Bis(catecholato)silanes: assessment, rationale and increase of silicon’s Lewis superacidity
Hartmann, Deborah; Schädler, Marcel; Greb, Lutz; Chemical Science  (2019) –; doi:10.1039/C9SC02167A

data_1551458
_publ_section_title
;
 Bis(catecholato)silanes: assessment, rationale and increase of
 silicon&#x2019;s Lewis superacidity
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC02167A
_journal_year                    2019
_chemical_formula_moiety         'C24 H30 F8 O6 P2 Si'
_chemical_formula_sum            'C24 H30 F8 O6 P2 Si'
_chemical_formula_weight         656.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-01-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-03-26 deposited with the CCDC.    2019-06-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.90(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.753(2)
_cell_length_b                   11.953(2)
_cell_length_c                   11.361(2)
_cell_measurement_reflns_used    2084
_cell_measurement_temperature    120
_cell_measurement_theta_max      26
_cell_measurement_theta_min      1
_cell_volume                     1389.6(5)
_computing_cell_refinement       'DENZO/SCALEPACK (Bruker AXS, 1997-2009)'
_computing_data_collection       'COLLECT (Bruker AXS, 1997-2009)'
_computing_data_reduction        'DENZO/SCALEPACK (Bruker AXS, 1997-2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'NONIUS KAPPA CCD'
_diffrn_measurement_method       O-Scan
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_unetI/netI     0.0617
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7789
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.052
_diffrn_reflns_theta_min         2.282
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.292
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_description       irregular
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.739
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         4058
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.1055
_refine_ls_R_factor_gt           0.0634
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0756P)^2^+1.5163P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1574
_refine_ls_wR_factor_ref         0.1769
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2738
_reflns_number_total             4058
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc02167a2.cif
_cod_data_source_block           ms29c_p2_1
_cod_original_cell_volume        1389.4(5)
_cod_database_code               1551458
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.892
_shelx_estimated_absorpt_t_min   0.880
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F4-C6 \\sim F4A-C6A
 with sigma of 0.02
 F2-C4 \\sim F2A-C4A
 with sigma of 0.02
 F3-C5 \\sim F3A-C5A
 with sigma of 0.02
 C1-C6 \\sim C1-C6A
 with sigma of 0.02
 C3-C4 \\sim C3-C4A
 with sigma of 0.02
 C6-C5 \\sim C6A-C5A
 with sigma of 0.02
 C4-C5 \\sim C4A-C5A
 with sigma of 0.02
 F4-C1 \\sim F4A-C1
 with sigma of 0.04
 F4-C5 \\sim F4A-C5A
 with sigma of 0.04
 F2-C3 \\sim F2A-C3
 with sigma of 0.04
 F2-C5 \\sim F2A-C5A
 with sigma of 0.04
 F3-C6 \\sim F3A-C6A
 with sigma of 0.04
 F3-C4 \\sim F3A-C4A
 with sigma of 0.04
 C1-C5 \\sim C1-C5A
 with sigma of 0.04
 C3-C5 \\sim C3-C5A
 with sigma of 0.04
 C6-C4 \\sim C6A-C4A
 with sigma of 0.04
 P1-C7 \\sim P1-C7A
 with sigma of 0.02
 C7-C8 \\sim C7A-C8A
 with sigma of 0.02
 P1-C8 \\sim P1-C8A
 with sigma of 0.04
 P1-C11 \\sim P1-C11A
 with sigma of 0.02
 C11-C12 \\sim C11A-C12A
 with sigma of 0.02
 P1-C12 \\sim P1-C12A
 with sigma of 0.04
3. Rigid body (RIGU) restrains
 C12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(F4A)=Sof(C6A)=Sof(F3A)=Sof(C5A)=Sof(C4A)=Sof(F2A)=1-FVAR(1)
 Sof(F4)=Sof(F2)=Sof(F3)=Sof(C6)=Sof(C4)=Sof(C5)=FVAR(1)
 Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=1-FVAR(2)
 Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=FVAR(2)
 Sof(C11A)=Sof(H11C)=Sof(H11D)=Sof(C12A)=Sof(H12D)=Sof(H12E)=Sof(H12F)=1-FVAR(3)
 Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=FVAR(3)
5.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C7(H7A,H7B), C11(H11A,H11B), C7A(H7AA,H7AB), C11A(H11C,H11D)
5.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C8(H8A,H8B,H8C), C12(H12A,H12B,H12C), C8A(H8AA,H8AB,
 H8AC), C12A(H12D,H12E,H12F)
;
_shelx_res_checksum              67736
_olex2_submission_special_instructions 'No special instructions were received'