Reactivity of uranium(iii) with H2E (E = S, Se, Te): synthesis of a series of mononuclear and dinuclear uranium(iv) hydrochalcogenido complexes
Franke, Sebastian M.; Rosenzweig, Michael W.; Heinemann, Frank W.; Meyer, Karsten; Chem. Sci. 6 (2015) 275–; doi:10.1039/C4SC02602K

data_1517855
_publ_section_title
;
 Reactivity of uranium(iii) with H2E (E = S, Se, Te): synthesis of a
 series of mononuclear and dinuclear uranium(iv) hydrochalcogenido
 complexes
;
_journal_issue                   1
_journal_name_full               'Chem. Sci.'
_journal_page_first              275
_journal_paper_doi               10.1039/C4SC02602K
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety         'C58 H77 N O5 Se U, C6 H6'
_chemical_formula_sum            'C64 H83 N O5 Se U'
_chemical_formula_weight         1263.30
_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                88.022(3)
_cell_angle_beta                 80.746(3)
_cell_angle_gamma                82.903(3)
_cell_formula_units_Z            4
_cell_length_a                   16.827(1)
_cell_length_b                   17.007(1)
_cell_length_c                   19.804(2)
_cell_measurement_reflns_used    9644
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.48
_cell_measurement_theta_min      2.41
_cell_volume                     5550.2(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      100(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 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  0.0439
_diffrn_reflns_av_sigmaI/netI    0.0288
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            158317
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         2.58
_exptl_absorpt_coefficient_mu    3.631
_exptl_absorpt_correction_T_max  0.421
_exptl_absorpt_correction_T_min  0.305
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2002'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2560
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.22
_refine_diff_density_max         4.391
_refine_diff_density_min         -1.842
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1371
_refine_ls_number_reflns         24462
_refine_ls_number_restraints     252
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0354
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0280P)^2^+24.9423P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0867
_reflns_number_gt                20123
_reflns_number_total             24462
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4sc02602k2.cif
_cod_data_source_block           sf1318
_cod_depositor_comments
'Adding full bibliography for 1517854--1517859.cif.'
_cod_original_cell_volume        5550.0(6)
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1517855