Oxidation of uranium(iv) mixed imido-amido complexes with PhEEPh and to generate uranium(vi) bis(imido) dichalcogenolates, U(NR)<sub>2</sub>(EPh)<sub>2</sub>(L)<sub>2</sub>.
Tomson, Neil C.; Anderson, Nickolas H.; Tondreau, Aaron M.; Scott, Brian L.; Boncella, James M.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 10865–10873; doi:10.1039/c9dt00680j

data_7049807
_publ_section_title
;
 Oxidation of uranium(iv) mixed imido-amido complexes with PhEEPh and to
 generate uranium(vi) bis(imido) dichalcogenolates,
 U(NR)<sub>2</sub>(EPh)<sub>2</sub>(L)<sub>2</sub>.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10865
_journal_page_last               10873
_journal_paper_doi               10.1039/c9dt00680j
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C72 H99 N7 U, 2.5(C7 H8)'
_chemical_formula_sum            'C89.5 H119 N7 U'
_chemical_formula_weight         1530.94
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-08-24
_audit_creation_method
;
Olex2 1.2
(compiled Nov 22 2016 11:51:51 for OlexSys, GUI svn.r5269)
;
_audit_update_record
;
2019-03-06 deposited with the CCDC.    2019-04-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.8483(16)
_cell_length_b                   20.707(2)
_cell_length_c                   26.010(3)
_cell_measurement_reflns_used    3083
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      21.26
_cell_measurement_theta_min      2.28
_cell_volume                     8535.7(15)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 V.2014.7-1 (Bruker AXS, 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0737
_diffrn_reflns_av_unetI/netI     0.0656
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            87023
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.718
_diffrn_reflns_theta_max         25.718
_diffrn_reflns_theta_min         1.798
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.947
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  .836
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'SADABS-2014/2 - Bruker AXS area detector scaling and absorption correction'
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.191
_exptl_crystal_description       block
_exptl_crystal_F_000             3188
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.258
_refine_diff_density_min         -0.821
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.017(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     866
_refine_ls_number_reflns         16182
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0433
_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^)+(0.0542P)^2^+7.8120P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1024
_refine_ls_wR_factor_ref         0.1080
_reflns_Friedel_coverage         0.834
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                14349
_reflns_number_total             16182
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00680j2.cif
_cod_data_source_block           apx2054
_cod_depositor_comments
'Adding full bibliography for 7049805--7049811.cif.'
_cod_original_cell_volume        8536.0(15)
_cod_original_formula_sum        'C89.50 H119 N7 U'
_cod_database_code               7049807
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.983(8) 0.017(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C3AA-C0AA
 2.5 with sigma of 0.01
 C4AA-C3AA
 2.5 with sigma of 0.01
 C1AA-C3AA
 1.53 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C4AA \\sim C1AA \\sim C0AA \\sim C6AA \\sim C5AA \\sim C2AA \\sim C3AA: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C4AA) \\sim Ueq, Uanis(C3AA) \\sim Ueq, Uanis(C1AA) \\sim Ueq,
Uanis(C0AA) \\sim Ueq, Uanis(C2AA) \\sim Ueq, Uanis(C6AA) \\sim Ueq,
Uanis(C5AA) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C81) = Uanis(C82) = Uanis(C83) = Uanis(C84) = Uanis(C85) = Uanis(C86) =
Uanis(C80) = Uanis(C73) = Uanis(C71) = Uanis(C72) = Uanis(C70)
5. Rigid body (RIGU) restrains
 C5AA, C0AA, C1AA, C6AA, C3AA, C4AA, C2AA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6. Others
 Fixed Sof: C3AA(0.5) H3AA(0.5) H3AB(0.5) H3AC(0.5) C4AA(0.5) H4AA(0.5)
 C2AA(0.5) H2AA(0.5) C5AA(0.5) H5AA(0.5) C6AA(0.5) H6AA(0.5) C0AA(0.5)
 H0AA(0.5) C1AA(0.5)
7.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C19(H19), C22(H22), C31(H31), C34(H34)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C15(H15), C16(H16), C17(H17), C27(H27), C28(H28),
 C29(H29), C37(H37), C38(H38), C40(H40), C47(H47), C49(H49), C50(H50), C55(H55),
  C56(H56), C58(H58), C65(H65), C67(H67), C68(H68), C82(H82), C83(H83),
 C84(H84), C85(H85), C86(H86), C75(H75), C76(H76), C77(H77), C78(H78), C79(H79),
  C4AA(H4AA), C2AA(H2AA), C5AA(H5AA), C6AA(H6AA), C0AA(H0AA)
7.c Fitted hexagon refined as free rotating group:
 C4AA(C2AA,C5AA,C6AA,C0AA,C1AA)
7.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C36(H36A,
 H36B,H36C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C),
 C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C61(H61A,H61B,
 H61C), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C), C70(H70A,H70B,H70C), C71(H71A,
 H71B,H71C), C72(H72A,H72B,H72C), C80(H80A,H80B,H80C), C73(H73A,H73B,H73C),
 C3AA(H3AA,H3AB,H3AC)
;
_shelx_res_checksum              46467
_shelx_shelxl_version_number     2018/3
_olex2_submission_special_instructions 'No special instructions were received'