#------------------------------------------------------------------------------
#$Date: 2019-11-17 08:43:43 +0200 (Sun, 17 Nov 2019) $
#$Revision: 228919 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/15/7231542.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_7231542
loop_
_publ_author_name
'Wang, Xiuli'
'Bai, Xue'
'Lin, Hongyan'
'Sun, Junjun'
'Liu, Guocheng'
'Wang, Xiang'
_publ_section_title
;
 Novel polyoxometalate-based cobalt complexes based on rigid
 pyridyl-triazole-tetrazole and pyridyl-bis(triazole) ligands
;
_journal_issue                   41
_journal_name_full               CrystEngComm
_journal_page_first              6438
_journal_paper_doi               10.1039/C8CE01158C
_journal_volume                  20
_journal_year                    2018
_chemical_formula_sum            'C16 H40 Co3 Mo6 N16 O38 Te'
_chemical_formula_weight         1944.67
_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   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-07-04 deposited with the CCDC.
2018-09-19 downloaded from the CCDC.
;
_cell_angle_alpha                100.1280(10)
_cell_angle_beta                 105.9920(10)
_cell_angle_gamma                91.2080(10)
_cell_formula_units_Z            1
_cell_length_a                   10.6300(5)
_cell_length_b                   11.3860(5)
_cell_length_c                   11.4910(5)
_cell_measurement_reflns_used    4357
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.1281
_cell_measurement_theta_min      2.3562
_cell_volume                     1312.58(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 0.996
_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  0.0146
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            7667
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.131
_diffrn_reflns_theta_max         25.131
_diffrn_reflns_theta_min         1.822
_exptl_absorpt_coefficient_mu    2.966
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6196
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    2.460
_exptl_crystal_description       block
_exptl_crystal_F_000             907
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.717
_refine_diff_density_min         -0.775
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         4680
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0296
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0542P)²+4.7526P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0918
_refine_ls_wR_factor_ref         0.0948
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4154
_reflns_number_total             4698
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8ce01158c2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7231541--7231543.cif.'
_cod_database_code               7231542
_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'
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
Te1 Te 0.0000 0.0000 0.0000 0.01257(12) Uani 1 2 d S . P
Co1 Co 0.39943(6) -0.34338(5) 0.01617(6) 0.01528(15) Uani 1 1 d . . .
O1 O 0.3073(3) -0.2448(3) 0.1321(3) 0.0204(7) Uani 1 1 d . . .
C1 C 0.4557(5) -0.3972(4) -0.2240(4) 0.0171(9) Uani 1 1 d . . .
N1 N 0.4809(4) -0.4380(3) -0.1187(3) 0.0168(8) Uani 1 1 d . . .
Mo1 Mo -0.30449(4) -0.07912(4) -0.16373(4) 0.01799(12) Uani 1 1 d . . .
O1W O 0.5568(3) -0.2143(3) 0.1014(3) 0.0278(8) Uani 1 1 d . . .
Co2 Co 0.5000 -0.5000 -0.5000 0.0219(2) Uani 1 2 d S . P
N2 N 0.3488(4) -0.2427(3) -0.1329(4) 0.0180(8) Uani 1 1 d . . .
C2 C 0.3841(4) -0.2907(4) -0.2320(4) 0.0163(9) Uani 1 1 d . . .
Mo2 Mo -0.13216(4) -0.26950(3) -0.01615(4) 0.02002(12) Uani 1 1 d . . .
O2W O 0.2175(3) -0.4361(3) -0.0773(3) 0.0270(8) Uani 1 1 d . . .
O2 O 0.1704(3) -0.0618(3) 0.0133(3) 0.0150(6) Uani 1 1 d . . .
N3 N 0.4984(4) -0.4696(4) -0.3083(4) 0.0213(9) Uani 1 1 d . . .
C3 C 0.2871(5) -0.1404(4) -0.2801(4) 0.0177(9) Uani 1 1 d . . .
Mo3 Mo 0.16570(4) -0.18692(3) 0.15705(4) 0.01661(12) Uani 1 1 d . . .
O3 O 0.0531(3) -0.2927(3) 0.0141(3) 0.0207(7) Uani 1 1 d . . .
O3W O 0.6718(6) -0.3901(5) -0.4571(5) 0.0761(19) Uani 1 1 d . . .
N4 N 0.5414(4) -0.5389(3) -0.1384(4) 0.0207(9) Uani 1 1 d . . .
C4 C 0.2327(5) -0.0465(4) -0.3481(4) 0.0202(10) Uani 1 1 d . . .
O4 O -0.0166(3) -0.0994(3) 0.1153(3) 0.0171(7) Uani 1 1 d . . .
O4W O 0.3880(6) -0.3575(5) -0.5334(4) 0.0707(19) Uani 1 1 d . . .
C5 C 0.1953(5) 0.0296(4) -0.5314(4) 0.0239(11) Uani 1 1 d . . .
H5A H 0.2020 0.0222 -0.6113 0.029 Uiso 1 1 calc R U .
N5 N 0.5518(4) -0.5587(4) -0.2514(4) 0.0240(9) Uani 1 1 d . . .
O5 O -0.0934(3) -0.1326(3) -0.1246(3) 0.0166(7) Uani 1 1 d . . .
O5W O 0.5047(11) -0.1350(13) -0.5913(13) 0.214(7) Uani 1 1 d . . .
N6 N 0.3485(4) -0.2308(3) -0.3256(3) 0.0179(8) Uani 1 1 d . . .
C6 C 0.2417(6) -0.0538(5) -0.4672(5) 0.0324(13) Uani 1 1 d . . .
H6A H 0.2805 -0.1178 -0.5024 0.039 Uiso 1 1 calc R U .
O6 O -0.2816(3) -0.1691(3) -0.0341(3) 0.0236(8) Uani 1 1 d . . .
O6W O 0.0735(14) -0.4676(9) 0.3409(14) 0.205(6) Uani 1 1 d . . .
O7 O -0.3542(4) -0.1904(3) -0.2905(4) 0.0319(9) Uani 1 1 d . . .
N7 N 0.2859(4) -0.1462(3) -0.1653(4) 0.0177(8) Uani 1 1 d . . .
H7A H 0.2510 -0.0970 -0.1197 0.021 Uiso 1 1 calc R U .
C7 C 0.1399(7) 0.1227(6) -0.4867(6) 0.0451(16) Uani 1 1 d . . .
H7B H 0.1066 0.1781 -0.5357 0.054 Uiso 1 1 calc R U .
O7W O 0.0037(6) -0.2711(6) -0.3106(5) 0.0752(17) Uani 1 1 d . . .
O8 O -0.1623(4) -0.3248(3) 0.1044(4) 0.0317(9) Uani 1 1 d . . .
C8 C 0.1775(6) 0.0508(5) -0.2977(6) 0.0366(14) Uani 1 1 d . . .
H8A H 0.1711 0.0581 -0.2177 0.044 Uiso 1 1 calc R U .
N8 N 0.1311(7) 0.1384(6) -0.3663(7) 0.070(2) Uani 1 1 d . . .
O9 O -0.1880(4) -0.3777(3) -0.1432(4) 0.0356(9) Uani 1 1 d . . .
O10 O 0.1380(4) -0.2449(3) 0.2757(4) 0.0308(9) Uani 1 1 d . . .
O11 O -0.2386(3) 0.0315(3) -0.2511(3) 0.0193(7) Uani 1 1 d . . .
O12 O -0.4412(3) -0.0090(3) -0.1474(4) 0.0278(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'
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'
Co Co 0.3494 0.9721 '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'
Te Te -0.5308 1.6751 '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
O5 Te1 O5 180.0 . 2
O5 Te1 O4 94.88(14) . 2
O5 Te1 O4 85.12(14) 2 2
O5 Te1 O4 85.12(14) . .
O5 Te1 O4 94.88(14) 2 .
O4 Te1 O4 180.0 2 .
O5 Te1 O2 94.52(13) . .
O5 Te1 O2 85.48(13) 2 .
O4 Te1 O2 94.02(13) 2 .
O4 Te1 O2 85.98(13) . .
O5 Te1 O2 85.48(13) . 2
O5 Te1 O2 94.51(13) 2 2
O4 Te1 O2 85.98(13) 2 2
O4 Te1 O2 94.02(13) . 2
O2 Te1 O2 180.0 . 2
O1 Co1 N4 91.42(14) . 2_645
O1 Co1 O2W 87.58(13) . .
N4 Co1 O2W 95.35(15) 2_645 .
O1 Co1 O1W 84.44(13) . .
N4 Co1 O1W 96.08(15) 2_645 .
O2W Co1 O1W 166.21(14) . .
O1 Co1 N1 173.97(14) . .
N4 Co1 N1 94.08(14) 2_645 .
O2W Co1 N1 89.46(15) . .
O1W Co1 N1 97.41(14) . .
O1 Co1 N2 98.04(13) . .
N4 Co1 N2 170.37(15) 2_645 .
O2W Co1 N2 83.30(15) . .
O1W Co1 N2 86.69(15) . .
N1 Co1 N2 76.39(14) . .
Mo3 O1 Co1 149.4(2) . .
N1 C1 N3 111.1(4) . .
N1 C1 C2 117.7(4) . .
N3 C1 C2 131.1(4) . .
C1 N1 N4 105.3(4) . .
C1 N1 Co1 115.1(3) . .
N4 N1 Co1 139.1(3) . .
O7 Mo1 O12 107.06(18) . .
O7 Mo1 O6 100.98(17) . .
O12 Mo1 O6 99.06(16) . .
O7 Mo1 O11 94.05(16) . .
O12 Mo1 O11 98.75(16) . .
O6 Mo1 O11 152.12(14) . .
O7 Mo1 O2 159.50(15) . 2
O12 Mo1 O2 91.75(15) . 2
O6 Mo1 O2 83.53(14) . 2
O11 Mo1 O2 74.66(12) . 2
O7 Mo1 O5 91.56(15) . .
O12 Mo1 O5 161.22(15) . .
O6 Mo1 O5 74.38(12) . .
O11 Mo1 O5 81.93(13) . .
O2 Mo1 O5 70.22(11) 2 .
O4W Co2 O4W 180.00(16) 2_644 .
O4W Co2 O3W 90.9(3) 2_644 2_644
O4W Co2 O3W 89.1(3) . 2_644
O4W Co2 O3W 89.1(3) 2_644 .
O4W Co2 O3W 90.9(3) . .
O3W Co2 O3W 180.0 2_644 .
O4W Co2 N3 88.23(16) 2_644 .
O4W Co2 N3 91.77(16) . .
O3W Co2 N3 88.16(19) 2_644 .
O3W Co2 N3 91.84(19) . .
O4W Co2 N3 91.77(16) 2_644 2_644
O4W Co2 N3 88.23(16) . 2_644
O3W Co2 N3 91.84(19) 2_644 2_644
O3W Co2 N3 88.16(19) . 2_644
N3 Co2 N3 180.0 . 2_644
C2 N2 N7 103.9(4) . .
C2 N2 Co1 114.1(3) . .
N7 N2 Co1 141.9(3) . .
N2 C2 N6 114.0(4) . .
N2 C2 C1 116.5(4) . .
N6 C2 C1 129.6(4) . .
O9 Mo2 O8 106.72(19) . .
O9 Mo2 O3 97.84(17) . .
O8 Mo2 O3 99.97(16) . .
O9 Mo2 O6 100.69(17) . .
O8 Mo2 O6 93.77(16) . .
O3 Mo2 O6 152.65(14) . .
O9 Mo2 O5 93.34(17) . .
O8 Mo2 O5 158.35(15) . .
O3 Mo2 O5 84.91(13) . .
O6 Mo2 O5 74.13(12) . .
O9 Mo2 O4 160.35(16) . .
O8 Mo2 O4 91.90(16) . .
O3 Mo2 O4 72.19(12) . .
O6 Mo2 O4 83.90(13) . .
O5 Mo2 O4 69.35(11) . .
Te1 O2 Mo1 102.18(13) . 2
Te1 O2 Mo3 98.01(12) . .
Mo1 O2 Mo3 91.24(11) 2 .
C1 N3 N5 105.0(4) . .
C1 N3 Co2 143.1(3) . .
N5 N3 Co2 111.7(3) . .
N6 C3 N7 110.8(4) . .
N6 C3 C4 123.5(4) . .
N7 C3 C4 125.7(4) . .
O10 Mo3 O1 106.66(17) . .
O10 Mo3 O11 97.07(16) . 2
O1 Mo3 O11 99.09(15) . 2
O10 Mo3 O3 102.27(17) . .
O1 Mo3 O3 93.08(15) . .
O11 Mo3 O3 153.14(14) 2 .
O10 Mo3 O4 95.71(15) . .
O1 Mo3 O4 156.77(14) . .
O11 Mo3 O4 83.98(13) 2 .
O3 Mo3 O4 75.76(13) . .
O10 Mo3 O2 163.58(14) . .
O1 Mo3 O2 88.13(13) . .
O11 Mo3 O2 73.05(12) 2 .
O3 Mo3 O2 83.58(13) . .
O4 Mo3 O2 70.62(11) . .
Mo3 O3 Mo2 114.68(16) . .
N5 N4 N1 109.7(4) . .
N5 N4 Co1 123.4(3) . 2_645
N1 N4 Co1 126.7(3) . 2_645
C8 C4 C6 118.3(5) . .
C8 C4 C3 123.2(4) . .
C6 C4 C3 118.5(4) . .
Te1 O4 Mo3 105.38(13) . .
Te1 O4 Mo2 101.58(14) . .
Mo3 O4 Mo2 92.89(11) . .
C7 C5 C6 122.7(5) . .
N4 N5 N3 108.9(4) . .
Te1 O5 Mo2 103.95(14) . .
Te1 O5 Mo1 102.08(13) . .
Mo2 O5 Mo1 92.10(11) . .
C3 N6 C2 102.8(4) . .
C5 C6 C4 120.5(5) . .
Mo1 O6 Mo2 114.73(16) . .
C3 N7 N2 108.5(4) . .
C5 C7 N8 120.3(5) . .
C4 C8 N8 120.2(5) . .
C7 N8 C8 118.0(6) . .
Mo3 O11 Mo1 116.96(16) 2 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Te1 O5 1.926(3) .
Te1 O5 1.926(3) 2
Te1 O4 1.927(3) 2
Te1 O4 1.927(3) .
Te1 O2 1.933(3) .
Te1 O2 1.933(3) 2
Co1 O1 2.058(3) .
Co1 N4 2.092(4) 2_645
Co1 O2W 2.093(4) .
Co1 O1W 2.099(4) .
Co1 N1 2.122(4) .
Co1 N2 2.178(4) .
O1 Mo3 1.730(3) .
C1 N1 1.333(6) .
C1 N3 1.342(6) .
C1 C2 1.448(6) .
N1 N4 1.344(5) .
Mo1 O7 1.704(4) .
Mo1 O12 1.712(3) .
Mo1 O6 1.917(3) .
Mo1 O11 1.970(3) .
Mo1 O2 2.272(3) 2
Mo1 O5 2.282(3) .
Co2 O4W 2.060(4) 2_644
Co2 O4W 2.060(4) .
Co2 O3W 2.082(5) 2_644
Co2 O3W 2.082(5) .
Co2 N3 2.174(4) .
Co2 N3 2.174(4) 2_644
N2 C2 1.328(6) .
N2 N7 1.353(5) .
C2 N6 1.345(6) .
Mo2 O9 1.691(4) .
Mo2 O8 1.720(4) .
Mo2 O3 1.936(3) .
Mo2 O6 1.963(3) .
Mo2 O5 2.257(3) .
Mo2 O4 2.322(3) .
O2 Mo1 2.272(3) 2
O2 Mo3 2.373(3) .
N3 N5 1.354(5) .
C3 N6 1.336(6) .
C3 N7 1.337(6) .
C3 C4 1.469(6) .
Mo3 O10 1.706(3) .
Mo3 O11 1.926(3) 2
Mo3 O3 1.934(3) .
Mo3 O4 2.172(3) .
N4 N5 1.313(5) .
N4 Co1 2.092(4) 2_645
C4 C8 1.378(7) .
C4 C6 1.386(7) .
C5 C7 1.317(8) .
C5 C6 1.325(7) .
C7 N8 1.393(9) .
C8 N8 1.394(8) .
O11 Mo3 1.926(3) 2
