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_7110401
_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            'C24 H34 Al3 Cl3 N2 O2'
_chemical_formula_weight         569.82
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.7057(15)
_cell_length_b                   9.7173(9)
_cell_length_c                   19.5089(15)
_cell_measurement_reflns_used    4023
_cell_measurement_temperature    230(2)
_cell_measurement_theta_max      23.00
_cell_measurement_theta_min      2.09
_cell_volume                     2977.4(5)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1994)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      230(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type
;
Siemens SMART 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  0.0477
_diffrn_reflns_av_sigmaI/netI    0.0977
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            5592
_diffrn_reflns_theta_full        23.00
_diffrn_reflns_theta_max         23.00
_diffrn_reflns_theta_min         2.09
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.419
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.338
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.10(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         3804
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.1187
_refine_ls_R_factor_gt           0.0735
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0827P)^2^+2.0618P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1607
_refine_ls_wR_factor_ref         0.1905
_reflns_number_gt                2555
_reflns_number_total             3804
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            808372jsup1.cif
_cod_data_source_block           tiets
_cod_original_sg_symbol_H-M      Pna2(1)
_cod_database_code               7110401