Synthesis of a Uranium(VI)-Carbene: Reductive Formation of Uranyl(V)-Methanides, Oxidative Preparation of a [R2C=U=O]2+ Analogue of the [O=U=O]2+ Uranyl Ion (R = Ph2PNSiMe3), and Comparison of the Nature of UIV=C, UV=C, and UVI=C Double Bonds
David P. Mills; Oliver J. Cooper; Floriana Tuna; Eric J. L. McInnes; E. Stephen Davies; Jonathan McMaster; Fabrizio Moro; William Lewis; Alexander J. Blake; Stephen T. Liddle; Journal of the American Chemical Society 134 (2012) 10047–10054; doi:10.1021/ja301333f

data_4118064
_publ_section_title
;
 Synthesis of a Uranium(VI)-Carbene: Reductive Formation of
 Uranyl(V)-Methanides, Oxidative Preparation of a [R2C=U=O]2+ Analogue of
 the [O=U=O]2+ Uranyl Ion (R = Ph2PNSiMe3), and Comparison of the Nature
 of UIV=C, UV=C, and UVI=C Double Bonds
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10047
_journal_page_last               10054
_journal_paper_doi               10.1021/ja301333f
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C62 H78 Cl N4 O4 P4 Si4 U2, 3(C7 H8)'
_chemical_formula_sum            'C83 H102 Cl N4 O4 P4 Si4 U2'
_chemical_formula_weight         1967.44
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   'geom, Me from difmap'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_cell_angle_alpha                90.983(2)
_cell_angle_beta                 101.845(3)
_cell_angle_gamma                108.449(2)
_cell_formula_units_Z            2
_cell_length_a                   12.2398(4)
_cell_length_b                   17.5642(4)
_cell_length_c                   21.2961(6)
_cell_measurement_reflns_used    18211
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      74.44
_cell_measurement_theta_min      3.26
_cell_volume                     4233.9(2)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_molecular_graphics    ' ? '
_computing_publication_material
'enCIFer (Allen et al., 2004); PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    ' ? '
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 10.3613
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.042
_diffrn_reflns_av_sigmaI/netI    0.047
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            37152
_diffrn_reflns_theta_full        67.50
_diffrn_reflns_theta_max         67.50
_diffrn_reflns_theta_min         3.55
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.616
_exptl_absorpt_correction_T_max  0.820
_exptl_absorpt_correction_T_min  0.331
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) 
(compiled Jan  5 2010,16:28:46) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_description       lath
_exptl_crystal_F_000             1954
_exptl_crystal_size_max          0.1401
_exptl_crystal_size_mid          0.0606
_exptl_crystal_size_min          0.0191
_refine_diff_density_max         3.40
_refine_diff_density_min         -1.17
_refine_diff_density_rms         0.16
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.06
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     934
_refine_ls_number_reflns         15255
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.06
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_gt           0.0380
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.047P)^2^+15.151P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0925
_refine_ls_wR_factor_ref         0.0974
_reflns_number_gt                13050
_reflns_number_total             15255
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja301333f_si_001_1.cif
_cod_data_source_block           2
_cod_original_cell_volume        4233.8(2)
_cod_database_code               4118064