Chalcogen-Atom Transfer and Exchange Reactions of NHC-Stabilized Heavier Silaacylium Ions
Sarkar, Debotra; Wendel, Daniel; Ahmad, Syed Usman; Szilvási, Tibor; Pöthig, Alexander; Inoue, Shigeyoshi; Dalton Trans.  (2017) –; doi:10.1039/C7DT03998K

data_7044576
_publ_section_title
;
 Chalcogen-Atom Transfer and Exchange Reactions of NHC-Stabilized Heavier
 Silaacylium Ions
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT03998K
_journal_year                    2017
_chemical_formula_moiety         'C38 H49 N4 Se Si, 3(C2 H3 N), Cl'
_chemical_formula_sum            'C44 H58 Cl N7 Se Si'
_chemical_formula_weight         827.47
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_update_record
;
2017-10-11 deposited with the CCDC.
2017-10-27 downloaded from the CCDC.
;
_cell_angle_alpha                75.462(2)
_cell_angle_beta                 77.484(2)
_cell_angle_gamma                82.684(2)
_cell_formula_units_Z            4
_cell_length_a                   15.2505(4)
_cell_length_b                   16.9089(4)
_cell_length_c                   17.7605(3)
_cell_measurement_reflns_used    14403
_cell_measurement_temperature    150
_cell_measurement_theta_max      73.3350
_cell_measurement_theta_min      2.6190
_cell_volume                     4314.98(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.02(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5435
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega   33.00   76.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.4393  -45.0000  -30.0000 43

  2 omega   40.00   66.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.4393  -30.0000   30.0000 26

  3 omega   38.00   66.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.4393  -30.0000   60.0000 28

  4 omega   37.00   66.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.4393  -30.0000   90.0000 29

  5 omega   37.00  135.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.4393  -77.0000   60.0000 98

  6 omega   69.00  119.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.4393 -125.0000   60.0000 50

  7 omega   34.00   84.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       41.7472 -125.0000  -60.0000 50

  8 omega   19.00   98.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       41.7472 -125.0000 -180.0000 79

  9 omega   35.00   69.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.4393  -45.0000 -120.0000 34

 10 omega   29.00   98.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.4393  -94.0000  -90.0000 69

 11 omega   96.00  121.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.4393 -125.0000 -120.0000 25

 12 omega   67.00  103.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.4393  -94.0000 -180.0000 36

 13 omega   44.00   70.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.4393 -125.0000 -120.0000 26

 14 omega   29.00   80.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.4393  -94.0000  -30.0000 51

 15 omega   34.00   59.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.4393  -30.0000    0.0000 25

 16 omega   33.00  157.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.4393    0.0000  -30.0000 124

 17 omega   82.00  157.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.4393   45.0000    0.0000 75

 18 omega   33.00   70.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.4393  -45.0000 -180.0000 37

 19 omega  -66.00   20.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.7472   39.0000   75.0000 86

 20 omega   30.00   59.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.4393  -30.0000  120.0000 29

 21 omega  -38.00   -4.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.7472  125.0000  150.0000 34

 22 omega -114.00   -9.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.7472  -19.0000 -120.0000 105

;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0848466000
_diffrn_orient_matrix_UB_12      0.0442220000
_diffrn_orient_matrix_UB_13      -0.0452527000
_diffrn_orient_matrix_UB_21      -0.0535900000
_diffrn_orient_matrix_UB_22      0.0833938000
_diffrn_orient_matrix_UB_23      0.0015547000
_diffrn_orient_matrix_UB_31      0.0264709000
_diffrn_orient_matrix_UB_32      -0.0014844000
_diffrn_orient_matrix_UB_33      0.0793004000
_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  0.0333
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            29348
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        66.60
_diffrn_reflns_theta_max         66.60
_diffrn_reflns_theta_min         2.62
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.310
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79294
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.184
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.082
_refine_diff_density_max         0.786
_refine_diff_density_min         -0.734
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1007
_refine_ls_number_reflns         15234
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0430
_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^)+(0.0663P)^2^+3.7690P] WHERE P=(FO^2^+2FC^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1169
_refine_ls_wR_factor_ref         0.1264
_reflns_number_gt                12998
_reflns_number_total             15234
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c7dt03998k2.cif
_cod_data_source_block           compound3
_cod_database_code               7044576
_shelx_res_checksum              59452