A donor-supported silavinylidene and silylium ylides: boroles as a flexible platform for versatile Si(ii) chemistry.
Sarcevic, Julijan; Heitkemper, Tobias; Ruth, Paul Niklas; Naß, Leonard; Kubis, Maximilian; Stalke, Dietmar; Sindlinger, Christian P.; Chemical science 14 (2023) 5148–5159; doi:10.1039/d3sc00808h

data_1568749
_publ_section_title
;
 A donor-supported silavinylidene and silylium ylides: boroles as a
 flexible platform for versatile Si(ii) chemistry.
;
_journal_issue                   19
_journal_name_full               'Chemical science'
_journal_page_first              5148
_journal_page_last               5159
_journal_paper_doi               10.1039/d3sc00808h
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         '4(C66 H99 B N2 Si3), (O C4 H10)'
_chemical_formula_sum            'C67 H101.5 B N2 O0.25 Si3'
_chemical_formula_weight         1034.08
_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 V113 by Daniel Kratzert, Freiburg 2023,
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2023-02-01 deposited with the CCDC.	2023-03-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.1790(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.8214(11)
_cell_length_b                   26.3082(18)
_cell_length_c                   17.7522(13)
_cell_measurement_reflns_used    6362
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.32
_cell_measurement_theta_min      2.21
_cell_volume                     6497.1(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ShelXle (H\"ubschle, 2011)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker APEX'
_diffrn_detector_type            CCD
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Apex CCD'
_diffrn_measurement_specimen_support 'glass fiber'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1290
_diffrn_reflns_av_unetI/netI     0.0537
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            157989
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         1.548
_exptl_absorpt_coefficient_mu    0.112
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6821
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction:
Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48
(2015) 3-10
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.057
_exptl_crystal_description       block
_exptl_crystal_F_000             2266
_exptl_crystal_recrystallization_method 'from ether solutions'
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.360
_refine_diff_density_min         -0.272
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     754
_refine_ls_number_reflns         13292
_refine_ls_number_restraints     216
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0821
_refine_ls_R_factor_gt           0.0503
_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^)+(0.0401P)^2^+4.7954P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1099
_refine_ls_wR_factor_ref         0.1269
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9488
_reflns_number_total             13292
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc00808h2.cif
_cod_data_source_block           sad_a_CCDC5
_cod_depositor_comments
'Adding full bibliography for 1568738--1568749.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C67 H101.50 B N2 O0.25 Si3'
_cod_database_code               1568749
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.967
_shelx_estimated_absorpt_t_max   0.967
_diffrn_measurement_ambient_temperature_device_make 'Oxford Cryostream'
_shelx_res_checksum              42297
_shelx_hkl_checksum              6273