#------------------------------------------------------------------------------
#$Date: 2023-12-22 17:07:40 +0200 (Fri, 22 Dec 2023) $
#$Revision: 288505 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/48/4344853.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_4344853
loop_
_publ_author_name
'Lysenko, Andrey B.'
'Senchyk, Ganna A.'
'Lukashuk, Liliana V.'
'Domasevitch, Konstantin V.'
'Handke, Marcel'
'Lincke, Jörg'
'Krautscheid, Harald'
'Rusanov, Eduard B.'
'Krämer, Karl W'
'Decurtins, Silvio'
'Liu, Shi-Xia'
_publ_section_title
;
 Composition Space Analysis in the Development of Copper Molybdate Hybrids
 Decorated by a Bifunctional Pyrazolyl/1,2,4-Triazole Ligand.
;
_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              239
_journal_paper_doi               10.1021/acs.inorgchem.5b02188
_journal_volume                  55
_journal_year                    2015
_chemical_formula_moiety         'C7 H9 Mo2 N5 O6, H2 O'
_chemical_formula_sum            'C7 H11 Mo2 N5 O7'
_chemical_formula_weight         469.09
_chemical_name_systematic
;
poly[di-μ-oxido-[4-(3,5-Dimethylpyrazol-4-yl)-1,2,4-triazole-
κ⁴N1:N2]-tetraoxodimolybdenum(VI)] Monohydrate
;
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                76.813(10)
_cell_angle_beta                 85.869(11)
_cell_angle_gamma                64.911(10)
_cell_formula_units_Z            2
_cell_length_a                   7.3278(9)
_cell_length_b                   8.2854(10)
_cell_length_c                   12.8319(11)
_cell_measurement_reflns_used    6588
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      2.78
_cell_volume                     686.69(15)
_computing_cell_refinement       'IPDS Software (Stoe & Cie, 2000)'
_computing_data_collection       'IPDS Software (Stoe & Cie, 2000)'
_computing_data_reduction        'IPDS Software (Stoe & Cie, 2000)'
_computing_molecular_graphics    'Diamond 2.1e (Brandenburg, 1999)'
_computing_publication_material  'WinGX 1.70.01 (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Stoe Imaging plate diffraction system'
_diffrn_measurement_method       'φ oscillation 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  0.0551
_diffrn_reflns_av_sigmaI/netI    0.0435
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6588
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         2.78
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.868
_exptl_absorpt_correction_T_max  0.7343
_exptl_absorpt_correction_T_min  0.6864
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'X-RED (Stoe & Cie, 2001) and X-SHAPE (Stoe & Cie, 1999)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.269
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             456
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.865
_refine_diff_density_min         -0.966
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         3202
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0319
_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)+(0.0591P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0815
_refine_ls_wR_factor_ref         0.0832
_reflns_number_gt                2825
_reflns_number_total             3202
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b02188_si_002.cif
_cod_data_source_block           (6)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

The following automatic conversions were performed:

data name '_iucr_refine_instruction_details' was replaced with
'_iucr_refine_instructions_details' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_database_code               4344853
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
Mo1 Mo 0.18808(3) 0.88770(3) -0.078723(19) 0.01654(9) Uani 1 1 d . . .
Mo2 Mo 0.29764(3) 1.14928(3) 0.052865(19) 0.01725(9) Uani 1 1 d . . .
O1 O 0.4075(3) 0.9592(3) -0.06048(17) 0.0184(4) Uani 1 1 d . . .
O2 O 0.0625(3) 1.1151(3) 0.01607(17) 0.0195(4) Uani 1 1 d . . .
O3 O 0.3143(4) 0.6799(3) -0.10733(19) 0.0258(5) Uani 1 1 d . . .
O4 O 0.0965(3) 1.0295(3) -0.19998(18) 0.0247(5) Uani 1 1 d . . .
O5 O 0.2377(4) 1.2168(3) 0.1714(2) 0.0278(5) Uani 1 1 d . . .
O6 O 0.2533(4) 1.3455(3) -0.0394(2) 0.0283(5) Uani 1 1 d . . .
N1 N 0.2978(4) 0.7483(3) 0.1043(2) 0.0191(5) Uani 1 1 d . . .
N2 N 0.3488(4) 0.8531(3) 0.1560(2) 0.0198(5) Uani 1 1 d . . .
N3 N 0.3350(4) 0.6246(3) 0.2754(2) 0.0217(5) Uani 1 1 d . . .
N4 N 0.3843(5) 0.2840(4) 0.5184(2) 0.0274(6) Uani 1 1 d . . .
N5 N 0.2521(4) 0.4441(4) 0.5424(2) 0.0266(6) Uani 1 1 d . . .
H5 H 0.1985 0.4523 0.6056 0.040 Uiso 1 1 calc R . .
C1 C 0.2893(5) 0.6131(4) 0.1772(2) 0.0221(6) Uani 1 1 d . . .
H1 H 0.2561 0.5206 0.1637 0.027 Uiso 1 1 calc R . .
C2 C 0.3704(5) 0.7774(4) 0.2578(2) 0.0223(6) Uani 1 1 d . . .
H2 H 0.4055 0.8219 0.3117 0.027 Uiso 1 1 calc R . .
C3 C 0.5712(6) 0.1868(5) 0.3600(3) 0.0310(7) Uani 1 1 d . . .
H3A H 0.6237 0.0673 0.4097 0.047 Uiso 1 1 calc R . .
H3B H 0.6832 0.2181 0.3330 0.047 Uiso 1 1 calc R . .
H3C H 0.4994 0.1824 0.2999 0.047 Uiso 1 1 calc R . .
C4 C 0.4307(5) 0.3271(4) 0.4165(2) 0.0239(6) Uani 1 1 d . . .
C5 C 0.3249(5) 0.5172(4) 0.3783(2) 0.0221(6) Uani 1 1 d . . .
C6 C 0.2115(5) 0.5883(4) 0.4603(3) 0.0250(6) Uani 1 1 d . . .
C7 C 0.0693(6) 0.7786(5) 0.4670(3) 0.0330(8) Uani 1 1 d . . .
H7A H -0.0193 0.7746 0.5275 0.050 Uiso 1 1 calc R . .
H7B H -0.0122 0.8397 0.4005 0.050 Uiso 1 1 calc R . .
H7C H 0.1462 0.8462 0.4772 0.050 Uiso 1 1 calc R . .
O7 O 0.1073(7) 0.5166(7) 0.7440(3) 0.0502(11) Uani 0.75 1 d P A -1
H1W H -0.0006 0.6032 0.7570 0.075 Uiso 0.75 1 d PR A -1
H2W H 0.1683 0.4524 0.8032 0.075 Uiso 0.75 1 d PR A -1
O7A O 0.120(2) 0.396(3) 0.7512(10) 0.053(3) Uani 0.25 1 d P B -2
H3W H 0.1605 0.3945 0.8119 0.079 Uiso 0.25 1 d PR B -2
H4W H 0.1076 0.2971 0.7554 0.079 Uiso 0.25 1 d PR B -2
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'
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
O3 Mo1 O4 103.99(12) . .
O3 Mo1 O2 104.63(10) . 2_575
O4 Mo1 O2 99.74(10) . 2_575
O3 Mo1 O1 102.61(10) . .
O4 Mo1 O1 97.74(10) . .
O2 Mo1 O1 142.78(9) 2_575 .
O3 Mo1 O2 160.72(10) . .
O4 Mo1 O2 95.20(10) . .
O2 Mo1 O2 73.35(9) 2_575 .
O1 Mo1 O2 72.54(8) . .
O3 Mo1 N1 88.02(10) . .
O4 Mo1 N1 167.64(10) . .
O2 Mo1 N1 79.66(9) 2_575 .
O1 Mo1 N1 76.42(8) . .
O2 Mo1 N1 72.73(8) . .
O6 Mo2 O5 104.31(12) . .
O6 Mo2 O1 99.93(10) . 2_675
O5 Mo2 O1 101.92(10) . 2_675
O6 Mo2 O2 97.42(10) . .
O5 Mo2 O2 103.96(10) . .
O1 Mo2 O2 144.02(9) 2_675 .
O6 Mo2 O1 97.17(10) . .
O5 Mo2 O1 158.48(10) . .
O1 Mo2 O1 72.72(9) 2_675 .
O2 Mo2 O1 74.01(8) . .
O6 Mo2 N2 169.45(11) . .
O5 Mo2 N2 85.22(11) . .
O1 Mo2 N2 82.19(8) 2_675 .
O2 Mo2 N2 75.56(9) . .
O1 Mo2 N2 73.48(8) . .
Mo2 O1 Mo1 138.65(11) 2_675 .
Mo2 O1 Mo2 107.28(9) 2_675 .
Mo1 O1 Mo2 106.83(9) . .
Mo1 O2 Mo2 139.85(12) 2_575 .
Mo1 O2 Mo1 106.65(9) 2_575 .
Mo2 O2 Mo1 105.24(9) . .
C1 N1 N2 107.3(2) . .
C1 N1 Mo1 137.0(2) . .
N2 N1 Mo1 114.28(16) . .
C2 N2 N1 107.7(2) . .
C2 N2 Mo2 134.8(2) . .
N1 N2 Mo2 115.41(17) . .
C1 N3 C2 105.4(2) . .
C1 N3 C5 128.9(3) . .
C2 N3 C5 125.3(3) . .
C4 N4 N5 105.5(3) . .
C6 N5 N4 113.4(3) . .
C6 N5 H5 123.3 . .
N4 N5 H5 123.3 . .
N1 C1 N3 109.9(3) . .
N1 C1 H1 125.0 . .
N3 C1 H1 125.0 . .
N2 C2 N3 109.7(3) . .
N2 C2 H2 125.1 . .
N3 C2 H2 125.1 . .
C4 C3 H3A 109.5 . .
C4 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
C4 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
N4 C4 C5 108.6(3) . .
N4 C4 C3 121.9(3) . .
C5 C4 C3 129.5(3) . .
C6 C5 C4 107.7(3) . .
C6 C5 N3 124.1(3) . .
C4 C5 N3 128.1(3) . .
N5 C6 C5 104.7(3) . .
N5 C6 C7 123.3(3) . .
C5 C6 C7 132.0(3) . .
C6 C7 H7A 109.5 . .
C6 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C6 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
H1W O7 H2W 108.4 . .
H3W O7A H4W 108.4 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 O3 1.686(2) .
Mo1 O4 1.703(2) .
Mo1 O2 1.958(2) 2_575
Mo1 O1 1.979(2) .
Mo1 O2 2.300(2) .
Mo1 N1 2.396(3) .
Mo2 O6 1.697(2) .
Mo2 O5 1.704(2) .
Mo2 O1 1.957(2) 2_675
Mo2 O2 1.966(2) .
Mo2 O1 2.246(2) .
Mo2 N2 2.392(2) .
O1 Mo2 1.957(2) 2_675
O2 Mo1 1.958(2) 2_575
N1 C1 1.306(4) .
N1 N2 1.382(4) .
N2 C2 1.303(4) .
N3 C1 1.360(4) .
N3 C2 1.364(4) .
N3 C5 1.431(4) .
N4 C4 1.334(4) .
N4 N5 1.359(4) .
N5 C6 1.340(4) .
N5 H5 0.8800 .
C1 H1 0.9500 .
C2 H2 0.9500 .
C3 C4 1.482(5) .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
C4 C5 1.411(4) .
C5 C6 1.374(5) .
C6 C7 1.495(5) .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
O7 H1W 0.8500 .
O7 H2W 0.8500 .
O7A H3W 0.8500 .
O7A H4W 0.8500 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O3 Mo1 O1 Mo2 -7.80(19) . 2_675
O4 Mo1 O1 Mo2 -114.09(18) . 2_675
O2 Mo1 O1 Mo2 128.45(16) 2_575 2_675
O2 Mo1 O1 Mo2 152.87(19) . 2_675
N1 Mo1 O1 Mo2 77.00(17) . 2_675
O3 Mo1 O1 Mo2 -152.22(10) . .
O4 Mo1 O1 Mo2 101.49(11) . .
O2 Mo1 O1 Mo2 -15.97(18) 2_575 .
O2 Mo1 O1 Mo2 8.45(7) . .
N1 Mo1 O1 Mo2 -67.42(9) . .
O6 Mo2 O1 Mo2 98.21(11) . 2_675
O5 Mo2 O1 Mo2 -78.5(3) . 2_675
O1 Mo2 O1 Mo2 0.0 2_675 2_675
O2 Mo2 O1 Mo2 -166.08(11) . 2_675
N2 Mo2 O1 Mo2 -86.78(10) . 2_675
O6 Mo2 O1 Mo1 -105.52(11) . .
O5 Mo2 O1 Mo1 77.8(3) . .
O1 Mo2 O1 Mo1 156.26(15) 2_675 .
O2 Mo2 O1 Mo1 -9.82(8) . .
N2 Mo2 O1 Mo1 69.49(10) . .
O6 Mo2 O2 Mo1 -114.66(18) . 2_575
O5 Mo2 O2 Mo1 -7.8(2) . 2_575
O1 Mo2 O2 Mo1 126.95(17) 2_675 2_575
O1 Mo2 O2 Mo1 149.96(19) . 2_575
N2 Mo2 O2 Mo1 73.36(17) . 2_575
O6 Mo2 O2 Mo1 103.75(11) . .
O5 Mo2 O2 Mo1 -149.44(10) . .
O1 Mo2 O2 Mo1 -14.64(19) 2_675 .
O1 Mo2 O2 Mo1 8.37(7) . .
N2 Mo2 O2 Mo1 -68.23(9) . .
O3 Mo1 O2 Mo1 -86.8(3) . 2_575
O4 Mo1 O2 Mo1 98.63(11) . 2_575
O2 Mo1 O2 Mo1 0.0 2_575 2_575
O1 Mo1 O2 Mo1 -164.87(12) . 2_575
N1 Mo1 O2 Mo1 -84.08(10) . 2_575
O3 Mo1 O2 Mo2 68.5(3) . .
O4 Mo1 O2 Mo2 -106.09(11) . .
O2 Mo1 O2 Mo2 155.28(15) 2_575 .
O1 Mo1 O2 Mo2 -9.59(8) . .
N1 Mo1 O2 Mo2 71.20(10) . .
O3 Mo1 N1 C1 -54.8(3) . .
O4 Mo1 N1 C1 138.8(4) . .
O2 Mo1 N1 C1 50.5(3) 2_575 .
O1 Mo1 N1 C1 -158.2(3) . .
O2 Mo1 N1 C1 126.1(3) . .
O3 Mo1 N1 N2 141.36(19) . .
O4 Mo1 N1 N2 -25.1(5) . .
O2 Mo1 N1 N2 -113.38(19) 2_575 .
O1 Mo1 N1 N2 37.88(18) . .
O2 Mo1 N1 N2 -37.76(18) . .
C1 N1 N2 C2 0.4(3) . .
Mo1 N1 N2 C2 168.9(2) . .
C1 N1 N2 Mo2 -165.5(2) . .
Mo1 N1 N2 Mo2 3.1(2) . .
O6 Mo2 N2 C2 -170.1(5) . .
O5 Mo2 N2 C2 -15.2(3) . .
O1 Mo2 N2 C2 87.5(3) 2_675 .
O2 Mo2 N2 C2 -121.0(3) . .
O1 Mo2 N2 C2 161.8(3) . .
O6 Mo2 N2 N1 -9.3(6) . .
O5 Mo2 N2 N1 145.6(2) . .
O1 Mo2 N2 N1 -111.6(2) 2_675 .
O2 Mo2 N2 N1 39.87(19) . .
O1 Mo2 N2 N1 -37.41(18) . .
C4 N4 N5 C6 0.0(4) . .
N2 N1 C1 N3 -0.6(3) . .
Mo1 N1 C1 N3 -165.2(2) . .
C2 N3 C1 N1 0.6(3) . .
C5 N3 C1 N1 173.2(3) . .
N1 N2 C2 N3 0.0(3) . .
Mo2 N2 C2 N3 161.8(2) . .
C1 N3 C2 N2 -0.3(3) . .
C5 N3 C2 N2 -173.3(3) . .
N5 N4 C4 C5 0.2(4) . .
N5 N4 C4 C3 -179.3(3) . .
N4 C4 C5 C6 -0.3(4) . .
C3 C4 C5 C6 179.1(4) . .
N4 C4 C5 N3 177.0(3) . .
C3 C4 C5 N3 -3.5(6) . .
C1 N3 C5 C6 -122.0(4) . .
C2 N3 C5 C6 49.3(5) . .
C1 N3 C5 C4 61.0(5) . .
C2 N3 C5 C4 -127.7(4) . .
N4 N5 C6 C5 -0.2(4) . .
N4 N5 C6 C7 179.5(3) . .
C4 C5 C6 N5 0.3(4) . .
N3 C5 C6 N5 -177.2(3) . .
C4 C5 C6 C7 -179.3(4) . .
N3 C5 C6 C7 3.2(6) . .
