Combination between lacunary polyoxometalates and high-nuclear transition metal clusters under hydrothermal conditions: first (3,6)-connected framework constructed from sandwich-type polyoxometalate building blocks containing a novel (Cu8) cluster.
Zhao, Jun-Wei; Zhang, Jie; Zheng, Shou-Tian; Yang, Guo-Yu; Chemical communications (Cambridge, England)  (2008) 570–572; doi:10.1039/b713510f

data_7102861
_publ_section_title
;
 Combination between lacunary polyoxometalates and high-nuclear
 transition metal clusters under hydrothermal conditions: first
 (3,6)-connected framework constructed from sandwich-type
 polyoxometalate building blocks containing a novel (Cu8) cluster.
;
_journal_issue                   5
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              570
_journal_page_last               572
_journal_paper_doi               10.1039/b713510f
_journal_year                    2008
_chemical_formula_sum            'C12 H50 Cu9 Ge2 N8 O72 W18'
_chemical_formula_weight         5484.94
_chemical_name_systematic
;
?
;
_space_group_IT_number           138
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4ac 2ac'
_symmetry_space_group_name_H-M   'P 42/n c m :2'
_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            4
_cell_length_a                   21.6769(2)
_cell_length_b                   21.6769(2)
_cell_length_c                   18.8529(3)
_cell_measurement_reflns_used    273
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.63
_cell_measurement_theta_min      2.54
_cell_volume                     8858.75(18)
_computing_cell_refinement       'Siemens SMART'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SMART'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Siemens Smart 1K'
_diffrn_measurement_method       CCD_Profile_fitting
_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  0.0763
_diffrn_reflns_av_sigmaI/netI    0.0299
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            44138
_diffrn_reflns_theta_full        25.63
_diffrn_reflns_theta_max         25.63
_diffrn_reflns_theta_min         2.54
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    26.137
_exptl_absorpt_correction_T_max  0.1751
_exptl_absorpt_correction_T_min  0.0555
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    4.113
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       ployhedron
_exptl_crystal_F_000             9644
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.984
_refine_diff_density_min         -1.619
_refine_diff_density_rms         0.289
_refine_ls_extinction_coef       0.000090(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         4235
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0308
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0182P)^2^+185.1553P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0596
_refine_ls_wR_factor_ref         0.0681
_reflns_number_gt                3404
_reflns_number_total             4235
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b713510f.txt
_cod_data_source_block           q
_cod_original_sg_symbol_H-M      P4(2)/ncm
_cod_database_code               7102861