Isolation and Structural Characterization of Triethanolaminotitanatranes: X-ray Structures of Partial Hydrolysis Condensates
Tim Kemmitt; Najeh I. Al-Salim; Graeme J. Gainsford; Inorganic Chemistry 39 (2000) 6067–6071; doi:10.1021/ic000510u

data_4321686
_publ_contact_author_email       t.kemmitt@irl.cri.nz
_publ_contact_author_fax         64(4)5690142
_publ_contact_author_name        'Kemmitt, T.'
_publ_contact_author_phone       64(4)5690000
_publ_section_title
;
 Isolation and Structural Characterization of Triethanolaminotitanatranes:
 X-ray Structures of Partial Hydrolysis Condensates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6067
_journal_page_last               6071
_journal_paper_doi               10.1021/ic000510u
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C31 H58 N4 O13 Ti3'
_chemical_formula_weight         838.51
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.2800(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.4237(7)
_cell_length_b                   19.9219(15)
_cell_length_c                   20.3520(15)
_cell_measurement_reflns_used    all
_cell_measurement_temperature    158(2)
_cell_measurement_theta_max      26.47
_cell_measurement_theta_min      2.80
_cell_volume                     3747.0(5)
_computing_cell_refinement       'Bruker P4 SMART'
_computing_data_collection       'Bruker P4 SMART'
_computing_data_reduction        'Bruker P4 SMART'
_computing_molecular_graphics    'WINGX (ORTEPIII), 1999)'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      158(2)
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       CCD
_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  0.0434
_diffrn_reflns_av_sigmaI/netI    0.0461
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            23554
_diffrn_reflns_theta_full        26.47
_diffrn_reflns_theta_max         26.47
_diffrn_reflns_theta_min         2.80
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.691
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.805
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'translucent colourless'
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'prismatic block'
_exptl_crystal_F_000             1768
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.556
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         7337
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0645P)^2^+3.0521P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1148
_refine_ls_wR_factor_ref         0.1287
_reflns_number_gt                5369
_reflns_number_total             7337
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000510u_2.cif
_cod_data_source_block           k451
_cod_database_code               4321686