Bis(perchlorocatecholato)silane and heteroleptic bidonors: hidden frustrated Lewis pairs resulting from ring strain.
Hartmann, Deborah; Braner, Sven; Greb, Lutz; Chemical communications (Cambridge, England) 57 (2021) 8572–8575; doi:10.1039/d1cc03452a

data_7128765
_publ_section_title
;
 Bis(perchlorocatecholato)silane and heteroleptic bidonors: hidden
 frustrated Lewis pairs resulting from ring strain.
;
_journal_issue                   69
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              8572
_journal_page_last               8575
_journal_paper_doi               10.1039/d1cc03452a
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C19 H10 Cl8 N2 O4 Si'
_chemical_formula_sum            'C19 H10 Cl8 N2 O4 Si'
_chemical_formula_weight         641.98
_chemical_properties_physical    Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-31
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-06-20 deposited with the CCDC.	2021-07-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.241(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.3910(13)
_cell_length_b                   8.8970(8)
_cell_length_c                   36.446(3)
_cell_measurement_reflns_used    9063
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      28.72
_cell_measurement_theta_min      2.69
_cell_volume                     4659.0(7)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker PhotonIII detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CPAD detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-III CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0676
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            89708
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.750
_diffrn_reflns_theta_min         2.239
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.052
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.5871
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1468 before and 0.0909 after correction. The Ratio of minimum to maximum transmission is 0.7872. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.831
_exptl_crystal_description       block
_exptl_crystal_F_000             2560
_exptl_crystal_size_max          0.344
_exptl_crystal_size_mid          0.239
_exptl_crystal_size_min          0.182
_refine_diff_density_max         0.782
_refine_diff_density_min         -0.547
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         6036
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0478
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0314P)^2^+35.7086P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1161
_refine_ls_wR_factor_ref         0.1220
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5316
_reflns_number_total             6036
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc03452a2.cif
_cod_data_source_block           mo_dh302h2_0m
_cod_depositor_comments
'Adding full bibliography for 7128765--7128778.cif.'
_cod_database_code               7128765
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.832
_shelx_estimated_absorpt_t_min   0.714
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C17(H17), C14(H14), C16(H16), C15(H15)
2.b Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              46958
_olex2_date_sample_data_collection 2019-12-04
_olex2_date_sample_submission    2019-12-04
_olex2_submission_special_instructions 'No special instructions were received'