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_7715580
_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         'C33 H59 B Li O P Si'
_chemical_formula_sum            'C33 H59 B Li O P Si'
_chemical_formula_weight         548.61
_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             2024-03-04
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-03-05 deposited with the CCDC.	2024-04-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.843(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.528(2)
_cell_length_b                   20.445(5)
_cell_length_c                   17.796(5)
_cell_measurement_reflns_used    3522
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      18.965
_cell_measurement_theta_min      2.292
_cell_volume                     3425.5(15)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'Graphite flat monochromator (002)'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1474
_diffrn_reflns_av_unetI/netI     0.0762
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6303
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.401
_diffrn_reflns_theta_min         1.527
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.138
_exptl_absorpt_correction_T_max  0.861965
_exptl_absorpt_correction_T_min  0.683673
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS 2012/1: Bruker AXS Inc., Madison, Wisconsin, USA
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.064
_exptl_crystal_description       plate
_exptl_crystal_F_000             1208
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: pentane'
_exptl_crystal_size_max          0.258
_exptl_crystal_size_mid          0.198
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.676
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         6303
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.1458
_refine_ls_R_factor_gt           0.0875
_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^)+(0.1443P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2221
_refine_ls_wR_factor_ref         0.2581
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3670
_reflns_number_total             6303
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00795f3.cif
_cod_data_source_block           PB(LiCCSiMe3)
_cod_depositor_comments
'Adding full bibliography for 7715580--7715582.cif.'
_cod_original_cell_volume        3425.2(15)
_cod_database_code               7715580
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.965
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C32-C33 = C30-C31
 1.5 with sigma of 0.01
 C19-C24B \\sim C24B-C24A \\sim C19-C20
 with sigma of 0.02
 C20-C21B \\sim C21B-C21A \\sim C24B-C23B \\sim C24A-C23A
 with sigma of 0.02
 C23B-C22B \\sim C23A-C22A \\sim C21A-C22A \\sim C21B-C22B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C33) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C32)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C31) = Uanis(C33)
4. Rigid body (RIGU) restrains
 C31, C30, C32, C33
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H19A)=Sof(H20C)=Sof(H20D)=Sof(C24B)=Sof(H24C)=Sof(H24D)=Sof(C23B)=
 Sof(H23C)=Sof(H23D)=Sof(C22B)=Sof(H22C)=Sof(H22D)=Sof(C21B)=Sof(H21C)=
 Sof(H21D)=1-FVAR(1)
 Sof(H19)=Sof(C24A)=Sof(H24A)=Sof(H24B)=Sof(C23A)=Sof(H23A)=Sof(H23B)=
 Sof(C22A)=Sof(H22A)=Sof(H22B)=Sof(C21A)=Sof(H21A)=Sof(H21B)=Sof(H20A)=
 Sof(H20B)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C10(H10), C7(H7), C19(H19), C19(H19A), C13(H13)
6.b Secondary CH2 refined with riding coordinates:
 C24A(H24A,H24B), C23A(H23A,H23B), C22A(H22A,H22B), C21A(H21A,H21B), C20(H20A,
 H20B), C20(H20C,H20D), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B),
 C17(H17A,H17B), C18(H18A,H18B), C32(H32A,H32B), C30(H30A,H30B), C24B(H24C,
 H24D), C23B(H23C,H23D), C22B(H22C,H22D), C21B(H21C,H21D)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6)
6.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C11(H11A,H11B,H11C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C),
 C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C33(H33A,H33B,
 H33C), C31(H31A,H31B,H31C)
;
_shelx_res_checksum              599
_olex2_submission_special_instructions 'No special instructions were received'