#------------------------------------------------------------------------------
#$Date: 2016-03-21 17:29:04 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178784 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/38/4103877.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_4103877
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            'C76 H36 Cu12 Ge N O112 W12'
_chemical_formula_weight         5795.86
_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_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            4
_cell_length_a                   26.3189(12)
_cell_length_b                   26.318(12)
_cell_length_c                   26.318(12)
_cell_measurement_reflns_used    4347
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.85
_cell_measurement_theta_min      2.19
_cell_volume                     18229(12)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0489
_diffrn_reflns_av_sigmaI/netI    0.0134
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            23342
_diffrn_reflns_theta_full        25.06
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         1.34
_exptl_absorpt_coefficient_mu    9.152
_exptl_absorpt_correction_T_max  0.348
_exptl_absorpt_correction_T_min  0.331
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR by T.Higashi    8 March, 1995'
_exptl_crystal_density_diffrn    2.098
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             10400
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         3.092
_refine_diff_density_min         -2.197
_refine_diff_density_rms         0.612
_refine_ls_extinction_coef       0.000132(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.295
_refine_ls_matrix_type           full
_refine_ls_number_parameters     62
_refine_ls_number_reflns         874
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.295
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0493
_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)+(0.0979P)²+171.7548P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1373
_refine_ls_wR_factor_ref         0.1608
_reflns_number_gt                758
_reflns_number_total             874
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja807357r_si_003.cif
_cod_data_source_block           2
_cod_original_cell_volume        18229.0
_cod_database_code               4103877
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -y, -z'
'y, x, -z'
'-x, y, -z'
'-y, -x, -z'
'z, x, y'
'-x, z, y'
'-z, -x, y'
'x, -z, y'
'z, -x, -y'
'x, z, -y'
'-z, x, -y'
'-x, -z, -y'
'y, z, x'
'-z, -y, -x'
'-z, y, x'
'z, y, -x'
'z, -y, x'
'y, -z, -x'
'-y, -z, x'
'-y, z, -x'
'x, y+1/2, z+1/2'
'-y, x+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'y, -x+1/2, z+1/2'
'x, -y+1/2, -z+1/2'
'y, x+1/2, -z+1/2'
'-x, y+1/2, -z+1/2'
'-y, -x+1/2, -z+1/2'
'z, x+1/2, y+1/2'
'-x, z+1/2, y+1/2'
'-z, -x+1/2, y+1/2'
'x, -z+1/2, y+1/2'
'z, -x+1/2, -y+1/2'
'x, z+1/2, -y+1/2'
'-z, x+1/2, -y+1/2'
'-x, -z+1/2, -y+1/2'
'y, 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, x+1/2'
'y, -z+1/2, -x+1/2'
'-y, -z+1/2, x+1/2'
'-y, z+1/2, -x+1/2'
'x+1/2, y, z+1/2'
'-y+1/2, x, z+1/2'
'-x+1/2, -y, z+1/2'
'y+1/2, -x, z+1/2'
'x+1/2, -y, -z+1/2'
'y+1/2, x, -z+1/2'
'-x+1/2, y, -z+1/2'
'-y+1/2, -x, -z+1/2'
'z+1/2, x, y+1/2'
'-x+1/2, z, y+1/2'
'-z+1/2, -x, y+1/2'
'x+1/2, -z, y+1/2'
'z+1/2, -x, -y+1/2'
'x+1/2, z, -y+1/2'
'-z+1/2, x, -y+1/2'
'-x+1/2, -z, -y+1/2'
'y+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, x+1/2'
'y+1/2, -z, -x+1/2'
'-y+1/2, -z, x+1/2'
'-y+1/2, z, -x+1/2'
'x+1/2, y+1/2, z'
'-y+1/2, x+1/2, z'
'-x+1/2, -y+1/2, z'
'y+1/2, -x+1/2, z'
'x+1/2, -y+1/2, -z'
'y+1/2, x+1/2, -z'
'-x+1/2, y+1/2, -z'
'-y+1/2, -x+1/2, -z'
'z+1/2, x+1/2, y'
'-x+1/2, z+1/2, y'
'-z+1/2, -x+1/2, y'
'x+1/2, -z+1/2, y'
'z+1/2, -x+1/2, -y'
'x+1/2, z+1/2, -y'
'-z+1/2, x+1/2, -y'
'-x+1/2, -z+1/2, -y'
'y+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, x'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z+1/2, x'
'-y+1/2, z+1/2, -x'
'-x, -y, -z'
'y, -x, -z'
'x, y, -z'
'-y, x, -z'
'-x, y, z'
'-y, -x, z'
'x, -y, z'
'y, x, z'
'-z, -x, -y'
'x, -z, -y'
'z, x, -y'
'-x, z, -y'
'-z, x, y'
'-x, -z, y'
'z, -x, y'
'x, z, y'
'-y, -z, -x'
'z, y, x'
'z, -y, -x'
'-z, -y, x'
'-z, y, -x'
'-y, z, x'
'y, z, -x'
'y, -z, x'
'-x, -y+1/2, -z+1/2'
'y, -x+1/2, -z+1/2'
'x, y+1/2, -z+1/2'
'-y, x+1/2, -z+1/2'
'-x, y+1/2, z+1/2'
'-y, -x+1/2, z+1/2'
'x, -y+1/2, z+1/2'
'y, x+1/2, z+1/2'
'-z, -x+1/2, -y+1/2'
'x, -z+1/2, -y+1/2'
'z, x+1/2, -y+1/2'
'-x, z+1/2, -y+1/2'
'-z, x+1/2, y+1/2'
'-x, -z+1/2, y+1/2'
'z, -x+1/2, y+1/2'
'x, z+1/2, y+1/2'
'-y, -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, -x+1/2'
'-y, z+1/2, x+1/2'
'y, z+1/2, -x+1/2'
'y, -z+1/2, x+1/2'
'-x+1/2, -y, -z+1/2'
'y+1/2, -x, -z+1/2'
'x+1/2, y, -z+1/2'
'-y+1/2, x, -z+1/2'
'-x+1/2, y, z+1/2'
'-y+1/2, -x, z+1/2'
'x+1/2, -y, z+1/2'
'y+1/2, x, z+1/2'
'-z+1/2, -x, -y+1/2'
'x+1/2, -z, -y+1/2'
'z+1/2, x, -y+1/2'
'-x+1/2, z, -y+1/2'
'-z+1/2, x, y+1/2'
'-x+1/2, -z, y+1/2'
'z+1/2, -x, y+1/2'
'x+1/2, z, y+1/2'
'-y+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, -x+1/2'
'-y+1/2, z, x+1/2'
'y+1/2, z, -x+1/2'
'y+1/2, -z, x+1/2'
'-x+1/2, -y+1/2, -z'
'y+1/2, -x+1/2, -z'
'x+1/2, y+1/2, -z'
'-y+1/2, x+1/2, -z'
'-x+1/2, y+1/2, z'
'-y+1/2, -x+1/2, z'
'x+1/2, -y+1/2, z'
'y+1/2, x+1/2, z'
'-z+1/2, -x+1/2, -y'
'x+1/2, -z+1/2, -y'
'z+1/2, x+1/2, -y'
'-x+1/2, z+1/2, -y'
'-z+1/2, x+1/2, y'
'-x+1/2, -z+1/2, y'
'z+1/2, -x+1/2, y'
'x+1/2, z+1/2, y'
'-y+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, -x'
'-y+1/2, z+1/2, x'
'y+1/2, z+1/2, -x'
'y+1/2, -z+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
Cu1 Cu 0.21480(4) 0.28520(4) 0.0000 0.0250(5) Uani 1 4 d S
Ge1 Ge 0.0000 0.0000 0.0000 0.0257(11) Uani 1.00 48 d SP
W1 W 0.0000 0.095011(18) 0.095011(18) 0.0428(4) Uani 1 4 d S
C1 C 0.1987(4) 0.1334(3) 0.1334(3) 0.033(2) Uani 1 2 d S
H1 H 0.2276 0.1191 0.1191 0.039 Uiso 1 2 calc SR
C2 C 0.2024(3) 0.2024(3) 0.0686(4) 0.032(2) Uani 1 2 d S
C3 C 0.1769(3) 0.1769(3) 0.1115(4) 0.033(2) Uani 1 2 d S
C4 C 0.2157(18) 0.2157(18) 0.2843(18) 0.10(2) Uiso 0.50 6 d SP
H4A H 0.1855 0.2064 0.2660 0.151 Uiso 0.08 1 calc PR
H4B H 0.2064 0.2340 0.3145 0.151 Uiso 0.08 1 calc PR
H4C H 0.2340 0.1855 0.2936 0.151 Uiso 0.08 1 calc PR
N1 N 0.2500 0.2500 0.2500 0.026(12) Uani 0.50 24 d SP
O1 O 0.1561(3) 0.3439(3) 0.0000 0.098(6) Uani 1 4 d S
O2 O 0.1832(2) 0.24355(19) 0.0527(2) 0.0368(12) Uani 1 1 d .
O3 O -0.0382(6) 0.0382(6) 0.0382(6) 0.033(5) Uani 0.50 6 d SP
O4 O 0.0000 0.1398(3) 0.1398(3) 0.067(4) Uani 1 4 d S
O5 O 0.0491(3) 0.0491(3) 0.1206(5) 0.092(4) Uani 1 2 d S
O6 O 0.0751(11) 0.2470(11) 0.0000 0.106(8) Uiso 0.50 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'
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 Cu1 O2 90.4(3) 174 80
O2 Cu1 O2 169.1(3) 174 99
O2 Cu1 O2 88.6(3) 80 99
O2 Cu1 O2 88.6(3) 174 .
O2 Cu1 O2 169.1(3) 80 .
O2 Cu1 O2 90.4(3) 99 .
O2 Cu1 O1 95.47(15) 174 .
O2 Cu1 O1 95.47(15) 80 .
O2 Cu1 O1 95.47(15) 99 .
O2 Cu1 O1 95.47(15) . .
O2 Cu1 Cu1 84.53(15) 174 169
O2 Cu1 Cu1 84.53(15) 80 169
O2 Cu1 Cu1 84.53(15) 99 169
O2 Cu1 Cu1 84.53(15) . 169
O1 Cu1 Cu1 180.0(3) . 169
O3 Ge1 O3 70.529(1) 4 3
O3 Ge1 O3 109.471(1) 4 97
O3 Ge1 O3 70.529(1) 3 97
O3 Ge1 O3 70.5 4 98
O3 Ge1 O3 109.471(1) 3 98
O3 Ge1 O3 70.529(1) 97 98
O3 Ge1 O3 180(2) 4 100
O3 Ge1 O3 109.471(1) 3 100
O3 Ge1 O3 70.5 97 100
O3 Ge1 O3 109.471(1) 98 100
O3 Ge1 O3 70.529(1) 4 .
O3 Ge1 O3 109.471(1) 3 .
O3 Ge1 O3 180(2) 97 .
O3 Ge1 O3 109.5 98 .
O3 Ge1 O3 109.471(1) 100 .
O3 Ge1 O3 109.471(1) 4 2
O3 Ge1 O3 70.529(1) 3 2
O3 Ge1 O3 109.471(1) 97 2
O3 Ge1 O3 180(2) 98 2
O3 Ge1 O3 70.529(1) 100 2
O3 Ge1 O3 70.529(1) . 2
O3 Ge1 O3 109.471(1) 4 99
O3 Ge1 O3 180(2) 3 99
O3 Ge1 O3 109.471(1) 97 99
O3 Ge1 O3 70.529(1) 98 99
O3 Ge1 O3 70.529(1) 100 99
O3 Ge1 O3 70.529(1) . 99
O3 Ge1 O3 109.471(1) 2 99
O4 W1 O5 101.5(4) . 112
O4 W1 O5 101.5(4) . .
O5 W1 O5 89.3(6) 112 .
O4 W1 O5 101.5(4) . 10
O5 W1 O5 86.2(7) 112 10
O5 W1 O5 157.0(9) . 10
O4 W1 O5 101.5(4) . 2
O5 W1 O5 157.0(9) 112 2
O5 W1 O5 86.2(7) . 2
O5 W1 O5 89.3(6) 10 2
O4 W1 O3 154.6(6) . .
O5 W1 O3 96.5(6) 112 .
O5 W1 O3 96.5(6) . .
O5 W1 O3 61.8(5) 10 .
O5 W1 O3 61.8(5) 2 .
O4 W1 O3 154.6(6) . 4
O5 W1 O3 61.8(5) 112 4
O5 W1 O3 61.8(5) . 4
O5 W1 O3 96.5(6) 10 4
O5 W1 O3 96.5(6) 2 4
O3 W1 O3 50.8(11) . 4
C3 C1 C3 120.2(10) . 112
O2 C2 O2 124.9(9) 104 .
O2 C2 C3 117.5(5) 104 .
O2 C2 C3 117.5(5) . .
C1 C3 C1 119.8(10) . 104
C1 C3 C2 120.0(5) . .
C1 C3 C2 120.0(5) 104 .
C4 N1 C4 109.47(2) 75 148
C4 N1 C4 109.471(3) 75 .
C4 N1 C4 109.471(11) 148 .
C4 N1 C4 109.471(11) 75 122
C4 N1 C4 109.5 148 122
C4 N1 C4 109.471(7) . 122
C2 O2 Cu1 123.0(5) . .
Ge1 O3 W1 119.3(6) . .
Ge1 O3 W1 119.3(6) . 19
W1 O3 W1 98.1(7) . 19
Ge1 O3 W1 119.3(6) . 2
W1 O3 W1 98.1(7) . 2
W1 O3 W1 98.1(7) 19 2
W1 O5 W1 138.1(8) 4 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O2 1.954(5) 174
Cu1 O2 1.954(5) 80
Cu1 O2 1.954(5) 99
Cu1 O2 1.954(5) .
Cu1 O1 2.183(13) .
Cu1 Cu1 2.620(3) 169
Ge1 O3 1.74(3) 4
Ge1 O3 1.74(3) 3
Ge1 O3 1.74(3) 97
Ge1 O3 1.74(3) 98
Ge1 O3 1.74(3) 100
Ge1 O3 1.74(3) .
Ge1 O3 1.74(3) 2
Ge1 O3 1.74(3) 99
W1 O4 1.668(12) .
W1 O5 1.893(5) 112
W1 O5 1.893(5) .
W1 O5 1.893(5) 10
W1 O5 1.893(5) 2
W1 O3 2.341(13) .
W1 O3 2.341(13) 4
C1 C3 1.404(6) .
C1 C3 1.404(6) 112
C2 O2 1.267(7) 104
C2 O2 1.267(7) .
C2 C3 1.473(13) .
C3 C1 1.404(6) 104
C4 N1 1.57(8) .
N1 C4 1.57(8) 75
N1 C4 1.57(8) 148
N1 C4 1.57(8) 122
O3 W1 2.341(13) 19
O3 W1 2.341(13) 2
O5 W1 1.893(5) 4
