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_7026037
_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 Li4 N4 P4, C7 H8'
_chemical_formula_sum            'C93 H92 Li4 N4 P4'
_chemical_formula_weight         1417.35
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   'geom, Me from difmap'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'enCIFer editing of SHELXL97 CIF output'
_cell_angle_alpha                90.00
_cell_angle_beta                 102.544(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.512(2)
_cell_length_b                   20.928(3)
_cell_length_c                   27.872(4)
_cell_measurement_reflns_used    1950
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.426
_cell_measurement_theta_min      2.43
_cell_volume                     7693.5(19)
_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      90(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.1322
_diffrn_reflns_av_sigmaI/netI    0.1705
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            38438
_diffrn_reflns_theta_full        24.50
_diffrn_reflns_theta_max         24.50
_diffrn_reflns_theta_min         1.86
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.148
_exptl_absorpt_correction_T_max  0.9926
_exptl_absorpt_correction_T_min  0.9824
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             3000
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.566
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     947
_refine_ls_number_reflns         12774
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.1566
_refine_ls_R_factor_gt           0.0765
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0680P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1476
_refine_ls_wR_factor_ref         0.1790
_reflns_number_gt                6885
_reflns_number_total             12774
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c0dt00152j.txt
_cod_data_source_block           pojccb
_cod_original_cell_volume        7693.2(19)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7026037