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_1568748
_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_absolute_configuration ad
_chemical_formula_sum            'C61 H81 B Cl2 N2 Si3'
_chemical_formula_weight         1008.25
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method
;FinalCif V113 by Daniel Kratzert, Freiburg 2022,
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2023-01-01 deposited with the CCDC.	2023-03-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.9046(13)
_cell_length_b                   16.4022(14)
_cell_length_c                   23.053(2)
_cell_measurement_reflns_used    9800
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.008
_cell_measurement_theta_min      2.159
_cell_volume                     6013.8(9)
_computing_cell_refinement       'SAINT V8.40B'
_computing_data_collection       'Bruker APEX II'
_computing_data_reduction        'SAINT V8.40B'
_computing_molecular_graphics
'ORTEP (Farrugia, 2012), 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                 CCD
_diffrn_detector_type            'Bruker APEX II'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX2'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            85184
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.742
_diffrn_reflns_theta_min         1.524
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           0.97
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.205
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6922
_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    1.114
_exptl_crystal_description       block
_exptl_crystal_F_000             2168
_exptl_crystal_recrystallization_method
'Crystallized from conc. solutions in hexane at -30\%C'
_exptl_crystal_size_max          0.155
_exptl_crystal_size_mid          0.142
_exptl_crystal_size_min          0.127
_refine_diff_density_max         0.266
_refine_diff_density_min         -0.191
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details
;
 Flack x determined using 4835 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.013(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     642
_refine_ls_number_reflns         12770
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0346
_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^)+(0.0400P)^2^+1.4299P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0843
_reflns_Friedel_coverage         0.824
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                11518
_reflns_number_total             12770
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc00808h2.cif
_cod_data_source_block           p212121_a
_cod_depositor_comments
'Adding full bibliography for 1568738--1568749.cif.'
_cod_original_cell_volume        6013.9(9)
_cod_database_code               1568748
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.969
_shelx_estimated_absorpt_t_max   0.974
_diffrn_measurement_ambient_temperature_device_make 'Oxford Cryostream'
_shelx_res_checksum              21738
_shelx_hkl_checksum              18795