Activation of elemental S, Se and Te with uranium(iii): bridging U–E–U (E = S, Se) and diamond-core complexes U–(E)2–U (E = O, S, Se, Te)
Lam, Oanh P.; Heinemann, Frank W.; Meyer, Karsten; Chemical Science 2 (2011) 1538–; doi:10.1039/c1sc00151e

data_1515596
_publ_section_title
;
 Activation of elemental S, Se and Te with uranium(iii): bridging U--E--U
 (E = S, Se) and diamond-core complexes U--(E)2--U (E = O, S, Se, Te)
;
_journal_issue                   8
_journal_name_full               'Chemical Science'
_journal_page_first              1538
_journal_paper_doi               10.1039/c1sc00151e
_journal_volume                  2
_journal_year                    2011
_chemical_formula_moiety         'C108 H132 N2 O6 S2 U2, 2(C12 H30 Na O6)'
_chemical_formula_sum            'C132 H192 N2 Na2 O18 S2 U2'
_chemical_formula_weight         2681.04
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 103.778(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   28.397(3)
_cell_length_b                   17.1610(19)
_cell_length_c                   55.426(11)
_cell_measurement_reflns_used    462
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      20.00
_cell_measurement_theta_min      6.00
_cell_volume                     26233(7)
_computing_cell_refinement       'EVALCCD (Duisenberg, 2003)'
_computing_data_collection       'COLLECT (Bruker-Nonius, 2002)'
_computing_data_reduction        'EVALCCD (Duisenberg, 2003)'
_computing_molecular_graphics    'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_publication_material  'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_structure_refinement  'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_structure_solution    'SHELXTL 6.12 (Bruker AXS, 2002)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method
;
\f- and \w-rotations with 0.30 \% and 140 sec per frame
;
_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  0.1075
_diffrn_reflns_av_sigmaI/netI    0.0832
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       66
_diffrn_reflns_limit_l_min       -67
_diffrn_reflns_number            124655
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         3.34
_exptl_absorpt_coefficient_mu    2.566
_exptl_absorpt_correction_T_max  0.615
_exptl_absorpt_correction_T_min  0.371
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2002'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             11040
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.934
_refine_diff_density_min         -1.969
_refine_diff_density_rms         0.169
_refine_ls_extinction_coef       0.00011(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.481
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1744
_refine_ls_number_reflns         23618
_refine_ls_number_restraints     877
_refine_ls_restrained_S_all      1.488
_refine_ls_R_factor_all          0.1004
_refine_ls_R_factor_gt           0.0805
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2101
_refine_ls_wR_factor_ref         0.2182
_reflns_number_gt                18973
_reflns_number_total             23618
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1sc00151e.txt
_cod_data_source_block           opl1003
_cod_original_sg_symbol_Hall     -C2yc
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               1515596