Decatantalate-The Last Member of the Group 5 Decametalate Family
Miki Matsumoto; Yoshiki Ozawa; Atsushi Yagasaki; Yang Zhe; Inorganic Chemistry 52 (2013) 7825–7827; doi:10.1021/ic400864e

data_4335480
_publ_contact_author_address
;Department of Chemistry
Kwansei Gakuin University
Sanda
669-1337
Japan
;
_publ_contact_author_email       yagasaki@kwansei.ac.jp
_publ_contact_author_fax         81(79)5658397
_publ_contact_author_name        'Yagasaki, Atsushi'
_publ_contact_author_phone       81(79)5658396
_publ_section_title
;
 Decatantalate-The Last Member of the Group 5 Decametalate Family
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7825
_journal_page_last               7827
_journal_paper_doi               10.1021/ic400864e
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         '{(C4 H9)4 N}6 [Ta10 O28], 6(H2 O)'
_chemical_formula_sum            'C96 H228 N6 O34 Ta10'
_chemical_formula_weight         3820.34
_chemical_name_systematic
;
 hexakis(tetrabutylammonium)decatantalate, hexahydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 95.1390(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.5165(3)
_cell_length_b                   19.4161(4)
_cell_length_c                   21.6413(5)
_cell_measurement_temperature    150(1)
_cell_volume                     6493.7(2)
_computing_cell_refinement       'Rapid Auto (Rigaku, 2006)'
_computing_data_collection       'Rapid Auto (Rigaku, 2006)'
_computing_data_reduction
'Rapid Auto (Rigaku, 2006), SORTAV (Blessing, 1995)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(1)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'RIGAKU R-AXIS RAPID'
_diffrn_measurement_method       '\w oscillatin'
_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  0.1160
_diffrn_reflns_av_sigmaI/netI    0.0843
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            94242
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    8.453
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5895
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.954
_exptl_crystal_description       block
_exptl_crystal_F_000             3696
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.035
_refine_diff_density_min         -3.501
_refine_diff_density_rms         0.287
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     657
_refine_ls_number_reflns         14900
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0874
_refine_ls_R_factor_gt           0.0555
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0723P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1261
_refine_ls_wR_factor_ref         0.1487
_reflns_number_gt                10295
_reflns_number_total             14900
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400864e_si_001_2.cif
_cod_data_source_block           ya1212_150k
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4335480