Complexation of a Heptanuclear Polyoxotantalate Anion with K+: Formation of a Supramolecular [K6-(μ-OH2)6-(OH2)8]6+ Ring Structure
Bernd Morgenstern; Jürgen Sander; Volker Huch; Kaspar Hegetschweiler; Inorganic Chemistry 40 (2001) 5307–5310; doi:10.1021/ic0010858

data_4320273
_publ_contact_author
;
        Kaspar Hegetschweiler
        Anorganische Chemie
        Universit\"at des Saarlandes
        Postfach 151150
        D-66041 Saarbr\"ucken
        Germany
;
_publ_contact_author_email       hegetsch@rz.uni-sb.de
_publ_contact_author_fax         '049 681 302-2663'
_publ_contact_author_phone       '049 681 302-2715'
_publ_section_title
;
 Complexation of a Heptanuclear Polyoxotantalate Anion with K+: Formation
 of a Supramolecular [K6-(\m-OH2)6-(OH2)8]6+ Ring Structure
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5307
_journal_page_last               5310
_journal_paper_doi               10.1021/ic0010858
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C36 H120 K7 O81 Ta7'
_chemical_formula_weight         3389.67
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           58
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2 2n'
_symmetry_space_group_name_H-M   'P n n m'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.539(3)
_cell_length_b                   17.010(3)
_cell_length_c                   21.027(4)
_cell_measurement_temperature    293(2)
_cell_volume                     4484.8(16)
_computing_cell_refinement       'Stoe IPDS Software, Vers. 2.87,1997.'
_computing_data_collection       'Stoe IPDS Software, Vers. 2.87,1997.'
_computing_data_reduction        'Stoe IPDS Software, Vers. 2.87,1997.'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       'image plate'
_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  0.0877
_diffrn_reflns_av_sigmaI/netI    0.0407
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            25098
_diffrn_reflns_theta_full        24.15
_diffrn_reflns_theta_max         24.15
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    8.958
_exptl_absorpt_correction_type   'not applied'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.510
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3256
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.597
_refine_diff_density_min         -1.305
_refine_diff_density_rms         0.187
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         3558
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0286
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0517P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0757
_refine_ls_wR_factor_ref         0.0778
_reflns_number_gt                3121
_reflns_number_total             3558
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0010858.cif
_cod_data_source_block           IC0010858
_cod_database_code               4320273