[MoV2MoVI6VIV8O40(PO4)]5−: the first polyanion with a tetra-capped Keggin structure
Xu, Yan; Zhu, Hao-Guo; Cai, Hu; You, Xiao-Zeng; Chemical Communications  (1999) 787–; doi:10.1039/a900928k

data_7110483
_publ_section_title
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 [MoV2MoVI6VIV8O40(PO4)]5&#x2212;: the first polyanion with a tetra-capped
 Keggin structure
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_journal_issue                   9
_journal_name_full               'Chemical Communications'
_journal_page_first              787
_journal_paper_doi               10.1039/a900928k
_journal_year                    1999
_chemical_formula_sum            'C12 H50 Mo8 N12 Na Ni2 O45 P V8'
_chemical_formula_weight         2429.06
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           95
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4cw 2c'
_symmetry_space_group_name_H-M   'P 43 2 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.829(2)
_cell_length_b                   15.829(2)
_cell_length_c                   28.712(6)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      5.23
_cell_measurement_theta_min      1.21
_cell_volume                     7194(2)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w 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  0.0250
_diffrn_reflns_av_sigmaI/netI    0.0925
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            12486
_diffrn_reflns_theta_max         23.05
_diffrn_reflns_theta_min         1.82
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.954
_exptl_absorpt_correction_T_max  0.2970
_exptl_absorpt_correction_T_min  0.2649
_exptl_absorpt_correction_type
;
empirical via \y scans
North,A.C.T., Phllips,D.C. & Mathews,F.S.(1968), Acta Cryst. A24, 351--359
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.243
_exptl_crystal_description       needle
_exptl_crystal_F_000             4672
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         3.443
_refine_diff_density_min         -1.076
_refine_diff_density_rms         0.268
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.54(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.161
_refine_ls_goodness_of_fit_obs   1.299
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         5046
_refine_ls_number_restraints     250
_refine_ls_restrained_S_all      1.166
_refine_ls_restrained_S_obs      1.255
_refine_ls_R_factor_all          0.1103
_refine_ls_R_factor_obs          0.0765
_refine_ls_shift/esd_max         0.375
_refine_ls_shift/esd_mean        0.022
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2256
_refine_ls_wR_factor_obs         0.1987
_reflns_number_observed          3384
_reflns_number_total             5048
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            900928Ksup1.cif
_cod_data_source_block           ee
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        7194.0(20)
_cod_original_sg_symbol_H-M      P4(3)22
_cod_database_code               7110483