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_4060032
_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         ' C48 H52 Cl2 N4 O4 Sc2 . 2 (CH2Cl2) '
_chemical_formula_sum            'C50 H56 Cl6 N4 O4 Sc2'
_chemical_formula_weight         1079.65
_chemical_name_systematic
;                                                                               
 [Sc2{(2-NC5H4)CH2N{CH2(2-O-4,6-C6H2Me2)}2}2Cl2] . 2(CH2Cl2)
;
_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                89.9518(6)
_cell_angle_beta                 84.0259(6)
_cell_angle_gamma                88.0933(5)
_cell_formula_units_Z            2
_cell_length_a                   11.7034(1)
_cell_length_b                   12.0006(1)
_cell_length_c                   18.5464(2)
_cell_measurement_reflns_used    10791
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     2589.21(4)
_computing_cell_refinement
; 
 Denzo/Scalepack (Otwinowski & Minor, 1996) 
;
_computing_data_collection
; 
 COLLECT (Nonius BV, 1997) 
;
_computing_data_reduction
; 
 Denzo/Scalepack (Otwinowski & Minor, 1996) 
;
_computing_molecular_graphics
; 
 CAMERON (Watkin et al 1996) 
;
_computing_publication_material
; 
 CRYSTALS (Watkin et al 2001) 
;
_computing_structure_refinement
; 
 CRYSTALS (Watkin et al 2001) 
;
_computing_structure_solution
; 
 SIR97 (Altomare et al, 1999) 
;
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type
; 
Enraf Nonius Kappa CCD 
;
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.02
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            21611
_diffrn_reflns_theta_full        23.812
_diffrn_reflns_theta_max         27.528
_diffrn_reflns_theta_min         1.104
_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    0.618
_exptl_absorpt_correction_T_max  0.74
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 Denzo/Scalepack (Otwinowski & Minor, 1996) 
;
_exptl_crystal_colour            ' colourless '
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       ' block '
_exptl_crystal_F_000             1120.000
_exptl_crystal_size_max          0.64
_exptl_crystal_size_mid          0.56
_exptl_crystal_size_min          0.48
_refine_diff_density_max         0.86
_refine_diff_density_min         -1.00
_refine_ls_abs_structure_Flack   none
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0799
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         8931
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0387
_refine_ls_shift/su_max          0.001946
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method = Prince modified Chebychev polynomial, (Watkin, 1994) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2]^2 
 
 1.15 0.835 0.992 0.281 0.237 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0456
_refine_ls_wR_factor_gt          0.0398
_refine_ls_wR_factor_ref         0.0398
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              15
_reflns_limit_k_min              -15
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                8939
_reflns_number_total             11772
_reflns_threshold_expression     I>3.00u(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        ' C50 H56 Cl6 N4 O4 Sc2 '
_cod_database_code               4060032