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_7128766
_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         'C38 H23 Cl8 O5 P Si, C H2 Cl2'
_chemical_formula_sum            'C39 H25 Cl10 O5 P Si'
_chemical_formula_weight         987.15
_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     dual
_audit_creation_date             2021-03-11
_audit_creation_method
;
Olex2 1.3
(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                94.060(3)
_cell_angle_beta                 106.632(3)
_cell_angle_gamma                117.844(3)
_cell_formula_units_Z            2
_cell_length_a                   11.9675(9)
_cell_length_b                   12.4047(10)
_cell_length_c                   16.8129(13)
_cell_measurement_reflns_used    9662
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      27.14
_cell_measurement_theta_min      2.61
_cell_volume                     2052.1(3)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (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 0.998
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II 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  0.0528
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            83194
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.262
_diffrn_reflns_theta_min         2.003
_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    0.792
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5926
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1012 before and 0.0696 after correction.
The Ratio of minimum to maximum transmission is 0.7949.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_description       block
_exptl_crystal_F_000             996
_exptl_crystal_size_max          0.271
_exptl_crystal_size_mid          0.103
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.723
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     516
_refine_ls_number_reflns         9087
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0331
_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^)+(0.0338P)^2^+2.0665P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0803
_refine_ls_wR_factor_ref         0.0843
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8071
_reflns_number_total             9087
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc03452a2.cif
_cod_data_source_block           mo_dh400_0m
_cod_depositor_comments
'Adding full bibliography for 7128765--7128778.cif.'
_cod_database_code               7128766
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.939
_shelx_estimated_absorpt_t_min   0.814
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl10-C39 \\sim Cl11-C39
 with sigma of 0.02
3. Others
 Sof(H39C)=Sof(H39D)=Sof(Cl11)=1-FVAR(1)
 Sof(Cl10)=Sof(H39A)=Sof(H39B)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C13(H13)
4.b Secondary CH2 refined with riding coordinates:
 C39(H39A,H39B), C39(H39C,H39D)
4.c Aromatic/amide H refined with riding coordinates:
 C22(H22), C34(H34), C26(H26), C15(H15), C19(H19), C25(H25), C24(H24),
 C18(H18), C28(H28), C32(H32), C16(H16), C23(H23), C38(H38), C29(H29), C36(H36),
  C35(H35), C37(H37), C31(H31), C30(H30)
4.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C)
;
_shelx_res_checksum              51829
_olex2_date_sample_data_collection 2021-01-10
_olex2_date_sample_submission    2021-01-10
_olex2_submission_special_instructions 'No special instructions were received'