An Investigation into the Brønsted Acidity of the Perfluorinated Alkoxy Silanes {(F3C)3CO}3SiH and {(F6C5)3CO}2Si(Cl)H
Feige, Felix; Malaspina, Lorraine A.; Kleemiss, Florian; Kögel, Julius F.; Ketkov, Sergey Yu.; Hupf, Emanuel; Grabowsky, Simon; Beckmann, Jens; Dalton Transactions  (2023) –; doi:10.1039/D3DT00299C

data_7712755
_publ_section_title
;
 An Investigation into the Br\/onsted Acidity of the Perfluorinated Alkoxy
 Silanes {(F3C)3CO}3SiH and {(F6C5)3CO}2Si(Cl)H
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00299C
_journal_year                    2023
_chemical_formula_moiety         'C12 H1 F27.025 O3 Si1'
_chemical_formula_sum            'C12 H F27.02 O3 Si'
_chemical_formula_weight         734.69
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      147
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_atom_sites_solution_hydrogens   difmap
_audit_creation_date             2021-12-02T20:43:57-00:00
_audit_update_record
;
2023-01-23 deposited with the CCDC.	2023-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   10.4987(3)
_cell_length_b                   10.4987(3)
_cell_length_c                   11.6734(4)
_cell_measurement_reflns_used    9935
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      34.64
_cell_measurement_theta_min      2.24
_cell_measurement_wavelength     0.71073
_cell_volume                     1114.29(6)
_computing_cell_refinement       'SAINT V8.40A integration software'
_computing_data_collection       'Bruker APEX2 software'
_computing_data_reduction        'SORTAV (Blessing, 1995)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      120.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       '\f or \w oscillation scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0108
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            53400
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.504
_diffrn_reflns_theta_min         2.84
_exptl_absorpt_coefficient_mu    0.348
_exptl_absorpt_correction_T_max  0.966
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.19
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             708
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.256
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.19
_refine_diff_density_min         -0.165
_refine_diff_density_rms         0.034
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         2264
_refine_ls_number_restraints     247
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0298
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0677P)^2^+0.0160P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0867
_refine_ls_wR_factor_ref         0.0925
_reflns_Friedel_coverage         0
_reflns_number_gt                1881
_reflns_number_total             2264
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00299c2.cif
_cod_data_source_block           FeigeF200507
_cod_original_cell_volume        1114.29(7)
_cod_database_code               7712755
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
        1. Twinned data refinement
 Scales: 0.501(4)
 0.499(4)
        2. Restrained distances
 Si1-H1 = Si1A-H1A
 1.458 with sigma of 0.05
 F2A-C2A \\sim F1A-C2A \\sim F3A-C2A
 with sigma of 0.02
 C4-C1 \\sim C2A-C1A \\sim C3A-C1A
 with sigma of 0.02
 F6A-C3A \\sim F5A-C3A \\sim F4A-C3A
 with sigma of 0.02
 C3-C1 \\sim C4A-C1A \\sim C2B-C1
 with sigma of 0.02
 F9-C4 \\sim F7-C4 \\sim F8-C4
 with sigma of 0.02
 C7-C1 \\sim C2A-C1A \\sim C2B-C1 \\sim C6-C1A \\sim C4A-C1A \\sim C4-C1 \\sim
        C5-C1 \\sim C3-C1 \\sim C3A-C1A
 with sigma of 0.002
 Si1A-O1A \\sim Si1-O1
 with sigma of 0.02
 F6-C3 \\sim F5-C3 \\sim F4-C3
 with sigma of 0.02
 F1-C2B \\sim F2-C2B \\sim F3-C2B
 with sigma of 0.02
 Si1A-H1A \\sim Si1-H1
 with sigma of 0.01
        3. Rigid bond restraints
 Si1A, O1A, C1A
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 F10, C7, F4A, F1A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F11, C6, F2A, F9
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C1, O1, Si1
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C3A, F6A, F5A, F4A
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 F6, C3, F5, F4
 with sigma for 1-2 distances of 0.006 and sigma for 1-3 distances of 0.006
 F13, C5, F14, F12
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
        4. Uiso/Uaniso restraints and constraints
F1 \\sim F1A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
        0.08 within 1.7A
C1 \\sim C1A: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
        0.004 within 1.7A
O1 \\sim O1A: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
        0.004 within 1.7A
C3 \\sim C3A: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
        0.004 within 1.7A
C4A \\sim C4: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
        0.004 within 1.7A
C2B \\sim C2A: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
        0.004 within 1.7A
Uanis(F6) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(F4A) \\sim Ueq, Uanis(F5) \\sim
Ueq, Uanis(F5A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
        0.02
Uanis(C7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F9A) \\sim Ueq, Uanis(F9) \\sim Ueq: with sigma of 0.01 and sigma for
        terminal atoms of 0.01
Uanis(O1) \\sim Ueq, Uanis(O1A) \\sim Ueq: with sigma of 0.01 and sigma for
        terminal atoms of 0.02
Uanis(C1A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C6) \\sim Ueq, Uanis(F11) \\sim Ueq: with sigma of 0.005 and sigma for
        terminal atoms of 0.01
Uanis(C4A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.015
Uanis(F4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C3A) \\sim Ueq, Uanis(F6A) \\sim Ueq: with sigma of 0.01 and sigma for
        terminal atoms of 0.01
Uanis(F7A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.005
Uanis(F12) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(F14) \\sim Ueq: with sigma of
        0.01 and sigma for terminal atoms of 0.02
Uanis(F10) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F8A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
        Uiso(H1A) = Uiso(H1)
        5. Others
 1*[Sof(C3)+Sof(F4)+Sof(F5)+Sof(F6)+Sof(C4)+Sof(F7)+Sof(F8)+Sof(C2B)+Sof(F1)+
 Sof(F2)+Sof(F3)]+1*[Sof(C2A)+Sof(F3A)+Sof(C3A)+Sof(F5A)+Sof(F6A)+Sof(C4A)+
 Sof(F7A)+Sof(F8A)+Sof(F9A)]+1*[Sof(C6)+Sof(C7)+Sof(F10)+Sof(F11)+Sof(F12)+
 Sof(F13)+Sof(F14)+Sof(C5)]=1 with esd of 0.0001
 Sof(C3)=Sof(F4)=Sof(F5)=Sof(F6)=Sof(C4)=Sof(F7)=Sof(F8)=Sof(C2B)=Sof(F1)=
 Sof(F2)=Sof(F3)=FVAR(1)
 Sof(C2A)=Sof(F3A)=Sof(C3A)=Sof(F5A)=Sof(F6A)=Sof(C4A)=Sof(F7A)=Sof(F8A)=
 Sof(F9A)=FVAR(2)
 Sof(C6)=Sof(C7)=Sof(F10)=Sof(F11)=Sof(F12)=Sof(F13)=Sof(F14)=Sof(C5)=FVAR(3)
 Sof(O1A)=Sof(C1A)=1-FVAR(4)
 Sof(O1)=Sof(C1)=FVAR(4)
 Fixed Sof: Si1A(0.16667) F1A(0.55326) F2A(0.55326) F9(0.55326) Si1(0.16667)
 F4A(0.55326) H1A(0.16667) H1(0.16667)
 Fixed X: C5(0.614341)
 Fixed Y: C5(0.63362)
 Fixed Z: C5(0.85155)
;
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_res_checksum              43351