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_7712756
_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         'C38 H1 Cl1 F30 O2 Si1'
_chemical_formula_sum            'C38 H Cl F30 O2 Si'
_chemical_formula_weight         1122.920
_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_Int_Tables_number      14
_audit_creation_date             2021-11-22
_audit_creation_method
;
Olex2 1.5-dev
(compiled Nov 19 2021 09:31:55, GUI svn.r6287)
;
_audit_update_record
;
2023-01-23 deposited with the CCDC.	2023-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.871(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2008(4)
_cell_length_b                   14.2304(4)
_cell_length_c                   20.1079(6)
_cell_measurement_reflns_used    9001
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.51
_cell_measurement_theta_min      2.53
_cell_volume                     3667.17(19)
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-dev (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      99.92
_diffrn_measured_fraction_theta_full 0.9995
_diffrn_measured_fraction_theta_max 0.9997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_Laue_measured_fraction_full 0.9995
_diffrn_reflns_Laue_measured_fraction_max 0.9997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            120588
_diffrn_reflns_point_group_measured_fraction_full 0.9995
_diffrn_reflns_point_group_measured_fraction_max 0.9997
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.09
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.331
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.7177
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0992 before and 0.0476 after correction.
The Ratio of minimum to maximum transmission is 0.9619.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.034
_exptl_crystal_description       plate
_exptl_crystal_F_000             2187.699
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.3099
_refine_diff_density_min         -0.3122
_refine_diff_density_rms         0.0636
_refine_ls_d_res_high            0.7500
_refine_ls_d_res_low             9.7608
_refine_ls_extinction_coef       0.00119(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0732
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    3
_refine_ls_number_parameters     667
_refine_ls_number_reflns         9084
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.0720
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0198
_refine_ls_shift/su_max          -0.0007
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0132P)^2^+0.3889P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0347
_refine_ls_wR_factor_ref         0.0369
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -17
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              -12
_reflns_number_gt                7687
_reflns_number_total             9084
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3dt00299c2.cif
_cod_data_source_block           FeigeF191018_0m
_cod_database_code               7712756
_olex2_refinement_description
;
1. Shared sites
{Si1, Si1a}
2. Restrained distances
 Cl1-Si1 \\sim Cl1a-Si1a
 with sigma of 0.001
 Cl1-H1 \\sim Cl1a-H1a
 with sigma of 0.04
 Si1-H1 \\sim Si1a-H1a
 with sigma of 0.001
 Cl1-O1 \\sim Cl1a-O1
 with sigma of 0.04
 O2-H1 \\sim O2-H1a
 with sigma of 0.04
 O1-H1 \\sim O1-H1a
 with sigma of 0.04
 Cl1-O2 \\sim Cl1a-O2
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Si1a \\sim Si1: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
4. Others
 Sof(Cl1a)=Sof(Si1a)=Sof(H1a)=1-FVAR(1)
 Sof(Cl1)=Sof(Si1)=Sof(H1)=FVAR(1)
 Uiso(H1)=Uiso(H1a)=FVAR(2)
 Fixed Uiso: Cl1a(0.03)
;
_olex2_submission_special_instructions 'No special instructions were received'