Controlled assembly and solution observation of a 2.6 nm polyoxometalate "super" tetrahedron cluster: [KFe12(OH)18(α-1,2,3-P2W15O56)4]29‒
Pradeep, Chullikkattil P.; Long, De-Liang; Kögerler, Paul; Cronin, Leroy; Chemical Communications (Cambridge, United Kingdom)  (2007) 4254–4256; doi:10.1039/b707202c

data_7113222
_publ_section_title
;
 Controlled assembly and solution observation of a 2.6 nm polyoxometalate
 "super" tetrahedron cluster: [KFe12(OH)18(\a-1,2,3-P2W15O56)4]29--
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   41
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              4254
_journal_page_last               4256
_journal_paper_doi               10.1039/b707202c
_journal_year                    2007
_chemical_formula_sum            'Fe12 H158 K22 Na8 O312 P8 W60'
_chemical_formula_weight         18144.34
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 122.929(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   47.8099(15)
_cell_length_b                   30.6240(15)
_cell_length_c                   29.8033(11)
_cell_measurement_reflns_used    8430
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.31
_cell_measurement_theta_min      2.51
_cell_volume                     36626(3)
_computing_cell_refinement       'Bruker Apex 2'
_computing_data_collection       'Bruker Apex 2'
_computing_data_reduction        'Apex 2'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-98 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker Apex II'
_diffrn_measurement_method       'omega and phi 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  0.1131
_diffrn_reflns_av_sigmaI/netI    0.0688
_diffrn_reflns_limit_h_max       57
_diffrn_reflns_limit_h_min       -57
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            254612
_diffrn_reflns_theta_full        25.44
_diffrn_reflns_theta_max         25.44
_diffrn_reflns_theta_min         0.96
_exptl_absorpt_coefficient_mu    19.608
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.289
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    3.291
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             32128
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.406
_refine_diff_density_min         -2.246
_refine_diff_density_rms         0.363
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2085
_refine_ls_number_reflns         34305
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0880
_refine_ls_R_factor_gt           0.0477
_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^)+(0.0442P)^2^+1988.0289P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1245
_reflns_number_gt                23476
_reflns_number_total             34305
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7102210
_cod_data_source_file            b707202c.txt
_cod_data_source_block           pc163c2m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      C2/m
_cod_original_formula_sum        'H158 Fe12 K22 Na8 O312 P8 W60'
_cod_database_code               7113222