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#$Date: 2016-03-23 20:38:18 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179416 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/13/4331302.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_4331302
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 H110 Cu Na6 O67 P8 Pd12'
_chemical_formula_weight         3485.40
_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                   15.928(3)
_cell_length_b                   15.928(3)
_cell_length_c                   24.313(5)
_cell_measurement_reflns_used    3576
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.98
_cell_measurement_theta_min      2.47
_cell_volume                     6168(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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.2369
_diffrn_reflns_av_sigmaI/netI    0.1096
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            20925
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         3.35
_exptl_absorpt_coefficient_mu    2.084
_exptl_absorpt_correction_T_max  0.5606
_exptl_absorpt_correction_T_min  0.2007
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.877
_exptl_crystal_description       octahedron
_exptl_crystal_F_000             3402
_exptl_crystal_size_max          0.69
_exptl_crystal_size_mid          0.64
_exptl_crystal_size_min          0.31
_refine_diff_density_max         1.873
_refine_diff_density_min         -1.448
_refine_diff_density_rms         0.250
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         2693
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1184
_refine_ls_R_factor_gt           0.0774
_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)+(0.1504P)²+29.7305P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2257
_refine_ls_wR_factor_ref         0.2624
_reflns_number_gt                1674
_reflns_number_total             2693
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301537n_si_001_08.cif
_cod_data_source_block           CuPd12(PhP)8_Na-2a
_cod_database_code               4331302
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
Cu1 Cu 0.5000 0.5000 0.5000 0.0201(9) Uani 1 8 d S
Pd2 Pd 0.57432(8) 0.30728(8) 0.5000 0.0294(5) Uani 1 2 d S
Pd3 Pd 0.44059(5) 0.36600(6) 0.59607(4) 0.0305(4) Uani 1 1 d .
P1 P 0.59434(19) 0.25381(19) 0.62125(14) 0.0332(8) Uani 1 1 d .
O1 O 0.5410(5) 0.3927(5) 0.5533(3) 0.034(2) Uani 1 1 d .
O3P1 O 0.6070(5) 0.2260(5) 0.5615(3) 0.043(2) Uani 1 1 d .
O2P1 O 0.6507(6) 0.3279(5) 0.6369(4) 0.047(2) Uani 1 1 d .
O1P1 O 0.5017(5) 0.2700(6) 0.6351(4) 0.046(2) Uani 1 1 d .
C1 C 0.6273(7) 0.1669(8) 0.6634(5) 0.036(3) Uiso 1 1 d .
C2 C 0.6844(9) 0.1788(9) 0.7075(6) 0.055(4) Uiso 1 1 d .
H2A H 0.7091 0.2322 0.7138 0.066 Uiso 1 1 calc R
C6 C 0.5960(10) 0.0898(10) 0.6549(8) 0.070(5) Uiso 1 1 d .
H6A H 0.5559 0.0814 0.6265 0.084 Uiso 1 1 calc R
C5 C 0.6218(11) 0.0207(12) 0.6876(8) 0.079(5) Uiso 1 1 d .
H5A H 0.6027 -0.0344 0.6795 0.095 Uiso 1 1 calc R
C4 C 0.6740(10) 0.0346(11) 0.7307(7) 0.068(4) Uiso 1 1 d .
H4A H 0.6901 -0.0106 0.7538 0.081 Uiso 1 1 calc R
C3 C 0.7033(11) 0.1126(11) 0.7407(8) 0.083(5) Uiso 1 1 d .
H3A H 0.7381 0.1216 0.7719 0.099 Uiso 1 1 calc R
Na1 Na 0.6868(18) 0.1353(18) 0.5000 0.065(8) Uiso 0.30 2 d SP
O1W O 0.5671(10) 0.3949(9) 0.7373(6) 0.052(4) Uiso 0.60 1 d P
O2W O 0.8339(17) -0.0949(17) 0.6509(12) 0.074(8) Uiso 0.40 1 d P
O3W O 0.823(3) 0.297(2) 0.6068(16) 0.057(10) Uiso 0.25 1 d P
O4W O 0.431(2) 0.126(2) 0.5575(16) 0.051(9) Uiso 0.25 1 d P
O5W O 0.799(3) 0.243(3) 0.5000 0.048(13) Uiso 0.25 2 d SP
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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 Cu1 O1 109.53(19) . 11_566
O1 Cu1 O1 70.47(19) . 3_655
O1 Cu1 O1 180.000(1) 11_566 3_655
O1 Cu1 O1 109.3(4) . 2_665
O1 Cu1 O1 109.53(19) 11_566 2_665
O1 Cu1 O1 70.47(19) 3_655 2_665
O1 Cu1 O1 70.7(4) . 10_556
O1 Cu1 O1 70.47(19) 11_566 10_556
O1 Cu1 O1 109.53(19) 3_655 10_556
O1 Cu1 O1 180.0(3) 2_665 10_556
O1 Cu1 O1 109.53(19) . 12_656
O1 Cu1 O1 109.3(4) 11_566 12_656
O1 Cu1 O1 70.7(4) 3_655 12_656
O1 Cu1 O1 109.53(19) 2_665 12_656
O1 Cu1 O1 70.47(19) 10_556 12_656
O1 Cu1 O1 70.47(19) . 4_565
O1 Cu1 O1 70.7(4) 11_566 4_565
O1 Cu1 O1 109.3(4) 3_655 4_565
O1 Cu1 O1 70.47(19) 2_665 4_565
O1 Cu1 O1 109.53(19) 10_556 4_565
O1 Cu1 O1 180.000(1) 12_656 4_565
O1 Cu1 O1 179.999(1) . 9_666
O1 Cu1 O1 70.47(19) 11_566 9_666
O1 Cu1 O1 109.53(19) 3_655 9_666
O1 Cu1 O1 70.7(4) 2_665 9_666
O1 Cu1 O1 109.3(4) 10_556 9_666
O1 Cu1 O1 70.47(19) 12_656 9_666
O1 Cu1 O1 109.53(19) 4_565 9_666
O1 Pd2 O1 83.2(5) . 10_556
O1 Pd2 O3P1 91.4(3) . .
O1 Pd2 O3P1 174.6(3) 10_556 .
O1 Pd2 O3P1 174.6(3) . 10_556
O1 Pd2 O3P1 91.4(3) 10_556 10_556
O3P1 Pd2 O3P1 94.0(5) . 10_556
O1 Pd2 Na1 137.1(3) . .
O1 Pd2 Na1 137.0(3) 10_556 .
O3P1 Pd2 Na1 48.0(3) . .
O3P1 Pd2 Na1 48.0(3) 10_556 .
O1 Pd3 O1 82.6(5) . 4_565
O1 Pd3 O1P1 91.2(3) . .
O1 Pd3 O1P1 173.7(3) 4_565 .
O1 Pd3 O2P1 173.4(3) . 4_565
O1 Pd3 O2P1 90.8(3) 4_565 4_565
O1P1 Pd3 O2P1 95.4(3) . 4_565
O2P1 P1 O3P1 112.4(5) . .
O2P1 P1 O1P1 112.3(5) . .
O3P1 P1 O1P1 112.6(5) . .
O2P1 P1 C1 106.3(5) . .
O3P1 P1 C1 106.2(5) . .
O1P1 P1 C1 106.5(5) . .
Pd3 O1 Pd2 115.1(4) . .
Pd3 O1 Pd3 114.9(4) . 3_655
Pd2 O1 Pd3 114.6(4) . 3_655
Pd3 O1 Cu1 103.6(3) . .
Pd2 O1 Cu1 103.1(3) . .
Pd3 O1 Cu1 103.3(3) 3_655 .
P1 O3P1 Pd2 118.5(5) . .
P1 O3P1 Na1 145.3(6) . .
Pd2 O3P1 Na1 93.4(5) . .
P1 O2P1 Pd3 118.4(5) . 3_655
P1 O1P1 Pd3 118.7(5) . .
C6 C1 C2 118.5(13) . .
C6 C1 P1 120.5(11) . .
C2 C1 P1 120.9(10) . .
C3 C2 C1 119.1(15) . .
C1 C6 C5 121.1(16) . .
C4 C5 C6 118.9(17) . .
C3 C4 C5 120.2(18) . .
C4 C3 C2 122.0(18) . .
O3P1 Na1 O3P1 75.7(9) . 10_556
O3P1 Na1 O5W 87.8(13) . .
O3P1 Na1 O5W 87.8(13) 10_556 .
O3P1 Na1 Pd2 38.6(5) . .
O3P1 Na1 Pd2 38.6(5) 10_556 .
O5W Na1 Pd2 79.1(14) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O1 2.242(8) .
Cu1 O1 2.242(8) 11_566
Cu1 O1 2.242(8) 3_655
Cu1 O1 2.242(8) 2_665
Cu1 O1 2.242(8) 10_556
Cu1 O1 2.242(8) 12_656
Cu1 O1 2.242(8) 4_565
Cu1 O1 2.242(8) 9_666
Pd2 O1 1.953(7) .
Pd2 O1 1.953(7) 10_556
Pd2 O3P1 2.045(8) .
Pd2 O3P1 2.045(8) 10_556
Pd2 Na1 3.27(3) .
Pd3 O1 1.954(7) .
Pd3 O1 1.964(7) 4_565
Pd3 O1P1 2.047(8) .
Pd3 O2P1 2.068(8) 4_565
P1 O2P1 1.530(9) .
P1 O3P1 1.531(9) .
P1 O1P1 1.536(9) .
P1 C1 1.801(13) .
O1 Pd3 1.964(7) 3_655
O3P1 Na1 2.44(2) .
O2P1 Pd3 2.068(8) 3_655
C1 C6 1.341(19) .
C1 C2 1.419(18) .
C2 C3 1.36(2) .
C6 C5 1.42(2) .
C5 C4 1.36(2) .
C4 C3 1.35(2) .
Na1 O3P1 2.44(2) 10_556
Na1 O5W 2.48(6) .
