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_4118630
_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            'C37 H72 N3 P Se Si6 U'
_chemical_formula_weight         1075.48
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 99.525(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.9733(4)
_cell_length_b                   12.0775(4)
_cell_length_c                   24.2638(7)
_cell_measurement_temperature    100(2)
_cell_volume                     4905.4(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0405
_diffrn_reflns_av_sigmaI/netI    0.0614
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            22147
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    4.257
_exptl_absorpt_correction_T_max  0.8153
_exptl_absorpt_correction_T_min  0.2808
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.05
_refine_diff_density_max         8.549
_refine_diff_density_min         -5.217
_refine_diff_density_rms         0.203
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.339
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         10698
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.339
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0555
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0511P)^2^+10.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1334
_refine_ls_wR_factor_ref         0.1399
_reflns_number_gt                8735
_reflns_number_total             10698
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja305712m_si_002_2.cif
_cod_data_source_block           Complex_3
_cod_database_code               4118630