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_1546249
_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         'C26 H48 K2 O12 S6'
_chemical_formula_sum            'C26 H48 K2 O12 S6'
_chemical_formula_weight         823.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                90
_cell_angle_beta                 111.465(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.133(2)
_cell_length_b                   9.4570(7)
_cell_length_c                   22.775(2)
_cell_measurement_reflns_used    3055
_cell_measurement_temperature    100.02(11)
_cell_measurement_theta_max      73.5940
_cell_measurement_theta_min      4.1580
_cell_volume                     3835.1(7)
_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      100.02(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.982
_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    -98.00  47.00   1.00   10.00    --  -40.66   0.00 150.00  145
  2  \w    -57.00   2.00   1.00   10.00    --  -40.66  57.00  30.00   59
  3  \w   -114.00 -60.00   1.00   10.00    --  -40.66 -38.00 150.00   54
  4  \w     28.00  97.00   1.00   10.00    --   40.66-125.00 150.00   69
  5  \w     27.00  76.00   1.00   10.00    --   40.66-125.00 -30.00   49
  6  \w     28.00  63.00   1.00   10.00    --   40.66-125.00 -90.00   35
  7  \w     31.00  56.00   1.00   10.00    --   40.66-125.00  65.00   25
  8  \w     37.00  65.00   1.00   40.00    --  110.60-125.00 150.00   28
  9  \w     38.00 140.00   1.00   40.00    --  110.60 -61.00-180.00  102
 10  \w     43.00 160.00   1.00   40.00    --  110.60 -15.00 120.00  117
 11  \w     96.00 124.00   1.00   40.00    --  110.60  77.00 -60.00   28
 12  \w     51.00  98.00   1.00   40.00    --  110.60 -94.00 -90.00   47
 13  \w     42.00 139.00   1.00   40.00    --  110.60 -61.00  60.00   97
 14  \w     44.00 134.00   1.00   40.00    --  110.60 -30.00 -60.00   90
 15  \w     95.00 122.00   1.00   40.00    --  110.60 125.00-120.00   27
 16  \w     93.00 119.00   1.00   40.00    --  110.60-125.00  30.00   26
 17  \w     38.00  63.00   1.00   40.00    --  110.60-125.00  30.00   25
 18  \w     59.00 104.00   1.00   40.00    --  110.60 -94.00-180.00   45
 19  \w     81.00 122.00   1.00   40.00    --  110.60-125.00 150.00   41
 20  \w     89.00 155.00   1.00   40.00    --  110.60  45.00 150.00   66
 21  \w     53.00 140.00   1.00   40.00    --  110.60 -77.00 -60.00   87
;
_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  0.0946
_diffrn_reflns_av_unetI/netI     0.1225
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            9167
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.784
_diffrn_reflns_theta_min         2.481
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.699
_exptl_absorpt_correction_T_max  0.801
_exptl_absorpt_correction_T_min  0.635
_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            'pale yellow'
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_description       prism
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.134
_exptl_crystal_size_mid          0.109
_exptl_crystal_size_min          0.084
_refine_diff_density_max         0.843
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.907
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         9167
_refine_ls_number_restraints     1778
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.1504
_refine_ls_R_factor_gt           0.0829
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1334P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2090
_refine_ls_wR_factor_ref         0.2432
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4237
_reflns_number_total             9167
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc01111c2.cif
_cod_data_source_block           shelx
_cod_database_code               1546249
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              51159