Linear Trimer Analogues of Calixarene as Chiral Coordinating Ligands: X-ray Crystallographic and NMR Spectroscopic Characterization of Chiral and Achiral Trisphenolates Complexed to Titanium(IV) and Aluminum(III)
William O. Appiah; Angela D. DeGreeff; Gina L. Razidlo; Sarah J. Spessard; Maren Pink; Victor G. Young,; Gretchen E. Hofmeister; Inorganic Chemistry 41 (2002) 3656–3667; doi:10.1021/ic010685j

data_4318184
_publ_section_title
;
 Linear Trimer Analogues of Calixarene as Chiral Coordinating Ligands:
 X-ray Crystallographic and NMR Spectroscopic Characterization of Chiral
 and Achiral Trisphenolates Complexed to Titanium(IV) and Aluminum(III)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3656
_journal_page_last               3667
_journal_paper_doi               10.1021/ic010685j
_journal_volume                  41
_journal_year                    2002
_chemical_compound_source        'G. Hofmeister - Gustavus Adolphus College'
_chemical_formula_sum            'C54 H71 Al O3'
_chemical_formula_weight         795.09
_chemical_name_common            99358aa_Al(trisphenolate)2
_chemical_name_systematic
;
   ?
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.311(2)
_cell_length_b                   20.250(2)
_cell_length_c                   23.093(2)
_cell_measurement_temperature    173(2)
_cell_volume                     10901.0(17)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_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  0.0440
_diffrn_reflns_av_sigmaI/netI    0.0282
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            53253
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         1.33
_exptl_absorpt_coefficient_mu    0.073
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.651
_exptl_absorpt_correction_type   'SADAB (Sheldrick, 1996)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    0.969
_exptl_crystal_description       'Multifaceted block'
_exptl_crystal_F_000             3456
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.338
_refine_diff_density_min         -0.255
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.100
_refine_ls_goodness_of_fit_obs   1.171
_refine_ls_matrix_type           full
_refine_ls_number_parameters     634
_refine_ls_number_reflns         9628
_refine_ls_number_restraints     182
_refine_ls_restrained_S_all      1.119
_refine_ls_restrained_S_obs      1.195
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_obs          0.0623
_refine_ls_shift/esd_max         -0.005
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1052P)^2^+2.7351P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2002
_refine_ls_wR_factor_obs         0.1775
_reflns_number_observed          6828
_reflns_number_total             9628
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic010685j_2.cif
_cod_data_source_block           99358aa_Al(trisphenolate)2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1052P)^2^+2.7351P] 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^)+(0.1052P)^2^+2.7351P] 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        10901.2(18)
_cod_database_code               4318184