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_4301084
_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 H172 Cu4 Ge2 N12 O82 W18 '
_chemical_formula_sum            'C48 H172 Cu4 Ge2 N12 O82 W18'
_chemical_formula_weight         5938.58
_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                108.740(7)
_cell_angle_beta                 94.934(6)
_cell_angle_gamma                98.701(8)
_cell_formula_units_Z            1
_cell_length_a                   12.598(7)
_cell_length_b                   16.115(10)
_cell_length_c                   16.337(10)
_cell_measurement_reflns_used    7956
_cell_measurement_temperature    300
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.2
_cell_volume                     3072(3)
_computing_cell_refinement       CrystalClear
_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_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.060
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24527
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    18.025
_exptl_absorpt_correction_T_max  0.5325
_exptl_absorpt_correction_T_min  0.2938
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
    Higashi, T. (1999). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    3.209
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2712.00
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_refine_diff_density_max         5.46
_refine_diff_density_min         -4.94
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_number_parameters     549
_refine_ls_number_reflns         13483
_refine_ls_R_factor_all          0.1018
_refine_ls_R_factor_gt           0.0742
_refine_ls_shift/su_max          0.0010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0884P)^2^+42.9697P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2196
_reflns_number_gt                9309
_reflns_number_total             13483
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic8013267_si_002.cif
_cod_data_source_block           '__GeW9Cu'
_cod_original_cell_volume        3073(3)
_cod_original_formula_sum        'C48 H172 Cu4 Ge2 N12 O82 W18 '
_cod_database_code               4301084