Double Sandwich Polyoxometalate and Its Fe(III) Substituted Derivative, [As2Fe5Mo21O82]17- and [As2Fe6Mo20O80(H2O)2]16-
Xiangqian Dong; Yanping Zhang; Bin Liu; Yanzhong Zhen; Huaiming Hu; Ganglin Xue; Inorganic Chemistry 51 (2012) 2318–2324; doi:10.1021/ic202314g

data_4328374
_publ_section_title
;
 Double Sandwich Polyoxometalate and Its Fe(III) Substituted Derivative,
 [As2Fe5Mo21O82]17- and [As2Fe6Mo20O80(H2O)2]16-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2318
_journal_page_last               2324
_journal_paper_doi               10.1021/ic202314g
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'As2 Fe5 H96 Mo21 N17 O96'
_chemical_formula_weight         4314.77
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 106.5630(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.5756(18)
_cell_length_b                   26.105(2)
_cell_length_c                   23.470(2)
_cell_measurement_temperature    296(2)
_cell_volume                     11496.0(17)
_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      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0719
_diffrn_reflns_av_sigmaI/netI    0.0989
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            56640
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    3.494
_exptl_absorpt_correction_T_max  0.752
_exptl_absorpt_correction_T_min  0.636
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadbas
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.493
_exptl_crystal_description       block
_exptl_crystal_F_000             8244
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.214
_refine_diff_density_min         -1.150
_refine_diff_density_rms         0.275
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1115
_refine_ls_number_reflns         20441
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.1246
_refine_ls_R_factor_gt           0.0664
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+1.1005P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1873
_refine_ls_wR_factor_ref         0.2215
_reflns_number_gt                11704
_reflns_number_total             20441
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202314g_si_002.cif
_cod_data_source_block           xb3742_0m
_cod_original_cell_volume        11495.9(18)
_cod_database_code               4328374