A Heterobimetallic Complex With an Unsupported Uranium(III)-Aluminum(I) Bond: (CpSiMe3)3U-AlCp* (Cp* = C5Me5)
Stefan G. Minasian; Jamin L. Krinsky; Valerie A. Williams; John Arnold; Journal of the American Chemical Society 130 (2008) 10086–10087; doi:10.1021/ja8042382

data_4108157
_publ_section_title
;
 A Heterobimetallic Complex With an Unsupported Uranium(III)-Aluminum(I)
 Bond: (CpSiMe3)3U-AlCp* (Cp* = C5Me5)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10086
_journal_page_last               10087
_journal_paper_doi               10.1021/ja8042382
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C34 H54 Al Si3 U'
_chemical_formula_sum            'C34 H54 Al Si3 U'
_chemical_formula_weight         812.05
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.255(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.516(6)
_cell_length_b                   12.874(4)
_cell_length_c                   17.540(6)
_cell_measurement_reflns_used    3825
_cell_measurement_temperature    156(2)
_cell_measurement_theta_max      48.120
_cell_measurement_theta_min      4.630
_cell_volume                     3729(2)
_computing_cell_refinement       'Bruker SAINT v7.07'
_computing_data_collection       'Bruker SMART v5.631'
_computing_data_reduction        'Bruker SAINT v7.07'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      156(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_measurement_method       '\w 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  0.0555
_diffrn_reflns_av_sigmaI/netI    0.1705
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20457
_diffrn_reflns_theta_full        26.35
_diffrn_reflns_theta_max         26.35
_diffrn_reflns_theta_min         2.31
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.492
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.777558
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_description       block
_exptl_crystal_F_000             1620
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.529
_refine_diff_density_min         -1.032
_refine_diff_density_rms         0.105
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.335(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.664
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     732
_refine_ls_number_reflns         12635
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.664
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0105P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0577
_refine_ls_wR_factor_ref         0.0604
_reflns_number_gt                7912
_reflns_number_total             12635
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8042382-file002.cif
_cod_data_source_block           sgm4149s
_cod_original_sg_symbol_H-M      'P c'
_cod_database_code               4108157