A Mild Protocol To Generate Uranium(IV) Mixed-Ligand Metallocene Complexes using Copper(I) Iodide
Graves, Christopher R.; Schelter, Eric J.; Cantat, Thibault; Scott, Brian L.; Kiplinger, Jaqueline L.; Organometallics 27 (2008) 5371–; doi:10.1021/om800622g

data_4072152
_publ_section_title
;
 A Mild Protocol To Generate Uranium(IV) Mixed-Ligand Metallocene
 Complexes using Copper(I) Iodide
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              5371
_journal_paper_doi               10.1021/om800622g
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C22.5 H51.5 I N Si2 U'
_chemical_formula_weight         817.30
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.73(3)
_cell_angle_beta                 100.47(3)
_cell_angle_gamma                93.31(3)
_cell_formula_units_Z            4
_cell_length_a                   9.760(2)
_cell_length_b                   17.856(4)
_cell_length_c                   18.371(4)
_cell_measurement_temperature    141(2)
_cell_volume                     3123.1(12)
_computing_cell_refinement       'SAINT 4.05 (Bruker, 1996)'
_computing_data_collection       'SMART 4.210 (Bruker, 1996)'
_computing_data_reduction        'SAINT 4.05 (Bruker, 1996)'
_computing_molecular_graphics    'SHELXTL 6.10 (Bruker, 2001)'
_computing_publication_material  'SHELXTL 6.10 (Bruker, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      141(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker SMART 1k CCD'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_sigmaI/netI    0.0457
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            36583
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    6.279
_exptl_absorpt_correction_T_max  0.7873
_exptl_absorpt_correction_T_min  0.1732
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.03 (Sheldrick, 2001)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.738
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1586
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.843
_refine_diff_density_min         -1.324
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     619
_refine_ls_number_reflns         14188
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0264
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0175P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0469
_refine_ls_wR_factor_ref         0.0496
_reflns_number_gt                11391
_reflns_number_total             14188
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800622g_si_001.cif
_cod_data_source_block           c:\frames\xpl052\work\squeezed
_cod_original_cell_volume        3122.9(11)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C22.5 H51.5 I1 N1 Si2 U1'
_cod_database_code               4072152