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_7128772
_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         '2(C37 H20 Cl8 N O7 P Si), 3(C H2 Cl2)'
_chemical_formula_sum            'C77 H46 Cl22 N2 O14 P2 Si2'
_chemical_formula_weight         2121.18
_chemical_properties_physical    Moisture-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method
;
FinalCif V85 by Daniel Kratzert, Freiburg 2021,
https://github.com/dkratzert/FinalCif
;
_audit_update_record
;
2021-06-20 deposited with the CCDC.	2021-07-27 downloaded from the CCDC.
;
_cell_angle_alpha                83.309(3)
_cell_angle_beta                 88.887(2)
_cell_angle_gamma                67.403(3)
_cell_formula_units_Z            1
_cell_length_a                   11.1778(8)
_cell_length_b                   11.9331(9)
_cell_length_c                   17.3665(12)
_cell_measurement_reflns_used    1432
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.066
_cell_measurement_theta_min      2.335
_cell_volume                     2123.2(3)
_computing_cell_refinement       'SAINT V8.40A'
_computing_data_collection       'Bruker BIS V6.2.14/2020-04-30'
_computing_data_reduction        'SAINT V8.40A'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III'
_diffrn_measured_fraction_theta_full 0.933
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE dual wavelength Mo/Cu'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_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  0.0835
_diffrn_reflns_av_unetI/netI     0.0668
_diffrn_reflns_Laue_measured_fraction_full 0.933
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_number            6981
_diffrn_reflns_point_group_measured_fraction_full 0.933
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_theta_full        24.996
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         1.974
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.837
_exptl_absorpt_correction_T_max  0.745492
_exptl_absorpt_correction_T_min  0.566613
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
TWINABS - Bruker AXS scaling for twinned crystals - Version 2012/1: Krause, L.,
Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.659
_exptl_crystal_description       block
_exptl_crystal_F_000             1066
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.186
_exptl_crystal_size_min          0.104
_refine_diff_density_max         0.555
_refine_diff_density_min         -0.419
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         6981
_refine_ls_number_restraints     477
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_gt           0.0530
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+6.1257P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1134
_refine_ls_wR_factor_ref         0.1207
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5828
_reflns_number_total             6981
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
'The data was integrated as a 2-component twin.'
_twin_individual_id              2
_twin_individual_twin_matrix_11  -0.00931
_twin_individual_twin_matrix_12  -0.03908
_twin_individual_twin_matrix_13  1.00304
_twin_individual_twin_matrix_21  0.99689
_twin_individual_twin_matrix_22  -0.02071
_twin_individual_twin_matrix_23  0.01685
_twin_individual_twin_matrix_31  0.01008
_twin_individual_twin_matrix_32  0.99611
_twin_individual_twin_matrix_33  0.09212
_cod_data_source_file            d1cc03452a2.cif
_cod_data_source_block           mo_dh431_0m_4
_cod_depositor_comments
'Adding full bibliography for 7128765--7128778.cif.'
_cod_database_code               7128772
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.837
_shelx_estimated_absorpt_t_max   0.918
_olex2_diffrn_ambient_temperature_device 'Oxford Cryostream 800'
_shelx_res_checksum              42989