Combination of lacunary polyoxometalates and high-nuclear transition-metal clusters under hydrothermal conditions. 5. A novel tetrameric cluster of [{Fe(II)Fe(III)(12)(mu(3)-OH)(12)(mu(4)-PO(4))(4)}(B-alpha-PW(9)O(34))(4)](22)(-).
Zhao, Jun-Wei; Zhang, Jie; Zheng, Shou-Tian; Yang, Guo-Yu; Inorganic chemistry 46 (2007) 10944–10946; doi:10.1021/ic701810t

data_4339124
_publ_section_title
;
 Combination of lacunary polyoxometalates and high-nuclear
 transition-metal clusters under hydrothermal conditions. 5. A novel
 tetrameric cluster of
 [{Fe(II)Fe(III)(12)(mu(3)-OH)(12)(mu(4)-PO(4))(4)}(B-alpha-PW(9)O(34))(4)](22)(-).
;
_journal_issue                   26
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10944
_journal_page_last               10946
_journal_paper_doi               10.1021/ic701810t
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C7 H134 Fe13 N7 O200 P8 W36'
_chemical_formula_weight         11109.62
_chemical_name_systematic
; 
 ? 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.891(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   36.666(7)
_cell_length_b                   25.887(5)
_cell_length_c                   21.682(4)
_cell_measurement_reflns_used    25585
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      2.5368
_cell_volume                     20505(7)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Saturn70 (4x4 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  0.0507
_diffrn_reflns_av_sigmaI/netI    0.0478
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            65164
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.80
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    21.166
_exptl_absorpt_correction_T_max  0.4785
_exptl_absorpt_correction_T_min  1.0000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2001)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    3.599
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             19788
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         4.74
_refine_diff_density_min         -1.815
_refine_diff_density_rms         0.330
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1237
_refine_ls_number_reflns         18318
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0526
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0628P)^2^+851.1826P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1327
_refine_ls_wR_factor_ref         0.1378
_reflns_number_gt                16160
_reflns_number_total             18318
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701810t-file001.cif
_cod_data_source_block           q
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/automatic-downloads/retrospective/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 
;
_cod_original_cell_volume        20505(6)
_cod_original_sg_symbol_H-M      C2/m
_cod_database_code               4339124