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_7128775
_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         'C37 H22 Cl8 N O5 P Si, 2(C H2 Cl2)'
_chemical_formula_sum            'C39 H26 Cl12 N O5 P Si'
_chemical_formula_weight         1073.07
_chemical_properties_physical    Moisture-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-12-21
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6208)
;
_audit_update_record
;
2021-06-20 deposited with the CCDC.	2021-07-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.5399(11)
_cell_length_b                   16.4844(12)
_cell_length_c                   17.4224(11)
_cell_measurement_reflns_used    9188
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      27.07
_cell_measurement_theta_min      2.47
_cell_volume                     4463.0(5)
_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 C14 detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CPAD detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8-Venture Dual Source'
_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  0.0954
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            239193
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.566
_diffrn_reflns_theta_min         2.147
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_type              'Incoatec I\ms 3.0'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.852
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6539
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1500 before and 0.0824 after correction.
The Ratio of minimum to maximum transmission is 0.8770.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_description       needle
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.315
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details
;
 Flack x determined using 4442 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.015(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         10295
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0269
_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^)+(0.0345P)^2^+1.2910P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0634
_refine_ls_wR_factor_ref         0.0654
_reflns_Friedel_coverage         0.934
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                9665
_reflns_number_total             10295
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc03452a2.cif
_cod_data_source_block           mo_dhsb43_0ma
_cod_depositor_comments
'Adding full bibliography for 7128765--7128778.cif.'
_cod_database_code               7128775
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C00Q(H00Q)
2.b Secondary CH2 refined with riding coordinates:
 C01E(H01L,H01M), C01L(H01N,H01O)
2.c Aromatic/amide H refined with riding coordinates:
 C00T(H00T), C00X(H00X), C00Y(H00Y), C010(H010), C012(H012), C014(H014),
 C015(H015), C017(H017), C018(H018), C019(H019), C01A(H01A), C01C(H01C),
 C01D(H01D), C01G(H01G), C01H(H01H), C01I(H01I), C01J(H01J), C01K(H01K)
2.d Idealised Me refined as rotating group:
 C01N(H01B,H01E,H01F)
;
_shelx_res_checksum              59492
_olex2_submission_special_instructions 'No special instructions were received'