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_4311930
_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         (2-Ph2CH-4,6-tert-Bu2-C6H2O)Ti[(OCH2CH2)3N]
_chemical_formula_sum            'C33 H43 N O4 Ti'
_chemical_formula_weight         565.58
_chemical_name_common
2-(Diphenylmethyl)-4,6-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   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.9430(10)
_cell_angle_beta                 102.2840(10)
_cell_angle_gamma                104.3430(10)
_cell_formula_units_Z            2
_cell_length_a                   10.4044(7)
_cell_length_b                   10.5516(7)
_cell_length_c                   14.9791(10)
_cell_measurement_reflns_used    5367
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      28.058
_cell_measurement_theta_min      2.352
_cell_volume                     1552.56(18)
_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  0.0162
_diffrn_reflns_av_sigmaI/netI    0.0552
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9696
_diffrn_reflns_theta_max         28.23
_diffrn_reflns_theta_min         1.40
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.311
_exptl_absorpt_correction_T_max  0.862107
_exptl_absorpt_correction_T_min  0.797962
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_description       irregular
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.681
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.984
_refine_ls_goodness_of_fit_obs   1.034
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         6831
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.984
_refine_ls_restrained_S_obs      1.034
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_obs          0.0500
_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^)+(0.0794P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1390
_refine_ls_wR_factor_obs         0.1270
_reflns_number_observed          5252
_reflns_number_total             6831
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0492901si20040531_034943_1.cif
_cod_data_source_block           mono
_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^)+(0.0794P)^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^)+(0.0794P)^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        1552.6(2)
_cod_database_code               4311930