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_7130994
_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 Np P2, C7 H8'
_chemical_formula_sum            'C37 H46 K Np P2'
_chemical_formula_weight         828.78
_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                   23.4277(12)
_cell_length_b                   10.0191(4)
_cell_length_c                   14.8503(6)
_cell_measurement_reflns_used    5755
_cell_measurement_temperature    119(5)
_cell_measurement_theta_max      27.6380
_cell_measurement_theta_min      2.1930
_cell_volume                     3485.7(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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      119(5)
_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    -60.56 142.44   0.50   40.00    --  -23.06  73.75-160.74  406
  2  \f    227.75 297.75   0.50   40.00 142.92 -23.03  73.75    --   140
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0600
_diffrn_reflns_av_unetI/netI     0.0755
_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       -26
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18677
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.677
_diffrn_reflns_theta_min         2.211
_exptl_absorpt_coefficient_mu    3.216
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.28674
_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 green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_description       plate
_exptl_crystal_F_000             1640
_exptl_crystal_preparation       'By CAPG.'
_exptl_crystal_recrystallization_method 'From toluene.'
_exptl_crystal_size_max          0.135
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.769
_refine_diff_density_min         -0.734
_refine_diff_density_rms         0.119
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.45(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         6532
_refine_ls_number_restraints     735
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0401
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0123P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0569
_refine_ls_wR_factor_ref         0.0631
_reflns_Friedel_coverage         0.897
_reflns_Friedel_fraction_full    0.976
_reflns_Friedel_fraction_max     0.974
_reflns_number_gt                5072
_reflns_number_total             6532
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04803e2.cif
_cod_data_source_block           ms0681
_cod_database_code               7130994
_manchester_internal_validation_user GFSW
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.856
_shelx_estimated_absorpt_t_min   0.671
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.54797
 0.45203
2. Restrained distances
 C31A-C32A = C31B-C32B
 1.54 with sigma of 0.02
 C37A-C31A \\sim C31A-C33A \\sim C37B-C31B \\sim C31B-C33B
 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
C22 \\sim C25 \\sim C27 \\sim C18 \\sim C1 \\sim C16 \\sim C20 \\sim C15 \\sim
C13 \\sim C17 \\sim C6 \\sim C14 \\sim C30 \\sim C7 \\sim C24 \\sim C3 \\sim P2
\\sim C4 \\sim C5 \\sim C9 \\sim C29 \\sim C10 \\sim C28 \\sim C11 \\sim C26
\\sim C2 \\sim C19 \\sim P1 \\sim C23 \\sim C8 \\sim C12 \\sim C21: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(C12) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
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 0.004 and sigma for 1-3 distances of 0.004
 C22, C25, C27, C18, C1, C16, C20, C15, C13, C17, C6, C14, C30, C7, C24, C3,
 P2, C4, C5, C9, C29, C10, C28, C11, C26, C2, C19, P1, C23, C8, C12, C21
 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(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:
 C23(H23), C22(H22), C21(H21), C20(H20), C19(H19), C26(H26), C27(H27),
 C28(H28), C29(H29), C30(H30), 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(C23,C22,C21,C20,C19), C25(C26,C27,C28,C29,C30), 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              10953
_shelx_hkl_checksum              48614
_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
;