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_1513686
_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
;
 0.93(C108 H132 N2 O6 Se4 U2), 0.07(C108 H132 N2 O6 Se2 U2), 2(C7 H8), 0.25(C6 H14)'
;
_chemical_formula_sum            'C123.5 H151.5 N2 O6 Se3.86 U2'
_chemical_formula_weight         2540.81
_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                85.729(2)
_cell_angle_beta                 87.925(2)
_cell_angle_gamma                89.368(2)
_cell_formula_units_Z            2
_cell_length_a                   11.2872(8)
_cell_length_b                   16.8161(12)
_cell_length_c                   28.943(2)
_cell_measurement_reflns_used    9649
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.71
_cell_measurement_theta_min      2.43
_cell_volume                     5474.5(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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      120(2)
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Kappa APEX II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Quazar focussing montel optics'
_diffrn_radiation_source         'ImuS micro-focus tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_sigmaI/netI    0.0293
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            100676
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         2.92
_exptl_absorpt_coefficient_mu    4.293
_exptl_absorpt_correction_T_max  0.604
_exptl_absorpt_correction_T_min  0.489
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2008'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2539
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.812
_refine_diff_density_min         -0.888
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1339
_refine_ls_number_reflns         26070
_refine_ls_number_restraints     315
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0296
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0367P)^2^+11.9614P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0752
_refine_ls_wR_factor_ref         0.0789
_reflns_number_gt                22409
_reflns_number_total             26070
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3sc52799a.txt
_cod_data_source_block           sf1217a
_cod_original_cell_volume        5474.6(7)
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C123.50 H151.50 N2 O6 Se3.86 U2'
_cod_database_code               1513686