Synthesis and structure of [U{C(PPh2NMes)2}2] (Mes = 2,4,6-Me3C6H2): A homoleptic uranium bis(carbene) complex with two formal UC double bonds
Cooper, Oliver J.; McMaster, Jonathan; Lewis, William; Blake, Alexander J.; Liddle, Stephen T.; Dalton Transactions 39 (2010) 5074–; doi:10.1039/c0dt00152j

data_7026038
_publ_section_title
;
 Synthesis and structure of [U{C(PPh2NMes)2}2] (Mes = 2,4,6-Me3C6H2): A
 homoleptic uranium bis(carbene) complex with two formal U&#xE001;C double
 bonds
;
_journal_issue                   21
_journal_name_full               'Dalton Transactions'
_journal_page_first              5074
_journal_paper_doi               10.1039/c0dt00152j
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C86 H84 N4 P4 U, 4 C7 H8'
_chemical_formula_sum            'C114 H116 N4 P4 U'
_chemical_formula_weight         1904.02
_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           SHELXL-97
_cell_angle_alpha                70.551(2)
_cell_angle_beta                 75.047(3)
_cell_angle_gamma                77.427(3)
_cell_formula_units_Z            2
_cell_length_a                   14.839(2)
_cell_length_b                   15.329(2)
_cell_length_c                   21.677(3)
_cell_measurement_reflns_used    5991
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.508
_cell_measurement_theta_min      2.336
_cell_volume                     4444.8(10)
_computing_cell_refinement       'Bruker SAINT version 6.36a (Bruker, 2000)'
_computing_data_collection       'Bruker SMART version 5.625 (Bruker, 2001)'
_computing_data_reduction        'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material
'enCIFer(Allen et al.,2004);PLATON(Spek,2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1012
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            15572
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.87
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.953
_exptl_absorpt_correction_T_max  0.4305
_exptl_absorpt_correction_T_min  0.3483
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             1960
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         6.471
_refine_diff_density_min         -2.718
_refine_diff_density_rms         0.200
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     869
_refine_ls_number_reflns         15572
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0881
_refine_ls_R_factor_gt           0.0742
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1306P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1892
_refine_ls_wR_factor_ref         0.1984
_reflns_number_gt                12667
_reflns_number_total             15572
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c0dt00152j.txt
_cod_data_source_block           uojcla
_cod_original_cell_volume        4444.8(12)
_cod_database_code               7026038