Polyoxopalladates Encapsulating 8-Coordinated Metal Ions, [MO8PdII12L8]n- (M = Sc3+, Mn2+, Fe3+, Co2+, Ni2+, Cu2+, Zn2+, Lu3+; L = PhAsO32-, PhPO32-, SeO32-)
Maria Barsukova-Stuckart; Natalya V. Izarova; Ryan A. Barrett; Zhenxing Wang; Johan van Tol; Harold W. Kroto; Naresh S. Dalal; Pablo Jiménez-Lozano; Jorge J. Carbó; Josep M. Poblet; Marc S. von Gernler; Thomas Drewello; Pedro de Oliveira; Bineta Keita; Ulrich Kortz; Inorganic Chemistry 51 (2012) 13214–13228; doi:10.1021/ic301537n

data_4331300
_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
;
 Polyoxopalladates Encapsulating 8-Coordinated Metal Ions, [MO8PdII12L8]n-
 (M = Sc3+, Mn2+, Fe3+, Co2+, Ni2+, Cu2+, Zn2+, Lu3+; L = PhAsO32-,
 PhPO32-, SeO32-)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              13214
_journal_page_last               13228
_journal_paper_doi               10.1021/ic301537n
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C48 H78 As8 Cu Na6 O51 Pd12'
_chemical_formula_weight         3548.74
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           87
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_atom_sites_solution_hydrogens   geom
_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            2
_cell_length_a                   15.8988(5)
_cell_length_b                   15.8988(5)
_cell_length_c                   25.1299(11)
_cell_measurement_reflns_used    9187
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      37.97
_cell_measurement_theta_min      3.72
_cell_volume                     6352.1(4)
_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      173(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.1012
_diffrn_reflns_av_sigmaI/netI    0.0463
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            31708
_diffrn_reflns_theta_full        33.15
_diffrn_reflns_theta_max         33.15
_diffrn_reflns_theta_min         3.62
_exptl_absorpt_coefficient_mu    3.974
_exptl_absorpt_correction_T_max  0.3628
_exptl_absorpt_correction_T_min  0.3368
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.855
_exptl_crystal_description       block
_exptl_crystal_F_000             3370
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.32
_refine_diff_density_max         4.610
_refine_diff_density_min         -1.777
_refine_diff_density_rms         0.452
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         6125
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0549
_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^)+(0.1396P)^2^+25.7083P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1764
_refine_ls_wR_factor_ref         0.2070
_reflns_number_gt                5224
_reflns_number_total             6125
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301537n_si_001_06.cif
_cod_data_source_block           CuPd12(PhAs)8_Na-1f
_cod_database_code               4331300