Frustrated Lewis pair-ligated tetrelenes.
Omaña, Alvaro A; Frenette, Brandon L.; Dornsiepen, Eike; Kobayashi, Ryo; Ferguson, Michael J.; Iwamoto, Takeaki; Rivard, Eric; Dalton transactions (Cambridge, England : 2003) 52 (2023) 774–786; doi:10.1039/d2dt03807b

data_7711983
_publ_section_title
;
 Frustrated Lewis pair-ligated tetrelenes.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              774
_journal_page_last               786
_journal_paper_doi               10.1039/d2dt03807b
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety         'C25 H42 B P'
_chemical_formula_sum            'C25 H42 B P'
_chemical_formula_weight         384.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-05-18
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-11-18 deposited with the CCDC.	2022-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.2950(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5854(3)
_cell_length_b                   9.8043(2)
_cell_length_c                   22.5734(5)
_cell_measurement_reflns_used    9942
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      73.493
_cell_measurement_theta_min      3.92
_cell_volume                     2342.12(10)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'Bruker APEX2'
_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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      173.05
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0637
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            88291
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         73.905
_diffrn_reflns_theta_min         3.917
_diffrn_source                   'Incoatec I\mS microfocus X-ray source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.058
_exptl_absorpt_correction_T_max  0.96752
_exptl_absorpt_correction_T_min  0.88950
_exptl_absorpt_correction_type   none
_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    1.090
_exptl_crystal_description       block
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.154
_exptl_crystal_size_mid          0.113
_exptl_crystal_size_min          0.045
_exptl_transmission_factor_max   0.96752
_exptl_transmission_factor_min   0.88950
_refine_diff_density_max         0.873
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         4607
_refine_ls_number_restraints     1529
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0479
_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^)+(0.0770P)^2^+0.9625P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1358
_refine_ls_wR_factor_ref         0.1408
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4070
_reflns_number_total             4607
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03807b3.cif
_cod_data_source_block           riv21c8m
_cod_depositor_comments
'Adding full bibliography for 7711983--7711989.cif.'
_cod_database_code               7711983
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.954
_shelx_estimated_absorpt_t_min   0.854
_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. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{P1A, B1A, C2A, C3A, C4A, C5A, C6A, C7A, C11A, C13A, C12A, C8A, C9A, C10A,
C14A, C15A, C16A, C17A, C18A, C19A, C20A, C21A, C22A, C23A, C24A, C25A, C1A}
sigma for 1-2: 0.02, 1-3: 0.04
as in
{P1B, B1B, C2B, C3B, C4B, C5B, C6B, C7B, C11B, C13B, C12B, C8B, C9B, C10B,
C14B, C15B, C16B, C17B, C18B, C19B, C20B, C21B, C22B, C23B, C24B, C25B, C1B}
6. Others
 Sof(P1B)=Sof(B1B)=Sof(C2B)=Sof(C3B)=Sof(H3B)=Sof(C4B)=Sof(H4B)=Sof(C5B)=
 Sof(H5B)=Sof(C6B)=Sof(H6B)=Sof(C7B)=Sof(C11B)=Sof(H11B)=Sof(C13B)=Sof(H13B)=
 Sof(H13C)=Sof(H13D)=Sof(C12B)=Sof(H12B)=Sof(H12C)=Sof(H12D)=Sof(C8B)=Sof(H8B)=
 Sof(C9B)=Sof(H9BA)=Sof(H9BB)=Sof(H9BC)=Sof(C10B)=Sof(H10B)=Sof(H10C)=Sof(H10D)=
 Sof(C14B)=Sof(H14B)=Sof(C15B)=Sof(H15B)=Sof(H15C)=Sof(C16B)=Sof(H16B)=
 Sof(H16C)=Sof(C17B)=Sof(H17B)=Sof(H17C)=Sof(C18B)=Sof(H18B)=Sof(H18C)=
 Sof(C19B)=Sof(H19B)=Sof(H19C)=Sof(C20B)=Sof(H20B)=Sof(C21B)=Sof(H21B)=
 Sof(H21C)=Sof(C22B)=Sof(H22B)=Sof(H22C)=Sof(C23B)=Sof(H23B)=Sof(H23C)=
 Sof(C24B)=Sof(H24B)=Sof(H24C)=Sof(C25B)=Sof(H25B)=Sof(H25C)=Sof(C1B)=Sof(H1BA)=
 Sof(H1BB)=1-FVAR(1)
 Sof(P1A)=Sof(B1A)=Sof(C2A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=
 Sof(H5A)=Sof(C6A)=Sof(H6A)=Sof(C7A)=Sof(C11A)=Sof(H11A)=Sof(C13A)=Sof(H13A)=
 Sof(H1)=Sof(H2)=Sof(C12A)=Sof(H12A)=Sof(H3)=Sof(H4)=Sof(C8A)=Sof(H8A)=Sof(C9A)=
 Sof(H9AB)=Sof(H9AC)=Sof(H9AA)=Sof(C10A)=Sof(H10A)=Sof(H5)=Sof(H6)=Sof(C14A)=
 Sof(H14A)=Sof(C15A)=Sof(H15A)=Sof(H7)=Sof(C16A)=Sof(H16A)=Sof(H8)=Sof(C17A)=
 Sof(H17A)=Sof(H9)=Sof(C18A)=Sof(H18A)=Sof(H10)=Sof(C19A)=Sof(H19A)=Sof(H11)=
 Sof(C20A)=Sof(H20A)=Sof(C21A)=Sof(H21A)=Sof(H12)=Sof(C22A)=Sof(H22A)=Sof(H13)=
 Sof(C23A)=Sof(H23A)=Sof(H14)=Sof(C24A)=Sof(H24A)=Sof(H15)=Sof(C25A)=Sof(H25A)=
 Sof(H16)=Sof(C1A)=Sof(H1A)=Sof(H2A)=FVAR(1)
7.a Ternary CH refined with riding coordinates:
 C11A(H11A), C8A(H8A), C14A(H14A), C20A(H20A), C11B(H11B), C8B(H8B),
 C14B(H14B), C20B(H20B)
7.b Secondary CH2 refined with riding coordinates:
 C15A(H15A,H7), C16A(H16A,H8), C17A(H17A,H9), C18A(H18A,H10), C19A(H19A,H11),
 C21A(H21A,H12), C22A(H22A,H13), C23A(H23A,H14), C24A(H24A,H15), C25A(H25A,H16),
  C1A(H1A,H2A), C15B(H15B,H15C), C16B(H16B,H16C), C17B(H17B,H17C), C18B(H18B,
 H18C), C19B(H19B,H19C), C21B(H21B,H21C), C22B(H22B,H22C), C23B(H23B,H23C),
 C24B(H24B,H24C), C25B(H25B,H25C), C1B(H1BA,H1BB)
7.c Aromatic/amide H refined with riding coordinates:
 C3A(H3A), C4A(H4A), C5A(H5A), C6A(H6A), C3B(H3B), C4B(H4B), C5B(H5B), C6B(H6B)
7.d Idealised Me refined as rotating group:
 C13A(H13A,H1,H2), C12A(H12A,H3,H4), C9A(H9AB,H9AC,H9AA), C10A(H10A,H5,H6),
 C13B(H13B,H13C,H13D), C12B(H12B,H12C,H12D), C9B(H9BA,H9BB,H9BC), C10B(H10B,
 H10C,H10D)
;
_shelx_res_checksum              1204
_shelx_hkl_checksum              87877
_olex2_submission_special_instructions 'No special instructions were received'