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_7711988
_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         'C34 H56.34 Li2 O2 P2'
_chemical_formula_sum            'C34 H56.34 Li2 O2 P2'
_chemical_formula_weight         572.95
_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     iterative
_audit_creation_date             2022-05-10
_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                 95.4640(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7778(6)
_cell_length_b                   18.1916(8)
_cell_length_c                   15.8870(7)
_cell_measurement_reflns_used    5258
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      2.24
_cell_measurement_theta_min      22.50
_cell_volume                     3676.1(3)
_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      173.15
_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_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0715
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            56424
_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         25.747
_diffrn_reflns_theta_min         1.706
_exptl_absorpt_coefficient_mu    0.143
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9270
_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_density_diffrn    1.035
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1249
_exptl_crystal_size_max          0.174
_exptl_crystal_size_mid          0.147
_exptl_crystal_size_min          0.061
_refine_diff_density_max         0.741
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.050
_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     393
_refine_ls_number_reflns         7023
_refine_ls_number_restraints     74
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0963
_refine_ls_R_factor_gt           0.0607
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0736P)^2^+3.0731P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1528
_refine_ls_wR_factor_ref         0.1769
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4690
_reflns_number_total             7023
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03807b3.cif
_cod_data_source_block           riv2213m3
_cod_depositor_comments
'Adding full bibliography for 7711983--7711989.cif.'
_cod_database_code               7711988
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.991
_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. Rigid bond restraints
 C4, C1, C012, C2, C00V, C3, C00X, C013, C00W, C00Z
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C4 \\sim C1 \\sim C012 \\sim C2 \\sim C00V \\sim C3 \\sim C00X \\sim C013 \\sim
C00W \\sim C00Z: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
4. Rigid body (RIGU) restrains
 C4, C1, C012, C2, C00V, C3, C00X, C013, C00W, C00Z
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C2)=Sof(H2A)=Sof(H2B)=1-FVAR(1)
 Sof(C012)=Sof(H012)=FVAR(1)
 Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=1-FVAR(2)
 Sof(C00V)=Sof(H3)=Sof(HJ)=Sof(HK)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C009(H009), C00B(H00C), C00D(H00F), C00E(H00G)
6.b Secondary CH2 refined with riding coordinates:
 C008(H00A,H00B), C00C(H00D,H00E), C013(H01A,H01B), C2(H2A,H2B)
6.c Aromatic/amide H refined with riding coordinates:
 C00F(H00H), C00G(H00I), C00H(H00J), C00I(H00K), C00J(H00L), C00K(H00M),
 C00L(H00N), C00M(H00O), C00W(H4), C012(H012), C1(H1A)
6.d X=CH2 refined with riding coordinates:
 C4(H4A,H4B)
6.e Idealised Me refined as rotating group:
 C00N(H00P,H00Q,H00R), C00O(H00S,H00T,H00U), C00P(H00V,H00W,H00X), C00Q(H00Y,H,
 HA), C00R(H00Z,HB,HC), C00S(H00,HD,HE), C00T(H1,HF,HG), C00U(H2,HH,HI),
 C00V(H3,HJ,HK), C00X(H5,HL,HM), C00Z(H6,HN,HO), C3(H3A,H3B,H3C)
;
_shelx_res_checksum              58541
_shelx_hkl_checksum              35613
_olex2_submission_special_instructions 'No special instructions were received'