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_4060031
_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
;
?
;
_chemical_formula_moiety         ' C41 H55 Cl1 N3 O2 Sc1 . C6 H6'
_chemical_formula_sum            'C47 H61 Cl N3 O2 Sc'
_chemical_formula_weight         780.43
_chemical_name_systematic
;                                                                               
 [ScCl{(2-C5H4N)CH2N{2-O-3,5-C6H2(t-Bu)2}2}(py)] . (C6H6)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90.00
_cell_angle_beta                 95.537(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   27.0551(8)
_cell_length_b                   17.8450(5)
_cell_length_c                   19.0419(8)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.910
_cell_volume                     9150.5(5)
_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_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       CCD
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.11
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            19772
_diffrn_reflns_theta_max         27.65
_diffrn_reflns_theta_min         2.91
_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    0.26
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_correction_T_min  0.987
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       needle
_exptl_crystal_F_000             3347.37
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.96
_refine_diff_density_min         -0.78
_refine_ls_abs_structure_Flack   none
_refine_ls_extinction_coef       'none required'
_refine_ls_goodness_of_fit_ref   1.0632
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         4820
_refine_ls_number_restraints     42
_refine_ls_R_factor_gt           0.0667
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Chebychev polynomial with 5 parameters, Carruthers & Watkin , 1979, 
 2.37     3.42     2.80     1.33    0.658    
;
_refine_ls_weighting_scheme      'Chebychev polynomial'
_refine_ls_wR_factor_ref         0.0882
_reflns_limit_h_max              34
_reflns_limit_h_min              -35
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                2577
_reflns_number_total             10384
_reflns_threshold_expression     >3.00\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:

'_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      'C 1 2/c 1 '
_cod_original_formula_sum        ' C47 H61 Cl1 N3 O2 Sc1 '
_cod_database_code               4060031