Noble Metals in Polyoxometalate Chemistry: Palladium-Containing Derivatives of the Monolacunary Keggin and Wells-Dawson Tungstophosphates
Natalya V. Izarova; Abhishek Banerjee; Ulrich Kortz; Inorganic Chemistry 50 (2011) 10379–10386; doi:10.1021/ic201451x

data_4326549
_publ_contact_author_address
;Jacobs University
School of Engineering and Science
P.O. Box 750 561
28725 Bremen
Germany
;
_publ_contact_author_email       u.kortz@jacobs-university.de
_publ_contact_author_fax         '+49-421-200 3229'
_publ_contact_author_name        'Ulrich Kortz'
_publ_contact_author_phone       '+49-421-200 3235'
_publ_section_title
;
 Noble Metals in Polyoxometalate Chemistry: Palladium-Containing
 Derivatives of the Monolacunary Keggin and Wells-Dawson Tungstophosphates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10379
_journal_page_last               10386
_journal_paper_doi               10.1021/ic201451x
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'H75 K9 O115 P2 Pd2 W22'
_chemical_formula_weight         6586.90
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'manual editing of SHELXL-97 file'
_cell_angle_alpha                90.00
_cell_angle_beta                 118.676(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.415(3)
_cell_length_b                   23.941(3)
_cell_length_c                   22.243(3)
_cell_measurement_reflns_used    2409
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.40
_cell_measurement_theta_min      3.66
_cell_volume                     10472(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, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.2720
_diffrn_reflns_av_sigmaI/netI    0.1191
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            187167
_diffrn_reflns_theta_full        22.46
_diffrn_reflns_theta_max         22.46
_diffrn_reflns_theta_min         4.08
_exptl_absorpt_coefficient_mu    24.940
_exptl_absorpt_correction_T_max  0.2285
_exptl_absorpt_correction_T_min  0.0220
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    4.178
_exptl_crystal_description       rode
_exptl_crystal_F_000             11656
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         4.863
_refine_diff_density_min         -2.013
_refine_diff_density_rms         0.491
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_matrix_type           full
_refine_ls_number_parameters     782
_refine_ls_number_reflns         13543
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1654
_refine_ls_R_factor_gt           0.0836
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0767P)^2^+1510.5417P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1978
_refine_ls_wR_factor_ref         0.2524
_reflns_number_gt                6908
_reflns_number_total             13543
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201451x_si_002_1.cif
_cod_data_source_block           K-1
_cod_database_code               4326549