In Situ Formation of Heterobimetallic Salen Complexes Containing Titanium and/or Vanadium Ions
Yuri N. Belokon'; William Clegg; Ross W. Harrington; Michael North; Carl Young; Inorganic Chemistry 47 (2008) 3801–3814; doi:10.1021/ic702451a

data_4304862
_publ_section_title
;
In Situ Formation of Heterobimetallic Salen Complexes Containing Titanium
and/or Vanadium Ions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3801
_journal_page_last               3814
_journal_paper_doi               10.1021/ic702451a
_journal_volume                  47
_journal_year                    2008
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C111 H163 N6 O13 S Ti3 +,C2 H5 O4 S -,C14 H22 O2'
_chemical_formula_sum            'C127 H190 N6 O19 S2 Ti3'
_chemical_formula_weight         2312.67
_space_group_IT_number           170
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 65'
_symmetry_space_group_name_H-M   'P 65'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   27.380(2)
_cell_length_b                   27.380(2)
_cell_length_c                   38.033(3)
_cell_measurement_reflns_used    9567
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      33.14
_cell_measurement_theta_min      3.09
_cell_volume                     24692(3)
_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 and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX2 CCD diffractometer'
_diffrn_measurement_method       'thin-slice \w scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6709
_diffrn_reflns_av_R_equivalents  0.0753
_diffrn_reflns_av_sigmaI/netI    0.0740
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            59945
_diffrn_reflns_theta_full        19.60
_diffrn_reflns_theta_max         19.60
_diffrn_reflns_theta_min         3.32
_diffrn_standards_decay_%        5
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.192
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.965
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    0.933
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7464
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.536
_refine_diff_density_min         -0.187
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_coef       0.0036(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1452
_refine_ls_number_reflns         17038
_refine_ls_number_restraints     868
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0549
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0868P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1300
_refine_ls_wR_factor_ref         0.1379
_reflns_number_gt                13456
_reflns_number_total             17038
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic702451a-file002.cif
_cod_data_source_block           mn8sq
_cod_database_code               4304862