Revisiting the Polyoxometalate-Based Late-Transition-Metal-Oxo Complexes: The "Oxo Wall" Stands
Kevin P. O'Halloran; Chongchao Zhao; Nicole S. Ando; Arthur J. Schultz; Thomas F. Koetzle; Paula M. B. Piccoli; Britt Hedman; Keith O. Hodgson; Elena Bobyr; Martin L. Kirk; Sushilla Knottenbelt; Ezra C. Depperman; Benjamin Stein; Travis M. Anderson; Rui Cao; Yurii V. Geletii; Kenneth I. Hardcastle; Djamaladdin G. Musaev; Wade A. Neiwert; Xikui Fang; Keiji Morokuma; Shaoxiong Wu; Paul Kögerler; Craig L. Hill; Inorganic Chemistry 51 (2012) 7025–7031; doi:10.1021/ic2008914

data_4329568
_publ_section_title
;
 Revisiting the Polyoxometalate-Based Late-Transition-Metal-Oxo Complexes:
 The "Oxo Wall" Stands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7025
_journal_page_last               7031
_journal_paper_doi               10.1021/ic2008914
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'K14 O84 H30 P2 W19'
_chemical_formula_sum            'H30 K14 O84 P2 W19'
_chemical_formula_weight         5476.47
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           70
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-F 2uv 2vw'
_symmetry_space_group_name_H-M   'F d d d :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   28.645(9)
_cell_length_b                   31.827(11)
_cell_length_c                   38.707(13)
_cell_measurement_reflns_used    9694
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.04
_cell_measurement_theta_min      2.18
_cell_volume                     35289(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \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  0.0933
_diffrn_reflns_av_sigmaI/netI    0.0399
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            158284
_diffrn_reflns_theta_full        29.13
_diffrn_reflns_theta_max         29.13
_diffrn_reflns_theta_min         1.09
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    25.274
_exptl_absorpt_correction_T_max  0.0810
_exptl_absorpt_correction_T_min  0.0512
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.983
_exptl_crystal_description       block
_exptl_crystal_F_000             36768
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_refine_diff_density_max         7.265
_refine_diff_density_min         -5.263
_refine_diff_density_rms         0.565
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         11898
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0497
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1629P)^2^+48.3672P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1844
_refine_ls_wR_factor_ref         0.2129
_reflns_number_gt                9700
_reflns_number_total             11898
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2008914_si_001_1.cif
_cod_data_source_block           kpo_3_179bs
_cod_original_cell_volume        35290(20)
_cod_original_sg_symbol_H-M      'F d d d'
_cod_original_formula_sum        'K14 O84 H30 P2 W19'
_cod_database_code               4329568