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_1513614
_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            'C30 H45 N6 Na O Si3 U'
_chemical_formula_weight         851.01
_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                 91.612(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.5247(3)
_cell_length_b                   18.5060(5)
_cell_length_c                   17.3041(6)
_cell_measurement_reflns_used    3591
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.4651
_cell_measurement_theta_min      3.4994
_cell_volume                     3368.99(18)
_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
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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)
;
_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)
;
_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 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
  1 omega    1.00   93.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051   77.0000   90.0000 92

  2 omega   34.00   60.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051  179.0000   60.0000 26

  3 omega  -54.00   42.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239   77.0000    0.0000 96

  4 omega -100.00  -59.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  -37.0000  -90.0000 41

;
_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  0.0530
_diffrn_reflns_av_sigmaI/netI    0.0950
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            20741
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         3.51
_exptl_absorpt_coefficient_mu    4.971
_exptl_absorpt_correction_T_max  0.7254
_exptl_absorpt_correction_T_min  0.4665
_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 bronze'
_exptl_crystal_density_diffrn    1.678
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.706
_refine_diff_density_min         -1.287
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         10190
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0959
_refine_ls_R_factor_gt           0.0496
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0306P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0799
_refine_ls_wR_factor_ref         0.0925
_reflns_number_gt                6769
_reflns_number_total             10190
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3sc52742e.txt
_cod_data_source_block           6
_cod_original_cell_volume        3368.97(18)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1513614