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_7711989
_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_absolute_configuration unk
_chemical_formula_moiety         'C34 H58 B Li O3 P'
_chemical_formula_sum            'C34 H58 B Li O3 P'
_chemical_formula_weight         563.52
_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     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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9428(10)
_cell_length_b                   16.8849(17)
_cell_length_c                   20.512(2)
_cell_measurement_reflns_used    3553
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      20.25
_cell_measurement_theta_min      2.28
_cell_volume                     3443.6(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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      193.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.0730
_diffrn_reflns_av_unetI/netI     0.0693
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            28282
_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         25.691
_diffrn_reflns_theta_min         1.562
_diffrn_source                   'Short anode X-ray tube fine focus 2kW'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.110
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8910
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.087
_exptl_crystal_description       block
_exptl_crystal_F_000             1236
_exptl_crystal_size_max          0.235
_exptl_crystal_size_mid          0.173
_exptl_crystal_size_min          0.132
_exptl_transmission_factor_max   0.98716
_exptl_transmission_factor_min   0.97985
_refine_diff_density_max         0.419
_refine_diff_density_min         -0.255
_refine_diff_density_rms         0.042
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.29(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         6531
_refine_ls_number_restraints     216
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0936
_refine_ls_R_factor_gt           0.0579
_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^)+(0.0768P)^2^+0.3556P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1361
_refine_ls_wR_factor_ref         0.1595
_reflns_Friedel_coverage         0.779
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                4451
_reflns_number_total             6531
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03807b3.cif
_cod_data_source_block           riv2226
_cod_depositor_comments
'Adding full bibliography for 7711983--7711989.cif.'
_cod_database_code               7711989
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.975
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.71(19)
 0.29(19)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
O2 \\sim O2A \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C45A \\sim C46A
\\sim C47A \\sim C48A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 O2, O2A, C45, C46, C47, C48, C45A, C46A, C47A, C48A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Sof(O2A)=Sof(C45A)=Sof(H45C)=Sof(H45D)=Sof(C46A)=Sof(H46C)=Sof(H46D)=
 Sof(C47A)=Sof(H47C)=Sof(H47D)=Sof(C48A)=Sof(H48A)=1-FVAR(1)
 Sof(O2)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(C47)=
 Sof(H47A)=Sof(H47B)=Sof(C48)=Sof(H48)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C11(H11), C21(H21), C31(H31)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B),
 C26(H26A,H26B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B),
  C36(H36A,H36B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,
 H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B), C45A(H45C,H45D),
 C46A(H46C,H46D), C47A(H47C,H47D), C49(H49A,H49B), C50(H50A,H50B), C51(H51A,
 H51B), C52(H52A,H52B)
6.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C48(H48), C48A(H48A)
6.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              43195
_shelx_hkl_checksum              72751
_olex2_submission_special_instructions 'No special instructions were received'