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_4326550
_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            'H38 K12 N2 O103 P2 Pd2 W22'
_chemical_formula_weight         6502.96
_chemical_name_systematic
; 
 ? 
;
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_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_angle_gamma                108.256(3)
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_cell_length_b                   12.1709(7)
_cell_length_c                   18.5502(11)
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_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.30
_cell_measurement_theta_min      2.36
_cell_volume                     2343.7(3)
_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 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0819
_diffrn_reflns_av_sigmaI/netI    0.0472
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            108499
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         3.43
_exptl_absorpt_coefficient_mu    27.937
_exptl_absorpt_correction_T_max  0.1574
_exptl_absorpt_correction_T_min  0.0191
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    4.607
_exptl_crystal_description       rode
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_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.11
_refine_diff_density_max         5.382
_refine_diff_density_min         -2.908
_refine_diff_density_rms         0.564
_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         11461
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0853
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_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^)+(0.0887P)^2^+147.5873P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_reflns_number_gt                8990
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_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201451x_si_002_2.cif
_cod_data_source_block           K-1N
_cod_original_cell_volume        2343.7(2)
_cod_database_code               4326550