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_1546250
_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
'C49 H108 O16 S3 Si4 U, C18 H36 K N2 O6, C7 H8'
_chemical_formula_sum            'C74 H152 K N2 O22 S3 Si4 U'
_chemical_formula_weight         1907.65
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2017-03-03 deposited with the CCDC.
2017-05-26 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 99.042(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.8270(3)
_cell_length_b                   24.6484(5)
_cell_length_c                   14.3945(4)
_cell_measurement_reflns_used    12887
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      75.4480
_cell_measurement_theta_min      3.6550
_cell_volume                     4844.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1333
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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    -60.00  31.00   1.00   10.00    --  -42.26  37.00  90.00   91
  2  \w    -32.00  73.00   1.00   10.00    --   42.26 -77.00-120.00  105
  3  \w     64.00 106.00   1.00   40.00    --  110.51 -94.00 -90.00   42
  4  \w     83.00 113.00   1.00   40.00    --  110.51-125.00-180.00   30
  5  \w     39.00 119.00   1.00   40.00    --  110.51 -45.00-150.00   80
  6  \w     87.00 157.00   1.00   40.00    --  110.51  30.00-180.00   70
  7  \w     85.00 174.00   1.00   40.00    --  110.51  45.00  30.00   89
  8  \w    114.00 176.00   1.00   40.00    --  110.51  45.00 120.00   62
  9  \w     87.00 171.00   1.00   40.00    --  110.51  30.00  90.00   84
 10  \w     82.00 109.00   1.00   40.00    --  110.51 -94.00  30.00   27
 11  \w     55.00 117.00   1.00   40.00    --  110.51 -61.00  90.00   62
 12  \w     40.00 135.00   1.00   40.00    --  110.51 -61.00   0.00   95
 13  \w     37.00 122.00   1.00   40.00    --  110.51-125.00 -90.00   85
 14  \w     35.00 106.00   1.00   40.00    --  110.51 -94.00   0.00   71
 15  \w     32.00  59.00   1.00   40.00    --  110.51 -94.00-150.00   27
 16  \w    -28.00  -1.00   1.00   10.00    --   42.26 -19.00-120.00   27
 17  \w    -28.00  13.00   1.00   10.00    --  -42.26  37.00-150.00   41
 18  \w   -104.00 -16.00   1.00   10.00    --  -42.26 -57.00 -60.00   88
 19  \w    -96.00  -3.00   1.00   10.00    --  -42.26 125.00  90.00   93
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_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  0.0802
_diffrn_reflns_av_sigmaI/netI    0.0916
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            37530
_diffrn_reflns_theta_full        76.47
_diffrn_reflns_theta_max         76.47
_diffrn_reflns_theta_min         3.24
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.686
_exptl_absorpt_correction_T_max  0.562
_exptl_absorpt_correction_T_min  0.292
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.38.41 (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 intense orange'
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2002
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_refine_diff_density_max         5.562
_refine_diff_density_min         -3.158
_refine_diff_density_rms         0.161
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.027(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     989
_refine_ls_number_reflns         15546
_refine_ls_number_restraints     457
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0722
_refine_ls_R_factor_gt           0.0627
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0887P)^2^+4.1312P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1516
_refine_ls_wR_factor_ref         0.1607
_reflns_number_gt                13787
_reflns_number_total             15546
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7sc01111c2.cif
_cod_data_source_block           mf230
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1546250
_publcif_datablock.id            {90840497-cb61-404c-ae9c-2aec6e2c724e}