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_1546246
_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         '2(C58 H123 K N O16 Si4 U), C7 H8'
_chemical_formula_sum            'C123 H254 K2 N2 O32 Si8 U2'
_chemical_formula_weight         3052.25
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_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                   92.6284(8)
_cell_length_b                   24.32104(17)
_cell_length_c                   13.71515(11)
_cell_measurement_reflns_used    26500
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      75.8030
_cell_measurement_theta_min      3.7000
_cell_volume                     30897.8(4)
_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 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     -6.00  32.00   0.50    1.00    --  -41.04  57.00 -90.00   76
  2  \w    -66.00  25.00   0.50    1.00    --  -41.04  38.00  90.00  182
  3  \w    -60.00  33.00   0.50    1.00    --  -41.04  38.00-180.00  186
  4  \w      3.00  71.00   0.50    1.00    --   41.04 -99.00 -30.00  136
  5  \w     63.00  89.00   0.50    1.00    --   41.04-125.00-180.00   52
  6  \w     87.00 113.00   0.50    4.00    --  111.85-125.00-150.00   52
  7  \w     60.00 122.00   0.50    4.00    --  111.85-125.00   0.00  124
  8  \w     62.00 104.00   0.50    4.00    --  111.85 -94.00 150.00   84
  9  \w     46.00 126.00   0.50    4.00    --  111.85 -45.00 120.00  160
 10  \w     42.00 123.00   0.50    4.00    --  111.85 -45.00  30.00  162
 11  \w    121.00 170.00   0.50    4.00    --  111.85  45.00-150.00   98
 12  \w     96.00 176.00   0.50    4.00    --  111.85  30.00-180.00  160
 13  \w     94.00 175.00   0.50    4.00    --  111.85 125.00  30.00  162
 14  \w     99.00 172.00   0.50    4.00    --  111.85 125.00 120.00  146
 15  \w     98.00 168.00   0.50    4.00    --  111.85  77.00  90.00  140
 16  \w     30.00 109.00   0.50    4.00    --  111.85 -94.00  60.00  158
 17  \w    -59.00 -16.00   0.50    1.00    --  -41.04  57.00 -90.00   86
;
_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  0.0395
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       112
_diffrn_reflns_limit_h_min       -116
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            48571
_diffrn_reflns_point_group_measured_fraction_full 0.808
_diffrn_reflns_point_group_measured_fraction_max 0.785
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.194
_diffrn_reflns_theta_min         3.731
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.453
_exptl_absorpt_correction_T_max  0.323
_exptl_absorpt_correction_T_min  0.162
_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            'dark brown'
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_description       plate
_exptl_crystal_F_000             12768
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.202
_refine_diff_density_max         1.108
_refine_diff_density_min         -1.151
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details
;
 Flack x determined using 4170 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.028(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     818
_refine_ls_number_reflns         12702
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0255
_refine_ls_R_factor_gt           0.0252
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0457P)^2^+20.6727P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0639
_refine_ls_wR_factor_ref         0.0642
_reflns_Friedel_coverage         0.517
_reflns_Friedel_fraction_full    0.597
_reflns_Friedel_fraction_max     0.559
_reflns_number_gt                12528
_reflns_number_total             12702
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc01111c2.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        30897.7(4)
_cod_database_code               1546246
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              72095