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#$Date: 2016-03-23 20:37:02 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179415 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/12/4331297.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4331297
loop_
_publ_author_name
'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'
_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 H86 As8 Fe Na5 O55 Pd12'
_chemical_formula_weight         3590.13
_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                   15.8607(13)
_cell_length_b                   15.8607(13)
_cell_length_c                   24.9466(19)
_cell_measurement_reflns_used    2887
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.40
_cell_measurement_theta_min      2.99
_cell_volume                     6275.6(9)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω 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  0.0877
_diffrn_reflns_av_sigmaI/netI    0.0938
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            22602
_diffrn_reflns_theta_full        29.53
_diffrn_reflns_theta_max         29.53
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    3.969
_exptl_absorpt_correction_T_max  0.5893
_exptl_absorpt_correction_T_min  0.4312
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.900
_exptl_crystal_description       octahedron
_exptl_crystal_F_000             3422
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.735
_refine_diff_density_min         -1.554
_refine_diff_density_rms         0.340
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         4485
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0508
_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/[σ²(Fo²)+(0.0929P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1538
_refine_ls_wR_factor_ref         0.1807
_reflns_number_gt                2695
_reflns_number_total             4485
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301537n_si_001_03.cif
_cod_data_source_block           FePd12(PhAs)8_Na-1c
_cod_database_code               4331297
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Fe Fe 0.0000 0.0000 0.0000 0.0095(5) Uiso 1 8 d S
Pd1 Pd 0.07256(5) 0.19581(5) 0.0000 0.0156(2) Uani 1 2 d S
Pd2 Pd 0.13404(4) 0.06149(4) -0.09395(2) 0.01697(17) Uani 1 1 d .
As1 As 0.09253(5) 0.25239(5) -0.12105(3) 0.0210(2) Uani 1 1 d .
C1 C 0.1287(6) 0.3429(5) -0.1650(3) 0.0264(18) Uani 1 1 d .
C2 C 0.1836(6) 0.3273(7) -0.2074(4) 0.045(3) Uani 1 1 d .
H2A H 0.2044 0.2718 -0.2131 0.054 Uiso 1 1 calc R
C3 C 0.2084(7) 0.3925(8) -0.2415(4) 0.052(3) Uani 1 1 d .
H3A H 0.2453 0.3814 -0.2707 0.063 Uiso 1 1 calc R
C4 C 0.1806(8) 0.4684(8) -0.2331(5) 0.059(3) Uani 1 1 d .
H4A H 0.1975 0.5129 -0.2561 0.071 Uiso 1 1 calc R
C5 C 0.1283(11) 0.4844(8) -0.1921(6) 0.086(5) Uani 1 1 d .
H5A H 0.1087 0.5404 -0.1870 0.103 Uiso 1 1 calc R
C6 C 0.1017(8) 0.4212(7) -0.1564(5) 0.057(3) Uani 1 1 d .
H6A H 0.0655 0.4340 -0.1272 0.068 Uiso 1 1 calc R
O1 O 0.0396(3) 0.1072(3) -0.05168(18) 0.0160(11) Uani 1 1 d .
O2 O 0.1059(4) 0.2822(4) -0.0569(2) 0.0285(13) Uani 1 1 d .
O3 O 0.1534(4) 0.1698(3) -0.1369(2) 0.0306(14) Uani 1 1 d .
O4 O -0.0083(4) 0.2319(4) -0.1350(2) 0.0348(15) Uani 1 1 d .
O1W O 0.4258(5) 0.3990(5) -0.2693(3) 0.053(2) Uiso 1 1 d .
O2W O 0.3975(8) 0.3292(8) -0.1643(5) 0.035(3) Uiso 0.50 1 d P
O3W O 0.3251(16) 0.1771(16) -0.1205(9) 0.102(8) Uiso 0.50 1 d P
O4W O 0.3270(13) 0.4525(12) -0.1065(7) 0.079(6) Uiso 0.50 1 d P
O5W O -0.073(3) 0.405(3) -0.0642(16) 0.077(14) Uiso 0.25 1 d P
O6W O 0.1909(17) 0.4249(17) -0.0339(10) 0.039(6) Uiso 0.25 1 d P
O7W O -0.051(5) 0.389(4) -0.049(3) 0.038(15) Uiso 0.13 1 d P
O8W O 0.306(3) 0.268(3) 0.0000 0.070(14) Uiso 0.25 2 d SP
O9W O -0.017(3) 0.408(3) 0.0357(19) 0.025(11) Uiso 0.13 1 d P
O10W O 0.195(4) 0.367(4) 0.0000 0.083(16) Uiso 0.25 2 d SP
O11W O 0.3192(19) 0.215(2) -0.1019(11) 0.042(7) Uiso 0.25 1 d P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O1 Fe O1 180.0(2) 10 2
O1 Fe O1 70.36(12) 10 11
O1 Fe O1 109.64(12) 2 11
O1 Fe O1 109.64(12) 10 3
O1 Fe O1 70.36(12) 2 3
O1 Fe O1 180.0(3) 11 3
O1 Fe O1 109.1(2) 10 9
O1 Fe O1 70.9(2) 2 9
O1 Fe O1 70.36(12) 11 9
O1 Fe O1 109.64(12) 3 9
O1 Fe O1 70.36(12) 10 12
O1 Fe O1 109.64(12) 2 12
O1 Fe O1 109.1(2) 11 12
O1 Fe O1 70.9(2) 3 12
O1 Fe O1 70.36(12) 9 12
O1 Fe O1 109.64(12) 10 4
O1 Fe O1 70.36(12) 2 4
O1 Fe O1 70.9(2) 11 4
O1 Fe O1 109.1(2) 3 4
O1 Fe O1 109.64(12) 9 4
O1 Fe O1 180.0(3) 12 4
O1 Fe O1 70.9(2) 10 .
O1 Fe O1 109.1(2) 2 .
O1 Fe O1 109.64(12) 11 .
O1 Fe O1 70.36(12) 3 .
O1 Fe O1 180.0 9 .
O1 Fe O1 109.64(12) 12 .
O1 Fe O1 70.36(12) 4 .
O1 Pd1 O1 81.4(3) 10 .
O1 Pd1 O2 176.6(2) 10 .
O1 Pd1 O2 95.3(2) . .
O1 Pd1 O2 95.3(2) 10 10
O1 Pd1 O2 176.6(2) . 10
O2 Pd1 O2 88.0(3) . 10
O1 Pd2 O1 81.3(3) 4 .
O1 Pd2 O4 95.6(2) 4 4
O1 Pd2 O4 176.8(2) . 4
O1 Pd2 O3 175.9(2) 4 .
O1 Pd2 O3 94.9(2) . .
O4 Pd2 O3 88.3(2) 4 .
O4 As1 O3 110.5(3) . .
O4 As1 O2 112.0(3) . .
O3 As1 O2 111.8(3) . .
O4 As1 C1 108.4(3) . .
O3 As1 C1 106.3(3) . .
O2 As1 C1 107.4(3) . .
C6 C1 C2 119.3(8) . .
C6 C1 As1 121.1(7) . .
C2 C1 As1 119.6(7) . .
C1 C2 C3 120.5(10) . .
C4 C3 C2 119.4(11) . .
C3 C4 C5 120.7(11) . .
C6 C5 C4 122.2(12) . .
C1 C6 C5 117.9(11) . .
Pd2 O1 Pd2 114.4(2) 3 .
Pd2 O1 Pd1 114.3(2) 3 .
Pd2 O1 Pd1 114.1(2) . .
Pd2 O1 Fe 104.3(2) 3 .
Pd2 O1 Fe 104.1(2) . .
Pd1 O1 Fe 103.9(2) . .
As1 O2 Pd1 116.1(3) . .
As1 O3 Pd2 116.5(3) . .
As1 O4 Pd2 116.0(3) . 3
O11W O3W O5W 104(3) . 4
O9W O5W O7W 36(9) . .
O9W O5W O3W 139(2) . 3
O7W O5W O3W 122(10) . 3
O10W O6W O6W 47(2) . 10
O9W O7W O5W 135(10) . .
O5W O9W O7W 9(2) . .
O6W O10W O6W 86(4) 10 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe O1 2.224(5) 10
Fe O1 2.224(5) 2
Fe O1 2.224(5) 11
Fe O1 2.224(5) 3
Fe O1 2.224(5) 9
Fe O1 2.224(5) 12
Fe O1 2.224(5) 4
Fe O1 2.224(5) .
Pd1 O1 1.978(5) 10
Pd1 O1 1.978(5) .
Pd1 O2 2.042(5) .
Pd1 O2 2.042(5) 10
Pd2 O1 1.965(5) 4
Pd2 O1 1.970(5) .
Pd2 O4 2.043(6) 4
Pd2 O3 2.049(5) .
As1 O4 1.669(6) .
As1 O3 1.674(6) .
As1 O2 1.683(6) .
As1 C1 1.895(8) .
C1 C6 1.331(14) .
C1 C2 1.393(13) .
C2 C3 1.396(13) .
C3 C4 1.300(16) .
C4 C5 1.341(18) .
C5 C6 1.405(15) .
O1 Pd2 1.965(5) 3
O4 Pd2 2.043(6) 3
O3W O11W 0.76(3) .
O3W O5W 2.52(5) 4
O5W O9W 2.65(7) .
O5W O7W 0.58(8) .
O5W O3W 2.52(5) 3
O6W O10W 1.25(4) .
O6W O6W 1.69(5) 10
O7W O9W 2.21(8) .
O10W O6W 1.25(4) 10
