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_7128768
_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         'C36 H20 Cl8 N O5 P Si, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C36.5 H21 Cl9 N O5 P Si'
_chemical_formula_weight         931.65
_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-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                109.982(5)
_cell_angle_beta                 90.192(5)
_cell_angle_gamma                107.734(6)
_cell_formula_units_Z            4
_cell_length_a                   15.162(2)
_cell_length_b                   16.186(2)
_cell_length_c                   18.463(3)
_cell_measurement_reflns_used    9145
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      27.10
_cell_measurement_theta_min      2.22
_cell_volume                     4026.6(10)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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_unetI/netI     0.1871
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            14102
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.954
_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    0.739
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 68210 reflections, Rint = 0.1095
 (15428 with I > 3sig(I), Rint = 0.0671)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_description       plates,
_exptl_crystal_F_000             1876
_exptl_crystal_size_max          0.124
_exptl_crystal_size_mid          0.116
_exptl_crystal_size_min          0.059
_refine_diff_density_max         0.728
_refine_diff_density_min         -0.748
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     964
_refine_ls_number_reflns         14102
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1742
_refine_ls_R_factor_gt           0.0827
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1206P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2036
_refine_ls_wR_factor_ref         0.2379
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6894
_reflns_number_total             14102
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc03452a2.cif
_cod_data_source_block           p-1_a
_cod_depositor_comments
'Adding full bibliography for 7128765--7128778.cif.'
_cod_original_formula_sum        'C36.50 H21 Cl9 N O5 P Si'
_cod_database_code               7128768
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.958
_shelx_estimated_absorpt_t_min   0.914
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C13B(H13B), C13A(H13A)
1.b Secondary CH2 refined with riding coordinates:
 C031(H03A,H03B)
1.c Aromatic/amide H refined with riding coordinates:
 C01F(H01F), C01G(H01G), C01H(H01H), C01O(H01O), C01Q(H01Q), C01R(H01R),
 C01T(H01T), C01V(H01V), C01X(H01X), C01Y(H01Y), C022(H022), C023(H023),
 C026(H026), C028(H028), C02A(H02A), C02B(H02B), C02D(H02D), C02E(H02E),
 C02G(H02G), C02H(H02H), C02I(H02I), C02J(H02J), C02K(H02K), C02L(H02L),
 C02M(H02M), C02N(H02N), C02O(H02O), C02Q(H02Q), C02R(H02R), C02S(H02S),
 C02T(H02T), C02U(H02U), C02V(H02V), C02W(H02W), C02X(H02X), C02Y(H02Y),
 C02Z(H02Z), C030(H030)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 88 electrons were 
found in a volume of 362\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 0.5[CH2Cl2] 
per Formula Unit which account for 84 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              46164
_shelx_fab_checksum              89392
_olex2_submission_special_instructions 'No special instructions were received'