Reactions of titanium imido complexes with α-diimines: complexation versus TiN/CN bond metathesis
McInnes, Jacqueline M.; Blake, Alexander J.; Mountford, Philip; Journal of the Chemical Society, Dalton Transactions  (1998) 3623–; doi:10.1039/a806393a

data_7027054
_publ_contact_author
;

 Dr P Mountford

 Department of Chemistry

 University of Nottingham

 Nottingham

 NG7 2RD

;
_publ_section_title
;
 Reactions of titanium imido complexes with \a-diimines: complexation
 versus Ti&#xE006;N/C&#xE006;N bond metathesis
;
_journal_issue                   21
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3623
_journal_paper_doi               10.1039/a806393a
_journal_year                    1998
_chemical_compound_source
;

 [Ti(N-2,6-C6H3Pri2)Cl2(py)3] + 1,2-N2(Ph)2C2Me2

;
_chemical_formula_moiety         ' C34 H40 Cl4 N4 Ti1'
_chemical_formula_sum            'C34 H40 Cl4 N4 Ti'
_chemical_formula_weight         694.43
_chemical_name_systematic
;

 [Ti(N-2,6-C6H3Pri2)Cl2(py){1,2-N2(Ph)2C2Me2}]

;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'direct methods: SIR92'
_audit_creation_date             98-08-08
_audit_creation_method           CRYSTALS
_cell_angle_alpha                82.49(3)
_cell_angle_beta                 85.22(3)
_cell_angle_gamma                85.28(3)
_cell_formula_units_Z            2
_cell_length_a                   11.093(3)
_cell_length_b                   12.533(5)
_cell_length_c                   12.687(5)
_cell_measurement_reflns_used    34
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      17.6
_cell_measurement_theta_min      12.5
_cell_volume                     1738.1(11)
_computing_cell_refinement       'STADI4 (Stoe & Cie 1995a)'
_computing_data_collection       'STADI4 (Stoe & Cie 1995a)'
_computing_data_reduction
;

X-RED (Stoe & Cie, 1995b)

CRYSTALS (Watkin et al, 1996)

;
_computing_molecular_graphics    'CAMERON (Watkin, Prout and Pearce, 1996)'
_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      150.0(2)
_diffrn_measurement_device       'STOE STADI4 4-circle-diffractometer'
_diffrn_measurement_method
; Scan width (omega) = 0.92 - 1.69, scan ratio 2theta:omega = 1.00

  I(Net) and sigma(I) from profile fitting (Clegg, 1981)

;
_diffrn_radiation_collimation    '0.5 mm'
_diffrn_radiation_detector       'NaI(Tl) scintillation counter'
_diffrn_radiation_monochromator  'planar graphite'
_diffrn_radiation_polarisn_norm  90
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.040
_diffrn_reflns_av_sigmaI/netI    0.0605
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6159
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         2.55
_diffrn_standards_decay_%        'variation +/-15'
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.58
_exptl_absorpt_correction_T_max  0.8683
_exptl_absorpt_correction_T_min  0.8004
_exptl_absorpt_correction_type   'Numerical: face indexing'
_exptl_crystal_colour            orange/brown
_exptl_crystal_density_diffrn    1.33
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             724
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.63
_refine_diff_density_min         -0.56
_refine_ls_abs_structure_Flack   'not measured'
_refine_ls_extinction_coef       'not measured'
_refine_ls_extinction_method     'not required'
_refine_ls_goodness_of_fit_obs   0.8766
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         4220
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0802
_refine_ls_shift/esd_max         0.018
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      'Chebychev polynomial'
_refine_ls_wR_factor_obs         0.0886
_reflns_d_resolution_high        0.840
_reflns_d_resolution_low         7.984
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              14
_reflns_limit_k_min              -14
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_observed          4220
_reflns_number_total             5722
_reflns_observed_criterion       >2.00\s(I)
_cod_data_source_file            806393asup1.cif
_cod_data_source_block           Dalton_8/06393A
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

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_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        1738.1(8)
_cod_original_formula_sum        ' C34 H40 Cl4 N4 Ti1'
_cod_database_code               7027054