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_4060037
_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_formula_moiety         ' C45 H64 N4 O2 Ti1 , 2(C6 H6) '
_chemical_formula_sum            'C57 H76 N4 O2 Ti'
_chemical_formula_weight         897.16
_chemical_name_systematic
;                                                                               
 [Ti(N-t-Bu){(2-C5H4N)CH2N{2-O-3,5-C6H3(t-Bu)2}2}(py)]
;
_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
_cell_angle_alpha                98.2396(7)
_cell_angle_beta                 106.5212(8)
_cell_angle_gamma                102.9245(9)
_cell_formula_units_Z            2
_cell_length_a                   10.9050(2)
_cell_length_b                   15.6222(3)
_cell_length_c                   16.7849(4)
_cell_measurement_reflns_used    11006
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.910
_cell_volume                     2605.6(1)
_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_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
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  2.12
_diffrn_reflns_av_sigmaI/netI    0.106
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21645
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         2.92
_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    0.21
_exptl_absorpt_correction_T_max  0.939
_exptl_absorpt_correction_T_min  0.882
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             968.64
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.72
_refine_diff_density_min         -0.52
_refine_ls_abs_structure_Flack   none
_refine_ls_extinction_coef       387(88)
_refine_ls_extinction_method
'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_ref   1.0118
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         6681
_refine_ls_number_restraints     102
_refine_ls_R_factor_gt           0.0668
_refine_ls_shift/su_max          0.0026
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Chebychev polynomial with 5 parameters, Carruthers & Watkin , 1979, 
 1.50     1.50     1.31    0.398    0.255    
;
_refine_ls_weighting_scheme      Chebychev
_refine_ls_wR_factor_ref         0.0725
_reflns_limit_h_max              13
_reflns_limit_h_min              -14
_reflns_limit_k_max              20
_reflns_limit_k_min              -20
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                6681
_reflns_number_total             11820
_reflns_threshold_expression     >3.00\s(I)
_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 2.4.1 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:

'_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 '
_cod_original_formula_sum        ' C57 H76 N4 O2 Ti1 '
_cod_database_code               4060037