Long Hydrogen-Bonded Rod of Molecular Oxide: A Hexatantalate Tetramer
Miki Matsumoto; Yoshiki Ozawa; Atsushi Yagasaki; Inorganic Chemistry 51 (2012) 5991–5993; doi:10.1021/ic3004883

data_4329362
_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
;
 Long Hydrogen-Bonded Rod of Molecular Oxide: A Hexatantalate Tetramer
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5991
_journal_page_last               5993
_journal_paper_doi               10.1021/ic3004883
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety
'7(C16 H36 N), 2(H4.5 Ta6 O19), 4(C4 H8 O), 11(H2 O)'
_chemical_formula_sum            'C128 H315 N7 O53 Ta12'
_chemical_formula_weight         4972.28
_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                77.0920(10)
_cell_angle_beta                 86.1770(10)
_cell_angle_gamma                88.6830(10)
_cell_formula_units_Z            4
_cell_length_a                   20.6354(5)
_cell_length_b                   25.5951(7)
_cell_length_c                   37.2058(8)
_cell_measurement_temperature    110(2)
_cell_volume                     19110.9(8)
_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_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'RIGAKU R-AXIS RAPID'
_diffrn_measurement_method       '\w oscillation'
_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  0.0810
_diffrn_reflns_av_sigmaI/netI    0.1200
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            187269
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    6.906
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.3393
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.728
_exptl_crystal_description       block
_exptl_crystal_F_000             9728
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.487
_refine_diff_density_min         -1.591
_refine_diff_density_rms         0.210
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1855
_refine_ls_number_reflns         86973
_refine_ls_number_restraints     196
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.2019
_refine_ls_R_factor_gt           0.0917
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1148P)^2^+101.6282P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2244
_refine_ls_wR_factor_ref         0.2794
_reflns_number_gt                38074
_reflns_number_total             86973
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3004883_si_001.cif
_cod_data_source_block           ya1103
_cod_original_formula_sum        'C64 H157.50 N3.50 O26.50 Ta6'
_cod_database_code               4329362