Synthesis and structural characterization of titanium and zirconium complexes containing half-salen ligands as catalysts for polymerization reactions
Mandal, Mrinmay; Monkowius, Uwe; Chakraborty, Debashis; New J. Chem. 40 (2016) 9824–9839; doi:10.1039/C6NJ02148D

data_7055792
_publ_section_title
;
 Synthesis and structural characterization of titanium and zirconium
 complexes containing half-salen ligands as catalysts for polymerization
 reactions
;
_journal_issue                   11
_journal_name_full               'New J. Chem.'
_journal_page_first              9824
_journal_page_last               9839
_journal_paper_doi               10.1039/C6NJ02148D
_journal_volume                  40
_journal_year                    2016
_chemical_formula_moiety         'C26 H26 Cl4 N2 O4 Ti'
_chemical_formula_sum            'C26 H26 Cl4 N2 O4 Ti'
_chemical_formula_weight         620.19
_chemical_name_systematic        Ti2
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-04-24 deposited with the CCDC.
2016-09-30 downloaded from the CCDC.
;
_cell_angle_alpha                63.2283(19)
_cell_angle_beta                 68.1217(13)
_cell_angle_gamma                66.2981(14)
_cell_formula_units_Z            2
_cell_length_a                   10.3126(3)
_cell_length_b                   12.8248(5)
_cell_length_c                   12.9776(4)
_cell_measurement_reflns_used    7548
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.58
_cell_measurement_theta_min      2.22
_cell_volume                     1364.07(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0202
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18344
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.985
_diffrn_reflns_theta_min         1.854
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.741
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_description       Block
_exptl_crystal_F_000             636
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.416
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         4790
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0316P)^2^+0.9027P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0776
_refine_ls_wR_factor_ref         0.0831
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3986
_reflns_number_total             4790
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj02148d2.cif
_cod_data_source_block           Ti2
_cod_database_code               7055792
_shelx_estimated_absorpt_t_min   0.836
_shelx_estimated_absorpt_t_max   0.930
_shelxl_version_number           2013-4
_shelx_res_checksum              71150
_solvent_exptl_crystal_recrystallization_method Toluene