Rare Sandwich-Type Polyoxomolybdates Constructed from Di-/Tetra-Nuclear Transition-Metal Clusters and Trivacant Keggin Germanomolybdate Fragments
Suzhi Li; Junwei Zhao; Pengtao Ma; Juan Du; Jingyang Niu; Jingping Wang; Inorganic Chemistry 48 (2009) 9819–9830; doi:10.1021/ic901330y

data_4303390
_publ_section_title
;
Rare Sandwich-Type Polyoxomolybdates Constructed from Di-/Tetra-Nuclear
Transition-Metal Clusters and Trivacant Keggin Germanomolybdate Fragments
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9819
_journal_page_last               9830
_journal_paper_doi               10.1021/ic901330y
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'Cu2 Ge2 H78 Mo18 Na12 O105'
_chemical_formula_weight         4033.68
_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   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                73.2850(10)
_cell_angle_beta                 66.56
_cell_angle_gamma                60.71
_cell_formula_units_Z            1
_cell_length_a                   13.2369(8)
_cell_length_b                   13.5286(8)
_cell_length_c                   16.6405(13)
_cell_measurement_temperature    293(2)
_cell_volume                     2368.3(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0584
_diffrn_reflns_av_sigmaI/netI    0.0380
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            10961
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.32
_exptl_absorpt_coefficient_mu    3.546
_exptl_absorpt_correction_T_max  0.6964
_exptl_absorpt_correction_T_min  0.6008
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    2.828
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1928
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.227
_refine_diff_density_min         -0.939
_refine_diff_density_rms         0.160
_refine_ls_extinction_coef       0.00249(8)
_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   1.076
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         8059
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0327
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0398P)^2^+12.6241P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0862
_refine_ls_wR_factor_ref         0.0875
_reflns_number_gt                7635
_reflns_number_total             8059
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901330y_si_002_1.cif
_cod_data_source_block           419901
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        2368.4(3)
_cod_original_formula_sum        'H78 Cu2 Ge2 Mo18 Na12 O105'
_cod_database_code               4303390