Macrocycle-Supported Titanium Complexes with Chelating Imido Ligands: Analogues of ansa-Metallocenes
Nigel A. H. Male; Michael E. G. Skinner; Sergei Y. Bylikin; Paul J. Wilson; Philip Mountford; Martin Schröder; Inorganic Chemistry 39 (2000) 5483–5491; doi:10.1021/ic9910357

data_4321617
_publ_contact_author
;
 Dr P Mountford
 Inorganic Chemistry Laboratory
 South Parks Road
 Oxford
 OX1 3QR        
;
_publ_contact_author_email       Philip.Mountford@chem.ox.ac.uk
_publ_contact_author_fax         '+44 1865 272690'
_publ_contact_author_phone       '+44 1865 272679'
_publ_section_title
;
 Macrocycle-Supported Titanium Complexes with Chelating Imido Ligands:
 Analogues of ansa-Metallocenes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5483
_journal_page_last               5491
_journal_paper_doi               10.1021/ic9910357
_journal_volume                  39
_journal_year                    2000
_chemical_compound_source
;
 H2L-1 + [Ti(NBu-t)Cl2(py(3] in benzene
;
_chemical_formula_moiety         ' C16 H32 Cl1 F3 N4 O3 S1 Ti1 '
_chemical_formula_sum            'C16 H32 Cl F3 N4 O3 S Ti'
_chemical_formula_weight         500.86
_chemical_name_systematic
;
 [Ti{i-Pr2(CH2CH2CH2N)[9]aneN3}Cl(OTf)]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             99-08-4
_audit_creation_method           CRYSTALS
_cell_angle_alpha                90
_cell_angle_beta                 99.091(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4.00
_cell_length_a                   9.2840(6)
_cell_length_b                   19.097(2)
_cell_length_c                   12.7810(7)
_cell_measurement_reflns_used    16824
_cell_measurement_temperature    170
_cell_measurement_theta_max      27
_cell_measurement_theta_min      0
_cell_volume                     2237.6(3)
_computing_cell_refinement
;
DIP2000 software 'DENZO' (Otwinowski & Minor, 1996)
;
_computing_data_collection       'DIP2000 software Xpress (MAC Science, 1989)'
_computing_data_reduction
;
DIP2000 software 'DENZO' (Otwinowski & Minor, 1996)
;
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1994)'
_computing_publication_material
;
CRYSTALS Issue 10 (Watkin et al, 1996)
;
_computing_structure_refinement
;
CRYSTALS Issue 10 (Watkin et al, 1996)
;
_computing_structure_solution    'SIR92 (Altomare, et al, 1994)'
_diffrn_ambient_temperature      170
_diffrn_measurement_device_type  'Enraf-nonius DIP2000 '
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.06
_diffrn_reflns_av_sigmaI/netI    0.0617
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16824
_diffrn_reflns_theta_max         26.43
_diffrn_reflns_theta_min         1.07
_diffrn_standards_decay_%        0.00
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.64
_exptl_absorpt_correction_T_max  0.852
_exptl_absorpt_correction_T_min  0.726
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.49
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.43
_refine_diff_density_min         -0.48
_refine_ls_abs_structure_Flack   none
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.17
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         2780
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0526
_refine_ls_shift/esd_max         0.0003
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      'Chebychev polynomial'
_refine_ls_wR_factor_obs         0.0359
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              23
_reflns_limit_k_min              0
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_observed          2780
_reflns_number_total             4207
_reflns_observed_criterion       >3\s(I)
_cod_data_source_file            ic9910357.cif
_cod_data_source_block           Compound_8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'direct methods' was changed to
'direct'.

'_atom_sites_solution_hydrogens' value 'geometric' was changed to
'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        2237.6
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        ' C16 H32 Cl1 F3 N4 O3 S1 Ti1 '
_cod_database_code               4321617