#------------------------------------------------------------------------------
#$Date: 2019-10-28 05:45:39 +0200 (Mon, 28 Oct 2019) $
#$Revision: 219765 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/45/4514581.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_4514581
loop_
_publ_author_name
'Hou, Yan'
'Chai, Dongfeng'
'Li, Bonan'
'Pang, Haijun'
'Ma, Huiyuan'
'Wang, Xinming'
'Tan, Lichao'
_publ_section_title
;
 Polyoxometalate-Incorporated Metallacalixarene@Graphene Composite
 Electrodes for High-Performance Supercapacitors.
;
_journal_issue                   23
_journal_name_full               'ACS applied materials & interfaces'
_journal_page_first              20845
_journal_page_last               20853
_journal_paper_doi               10.1021/acsami.9b04649
_journal_volume                  11
_journal_year                    2019
_chemical_formula_moiety         'C12 H17 Ag5 N18 O40 Si W12'
_chemical_formula_sum            'C12 H17 Ag5 N18 O40 Si W12'
_chemical_formula_weight         3826.86
_space_group_IT_number           162
_space_group_name_Hall           '-P 3 2'
_space_group_name_H-M_alt        'P -3 1 m'
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 3 2'
_symmetry_space_group_name_H-M   'P -3 1 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                120.00
_cell_formula_units_Z            1
_cell_length_a                   12.1796(7)
_cell_length_b                   12.1796(7)
_cell_length_c                   10.4736(8)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.300
_cell_measurement_theta_min      7
_cell_volume                     1345.53(15)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    'Bruker SMART'
_computing_publication_material  'Bruker SMART'
_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     0.71000
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_av_sigmaI/netI    0.0261
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10112
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    27.404
_exptl_absorpt_correction_T_max  0.007
_exptl_absorpt_correction_T_min  0.001
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    4.706
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1663.2
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_refine_diff_density_max         3.246
_refine_diff_density_min         -2.644
_refine_diff_density_rms         0.327
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     87
_refine_ls_number_reflns         1222
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0374
_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)+(0.0466P)²+29.3777P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0906
_refine_ls_wR_factor_ref         0.0977
_reflns_number_gt                1033
_reflns_number_total             1224
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            am9b04649_si_003.cif
_cod_data_source_block           haa
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal'
according to
/home/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        1345.5(2)
_cod_original_sg_symbol_Hall     -P32
_cod_original_sg_symbol_H-M      'P-31m  '
_cod_database_code               4514581
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, -z'
'-x+y, y, -z'
'x, x-y, -z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'y, x, z'
'x-y, -y, z'
'-x, -x+y, z'
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
W1 W 0.16703(5) 0.0000 0.22478(6) 0.02601(19) Uani 1 2 d SU
W2 W 0.33406(5) 0.16703(3) 0.5000 0.02603(19) Uani 1 2 d SU
Ag2 Ag 0.6667 0.3333 0.2846(4) 0.0484(10) Uani 0.48 3 d SPU
Ag1 Ag 0.77517(18) 0.22483(18) 0.0000 0.0547(8) Uani 0.50 2 d SP
Si1 Si 0.0000 0.0000 0.5000 0.0142(16) Uani 1 12 d SU
O4 O 0.2996(13) 0.1253(9) 0.3252(10) 0.065(3) Uani 1 1 d U
O2 O 0.2500(13) 0.0000 0.0964(14) 0.054(4) Uani 1 2 d S
O1 O 0.1243(11) 0.1243(11) 0.186(2) 0.073(6) Uani 1 2 d S
O5 O 0.4915(12) 0.2458(6) 0.5000 0.056(4) Uani 1 2 d S
O6 O 0.302(2) 0.302(2) 0.4701(15) 0.086(7) Uani 1 2 d SU
O3 O 0.1263(15) 0.0000 0.4464(18) 0.017(3) Uani 0.50 2 d SPU
C1 C 0.5825(15) 0.104(2) 0.2282(15) 0.062(4) Uani 1 1 d U
H1A H 0.6076 0.1867 0.2530 0.074 Uiso 1 1 calc R
N2 N 0.4936(19) 0.0000 0.289(2) 0.076(6) Uani 1 2 d SU
N1 N 0.6310(17) 0.074(2) 0.1263(15) 0.109(7) Uani 1 1 d U
O7 O 0.0000 0.0000 0.347(3) 0.021(6) Uani 0.50 6 d SPU
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 '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'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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'
N N 0.0061 0.0033 '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
O2 W1 O1 103.6(8) . 3
O2 W1 O1 103.6(8) . .
O1 W1 O1 88.8(8) 3 .
O2 W1 O4 100.0(6) . .
O1 W1 O4 156.3(8) 3 .
O1 W1 O4 86.5(6) . .
O2 W1 O4 100.0(6) . 11
O1 W1 O4 86.5(6) 3 11
O1 W1 O4 156.3(8) . 11
O4 W1 O4 88.6(6) . 11
O2 W1 O3 155.2(7) . .
O1 W1 O3 94.0(8) 3 .
O1 W1 O3 94.0(8) . .
O4 W1 O3 63.3(5) . .
O4 W1 O3 63.3(5) 11 .
O2 W1 O7 159.1(9) . .
O1 W1 O7 62.5(7) 3 .
O1 W1 O7 62.5(7) . .
O4 W1 O7 94.9(6) . .
O4 W1 O7 94.9(6) 11 .
O3 W1 O7 45.8(8) . .
O5 W2 O4 101.1(4) . .
O5 W2 O4 101.1(4) . 6_556
O4 W2 O4 157.8(8) . 6_556
O5 W2 O6 100.4(7) . 8_556
O4 W2 O6 88.4(6) . 8_556
O4 W2 O6 87.6(7) 6_556 8_556
O5 W2 O6 100.4(7) . .
O4 W2 O6 87.6(7) . .
O4 W2 O6 88.4(6) 6_556 .
O6 W2 O6 159.2(14) 8_556 .
O5 W2 O3 156.5(4) . .
O4 W2 O3 63.0(6) . .
O4 W2 O3 95.8(6) 6_556 .
O6 W2 O3 64.0(7) 8_556 .
O6 W2 O3 96.2(8) . .
O5 W2 O3 156.5(4) . 9_556
O4 W2 O3 95.8(6) . 9_556
O4 W2 O3 63.0(6) 6_556 9_556
O6 W2 O3 96.2(8) 8_556 9_556
O6 W2 O3 64.0(7) . 9_556
O3 W2 O3 46.9(8) . 9_556
C1 Ag2 C1 114.7(3) . 2_655
C1 Ag2 C1 114.7(3) . 3_665
C1 Ag2 C1 114.7(3) 2_655 3_665
N1 Ag1 N1 176.3(11) 4_665 .
O7 Si1 O7 180.000(3) 7_556 .
O7 Si1 O3 110.0(7) 7_556 3
O7 Si1 O3 70.0(7) . 3
O7 Si1 O3 70.0(7) 7_556 9_556
O7 Si1 O3 110.0(7) . 9_556
O3 Si1 O3 180(2) 3 9_556
O7 Si1 O3 110.0(7) 7_556 .
O7 Si1 O3 70.0(6) . .
O3 Si1 O3 108.9(7) 3 .
O3 Si1 O3 71.1(7) 9_556 .
O7 Si1 O3 110.0(7) 7_556 2
O7 Si1 O3 70.0(6) . 2
O3 Si1 O3 108.9(7) 3 2
O3 Si1 O3 71.1(7) 9_556 2
O3 Si1 O3 108.9(7) . 2
O7 Si1 O3 70.0(7) 7_556 8_556
O7 Si1 O3 110.0(7) . 8_556
O3 Si1 O3 71.1(7) 3 8_556
O3 Si1 O3 108.9(7) 9_556 8_556
O3 Si1 O3 71.1(7) . 8_556
O3 Si1 O3 180.0(5) 2 8_556
O7 Si1 O3 70.0(6) 7_556 7_556
O7 Si1 O3 110.0(7) . 7_556
O3 Si1 O3 71.1(7) 3 7_556
O3 Si1 O3 108.9(7) 9_556 7_556
O3 Si1 O3 180.0(5) . 7_556
O3 Si1 O3 71.1(7) 2 7_556
O3 Si1 O3 108.9(7) 8_556 7_556
W2 O4 W1 137.8(7) . .
W1 O1 W1 139.9(11) 2 .
W2 O6 W2 136.9(12) . 9_556
Si1 O3 W1 122.1(10) . .
Si1 O3 W2 121.0(6) . .
W1 O3 W2 95.6(6) . .
Si1 O3 W2 121.0(6) . 8_556
W1 O3 W2 95.6(6) . 8_556
W2 O3 W2 95.0(7) . 8_556
N2 C1 N1 112(2) . .
N2 C1 Ag2 128.5(12) . .
N1 C1 Ag2 119.6(16) . .
N2 C1 H1A 124.1 . .
N1 C1 H1A 124.1 . .
Ag2 C1 H1A 4.7 . .
C1 N2 C1 109(2) 11 .
C1 N1 N1 103.6(14) . 11
C1 N1 Ag1 120.8(18) . .
N1 N1 Ag1 135.5(6) 11 .
Si1 O7 W1 122.2(6) . 3
Si1 O7 W1 122.2(6) . .
W1 O7 W1 94.3(8) 3 .
Si1 O7 W1 122.2(6) . 2
W1 O7 W1 94.3(8) 3 2
W1 O7 W1 94.3(8) . 2
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 O2 1.682(12) .
W1 O1 1.875(6) 3
W1 O1 1.875(6) .
W1 O4 1.891(10) .
W1 O4 1.891(10) 11
W1 O3 2.374(19) .
W1 O7 2.403(16) .
W2 O5 1.661(12) .
W2 O4 1.890(10) .
W2 O4 1.890(10) 6_556
W2 O6 1.894(8) 8_556
W2 O6 1.894(8) .
W2 O3 2.389(13) .
W2 O3 2.389(13) 9_556
Ag2 C1 2.52(2) .
Ag2 C1 2.52(2) 2_655
Ag2 C1 2.52(2) 3_665
Ag1 N1 2.23(2) 4_665
Ag1 N1 2.23(2) .
Si1 O7 1.60(3) 7_556
Si1 O7 1.60(3) .
Si1 O3 1.637(19) 3
Si1 O3 1.637(19) 9_556
Si1 O3 1.637(19) .
Si1 O3 1.637(19) 2
Si1 O3 1.637(19) 8_556
Si1 O3 1.637(19) 7_556
O1 W1 1.875(6) 2
O6 W2 1.894(8) 9_556
O3 W2 2.389(13) 8_556
C1 N2 1.35(2) .
C1 N1 1.36(2) .
C1 H1A 0.9300 .
N2 C1 1.35(2) 11
N1 N1 1.56(5) 11
O7 W1 2.403(16) 3
O7 W1 2.403(16) 2
