Investigations on Non-Classical Silylium Ions Leading to a Cyclobutenyl Cation
Martens, Arthur; Kreuzer, Marvin; Ripp, Alexander Johannes Christoph; Schneider, Marius; Himmel, Daniel; Scherer, Harald; Krossing, Ingo; Chemical Science  (2019) –; doi:10.1039/C8SC04591G

data_1550411
_publ_section_title
;
 Investigations on Non-Classical Silylium Ions Leading to a Cyclobutenyl
 Cation
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC04591G
_journal_year                    2019
_chemical_formula_moiety         'C12 Al F28 O3, C18 H31 N2 Si'
_chemical_formula_sum            'C30 H31 Al F28 N2 O3 Si'
_chemical_formula_weight         1054.64
_chemical_properties_physical    Air-sensitive,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'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-09-17 deposited with the CCDC.
2019-01-10 downloaded from the CCDC.
;
_cell_angle_alpha                78.2070(10)
_cell_angle_beta                 88.952(2)
_cell_angle_gamma                83.352(2)
_cell_formula_units_Z            2
_cell_length_a                   9.4236(2)
_cell_length_b                   10.9684(3)
_cell_length_c                   20.6676(5)
_cell_measurement_reflns_used    9843
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      59.670
_cell_measurement_theta_min      4.666
_cell_volume                     2077.06(9)
_computing_cell_refinement       'SAINT V8.37A'
_computing_data_collection       'APEX3 v2016.1-0'
_computing_data_reduction        'SAINT V8.37A'
_computing_publication_material  ShelXle-780
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'Bruker Smart Apex II Quazar'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            53293
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.547
_diffrn_reflns_theta_min         1.006
_diffrn_source                   'INCOATEC Mo Microsource'
_exptl_absorpt_coefficient_mu    0.239
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6945
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2014/5
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_description       block
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.495
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         12146
_refine_ls_number_restraints     372
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0475
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0728P)^2^+0.5290P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1241
_refine_ls_wR_factor_ref         0.1330
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9199
_reflns_number_total             12146
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc04591g2.cif
_cod_data_source_block           p-1_a
_cod_database_code               1550411
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              79009