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_7130990
_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         '2(C9 H14.5 Cl K0.5 Np0.5 O0.5 P)'
_chemical_formula_sum            'C18 H29 Cl2 K Np O P2'
_chemical_formula_weight         670.35
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                89.425(2)
_cell_angle_beta                 89.166(2)
_cell_angle_gamma                79.460(2)
_cell_formula_units_Z            8
_cell_length_a                   8.5818(2)
_cell_length_b                   19.2369(4)
_cell_length_c                   29.3792(7)
_cell_measurement_reflns_used    19820
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.7320
_cell_measurement_theta_min      1.8000
_cell_volume                     4767.66(19)
_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      150(1)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.982
_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    -55.89 147.11   0.50   30.00    --  -18.39  73.75  25.26  406
  2  \w    -55.89 147.11   0.50   30.00    --  -18.39  73.75 -79.74  406
  3  \w     70.11 147.11   0.50   30.00    --  -18.39  73.75 178.26  154
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1403
_diffrn_reflns_av_unetI/netI     0.2497
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            31266
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        21.966
_diffrn_reflns_theta_max         21.966
_diffrn_reflns_theta_min         1.749
_exptl_absorpt_coefficient_mu    4.897
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52557
_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 blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.868
_exptl_crystal_description       plate
_exptl_crystal_F_000             2568
_exptl_crystal_preparation       'By CAPG.'
_exptl_crystal_recrystallization_method 'From Et2O.'
_exptl_crystal_size_max          0.254
_exptl_crystal_size_mid          0.235
_exptl_crystal_size_min          0.085
_refine_diff_density_max         4.698
_refine_diff_density_min         -2.499
_refine_diff_density_rms         0.442
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.168
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1111
_refine_ls_number_reflns         31266
_refine_ls_number_restraints     3558
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.1497
_refine_ls_R_factor_gt           0.0946
_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^)+(0.1402P)^2^+48.4313P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2822
_refine_ls_wR_factor_ref         0.3036
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16688
_reflns_number_total             31266
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 10.5942\% 
around [0.95 0.25 0.18] (reciprocal) or [1.00 -0.03 0.01] (direct)
Component 3 rotated by 12.3417\% 
around [-0.52 -0.18 0.84] (reciprocal) or [-0.99 0.01 0.14] (direct)
;
_cod_data_source_file            d2cc04803e2.cif
_cod_data_source_block           ms0711
_cod_database_code               7130990
_manchester_internal_validation_user GFSW
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.681
_shelx_estimated_absorpt_t_min   0.369
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.87279
 0.07218 0.05503
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.008 and sigma
for terminal atoms of 0.008 within 2A
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Same fragment restrains
{P1, C4, C3, C2, C1, C8, C7, C6, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{P2, C9, C10, C11, C12, C13, C14, C15, C16}
{P1, C4, C3, C2, C1, C8, C7, C6, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{P3A, C17A, C18A, C19A, C20A, C21A, C22A, C23A, C24A}
{P1, C4, C3, C2, C1, C8, C7, C6, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{P4A, C25A, C26A, C27A, C28A, C29A, C30A, C31A, C32A}
{P1, C4, C3, C2, C1, C8, C7, C6, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{P3B, C17B, C18B, C19B, C20B, C21B, C22B, C23B, C24B}
{P1, C4, C3, C2, C1, C8, C7, C6, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{P4B, C25B, C26B, C27B, C28B, C29B, C30B, C31B, C32B}
{P1, C1, C2, C3, C4, C5, C6, C7, C8} sigma for 1-2: 0.02, 1-3: 0.04
as in
{P5, C33, C34, C35, C36, C37, C38, C39, C40}
{P1, C4, C3, C2, C1, C8, C7, C6, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{P6, C41, C42, C43, C44, C45, C46, C47, C48}
{P1, C4, C3, C2, C1, C8, C7, C6, C5} sigma for 1-2: 0.02, 1-3: 0.04
as in
{P7, C49, C50, C51, C52, C53, C54, C55, C56}
{P1, C1, C2, C3, C4, C5, C6, C7, C8} sigma for 1-2: 0.02, 1-3: 0.04
as in
{P8, C57, C58, C59, C60, C61, C62, C63, C64}
5. Others
 Sof(P4B)=Sof(C25B)=Sof(C26B)=Sof(C27B)=Sof(C28B)=Sof(C29B)=Sof(H29D)=
 Sof(H29E)=Sof(H29F)=Sof(C30B)=Sof(H30D)=Sof(H30E)=Sof(H30F)=Sof(C31B)=
 Sof(H31D)=Sof(H31E)=Sof(H31F)=Sof(C32B)=Sof(H32D)=Sof(H32E)=Sof(H32F)=1-FVAR(1)
 Sof(P4A)=Sof(C25A)=Sof(C26A)=Sof(C27A)=Sof(C28A)=Sof(C29A)=Sof(H29A)=
 Sof(H29B)=Sof(H29C)=Sof(C30A)=Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(C31A)=
 Sof(H31A)=Sof(H31B)=Sof(H31C)=Sof(C32A)=Sof(H32A)=Sof(H32B)=Sof(H32C)=FVAR(1)
 Sof(P3B)=Sof(C17B)=Sof(C18B)=Sof(C19B)=Sof(C20B)=Sof(C21B)=Sof(H21D)=
 Sof(H21E)=Sof(H21F)=Sof(C22B)=Sof(H22D)=Sof(H22E)=Sof(H22F)=Sof(C23B)=
 Sof(H23D)=Sof(H23F)=Sof(H23E)=Sof(C24B)=Sof(H24D)=Sof(H24E)=Sof(H24F)=1-FVAR(2)
 Sof(P3A)=Sof(C17A)=Sof(C18A)=Sof(C19A)=Sof(C20A)=Sof(C21A)=Sof(H21A)=
 Sof(H21B)=Sof(H21C)=Sof(C22A)=Sof(H22A)=Sof(H22B)=Sof(H22C)=Sof(C23A)=
 Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C24A)=Sof(H24A)=Sof(H24B)=Sof(H24C)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C66(H66A,H66B), C67(H67A,H67B), C70(H70A,H70B), C71(H71A,H71B)
6.b 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),
 C65(H65A,H65B,H65C), C68(H68A,H68B,H68C), C21A(H21A,H21B,H21C), C22A(H22A,H22B,
 H22C), C23A(H23A,H23B,H23C), C24A(H24A,H24B,H24C), C29A(H29A,H29B,H29C),
 C30A(H30A,H30B,H30C), C31A(H31A,H31B,H31C), C32A(H32A,H32B,H32C), C21B(H21D,
 H21E,H21F), C22B(H22D,H22E,H22F), C23B(H23D,H23F,H23E), C24B(H24D,H24E,H24F),
 C29B(H29D,H29E,H29F), C30B(H30D,H30E,H30F), C31B(H31D,H31E,H31F), C32B(H32D,
 H32E,H32F), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C),
 C40(H40A,H40B,H40C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C47(H47A,H47B,
 H47C), C48(H48A,H48B,H48C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C55(H55A,
 H55B,H55C), C56(H56A,H56B,H56C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C),
 C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C69(H69A,H69B,H69C), C72(H72A,H72B,
 H72C)
;
_shelx_res_checksum              85960
_shelx_hkl_checksum              73273
_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
;