Crystal structures of the Lewis acid–base adducts {[(C~6~H~11~)~2~N]~3~Ti–<i>LB</i>}^+^[MeB(C~6~F~5~)~3~]^{-^}·1.5C~7~H~8~; LB = (C~6~H~5~)~3~PO (1), <i>p</i>-F—C~6~H~4~CN (2)
Fitschen, Kerstin; Frerichs, Nils; Yusufzadeh, Zainab; Schmidtmann, Marc; Beckhaus, Rüdiger; Acta Crystallographica Section E 78 (2022) –; doi:10.1107/S2056989022007952

data_2244146
_publ_section_title
;
 Crystal structures of the Lewis acid--base adducts
 {[(C~6~H~11~)~2~N]~3~Ti--<i>LB</i>}^+^[MeB(C~6~F~5~)~3~]^{-^}&#x00B7;1.5C~7~H~8~;
 LB = (C~6~H~5~)~3~PO (1), <i>p</i>-F---C~6~H~4~CN (2)
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2056989022007952
_journal_volume                  78
_journal_year                    2022
_chemical_formula_iupac
'[Ti (C12 H22 N)3 (C7 H4 F N)] (C19 H3 F15 B), 1.5C7 H8'
_chemical_formula_moiety         'C43 H70 F N4 Ti +, C19 H3 F15 B -, 1.5C7 H8'
_chemical_formula_structural
'[Ti(N(C6H11)2)3(C6H4FCN)] [B(CH3)(C6F5)3] *1.5C7H8'
_chemical_formula_sum            'C72.5 H85 B F16 N4 Ti'
_chemical_formula_weight         1375.15
_chemical_name_systematic
;
Tris(dicyclohexylamido)(4-fluorobenzonitrile)titanium
methyltris(pentafluorophenyl)borate toluene sesquisolvate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                77.9160(19)
_cell_angle_beta                 88.8857(18)
_cell_angle_gamma                87.9827(18)
_cell_formula_units_Z            2
_cell_length_a                   12.1151(5)
_cell_length_b                   13.2796(6)
_cell_length_c                   21.1662(10)
_cell_measurement_reflns_used    9902
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.35
_cell_measurement_theta_min      2.25
_cell_volume                     3327.5(3)
_computing_cell_refinement
;
SAINT (Bruker, 2018)
;
_computing_data_collection
;
APEX3 (Bruker, 2018)
;
_computing_data_reduction
;
SAINT (Bruker, 2018)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXS (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            146764
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.726
_diffrn_reflns_theta_min         1.569
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.220
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9628
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Krause <i>et al.</i>, 2015)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_description       plate
_exptl_crystal_F_000             1438
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.740
_refine_diff_density_min         -0.956
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     979
_refine_ls_number_reflns         26559
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0658
_refine_ls_R_factor_gt           0.0442
_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^)+(0.0500P)^2^+1.3000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1053
_refine_ls_wR_factor_ref         0.1177
_reflns_number_gt                20132
_reflns_number_total             26559
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5649sup1.cif
_cod_data_source_block           2
_cod_original_formula_sum        'C72.50 H85 B F16 N4 Ti'
_cod_database_code               2244146
_shelx_estimated_absorpt_t_min   0.933
_shelx_estimated_absorpt_t_max   0.983
_shelx_hkl_checksum              69871
_shelx_res_checksum              36626
_cod_database_fobs_code 2244146