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_7711986
_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         'C32 H44 B P'
_chemical_formula_sum            'C32 H44 B P'
_chemical_formula_weight         470.45
_chemical_name_common            CH2PBMes(CH2)
_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             2022-11-01
_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                 102.935(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.230(2)
_cell_length_b                   19.008(4)
_cell_length_c                   14.985(4)
_cell_measurement_reflns_used    3917
_cell_measurement_temperature    193.15
_cell_measurement_theta_max      23.39
_cell_measurement_theta_min      2.31
_cell_volume                     2839.9(11)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      193.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22944
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.100
_diffrn_reflns_theta_min         1.758
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.114
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9068
_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    1.100
_exptl_crystal_description       block
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.213
_exptl_crystal_size_mid          0.196
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.385
_refine_diff_density_min         -0.240
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         5632
_refine_ls_number_restraints     151
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0486
_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^)+(0.0650P)^2^+0.6966P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1226
_refine_ls_wR_factor_ref         0.1405
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3991
_reflns_number_total             5632
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03807b3.cif
_cod_data_source_block           CH2PBMes-CH2
_cod_depositor_comments
'Adding full bibliography for 7711983--7711989.cif.'
_cod_original_cell_volume        2840.0(12)
_cod_database_code               7711986
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.976
_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
 C15-C16A \\sim C15-C16B \\sim C15-C20A \\sim C15-C20B
 with sigma of 0.01
 C16A-C17A \\sim C16B-C17B \\sim C20A-C19A \\sim C20B-C19B
 with sigma of 0.01
 C16A-C21A \\sim C16B-C21B \\sim C20A-C23A \\sim C20B-C23B
 with sigma of 0.01
 C17A-C18A \\sim C17B-C18B \\sim C18A-C19A \\sim C18B-C19B
 with sigma of 0.01
 C18A-C22A \\sim C18B-C22B
 with sigma of 0.01
3. Rigid body (RIGU) restrains
 C15, C16B, C17B, C18B, C19B, C20B, C21B, C22B, C23B, C16A, C17A, C18A, C19A,
 C20A, C21A, C22A, C23A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C16B)=Sof(C17B)=Sof(H17B)=Sof(C18B)=Sof(C19B)=Sof(H19B)=Sof(C20B)=
 Sof(C21B)=Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(C22B)=Sof(H22A)=Sof(H22B)=
 Sof(H22C)=Sof(C23B)=Sof(H23A)=Sof(H23B)=Sof(H23C)=1-FVAR(1)
 Sof(C16A)=Sof(C17A)=Sof(H17A)=Sof(C18A)=Sof(C19A)=Sof(H19A)=Sof(C20A)=
 Sof(C21A)=Sof(H1)=Sof(H2)=Sof(H3)=Sof(C22A)=Sof(H8)=Sof(H10)=Sof(H11)=
 Sof(C23A)=Sof(H13)=Sof(H14)=Sof(H15)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C9(H9), C12(H12)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C8(H8A,H8B)
5.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C17B(H17B), C19B(H19B), C26(H26), C28(H28),
 C17A(H17A), C19A(H19A)
5.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C21B(H21A,H21B,H21C), C22B(H22A,H22B,H22C), C23B(H23A,H23B,H23C),
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C21A(H1,H2,H3),
 C22A(H8,H10,H11), C23A(H13,H14,H15)
;
_shelx_res_checksum              35839
_shelx_hkl_checksum              88040
_olex2_submission_special_instructions 'No special instructions were received'