Six-Coordinate Titanium Complexes of a Tripodal Aminetris(phenoxide) Ligand: Synthesis, Structure, and Dynamics
Fortner, Kevin C.; Bigi, Julian P.; Brown, Seth N.; Inorganic Chemistry 44 (2005) 2803–2814; doi:10.1021/ic048403d

data_4300816
_publ_section_title
;
 Six-Coordinate Titanium Complexes of a Tripodal Aminetris(phenoxide)
 Ligand: Synthesis, Structure, and Dynamics
;
_journal_coden_ASTM              INOCAJ
_journal_issue                   8
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2803
_journal_page_last               2814
_journal_paper_doi               10.1021/ic048403d
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         '[N(CH2C6H2-t-Bu2O)3]Ti(hq) . CH3CN . 0.5 C6H6'
_chemical_formula_sum            'C59 H78 N3 O4 Ti'
_chemical_formula_weight         941.14
_chemical_name_common
;
[Nitrilotris(3,5-di-tert-butyl-2-cresolato)](8-oxyquinolinato)titanium(IV) 
acetonitrile hemibenzene solvate
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                81.1100(10)
_cell_angle_beta                 69.2120(10)
_cell_angle_gamma                65.4030(10)
_cell_formula_units_Z            2
_cell_length_a                   12.6377(8)
_cell_length_b                   14.5709(9)
_cell_length_c                   16.8667(10)
_cell_measurement_reflns_used    5717
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.96
_cell_measurement_theta_min      2.58
_cell_volume                     2640.1(3)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker XP'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measurement_device       'Bruker APEX'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_av_sigmaI/netI    0.0740
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19331
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    0.210
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86618
_exptl_absorpt_correction_type   'empirical using SADABS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_description       rod
_exptl_crystal_F_000             1014
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.005
_refine_ls_goodness_of_fit_obs   1.066
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         9281
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_restrained_S_obs      1.066
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_obs          0.0475
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0549P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1189
_refine_ls_wR_factor_obs         0.1054
_reflns_number_observed          6657
_reflns_number_total             9283
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic048403dsi20041112_054527_3.cif
_cod_data_source_block           tihq
_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:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0549P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0549P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4300816