#------------------------------------------------------------------------------
#$Date: 2016-03-26 17:12:40 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180381 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/50/7205056.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_7205056
loop_
_publ_author_name
'Li, Ming-Xing'
'Chen, Hui-Ling'
'Geng, Jin-Peng'
'He, Xiang'
'Shao, Min'
'Zhu, Shou-Rong'
'Wang, Zhao-Xi'
_publ_section_title
;
 Unprecedented cyclic [Mo6O19]2− cluster and five
 organic--inorganic hybrids based on polyoxomolybdates and
 4-amino-3,5-bis(pyridyl)-1,2,4-triazole
;
_journal_issue                   5
_journal_name_full               CrystEngComm
_journal_page_first              1687
_journal_paper_doi               10.1039/c002063j
_journal_volume                  13
_journal_year                    2011
_chemical_formula_sum            'C12 H14 Cu Mo4 N6 O15'
_chemical_formula_weight         929.59
_chemical_name_systematic
;

?

;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                99.395(2)
_cell_angle_beta                 109.368(2)
_cell_angle_gamma                101.945(2)
_cell_formula_units_Z            2
_cell_length_a                   9.6892(16)
_cell_length_b                   9.8474(16)
_cell_length_c                   13.533(2)
_cell_measurement_reflns_used    3925
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      0.00
_cell_volume                     1153.6(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0193
_diffrn_reflns_av_sigmaI/netI    0.0352
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5993
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    3.109
_exptl_absorpt_correction_T_max  0.5752
_exptl_absorpt_correction_T_min  0.5104
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_density_diffrn    2.676
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             890
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.355
_refine_diff_density_min         -1.236
_refine_diff_density_rms         0.212
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         4012
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0350
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0644P)²+2.3258P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.1040
_reflns_number_gt                3595
_reflns_number_total             4012
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C002063J.TXT
_cod_data_source_block           090225b_0m
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7205056
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.59089(7) 0.18133(7) 0.02505(6) 0.02699(19) Uani 1 1 d . . .
Mo1 Mo 0.54582(5) 0.30702(4) 0.35944(3) 0.01648(14) Uani 1 1 d . . .
Mo2 Mo 0.40530(5) 0.30006(4) 0.55554(3) 0.01632(14) Uani 1 1 d . . .
Mo3 Mo 0.67600(4) 0.12113(4) 0.53650(3) 0.01290(14) Uani 1 1 d . . .
Mo4 Mo 0.48809(5) 0.09143(4) 0.71241(3) 0.01589(14) Uani 1 1 d . . .
C1 C 0.6546(6) 0.4516(6) -0.0306(4) 0.0221(11) Uani 1 1 d . . .
H1 H 0.6270 0.3932 -0.0994 0.027 Uiso 1 1 calc R . .
C2 C 0.6778(6) 0.5977(5) -0.0187(4) 0.0197(11) Uani 1 1 d . . .
H2 H 0.6637 0.6360 -0.0786 0.024 Uiso 1 1 calc R . .
C3 C 0.7225(5) 0.6864(5) 0.0838(4) 0.0157(10) Uani 1 1 d . . .
C4 C 0.7441(6) 0.6249(5) 0.1710(4) 0.0223(11) Uani 1 1 d . . .
H4 H 0.7766 0.6815 0.2411 0.027 Uiso 1 1 calc R . .
C5 C 0.7162(6) 0.4776(6) 0.1515(4) 0.0225(11) Uani 1 1 d . . .
H5 H 0.7303 0.4369 0.2102 0.027 Uiso 1 1 calc R . .
C6 C 0.7401(5) 0.8411(5) 0.0963(4) 0.0153(10) Uani 1 1 d . . .
C7 C 0.8374(5) 1.0713(5) 0.1545(4) 0.0165(10) Uani 1 1 d . . .
C8 C 0.9431(5) 1.2125(5) 0.2197(4) 0.0198(11) Uani 1 1 d . . .
C9 C 1.0143(7) 1.3042(6) 0.1717(5) 0.0318(13) Uani 1 1 d . . .
H9 H 0.9941 1.2784 0.0980 0.038 Uiso 1 1 calc R . .
C10 C 1.1143(7) 1.4327(7) 0.2353(6) 0.0404(16) Uani 1 1 d . . .
H10 H 1.1648 1.4943 0.2052 0.048 Uiso 1 1 calc R . .
C11 C 1.0707(7) 1.3857(6) 0.3873(5) 0.0312(14) Uani 1 1 d . . .
H11 H 1.0897 1.4164 0.4605 0.037 Uiso 1 1 calc R . .
C12 C 0.9701(6) 1.2522(6) 0.3278(4) 0.0272(12) Uani 1 1 d . . .
H12 H 0.9227 1.1918 0.3603 0.033 Uiso 1 1 calc R . .
N1 N 0.6699(5) 0.3900(5) 0.0525(4) 0.0216(9) Uani 1 1 d . . .
N2 N 0.6393(5) 0.8990(4) 0.0437(3) 0.0167(9) Uani 1 1 d . . .
N3 N 0.7027(5) 1.0473(4) 0.0795(3) 0.0185(9) Uani 1 1 d . . .
N4 N 0.8660(5) 0.9450(4) 0.1668(3) 0.0166(9) Uani 1 1 d . . .
N5 N 0.9934(5) 0.9190(5) 0.2392(4) 0.0339(12) Uani 1 1 d . . .
H5A H 1.0680 0.9897 0.2843 0.041 Uiso 1 1 calc R . .
H5B H 0.9971 0.8324 0.2386 0.041 Uiso 1 1 calc R . .
N6 N 1.1400(6) 1.4701(5) 0.3401(4) 0.0359(12) Uani 1 1 d . . .
O1 O 0.4432(5) 0.2678(4) 0.2243(3) 0.0326(10) Uani 1 1 d . . .
O2 O 0.5294(5) 0.5066(4) 0.4018(3) 0.0261(9) Uani 1 1 d . . .
O3 O 0.7307(4) 0.3736(4) 0.3748(3) 0.0275(9) Uani 1 1 d . . .
O4 O 0.3618(4) 0.2705(4) 0.4121(3) 0.0200(8) Uani 1 1 d . . .
O5 O 0.2310(4) 0.2593(5) 0.5605(3) 0.0299(9) Uani 1 1 d . . .
O6 O 0.5248(4) 0.2823(4) 0.7028(3) 0.0197(8) Uani 1 1 d . . .
O7 O 0.4209(4) 0.0813(3) 0.5362(3) 0.0138(7) Uani 1 1 d . . .
O8 O 0.6374(4) 0.3030(4) 0.5396(3) 0.0165(7) Uani 1 1 d . . .
O9 O 0.5469(4) 0.1099(4) 0.3678(3) 0.0176(7) Uani 1 1 d . . .
O10 O 0.8520(4) 0.1503(4) 0.5330(3) 0.0256(9) Uani 1 1 d . . .
O11 O 0.7036(4) 0.1094(4) 0.6688(3) 0.0202(8) Uani 1 1 d . . .
O12 O 0.6048(5) 0.1043(4) 0.8435(3) 0.0274(9) Uani 1 1 d . . .
O13 O 0.3095(4) 0.0613(4) 0.7123(3) 0.0261(9) Uani 1 1 d . . .
O1W O 0.1493(7) 0.0492(7) 0.1047(5) 0.0732(17) Uani 1 1 d . . .
O2W O 0.9172(9) 0.3106(9) 0.9057(7) 0.115(3) Uani 1 1 d . . .
H1WA H 0.1199 -0.0420 0.0857 0.138 Uiso 1 1 d R . .
H1WB H 0.0676 0.0596 0.1113 0.138 Uiso 1 1 d R . .
H2WB H 0.8313 0.3234 0.9006 0.138 Uiso 1 1 d R . .
H2WA H 0.9289 0.2403 0.8666 0.138 Uiso 1 1 d R . .
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'
Cu Cu 0.3201 1.2651 '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
_geom_angle_publ_flag
N3 Cu1 N1 127.61(17) 1_545 . ?
N3 Cu1 N2 115.57(16) 1_545 2_665 ?
N1 Cu1 N2 115.78(17) . 2_665 ?
O1 Mo1 O3 105.5(2) . . ?
O1 Mo1 O9 96.78(17) . . ?
O3 Mo1 O9 99.04(16) . . ?
O1 Mo1 O2 99.13(18) . . ?
O3 Mo1 O2 90.70(17) . . ?
O9 Mo1 O2 158.40(15) . . ?
O1 Mo1 O4 98.27(18) . . ?
O3 Mo1 O4 155.09(17) . . ?
O9 Mo1 O4 85.29(14) . . ?
O2 Mo1 O4 78.06(15) . . ?
O1 Mo1 O8 164.18(17) . . ?
O3 Mo1 O8 87.14(16) . . ?
O9 Mo1 O8 71.40(13) . . ?
O2 Mo1 O8 90.04(14) . . ?
O4 Mo1 O8 70.90(13) . . ?
O5 Mo2 O4 102.21(19) . . ?
O5 Mo2 O2 104.30(19) . 2_666 ?
O4 Mo2 O2 100.97(16) . 2_666 ?
O5 Mo2 O6 98.45(17) . . ?
O4 Mo2 O6 151.95(15) . . ?
O2 Mo2 O6 92.00(16) 2_666 . ?
O5 Mo2 O7 94.59(17) . . ?
O4 Mo2 O7 86.22(14) . . ?
O2 Mo2 O7 157.70(17) 2_666 . ?
O6 Mo2 O7 73.32(13) . . ?
O5 Mo2 O8 167.59(17) . . ?
O4 Mo2 O8 75.96(14) . . ?
O2 Mo2 O8 88.07(15) 2_666 . ?
O6 Mo2 O8 79.77(14) . . ?
O7 Mo2 O8 73.10(12) . . ?
O10 Mo3 O11 104.33(18) . . ?
O10 Mo3 O8 103.58(17) . . ?
O11 Mo3 O8 101.15(16) . . ?
O10 Mo3 O7 103.99(17) . 2_656 ?
O11 Mo3 O7 98.23(15) . 2_656 ?
O8 Mo3 O7 140.93(15) . 2_656 ?
O10 Mo3 O9 98.85(16) . . ?
O11 Mo3 O9 156.67(15) . . ?
O8 Mo3 O9 75.60(13) . . ?
O7 Mo3 O9 73.25(13) 2_656 . ?
O10 Mo3 O7 178.24(15) . . ?
O11 Mo3 O7 77.39(14) . . ?
O8 Mo3 O7 75.57(13) . . ?
O7 Mo3 O7 76.05(14) 2_656 . ?
O9 Mo3 O7 79.45(12) . . ?
O13 Mo4 O12 105.45(19) . . ?
O13 Mo4 O6 100.14(17) . . ?
O12 Mo4 O6 103.25(17) . . ?
O13 Mo4 O9 93.92(16) . 2_656 ?
O12 Mo4 O9 104.83(16) . 2_656 ?
O6 Mo4 O9 143.81(15) . 2_656 ?
O13 Mo4 O7 96.08(16) . . ?
O12 Mo4 O7 158.39(16) . . ?
O6 Mo4 O7 74.26(13) . . ?
O9 Mo4 O7 71.19(13) 2_656 . ?
O13 Mo4 O11 166.48(16) . . ?
O12 Mo4 O11 87.20(16) . . ?
O6 Mo4 O11 81.14(14) . . ?
O9 Mo4 O11 77.93(13) 2_656 . ?
O7 Mo4 O11 71.19(12) . . ?
N1 C1 C2 123.1(5) . . ?
N1 C1 H1 118.5 . . ?
C2 C1 H1 118.5 . . ?
C1 C2 C3 119.0(5) . . ?
C1 C2 H2 120.5 . . ?
C3 C2 H2 120.5 . . ?
C2 C3 C4 118.6(5) . . ?
C2 C3 C6 119.2(4) . . ?
C4 C3 C6 122.2(4) . . ?
C5 C4 C3 118.5(5) . . ?
C5 C4 H4 120.7 . . ?
C3 C4 H4 120.7 . . ?
N1 C5 C4 123.7(5) . . ?
N1 C5 H5 118.2 . . ?
C4 C5 H5 118.2 . . ?
N2 C6 N4 109.8(4) . . ?
N2 C6 C3 126.1(4) . . ?
N4 C6 C3 124.1(4) . . ?
N3 C7 N4 109.6(4) . . ?
N3 C7 C8 126.5(4) . . ?
N4 C7 C8 123.8(4) . . ?
C12 C8 C9 120.6(5) . . ?
C12 C8 C7 119.2(5) . . ?
C9 C8 C7 120.2(5) . . ?
C10 C9 C8 118.5(6) . . ?
C10 C9 H9 120.7 . . ?
C8 C9 H9 120.7 . . ?
N6 C10 C9 120.4(6) . . ?
N6 C10 H10 119.8 . . ?
C9 C10 H10 119.8 . . ?
N6 C11 C12 120.4(6) . . ?
N6 C11 H11 119.8 . . ?
C12 C11 H11 119.8 . . ?
C8 C12 C11 117.9(6) . . ?
C8 C12 H12 121.1 . . ?
C11 C12 H12 121.1 . . ?
C1 N1 C5 117.1(4) . . ?
C1 N1 Cu1 120.2(4) . . ?
C5 N1 Cu1 121.8(4) . . ?
C6 N2 N3 107.3(4) . . ?
C6 N2 Cu1 129.1(3) . 2_665 ?
N3 N2 Cu1 118.9(3) . 2_665 ?
C7 N3 N2 107.1(4) . . ?
C7 N3 Cu1 130.5(3) . 1_565 ?
N2 N3 Cu1 122.3(3) . 1_565 ?
C7 N4 C6 106.1(4) . . ?
C7 N4 N5 129.4(4) . . ?
C6 N4 N5 124.4(4) . . ?
N4 N5 H5A 120.0 . . ?
N4 N5 H5B 120.0 . . ?
H5A N5 H5B 120.0 . . ?
C10 N6 C11 122.2(5) . . ?
Mo2 O2 Mo1 156.4(2) 2_666 . ?
Mo2 O4 Mo1 118.05(18) . . ?
Mo4 O6 Mo2 112.15(17) . . ?
Mo3 O7 Mo2 148.13(18) 2_656 . ?
Mo3 O7 Mo4 104.95(14) 2_656 . ?
Mo2 O7 Mo4 93.88(12) . . ?
Mo3 O7 Mo3 103.95(14) 2_656 . ?
Mo2 O7 Mo3 99.31(13) . . ?
Mo4 O7 Mo3 95.89(12) . . ?
Mo3 O8 Mo1 103.88(14) . . ?
Mo3 O8 Mo2 111.59(15) . . ?
Mo1 O8 Mo2 93.04(12) . . ?
Mo1 O9 Mo4 147.14(18) . 2_656 ?
Mo1 O9 Mo3 106.61(15) . . ?
Mo4 O9 Mo3 105.07(15) 2_656 . ?
Mo3 O11 Mo4 115.10(17) . . ?
H1WA O1W H1WB 95.7 . . ?
H2WB O2W H2WB 0.0 . . ?
H2WB O2W H2WA 124.3 . . ?
H2WB O2W H2WA 124.3 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N3 1.959(4) 1_545 ?
Cu1 N1 1.964(4) . ?
Cu1 N2 2.029(4) 2_665 ?
Mo1 O1 1.699(4) . ?
Mo1 O3 1.704(4) . ?
Mo1 O9 1.964(3) . ?
Mo1 O2 2.009(4) . ?
Mo1 O4 2.116(4) . ?
Mo1 O8 2.312(3) . ?
Mo2 O5 1.680(4) . ?
Mo2 O4 1.804(4) . ?
Mo2 O2 1.805(4) 2_666 ?
Mo2 O6 2.003(3) . ?
Mo2 O7 2.170(3) . ?
Mo2 O8 2.324(3) . ?
Mo3 O10 1.687(4) . ?
Mo3 O11 1.748(3) . ?
Mo3 O8 1.900(3) . ?
Mo3 O7 1.948(3) 2_656 ?
Mo3 O9 2.181(3) . ?
Mo3 O7 2.420(3) . ?
Mo4 O13 1.694(4) . ?
Mo4 O12 1.726(4) . ?
Mo4 O6 1.873(3) . ?
Mo4 O9 2.000(3) 2_656 ?
Mo4 O7 2.233(3) . ?
Mo4 O11 2.332(4) . ?
C1 N1 1.343(7) . ?
C1 C2 1.383(7) . ?
C1 H1 0.9300 . ?
C2 C3 1.387(7) . ?
C2 H2 0.9300 . ?
C3 C4 1.387(7) . ?
C3 C6 1.473(7) . ?
C4 C5 1.383(7) . ?
C4 H4 0.9300 . ?
C5 N1 1.344(7) . ?
C5 H5 0.9300 . ?
C6 N2 1.299(6) . ?
C6 N4 1.356(6) . ?
C7 N3 1.306(6) . ?
C7 N4 1.353(6) . ?
C7 C8 1.474(7) . ?
C8 C12 1.370(7) . ?
C8 C9 1.395(8) . ?
C9 C10 1.365(8) . ?
C9 H9 0.9300 . ?
C10 N6 1.329(8) . ?
C10 H10 0.9300 . ?
C11 N6 1.333(8) . ?
C11 C12 1.389(8) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
N2 N3 1.395(6) . ?
N2 Cu1 2.029(4) 2_665 ?
N3 Cu1 1.959(4) 1_565 ?
N4 N5 1.400(6) . ?
N5 H5A 0.8600 . ?
N5 H5B 0.8600 . ?
O2 Mo2 1.806(4) 2_666 ?
O7 Mo3 1.948(3) 2_656 ?
O9 Mo4 2.000(3) 2_656 ?
O1W H1WA 0.8506 . ?
O1W H1WB 0.8505 . ?
O2W H2WB 0.8500 . ?
O2W H2WB 0.8500 . ?
O2W H2WA 0.8500 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2W H2WA N5 0.85 2.36 3.193(9) 168.1 2_766
O2W H2WB O12 0.85 2.54 3.034(9) 118.3 .
O1W H1WB N5 0.85 2.57 3.004(7) 112.5 1_445
O1W H1WB N4 0.85 2.45 3.153(7) 140.9 1_445
O1W H1WA O2W 0.85 2.62 3.438(11) 161.2 2_656
