Synergistic Combination of Multi-Zr(IV) Cations and Lacunary Keggin Germanotungstates Leading to a Gigantic Zr24-Cluster-Substituted Polyoxometalate.
Huang, Ling; Wang, Sa-Sa; Zhao, Jun-Wei; Cheng, Lin; Yang, Guo-Yu; Journal of the American Chemical Society 136 (2014) 7637–7642; doi:10.1021/ja413134w

data_4121855
_publ_section_title
;
 Synergistic Combination of Multi-Zr(IV) Cations and Lacunary Keggin
 Germanotungstates Leading to a Gigantic Zr24-Cluster-Substituted
 Polyoxometalate.
;
_journal_issue                   21
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7637
_journal_page_last               7642
_journal_paper_doi               10.1021/ja413134w
_journal_volume                  136
_journal_year                    2014
_chemical_formula_sum            'Ge6 H186 K22 Na10 O337 W56 Zr24'
_chemical_formula_weight         19590.01
_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_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                67.465(2)
_cell_angle_beta                 76.759(2)
_cell_angle_gamma                73.217(2)
_cell_formula_units_Z            1
_cell_length_a                   17.1764(4)
_cell_length_b                   20.7259(6)
_cell_length_c                   23.1192(5)
_cell_measurement_reflns_used    25299
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.82
_cell_volume                     7212.6(3)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean none
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Mercury2 (2x2 bin mode)'
_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  0.0634
_diffrn_reflns_av_sigmaI/netI    0.0652
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
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_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            70793
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.82
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    24.131
_exptl_absorpt_correction_T_max  0.1598
_exptl_absorpt_correction_T_min  0.0433
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    4.510
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             8706
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         4.919
_refine_diff_density_min         -4.602
_refine_diff_density_rms         0.420
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1849
_refine_ls_number_reflns         25299
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0498
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0549P)^2^+160.6426P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1222
_refine_ls_wR_factor_ref         0.1311
_reflns_number_gt                20748
_reflns_number_total             25299
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja413134w_si_002.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4121855.cif.
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'H186 Ge6 K22 Na10 O337 W56 Zr24'
_cod_database_code               4121855