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_4311931
_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
PhCH(2-OH-3,5-tert-Bu2C6H2)(3,5-tert-Bu2C6H2-2-OTi[(OCH2CH2)3N])
_chemical_formula_sum            'C41 H59 N O5 Ti'
_chemical_formula_weight         693.79
_chemical_name_common
;
2-(\a-(2-hydroxy-3,5-di-tert-butylphenyl)benzyl)-
4,6-di-tert-butylphenoxytitanatrane
;
_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   mixed
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                80.299(2)
_cell_angle_beta                 74.070(2)
_cell_angle_gamma                79.102(2)
_cell_formula_units_Z            2
_cell_length_a                   10.9755(11)
_cell_length_b                   11.3514(11)
_cell_length_c                   16.730(2)
_cell_measurement_reflns_used    5568
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      28.250
_cell_measurement_theta_min      2.432
_cell_volume                     1953.1(4)
_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      170(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  0.0364
_diffrn_reflns_av_sigmaI/netI    0.0450
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17541
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         1.84
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.261
_exptl_absorpt_correction_T_max  0.801471
_exptl_absorpt_correction_T_min  0.491751
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.180
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.43
_refine_diff_density_max         1.362
_refine_diff_density_min         -0.554
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.998
_refine_ls_goodness_of_fit_obs   1.024
_refine_ls_hydrogen_treatment    'isotropic + riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     633
_refine_ls_number_reflns         8898
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.998
_refine_ls_restrained_S_obs      1.024
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_obs          0.0605
_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^)+(0.1304P)^2^+0.3112P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1835
_refine_ls_wR_factor_obs         0.1702
_reflns_number_observed          7349
_reflns_number_total             8898
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0492901si20040531_034943_2.cif
_cod_data_source_block           monobis
_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^)+(0.1304P)^2^+0.3112P] 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^)+(0.1304P)^2^+0.3112P] where P=(Fo^2^+2Fc^2^)/3'.

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

The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'difmap + geom' was changed to
'mixed'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        1953.1(3)
_cod_database_code               4311931