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_4321685
_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            'C24.5 H47 N3 O11 Ti3'
_chemical_formula_weight         703.35
_chemical_name_systematic
;
 ?
;
_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                81.996(3)
_cell_angle_beta                 88.815(3)
_cell_angle_gamma                73.583(2)
_cell_formula_units_Z            2
_cell_length_a                   10.891(2)
_cell_length_b                   12.417(3)
_cell_length_c                   12.432(3)
_cell_measurement_reflns_used    all
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      26.42
_cell_measurement_theta_min      1.95
_cell_volume                     1596.7(6)
_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      170(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0199
_diffrn_reflns_av_sigmaI/netI    0.0221
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20540
_diffrn_reflns_theta_full        26.42
_diffrn_reflns_theta_max         26.42
_diffrn_reflns_theta_min         1.95
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.790
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.8709
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'transculent colourless'
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             738
_exptl_crystal_size_max          0.72
_exptl_crystal_size_mid          0.57
_exptl_crystal_size_min          0.41
_refine_diff_density_max         0.765
_refine_diff_density_min         -0.705
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         6490
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0.585
_refine_ls_shift/su_mean         0.015
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0544P)^2^+2.3782P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1201
_refine_ls_wR_factor_ref         0.1229
_reflns_number_gt                5751
_reflns_number_total             6490
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000510u_1.cif
_cod_data_source_block           tktt
_cod_original_cell_volume        1596.6(6)
_cod_original_formula_sum        'C24.50 H47 N3 O11 Ti3'
_cod_database_code               4321685