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_2242000
_publ_section_title
;
 Crystal structures of a novel NNN pincer ligand and its dinuclear
 titanium(IV) alkoxide pincer complex
;
_journal_coeditor_code           LH5823
_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 Br2 (C24 H33 N3) (C4 H10 O1)2]'
_chemical_formula_moiety         'C32 H53 Br2 Li2 N3 O2'
_chemical_formula_sum            'C32 H53 Br2 Li2 N3 O2'
_chemical_formula_weight         685.47
_chemical_name_systematic
;Di-\m-bromido-\m-{2-(2,2-dimethylpropanimidoyl)-<i>N</i>-[2-(2,2-dimethylpropanimidoyl)-4-methylphenyl]-4-methylaniline}-bis[(diethyl
ether)lithium]
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8301(7)
_cell_length_b                   22.3946(13)
_cell_length_c                   13.4254(8)
_cell_measurement_reflns_used    9991
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.0
_cell_volume                     3556.8(4)
_computing_cell_refinement
;
APEX2 (Bruker, 2008)
;
_computing_data_collection
;
APEX2 (Bruker, 2008)
;
_computing_data_reduction
;
SAINT (Bruker, 2008)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2014)
;
_computing_publication_material
;
SHELXL2013 (Sheldrick, 2015b)
;
_computing_structure_refinement
;
SHELXL2013 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2013 (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 DUO'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            45357
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.494
_diffrn_reflns_theta_min         1.819
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.309
_exptl_absorpt_correction_T_max  0.8913
_exptl_absorpt_correction_T_min  0.7580
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
[based on measured indexed crystal faces (SHELXTL; Sheldrick, 2008)]
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_description       platelets
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.057
_refine_diff_density_max         1.011
_refine_diff_density_min         -0.785
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     189
_refine_ls_number_reflns         4096
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0521
_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^+7.3069P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1329
_refine_ls_wR_factor_ref         0.1399
_reflns_number_gt                3116
_reflns_number_total             4096
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lh5823sup1.cif
_cod_data_source_block           1
_cod_database_code               2242000
_cod_database_fobs_code          2242000
_shelx_estimated_absorpt_t_min   0.723
_shelx_estimated_absorpt_t_max   0.880
_shelx_hkl_checksum              39059
_shelx_res_checksum              43519
_shelxl_version_number           2.013