#------------------------------------------------------------------------------
#$Date: 2019-04-17 04:34:03 +0300 (Wed, 17 Apr 2019) $
#$Revision: 214664 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/26/7232611.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_7232611
loop_
_publ_author_name
'Wu, Yingying'
'Li, Xuefei'
'Liu, Ying'
'Xiao, Ge'
'Huang, Yijiao'
'Li, Yamin'
'Dang, Dongbin'
'Bai, Yan'
_publ_section_title
;
 Three novel polyoxometalate-based inorganic--organic hybrid materials
 based on 2,6-bis(1,2,4-triazol-1-yl)pyridine
;
_journal_issue                   21
_journal_name_full               'RSC Advances'
_journal_page_first              11932
_journal_paper_doi               10.1039/C9RA01451A
_journal_volume                  9
_journal_year                    2019
_chemical_formula_sum            'C18 H16 Co N14 O17 P0 W5'
_chemical_formula_weight         1678.63
_space_group_crystal_system      orthorhombic
_space_group_IT_number           66
_space_group_name_Hall           '-C 2 2c'
_space_group_name_H-M_alt        'C c c m'
_symmetry_space_group_name_Hall  '-C 2 2c'
_symmetry_space_group_name_H-M   'C c c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-02-01 deposited with the CCDC.    2019-04-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.0024(8)
_cell_length_b                   21.9573(13)
_cell_length_c                   22.2526(14)
_cell_measurement_reflns_used    3687
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.584
_cell_volume                     6353.1(7)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Apex-II CCD detector diffractometer'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0547
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            15772
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.820
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    18.643
_exptl_absorpt_correction_T_max  0.129
_exptl_absorpt_correction_T_min  0.059
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.510
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       granular
_exptl_crystal_F_000             6040
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.460
_refine_diff_density_min         -1.822
_refine_diff_density_rms         0.211
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         2897
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0305
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0277P)²+31.3472P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0621
_refine_ls_wR_factor_ref         0.0651
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2359
_reflns_number_total             2897
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9ra01451a2.cif
_cod_data_source_block           l
_cod_database_code               7232611
_shelx_shelxl_version_number     2014/7
_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'
'-x, -y, z'
'-x, y, -z+1/2'
'x, -y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x, -y, z-1/2'
'-x, y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
'-x+1/2, y+1/2, 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
W1 W 0.18728(4) 0.07947(2) 0.0000 0.02286(13) Uani 1 2 d S T P
W2 W 0.14162(3) -0.02096(2) -0.10434(2) 0.02624(11) Uani 1 1 d . . .
W3 W -0.09526(4) 0.12312(2) 0.0000 0.02666(14) Uani 1 2 d S T P
W4 W 0.31641(4) -0.04821(2) 0.0000 0.03100(15) Uani 1 2 d S T P
Co1 Co 0.0000 0.5000 0.2500 0.0259(5) Uani 1 4 d S T P
O1 O 0.2298(6) 0.1539(3) 0.0000 0.0251(19) Uani 1 2 d S T P
O2 O 0.1463(6) -0.0195(3) 0.0000 0.0221(18) Uani 1 2 d S T P
O3 O 0.3185(6) 0.0401(4) 0.0000 0.032(2) Uani 1 2 d S T P
O4 O 0.1754(4) 0.0623(2) 0.0834(2) 0.0265(13) Uani 1 1 d . . .
O5 O 0.0426(7) 0.0968(3) 0.0000 0.030(2) Uani 1 2 d S T P
O6 O 0.0000 0.0000 -0.1014(3) 0.0250(19) Uani 1 2 d S T P
O7 O -0.1062(4) 0.1020(2) 0.0832(2) 0.0278(14) Uani 1 1 d . . .
O8 O 0.2855(4) -0.0403(3) 0.0842(3) 0.0310(14) Uani 1 1 d . . .
O9 O 0.1578(5) -0.0234(3) -0.1798(3) 0.0416(18) Uani 1 1 d . . .
O10 O -0.2465(7) 0.1239(4) 0.0000 0.035(2) Uani 1 2 d S T P
O11 O -0.0782(7) 0.1994(4) 0.0000 0.038(2) Uani 1 2 d S T P
O12 O 0.4421(7) -0.0678(4) 0.0000 0.055(3) Uani 1 2 d S T P
O1W O 0.0000 0.5000 0.1457(4) 0.057(3) Uani 1 2 d S T P
N1 N 0.1109(6) 0.4327(3) 0.2473(3) 0.0326(19) Uani 1 1 d . . .
N2 N 0.1393(5) 0.2606(3) 0.0679(3) 0.0245(16) Uani 1 1 d . . .
N3 N 0.0595(5) 0.2385(3) 0.1507(3) 0.0274(17) Uani 1 1 d . . .
N4 N 0.0239(7) 0.2943(4) 0.1349(3) 0.043(2) Uani 1 1 d . . .
N5 N 0.1915(5) 0.3498(3) 0.2712(3) 0.0279(17) Uani 1 1 d . . .
N6 N 0.2256(7) 0.3641(4) 0.2145(3) 0.042(2) Uani 1 1 d . . .
N7 N 0.0000 0.2380(4) 0.2500 0.025(2) Uani 1 2 d S T P
N8 N 0.2500 0.2500 0.2720(5) 0.029(2) Uani 1 2 d S T P
C1 C 0.1228(7) 0.3909(4) 0.2887(4) 0.030(2) Uani 1 1 d . . .
H1A H 0.0881 0.3902 0.3252 0.036 Uiso 1 1 calc R U .
C2 C 0.1760(9) 0.4143(4) 0.2029(5) 0.047(3) Uani 1 1 d . . .
H2A H 0.1844 0.4358 0.1672 0.056 Uiso 1 1 calc R U .
C3 C 0.1281(7) 0.2197(4) 0.1116(4) 0.035(2) Uani 1 1 d . . .
H3A H 0.1639 0.1831 0.1142 0.043 Uiso 1 1 calc R U .
C4 C 0.0743(8) 0.3048(4) 0.0845(4) 0.036(2) Uani 1 1 d . . .
H4A H 0.0653 0.3402 0.0622 0.043 Uiso 1 1 calc R U .
C5 C 0.0251(7) 0.2048(4) 0.2023(4) 0.028(2) Uani 1 1 d . . .
C6 C 0.0253(7) 0.1426(4) 0.1987(4) 0.036(2) Uani 1 1 d . . .
H6A H 0.0417 0.1225 0.1632 0.044 Uiso 1 1 calc R U .
C7 C 0.0000 0.1111(6) 0.2500 0.036(3) Uani 1 2 d S T P
H7A H 0.0000 0.0687 0.2500 0.044 Uiso 1 2 calc R U P
C8 C 0.2239(7) 0.2983(4) 0.3053(4) 0.027(2) Uani 1 1 d . . .
C9 C 0.2260(7) 0.3020(4) 0.3660(4) 0.036(2) Uani 1 1 d . . .
H9A H 0.2118 0.3385 0.3856 0.043 Uiso 1 1 calc R U .
C10 C 0.2500 0.2500 0.3982(6) 0.037(3) Uani 1 2 d S T P
H10A H 0.2500 0.2500 0.4400 0.045 Uiso 1 2 calc R U P
Co2 Co 0.2500 0.2500 0.0000 0.0147(5) Uani 1 4 d S T P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
O O 0.0106 0.0060 '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'
Co Co 0.3494 0.9721 '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'
C C 0.0033 0.0016 '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
O1 W1 O4 102.34(16) . 10
O1 W1 O4 102.34(16) . .
O4 W1 O4 155.3(3) 10 .
O1 W1 O3 98.1(4) . .
O4 W1 O3 89.05(18) 10 .
O4 W1 O3 89.05(18) . .
O1 W1 O5 97.3(4) . .
O4 W1 O5 87.66(18) 10 .
O4 W1 O5 87.66(18) . .
O3 W1 O5 164.6(3) . .
O1 W1 O2 175.1(3) . .
O4 W1 O2 77.77(16) 10 .
O4 W1 O2 77.77(16) . .
O3 W1 O2 76.9(3) . .
O5 W1 O2 87.6(3) . .
O9 W2 O7 104.3(3) . 9
O9 W2 O6 99.3(3) . .
O7 W2 O6 89.06(19) 9 .
O9 W2 O4 103.9(3) . 10
O7 W2 O4 151.7(2) 9 10
O6 W2 O4 88.99(18) . 10
O9 W2 O8 95.8(3) . 10
O7 W2 O8 88.4(2) 9 10
O6 W2 O8 164.8(3) . 10
O4 W2 O8 86.2(2) 10 10
O9 W2 O2 171.3(3) . .
O7 W2 O2 76.8(2) 9 .
O6 W2 O2 89.3(3) . .
O4 W2 O2 74.9(2) 10 .
O8 W2 O2 75.5(3) 10 .
O11 W3 O5 100.4(4) . .
O11 W3 O7 104.45(16) . 10
O5 W3 O7 89.80(19) . 10
O11 W3 O7 104.45(16) . .
O5 W3 O7 89.80(19) . .
O7 W3 O7 150.7(3) 10 .
O11 W3 O10 97.0(4) . .
O5 W3 O10 162.6(3) . .
O7 W3 O10 85.86(18) 10 .
O7 W3 O10 85.86(18) . .
O11 W3 O2 171.3(4) . 9
O5 W3 O2 88.4(3) . 9
O7 W3 O2 75.34(16) 10 9
O7 W3 O2 75.34(16) . 9
O10 W3 O2 74.3(3) . 9
O12 W4 O10 103.9(4) . 9
O12 W4 O8 103.00(17) . .
O10 W4 O8 88.80(18) 9 .
O12 W4 O8 103.00(17) . 10
O10 W4 O8 88.80(18) 9 10
O8 W4 O8 153.7(3) . 10
O12 W4 O3 103.9(4) . .
O10 W4 O3 152.1(4) 9 .
O8 W4 O3 84.99(18) . .
O8 W4 O3 84.99(18) 10 .
O12 W4 O2 178.8(4) . .
O10 W4 O2 77.2(3) 9 .
O8 W4 O2 76.96(17) . .
O8 W4 O2 76.96(17) 10 .
O3 W4 O2 74.9(3) . .
N1 Co1 N1 176.7(4) 4_565 3
N1 Co1 N1 88.6(4) 4_565 2_565
N1 Co1 N1 91.5(4) 3 2_565
N1 Co1 N1 91.5(4) 4_565 .
N1 Co1 N1 88.6(4) 3 .
N1 Co1 N1 176.7(4) 2_565 .
N1 Co1 O1W 91.6(2) 4_565 .
N1 Co1 O1W 91.6(2) 3 .
N1 Co1 O1W 88.4(2) 2_565 .
N1 Co1 O1W 88.4(2) . .
N1 Co1 O1W 88.4(2) 4_565 3
N1 Co1 O1W 88.4(2) 3 3
N1 Co1 O1W 91.6(2) 2_565 3
N1 Co1 O1W 91.6(2) . 3
O1W Co1 O1W 180.0 . 3
W1 O1 Co2 168.4(5) . .
W1 O2 W4 92.1(3) . .
W1 O2 W2 91.13(18) . 10
W4 O2 W2 91.23(19) . 10
W1 O2 W2 91.13(18) . .
W4 O2 W2 91.24(19) . .
W2 O2 W2 176.6(4) 10 .
W1 O2 W3 177.5(4) . 9
W4 O2 W3 90.4(3) . 9
W2 O2 W3 88.81(18) 10 9
W2 O2 W3 88.81(18) . 9
W1 O3 W4 116.0(4) . .
W1 O4 W2 116.1(3) . 10
W3 O5 W1 173.5(5) . .
W2 O6 W2 176.1(5) . 2
W2 O7 W3 119.0(3) 9 .
W4 O8 W2 116.1(3) . 10
W4 O10 W3 118.1(4) 9 .
C1 N1 C2 103.3(7) . .
C1 N1 Co1 124.3(6) . .
C2 N1 Co1 131.8(6) . .
C3 N2 C4 102.6(7) . .
C3 N2 Co2 121.7(6) . .
C4 N2 Co2 135.4(6) . .
C3 N3 N4 110.2(7) . .
C3 N3 C5 125.3(8) . .
N4 N3 C5 124.5(7) . .
C4 N4 N3 102.1(7) . .
C1 N5 N6 109.2(7) . .
C1 N5 C8 125.7(8) . .
N6 N5 C8 125.1(7) . .
C2 N6 N5 102.5(7) . .
C5 N7 C5 113.5(10) 3 .
C8 N8 C8 112.7(11) 6 .
N1 C1 N5 110.5(8) . .
N1 C1 H1A 124.7 . .
N5 C1 H1A 124.7 . .
N6 C2 N1 114.5(8) . .
N6 C2 H2A 122.7 . .
N1 C2 H2A 122.7 . .
N3 C3 N2 110.2(8) . .
N3 C3 H3A 124.9 . .
N2 C3 H3A 124.9 . .
N4 C4 N2 114.9(8) . .
N4 C4 H4A 122.5 . .
N2 C4 H4A 122.5 . .
N7 C5 C6 126.5(8) . .
N7 C5 N3 115.6(8) . .
C6 C5 N3 117.8(8) . .
C5 C6 C7 116.9(9) . .
C5 C6 H6A 121.5 . .
C7 C6 H6A 121.5 . .
C6 C7 C6 119.6(13) 3 .
C6 C7 H7A 120.2 3 .
C6 C7 H7A 120.2 . .
N8 C8 C9 126.6(9) . .
N8 C8 N5 114.2(8) . .
C9 C8 N5 119.2(8) . .
C8 C9 C10 118.1(10) . .
C8 C9 H9A 120.9 . .
C10 C9 H9A 120.9 . .
C9 C10 C9 117.6(13) . 6
C9 C10 H10A 121.2 . .
C9 C10 H10A 121.2 6 .
N2 Co2 N2 180.0(5) 10 6
N2 Co2 N2 88.0(4) 10 13
N2 Co2 N2 92.0(4) 6 13
N2 Co2 N2 92.0(4) 10 .
N2 Co2 N2 88.0(4) 6 .
N2 Co2 N2 180.0(3) 13 .
N2 Co2 O1 91.4(2) 10 .
N2 Co2 O1 88.6(2) 6 .
N2 Co2 O1 88.6(2) 13 .
N2 Co2 O1 91.4(2) . .
N2 Co2 O1 88.6(2) 10 13
N2 Co2 O1 91.4(2) 6 13
N2 Co2 O1 91.4(2) 13 13
N2 Co2 O1 88.6(2) . 13
O1 Co2 O1 180.0 . 13
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 O1 1.725(7) .
W1 O4 1.899(5) 10
W1 O4 1.899(5) .
W1 O3 1.912(8) .
W1 O5 1.920(9) .
W1 O2 2.237(7) .
W2 O9 1.693(6) .
W2 O7 1.898(5) 9
W2 O6 1.8992(5) .
W2 O4 1.938(5) 10
W2 O8 1.970(6) 10
W2 O2 2.3230(4) .
W3 O11 1.689(8) .
W3 O5 1.883(9) .
W3 O7 1.913(6) 10
W3 O7 1.913(6) .
W3 O10 1.967(9) .
W3 O2 2.370(7) 9
W4 O12 1.689(9) .
W4 O10 1.895(8) 9
W4 O8 1.924(6) .
W4 O8 1.924(6) 10
W4 O3 1.940(8) .
W4 O2 2.299(8) .
Co1 N1 2.066(7) 4_565
Co1 N1 2.066(7) 3
Co1 N1 2.066(7) 2_565
Co1 N1 2.066(7) .
Co1 O1W 2.320(10) .
Co1 O1W 2.320(10) 3
O1 Co2 2.127(7) .
O2 W2 2.3229(4) 10
O2 W3 2.370(7) 9
O4 W2 1.938(5) 10
O6 W2 1.8993(5) 2
O7 W2 1.898(5) 9
O8 W2 1.970(6) 10
O10 W4 1.895(8) 9
N1 C1 1.308(10) .
N1 C2 1.363(12) .
N2 C3 1.333(11) .
N2 C4 1.340(11) .
N2 Co2 2.099(7) .
N3 C3 1.313(11) .
N3 N4 1.356(10) .
N3 C5 1.438(10) .
N4 C4 1.318(11) .
N5 C1 1.329(11) .
N5 N6 1.375(10) .
N5 C8 1.424(10) .
N6 C2 1.302(12) .
N7 C5 1.328(10) 3
N7 C5 1.328(10) .
N8 C8 1.337(10) 6
N8 C8 1.337(10) .
C1 H1A 0.9300 .
C2 H2A 0.9300 .
C3 H3A 0.9300 .
C4 H4A 0.9300 .
C5 C6 1.369(12) .
C6 C7 1.375(11) .
C6 H6A 0.9300 .
C7 C6 1.375(11) 3
C7 H7A 0.9300 .
C8 C9 1.355(12) .
C9 C10 1.384(11) .
C9 H9A 0.9300 .
C10 C9 1.384(11) 6
C10 H10A 0.9300 .
Co2 N2 2.099(7) 10
Co2 N2 2.099(7) 6
Co2 N2 2.099(7) 13
Co2 O1 2.127(7) 13
