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_4119568
_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            'C54 H104 Co N3 O2 Se Si6 U'
_chemical_formula_weight         1371.86
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.5018(13)
_cell_length_b                   12.0015(6)
_cell_length_c                   23.5553(13)
_cell_measurement_temperature    100(2)
_cell_volume                     6643.9(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0548
_diffrn_reflns_av_sigmaI/netI    0.0603
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            45150
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    3.377
_exptl_absorpt_correction_T_max  0.7288
_exptl_absorpt_correction_T_min  0.5516
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_description       block
_exptl_crystal_F_000             2808
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.228
_refine_diff_density_min         -1.569
_refine_diff_density_rms         0.147
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.321(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         16430
_refine_ls_number_restraints     86
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.0808
_refine_ls_R_factor_gt           0.0548
_refine_ls_shift/su_max          0.047
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+0.7148P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1424
_refine_ls_wR_factor_ref         0.1531
_reflns_number_gt                12027
_reflns_number_total             16430
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja402068j_si_001_2.cif
_cod_data_source_block           Complex_2
_cod_database_code               4119568