Metathesis of a UV imido complex: a route to a terminal UV sulfide
Kelly, Rory P.; Falcone, Marta; Lamsfus, Carlos Alvarez; Scopelliti, Rosario; Maron, Laurent; Meyer, Karsten; Mazzanti, Marinella; Chem. Sci.  (2017) –; doi:10.1039/C7SC01111C

data_1546248
_publ_section_title
;
 Metathesis of a UV imido complex: a route to a terminal UV sulfide
;
_journal_name_full               'Chem. Sci.'
_journal_paper_doi               10.1039/C7SC01111C
_journal_year                    2017
_chemical_formula_moiety         'C48 H108 O16 S Si4 U, C18 H36 K N2 O6, C7 H8'
_chemical_formula_sum            'C73 H152 K N2 O22 S Si4 U'
_chemical_formula_weight         1831.51
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-02-28 deposited with the CCDC.
2017-05-26 downloaded from the CCDC.
;
_cell_angle_alpha                82.352(3)
_cell_angle_beta                 84.245(3)
_cell_angle_gamma                78.583(3)
_cell_formula_units_Z            4
_cell_length_a                   14.4445(4)
_cell_length_b                   14.4565(6)
_cell_length_c                   47.0418(18)
_cell_measurement_reflns_used    12905
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      75.4490
_cell_measurement_theta_min      3.1450
_cell_volume                     9515.4(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'CIFTAB (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5633
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -44.00 -16.00   1.00    2.00    --  -40.41 -57.00 120.00   28
  2  \w    -65.00  28.00   1.00    2.00    --  -40.41  38.00 150.00   93
  3  \w     38.00  72.00   1.00    2.00    --   40.41 -99.00 120.00   34
  4  \w     39.00  66.00   1.00    8.00    --  111.85-125.00  60.00   27
  5  \w     69.00 108.00   1.00    8.00    --  111.85 -94.00  30.00   39
  6  \w     98.00 144.00   1.00    8.00    --  111.85 -77.00   0.00   46
  7  \w     93.00 120.00   1.00    8.00    --  111.85-125.00  60.00   27
  8  \w     57.00 108.00   1.00    8.00    --  111.85 -94.00 -90.00   51
  9  \w     91.00 121.00   1.00    8.00    --  111.85-125.00-150.00   30
 10  \w     49.00  76.00   1.00    8.00    --  111.85-125.00-150.00   27
 11  \w     41.00 127.00   1.00    8.00    --  111.85 -61.00 -60.00   86
 12  \w     89.00 173.00   1.00    8.00    --  111.85  30.00  60.00   84
 13  \w    106.00 176.00   1.00    8.00    --  111.85 125.00 -30.00   70
 14  \w    139.00 177.00   1.00    8.00    --  111.85  77.00-150.00   38
 15  \w    119.00 178.00   1.00    8.00    --  111.85 125.00 -90.00   59
 16  \w     59.00 140.00   1.00    8.00    --  111.85 -30.00-150.00   81
 17  \w     40.00 160.00   1.00    8.00    --  111.85 -15.00  30.00  120
 18  \w     40.00 114.00   1.00    8.00    --  111.85 -45.00-180.00   74
 19  \w     28.00 115.00   1.00    2.00    --   40.41  38.00-120.00   87
 20  \w    -95.00  -5.00   1.00    2.00    --  -40.41 125.00-120.00   90
 21  \w   -114.00 -12.00   1.00    2.00    --  -40.41 -77.00   0.00  102
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0811
_diffrn_reflns_av_unetI/netI     0.0375
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       59
_diffrn_reflns_limit_l_min       -59
_diffrn_reflns_number            37472
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.401
_diffrn_reflns_theta_min         2.852
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.387
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.401
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark brown'
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_description       plate
_exptl_crystal_F_000             3852
_exptl_crystal_size_max          0.264
_exptl_crystal_size_mid          0.111
_exptl_crystal_size_min          0.052
_refine_diff_density_max         4.635
_refine_diff_density_min         -4.135
_refine_diff_density_rms         0.209
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1973
_refine_ls_number_reflns         37472
_refine_ls_number_restraints     978
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0931
_refine_ls_R_factor_gt           0.0906
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0799P)^2^+213.4700P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2307
_refine_ls_wR_factor_ref         0.2320
_reflns_Friedel_coverage         0.000
_reflns_number_gt                35377
_reflns_number_total             37472
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc01111c2.cif
_cod_data_source_block           shelx
_cod_database_code               1546248
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              15321