Structure and Magnetism of [n-BuNH3]12[Cu4(GeW9O34)2].14H2O Sandwiching a Rhomblike Cu48+ Tetragon through α-Keggin Linkage
Toshihiro Yamase; Hiroko Abe; Eri Ishikawa; Hiroyuki Nojiri; Yuhgo Ohshima; Inorganic Chemistry 48 (2009) 138–148; doi:10.1021/ic8013267

data_4301085
_publ_contact_author_email       tyamase@res.titech.ac.jp
_publ_contact_author_fax         +81-45-924-5260
_publ_contact_author_name        'Toshihiro Yamase'
_publ_contact_author_phone       +81-45-924-5260
_publ_section_title
;
Structure and Magnetism of [n-BuNH3]12[Cu4(GeW9O34)2].14H2O Sandwiching a
Rhomblike Cu48+ Tetragon through \a-Keggin Linkage
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              138
_journal_page_last               148
_journal_paper_doi               10.1021/ic8013267
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C48 H162 Cu4 Ge2 N12 O77 W18 '
_chemical_formula_sum            'C48 H162 Cu4 Ge2 N12 O77 W18'
_chemical_formula_weight         5848.51
_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'
_audit_creation_date             2008-07-14
_audit_creation_method           'by CrystalStructure 3.8'
_cell_angle_alpha                110.526(1)
_cell_angle_beta                 92.662(1)
_cell_angle_gamma                91.344(1)
_cell_formula_units_Z            1
_cell_length_a                   12.064(1)
_cell_length_b                   16.191(1)
_cell_length_c                   16.317(1)
_cell_measurement_reflns_used    8332
_cell_measurement_temperature    10
_cell_measurement_theta_max      29.63
_cell_measurement_theta_min      2.2
_cell_volume                     2978.9(4)
_computing_cell_refinement       HKL2000
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  'Rigaku AFC7'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.023
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27093
_diffrn_reflns_theta_full        29.63
_diffrn_reflns_theta_max         29.63
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    18.586
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6787
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    3.260
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2662.00
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         4.03
_refine_diff_density_min         -2.02
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_number_parameters     701
_refine_ls_number_reflns         16797
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0312
_refine_ls_shift/su_max          0.0010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0341P)^2^+26.8069P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0845
_reflns_number_gt                13757
_reflns_number_total             16767
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic8013267_si_003.cif
_cod_data_source_block           '_GeW9CuHe'
_cod_original_cell_volume        2977.0
_cod_original_formula_sum        'C48 H162 Cu4 Ge2 N12 O77 W18 '
_cod_database_code               4301085