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_1517857
_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
;
 C108 H134 N2 O6 S2 U2, 2.25(C6 H6), 0.5(C6 H14)
;
_chemical_formula_sum            'C124.5 H154.5 N2 O6 S2 U2'
_chemical_formula_weight         2315.18
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                85.233(5)
_cell_angle_beta                 87.451(5)
_cell_angle_gamma                88.366(5)
_cell_formula_units_Z            2
_cell_length_a                   11.1756(16)
_cell_length_b                   16.817(2)
_cell_length_c                   28.662(4)
_cell_measurement_reflns_used    9453
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.56
_cell_measurement_theta_min      2.43
_cell_volume                     5361.1(12)
_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 0.999
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker Smart APEX II'
_diffrn_measurement_method       '\f and \w 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  0.0427
_diffrn_reflns_av_sigmaI/netI    0.0220
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            334803
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         29.80
_diffrn_reflns_theta_min         1.22
_exptl_absorpt_coefficient_mu    3.112
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.587
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2008'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2359
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.937
_refine_diff_density_min         -1.875
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1232
_refine_ls_number_reflns         30030
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0257
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0240P)^2^+9.3776P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0608
_refine_ls_wR_factor_ref         0.0629
_reflns_number_gt                26603
_reflns_number_total             30030
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4sc02602k2.cif
_cod_data_source_block           sf1406
_cod_depositor_comments
'Adding full bibliography for 1517854--1517859.cif.'
_cod_original_cell_volume        5361.0(13)
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C124.50 H154.50 N2 O6 S2 U2'
_cod_database_code               1517857