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_1551460
_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         'C18 H15 Br8 O5 P Si, C H2 Cl2'
_chemical_formula_sum            'C19 H17 Br8 Cl2 O5 P Si'
_chemical_formula_weight         1094.56
_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
_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                86.42(3)
_cell_angle_beta                 79.44(3)
_cell_angle_gamma                67.26(3)
_cell_formula_units_Z            4
_cell_length_a                   11.061(2)
_cell_length_b                   12.978(3)
_cell_length_c                   22.591(5)
_cell_measurement_reflns_used    1643
_cell_measurement_temperature    120
_cell_measurement_theta_max      26
_cell_measurement_theta_min      1.0
_cell_volume                     2940.1(13)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0630
_diffrn_reflns_av_unetI/netI     0.1036
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            29044
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.999
_diffrn_reflns_theta_min         1.834
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    11.219
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.57484
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    2.473
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.927
_refine_diff_density_min         -1.099
_refine_diff_density_rms         0.205
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.957
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     655
_refine_ls_number_reflns         15631
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.957
_refine_ls_R_factor_all          0.1004
_refine_ls_R_factor_gt           0.0437
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0259P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0669
_refine_ls_wR_factor_ref         0.0780
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9732
_reflns_number_total             15631
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc02167a2.cif
_cod_data_source_block           ms19f
_cod_original_cell_volume        2940.2(12)
_cod_database_code               1551460
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.213
_shelx_estimated_absorpt_t_min   0.134
_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.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C15(H15A,H15B), C17(H17A,H17B), C13A(H13C,H13D), C15A(H15C,
 H15D), C17A(H17C,H17D), C1B(H1BA,H1BB), C2B(H2BA,H2BB)
2.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C14A(H14D,H14E,
 H14F), C16A(H16D,H16E,H16F), C18A(H18D,H18E,H18F)
;
_shelx_res_checksum              66084
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'