Crystal structures of a novel NNN pincer ligand and its dinuclear titanium(IV) alkoxide pincer complex
Pedziwiatr, Jakub; Ghiviriga, Ion; Abboud, Khalil A.; Veige, Adam S.; Acta Crystallographica Section E 73 (2017) 122–126; doi:10.1107/S2056989016019964

data_2242001
_publ_section_title
;
 Crystal structures of a novel NNN pincer ligand and its dinuclear
 titanium(IV) alkoxide pincer complex
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              122
_journal_page_last               126
_journal_paper_doi               10.1107/S2056989016019964
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac
'[Li2 Ti2 Br2 (C24 H32 N3)2 (C3 H7 O1)6] , 1.5C7 H8'
_chemical_formula_moiety         'C87 H128 Br2 Li2 N6 O6 Ti2 , 1.5(C7 H8)'
_chemical_formula_sum            'C97.5 H140 Br2 Li2 N6 O6 Ti2'
_chemical_formula_weight         1761.7051
_chemical_name_systematic
Di-\m-bromido-2:3\k^4^<i>Br</i>:<i>Br</i>-bis{2-(2,2-dimethylpropanimidoyl)-<i>N</i>-[2-(2,2-dimethylpropanimidoyl)-4-methylphenyl]-4-methylaniline}-1\k^3^<i>N</i>,<i>N</i>',<i>N</i>'';4\k^3^<i>N</i>,<i>N</i>',<i>N</i>''-tetra-\m-isopropanolato-1:2\k^4^<i>O</i>:<i>O</i>;3:4\k^4^<i>O</i>:<i>O</i>-diisopropanolato-1\k<i>O</i>,4\k<i>O</i>-2,3-dilithium-1,4-dititanium
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                75.8613(15)
_cell_angle_beta                 68.0449(15)
_cell_angle_gamma                83.2200(17)
_cell_formula_units_Z            1
_cell_length_a                   12.2546(3)
_cell_length_b                   12.7240(3)
_cell_length_c                   15.9477(5)
_cell_measurement_reflns_used    16469
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.0
_cell_volume                     2235.49(11)
_computing_cell_refinement
;
APEX2 (Bruker, 2008)
;
_computing_data_collection
;
APEX2 (Bruker, 2008)
;
_computing_data_reduction
;
SAINT (Bruker, 2008)
;
_computing_molecular_graphics
;
SHELXTL2014 (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL2014 (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXTL2014 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXTL2014 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Bruker APEXII DUO'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0831
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            30419
_diffrn_reflns_theta_full        66.498
_diffrn_reflns_theta_max         66.498
_diffrn_reflns_theta_min         3.061
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.003
_exptl_absorpt_correction_T_max  0.8901
_exptl_absorpt_correction_T_min  0.6672
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
[based on measured indexed crystal faces (SHELXTL2014; Sheldrick, 2008)]
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_description       plates
_exptl_crystal_F_000             860
_exptl_crystal_size_max          0.253
_exptl_crystal_size_mid          0.198
_exptl_crystal_size_min          0.042
_refine_diff_density_max         0.718
_refine_diff_density_min         -0.430
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         7594
_refine_ls_number_restraints     324
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0579
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1092P)^2^+0.3301P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1635
_refine_ls_wR_factor_ref         0.1723
_reflns_number_gt                6139
_reflns_number_total             7594
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lh5823sup1.cif
_cod_data_source_block           2
_cod_database_code               2242001
_shelx_estimated_absorpt_t_min   0.521
_shelx_estimated_absorpt_t_max   0.886
_shelx_hkl_checksum              40907
_shelx_res_checksum              30067
_cod_database_fobs_code 2242001