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_1513611
_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 Se Si6 U2'
_chemical_formula_weight         1795.13
_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                 90.9355(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.1375(3)
_cell_length_b                   17.5716(4)
_cell_length_c                   22.6446(5)
_cell_measurement_reflns_used    6210
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.3189
_cell_measurement_theta_min      3.3352
_cell_volume                     7216.0(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_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   10.00   94.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051   57.0000   30.0000 84

  2 omega  -43.00   47.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051  -57.0000 -120.0000 90

  3 omega  -43.00   47.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051  -57.0000   60.0000 90

  4 omega  -15.00   93.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051   19.0000 -120.0000 108

  5 omega   34.00   66.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051  179.0000  -90.0000 32

  6 omega    5.00   63.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051   57.0000  -60.0000 58

;
_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  0.0987
_diffrn_reflns_av_sigmaI/netI    0.0983
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            69833
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         3.34
_exptl_absorpt_coefficient_mu    5.135
_exptl_absorpt_correction_T_max  0.8248
_exptl_absorpt_correction_T_min  0.4266
_exptl_absorpt_correction_type   analytical
_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)
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            orange
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3544
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.075
_refine_diff_density_min         -0.913
_refine_diff_density_rms         0.187
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     806
_refine_ls_number_reflns         17890
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.0958
_refine_ls_R_factor_gt           0.0470
_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^)+(0.0125P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0629
_refine_ls_wR_factor_ref         0.0742
_reflns_number_gt                11665
_reflns_number_total             17890
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3sc52742e.txt
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1513611