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_1513613
_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            'C60 H90 N12 S2 Si6 U2'
_chemical_formula_weight         1688.16
_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                 108.259(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.1895(9)
_cell_length_b                   12.4113(5)
_cell_length_c                   20.2745(10)
_cell_measurement_reflns_used    5709
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.4894
_cell_measurement_theta_min      3.2762
_cell_volume                     3390.8(3)
_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_molecular_graphics
;
Mercury 3.1 New software for searching the Cambridge Structural Database 
and visualizing crystal structures (I.J. Bruno, J.C. Cole, P.R. Edgington, 
M. Kessler, C.F. Macrae, P. McCabe, J. Pearson, R. Taylor, 
Acta Cryst., 2002, B58, 389-397)
;
_computing_publication_material  'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement
;
OLEX2: a complete structure solution, refinement and analysis program 
(O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and 
H. Puschmann. J. Appl. Cryst. 2009, 42, 339-34).
;
_computing_structure_solution
;
SUPERFLIP program (Palatinus, L. & Chapuis, G. J. Appl. Cryst., 2007,
 40, 786-790)
;
_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  -25.00   67.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051  -99.0000 -150.0000 92

  2 omega -103.00  -62.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239 -179.0000 -180.0000 41

  3 omega  -88.00   33.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239    0.0000    0.0000 121

  4 omega -100.00   17.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  -19.0000  120.0000 117

  5 omega    5.00   94.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051   57.0000  -30.0000 89

  6 omega  -49.00  -20.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239   57.0000   90.0000 29

;
_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  0.0942
_diffrn_reflns_av_sigmaI/netI    0.0827
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            33752
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         3.28
_exptl_absorpt_coefficient_mu    4.984
_exptl_absorpt_correction_T_max  0.8813
_exptl_absorpt_correction_T_min  0.4401
_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            'translucent light brown'
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1668
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.03
_refine_diff_density_max         5.558
_refine_diff_density_min         -1.861
_refine_diff_density_rms         0.246
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         8390
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.1010
_refine_ls_R_factor_gt           0.0706
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0782P)^2^+13.7055P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1627
_refine_ls_wR_factor_ref         0.1820
_reflns_number_gt                6084
_reflns_number_total             8390
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3sc52742e.txt
_cod_data_source_block           5
_cod_database_code               1513613