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_4318183
_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_formula_sum            'C116 H184 O15 Ti2'
_chemical_formula_weight         1914.43
_chemical_name_common            99323m_Ti2(trisphenolate)2(O-t-Bu)2
_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-97
_cell_angle_alpha                117.3210(10)
_cell_angle_beta                 108.001(2)
_cell_angle_gamma                99.821(2)
_cell_formula_units_Z            1
_cell_length_a                   14.6880(13)
_cell_length_b                   15.4702(14)
_cell_length_c                   15.8721(14)
_cell_measurement_temperature    173(2)
_cell_volume                     2831.5(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_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  0.0548
_diffrn_reflns_av_sigmaI/netI    0.1031
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25238
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    0.200
_exptl_crystal_density_diffrn    1.123
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1044
_refine_diff_density_max         0.671
_refine_diff_density_min         -0.769
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.936
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     686
_refine_ls_number_reflns         12507
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.1371
_refine_ls_R_factor_gt           0.0705
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1204P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1785
_refine_ls_wR_factor_ref         0.2177
_reflns_number_gt                6526
_reflns_number_total             12507
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010685j_1.cif
_cod_data_source_block           99323m_Ti2(trisphenolate)2(O-t-Bu)2
_cod_database_code               4318183