Synthesis, Structures, and Solution Behavior of Di- and Trinuclear Titanium(IV)-Cyclophosphato Complexes
Sou Kamimura; Tsukasa Matsunaga; Shigeki Kuwata; Masakazu Iwasaki; Youichi Ishii; Inorganic Chemistry 43 (2004) 6127–6129; doi:10.1021/ic049206h

data_4311650
_publ_contact_author_email       ishii@chem.chuo-u.ac.jp
_publ_contact_author_fax         +81-3-3817-1895
_publ_contact_author_name        'Youichi Ishii'
_publ_contact_author_phone       +81-3-3817-1901
_publ_section_title
;
 Synthesis, Structures, and Solution Behavior of Di- and Trinuclear
 Titanium(IV)-Cyclophosphato Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6127
_journal_page_last               6129
_journal_paper_doi               10.1021/ic049206h
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         'C67 H77 Cl2 N O12 P5 Ti3 '
_chemical_formula_sum            'C67 H77 Cl2 N O12 P5 Ti3'
_chemical_formula_weight         1457.82
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                94.55(4)
_cell_angle_beta                 97.81(4)
_cell_angle_gamma                92.84(4)
_cell_formula_units_Z            2
_cell_length_a                   11.44(1)
_cell_length_b                   14.128(4)
_cell_length_c                   22.247(8)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    294.1
_cell_measurement_theta_max      19.9
_cell_measurement_theta_min      18.4
_cell_volume                     3544(4)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure Ver. 3.00'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR97
_diffrn_measured_fraction_theta_full 0.9980
_diffrn_measured_fraction_theta_max 0.9980
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.045
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            16918
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_standards_decay_%        -0.96
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.576
_exptl_absorpt_correction_T_max  0.891
_exptl_absorpt_correction_T_min  0.809
_exptl_absorpt_correction_type
;
\y scans (North,Phillips & Matthews, 1968)
;
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1514.00
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.35
_refine_diff_density_min         -0.35
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     888
_refine_ls_number_reflns         7048
_refine_ls_R_factor_gt           0.0510
_refine_ls_shift/su_max          0.0440
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
'w = 1/[0.0003Fo^2^ + 1.0000\s^2^(Fo) + 0.5000]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0560
_reflns_number_gt                7048
_reflns_number_total             16258
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic049206hsi20040618_024436_1.cif
_cod_data_source_block           '_(PPN)[(Cp*TiO)3Cl(P3O9)](4)'
_cod_original_cell_volume        3544.6(4)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C67 H77 Cl2 N O12 P5 Ti3 '
_cod_database_code               4311650