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_1513688
_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         '2(C108 H132 N2 O6 S2 U2), 5(C4 H10 O2)'
_chemical_formula_sum            'C236 H314 N4 O22 S8 U4'
_chemical_formula_weight         4767.51
_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                88.4070(10)
_cell_angle_beta                 84.0550(10)
_cell_angle_gamma                75.5040(10)
_cell_formula_units_Z            2
_cell_length_a                   20.5440(3)
_cell_length_b                   22.5155(3)
_cell_length_c                   24.1171(3)
_cell_measurement_reflns_used    9160
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.61
_cell_measurement_theta_min      2.46
_cell_volume                     10742.3(3)
_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      100(2)
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_device_type  'Bruker Smart APEX II CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0597
_diffrn_reflns_av_sigmaI/netI    0.0645
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            165269
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         2.55
_exptl_absorpt_coefficient_mu    3.149
_exptl_absorpt_correction_T_max  0.501
_exptl_absorpt_correction_T_min  0.314
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2002'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4860
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.32
_refine_diff_density_max         2.790
_refine_diff_density_min         -1.539
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.217
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     2570
_refine_ls_number_reflns         43190
_refine_ls_number_restraints     417
_refine_ls_restrained_S_all      1.240
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0410P)^2^+3.7304P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0980
_refine_ls_wR_factor_ref         0.1063
_reflns_number_gt                32834
_reflns_number_total             43190
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3sc52799a.txt
_cod_data_source_block           sf1117
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1513688