Acetate-driven polyoxometalate demetalation: An open-shell diiron polytungstate comprising two rotational Keggin isomers
Botar, Bogdan; Kögerler, Paul; Dalton Transactions  (2008) 3150–3152; doi:10.1039/b802147c

data_7004034
_publ_section_title
;
 Acetate-driven polyoxometalate demetalation: An open-shell diiron
 polytungstate comprising two rotational Keggin isomers
;
_journal_issue                   24
_journal_name_full               'Dalton Transactions'
_journal_page_first              3150
_journal_page_last               3152
_journal_paper_doi               10.1039/b802147c
_journal_year                    2008
_chemical_formula_moiety         'Fe2 O73 OH Si2 W20, 5(C2 H8 N), K8, 17(H2O)'
_chemical_formula_sum            'C10 H75 Fe2 K8 N5 O91 Si2 W20'
_chemical_formula_weight         5879.43
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                64.248(4)
_cell_angle_beta                 88.096(7)
_cell_angle_gamma                80.864(5)
_cell_formula_units_Z            2
_cell_length_a                   12.428(3)
_cell_length_b                   19.803(5)
_cell_length_c                   22.591(8)
_cell_measurement_reflns_used    1015
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.12
_cell_measurement_theta_min      2.62
_cell_volume                     4940(2)
_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      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.983
_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  0.0553
_diffrn_reflns_av_sigmaI/netI    0.0793
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            50845
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    23.934
_exptl_absorpt_correction_T_max  0.1143
_exptl_absorpt_correction_T_min  0.0375
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            yellow-green
_exptl_crystal_density_diffrn    3.952
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             5220
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         5.383
_refine_diff_density_min         -3.936
_refine_diff_density_rms         0.506
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1279
_refine_ls_number_reflns         24267
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0505
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0574P)^2^+70.4767P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1239
_refine_ls_wR_factor_ref         0.1295
_reflns_number_gt                20346
_reflns_number_total             24267
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b802147c.txt
_cod_data_source_block           fe1m
_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 

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      P-1
_cod_database_code               7004034