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_7055793
_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         'C36 H50 N2 O4 Ti'
_chemical_formula_sum            'C36 H50 N2 O4 Ti'
_chemical_formula_weight         622.68
_chemical_name_systematic        Ti1
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'APEX2 v2010.1-2'
_audit_update_record
;
2016-04-24 deposited with the CCDC.
2016-09-30 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 104.720(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.4864(9)
_cell_length_b                   17.4311(13)
_cell_length_c                   16.5711(16)
_cell_measurement_reflns_used    7841
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.80
_cell_measurement_theta_min      2.34
_cell_volume                     4047.1(6)
_computing_cell_refinement       'APEXII/SAINT (Bruker, 2004)'
_computing_data_collection       'APEXII (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004)'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0210
_diffrn_reflns_av_sigmaI/netI    0.0243
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19126
_diffrn_reflns_theta_full        28.34
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    0.245
_exptl_absorpt_correction_T_max  0.9642
_exptl_absorpt_correction_T_min  0.9193
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker,2004)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.022
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.265
_refine_diff_density_min         -0.164
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         5037
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0626
_refine_ls_R_factor_gt           0.0451
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0754P)^2^+0.6354P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1357
_refine_ls_wR_factor_ref         0.1426
_reflns_number_gt                3664
_reflns_number_total             5037
_reflns_threshold_expression     >2sigma(I)
_publcif_datablock.id            {1ca9f957-dee2-423c-8aa0-77e1010ccb34}
_cod_data_source_file            c6nj02148d2.cif
_cod_data_source_block           Ti1
_cod_original_sg_symbol_H-M      I2/a
_cod_database_code               7055793