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_7049808
_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         'C47.99 H69 Li2 N2 O4 S4 U'
_chemical_formula_sum            'C47.98 H69 Li2 N2 O4 S4 U'
_chemical_formula_weight         1118.02
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 99.345(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.790(2)
_cell_length_b                   22.803(5)
_cell_length_c                   21.399(5)
_cell_measurement_reflns_used    3083
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      21.26
_cell_measurement_theta_min      2.28
_cell_volume                     5195.2(19)
_computing_cell_refinement       'APEX2 V.2014.7-1 (Bruker AXS, 2014)'
_computing_data_collection       'APEX2 V.2014.7-1 (Bruker AXS, 2014)'
_computing_data_reduction        'SAINT, v. 8.34A (Bruker AXS, 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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.1206
_diffrn_reflns_av_unetI/netI     0.0917
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            47137
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.709
_diffrn_reflns_theta_max         24.709
_diffrn_reflns_theta_min         1.929
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.326
_exptl_absorpt_correction_T_max  .865
_exptl_absorpt_correction_T_min  .788
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'SADABS-2014/2 - Bruker AXS area detector scaling and absorption correction'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_description       block
_exptl_crystal_F_000             2260
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.036
_refine_diff_density_min         -1.380
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     603
_refine_ls_number_reflns         8850
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0918
_refine_ls_R_factor_gt           0.0486
_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^)+(0.0515P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0971
_refine_ls_wR_factor_ref         0.1124
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5929
_reflns_number_total             8850
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00680j2.cif
_cod_data_source_block           apx1763
_cod_depositor_comments
'Adding full bibliography for 7049805--7049811.cif.'
_cod_original_cell_volume        5195.0(19)
_cod_database_code               7049808
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(Li1) = Uanis(Li2) = Uanis(C45) = Uanis(C45A)
Uanis(C53) = Uanis(C54) = Uanis(C1C)
Uanis(C65) = Uanis(C65A) = Uanis(C71A) = Uanis(C71) = Uanis(C73A) = Uanis(C73)
= Uanis(C72A) = Uanis(C72) = Uanis(C46) = Uanis(C46A) = Uanis(C1D)
Uanis(C1J) = Uanis(C1K) = Uanis(C1I) = Uanis(C1H)
Uanis(C2) = Uanis(C1) = Uanis(C11) = Uanis(C3)
3. Others
 Sof(C58)=Sof(H58A)=Sof(H58B)=Sof(C1C)=Sof(H1CA)=Sof(H1CB)=Sof(C1D)=Sof(H1DA)=
 Sof(H1DB)=Sof(C65A)=Sof(C70A)=Sof(H70A)=Sof(C69A)=Sof(H69A)=Sof(C68A)=
 Sof(H68A)=Sof(C67A)=Sof(H67A)=Sof(C66A)=Sof(H66A)=1-FVAR(1)
 Sof(C65)=Sof(C66)=Sof(H66)=Sof(C69)=Sof(H69)=Sof(C68)=Sof(H68)=Sof(C59)=
 Sof(H59A)=Sof(H59B)=Sof(C67)=Sof(H67)=Sof(C70)=Sof(H70)=Sof(C54)=Sof(H54A)=
 Sof(H54B)=Sof(C1E)=Sof(H1EA)=Sof(H1EB)=FVAR(1)
 Sof(C45A)=Sof(C46A)=Sof(H46A)=Sof(C72A)=Sof(H72A)=Sof(C73A)=Sof(H73A)=
 Sof(C71A)=Sof(H71A)=Sof(C44A)=Sof(H44A)=1-FVAR(2)
 Sof(C45)=Sof(C44)=Sof(H44)=Sof(C46)=Sof(H46)=Sof(C72)=Sof(H72)=Sof(C71)=
 Sof(H71)=Sof(H73)=FVAR(2)
 Fixed Sof: H49A(0.5) H49B(0.5) H49C(0.5) H49D(0.5) H55C(0.5) H55D(0.5)
 H55A(0.5) H55B(0.5) H53C(0.5) H53D(0.5) H53A(0.5) H53B(0.5) H57A(0.5)
 H57B(0.5) H60A(0.5) H60B(0.5) H60C(0.5) H60D(0.5) C62(0.5) H62A(0.5) H62B(0.5)
 C73(0.5) C4(0.5) H4A(0.5) H4B(0.5) C9(0.5) H9A(0.5) H9B(0.5) C10(0.5)
 H10A(0.5) H10B(0.5) C1A(0.5) H1AA(0.5) H1AB(0.5) C1B(0.5) H1BA(0.5) H1BB(0.5)
 C1F(0.5) H1FA(0.5) H1FB(0.5) C1G(0.5) H1GA(0.5) H1GB(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B), C49(H49A,H49B), C49(H49C,H49D), C50(H50A,H50B), C52(H52A,
 H52B), C55(H55C,H55D), C55(H55A,H55B), C53(H53C,H53D), C53(H53A,H53B),
 C56(H56A,H56B), C57(H57A,H57B), C60(H60A,H60B), C60(H60C,H60D), C59(H59A,H59B),
  C58(H58A,H58B), C62(H62A,H62B), C54(H54A,H54B), C4(H4A,H4B), C9(H9A,H9B),
 C10(H10A,H10B), C1A(H1AA,H1AB), C1B(H1BA,H1BB), C1C(H1CA,H1CB), C1D(H1DA,H1DB),
  C1E(H1EA,H1EB), C1F(H1FA,H1FB), C1G(H1GA,H1GB)
4.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C66(H66), C17(H17), C16(H16), C13(H13), C15(H15), C69(H69),
 C68(H68), C44(H44), C46(H46), C67(H67), C70(H70), C72(H72), C71(H71), C73(H73),
  C46A(H46A), C72A(H72A), C73A(H73A), C71A(H71A), C44A(H44A), C70A(H70A),
 C69A(H69A), C68A(H68A), C67A(H67A), C66A(H66A), C19(H19), C1H(H1H), C1I(H1I),
 C1J(H1J), C1K(H1K)
4.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C11(H11A,H11B,H11C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C),
 C3(H3A,H3B,H3C), C2(H2A,H2B,H2C)
;
_shelx_res_checksum              74317
_shelx_shelxl_version_number     2018/3
_olex2_submission_special_instructions 'No special instructions were received'