#------------------------------------------------------------------------------
#$Date: 2018-06-20 17:18:31 +0200 (Wed 20 de Jun de 2018) $
#$Revision: 208564 $
#$URL: svn://www.crystallography.net/cod/cif/7/23/09/7230962.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_7230962
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 Mo8 N14 Ni3 O42'
_chemical_formula_weight         2072.32
_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                106.8430(10)
_cell_angle_beta                 113.5710(10)
_cell_angle_gamma                102.6890(10)
_cell_formula_units_Z            1
_cell_length_a                   10.8810(4)
_cell_length_b                   12.3290(5)
_cell_length_c                   12.4580(5)
_cell_measurement_reflns_used    5091
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.2960
_cell_measurement_theta_min      2.2838
_cell_volume                     1354.64(9)
_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 0.998
_diffrn_measured_fraction_theta_max 0.992
_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  0.0182
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10123
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         28.311
_diffrn_reflns_theta_min         1.967
_exptl_absorpt_coefficient_mu    2.922
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6203
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.540
_exptl_crystal_description       block
_exptl_crystal_F_000             1006
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.170
_refine_diff_density_max         0.856
_refine_diff_density_min         -0.977
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         6702
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0252
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0240P)²+1.7341P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0570
_refine_ls_wR_factor_ref         0.0594
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5915
_reflns_number_total             6702
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8ra03277g2.cif
_cod_data_source_block           4
_cod_original_cell_volume        1354.63(9)
_cod_database_code               7230962
_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   0.607
_shelx_estimated_absorpt_t_max   0.636
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
Ni1 Ni 0.77559(4) 1.03884(3) 0.62633(4) 0.01222(8) Uani 1 1 d . . .
Ni2 Ni 0.5000 0.5000 0.5000 0.01660(12) Uani 1 2 d S . P
Mo1 Mo 0.59547(3) 0.93469(2) 0.93610(2) 0.01096(6) Uani 1 1 d . . .
Mo2 Mo 0.49638(3) 1.03491(2) 0.70129(2) 0.01049(6) Uani 1 1 d . . .
Mo3 Mo 0.23799(3) 0.82329(2) 0.76089(2) 0.01140(6) Uani 1 1 d . . .
Mo4 Mo 0.70431(3) 1.24530(2) 0.99570(2) 0.01475(6) Uani 1 1 d . . .
O1 O 0.3328(2) 0.99864(19) 0.5698(2) 0.0159(4) Uani 1 1 d . . .
O2 O 0.6249(2) 1.09233(18) 0.6618(2) 0.0146(4) Uani 1 1 d . . .
O3 O 0.6764(2) 1.05077(18) 0.8855(2) 0.0136(4) Uani 1 1 d . . .
O4 O 0.8211(3) 1.3045(2) 0.9498(2) 0.0292(6) Uani 1 1 d . . .
O5 O 0.5196(2) 1.17457(18) 0.8263(2) 0.0156(4) Uani 1 1 d . . .
O6 O 0.6710(3) 1.3654(2) 1.0686(2) 0.0282(5) Uani 1 1 d . . .
O7 O 0.4271(2) 0.87750(18) 0.9537(2) 0.0138(4) Uani 1 1 d . . .
O8 O 0.6099(2) 0.8048(2) 0.8588(2) 0.0215(5) Uani 1 1 d . . .
O9 O 0.2290(2) 0.68310(19) 0.6710(2) 0.0202(5) Uani 1 1 d . . .
O10 O 0.4106(2) 0.92276(18) 0.76814(19) 0.0127(4) Uani 1 1 d . . .
O11 O 0.1026(2) 0.8476(2) 0.6549(2) 0.0236(5) Uani 1 1 d . . .
O12 O 0.8431(2) 1.23162(19) 1.1438(2) 0.0166(4) Uani 1 1 d . . .
O13 O 0.7302(2) 0.98860(19) 1.0965(2) 0.0170(4) Uani 1 1 d . . .
N1 N 0.5012(3) 0.6724(2) 0.5286(3) 0.0171(5) Uani 1 1 d . . .
N2 N 0.6589(3) 0.5711(2) 0.4504(3) 0.0211(6) Uani 1 1 d . . .
N3 N 0.5248(3) 0.8649(2) 0.6117(2) 0.0136(5) Uani 1 1 d . . .
N4 N 0.6298(3) 0.8647(2) 0.5761(2) 0.0129(5) Uani 1 1 d . . .
N5 N 0.7487(3) 0.5442(2) 0.4067(3) 0.0206(6) Uani 1 1 d . . .
H5 H 0.7545 0.4735 0.3828 0.025 Uiso 1 1 calc R U .
N6 N 0.7916(3) 0.7381(2) 0.4496(3) 0.0174(5) Uani 1 1 d . . .
N7 N 1.1103(3) 0.7831(2) 0.3387(2) 0.0154(5) Uani 1 1 d . . .
C1 C 0.4518(3) 0.7496(3) 0.5820(3) 0.0173(6) Uani 1 1 d . . .
H1 H 0.3751 0.7252 0.5967 0.021 Uiso 1 1 calc R U .
C2 C 0.6111(3) 0.7480(3) 0.5273(3) 0.0152(6) Uani 1 1 d . . .
C3 C 0.6898(3) 0.6891(3) 0.4754(3) 0.0167(6) Uani 1 1 d . . .
C4 C 0.8276(3) 0.6444(3) 0.4061(3) 0.0172(6) Uani 1 1 d . . .
C5 C 0.9369(3) 0.6518(3) 0.3655(3) 0.0167(6) Uani 1 1 d . . .
C6 C 0.9715(4) 0.5536(3) 0.3194(4) 0.0263(8) Uani 1 1 d . . .
H6 H 0.9256 0.4770 0.3130 0.032 Uiso 1 1 calc R U .
C7 C 1.1423(4) 0.6870(3) 0.2931(4) 0.0261(7) Uani 1 1 d . . .
H7 H 1.2117 0.6981 0.2674 0.031 Uiso 1 1 calc R U .
C8 C 1.0088(3) 0.7642(3) 0.3738(3) 0.0190(6) Uani 1 1 d . . .
H8 H 0.9855 0.8301 0.4054 0.023 Uiso 1 1 calc R U .
C9 C 1.0767(4) 0.5724(3) 0.2828(4) 0.0338(9) Uani 1 1 d . . .
H9 H 1.1027 0.5081 0.2517 0.041 Uiso 1 1 calc R U .
O1W O 0.9250(2) 0.9821(2) 0.5956(2) 0.0213(5) Uani 1 1 d . . .
H1WA H 1.0035 0.9885 0.6558 0.032 Uiso 1 1 d R U .
H1WB H 0.8912 0.9086 0.5400 0.032 Uiso 1 1 d R U .
O2W O 0.8834(2) 1.0553(2) 0.8134(2) 0.0236(5) Uani 1 1 d . . .
H2WA H 0.9668 1.1126 0.8633 0.035 Uiso 1 1 d R U .
H2WB H 0.8296 1.0665 0.8462 0.035 Uiso 1 1 d R U .
O3W O 0.3345(3) 0.4281(2) 0.3114(3) 0.0364(6) Uani 1 1 d . . .
H3WA H 0.3255 0.4462 0.2486 0.044 Uiso 1 1 d R U .
H3WB H 0.2605 0.3645 0.2832 0.044 Uiso 1 1 d R U .
O4W O 0.8580(4) 0.7624(3) 0.0398(3) 0.0619(10) Uani 1 1 d . . .
H4WA H 0.7878 0.7747 -0.0106 0.074 Uiso 1 1 d R U .
H4WB H 0.8622 0.6966 -0.0020 0.093 Uiso 1 1 d R U .
O5W O 0.2547(8) 0.4908(5) 0.1035(6) 0.145(3) Uani 1 1 d . U .
H5WA H 0.2432 0.5583 0.1250 0.218 Uiso 1 1 d R U .
H5WB H 0.3214 0.4991 0.0838 0.218 Uiso 1 1 d R U .
O6W O 0.7141(8) 0.7575(8) 0.1702(7) 0.172(3) Uani 1 1 d . U .
H6WA H 0.6505 0.7887 0.1630 0.206 Uiso 1 1 d R U .
H6WB H 0.7825 0.8055 0.1691 0.206 Uiso 1 1 d R U .
O7W O 0.5324(8) 0.5351(7) 0.1420(6) 0.196(4) Uani 1 1 d . U .
H7WA H 0.5982 0.6024 0.1643 0.235 Uiso 1 1 d R U .
H7WB H 0.5652 0.4789 0.1293 0.235 Uiso 1 1 d R U .
O8W O 0.8886(3) 0.8061(3) 0.8100(4) 0.0544(9) Uani 1 1 d . . .
H8WA H 0.8892 0.8190 0.8811 0.065 Uiso 1 1 d R U .
H8WB H 0.9608 0.7871 0.8156 0.065 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'
Ni Ni 0.3393 1.1124 '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'
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 Ni1 O2 177.73(9) . .
O1W Ni1 O2W 88.11(9) . .
O2 Ni1 O2W 90.10(9) . .
O1W Ni1 N7 90.52(9) . 2_776
O2 Ni1 N7 91.10(9) . 2_776
O2W Ni1 N7 97.62(10) . 2_776
O1W Ni1 O1 87.46(9) . 2_676
O2 Ni1 O1 94.20(8) . 2_676
O2W Ni1 O1 173.17(9) . 2_676
N7 Ni1 O1 87.61(9) 2_776 2_676
O1W Ni1 N4 96.92(9) . .
O2 Ni1 N4 81.63(9) . .
O2W Ni1 N4 88.31(10) . .
N7 Ni1 N4 170.66(10) 2_776 .
O1 Ni1 N4 87.08(9) 2_676 .
N1 Ni2 N1 180.0 2_666 .
N1 Ni2 O3W 88.71(11) 2_666 .
N1 Ni2 O3W 91.29(10) . .
N1 Ni2 O3W 91.29(10) 2_666 2_666
N1 Ni2 O3W 88.71(11) . 2_666
O3W Ni2 O3W 180.0 . 2_666
N1 Ni2 N2 101.80(10) 2_666 .
N1 Ni2 N2 78.20(10) . .
O3W Ni2 N2 91.80(11) . .
O3W Ni2 N2 88.20(11) 2_666 .
N1 Ni2 N2 78.20(10) 2_666 2_666
N1 Ni2 N2 101.79(10) . 2_666
O3W Ni2 N2 88.20(11) . 2_666
O3W Ni2 N2 91.80(11) 2_666 2_666
N2 Ni2 N2 180.00(13) . 2_666
O8 Mo1 O13 104.03(11) . .
O8 Mo1 O3 104.37(10) . .
O13 Mo1 O3 101.24(10) . .
O8 Mo1 O7 104.24(10) . .
O13 Mo1 O7 98.90(9) . .
O3 Mo1 O7 139.53(9) . .
O8 Mo1 O10 96.57(10) . .
O13 Mo1 O10 159.31(9) . .
O3 Mo1 O10 75.12(8) . .
O7 Mo1 O10 73.71(8) . .
O8 Mo1 O7 179.50(10) . 2_677
O13 Mo1 O7 76.46(8) . 2_677
O3 Mo1 O7 75.49(8) . 2_677
O7 Mo1 O7 75.65(8) . 2_677
O10 Mo1 O7 82.94(7) . 2_677
O1 Mo2 O2 104.54(10) . .
O1 Mo2 O5 104.27(10) . .
O2 Mo2 O5 101.86(9) . .
O1 Mo2 O10 94.61(9) . .
O2 Mo2 O10 151.98(9) . .
O5 Mo2 O10 92.80(9) . .
O1 Mo2 N3 94.60(10) . .
O2 Mo2 N3 79.42(9) . .
O5 Mo2 N3 159.96(9) . .
O10 Mo2 N3 78.81(8) . .
O1 Mo2 O3 165.41(9) . .
O2 Mo2 O3 89.37(9) . .
O5 Mo2 O3 76.56(8) . .
O10 Mo2 O3 70.82(8) . .
N3 Mo2 O3 83.48(8) . .
O11 Mo3 O9 104.37(11) . .
O11 Mo3 O12 103.49(10) . 2_677
O9 Mo3 O12 96.87(10) . 2_677
O11 Mo3 O10 102.91(10) . .
O9 Mo3 O10 96.43(9) . .
O12 Mo3 O10 146.33(9) 2_677 .
O11 Mo3 O7 153.33(10) . .
O9 Mo3 O7 102.25(10) . .
O12 Mo3 O7 74.67(8) 2_677 .
O10 Mo3 O7 72.34(8) . .
O11 Mo3 O13 82.29(9) . 2_677
O9 Mo3 O13 173.26(10) . 2_677
O12 Mo3 O13 80.36(8) 2_677 2_677
O10 Mo3 O13 82.88(8) . 2_677
O7 Mo3 O13 71.13(7) . 2_677
O6 Mo4 O4 105.00(13) . .
O6 Mo4 O12 101.46(11) . .
O4 Mo4 O12 98.08(11) . .
O6 Mo4 O5 95.68(10) . .
O4 Mo4 O5 98.49(11) . .
O12 Mo4 O5 152.13(9) . .
O6 Mo4 O7 91.02(10) . 2_677
O4 Mo4 O7 163.32(11) . 2_677
O12 Mo4 O7 73.74(8) . 2_677
O5 Mo4 O7 84.22(8) . 2_677
O6 Mo4 O3 161.40(10) . .
O4 Mo4 O3 91.66(10) . .
O12 Mo4 O3 83.97(8) . .
O5 Mo4 O3 73.31(8) . .
O7 Mo4 O3 73.27(7) 2_677 .
Mo2 O1 Ni1 145.62(12) . 2_676
Mo2 O2 Ni1 135.90(11) . .
Mo1 O3 Mo2 107.91(9) . .
Mo1 O3 Mo4 113.61(9) . .
Mo2 O3 Mo4 91.60(7) . .
Mo2 O5 Mo4 115.25(10) . .
Mo1 O7 Mo3 104.79(9) . .
Mo1 O7 Mo4 151.01(11) . 2_677
Mo3 O7 Mo4 92.75(7) . 2_677
Mo1 O7 Mo1 104.35(8) . 2_677
Mo3 O7 Mo1 95.88(7) . 2_677
Mo4 O7 Mo1 96.43(7) 2_677 2_677
Mo3 O10 Mo2 148.10(11) . .
Mo3 O10 Mo1 105.66(9) . .
Mo2 O10 Mo1 105.77(8) . .
Mo3 O12 Mo4 114.02(10) 2_677 .
Mo1 O13 Mo3 116.27(10) . 2_677
C1 N1 C2 102.8(2) . .
C1 N1 Ni2 139.2(2) . .
C2 N1 Ni2 115.1(2) . .
C3 N2 N5 102.9(2) . .
C3 N2 Ni2 112.5(2) . .
N5 N2 Ni2 144.5(2) . .
C1 N3 N4 107.1(2) . .
C1 N3 Mo2 129.9(2) . .
N4 N3 Mo2 123.06(18) . .
C2 N4 N3 104.5(2) . .
C2 N4 Ni1 139.5(2) . .
N3 N4 Ni1 115.69(17) . .
C4 N5 N2 109.8(2) . .
C4 N6 C3 103.5(2) . .
C8 N7 C7 117.4(3) . .
C8 N7 Ni1 119.3(2) . 2_776
C7 N7 Ni1 123.1(2) . 2_776
N3 C1 N1 112.2(3) . .
N4 C2 N1 113.4(3) . .
N4 C2 C3 130.9(3) . .
N1 C2 C3 115.8(3) . .
N2 C3 N6 114.5(3) . .
N2 C3 C2 116.8(3) . .
N6 C3 C2 128.7(3) . .
N6 C4 N5 109.3(3) . .
N6 C4 C5 124.6(3) . .
N5 C4 C5 126.0(3) . .
C6 C5 C8 118.7(3) . .
C6 C5 C4 123.8(3) . .
C8 C5 C4 117.6(3) . .
C5 C6 C9 118.2(3) . .
N7 C7 C9 122.8(3) . .
N7 C8 C5 123.5(3) . .
C7 C9 C6 119.5(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O1W 2.030(2) .
Ni1 O2 2.050(2) .
Ni1 O2W 2.070(2) .
Ni1 N7 2.089(2) 2_776
Ni1 O1 2.092(2) 2_676
Ni1 N4 2.110(2) .
Ni2 N1 2.047(2) 2_666
Ni2 N1 2.047(2) .
Ni2 O3W 2.063(3) .
Ni2 O3W 2.063(3) 2_666
Ni2 N2 2.154(3) .
Ni2 N2 2.154(3) 2_666
Mo1 O8 1.689(2) .
Mo1 O13 1.744(2) .
Mo1 O3 1.907(2) .
Mo1 O7 1.935(2) .
Mo1 O10 2.184(2) .
Mo1 O7 2.446(2) 2_677
Mo2 O1 1.716(2) .
Mo2 O2 1.737(2) .
Mo2 O5 1.842(2) .
Mo2 O10 2.0492(19) .
Mo2 N3 2.223(2) .
Mo2 O3 2.262(2) .
Mo3 O11 1.694(2) .
Mo3 O9 1.723(2) .
Mo3 O12 1.920(2) 2_677
Mo3 O10 1.956(2) .
Mo3 O7 2.228(2) .
Mo3 O13 2.329(2) 2_677
Mo4 O6 1.693(2) .
Mo4 O4 1.700(2) .
Mo4 O12 1.943(2) .
Mo4 O5 2.006(2) .
Mo4 O7 2.249(2) 2_677
Mo4 O3 2.273(2) .
O1 Ni1 2.092(2) 2_676
O7 Mo4 2.249(2) 2_677
O7 Mo1 2.446(2) 2_677
O12 Mo3 1.920(2) 2_677
O13 Mo3 2.329(2) 2_677
N1 C1 1.334(4) .
N1 C2 1.354(4) .
N2 C3 1.328(4) .
N2 N5 1.350(3) .
N3 C1 1.324(4) .
N3 N4 1.381(3) .
N4 C2 1.321(4) .
N5 C4 1.345(4) .
N6 C4 1.337(4) .
N6 C3 1.341(4) .
N7 C8 1.341(4) .
N7 C7 1.341(4) .
N7 Ni1 2.089(2) 2_776
C2 C3 1.458(4) .
C4 C5 1.462(4) .
C5 C6 1.381(4) .
C5 C8 1.385(4) .
C6 C9 1.391(5) .
C7 C9 1.379(5) .
