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_4119567
_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            'C56 H102 Co N3 O S Si6 U'
_chemical_formula_weight         1330.97
_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                   23.5047(6)
_cell_length_b                   11.9644(3)
_cell_length_c                   23.5149(6)
_cell_measurement_temperature    100(2)
_cell_volume                     6612.9(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0307
_diffrn_reflns_av_sigmaI/netI    0.0491
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            46349
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    2.873
_exptl_absorpt_correction_T_max  0.6725
_exptl_absorpt_correction_T_min  0.5973
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_description       block
_exptl_crystal_F_000             2744
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.921
_refine_diff_density_min         -1.989
_refine_diff_density_rms         0.148
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.033(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         13942
_refine_ls_number_restraints     65
_refine_ls_restrained_S_all      1.915
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0532
_refine_ls_shift/su_max          0.100
_refine_ls_shift/su_mean         0.017
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+40.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1268
_refine_ls_wR_factor_ref         0.1385
_reflns_number_gt                11726
_reflns_number_total             13942
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja402068j_si_001_1.cif
_cod_data_source_block           Complex_1
_cod_database_code               4119567