A Complete Family of Terminal Uranium Chalcogenides, [U(E)(N{SiMe3}2)3]- (E = O, S, Se, Te)
Jessie L. Brown; Skye Fortier; Richard A. Lewis; Guang Wu; Trevor W. Hayton; Journal of the American Chemical Society 134 (2012) 15468–15475; doi:10.1021/ja305712m

data_4118632
_publ_section_title
;
 A Complete Family of Terminal Uranium Chalcogenides, [U(E)(N{SiMe3}2)3]-
 (E = O, S, Se, Te)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15468
_journal_page_last               15475
_journal_paper_doi               10.1021/ja305712m
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C38 H84 Co N3 O Si6 U'
_chemical_formula_weight         1064.58
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 115.802(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.8951(15)
_cell_length_b                   14.0270(10)
_cell_length_c                   20.5125(13)
_cell_measurement_temperature    100(2)
_cell_volume                     5153.7(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'ccd area detector'
_diffrn_measurement_method       'omega scan'
_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  0.0457
_diffrn_reflns_av_sigmaI/netI    0.0540
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            30687
_diffrn_reflns_theta_full        26.48
_diffrn_reflns_theta_max         26.48
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    3.629
_exptl_absorpt_correction_T_max  0.6401
_exptl_absorpt_correction_T_min  0.4386
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_F_000             2176
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.13
_refine_diff_density_max         4.119
_refine_diff_density_min         -2.828
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         10537
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0461
_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^)+(0.0000P)^2^+46.5497P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0917
_refine_ls_wR_factor_ref         0.0986
_reflns_number_gt                7707
_reflns_number_total             10537
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja305712m_si_002_4.cif
_cod_data_source_block           Complex_5
_cod_original_cell_volume        5153.7(6)
_cod_database_code               4118632