Ga±catalyzed hydrosilylation? About the surprising system Ga+/HSiR3/olefin, proof of oxidation with subvalent Ga+ and silylium catalysis with perfluoroalkoxyaluminate anions
Barthélemy, Antoine; Glootz, Kim; Scherer, Harald; Hanske, Annaleah; Krossing, Ingo; Chemical Science 13 (2022) 439–453; doi:10.1039/D1SC05331K

data_1565762
_publ_section_title
;
 Ga+-catalyzed hydrosilylation? About the surprising system
 Ga+/HSiR3/olefin, proof of oxidation with subvalent Ga+ and silylium
 catalysis with perfluoroalkoxyaluminate anions
;
_journal_issue                   2
_journal_name_full               'Chemical Science'
_journal_page_first              439
_journal_page_last               453
_journal_paper_doi               10.1039/D1SC05331K
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety         'C18 H15 Al F28 O3 Si'
_chemical_formula_sum            'C18 H15 Al F28 O3 Si'
_chemical_formula_weight         866.37
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method
;
FinalCif V86 by Daniel Kratzert, Freiburg 2021,
https://github.com/dkratzert/FinalCif
;
_audit_update_record
;
2021-08-10 deposited with the CCDC.	2021-11-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.187(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.757(5)
_cell_length_b                   17.585(10)
_cell_length_c                   17.518(9)
_cell_measurement_reflns_used    7196
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.632
_cell_measurement_theta_min      2.3115
_cell_volume                     3006(3)
_computing_cell_refinement       'SAINT V8.40A'
_computing_data_collection
'Bruker BIS 2018.9.0.3/05-Dec-2018 && APEX3_2019.1-0'
_computing_data_reduction        'SAINT V8.40A'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 8.3
_diffrn_detector_type            'Bruker APEXII'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX2 QUAZAR'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_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  0.1070
_diffrn_reflns_av_unetI/netI     0.0420
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            67382
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.800
_diffrn_reflns_theta_max         24.800
_diffrn_reflns_theta_min         1.641
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           0.6
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.305
_exptl_absorpt_correction_T_max  0.8619
_exptl_absorpt_correction_T_min  0.7606
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.914
_exptl_crystal_description       block
_exptl_crystal_F_000             1704
_exptl_crystal_recrystallization_method
'Crystals were obtained from ortho-difluorobenzene at -25 \%C.'
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.636
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     590
_refine_ls_number_reflns         5180
_refine_ls_number_restraints     3138
_refine_ls_restrained_S_all      0.846
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0366
_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^)+(0.0466P)^2^+2.1987P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0919
_refine_ls_wR_factor_ref         0.1017
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4079
_reflns_number_total             5180
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc05331k2.cif
_cod_data_source_block           IK_KG_AB_23_0m
_cod_depositor_comments          'Adding full bibliography for 1565762.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1565762
_shelx_shelxl_version_number     2018/3
_olex2_diffrn_ambient_temperature_device 'Oxford Cryostream 800'
_shelx_res_checksum              3014
_shelx_hkl_checksum              23728