Pendulum-like hemilability in a Ti-based frustrated Lewis Trio.
Kounalis, Errikos; van Tongeren, Dylan; Melnikov, Stanislav; Lutz, Martin; Broere, Daniël L J; Chemical science 15 (2024) 5555–5563; doi:10.1039/d3sc06789k

data_1571206
_publ_section_title
;
 Pendulum-like hemilability in a Ti-based frustrated Lewis Trio.
;
_journal_issue                   15
_journal_name_full               'Chemical science'
_journal_page_first              5555
_journal_page_last               5563
_journal_paper_doi               10.1039/d3sc06789k
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C26 H44 Cl4 N2 P2 Ti, 0.5(C6 H6), C5 H12'
_chemical_formula_sum            'C34 H59 Cl4 N2 P2 Ti'
_chemical_formula_weight         747.47
_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     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-10-26 deposited with the CCDC.	2024-03-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.688(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.8812(14)
_cell_length_b                   16.6100(11)
_cell_length_c                   15.6315(9)
_cell_measurement_reflns_used    19886
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.56
_cell_measurement_theta_min      1.32
_cell_volume                     4072.7(5)
_computing_cell_refinement       Peakref
_computing_data_collection       Apex3
_computing_data_reduction        'Eval15, Sadabs'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    SHELXT
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Kappa ApexII'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1485
_diffrn_reflns_av_unetI/netI     0.1132
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            56073
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.506
_diffrn_reflns_theta_min         1.298
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.575
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6934
_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            orange
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_description       needle
_exptl_crystal_F_000             1588
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.886
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         7587
_refine_ls_number_restraints     416
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1489
_refine_ls_R_factor_gt           0.0715
_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^)+(0.0691P)^2^+14.6931P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1625
_refine_ls_wR_factor_ref         0.1987
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4198
_reflns_number_total             7587
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc06789k2.cif
_cod_data_source_block           l1211a
_cod_depositor_comments
'Adding full bibliography for 1571205--1571209.cif.'
_cod_original_cell_volume        4072.8(5)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1571206
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              10468