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_7130988
_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         'C16 H28 K O2 P'
_chemical_formula_sum            'C16 H28 K O2 P'
_chemical_formula_weight         322.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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                 101.128(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1277(6)
_cell_length_b                   10.5943(5)
_cell_length_c                   18.8451(10)
_cell_measurement_reflns_used    4986
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      78.7720
_cell_measurement_theta_min      4.6930
_cell_volume                     1788.09(18)
_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      100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.946
_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    -75.00  -1.00   1.00   15.00    --  -47.01 109.00-125.00   74
  2  \w     35.00  86.00   1.00   15.00    --   47.01-109.00 137.00   51
  3  \w   -147.00 -86.00   1.00   30.00    --  -91.75-109.00 137.00   61
  4  \w    -55.00 -30.00   1.00   30.00    --  -91.75 109.00-125.00   25
  5  \w     72.00 107.00   1.00   30.00    --  113.25-109.00 137.00   35
  6  \w    104.00 169.00   1.00   30.00    --  113.25 109.00-125.00   65
  7  \w    -26.00  29.00   1.00   15.00    --  -47.01  19.00 150.00   55
  8  \w   -119.00 -73.00   1.00   15.00    --  -47.01-125.00 -60.00   46
  9  \w    -26.00  29.00   1.00   15.00    --  -47.01  19.00  30.00   55
 10  \w     42.00  71.00   1.00   30.00    --  113.25 -61.00 -30.00   29
 11  \w    101.00 170.00   1.00   30.00    --  113.25  15.00 -30.00   69
 12  \w     42.00 106.00   1.00   30.00    --  113.25 -94.00-120.00   64
 13  \w     43.00 105.00   1.00   30.00    --  113.25 -94.00 150.00   62
 14  \w     99.00 175.00   1.00   30.00    --  113.25  61.00 150.00   76
 15  \w     99.00 172.00   1.00   30.00    --  113.25  61.00 120.00   73
 16  \w     97.00 125.00   1.00   30.00    --  113.25  61.00 -90.00   28
 17  \w    134.00 173.00   1.00   30.00    --  113.25  61.00 -90.00   39
 18  \w     43.00 106.00   1.00   30.00    --  113.25 -77.00 -60.00   63
 19  \w     44.00  71.00   1.00   30.00    --  113.25 -61.00 -60.00   27
 20  \w     46.00 106.00   1.00   30.00    --  113.25 -94.00-180.00   60
 21  \w     42.00  71.00   1.00   30.00    --  113.25 -61.00 -90.00   29
;
_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  0.0615
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            6337
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.362
_diffrn_reflns_theta_min         4.783
_exptl_absorpt_coefficient_mu    3.433
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83460
_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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_description       block
_exptl_crystal_F_000             696
_exptl_crystal_preparation       'By MC.'
_exptl_crystal_recrystallization_method 'From THF.'
_exptl_crystal_size_max          0.256
_exptl_crystal_size_mid          0.254
_exptl_crystal_size_min          0.121
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         6337
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0582
_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^)+(0.0785P)^2^+2.0148P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1574
_refine_ls_wR_factor_ref         0.1648
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5513
_reflns_number_total             6337
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.8391\% 
around [0.71 0.00 -0.71] (reciprocal) or [0.99 -0.00 -0.15] (direct)
;
_cod_data_source_file            d2cc04803e2.cif
_cod_data_source_block           ccapg2
_cod_database_code               7130988
_manchester_internal_validation_user GFSW
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.681
_shelx_estimated_absorpt_t_min   0.474
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.50368
 0.49632
2.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B),
 C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B)
2.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              15835
_shelx_hkl_checksum              24579
_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
;