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_4329569
_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         'K12 O86.50 H35 P2 Pd W19'
_chemical_formula_sum            'H35 K12 O86.5 P2 Pd W19'
_chemical_formula_weight         5549.76
_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   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.382(3)
_cell_angle_beta                 103.293(3)
_cell_angle_gamma                108.724(3)
_cell_formula_units_Z            2
_cell_length_a                   11.984(2)
_cell_length_b                   17.335(4)
_cell_length_c                   23.029(5)
_cell_measurement_reflns_used    9983
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.54
_cell_measurement_theta_min      2.22
_cell_volume                     4392.7(16)
_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 0.996
_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  0.0720
_diffrn_reflns_av_sigmaI/netI    0.0730
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            76467
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    25.679
_exptl_absorpt_correction_T_max  0.0931
_exptl_absorpt_correction_T_min  0.0300
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    4.169
_exptl_crystal_description       plate
_exptl_crystal_F_000             4804
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_refine_diff_density_max         16.846
_refine_diff_density_min         -3.783
_refine_diff_density_rms         0.544
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     661
_refine_ls_number_reflns         21689
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0547
_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^)+(0.1041P)^2^+58.1965P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1595
_refine_ls_wR_factor_ref         0.1754
_reflns_number_gt                16435
_reflns_number_total             21689
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2008914_si_001_2.cif
_cod_data_source_block           nsa_75_01
_cod_original_cell_volume        4392.7(15)
_cod_original_formula_sum        'K12 O86.50 H35 P2 Pd W19'
_cod_database_code               4329569