#------------------------------------------------------------------------------
#$Date: 2018-06-20 18:18:31 +0300 (Wed, 20 Jun 2018) $
#$Revision: 208564 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/09/7230963.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_7230963
loop_
_publ_author_name
'Wang, Xiuli'
'Bai, Xue'
'Lin, Hongyan'
'Sun, Junjun'
'Wang, Xiang'
'Liu, Guocheng'
_publ_section_title
;
 A series of new polyoxometalate-based metal--organic complexes with
 different rigid pyridyl-bis(triazole) ligands: assembly, structures and
 electrochemical properties
;
_journal_issue                   40
_journal_name_full               'RSC Advances'
_journal_page_first              22676
_journal_paper_doi               10.1039/C8RA03277G
_journal_volume                  8
_journal_year                    2018
_chemical_formula_sum            'C18 H44 Co3 Mo8 N14 O42'
_chemical_formula_weight         2072.98
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-06-11 deposited with the CCDC.
2018-06-12 downloaded from the CCDC.
;
_cell_angle_alpha                107.4950(10)
_cell_angle_beta                 113.3740(10)
_cell_angle_gamma                102.0980(10)
_cell_formula_units_Z            1
_cell_length_a                   10.9150(4)
_cell_length_b                   12.4010(5)
_cell_length_c                   12.5140(5)
_cell_measurement_reflns_used    1427
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.8704
_cell_measurement_theta_min      2.2806
_cell_volume                     1374.33(10)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker Smart'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'XT, VERSION 2014/5'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker Smart Apex II'
_diffrn_measurement_method       'w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_unetI/netI     0.0782
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7755
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         25.334
_diffrn_reflns_theta_min         1.858
_exptl_absorpt_coefficient_mu    2.758
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6212
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    2.505
_exptl_crystal_description       block
_exptl_crystal_F_000             1003
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.170
_refine_diff_density_max         1.022
_refine_diff_density_min         -0.849
_refine_diff_density_rms         0.186
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         4967
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0770
_refine_ls_R_factor_gt           0.0441
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0389P)²+1.0639P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0864
_refine_ls_wR_factor_ref         0.0988
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3550
_reflns_number_total             4967
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8ra03277g2.cif
_cod_data_source_block           3
_cod_original_cell_volume        1374.33(9)
_cod_database_code               7230963
_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.
;
_shelx_estimated_absorpt_t_min   0.622
_shelx_estimated_absorpt_t_max   0.651
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Co1 Co 0.77685(11) 1.04146(10) 0.62774(10) 0.0171(2) Uani 1 1 d . . .
Co2 Co 0.5000 0.5000 0.5000 0.0224(4) Uani 1 2 d S . P
Mo1 Mo 0.59533(7) 0.93550(6) 0.93468(6) 0.01387(17) Uani 1 1 d . . .
Mo2 Mo 0.49558(7) 1.03619(6) 0.70281(6) 0.01400(17) Uani 1 1 d . . .
Mo3 Mo 0.24050(7) 0.82378(6) 0.76174(6) 0.01456(17) Uani 1 1 d . . .
Mo4 Mo 0.70042(8) 1.24532(6) 0.99709(6) 0.01801(18) Uani 1 1 d . . .
O1 O 0.3320(6) 1.0002(5) 0.5725(5) 0.0202(12) Uani 1 1 d . . .
O2 O 0.6230(5) 1.0944(5) 0.6640(5) 0.0167(12) Uani 1 1 d . . .
O3 O 0.6750(5) 1.0519(5) 0.8862(5) 0.0154(12) Uani 1 1 d . . .
O4 O 0.8149(6) 1.3049(6) 0.9507(5) 0.0323(15) Uani 1 1 d . . .
O5 O 0.5165(5) 1.1740(5) 0.8289(5) 0.0185(12) Uani 1 1 d . . .
O6 O 0.6676(6) 1.3651(5) 1.0718(5) 0.0305(15) Uani 1 1 d . . .
O7 O 0.4296(5) 0.8781(5) 0.9532(5) 0.0158(11) Uani 1 1 d . . .
O8 O 0.6108(6) 0.8061(5) 0.8566(5) 0.0252(14) Uani 1 1 d . . .
O9 O 0.2337(6) 0.6850(5) 0.6720(5) 0.0261(13) Uani 1 1 d . . .
O10 O 0.4107(5) 0.9238(5) 0.7682(5) 0.0161(12) Uani 1 1 d . . .
O11 O 0.1049(6) 0.8476(5) 0.6581(5) 0.0236(13) Uani 1 1 d . . .
O12 O 0.8388(5) 1.2304(5) 1.1430(5) 0.0207(12) Uani 1 1 d . . .
O13 O 0.7282(5) 0.9886(5) 1.0926(5) 0.0179(12) Uani 1 1 d . . .
N1 N 0.5004(7) 0.6741(6) 0.5256(7) 0.0216(16) Uani 1 1 d . . .
N2 N 0.6597(7) 0.5722(6) 0.4491(7) 0.0238(16) Uani 1 1 d . . .
N3 N 0.5235(7) 0.8664(6) 0.6106(6) 0.0154(14) Uani 1 1 d . . .
N4 N 0.6291(7) 0.8656(6) 0.5764(6) 0.0160(14) Uani 1 1 d . . .
N5 N 0.7522(7) 0.5466(6) 0.4076(7) 0.0262(17) Uani 1 1 d . . .
H5 H 0.7587 0.4764 0.3836 0.031 Uiso 1 1 calc R U .
N6 N 0.7956(7) 0.7398(6) 0.4538(6) 0.0212(15) Uani 1 1 d . . .
N7 N 1.1110(7) 0.7790(6) 0.3405(6) 0.0208(15) Uani 1 1 d . . .
C1 C 0.4504(8) 0.7513(7) 0.5781(7) 0.0194(18) Uani 1 1 d . . .
H1 H 0.3725 0.7271 0.5906 0.023 Uiso 1 1 calc R U .
C2 C 0.6114(8) 0.7503(7) 0.5261(7) 0.0183(18) Uani 1 1 d . . .
C3 C 0.6916(9) 0.6906(7) 0.4764(8) 0.0202(18) Uani 1 1 d . . .
C4 C 0.8316(9) 0.6454(8) 0.4094(8) 0.0219(19) Uani 1 1 d . . .
C5 C 0.9393(8) 0.6510(7) 0.3678(8) 0.0192(18) Uani 1 1 d . . .
C6 C 0.9723(9) 0.5515(8) 0.3190(9) 0.030(2) Uani 1 1 d . . .
H6 H 0.9267 0.4756 0.3125 0.036 Uiso 1 1 calc R U .
C7 C 1.1382(9) 0.6806(8) 0.2905(9) 0.029(2) Uani 1 1 d . . .
H7 H 1.2040 0.6897 0.2611 0.034 Uiso 1 1 calc R U .
C8 C 1.0120(8) 0.7614(7) 0.3764(7) 0.0206(18) Uani 1 1 d . . .
H8 H 0.9901 0.8280 0.4095 0.025 Uiso 1 1 calc R U .
C9 C 1.0743(10) 0.5680(8) 0.2806(10) 0.037(2) Uani 1 1 d . . .
H9 H 1.0993 0.5034 0.2482 0.044 Uiso 1 1 calc R U .
O1W O 0.9291(6) 0.9845(5) 0.5985(6) 0.0283(14) Uani 1 1 d . . .
H1WA H 1.0071 0.9909 0.6584 0.034 Uiso 1 1 d R U .
H1WB H 0.8954 0.9111 0.5430 0.034 Uiso 1 1 d R U .
O2W O 0.8836(6) 1.0581(5) 0.8165(5) 0.0277(14) Uani 1 1 d . . .
H2WA H 0.9663 1.1149 0.8660 0.033 Uiso 1 1 d R U .
H2WB H 0.8299 1.0694 0.8494 0.033 Uiso 1 1 d R U .
O3W O 0.3339(6) 0.4260(6) 0.3118(6) 0.0402(17) Uani 1 1 d . . .
H3WA H 0.3250 0.4440 0.2495 0.048 Uiso 1 1 d R U .
H3WB H 0.2607 0.3630 0.2839 0.048 Uiso 1 1 d R U .
O4W O 0.8553(8) 0.7611(7) 0.0371(7) 0.073(3) Uani 1 1 d . . .
H4WA H 0.7855 0.7733 -0.0130 0.087 Uiso 1 1 d R U .
H4WB H 0.8595 0.6952 -0.0048 0.109 Uiso 1 1 d R U .
O5W O 0.2734(15) 0.4964(11) 0.1108(11) 0.154(5) Uani 1 1 d . U .
H5WA H 0.2619 0.5638 0.1322 0.185 Uiso 1 1 d R U .
H5WB H 0.3399 0.5045 0.0911 0.185 Uiso 1 1 d R U .
O6W O 0.7475(13) 0.7953(14) 0.1974(12) 0.163(5) Uani 1 1 d . U .
H6WA H 0.6839 0.8264 0.1902 0.195 Uiso 1 1 d R U .
H6WB H 0.8151 0.8427 0.1962 0.195 Uiso 1 1 d R U .
O7W O 0.5489(14) 0.5507(14) 0.1398(11) 0.189(7) Uani 1 1 d . U .
H7WA H 0.6139 0.6172 0.1619 0.226 Uiso 1 1 d R U .
H7WB H 0.5816 0.4945 0.1271 0.226 Uiso 1 1 d R U .
O8W O 0.8911(7) 0.8056(7) 0.8065(7) 0.062(2) Uani 1 1 d . . .
H8WA H 0.8917 0.8185 0.8774 0.074 Uiso 1 1 d R U .
H8WB H 0.9632 0.7867 0.8121 0.074 Uiso 1 1 d R U .
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'
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'
Mo Mo -1.6832 0.6857 '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'
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
O1W Co1 O2 176.8(2) . .
O1W Co1 O2W 87.8(2) . .
O2 Co1 O2W 89.6(2) . .
O1W Co1 N7 90.4(2) . 2_776
O2 Co1 N7 91.7(2) . 2_776
O2W Co1 N7 99.1(2) . 2_776
O1W Co1 O1 87.4(2) . 2_676
O2 Co1 O1 95.03(19) . 2_676
O2W Co1 O1 172.2(2) . 2_676
N7 Co1 O1 87.1(2) 2_776 2_676
O1W Co1 N4 97.4(2) . .
O2 Co1 N4 80.7(2) . .
O2W Co1 N4 88.1(2) . .
N7 Co1 N4 169.6(2) 2_776 .
O1 Co1 N4 86.4(2) 2_676 .
O3W Co2 O3W 180.0 2_666 .
O3W Co2 N1 91.0(3) 2_666 2_666
O3W Co2 N1 89.0(3) . 2_666
O3W Co2 N1 89.0(3) 2_666 .
O3W Co2 N1 91.0(3) . .
N1 Co2 N1 180.0 2_666 .
O3W Co2 N2 92.3(3) 2_666 2_666
O3W Co2 N2 87.7(3) . 2_666
N1 Co2 N2 76.7(2) 2_666 2_666
N1 Co2 N2 103.3(2) . 2_666
O3W Co2 N2 87.7(3) 2_666 .
O3W Co2 N2 92.3(3) . .
N1 Co2 N2 103.3(2) 2_666 .
N1 Co2 N2 76.7(2) . .
N2 Co2 N2 180.0(3) 2_666 .
O8 Mo1 O13 103.9(2) . .
O8 Mo1 O3 104.9(2) . .
O13 Mo1 O3 100.8(2) . .
O8 Mo1 O7 103.9(3) . .
O13 Mo1 O7 98.7(2) . .
O3 Mo1 O7 139.9(2) . .
O8 Mo1 O10 96.7(2) . .
O13 Mo1 O10 159.3(2) . .
O3 Mo1 O10 75.41(19) . .
O7 Mo1 O10 73.98(19) . .
O8 Mo1 O7 179.4(2) . 2_677
O13 Mo1 O7 76.4(2) . 2_677
O3 Mo1 O7 75.44(19) . 2_677
O7 Mo1 O7 75.6(2) . 2_677
O10 Mo1 O7 82.89(18) . 2_677
O1 Mo2 O2 104.9(2) . .
O1 Mo2 O5 104.0(2) . .
O2 Mo2 O5 102.0(2) . .
O1 Mo2 O10 94.2(2) . .
O2 Mo2 O10 152.2(2) . .
O5 Mo2 O10 92.4(2) . .
O1 Mo2 N3 94.3(2) . .
O2 Mo2 N3 80.0(2) . .
O5 Mo2 N3 160.2(2) . .
O10 Mo2 N3 78.6(2) . .
O1 Mo2 O3 165.1(2) . .
O2 Mo2 O3 89.4(2) . .
O5 Mo2 O3 76.3(2) . .
O10 Mo2 O3 70.90(19) . .
N3 Mo2 O3 84.0(2) . .
O11 Mo3 O9 104.8(3) . .
O11 Mo3 O12 103.1(2) . 2_677
O9 Mo3 O12 97.0(2) . 2_677
O11 Mo3 O10 102.9(2) . .
O9 Mo3 O10 96.5(2) . .
O12 Mo3 O10 146.5(2) 2_677 .
O11 Mo3 O7 153.3(2) . .
O9 Mo3 O7 101.9(2) . .
O12 Mo3 O7 74.9(2) 2_677 .
O10 Mo3 O7 72.38(19) . .
O11 Mo3 O13 82.6(2) . 2_677
O9 Mo3 O13 172.5(2) . 2_677
O12 Mo3 O13 80.0(2) 2_677 2_677
O10 Mo3 O13 82.70(19) . 2_677
O7 Mo3 O13 70.75(18) . 2_677
O6 Mo4 O4 104.5(3) . .
O6 Mo4 O12 101.5(2) . .
O4 Mo4 O12 98.5(3) . .
O6 Mo4 O5 96.3(2) . .
O4 Mo4 O5 98.5(2) . .
O12 Mo4 O5 151.4(2) . .
O6 Mo4 O7 91.3(2) . 2_677
O4 Mo4 O7 163.6(2) . 2_677
O12 Mo4 O7 73.7(2) . 2_677
O5 Mo4 O7 83.8(2) . 2_677
O6 Mo4 O3 161.8(2) . .
O4 Mo4 O3 91.9(2) . .
O12 Mo4 O3 83.4(2) . .
O5 Mo4 O3 73.23(19) . .
O7 Mo4 O3 73.09(18) 2_677 .
Mo2 O1 Co1 144.7(3) . 2_676
Mo2 O2 Co1 135.8(3) . .
Mo1 O3 Mo2 107.7(2) . .
Mo1 O3 Mo4 114.1(2) . .
Mo2 O3 Mo4 91.50(17) . .
Mo2 O5 Mo4 115.4(2) . .
Mo1 O7 Mo3 104.8(2) . .
Mo1 O7 Mo4 151.3(3) . 2_677
Mo3 O7 Mo4 92.36(19) . 2_677
Mo1 O7 Mo1 104.4(2) . 2_677
Mo3 O7 Mo1 95.82(18) . 2_677
Mo4 O7 Mo1 96.28(17) 2_677 2_677
Mo3 O10 Mo2 148.7(3) . .
Mo3 O10 Mo1 105.3(2) . .
Mo2 O10 Mo1 105.5(2) . .
Mo3 O12 Mo4 114.1(3) 2_677 .
Mo1 O13 Mo3 116.7(2) . 2_677
C1 N1 C2 102.3(6) . .
C1 N1 Co2 138.3(5) . .
C2 N1 Co2 116.0(5) . .
C3 N2 N5 102.2(6) . .
C3 N2 Co2 113.0(5) . .
N5 N2 Co2 144.6(5) . .
C1 N3 N4 106.6(6) . .
C1 N3 Mo2 130.2(5) . .
N4 N3 Mo2 123.2(5) . .
C2 N4 N3 105.2(6) . .
C2 N4 Co1 138.7(5) . .
N3 N4 Co1 115.9(4) . .
C4 N5 N2 110.6(6) . .
C3 N6 C4 103.2(7) . .
C8 N7 C7 116.5(7) . .
C8 N7 Co1 119.4(5) . 2_776
C7 N7 Co1 124.0(5) . 2_776
N3 C1 N1 112.8(7) . .
N4 C2 N1 113.1(6) . .
N4 C2 C3 131.8(7) . .
N1 C2 C3 115.1(7) . .
N2 C3 N6 114.6(7) . .
N2 C3 C2 117.2(7) . .
N6 C3 C2 128.1(7) . .
N5 C4 N6 109.4(7) . .
N5 C4 C5 125.8(7) . .
N6 C4 C5 124.8(7) . .
C8 C5 C6 118.0(7) . .
C8 C5 C4 118.1(7) . .
C6 C5 C4 123.9(7) . .
C9 C6 C5 118.4(8) . .
N7 C7 C9 123.6(8) . .
N7 C8 C5 124.4(7) . .
C7 C9 C6 119.2(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O1W 2.053(5) .
Co1 O2 2.085(5) .
Co1 O2W 2.099(5) .
Co1 N7 2.134(7) 2_776
Co1 O1 2.135(5) 2_676
Co1 N4 2.152(7) .
Co2 O3W 2.071(6) 2_666
Co2 O3W 2.071(6) .
Co2 N1 2.084(6) 2_666
Co2 N1 2.084(6) .
Co2 N2 2.194(6) 2_666
Co2 N2 2.194(6) .
Mo1 O8 1.691(5) .
Mo1 O13 1.728(5) .
Mo1 O3 1.905(5) .
Mo1 O7 1.929(5) .
Mo1 O10 2.187(5) .
Mo1 O7 2.451(5) 2_677
Mo2 O1 1.722(5) .
Mo2 O2 1.737(5) .
Mo2 O5 1.841(5) .
Mo2 O10 2.054(5) .
Mo2 N3 2.224(6) .
Mo2 O3 2.268(5) .
Mo3 O11 1.688(5) .
Mo3 O9 1.717(6) .
Mo3 O12 1.917(5) 2_677
Mo3 O10 1.963(5) .
Mo3 O7 2.231(5) .
Mo3 O13 2.339(5) 2_677
Mo4 O6 1.692(5) .
Mo4 O4 1.701(6) .
Mo4 O12 1.945(5) .
Mo4 O5 2.006(5) .
Mo4 O7 2.260(5) 2_677
Mo4 O3 2.273(5) .
O1 Co1 2.135(5) 2_676
O7 Mo4 2.260(5) 2_677
O7 Mo1 2.451(5) 2_677
O12 Mo3 1.917(5) 2_677
O13 Mo3 2.339(5) 2_677
N1 C1 1.331(9) .
N1 C2 1.368(10) .
N2 C3 1.336(10) .
N2 N5 1.357(8) .
N3 C1 1.324(10) .
N3 N4 1.380(8) .
N4 C2 1.313(10) .
N5 C4 1.332(10) .
N6 C3 1.345(10) .
N6 C4 1.345(10) .
N7 C8 1.328(9) .
N7 C7 1.344(10) .
N7 Co1 2.134(7) 2_776
C2 C3 1.459(10) .
C4 C5 1.460(10) .
C5 C8 1.381(11) .
C5 C6 1.390(11) .
C6 C9 1.379(11) .
C7 C9 1.368(12) .
