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_4311652
_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_sum            'C69.5 H79 N O15 P6 Ti3'
_chemical_formula_weight         1497.93
_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                79.799(3)
_cell_angle_beta                 89.912(5)
_cell_angle_gamma                65.218(2)
_cell_formula_units_Z            2
_cell_length_a                   11.2743(9)
_cell_length_b                   13.313(1)
_cell_length_c                   26.442(2)
_cell_measurement_reflns_used    14312
_cell_measurement_temperature    103.2
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      2.4
_cell_volume                     3534.6(5)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    'DIRDIF94 (PATTY)'
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.9788
_diffrn_measured_fraction_theta_max 0.9788
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.040
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            31333
_diffrn_reflns_theta_full        27.36
_diffrn_reflns_theta_max         27.36
_exptl_absorpt_coefficient_mu    0.532
_exptl_absorpt_correction_T_max  0.899
_exptl_absorpt_correction_T_min  0.769
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.56
_refine_diff_density_min         -0.82
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.445
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     820
_refine_ls_number_reflns         15657
_refine_ls_R_factor_gt           0.0551
_refine_ls_shift/su_max          0.0007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.04000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1214
_reflns_number_gt                10676
_reflns_number_total             15670
_cod_data_source_file            ic049206hsi20040618_024436_3.cif
_cod_data_source_block           (PPN)[(Cp*TiO)(P4O12)](2)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C69.50 H79 N O15 P6 Ti3 '
_cod_database_code               4311652
_reflns_threshold_criterion      F^2^>2.0\s(F^2^)