0.50    1.00    --  -46.18 -11.00-170.00   50
 10  \w    -74.00 -23.00   0.50    2.00    -- -107.20  76.00 -30.00  102
 11  \w    -88.00 -19.00   0.50    2.00    -- -107.20  76.00  30.00  138
 12  \w   -125.00 -97.00   0.50    2.00    -- -107.20  72.00 160.86   56
 13  \w   -148.00 -18.00   0.50    2.00    -- -107.20  37.00 -30.00  260
 14  \w   -127.00-101.00   0.50    2.00    -- -107.20  76.00 -30.00   52
 15  \w    -72.00 -19.00   0.50    2.00    -- -107.20  76.00 120.00  106
 16  \w   -147.00 -77.00   0.50    2.00    -- -107.20  37.00 150.00  140
 17  \w    -43.00 -18.00   0.50    2.00    -- -107.20  37.00 150.00   50
 18  \w   -145.00 -19.00   0.50    2.00    -- -107.20  76.00 150.00  252
 19  \w   -140.00-114.00   0.50    2.00    -- -107.20  57.00 120.00   52
 20  \w    -44.00 -19.00   0.50    2.00    -- -107.20  76.00-150.00   50
 21  \w    -49.00 -19.00   0.50    2.00    -- -107.20  76.00-120.00   60
 22  \w   -145.00 -81.00   0.50    2.00    -- -107.20  76.00-150.00  128
 23  \w   -174.00-148.00   0.50    2.00    -- -107.20 -57.00 120.00   52
 24  \w   -102.00 -76.00   0.50    2.00    -- -107.20 -57.00 120.00   52
 25  \w    -68.00 -25.00   0.50    2.00    -- -107.20  57.00 120.00   86
 26  \w    -53.00 -22.00   0.50    2.00    -- -107.20  72.00 160.86   62
 27  \w   -133.00-108.00   0.50    2.00    -- -107.20  57.00-180.00   50
 28  \w   -117.00 -92.00   0.50    2.00    -- -107.20  76.00  90.00   50
 29  \w   -193.00-127.00   0.50    2.00    -- -107.20 -11.00-170.00  132
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            32686
_diffrn_reflns_point_group_measured_fraction_full 0.799
_diffrn_reflns_point_group_measured_fraction_max 0.774
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.806
_diffrn_reflns_theta_min         3.772
_exptl_absorpt_coefficient_mu    12.142
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.06135
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.54a (Rigaku Oxford Diffraction, 2022)
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    1.389
_exptl_crystal_description       block
_exptl_crystal_F_000             1500
_exptl_crystal_preparation       'By MC.'
_exptl_crystal_recrystallization_method 'From toluene.'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.168
_exptl_crystal_size_min          0.13
_refine_diff_density_max         2.036
_refine_diff_density_min         -1.411
_refine_diff_density_rms         0.157
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.282(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.174
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         5642
_refine_ls_number_restraints     321
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0429
_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^)+(0.1147P)^2^+2.7710P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1509
_refine_ls_wR_factor_ref         0.1511
_reflns_Friedel_coverage         0.505
_reflns_Friedel_fraction_full    0.580
_reflns_Friedel_fraction_max     0.541
_reflns_number_gt                5580
_reflns_number_total             5642
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.8778\% 
around [0.01 0.06 1.00] (reciprocal) or [0.00 0.14 0.99] (direct)
;
_cod_data_source_file            d2cc04803e2.cif
_cod_data_source_block           rcapg3
_cod_database_code               7130995
_manchester_internal_validation_user GFSW
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.301
_shelx_estimated_absorpt_t_min   0.151
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.71827
 0.28173
2. Restrained distances
 C31A-C32A
 1.54 with sigma of 0.02
 C31B-C32B
 1.54 with sigma of 0.02
 C17-C18
 1.43 with sigma of 0.02
 C24-C25
 1.54 with sigma of 0.02
 C37A-C31A \\sim C31A-C33A
 with sigma of 0.02
 C37B-C31B \\sim C31B-C33B
 with sigma of 0.02
 C23-C17 \\sim C17-C19
 with sigma of 0.02
 C30-C24 \\sim C24-C26
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C31A \\sim C32A \\sim C37A \\sim C36A \\sim C35A \\sim C34A \\sim C33A \\sim
C31B \\sim C32B \\sim C37B \\sim C36B \\sim C35B \\sim C34B \\sim C33B: within
2A with sigma of 0.02 and sigma for terminal atoms of 0.02 within 2A
4. Rigid body (RIGU) restrains
 C31A, C32A, C37A, C36A, C35A, C34A, C33A, C31B, C32B, C37B, C36B, C35B, C34B,
 C33B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Sof(C31B)=Sof(H31D)=Sof(H31E)=Sof(H31F)=Sof(C32B)=Sof(C37B)=Sof(H37B)=
 Sof(C36B)=Sof(H36B)=Sof(C35B)=Sof(H35B)=Sof(C34B)=Sof(H34B)=Sof(C33B)=
 Sof(H33B)=1-FVAR(1)
 Sof(C31A)=Sof(H31A)=Sof(H31B)=Sof(H31C)=Sof(C32A)=Sof(C37A)=Sof(H37A)=
 Sof(C36A)=Sof(H36A)=Sof(C35A)=Sof(H35A)=Sof(C34A)=Sof(H34A)=Sof(C33A)=
 Sof(H33A)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C24(H24A,H24B)
6.b Aromatic/amide H refined with riding coordinates:
 C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C30(H30), C29(H29),
 C28(H28), C27(H27), C26(H26), C37A(H37A), C36A(H36A), C35A(H35A), C34A(H34A),
 C33A(H33A), C37B(H37B), C36B(H36B), C35B(H35B), C34B(H34B), C33B(H33B)
6.c Fitted hexagon refined as free rotating group:
 C18(C19,C20,C21,C22,C23), C25(C30,C29,C28,C27,C26), C32A(C37A,C36A,C35A,C34A,
 C33A), C32B(C37B,C36B,C35B,C34B,C33B)
6.d 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),
 C31A(H31A,H31B,H31C), C31B(H31D,H31E,H31F)
;
_shelx_res_checksum              64037
_shelx_hkl_checksum              54972
_olex2_exptl_crystal_mounting_method
'From fomblin 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
;