#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/38/4103878.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_4103878
loop_
_publ_author_name
'Chun-Yan Sun'
'Shu-Xia Liu'
'Da-Dong Liang'
'Kui-Zhan Shao'
'Yuan-Hang Ren'
'Zhong-Min Su'
_publ_section_title
;
 Highly Stable Crystalline Catalysts Based on a Microporous Metal-Organic
 Framework and Polyoxometalates
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1883
_journal_page_last               1888
_journal_paper_doi               10.1021/ja807357r
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C148 H48 Cu24 N2 O221.84 P2 W24'
_chemical_formula_weight         11402.62
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           225
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-F 4 2 3'
_symmetry_space_group_name_H-M   'F m -3 m'
_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                   26.3141(12)
_cell_length_b                   26.3141(12)
_cell_length_c                   26.3141(12)
_cell_measurement_reflns_used    6667
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.17
_cell_measurement_theta_min      2.19
_cell_volume                     18220.7(14)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0433
_diffrn_reflns_av_sigmaI/netI    0.0137
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            28325
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.34
_exptl_absorpt_coefficient_mu    9.01
_exptl_absorpt_correction_T_max  0.407
_exptl_absorpt_correction_T_min  0.351
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR by T.Higashi    8 March, 1995'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    2.078
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             20484
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.551
_refine_diff_density_min         -1.903
_refine_diff_density_rms         0.582
_refine_ls_extinction_coef       0.000164(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.275
_refine_ls_matrix_type           full
_refine_ls_number_parameters     63
_refine_ls_number_reflns         1189
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.275
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0411
_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)+(0.0795P)²+173.3779P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1214
_refine_ls_wR_factor_ref         0.1393
_reflns_number_gt                1057
_reflns_number_total             1189
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja807357r_si_004.cif
_cod_data_source_block           3
_cod_original_formula_sum        'C148 H48 Cu24 N2 O221.84 P2 W24 '
_cod_database_code               4103878
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, -z'
'-y, -x, -z'
'y, -x, z'
'-y, x, z'
'x, z, -y'
'-x, z, y'
'-x, -z, -y'
'x, -z, y'
'z, y, -x'
'z, -y, x'
'-z, y, x'
'-z, -y, -x'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y+1/2, -z+1/2'
'z, x+1/2, y+1/2'
'z, -x+1/2, -y+1/2'
'-z, -x+1/2, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z+1/2, x+1/2'
'-y, z+1/2, -x+1/2'
'y, -z+1/2, -x+1/2'
'-y, -z+1/2, x+1/2'
'y, x+1/2, -z+1/2'
'-y, -x+1/2, -z+1/2'
'y, -x+1/2, z+1/2'
'-y, x+1/2, z+1/2'
'x, z+1/2, -y+1/2'
'-x, z+1/2, y+1/2'
'-x, -z+1/2, -y+1/2'
'x, -z+1/2, y+1/2'
'z, y+1/2, -x+1/2'
'z, -y+1/2, x+1/2'
'-z, y+1/2, x+1/2'
'-z, -y+1/2, -x+1/2'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'-x+1/2, y, -z+1/2'
'x+1/2, -y, -z+1/2'
'z+1/2, x, y+1/2'
'z+1/2, -x, -y+1/2'
'-z+1/2, -x, y+1/2'
'-z+1/2, x, -y+1/2'
'y+1/2, z, x+1/2'
'-y+1/2, z, -x+1/2'
'y+1/2, -z, -x+1/2'
'-y+1/2, -z, x+1/2'
'y+1/2, x, -z+1/2'
'-y+1/2, -x, -z+1/2'
'y+1/2, -x, z+1/2'
'-y+1/2, x, z+1/2'
'x+1/2, z, -y+1/2'
'-x+1/2, z, y+1/2'
'-x+1/2, -z, -y+1/2'
'x+1/2, -z, y+1/2'
'z+1/2, y, -x+1/2'
'z+1/2, -y, x+1/2'
'-z+1/2, y, x+1/2'
'-z+1/2, -y, -x+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
'z+1/2, x+1/2, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x+1/2, y'
'-z+1/2, x+1/2, -y'
'y+1/2, z+1/2, x'
'-y+1/2, z+1/2, -x'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z+1/2, x'
'y+1/2, x+1/2, -z'
'-y+1/2, -x+1/2, -z'
'y+1/2, -x+1/2, z'
'-y+1/2, x+1/2, z'
'x+1/2, z+1/2, -y'
'-x+1/2, z+1/2, y'
'-x+1/2, -z+1/2, -y'
'x+1/2, -z+1/2, y'
'z+1/2, y+1/2, -x'
'z+1/2, -y+1/2, x'
'-z+1/2, y+1/2, x'
'-z+1/2, -y+1/2, -x'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-y, -x, z'
'y, x, z'
'-y, x, -z'
'y, -x, -z'
'-x, -z, y'
'x, -z, -y'
'x, z, y'
'-x, z, -y'
'-z, -y, x'
'-z, y, -x'
'z, -y, -x'
'z, y, x'
'-x, -y+1/2, -z+1/2'
'x, y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'
'-x, y+1/2, z+1/2'
'-z, -x+1/2, -y+1/2'
'-z, x+1/2, y+1/2'
'z, x+1/2, -y+1/2'
'z, -x+1/2, y+1/2'
'-y, -z+1/2, -x+1/2'
'y, -z+1/2, x+1/2'
'-y, z+1/2, x+1/2'
'y, z+1/2, -x+1/2'
'-y, -x+1/2, z+1/2'
'y, x+1/2, z+1/2'
'-y, x+1/2, -z+1/2'
'y, -x+1/2, -z+1/2'
'-x, -z+1/2, y+1/2'
'x, -z+1/2, -y+1/2'
'x, z+1/2, y+1/2'
'-x, z+1/2, -y+1/2'
'-z, -y+1/2, x+1/2'
'-z, y+1/2, -x+1/2'
'z, -y+1/2, -x+1/2'
'z, y+1/2, x+1/2'
'-x+1/2, -y, -z+1/2'
'x+1/2, y, -z+1/2'
'x+1/2, -y, z+1/2'
'-x+1/2, y, z+1/2'
'-z+1/2, -x, -y+1/2'
'-z+1/2, x, y+1/2'
'z+1/2, x, -y+1/2'
'z+1/2, -x, y+1/2'
'-y+1/2, -z, -x+1/2'
'y+1/2, -z, x+1/2'
'-y+1/2, z, x+1/2'
'y+1/2, z, -x+1/2'
'-y+1/2, -x, z+1/2'
'y+1/2, x, z+1/2'
'-y+1/2, x, -z+1/2'
'y+1/2, -x, -z+1/2'
'-x+1/2, -z, y+1/2'
'x+1/2, -z, -y+1/2'
'x+1/2, z, y+1/2'
'-x+1/2, z, -y+1/2'
'-z+1/2, -y, x+1/2'
'-z+1/2, y, -x+1/2'
'z+1/2, -y, -x+1/2'
'z+1/2, y, x+1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'-z+1/2, -x+1/2, -y'
'-z+1/2, x+1/2, y'
'z+1/2, x+1/2, -y'
'z+1/2, -x+1/2, y'
'-y+1/2, -z+1/2, -x'
'y+1/2, -z+1/2, x'
'-y+1/2, z+1/2, x'
'y+1/2, z+1/2, -x'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'
'-y+1/2, x+1/2, -z'
'y+1/2, -x+1/2, -z'
'-x+1/2, -z+1/2, y'
'x+1/2, -z+1/2, -y'
'x+1/2, z+1/2, y'
'-x+1/2, z+1/2, -y'
'-z+1/2, -y+1/2, x'
'-z+1/2, y+1/2, -x'
'z+1/2, -y+1/2, -x'
'z+1/2, y+1/2, x'
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
C3 C 0.0685(3) 0.20282(18) 0.20282(18) 0.0259(14) Uani 1 2 d S
Cu1 Cu 0.0000 0.21472(3) 0.28528(3) 0.0210(3) Uani 1 4 d S
P1 P 0.0000 0.0000 0.0000 0.0186(16) Uani 1 48 d S
O1 O 0.0493(3) 0.0493(3) 0.1200(3) 0.072(3) Uani 1 2 d S
O2 O 0.05267(15) 0.18302(15) 0.24353(14) 0.0327(9) Uani 1 1 d .
O3 O 0.0000 0.1408(2) 0.1408(2) 0.056(3) Uani 1 4 d S
O4 O 0.0000 0.1549(3) 0.3451(3) 0.081(4) Uani 1 4 d S
W2 W 0.0000 0.095615(12) 0.095615(12) 0.0338(3) Uani 1 4 d S
C5 C 0.1336(2) 0.1987(3) 0.1336(2) 0.0287(15) Uani 1 2 d S
H5 H 0.1194 0.2278 0.1194 0.034 Uiso 1 2 calc SR
C4 C 0.1117(3) 0.1768(2) 0.1768(2) 0.0292(15) Uani 1 2 d S
O5 O 0.0341(4) 0.0341(4) 0.0341(4) 0.025(3) Uani 0.50 6 d SP
N1 N 0.2500 0.2500 0.2500 0.061(17) Uiso 0.50 24 d SP
C12 C 0.284(2) 0.216(2) 0.216(2) 0.07(2) Uiso 0.25 6 d SP
O6 O 0.0000 0.0000 0.2683(18) 0.088(12) Uiso 0.50 8 d SP
O8 O 0.0760(13) 0.0000 0.2501(13) 0.087(9) Uiso 0.33 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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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'
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
O2 C3 O2 126.4(7) 115 .
O2 C3 C4 116.8(3) 115 .
O2 C3 C4 116.8(3) . .
O2 Cu1 O2 88.7(2) 100 43
O2 Cu1 O2 169.0(2) 100 138
O2 Cu1 O2 90.3(2) 43 138
O2 Cu1 O2 90.3(2) 100 .
O2 Cu1 O2 169.0(2) 43 .
O2 Cu1 O2 88.7(2) 138 .
O2 Cu1 O4 95.50(12) 100 .
O2 Cu1 O4 95.50(12) 43 .
O2 Cu1 O4 95.50(12) 138 .
O2 Cu1 O4 95.50(12) . .
O2 Cu1 Cu1 84.50(12) 100 121
O2 Cu1 Cu1 84.50(12) 43 121
O2 Cu1 Cu1 84.50(12) 138 121
O2 Cu1 Cu1 84.50(12) . 121
O4 Cu1 Cu1 180.0(3) . 121
O5 P1 O5 109.471(1) 97 100
O5 P1 O5 70.529(1) 97 3
O5 P1 O5 70.5 100 3
O5 P1 O5 70.5 97 2
O5 P1 O5 70.529(1) 100 2
O5 P1 O5 109.5 3 2
O5 P1 O5 180.0(17) 97 .
O5 P1 O5 70.5 100 .
O5 P1 O5 109.5 3 .
O5 P1 O5 109.471(1) 2 .
O5 P1 O5 109.5 97 98
O5 P1 O5 109.471(1) 100 98
O5 P1 O5 70.529(1) 3 98
O5 P1 O5 180.0(17) 2 98
O5 P1 O5 70.529(1) . 98
O5 P1 O5 109.471(1) 97 99
O5 P1 O5 109.5 100 99
O5 P1 O5 180.0(17) 3 99
O5 P1 O5 70.529(1) 2 99
O5 P1 O5 70.529(1) . 99
O5 P1 O5 109.5 98 99
O5 P1 O5 70.529(1) 97 4
O5 P1 O5 180.0(17) 100 4
O5 P1 O5 109.5 3 4
O5 P1 O5 109.5 2 4
O5 P1 O5 109.471(1) . 4
O5 P1 O5 70.5 98 4
O5 P1 O5 70.5 99 4
W2 O1 W2 140.2(5) . 5
C3 O2 Cu1 122.3(4) . .
O3 W2 O1 102.4(3) . .
O3 W2 O1 102.4(3) . 107
O1 W2 O1 155.1(6) . 107
O3 W2 O1 102.4(3) . 100
O1 W2 O1 86.7(5) . 100
O1 W2 O1 88.0(4) 107 100
O3 W2 O1 102.4(3) . 9
O1 W2 O1 88.0(4) . 9
O1 W2 O1 86.7(5) 107 9
O1 W2 O1 155.1(6) 100 9
O3 W2 O5 158.6(3) . 100
O1 W2 O5 92.8(4) . 100
O1 W2 O5 63.2(3) 107 100
O1 W2 O5 63.2(3) 100 100
O1 W2 O5 92.8(4) 9 100
O3 W2 O5 158.6(3) . .
O1 W2 O5 63.2(3) . .
O1 W2 O5 92.8(4) 107 .
O1 W2 O5 92.8(4) 100 .
O1 W2 O5 63.2(3) 9 .
O5 W2 O5 42.8(6) 100 .
C4 C5 C4 120.1(8) 9 .
C5 C4 C5 119.9(8) 5 .
C5 C4 C3 119.9(4) 5 .
C5 C4 C3 119.9(4) . .
P1 O5 O5 54.736(2) . 100
P1 O5 O5 54.736(2) . 99
O5 O5 O5 90.000(1) 100 99
P1 O5 O5 54.736(2) . 98
O5 O5 O5 90.000(1) 100 98
O5 O5 O5 90.000(1) 99 98
P1 O5 W2 123.4(3) . .
O5 O5 W2 68.6(3) 100 .
O5 O5 W2 131.18(11) 99 .
O5 O5 W2 131.18(11) 98 .
P1 O5 W2 123.4(3) . 9
O5 O5 W2 131.18(11) 100 9
O5 O5 W2 131.18(11) 99 9
O5 O5 W2 68.6(3) 98 9
W2 O5 W2 92.7(4) . 9
P1 O5 W2 123.4(3) . 5
O5 O5 W2 131.18(11) 100 5
O5 O5 W2 68.6(3) 99 5
O5 O5 W2 131.18(11) 98 5
W2 O5 W2 92.7(4) . 5
W2 O5 W2 92.7(4) 9 5
C12 N1 C12 109.471(4) 28 51
C12 N1 C12 109.471(13) 28 74
C12 N1 C12 109.471(9) 51 74
C12 N1 C12 109.47(3) 28 .
C12 N1 C12 109.471(7) 51 .
C12 N1 C12 109.471(5) 74 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C3 O2 1.262(5) 115
C3 O2 1.262(5) .
C3 C4 1.492(10) .
Cu1 O2 1.955(4) 100
Cu1 O2 1.955(4) 43
Cu1 O2 1.955(4) 138
Cu1 O2 1.955(4) .
Cu1 O4 2.228(11) .
Cu1 Cu1 2.626(2) 121
P1 O5 1.553(16) 97
P1 O5 1.553(16) 100
P1 O5 1.553(16) 3
P1 O5 1.553(16) 2
P1 O5 1.553(16) .
P1 O5 1.553(16) 98
P1 O5 1.553(16) 99
P1 O5 1.553(16) 4
O1 W2 1.892(3) .
O1 W2 1.892(3) 5
O3 W2 1.681(9) .
W2 O1 1.892(3) 107
W2 O1 1.892(3) 100
W2 O1 1.892(3) 9
W2 O5 2.460(9) 100
W2 O5 2.460(9) .
C5 C4 1.400(5) 9
C5 C4 1.400(5) .
C4 C5 1.400(5) 5
O5 O5 1.793(19) 100
O5 O5 1.793(19) 99
O5 O5 1.793(19) 98
O5 W2 2.460(9) 9
O5 W2 2.460(9) 5
N1 C12 1.56(10) 28
N1 C12 1.56(10) 51
N1 C12 1.56(10) 74
N1 C12 1.56(10) .
