Two-electron versus one-electron reduction of chalcogens by uranium(iii): synthesis of a terminal U(v) persulfide complex
Camp, Clément; Antunes, Maria Augusta; García, Gregorio; Ciofini, Ilaria; Santos, Isabel C.; Pécaut, Jacques; Almeida, Manuel; Marçalo, Joaquim; Mazzanti, Marinella; Chemical Science 5 (2014) 841–; doi:10.1039/c3sc52742e

data_1513612
_publ_section_title
;
 Two-electron versus one-electron reduction of chalcogens by uranium(iii):
 synthesis of a terminal U(v) persulfide complex
;
_journal_issue                   2
_journal_name_full               'Chemical Science'
_journal_page_first              841
_journal_paper_doi               10.1039/c3sc52742e
_journal_volume                  5
_journal_year                    2014
_chemical_formula_sum            'C35.25 H51 N6 S2 Si3 U'
_chemical_formula_weight         945.24
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 145.19(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.725(4)
_cell_length_b                   19.8120(7)
_cell_length_c                   30.101(5)
_cell_measurement_reflns_used    11153
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.5033
_cell_measurement_theta_min      3.2981
_cell_volume                     7736(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 15.9653
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega   20.00   94.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5614   57.0000    0.0000 74

  2 omega  -43.00   32.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5614  -37.0000 -180.0000 75

  3 omega  -19.00   63.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5614  -99.0000    0.0000 82

  4 omega   12.00   93.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5614   57.0000  150.0000 81

  5 omega    0.00   67.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5614   37.0000  120.0000 67

  6 omega  -87.00   -6.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  -57.0000 -120.0000 81

  7 omega   34.00   78.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5614  179.0000 -150.0000 44

;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\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  0.0761
_diffrn_reflns_av_sigmaI/netI    0.0693
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            70075
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.30
_exptl_absorpt_coefficient_mu    4.431
_exptl_absorpt_correction_T_max  0.6757
_exptl_absorpt_correction_T_min  0.4622
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.623
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3764
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         4.615
_refine_diff_density_min         -1.842
_refine_diff_density_rms         0.192
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     908
_refine_ls_number_reflns         15789
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.1129
_refine_ls_R_factor_gt           0.0728
_refine_ls_shift/su_max          0.041
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0647P)^2^+102.8062P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1718
_refine_ls_wR_factor_ref         0.1945
_reflns_number_gt                10241
_reflns_number_total             15789
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3sc52742e.txt
_cod_data_source_block           4
_cod_original_cell_volume        7736.4(18)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1513612