Thermodynamic <i>versus</i> kinetic control in substituent redistribution reactions of silylium ions steered by the counteranion.
Omann, Lukas; Pudasaini, Bimal; Irran, Elisabeth; Klare, Hendrik F. T.; Baik, Mu-Hyun; Oestreich, Martin; Chemical science 9 (2018) 5600–5607; doi:10.1039/c8sc01833b

data_1549432
_publ_section_title
;
 Thermodynamic <i>versus</i> kinetic control in substituent redistribution
 reactions of silylium ions steered by the counteranion.
;
_journal_issue                   25
_journal_name_full               'Chemical science'
_journal_page_first              5600
_journal_page_last               5607
_journal_paper_doi               10.1039/c8sc01833b
_journal_volume                  9
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C13 H25 B11 Br6 Si, C6 H4 Cl2'
_chemical_formula_sum            'C19 H29 B11 Br6 Cl2 Si'
_chemical_formula_weight         954.78
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Hygroscopic,Oxygen-sensitive
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_audit_update_record
;
2018-01-22 deposited with the CCDC.
2018-05-21 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 100.5518(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.26054(14)
_cell_length_b                   38.4104(6)
_cell_length_c                   8.64061(13)
_cell_measurement_reflns_used    5274
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      73.3700
_cell_measurement_theta_min      4.5150
_cell_volume                     3347.78(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5435
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, 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  0.0309
_diffrn_reflns_av_sigmaI/netI    0.0298
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            6169
_diffrn_reflns_theta_full        67.49
_diffrn_reflns_theta_max         67.49
_diffrn_reflns_theta_min         4.53
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.566
_exptl_absorpt_correction_T_max  0.1949
_exptl_absorpt_correction_T_min  0.0988
_exptl_absorpt_correction_type   analytical
_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)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.894
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1824
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.029
_refine_diff_density_min         -1.757
_refine_diff_density_rms         0.194
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.07(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         3859
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0517
_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^)+(0.0878P)^2^+31.1853P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1337
_refine_ls_wR_factor_ref         0.1345
_reflns_number_gt                3817
_reflns_number_total             3859
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8sc01833b2.cif
_cod_data_source_block           cu-2481
_cod_depositor_comments
'Adding full bibliography for 1549430--1549432.cif.'
_cod_original_cell_volume        3347.77(9)
_cod_original_sg_symbol_H-M      Cc
_cod_database_code               1549432