Synthesis, Structures, and Reactions of Titanium, Scandium, and Yttrium Complexes of Diamino-bis(phenolate) Ligands: Monomeric, Dimeric, Neutral, Cationic, and Multiply Bonded Derivatives
Catherine L. Boyd; Thierry Toupance; Ben R. Tyrrell; Benjamin D. Ward; Claire R. Wilson; Andrew R. Cowley; Philip Mountford; Organometallics 24 (2005) 309–330; doi:10.1021/om0493661

data_4060035
_publ_section_title
;
 Synthesis, Structures, and Reactions of Titanium, Scandium, and
 Yttrium Complexes of Diamino-bis(phenolate) Ligands: Monomeric,
 Dimeric, Neutral, Cationic, and Multiply Bonded Derivatives
;
_journal_name_full               Organometallics
_journal_page_first              309
_journal_page_last               330
_journal_paper_doi               10.1021/om0493661
_journal_volume                  24
_journal_year                    2005
_chemical_compound_source
; 
 [TiCl4(THF)2] + K2[{(2-NC5H4)CH2N{CH2(2-O-4,6-C6H2Me2)}2] 
;
_chemical_formula_moiety         ' C24 H26 Cl2 N2 O2 Ti1 , 2.5 (C6H6)'
_chemical_formula_sum            'C39 H41 Cl2 N2 O2 Ti'
_chemical_formula_weight         688.57
_chemical_name_systematic
;
 [TiCl2{(2-NC5H4)CH2N{CH2(2-O-4,6-C6H2Me2)}2] . 2.5(C6H6)
;
_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
_cell_angle_alpha                90
_cell_angle_beta                 92.4510(23)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7447(7)
_cell_length_b                   9.0987(4)
_cell_length_c                   24.7923(16)
_cell_measurement_reflns_used    19769
_cell_measurement_temperature    150
_cell_measurement_theta_max      23.2
_cell_measurement_theta_min      5.0
_cell_volume                     3548.4
_computing_cell_refinement
;                                                                               
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996)
;
_computing_data_collection
;                                                                               
KappaCCD software 'Collect' (Nonius, 2000)                                   
;
_computing_data_reduction
;                                                                               
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996)
;
_computing_publication_material
;                                                                               
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)                
;
_computing_structure_refinement
;                                                                               
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)                
;
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'
_diffrn_ambient_temperature      150
_diffrn_measurement_method       2\q/\w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.068
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            19769
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         5.12
_diffrn_standards_decay_%        'not measured'
_diffrn_standards_interval_count 'not measured'
_diffrn_standards_interval_time  'not measured'
_diffrn_standards_number         'not measured'
_exptl_absorpt_coefficient_mu    0.42
_exptl_absorpt_correction_T_max  0.959
_exptl_absorpt_correction_T_min  0.959
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.29
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       needle
_exptl_crystal_F_000             1444
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.37
_refine_diff_density_min         -0.31
_refine_ls_abs_structure_Flack   none
_refine_ls_extinction_coef       102.2(115)
_refine_ls_extinction_method
'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_obs   0.5458
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         3047
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0581
_refine_ls_shift/esd_max         0.0260
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      unit
_refine_ls_wR_factor_obs         0.0641
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              10
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_observed          3047
_reflns_number_total             4850
_reflns_observed_criterion       >2.00\s(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic ' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'Unit weights' was changed to
'unit'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z 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_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        ' C39 H41 Cl2 N2 O2 Ti1 '
_cod_database_code               4060035