Halide, Amide, Cationic, Manganese Carbonylate, and Oxide Derivatives of Triamidosilylamine Uranium Complexes
Benedict M. Gardner; William Lewis; Alexander J. Blake; Stephen T. Liddle; Inorganic Chemistry 50 (2011) 9631–9641; doi:10.1021/ic201372a

data_4326387
_publ_section_title
;
 Halide, Amide, Cationic, Manganese Carbonylate, and Oxide Derivatives of
 Triamidosilylamine Uranium Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9631
_journal_page_last               9641
_journal_paper_doi               10.1021/ic201372a
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C30 H78 I2 N8 SI6 U2, 2 C7 H8'
_chemical_formula_sum            'C44 H94 I2 N8 Si6 U2'
_chemical_formula_weight         1633.67
_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           'enCIFer editing of SHELXL97 CIF output'
_cell_angle_alpha                76.014(2)
_cell_angle_beta                 73.693(2)
_cell_angle_gamma                78.467(2)
_cell_formula_units_Z            1
_cell_length_a                   9.4693(10)
_cell_length_b                   10.8245(11)
_cell_length_c                   15.0764(15)
_cell_measurement_reflns_used    7949
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      2.37
_cell_volume                     1424.7(3)
_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; SHELXTL (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'enCIFer (Allen et al., 2004);PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'Bruker SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker SMART 1000 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  0.0178
_diffrn_reflns_av_sigmaI/netI    0.0242
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10712
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.26
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.924
_exptl_absorpt_correction_T_max  0.6429
_exptl_absorpt_correction_T_min  0.1682
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.904
_exptl_crystal_description       Needle
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.76
_refine_diff_density_min         -2.08
_refine_diff_density_rms         0.14
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.09
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         4980
_refine_ls_number_restraints     141
_refine_ls_restrained_S_all      1.27
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.033
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.056P)^2^+4.556P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0926
_refine_ls_wR_factor_ref         0.0943
_reflns_number_gt                4612
_reflns_number_total             4980
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic201372a_si_001_03.cif
_cod_data_source_block           32toluene
_cod_database_code               4326387