#------------------------------------------------------------------------------
#$Date: 2021-03-15 10:19:22 +0200 (Mon, 15 Mar 2021) $
#$Revision: 263036 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/10/1561015.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_1561015
loop_
_publ_author_name
'Li, Xiao'
'Zhou, Kunfeng'
'Tong, Zhibo'
'Yang, Jianbo'
'Sheng, Ning'
'Li, Jisen'
'Sha, Jingquan'
_publ_section_title
;
 Keggin polyoxometalates based hybrid compounds containing helix/nanocages
 for colorimetric biosensing
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              372
_journal_page_last               380
_journal_paper_doi               10.1016/j.jssc.2018.06.020
_journal_volume                  265
_journal_year                    2018
_chemical_formula_moiety         'O40 Si W12, 3(C13 F2 N6 O)'
_chemical_formula_sum            'C39 F6 N18 O43 Si W12'
_chemical_formula_weight         3756.74
_space_group_crystal_system      trigonal
_space_group_IT_number           165
_space_group_name_Hall           '-P 3 2"c'
_space_group_name_H-M_alt        'P -3 c 1'
_atom_sites_solution_hydrogens   .
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            4
_cell_length_a                   18.8360(8)
_cell_length_b                   18.8360(8)
_cell_length_c                   25.942(2)
_cell_measurement_reflns_used    38367
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.999
_cell_measurement_theta_min      2.006
_cell_volume                     7971.0(8)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            38367
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.006
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    17.364
_exptl_crystal_density_diffrn    3.131
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             6640
_refine_diff_density_max         2.880
_refine_diff_density_min         -1.476
_refine_diff_density_rms         0.265
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         4704
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0392
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0534P)²+170.8710P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1081
_refine_ls_wR_factor_ref         0.1256
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3655
_reflns_number_total             4707
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            2.cif
_cod_data_source_block           2
_cod_original_cell_volume        7970.8(10)
_cod_database_code               1561015
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.66580(3) 0.21990(3) 0.42765(2) 0.03331(17) Uani 1 1 d . . . . .
W2 W 0.76653(4) 0.21740(4) 0.32182(2) 0.03661(17) Uani 1 1 d . . . . .
W3 W 0.56134(4) 0.11775(3) 0.32283(2) 0.03608(17) Uani 1 1 d . . . . .
W4 W 0.76980(4) 0.33371(4) 0.20637(2) 0.03702(17) Uani 1 1 d . . . . .
Si1 Si 0.6667 0.3333 0.32014(18) 0.0152(10) Uani 1 3 d S T P . .
N1 N 0.6743(13) 0.0783(12) 0.1805(8) 0.091(6) Uani 1 1 d . . . . .
O1 O 0.5860(5) 0.2534(5) 0.4352(3) 0.0286(19) Uani 1 1 d . . . . .
O2 O 0.6666(6) 0.2525(6) 0.1779(4) 0.038(2) Uani 1 1 d . . . . .
O4 O 0.6667 0.3333 0.2574(5) 0.027(3) Uani 1 3 d S T P . .
O5 O 0.4893(5) 0.1588(5) 0.3356(3) 0.034(2) Uani 1 1 d . . . . .
O6 O 0.4945(6) 0.0157(6) 0.3161(4) 0.044(2) Uani 1 1 d . . . . .
O7 O 0.6634(6) 0.1200(5) 0.3120(4) 0.039(2) Uani 1 1 d . . . . .
O8 O 0.8321(7) 0.1803(7) 0.3147(4) 0.049(3) Uani 1 1 d . . . . .
O9 O 0.7621(6) 0.2529(6) 0.2537(3) 0.036(2) Uani 1 1 d . . . . .
O10 O 0.5688(6) 0.1579(6) 0.2543(3) 0.035(2) Uani 1 1 d . . . . .
O11 O 0.7470(6) 0.2019(5) 0.3948(3) 0.034(2) Uani 1 1 d . . . . .
O12 O 0.5826(5) 0.1207(5) 0.3957(3) 0.033(2) Uani 1 1 d . . . . .
O13 O 0.6659(5) 0.2514(5) 0.3411(3) 0.0268(18) Uani 1 1 d . . . . .
C1 C 0.7149(11) 0.1619(10) 0.0973(7) 0.058(4) Uani 1 1 d . . . . .
O14 O 0.6663(6) 0.1839(6) 0.4879(4) 0.043(2) Uani 1 1 d . . . . .
O15 O 0.8343(7) 0.3337(7) 0.1601(4) 0.052(3) Uani 1 1 d . . . . .
N2 N 0.7319(8) 0.1334(8) 0.1462(5) 0.051(3) Uani 1 1 d . . . . .
F2 F 0.8507(7) 0.1736(7) 0.0284(5) 0.097(4) Uani 1 1 d . . . . .
C2 C 0.7114(10) 0.0563(10) 0.2140(6) 0.043(3) Uani 1 1 d . . . . .
C3 C 0.8060(9) 0.1474(10) 0.1585(5) 0.043(4) Uani 1 1 d . . . . .
O16 O 0.6030(7) 0.0341(8) 0.0730(7) 0.097(6) Uani 1 1 d . . . . .
C4 C 0.7385(10) 0.0521(9) 0.0577(5) 0.047(4) Uani 1 1 d . . . . .
N3 N 0.7895(14) 0.0999(13) 0.2005(7) 0.097(7) Uani 1 1 d . . . . .
C5 C 0.6837(10) 0.0919(9) 0.0583(7) 0.058(5) Uani 1 1 d . . . . .
C6 C 0.7092(10) -0.0279(11) 0.0759(6) 0.054(4) Uani 1 1 d . . . . .
C7 C 0.8177(12) 0.0957(11) 0.0450(7) 0.064(5) Uani 1 1 d . . . . .
F1 F 0.8889(10) -0.0462(11) 0.0710(7) 0.140(7) Uani 1 1 d . . . . .
C8 C 0.7590(13) -0.0597(13) 0.0816(8) 0.072(5) Uani 1 1 d . . . . .
C9 C 0.8701(13) 0.0669(14) 0.0467(9) 0.082(7) Uani 1 1 d . . . . .
C10 C 0.8397(17) -0.0111(19) 0.0659(9) 0.094(8) Uani 1 1 d . . . . .
C11 C 0.6787(14) 0.1269(11) 0.0063(8) 0.088(8) Uani 1 1 d . . . . .
C13 C 0.708(2) 0.0632(19) -0.0678(8) 0.21(3) Uani 1 1 d . . . . .
N5 N 0.651(2) -0.0072(16) -0.1000(7) 0.181(16) Uani 1 1 d . . . . .
C12 C 0.586(2) -0.037(2) -0.0784(14) 0.121(9) Uani 1 1 d . U . . .
N4 N 0.579(2) 0.001(2) -0.0407(13) 0.164(10) Uani 1 1 d . U . . .
N6 N 0.6554(11) 0.0666(11) -0.0348(8) 0.106(8) Uani 1 1 d . . . . .
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'
N N 0.0061 0.0033 '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'
F F 0.0171 0.0103 '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'
Ag Ag -0.8971 1.1015 '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'
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
O14 W1 O1 100.9(4) . 2_655
O14 W1 O1 101.5(4) . .
O1 W1 O1 86.8(5) 2_655 .
O14 W1 O12 99.9(4) . .
O1 W1 O12 159.2(4) 2_655 .
O1 W1 O12 88.3(4) . .
O14 W1 O11 100.0(4) . .
O1 W1 O11 88.8(4) 2_655 .
O1 W1 O11 158.5(4) . .
O12 W1 O11 88.4(4) . .
O14 W1 O13 171.1(4) . .
O1 W1 O13 85.3(3) 2_655 .
O1 W1 O13 85.1(3) . .
O12 W1 O13 74.2(3) . .
O11 W1 O13 73.6(3) . .
O8 W2 O9 102.2(4) . .
O8 W2 O7 100.9(5) . .
O9 W2 O7 90.6(4) . .
O8 W2 O5 101.3(5) . 2_655
O9 W2 O5 85.4(4) . 2_655
O7 W2 O5 157.7(4) . 2_655
O8 W2 O11 99.6(4) . .
O9 W2 O11 158.0(4) . .
O7 W2 O11 87.7(4) . .
O5 W2 O11 87.9(4) 2_655 .
O8 W2 O13 170.9(4) . .
O9 W2 O13 85.3(3) . .
O7 W2 O13 73.5(3) . .
O5 W2 O13 84.3(3) 2_655 .
O11 W2 O13 73.2(3) . .
O6 W3 O5 101.7(4) . .
O6 W3 O10 102.6(4) . .
O5 W3 O10 85.8(4) . .
O6 W3 O7 100.2(4) . .
O5 W3 O7 158.1(4) . .
O10 W3 O7 88.8(4) . .
O6 W3 O12 99.2(4) . .
O5 W3 O12 89.9(4) . .
O10 W3 O12 158.2(4) . .
O7 W3 O12 87.3(4) . .
O6 W3 O13 170.2(4) . .
O5 W3 O13 85.1(3) . .
O10 W3 O13 84.6(3) . .
O7 W3 O13 73.2(3) . .
O12 W3 O13 73.7(3) . .
O15 W4 O10 103.0(5) . 2_655
O15 W4 O9 102.9(5) . .
O10 W4 O9 85.9(4) 2_655 .
O15 W4 O2 99.6(5) . 2_655
O10 W4 O2 90.2(4) 2_655 2_655
O9 W4 O2 157.5(4) . 2_655
O15 W4 O2 99.6(5) . .
O10 W4 O2 157.4(4) 2_655 .
O9 W4 O2 88.2(4) . .
O2 W4 O2 87.0(6) 2_655 .
O15 W4 O4 169.7(5) . .
O10 W4 O4 84.7(3) 2_655 .
O9 W4 O4 84.4(3) . .
O2 W4 O4 73.2(3) 2_655 .
O2 W4 O4 73.0(3) . .
O4 Si1 O13 109.5(3) . 2_655
O4 Si1 O13 109.5(3) . .
O13 Si1 O13 109.5(3) 2_655 .
O4 Si1 O13 109.5(3) . 3_665
O13 Si1 O13 109.5(3) 2_655 3_665
O13 Si1 O13 109.5(3) . 3_665
C2 N1 N2 108.8(17) . .
W1 O1 W1 150.2(5) 3_665 .
W4 O2 W4 122.4(5) 3_665 .
Si1 O4 W4 124.3(3) . .
Si1 O4 W4 124.3(3) . 3_665
W4 O4 W4 91.3(4) . 3_665
Si1 O4 W4 124.3(3) . 2_655
W4 O4 W4 91.3(4) . 2_655
W4 O4 W4 91.3(4) 3_665 2_655
W3 O5 W2 151.6(5) . 3_665
W2 O7 W3 121.9(5) . .
W4 O9 W2 151.5(5) . .
W4 O10 W3 151.9(5) 3_665 .
W2 O11 W1 121.2(4) . .
W1 O12 W3 120.4(4) . .
Si1 O13 W1 124.3(5) . .
Si1 O13 W2 124.3(4) . .
W1 O13 W2 92.0(3) . .
Si1 O13 W3 123.7(4) . .
W1 O13 W3 91.6(3) . .
W2 O13 W3 91.4(3) . .
N2 C1 C5 108.5(13) . .
C3 N2 N1 110.3(15) . .
C3 N2 C1 122.3(13) . .
N1 N2 C1 126.4(15) . .
N1 C2 N3 103.4(16) . .
N2 C3 N3 101.2(15) . .
C7 C4 C6 117.5(17) . .
C7 C4 C5 121.0(15) . .
C6 C4 C5 121.1(13) . .
C2 N3 C3 116.3(17) . .
O16 C5 C11 107.3(14) . .
O16 C5 C1 106.7(17) . .
C11 C5 C1 107.0(14) . .
O16 C5 C4 110.6(12) . .
C11 C5 C4 113.6(18) . .
C1 C5 C4 111.3(13) . .
C8 C6 C4 121.8(17) . .
C4 C7 C9 124.3(19) . .
C4 C7 F2 121.0(19) . .
C9 C7 F2 114.7(18) . .
C6 C8 C10 117(2) . .
C7 C9 C10 117(2) . .
C9 C10 F1 122(3) . .
C9 C10 C8 123(2) . .
F1 C10 C8 116(3) . .
N6 C11 C5 111.7(16) . .
N6 C13 N5 100(3) . .
C12 N5 C13 106(3) . .
N5 C12 N4 118(4) . .
C12 N4 N6 104(3) . .
C13 N6 N4 111(3) . .
C13 N6 C11 124.3(18) . .
N4 N6 C11 124(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 O14 1.706(9) .
W1 O1 1.905(8) 2_655
W1 O1 1.910(8) .
W1 O12 1.924(9) .
W1 O11 1.924(9) .
W1 O13 2.322(8) .
W2 O8 1.706(10) .
W2 O9 1.906(9) .
W2 O7 1.907(9) .
W2 O5 1.910(9) 2_655
W2 O11 1.922(9) .
W2 O13 2.338(8) .
W3 O6 1.701(9) .
W3 O5 1.897(9) .
W3 O10 1.910(9) .
W3 O7 1.923(9) .
W3 O12 1.928(9) .
W3 O13 2.341(8) .
W4 O15 1.708(10) .
W4 O10 1.880(9) 2_655
W4 O9 1.904(9) .
W4 O2 1.911(9) 2_655
W4 O2 1.921(9) .
W4 O4 2.347(7) .
Si1 O4 1.629(13) .
Si1 O13 1.630(8) 2_655
Si1 O13 1.630(8) .
Si1 O13 1.630(8) 3_665
N1 C2 1.31(2) .
N1 N2 1.38(2) .
O1 W1 1.905(8) 3_665
O2 W4 1.912(9) 3_665
O4 W4 2.347(7) 3_665
O4 W4 2.347(7) 2_655
O5 W2 1.910(9) 3_665
O10 W4 1.880(9) 3_665
C1 N2 1.47(2) .
C1 C5 1.53(2) .
N2 C3 1.32(2) .
F2 C7 1.35(2) .
C2 N3 1.32(3) .
C3 N3 1.34(2) .
O16 C5 1.410(19) .
C4 C7 1.34(2) .
C4 C6 1.40(2) .
C4 C5 1.55(3) .
C5 C11 1.52(2) .
C6 C8 1.35(3) .
C7 C9 1.34(3) .
F1 C10 1.39(3) .
C8 C10 1.39(3) .
C9 C10 1.38(3) .
C11 N6 1.46(3) .
C13 N6 1.34(4) .
C13 N5 1.48(3) .
N5 C12 1.20(4) .
C12 N4 1.26(4) .
N4 N6 1.36(3) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
O13 Si1 O4 W4 59.3(3) 2_655 . . .
O13 Si1 O4 W4 -60.7(3) . . . .
O13 Si1 O4 W4 179.3(3) 3_665 . . .
O13 Si1 O4 W4 179.3(3) 2_655 . . 3_665
O13 Si1 O4 W4 59.3(3) . . . 3_665
O13 Si1 O4 W4 -60.7(3) 3_665 . . 3_665
O13 Si1 O4 W4 -60.7(3) 2_655 . . 2_655
O13 Si1 O4 W4 179.3(3) . . . 2_655
O13 Si1 O4 W4 59.3(3) 3_665 . . 2_655
O6 W3 O5 W2 -129.5(11) . . . 3_665
O10 W3 O5 W2 -27.4(11) . . . 3_665
O7 W3 O5 W2 48.9(17) . . . 3_665
O12 W3 O5 W2 131.2(11) . . . 3_665
O13 W3 O5 W2 57.6(11) . . . 3_665
O4 Si1 O13 W1 179.9(3) . . . .
O13 Si1 O13 W1 59.9(5) 2_655 . . .
O13 Si1 O13 W1 -60.1(5) 3_665 . . .
O4 Si1 O13 W2 58.9(5) . . . .
O13 Si1 O13 W2 -61.1(8) 2_655 . . .
O13 Si1 O13 W2 179.0(3) 3_665 . . .
O4 Si1 O13 W3 -60.4(5) . . . .
O13 Si1 O13 W3 179.6(3) 2_655 . . .
O13 Si1 O13 W3 59.7(8) 3_665 . . .
C2 N1 N2 C3 -1(2) . . . .
C2 N1 N2 C1 168.1(16) . . . .
C5 C1 N2 C3 95.2(18) . . . .
C5 C1 N2 N1 -73(2) . . . .
N2 N1 C2 N3 1.9(19) . . . .
N1 N2 C3 N3 -0.5(18) . . . .
C1 N2 C3 N3 -170.0(14) . . . .
N1 C2 N3 C3 -2(2) . . . .
N2 C3 N3 C2 2(2) . . . .
N2 C1 C5 O16 73.5(17) . . . .
N2 C1 C5 C11 -171.9(16) . . . .
N2 C1 C5 C4 -47.3(17) . . . .
C7 C4 C5 O16 -179.7(16) . . . .
C6 C4 C5 O16 -7(2) . . . .
C7 C4 C5 C11 59(2) . . . .
C6 C4 C5 C11 -127.7(15) . . . .
C7 C4 C5 C1 -61.4(19) . . . .
C6 C4 C5 C1 111.5(16) . . . .
C7 C4 C6 C8 1(3) . . . .
C5 C4 C6 C8 -171.7(17) . . . .
C6 C4 C7 C9 3(3) . . . .
C5 C4 C7 C9 175.7(18) . . . .
C6 C4 C7 F2 -178.4(15) . . . .
C5 C4 C7 F2 -5(2) . . . .
C4 C6 C8 C10 -3(3) . . . .
C4 C7 C9 C10 -4(3) . . . .
F2 C7 C9 C10 176.9(18) . . . .
C7 C9 C10 F1 -177.9(19) . . . .
C7 C9 C10 C8 2(3) . . . .
C6 C8 C10 C9 2(3) . . . .
C6 C8 C10 F1 -178.5(18) . . . .
O16 C5 C11 N6 -70(2) . . . .
C1 C5 C11 N6 175.7(18) . . . .
C4 C5 C11 N6 52(2) . . . .
N6 C13 N5 C12 -10(4) . . . .
C13 N5 C12 N4 9(5) . . . .
N5 C12 N4 N6 -3(5) . . . .
N5 C13 N6 N4 8(4) . . . .
N5 C13 N6 C11 -179.3(19) . . . .
C12 N4 N6 C13 -4(4) . . . .
C12 N4 N6 C11 -177(2) . . . .
C5 C11 N6 C13 -100(3) . . . .
C5 C11 N6 N4 72(3) . . . .
