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_7130992
_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 La K P2, C7 H8'
_chemical_formula_sum            'C37 H46 K La P2'
_chemical_formula_weight         730.69
_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
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.4224(2)
_cell_length_b                   10.06770(10)
_cell_length_c                   14.90600(10)
_cell_measurement_reflns_used    21340
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      79.1500
_cell_measurement_theta_min      3.5530
_cell_volume                     3514.98(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_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_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    -35.00  27.00   0.50    1.00    --  -47.67  30.00 -38.00  124
  2  \w   -106.00 -51.00   0.50    1.00    --  -47.67 -30.00 160.00  110
  3  \w    -20.00   6.00   0.50    1.00    --   47.67 -30.00 160.00   52
  4  \w     62.00 105.00   0.50    1.00    --   47.67  30.00 -38.00   86
  5  \w   -147.00-122.00   0.50    2.00    --  -91.75 -30.00 160.00   50
  6  \w    101.00 169.00   0.50    2.00    --  113.25  30.00 -38.00  136
  7  \w   -119.00 -74.00   0.50    1.00    --  -47.67-125.00-120.00   90
  8  \w    -16.00  28.00   0.50    1.00    --  -47.67  19.00  90.00   88
  9  \w     52.00  78.00   0.50    1.00    --   47.67-125.00   0.00   52
 10  \w    -51.00 -26.00   0.50    2.00    --  -91.75  45.00  60.00   50
 11  \w    -51.00 -20.00   0.50    2.00    --  -91.75  61.00 120.00   62
 12  \w    -48.00 -23.00   0.50    2.00    --  -91.75  45.00-180.00   50
 13  \w     42.00  67.00   0.50    2.00    --  113.25 -61.00  30.00   50
 14  \w     42.00  70.00   0.50    2.00    --  113.25 -61.00-150.00   56
 15  \w     43.00  69.00   0.50    2.00    --  113.25 -61.00-180.00   52
 16  \w    101.00 148.00   0.50    2.00    --  113.25  15.00  90.00   94
 17  \w    153.00 178.00   0.50    2.00    --  113.25  15.00  90.00   50
 18  \w     95.00 121.00   0.50    2.00    --  113.25 125.00-150.00   52
 19  \w     42.00  68.00   0.50    2.00    --  113.25 -61.00 120.00   52
 20  \w     59.00  96.00   0.50    2.00    --  113.25 -77.00  30.00   74
 21  \w     60.00 104.00   0.50    2.00    --  113.25 -94.00   0.00   88
 22  \w     42.00  67.00   0.50    2.00    --  113.25 -61.00 -60.00   50
 23  \w    110.00 176.00   0.50    2.00    --  113.25  30.00-180.00  132
 24  \w     46.00  86.00   0.50    2.00    --  113.25-125.00 150.00   80
 25  \w     43.00  68.00   0.50    2.00    --  113.25 -61.00  60.00   50
 26  \w    116.00 174.00   0.50    2.00    --  113.25  30.00 -90.00  116
 27  \w     46.00  75.00   0.50    2.00    --  113.25 -77.00  60.00   58
 28  \w     42.00 104.00   0.50    2.00    --  113.25 -77.00   0.00  124
 29  \w    108.00 143.00   0.50    2.00    --  113.25  45.00-150.00   70
 30  \w    108.00 178.00   0.50    2.00    --  113.25  45.00  30.00  140
 31  \w     42.00  67.00   0.50    2.00    --  113.25 -61.00 150.00   50
 32  \w    135.00 175.00   0.50    2.00    --  113.25 125.00-150.00   80
 33  \w     46.00  71.00   0.50    2.00    --  113.25 -61.00   0.00   50
 34  \w     66.00  92.00   0.50    2.00    --  113.25 -77.00-120.00   52
 35  \w     44.00  70.00   0.50    2.00    --  113.25-125.00-180.00   52
 36  \w     42.00  67.00   0.50    2.00    --  113.25 -61.00 -30.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            29350
_diffrn_reflns_point_group_measured_fraction_full 0.869
_diffrn_reflns_point_group_measured_fraction_max 0.844
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.004
_diffrn_reflns_theta_min         3.774
_exptl_absorpt_coefficient_mu    11.473
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49114
_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    1.381
_exptl_crystal_description       block
_exptl_crystal_F_000             1496
_exptl_crystal_preparation       'By MC.'
_exptl_crystal_recrystallization_method 'From toluene.'
_exptl_crystal_size_max          0.197
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.071
_refine_diff_density_max         1.024
_refine_diff_density_min         -1.287
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.341(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         6468
_refine_ls_number_restraints     385
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0363
_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^)+(0.0575P)^2^+4.4052P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0982
_refine_ls_wR_factor_ref         0.0988
_reflns_Friedel_coverage         0.634
_reflns_Friedel_fraction_full    0.726
_reflns_Friedel_fraction_max     0.682
_reflns_number_gt                6294
_reflns_number_total             6468
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 47.3338\% 
around [-0.82 -0.57 -0.03] (reciprocal) or [-0.26 -0.97 -0.02] (direct)
;
_cod_data_source_file            d2cc04803e2.cif
_cod_data_source_block           ccapg4
_cod_database_code               7130992
_manchester_internal_validation_user GFSW
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.496
_shelx_estimated_absorpt_t_min   0.211
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.65901
 0.34099
2. Restrained distances
 C36B-C35B \\sim C35B-C34B \\sim C34B-C33B \\sim C33B-C32B \\sim C37B-C32B
\\sim C37B-C36B \\sim C33A-
 C32A \\sim C37A-C32A \\sim C37A-C36A \\sim C36A-C35A \\sim C34A-C35A \\sim
C34A-C33A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C31A \\sim C32A \\sim C33A \\sim C34A \\sim C35A \\sim C36A \\sim C37A \\sim
C31B \\sim C32B \\sim C33B \\sim C34B \\sim C35B \\sim C36B \\sim C37B: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 C31A, C32A, C33A, C34A, C35A, C36A, C37A, C31B, C32B, C33B, C34B, C35B, C36B,
 C37B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C31B)=Sof(H31D)=Sof(H31E)=Sof(H31F)=Sof(C32B)=Sof(C33B)=Sof(H33B)=
 Sof(C34B)=Sof(H34B)=Sof(C35B)=Sof(H35B)=Sof(C36B)=Sof(H36B)=Sof(C37B)=
 Sof(H37B)=1-FVAR(1)
 Sof(C31A)=Sof(H31A)=Sof(H31B)=Sof(H31C)=Sof(C32A)=Sof(C33A)=Sof(H33A)=
 Sof(C34A)=Sof(H34A)=Sof(C35A)=Sof(H35A)=Sof(C36A)=Sof(H36A)=Sof(C37A)=
 Sof(H37A)=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), C26(H26), C27(H27),
 C28(H28), C29(H29), C30(H30), C33A(H33A), C34A(H34A), C35A(H35A), C36A(H36A),
 C37A(H37A), C33B(H33B), C34B(H34B), C35B(H35B), C36B(H36B), C37B(H37B)
6.c 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              96995
_shelx_hkl_checksum              65393
_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
;