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_1546247
_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_absolute_configuration rmad
_chemical_formula_moiety         'C48 H108 O16 Si4 U, C18 H36 K N2 O6'
_chemical_formula_sum            'C66 H144 K N2 O22 Si4 U'
_chemical_formula_weight         1707.31
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.92909(16)
_cell_length_b                   26.18261(18)
_cell_length_c                   26.16679(16)
_cell_measurement_reflns_used    75093
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      75.2310
_cell_measurement_theta_min      3.7350
_cell_volume                     17764.4(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (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 5.1333
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_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    -22.00  25.00   1.00    1.50    --  -42.20  77.00 -30.00   47
  2  \w    -67.00  27.00   1.00    1.50    --  -42.20  37.00-120.00   94
  3  \w      2.00  49.00   1.00    1.50    --   42.20 -99.00 -60.00   47
  4  \w     60.00  86.00   1.00    1.50    --   42.20-125.00-150.00   26
  5  \w     40.00 119.00   1.00    6.00    --  109.26 -45.00-180.00   79
  6  \w     64.00 114.00   1.00    6.00    --  109.26-111.00 -30.00   50
  7  \w     89.00 115.00   1.00    6.00    --  109.26-111.00  90.00   26
  8  \w     92.00 118.00   1.00    6.00    --  109.26 -30.00 150.00   26
  9  \w     96.00 177.00   1.00    6.00    --  109.26  45.00  90.00   81
 10  \w    133.00 174.00   1.00    6.00    --  109.26 111.00  90.00   41
 11  \w    132.00 158.00   1.00    6.00    --  109.26 111.00 150.00   26
 12  \w     50.00  77.00   1.00    6.00    --  109.26 -30.00 150.00   27
 13  \w     38.00 138.00   1.00    6.00    --  109.26 -30.00  60.00  100
 14  \w     51.00 108.00   1.00    6.00    --  109.26 -94.00 150.00   57
 15  \w     36.00  62.00   1.00    6.00    --  109.26-111.00  90.00   26
 16  \w     34.00 128.00   1.00    6.00    --  109.26 -77.00   0.00   94
 17  \w     37.00 106.00   1.00    6.00    --  109.26 -94.00-150.00   69
 18  \w     31.00 149.00   1.00    6.00    --  109.26 -15.00 -90.00  118
 19  \w     23.00  97.00   1.00    1.50    --   42.20-125.00  60.00   74
 20  \w   -115.00 -18.00   1.00    1.50    --  -42.20 -37.00  60.00   97
;
_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  0.0346
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            134443
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.505
_diffrn_reflns_theta_min         3.376
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.590
_exptl_absorpt_correction_T_max  0.38803
_exptl_absorpt_correction_T_min  0.31635
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Spherical absorption correction using equivalent radius
and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_description       plate
_exptl_crystal_F_000             7176
_exptl_crystal_size_max          0.398
_exptl_crystal_size_mid          0.261
_exptl_crystal_size_min          0.144
_exptl_crystal_size_rad          0.1212
_refine_diff_density_max         1.753
_refine_diff_density_min         -1.698
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.108(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1802
_refine_ls_number_reflns         36333
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0301
_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^)+(0.0157P)^2^+30.2146P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0677
_refine_ls_wR_factor_ref         0.0683
_reflns_Friedel_coverage         0.875
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                35302
_reflns_number_total             36333
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc01111c2.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        17764.41(19)
_cod_database_code               1546247
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              33073