#------------------------------------------------------------------------------
#$Date: 2016-03-24 01:36:23 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179538 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/07/4500750.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_4500750
loop_
_publ_author_name
'McGlone, Thomas'
'Streb, Carsten'
'Busquets-Fité, Martí'
'Yan, Jun'
'Gabb, David'
'Long, De-Liang'
'Cronin, Leroy'
_publ_section_title
;
 Silver Linked Polyoxometalate Open Frameworks (Ag-POMOFs) for the
 Directed Fabrication of Silver Nanomaterials
;
_journal_issue                   6
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              2471
_journal_paper_doi               10.1021/cg2002496
_journal_volume                  11
_journal_year                    2011
_chemical_formula_sum            'C24 H36 Ag4 Bi N12 O60 W18'
_chemical_formula_weight         5402.41
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_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                120.00
_cell_formula_units_Z            6
_cell_length_a                   20.5547(9)
_cell_length_b                   20.5547(9)
_cell_length_c                   33.1479(19)
_cell_measurement_reflns_used    7278
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.2220
_cell_measurement_theta_min      3.0832
_cell_volume                     12128.6(10)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
;
_computing_data_reduction
;       
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Oxford Diffraction CCD'
_diffrn_measurement_method       '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  0.0864
_diffrn_reflns_av_sigmaI/netI    0.0350
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            23492
_diffrn_reflns_theta_full        25.49
_diffrn_reflns_theta_max         25.49
_diffrn_reflns_theta_min         3.09
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    28.699
_exptl_absorpt_correction_T_max  0.0989
_exptl_absorpt_correction_T_min  0.0440
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    4.438
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             14082
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.054
_refine_diff_density_min         -1.529
_refine_diff_density_rms         0.306
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         2514
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0543
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0545P)²+1180.7531P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1327
_refine_ls_wR_factor_ref         0.1571
_reflns_number_gt                1846
_reflns_number_total             2514
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            cg2002496_si_002.cif
_cod_data_source_block           Ag-3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        12128.5(10)
_cod_original_sg_symbol_H-M      R-3c
_cod_database_code               4500750
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z+1/2'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'-y+2/3, -x+1/3, z+5/6'
'-x+y+2/3, y+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-y+1/3, -x+2/3, z+7/6'
'-x+y+1/3, y+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'y, x, -z-1/2'
'x-y, -y, -z-1/2'
'-x, -x+y, -z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'y+2/3, x+1/3, -z-1/6'
'x-y+2/3, -y+1/3, -z-1/6'
'-x+2/3, -x+y+1/3, -z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'y+1/3, x+2/3, -z+1/6'
'x-y+1/3, -y+2/3, -z+1/6'
'-x+1/3, -x+y+2/3, -z+1/6'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.82977(5) 0.82778(5) 0.05444(3) 0.0534(3) Uani 0.948(3) 1 d P . 1
W2 W 0.98742(5) 0.82278(5) 0.05448(3) 0.0518(3) Uani 0.948(3) 1 d P . 1
W3 W 0.93751(5) 0.88023(5) 0.13540(2) 0.0486(3) Uani 0.948(3) 1 d P . 1
Bi1 Bi 1.0000 1.0000 0.02821(18) 0.0343(14) Uani 0.44 3 d SP . 1
Bi1' Bi 1.0000 1.0000 0.0415(14) 0.040(12) Uani 0.06 3 d SP . 1
Ag1 Ag 0.95247(18) 0.61913(18) 0.0833 0.0825(11) Uani 0.76 2 d SP . 1
Ag2 Ag 0.8677(3) 0.8677(3) 0.2500 0.0828(16) Uani 0.52 2 d SP . 1
Ag3 Ag 1.0000 1.0000 0.2500 0.090(17) Uiso 0.09 6 d SP . 1
O1 O 0.9506(6) 0.9060(7) 0.0676(4) 0.043(3) Uani 1 1 d . . 1
O2 O 0.8805(9) 0.7693(10) 0.0480(5) 0.062(4) Uani 1 1 d . . 1
O3 O 0.8563(7) 0.8606(7) 0.0000(4) 0.049(3) Uani 1 1 d . . 1
O4 O 1.0033(9) 0.7490(8) 0.0494(5) 0.069(4) Uani 1 1 d . . 1
O5 O 0.9695(8) 0.8149(9) 0.1117(4) 0.058(4) Uani 1 1 d . . 1
O6 O 0.9194(8) 0.8437(9) 0.1840(5) 0.067(4) Uani 1 1 d . . 1
O7 O 0.8401(8) 0.8183(8) 0.1117(4) 0.055(3) Uani 1 1 d . . 1
O8 O 0.9139(8) 0.9581(7) 0.1398(4) 0.053(3) Uani 1 1 d . . 1
O9 O 0.7396(8) 0.7566(8) 0.0487(5) 0.068(4) Uani 1 1 d . . 1
O10 O 0.8153(7) 0.9112(7) 0.0635(4) 0.053(3) Uani 1 1 d . . 1
N1 N 0.9749(16) 0.5861(15) 0.0268(9) 0.112(8) Uiso 1 1 d . A 1
C1 C 0.9972(18) 0.5920(19) -0.0052(10) 0.106(10) Uiso 1 1 d . A 1
C2 C 1.026(2) 0.585(2) -0.0450(10) 0.119(11) Uiso 1 1 d . A 1
H2A H 1.0799 0.6036 -0.0432 0.179 Uiso 1 1 calc R A 1
H2B H 1.0166 0.6143 -0.0651 0.179 Uiso 1 1 calc R A 1
H2C H 1.0000 0.5320 -0.0532 0.179 Uiso 1 1 calc R A 1
C3 C 0.746(2) 0.8702(19) 0.1859(12) 0.115(11) Uiso 1 1 d . B 1
N3 N 0.783(2) 0.879(2) 0.2153(12) 0.099(11) Uiso 0.70 1 d P B 1
C4 C 0.705(2) 0.865(2) 0.1477(12) 0.090(12) Uiso 0.70 1 d P B 1
H4A H 0.6958 0.9070 0.1460 0.135 Uiso 0.70 1 calc PR B 1
H4B H 0.6574 0.8174 0.1472 0.135 Uiso 0.70 1 calc PR B 1
H4C H 0.7362 0.8667 0.1247 0.135 Uiso 0.70 1 calc PR B 1
W1' W 0.8460(14) 0.8690(16) 0.1129(8) 0.088(8) Uiso 0.052(3) 1 d P . 2
W3' W 1.0029(16) 0.8623(18) 0.1142(8) 0.091(9) Uiso 0.052(3) 1 d P . 2
W2' W 0.8883(16) 0.7953(17) 0.0354(9) 0.080(9) Uiso 0.052(3) 1 d P . 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -0.8971 1.1015 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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
O9 W1 O10 101.5(7) . .
O9 W1 O3 101.2(7) . .
O10 W1 O3 88.6(5) . .
O9 W1 O7 98.6(7) . .
O10 W1 O7 90.6(6) . .
O3 W1 O7 159.9(6) . .
O9 W1 O2 98.3(7) . .
O10 W1 O2 160.2(6) . .
O3 W1 O2 88.2(6) . .
O7 W1 O2 85.8(7) . .
O9 W1 O1 170.0(6) . .
O10 W1 O1 86.5(5) . .
O3 W1 O1 84.9(5) . .
O7 W1 O1 75.0(5) . .
O2 W1 O1 73.7(6) . .
O4 W2 O3 101.9(7) . 21_655
O4 W2 O2 98.8(8) . .
O3 W2 O2 88.3(6) 21_655 .
O4 W2 O5 97.8(7) . .
O3 W2 O5 160.3(6) 21_655 .
O2 W2 O5 86.9(7) . .
O4 W2 O10 100.4(7) . 2_765
O3 W2 O10 88.4(5) 21_655 2_765
O2 W2 O10 160.8(6) . 2_765
O5 W2 O10 89.9(6) . 2_765
O4 W2 O1 170.4(6) . .
O3 W2 O1 84.9(5) 21_655 .
O2 W2 O1 74.3(6) . .
O5 W2 O1 75.4(5) . .
O10 W2 O1 86.5(5) 2_765 .
O6 W3 O8 101.8(6) . .
O6 W3 O7 99.5(7) . .
O8 W3 O7 88.2(6) . .
O6 W3 O8 101.0(6) . 2_765
O8 W3 O8 88.1(9) . 2_765
O7 W3 O8 159.5(6) . 2_765
O6 W3 O5 98.6(7) . .
O8 W3 O5 159.6(6) . .
O7 W3 O5 88.7(6) . .
O8 W3 O5 87.8(6) 2_765 .
O6 W3 O1 169.5(6) . .
O8 W3 O1 86.0(5) . .
O7 W3 O1 73.5(5) . .
O8 W3 O1 86.1(5) 2_765 .
O5 W3 O1 73.8(5) . .
Bi1 Bi1 O1 127.9(4) 19_775 2_765
Bi1 Bi1 O1 127.9(4) 19_775 3_675
O1 Bi1 O1 86.2(5) 2_765 3_675
Bi1 Bi1 O1 127.9(4) 19_775 .
O1 Bi1 O1 86.2(5) 2_765 .
O1 Bi1 O1 86.2(5) 3_675 .
Bi1 Bi1 Bi1' 0.000(1) 19_775 19_775
O1 Bi1 Bi1' 127.9(4) 2_765 19_775
O1 Bi1 Bi1' 127.9(4) 3_675 19_775
O1 Bi1 Bi1' 127.9(4) . 19_775
O1 Bi1' O1 100.6(17) 2_765 3_675
O1 Bi1' O1 100.6(17) 2_765 .
O1 Bi1' O1 100.6(17) 3_675 .
O1 Bi1' Bi1 117.3(13) 2_765 19_775
O1 Bi1' Bi1 117.3(13) 3_675 19_775
O1 Bi1' Bi1 117.3(13) . 19_775
O1 Bi1' Bi1' 117.3(13) 2_765 19_775
O1 Bi1' Bi1' 117.3(13) 3_675 19_775
O1 Bi1' Bi1' 117.3(13) . 19_775
Bi1 Bi1' Bi1' 0.000(1) 19_775 19_775
N1 Ag1 N1 174.1(15) 34_545 .
N1 Ag1 O4 99.6(8) 34_545 .
N1 Ag1 O4 84.6(8) . .
N1 Ag1 O4 84.6(8) 34_545 34_545
N1 Ag1 O4 99.6(8) . 34_545
O4 Ag1 O4 88.2(7) . 34_545
N1 Ag1 Ag2 87.0(8) 34_545 25_665
N1 Ag1 Ag2 87.1(8) . 25_665
O4 Ag1 Ag2 135.9(3) . 25_665
O4 Ag1 Ag2 135.9(3) 34_545 25_665
N3 Ag2 N3 139.6(19) . 22_556
N3 Ag2 O6 94.4(10) . 22_556
N3 Ag2 O6 89.9(10) 22_556 22_556
N3 Ag2 O6 89.9(10) . .
N3 Ag2 O6 94.4(10) 22_556 .
O6 Ag2 O6 167.3(8) 22_556 .
N3 Ag2 Ag3 110.2(10) . .
N3 Ag2 Ag3 110.2(10) 22_556 .
O6 Ag2 Ag3 83.7(4) 22_556 .
O6 Ag2 Ag3 83.7(4) . .
N3 Ag2 Ag1 69.8(10) . 25_665
N3 Ag2 Ag1 69.8(10) 22_556 25_665
O6 Ag2 Ag1 96.3(4) 22_556 25_665
O6 Ag2 Ag1 96.3(4) . 25_665
Ag3 Ag2 Ag1 180.0 . 25_665
Ag2 Ag3 Ag2 120.000(1) . 3_675
Ag2 Ag3 Ag2 120.000(1) . 2_765
Ag2 Ag3 Ag2 120.000(1) 3_675 2_765
Bi1' O1 Bi1 10.6(13) . .
Bi1' O1 W1 119.0(9) . .
Bi1 O1 W1 113.0(5) . .
Bi1' O1 W2 118.8(9) . .
Bi1 O1 W2 112.7(5) . .
W1 O1 W2 95.3(5) . .
Bi1' O1 W3 128.8(14) . .
Bi1 O1 W3 139.4(6) . .
W1 O1 W3 93.8(4) . .
W2 O1 W3 93.4(4) . .
W2 O2 W1 116.5(9) . .
W1 O3 W2 142.9(8) . 20_565
W2 O4 Ag1 135.6(8) . .
W2 O5 W3 117.4(7) . .
W3 O6 Ag2 136.2(8) . .
W3 O7 W1 117.7(7) . .
W3 O8 W3 150.3(8) . 3_675
W1 O10 W2 154.2(8) . 3_675
C1 N1 Ag1 158(3) . .
N1 C1 C2 168(4) . .
N3 C3 C4 175(4) . .
C3 N3 Ag2 154(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 O9 1.704(14) .
W1 O10 1.906(12) .
W1 O3 1.909(13) .
W1 O7 1.930(14) .
W1 O2 1.956(16) .
W1 O1 2.225(12) .
W2 O4 1.712(13) .
W2 O3 1.909(12) 21_655
W2 O2 1.916(17) .
W2 O5 1.924(14) .
W2 O10 1.934(12) 2_765
W2 O1 2.232(12) .
W3 O6 1.738(15) .
W3 O8 1.896(12) .
W3 O7 1.924(14) .
W3 O8 1.925(12) 2_765
W3 O5 1.932(15) .
W3 O1 2.294(12) .
Bi1 Bi1 1.870(12) 19_775
Bi1 O1 2.123(12) 2_765
Bi1 O1 2.123(12) 3_675
Bi1 O1 2.123(12) .
Bi1 Bi1' 2.31(4) 19_775
Bi1' O1 1.89(2) 2_765
Bi1' O1 1.89(2) 3_675
Bi1' O1 1.89(2) .
Bi1' Bi1 2.31(4) 19_775
Bi1' Bi1' 2.75(9) 19_775
Ag1 N1 2.12(3) 34_545
Ag1 N1 2.12(3) .
Ag1 O4 2.586(15) .
Ag1 O4 2.586(15) 34_545
Ag1 Ag2 3.154(7) 25_665
Ag2 N3 2.19(4) .
Ag2 N3 2.19(4) 22_556
Ag2 O6 2.585(15) 22_556
Ag2 O6 2.585(15) .
Ag2 Ag3 2.720(6) .
Ag2 Ag1 3.154(7) 25_665
Ag3 Ag2 2.720(6) 3_675
Ag3 Ag2 2.720(6) 2_765
O3 W2 1.909(12) 20_565
O8 W3 1.925(12) 3_675
O10 W2 1.934(12) 3_675
N1 C1 1.14(4) .
C1 C2 1.48(4) .
C3 N3 1.20(5) .
C3 C4 1.49(5) .
W1' W3' 2.51(5) 3_675
W3' W1' 2.51(5) 2_765
