Titanatranes Derailed: Static and Dynamic Triethanolamine Slippage Induced by Polyphenoxide Chelation
Aaron G. Maestri; Seth N. Brown; Inorganic Chemistry 43 (2004) 6995–7004; doi:10.1021/ic0492901

data_4311932
_publ_section_title
;
 Titanatranes Derailed: Static and Dynamic Triethanolamine Slippage
 Induced by Polyphenoxide Chelation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6995
_journal_page_last               7004
_journal_paper_doi               10.1021/ic0492901
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety
'[{N(CH2CH2O)3}(PhCH(C6H2-t-Bu2O)2)Ti2]4 . 2 C5H12 . 8.5 CH2Cl2'
_chemical_formula_sum            'C206.5 H321 Cl17 N8 O32 Ti8'
_chemical_formula_weight         4413.56
_chemical_name_common
;
Bis(nitrilotriethoxy)-benzylidenedi-3,5-di-tert-butyl-2-phenoxy)dititanium(IV) 
tetramer dipentane octasesqui(dichloromethane) solvate
;
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 95.7410(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.581(2)
_cell_length_b                   30.981(2)
_cell_length_c                   28.825(2)
_cell_measurement_reflns_used    8441
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.144
_cell_measurement_theta_min      2.351
_cell_volume                     24507(3)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measurement_device       'Bruker SMART 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  0.0381
_diffrn_reflns_av_sigmaI/netI    0.0761
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            77317
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.31
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.493
_exptl_absorpt_correction_T_max  0.492022
_exptl_absorpt_correction_T_min  0.403354
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.196
_exptl_crystal_description       block
_exptl_crystal_F_000             9348
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.50
_refine_diff_density_max         2.001
_refine_diff_density_min         -1.051
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.000
_refine_ls_goodness_of_fit_obs   1.135
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1270
_refine_ls_number_reflns         28593
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_restrained_S_obs      1.135
_refine_ls_R_factor_all          0.1171
_refine_ls_R_factor_obs          0.0759
_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^)+(0.1647P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2639
_refine_ls_wR_factor_obs         0.2330
_reflns_number_observed          17366
_reflns_number_total             28593
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0492901si20040531_034943_3.cif
_cod_data_source_block           bisphen
_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 'calc
w=1/[\s^2^(Fo^2^)+(0.1647P)^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^)+(0.1647P)^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 
;
_cod_original_cell_volume        24507.3(29)
_cod_original_formula_sum        'C206.50 H321 Cl17 N8 O32 Ti8'
_cod_database_code               4311932