Frustrated Lewis pair adducts of alkynyl-capped tetrelenes.
Muralidharan, Abhishek V.; Frenette, Brandon L.; Wicke, Julius; Omaña, Alvaro A; Ferguson, Michael J.; Rivard, Eric; Dalton transactions (Cambridge, England : 2003) 53 (2024) 7206–7212; doi:10.1039/d4dt00795f

data_7715582
_publ_section_title
;
 Frustrated Lewis pair adducts of alkynyl-capped tetrelenes.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7206
_journal_page_last               7212
_journal_paper_doi               10.1039/d4dt00795f
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C34 H58 B P Si3'
_chemical_formula_sum            'C34 H58 B P Si3'
_chemical_formula_weight         592.85
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_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     dual
_audit_creation_date             2023-01-20
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-03-05 deposited with the CCDC.	2024-04-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.0956(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7526(12)
_cell_length_b                   19.307(2)
_cell_length_c                   16.8909(17)
_cell_measurement_reflns_used    9173
_cell_measurement_temperature    193.15
_cell_measurement_theta_max      26.80
_cell_measurement_theta_min      2.17
_cell_volume                     3700.4(7)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      193.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            86565
_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         28.329
_diffrn_reflns_theta_min         1.635
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.192
_exptl_absorpt_correction_T_max  0.9953
_exptl_absorpt_correction_T_min  0.9352
_exptl_absorpt_correction_type   numerical
_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_colour_primary    colourless
_exptl_crystal_density_diffrn    1.064
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1296
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: diethylether/pentane'
_exptl_crystal_size_max          0.469
_exptl_crystal_size_mid          0.372
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.326
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         9233
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0433
_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^)+(0.0649P)^2^+1.3022P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1149
_refine_ls_wR_factor_ref         0.1260
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7489
_reflns_number_total             9233
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00795f3.cif
_cod_data_source_block           PB(SiCCSiMe3_2)
_cod_depositor_comments
'Adding full bibliography for 7715580--7715582.cif.'
_cod_original_cell_volume        3700.5(7)
_cod_database_code               7715582
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.974
_shelx_estimated_absorpt_t_min   0.915
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Si2-C29B \\sim Si2-C27B \\sim Si2-C28B
 with sigma of 0.01
3. Others
 Sof(C29B)=Sof(H29D)=Sof(H29E)=Sof(H29F)=Sof(C27B)=Sof(H27D)=Sof(H27E)=
 Sof(H27F)=Sof(C28B)=Sof(H28D)=Sof(H28E)=Sof(H28F)=1-FVAR(1)
 Sof(C28A)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C29A)=Sof(H29A)=Sof(H29B)=
 Sof(H29C)=Sof(C27A)=Sof(H27A)=Sof(H27B)=Sof(H27C)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C10(H10), C7(H7), C19(H19), C13(H13)
4.b Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,
 H24B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B),
 C18(H18A,H18B)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6)
4.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C),
 C28A(H28A,H28B,H28C), C29A(H29A,H29B,H29C), C27A(H27A,H27B,H27C), C32(H32A,
 H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C29B(H29D,H29E,H29F),
 C27B(H27D,H27E,H27F), C28B(H28D,H28E,H28F)
;
_shelx_res_checksum              38929
_olex2_submission_special_instructions 'No special instructions were received'