Synthesis and Spectroscopic and Computational Characterization of the Chalcogenido-Substituted Analogues of the Uranyl Ion, [OUE]2+ (E = S, Se)
Jessie L. Brown; Skye Fortier; Guang Wu; Nikolas Kaltsoyannis; Trevor W. Hayton; Journal of the American Chemical Society 135 (2013) 5352–5355; doi:10.1021/ja402068j

data_4119569
_publ_section_title
;
 Synthesis and Spectroscopic and Computational Characterization of the
 Chalcogenido-Substituted Analogues of the Uranyl Ion, [OUE]2+ (E = S, Se)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5352
_journal_page_last               5355
_journal_paper_doi               10.1021/ja402068j
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C38 H84 Co N3 O2 Si6 U'
_chemical_formula_weight         1080.58
_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                88.5800(10)
_cell_angle_beta                 84.5250(10)
_cell_angle_gamma                73.109(2)
_cell_formula_units_Z            2
_cell_length_a                   11.0157(3)
_cell_length_b                   15.1067(3)
_cell_length_c                   16.2338(4)
_cell_measurement_temperature    100(2)
_cell_volume                     2573.13(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker Kappa apex'
_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  0.0387
_diffrn_reflns_av_sigmaI/netI    0.0660
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            24787
_diffrn_reflns_theta_full        27.18
_diffrn_reflns_theta_max         27.18
_diffrn_reflns_theta_min         1.26
_exptl_absorpt_coefficient_mu    3.636
_exptl_absorpt_correction_T_max  0.7125
_exptl_absorpt_correction_T_min  0.7125
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_description       block
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         6.853
_refine_diff_density_min         -1.503
_refine_diff_density_rms         0.210
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         11181
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0520
_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^)+(0.0663P)^2^+32.2659P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1320
_refine_ls_wR_factor_ref         0.1457
_reflns_number_gt                9063
_reflns_number_total             11181
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja402068j_si_001_3.cif
_cod_data_source_block           Complex_3
_cod_database_code               4119569