Reactivity of uranium(iv) bridged chalcogenido complexes UIV–E–UIV (E = S, Se) with elemental sulfur and selenium: synthesis of polychalcogenido-bridged uranium complexes
Franke, Sebastian M.; Heinemann, Frank W.; Meyer, Karsten; Chemical Science 5 (2014) 942–; doi:10.1039/c3sc52799a

data_1513687
_publ_section_title
;
 Reactivity of uranium(iv) bridged chalcogenido complexes UIV--E--UIV (E =
 S, Se) with elemental sulfur and selenium: synthesis of
 polychalcogenido-bridged uranium complexes
;
_journal_issue                   3
_journal_name_full               'Chemical Science'
_journal_page_first              942
_journal_paper_doi               10.1039/c3sc52799a
_journal_volume                  5
_journal_year                    2014
_chemical_formula_moiety         'C116 H148 N2 O8 Se4.11 U2, 2(C7 H8)'
_chemical_formula_sum            'C130 H164 N2 O8 Se4.11 U2'
_chemical_formula_weight         2683.22
_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                90.000(7)
_cell_angle_beta                 118.117(12)
_cell_angle_gamma                90.000(8)
_cell_formula_units_Z            2
_cell_length_a                   18.092(2)
_cell_length_b                   12.3650(6)
_cell_length_c                   28.315(3)
_cell_measurement_reflns_used    175
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.00
_cell_measurement_theta_min      6.00
_cell_volume                     5586.8(11)
_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      100(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method
;
 \f- and \w-rotations with 1.30 \% and 90 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  0.0640
_diffrn_reflns_av_sigmaI/netI    0.0467
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            85074
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         3.33
_exptl_absorpt_coefficient_mu    4.294
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.601
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2002'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2691
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.937
_refine_diff_density_min         -1.597
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.573
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     732
_refine_ls_number_reflns         12292
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.585
_refine_ls_R_factor_all          0.0711
_refine_ls_R_factor_gt           0.0441
_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^)+(0.0170P)^2^+3.1510P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0754
_refine_ls_wR_factor_ref         0.0802
_reflns_number_gt                9440
_reflns_number_total             12292
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3sc52799a.txt
_cod_data_source_block           sf1309
_cod_original_cell_volume        5586.8(9)
_cod_original_sg_symbol_Hall     -P2ybc
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               1513687