#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:37:02 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179415 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/12/4331296.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_4331296
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 H94 As8 Mn Na6 O59 Pd12'
_chemical_formula_weight         3684.27
_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                   16.109(3)
_cell_length_b                   16.109(3)
_cell_length_c                   24.770(6)
_cell_measurement_reflns_used    4416
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.68
_cell_measurement_theta_min      2.43
_cell_volume                     6428(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      173(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  0.0750
_diffrn_reflns_av_sigmaI/netI    0.0531
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            26771
_diffrn_reflns_theta_full        27.87
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_min         3.29
_exptl_absorpt_coefficient_mu    3.868
_exptl_absorpt_correction_T_max  0.2177
_exptl_absorpt_correction_T_min  0.0632
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.903
_exptl_crystal_description       octahedron
_exptl_crystal_F_000             3522
_exptl_crystal_size_max          0.82
_exptl_crystal_size_mid          0.62
_exptl_crystal_size_min          0.57
_refine_diff_density_max         1.657
_refine_diff_density_min         -0.807
_refine_diff_density_rms         0.237
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.254
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     133
_refine_ls_number_reflns         3929
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.254
_refine_ls_R_factor_all          0.0989
_refine_ls_R_factor_gt           0.0551
_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)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1750
_refine_ls_wR_factor_ref         0.2015
_reflns_number_gt                2538
_reflns_number_total             3929
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301537n_si_001_02.cif
_cod_data_source_block           MnPd12(PhAs)8_Na-1b
_cod_database_code               4331296
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
Mn1 Mn 0.0000 0.0000 0.0000 0.0234(6) Uani 1 8 d S
Pd1 Pd 0.07387(6) 0.19309(5) 0.0000 0.0313(3) Uani 1 2 d S
Pd2 Pd 0.13345(4) 0.05987(4) -0.09523(3) 0.0316(2) Uani 1 1 d .
As1 As 0.09387(6) 0.24749(5) -0.12167(4) 0.0361(3) Uani 1 1 d .
O1 O 0.0409(3) 0.1089(3) -0.0535(2) 0.0289(12) Uani 1 1 d .
O2 O 0.1533(5) 0.1667(4) -0.1375(3) 0.0553(19) Uani 1 1 d .
O3 O 0.1076(5) 0.2770(4) -0.0575(3) 0.0551(18) Uani 1 1 d .
O4 O -0.0057(4) 0.2295(4) -0.1361(3) 0.0554(19) Uani 1 1 d .
C1 C 0.1296(6) 0.3379(6) -0.1660(4) 0.046(2) Uani 1 1 d .
C2 C 0.1826(7) 0.3210(8) -0.2099(5) 0.071(4) Uani 1 1 d .
H2A H 0.2032 0.2667 -0.2166 0.085 Uiso 1 1 calc R
C3 C 0.2034(9) 0.3877(11) -0.2431(6) 0.092(5) Uani 1 1 d .
H3A H 0.2362 0.3782 -0.2743 0.110 Uiso 1 1 calc R
C6 C 0.1032(11) 0.4141(8) -0.1555(6) 0.092(5) Uani 1 1 d .
H6A H 0.0696 0.4256 -0.1249 0.111 Uiso 1 1 calc R
C4 C 0.1777(10) 0.4664(9) -0.2316(7) 0.090(5) Uani 1 1 d .
H4A H 0.1971 0.5117 -0.2527 0.108 Uiso 1 1 calc R
C5 C 0.1278(13) 0.4793(8) -0.1927(8) 0.110(6) Uani 1 1 d .
H5A H 0.1058 0.5335 -0.1879 0.131 Uiso 1 1 calc R
O1W O -0.068(2) 0.373(2) -0.0638(14) 0.073(9) Uiso 0.25 1 d P
O2W O 0.0755(8) 0.0990(8) -0.2357(5) 0.047(3) Uiso 0.50 1 d P
O3W O 0.3967(18) 0.3329(18) -0.1628(12) 0.059(7) Uiso 0.25 1 d P
O4W O 0.319(2) 0.189(2) -0.1197(16) 0.087(11) 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'
Mn Mn 0.3368 0.7283 '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 Mn1 O1 70.5(3) . 10
O1 Mn1 O1 109.5(3) . 2
O1 Mn1 O1 180.0(3) 10 2
O1 Mn1 O1 109.46(13) . 11
O1 Mn1 O1 70.54(13) 10 11
O1 Mn1 O1 109.46(13) 2 11
O1 Mn1 O1 70.54(13) . 3
O1 Mn1 O1 109.46(13) 10 3
O1 Mn1 O1 70.54(13) 2 3
O1 Mn1 O1 180.0(4) 11 3
O1 Mn1 O1 180.0 . 9
O1 Mn1 O1 109.5(3) 10 9
O1 Mn1 O1 70.5(3) 2 9
O1 Mn1 O1 70.54(13) 11 9
O1 Mn1 O1 109.46(13) 3 9
O1 Mn1 O1 109.46(13) . 12
O1 Mn1 O1 70.54(13) 10 12
O1 Mn1 O1 109.46(13) 2 12
O1 Mn1 O1 109.5(3) 11 12
O1 Mn1 O1 70.5(3) 3 12
O1 Mn1 O1 70.54(13) 9 12
O1 Mn1 O1 70.54(13) . 4
O1 Mn1 O1 109.46(13) 10 4
O1 Mn1 O1 70.54(13) 2 4
O1 Mn1 O1 70.5(3) 11 4
O1 Mn1 O1 109.5(3) 3 4
O1 Mn1 O1 109.46(13) 9 4
O1 Mn1 O1 180.0(4) 12 4
O1 Pd1 O1 84.5(3) . 10
O1 Pd1 O3 177.9(2) . 10
O1 Pd1 O3 93.4(2) 10 10
O1 Pd1 O3 93.4(2) . .
O1 Pd1 O3 177.9(2) 10 .
O3 Pd1 O3 88.7(4) 10 .
O1 Pd2 O1 84.4(3) 4 .
O1 Pd2 O4 93.5(2) 4 4
O1 Pd2 O4 177.7(2) . 4
O1 Pd2 O2 177.2(3) 4 .
O1 Pd2 O2 92.9(3) . .
O4 Pd2 O2 89.3(3) 4 .
O2 As1 O4 111.6(4) . .
O2 As1 O3 111.7(4) . .
O4 As1 O3 112.4(4) . .
O2 As1 C1 106.7(4) . .
O4 As1 C1 107.4(4) . .
O3 As1 C1 106.8(4) . .
Pd2 O1 Pd1 116.0(2) 3 .
Pd2 O1 Pd2 115.3(3) 3 .
Pd1 O1 Pd2 115.1(2) . .
Pd2 O1 Mn1 102.7(2) 3 .
Pd1 O1 Mn1 102.5(2) . .
Pd2 O1 Mn1 102.3(2) . .
As1 O2 Pd2 116.7(4) . .
As1 O3 Pd1 116.1(4) . .
As1 O4 Pd2 115.8(3) . 3
C6 C1 C2 121.7(10) . .
C6 C1 As1 119.7(8) . .
C2 C1 As1 118.6(8) . .
C3 C2 C1 116.9(12) . .
C4 C3 C2 121.4(13) . .
C1 C6 C5 117.2(13) . .
C5 C4 C3 120.1(12) . .
C4 C5 C6 122.3(14) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O1 2.294(5) .
Mn1 O1 2.294(5) 10
Mn1 O1 2.294(5) 2
Mn1 O1 2.294(5) 11
Mn1 O1 2.294(5) 3
Mn1 O1 2.294(5) 9
Mn1 O1 2.294(5) 12
Mn1 O1 2.294(5) 4
Pd1 O1 1.969(5) .
Pd1 O1 1.969(5) 10
Pd1 O3 2.038(6) 10
Pd1 O3 2.038(6) .
Pd2 O1 1.966(5) 4
Pd2 O1 1.979(5) .
Pd2 O4 2.045(6) 4
Pd2 O2 2.039(6) .
As1 O2 1.663(7) .
As1 O4 1.669(7) .
As1 O3 1.674(7) .
As1 C1 1.914(8) .
O1 Pd2 1.966(5) 3
O4 Pd2 2.045(6) 3
C1 C6 1.325(16) .
C1 C2 1.407(15) .
C2 C3 1.394(16) .
C3 C4 1.36(2) .
C6 C5 1.454(18) .
C4 C5 1.27(2) .
