Stereochemical control of cis- and trans-TiCl2 groups in six-coordinate complexes [(L)TiCl2] (L2− = N2O2-donor Schiff base) and reactions with trimethylaluminium to form cationic aluminium species
Corden, Jonathan P.; Errington, William; Moore, Peter; Wallbridge, Malcolm G. H.; Chemical Communications  (1999) 323–; doi:10.1039/a808372j

data_7110400
_publ_section_title
;
 Stereochemical control of cis- and trans-TiCl2 groups in six-coordinate
 complexes [(L)TiCl2] (L2&#x2212; = N2O2-donor Schiff base) and reactions
 with trimethylaluminium to form cationic aluminium species
;
_journal_issue                   4
_journal_name_full               'Chemical Communications'
_journal_page_first              323
_journal_paper_doi               10.1039/a808372j
_journal_year                    1999
_chemical_formula_sum            'C25 H29 Cl5 N2 O2 Ti'
_chemical_formula_weight         614.65
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 111.32(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.446(3)
_cell_length_b                   9.796(2)
_cell_length_c                   18.160(4)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.12
_cell_measurement_theta_min      2.29
_cell_volume                     2725.4(11)
_computing_cell_refinement       'MADNES (Plugrath & Messerschmidt, 1992)'
_computing_data_collection       'MADNES (Plugrath & Messerschmidt, 1992)'
_computing_data_reduction        'SHELXTL-Plus (Sheldrick, 1990)'
_computing_molecular_graphics    'SHELXTL-Plus (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.881
_diffrn_measured_fraction_theta_max 0.881
_diffrn_measurement_device_type
;
Delft Instruments FAST TV area-detector diffractometer
;
_diffrn_measurement_method       '/w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1880
_diffrn_reflns_av_sigmaI/netI    0.4004
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12060
_diffrn_reflns_theta_full        25.12
_diffrn_reflns_theta_max         25.12
_diffrn_reflns_theta_min         2.29
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.831
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.481
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.597
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         4283
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      0.596
_refine_ls_R_factor_all          0.1820
_refine_ls_R_factor_gt           0.0539
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0998
_refine_ls_wR_factor_ref         0.1248
_reflns_number_gt                1206
_reflns_number_total             4283
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            808372jsup1.cif
_cod_data_source_block           tiet
_cod_original_cell_volume        2725.3(9)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7110400