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_1513610
_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            'C67 H98 N12 S Si6 U2'
_chemical_formula_weight         1748.23
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_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
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_atom_sites_solution_hydrogens   geom
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_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
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_computing_molecular_graphics
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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)
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_computing_structure_refinement
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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).
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SUPERFLIP program (Palatinus, L. & Chapuis, G. J. Appl. Cryst., 2007,
 40, 786-790)
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_diffrn_ambient_temperature      150(2)
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_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
  1 omega  -57.00   43.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239   77.0000  120.0000 100

  2 omega  -67.00   41.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239   19.0000  120.0000 108

  3 omega  -97.00  -51.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  -77.0000   90.0000 46

;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
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_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0888
_diffrn_reflns_av_unetI/netI     0.1358
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -19
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_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            43397
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.989
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_diffrn_reflns_theta_max         30.508
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_exptl_absorpt_coefficient_mu    4.690
_exptl_absorpt_correction_T_max  0.686
_exptl_absorpt_correction_T_min  0.449
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            octahedral
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             3472
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.199
_exptl_crystal_size_min          0.126
_refine_diff_density_max         7.846
_refine_diff_density_min         -4.305
_refine_diff_density_rms         0.339
_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
_refine_ls_number_parameters     806
_refine_ls_number_reflns         21646
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.1668
_refine_ls_R_factor_gt           0.1092
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1134P)^2^+81.3761P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2646
_refine_ls_wR_factor_ref         0.3128
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12215
_reflns_number_total             21646
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3sc52742e.txt
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_cod_original_cell_volume        7169.4(6)
_cod_database_code               1513610
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_shelxl_version_number           2013-4
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