#------------------------------------------------------------------------------
#$Date: 2017-06-15 07:02:21 +0200 (jue 15 de jun de 2017) $
#$Revision: 197843 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/84/7228473.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_7228473
loop_
_publ_author_name
'Tian, Aixiang'
'Ni, Huaiping'
'Ji, Xuebin'
'Tian, Yan'
'Liu, Guocheng'
'Ying, Jun'
_publ_section_title
;
 Influence of pendant 2-[1,2,4]triazol-4-yl-ethylamine and symmetrical
 bis(pyrazol) ligands on dimensional extension of POM-based compounds
;
_journal_issue                   49
_journal_name_full               'RSC Adv.'
_journal_page_first              30573
_journal_paper_doi               10.1039/C7RA03884D
_journal_volume                  7
_journal_year                    2017
_chemical_formula_sum            'C4 H10 Ag Mo4 N4 O13'
_chemical_formula_weight         813.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-02-06 deposited with the CCDC.
2017-06-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.9570(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1653(5)
_cell_length_b                   12.4265(6)
_cell_length_c                   12.5934(6)
_cell_measurement_reflns_used    8783
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.32
_cell_volume                     1566.83(13)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10966
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.312
_diffrn_reflns_theta_min         2.320
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.420
_exptl_absorpt_correction_T_max  0.515
_exptl_absorpt_correction_T_min  0.449
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    3.441
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       black
_exptl_crystal_F_000             1516
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.150
_refine_diff_density_max         2.958
_refine_diff_density_min         -2.785
_refine_diff_density_rms         0.145
_refine_ls_extinction_coef       0.00490(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         3913
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0280
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0246P)²+9.2664P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0649
_refine_ls_wR_factor_ref         0.0668
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3604
_reflns_number_total             3913
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7ra03884d2.cif
_cod_data_source_block           compound-4
_cod_database_code               7228473
_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   0.487
_shelx_estimated_absorpt_t_max   0.557
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
Mo1 Mo -0.04475(3) 0.12971(3) 0.30673(3) 0.01590(9) Uani 1 1 d . .
Ag1 Ag -0.46404(4) 0.03297(5) 0.14005(3) 0.04716(14) Uani 1 1 d . .
O1 O -0.3839(3) 0.0712(3) 0.3200(2) 0.0245(6) Uani 1 1 d . .
N1 N -0.3222(4) -0.0724(3) 0.0677(3) 0.0291(8) Uani 1 1 d . .
C1 C -0.2078(5) -0.1179(4) 0.1059(4) 0.0331(10) Uani 1 1 d . .
H1A H -0.1667 -0.1163 0.1778 0.040 Uiso 1 1 calc R U
Mo2 Mo -0.23994(3) -0.00442(3) 0.67893(3) 0.01627(9) Uani 1 1 d . .
O2 O -0.1321(3) 0.1423(2) 0.4371(2) 0.0156(5) Uani 1 1 d . .
N2 N -0.3481(3) -0.0938(3) -0.0417(3) 0.0243(7) Uani 1 1 d . .
C2 C -0.2489(4) -0.1510(4) -0.0634(3) 0.0248(8) Uani 1 1 d . .
H2A H -0.2416 -0.1769 -0.1315 0.030 Uiso 1 1 calc R U
O5 O -0.3129(3) 0.0601(3) 0.7728(2) 0.0269(6) Uani 1 1 d . .
Mo3 Mo -0.00070(3) -0.12562(2) 0.43307(2) 0.01318(8) Uani 1 1 d . .
O3 O -0.1075(3) 0.1391(2) 0.6603(2) 0.0192(5) Uani 1 1 d . .
N3 N -0.1578(3) -0.1674(3) 0.0268(3) 0.0233(7) Uani 1 1 d . .
Mo4 Mo -0.28272(3) -0.00016(3) 0.41782(3) 0.01489(9) Uani 1 1 d . .
O4 O -0.0988(3) -0.0464(2) 0.5486(2) 0.0153(5) Uani 1 1 d . .
C3 C -0.0272(4) -0.2201(4) 0.0346(5) 0.0331(11) Uani 1 1 d . .
H3A H -0.0287 -0.2702 -0.0247 0.040 Uiso 1 1 calc R U
H3B H -0.0068 -0.2600 0.1017 0.040 Uiso 1 1 calc R U
C4 C 0.0774(4) -0.1351(3) 0.0307(4) 0.0229(8) Uani 1 1 d . .
H4A H 0.0559 -0.0951 -0.0362 0.027 Uiso 1 1 calc R U
H4B H 0.0779 -0.0851 0.0899 0.027 Uiso 1 1 calc R U
O6 O -0.1742(3) 0.1486(3) 0.2034(2) 0.0272(7) Uani 1 1 d . .
N4 N 0.2115(3) -0.1847(3) 0.0381(3) 0.0260(8) Uani 1 1 d . .
H4C H 0.2205 -0.2534 0.0438 0.031 Uiso 1 1 calc R U
H4D H 0.2803 -0.1447 0.0368 0.031 Uiso 1 1 calc R U
O7 O -0.0823(3) -0.2445(2) 0.4282(2) 0.0220(6) Uani 1 1 d . .
O8 O 0.0383(3) 0.2484(3) 0.3227(3) 0.0296(7) Uani 1 1 d . .
O9 O -0.3288(3) 0.0562(2) 0.5454(2) 0.0198(6) Uani 1 1 d . .
O10 O -0.3500(3) -0.1253(2) 0.4142(3) 0.0249(6) Uani 1 1 d . .
O11 O -0.0705(3) -0.0457(2) 0.7644(2) 0.0202(6) Uani 1 1 d . .
O13 O -0.1327(3) -0.0372(2) 0.3404(2) 0.0160(5) Uani 1 1 d . .
O14 O -0.3101(3) -0.1298(3) 0.6684(3) 0.0259(6) 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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -0.8971 1.1015 '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
O8 Mo1 O6 105.94(16) . .
O8 Mo1 O11 101.48(15) . 3_556
O6 Mo1 O11 99.98(14) . 3_556
O8 Mo1 O2 96.71(14) . .
O6 Mo1 O2 102.85(13) . .
O11 Mo1 O2 145.51(11) 3_556 .
O8 Mo1 O13 162.53(13) . .
O6 Mo1 O13 89.52(13) . .
O11 Mo1 O13 83.33(11) 3_556 .
O2 Mo1 O13 71.43(10) . .
O8 Mo1 O4 93.51(13) . 3_556
O6 Mo1 O4 160.50(13) . 3_556
O11 Mo1 O4 76.97(10) 3_556 3_556
O2 Mo1 O4 72.86(10) . 3_556
O13 Mo1 O4 71.03(9) . 3_556
N2 Ag1 N1 121.40(13) 3_455 .
N2 Ag1 O1 126.70(12) 3_455 .
N1 Ag1 O1 111.86(12) . .
Mo4 O1 Ag1 131.57(17) . .
C1 N1 N2 106.7(4) . .
C1 N1 Ag1 133.9(3) . .
N2 N1 Ag1 119.3(3) . .
N1 C1 N3 110.6(4) . .
O5 Mo2 O14 104.92(16) . .
O5 Mo2 O9 103.15(14) . .
O14 Mo2 O9 99.36(14) . .
O5 Mo2 O11 101.05(13) . .
O14 Mo2 O11 96.95(14) . .
O9 Mo2 O11 146.08(12) . .
O5 Mo2 O3 92.23(13) . .
O14 Mo2 O3 162.71(13) . .
O9 Mo2 O3 78.40(11) . .
O11 Mo2 O3 77.25(11) . .
O5 Mo2 O4 162.79(13) . .
O14 Mo2 O4 92.25(12) . .
O9 Mo2 O4 74.61(10) . .
O11 Mo2 O4 75.22(10) . .
O3 Mo2 O4 70.56(9) . .
Mo3 O2 Mo1 109.83(12) 3_556 .
Mo3 O2 Mo4 110.84(12) 3_556 .
Mo1 O2 Mo4 103.41(11) . .
C2 N2 N1 107.0(3) . .
C2 N2 Ag1 133.8(3) . 3_455
N1 N2 Ag1 119.2(3) . 3_455
N2 C2 N3 110.4(4) . .
O7 Mo3 O3 104.66(14) . 3_556
O7 Mo3 O2 101.69(13) . 3_556
O3 Mo3 O2 97.39(12) 3_556 3_556
O7 Mo3 O13 100.80(13) . .
O3 Mo3 O13 95.70(12) 3_556 .
O2 Mo3 O13 150.11(11) 3_556 .
O7 Mo3 O4 98.22(12) . .
O3 Mo3 O4 157.05(12) 3_556 .
O2 Mo3 O4 79.33(10) 3_556 .
O13 Mo3 O4 78.18(10) . .
O7 Mo3 O4 174.29(12) . 3_556
O3 Mo3 O4 81.01(11) 3_556 3_556
O2 Mo3 O4 77.92(10) 3_556 3_556
O13 Mo3 O4 77.75(10) . 3_556
O4 Mo3 O4 76.09(11) . 3_556
Mo3 O3 Mo2 116.52(14) 3_556 .
C1 N3 C2 105.2(4) . .
C1 N3 C3 127.4(4) . .
C2 N3 C3 127.2(4) . .
O10 Mo4 O1 105.47(15) . .
O10 Mo4 O9 101.82(14) . .
O1 Mo4 O9 102.39(13) . .
O10 Mo4 O13 96.52(13) . .
O1 Mo4 O13 100.52(13) . .
O9 Mo4 O13 145.47(11) . .
O10 Mo4 O2 162.88(12) . .
O1 Mo4 O2 89.07(12) . .
O9 Mo4 O2 83.36(11) . .
O13 Mo4 O2 71.50(10) . .
O10 Mo4 O4 93.59(12) . .
O1 Mo4 O4 160.49(13) . .
O9 Mo4 O4 77.12(10) . .
O13 Mo4 O4 72.72(10) . .
O2 Mo4 O4 71.46(9) . .
Mo3 O4 Mo4 92.50(9) . .
Mo3 O4 Mo3 103.91(11) . 3_556
Mo4 O4 Mo3 97.07(10) . 3_556
Mo3 O4 Mo1 91.39(9) . 3_556
Mo4 O4 Mo1 163.91(13) . 3_556
Mo3 O4 Mo1 97.13(9) 3_556 3_556
Mo3 O4 Mo2 164.18(13) . .
Mo4 O4 Mo2 85.95(9) . .
Mo3 O4 Mo2 91.89(9) 3_556 .
Mo1 O4 Mo2 86.06(8) 3_556 .
N3 C3 C4 108.7(4) . .
N4 C4 C3 110.7(3) . .
Mo4 O9 Mo2 116.89(14) . .
Mo1 O11 Mo2 116.35(13) 3_556 .
Mo3 O13 Mo4 109.93(12) . .
Mo3 O13 Mo1 111.34(11) . .
Mo4 O13 Mo1 103.46(12) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 O8 1.694(3) .
Mo1 O6 1.699(3) .
Mo1 O11 1.905(3) 3_556
Mo1 O2 2.004(3) .
Mo1 O13 2.327(3) .
Mo1 O4 2.367(3) 3_556
Ag1 N2 2.221(4) 3_455
Ag1 N1 2.253(4) .
Ag1 O1 2.320(3) .
O1 Mo4 1.710(3) .
N1 C1 1.308(6) .
N1 N2 1.384(5) .
C1 N3 1.343(6) .
Mo2 O5 1.701(3) .
Mo2 O14 1.709(3) .
Mo2 O9 1.920(3) .
Mo2 O11 1.936(3) .
Mo2 O3 2.271(3) .
Mo2 O4 2.416(3) .
O2 Mo3 1.943(3) 3_556
O2 Mo4 2.326(3) .
N2 C2 1.301(6) .
N2 Ag1 2.221(4) 3_455
C2 N3 1.351(5) .
Mo3 O7 1.690(3) .
Mo3 O3 1.751(3) 3_556
Mo3 O2 1.943(3) 3_556
Mo3 O13 1.956(3) .
Mo3 O4 2.141(3) .
Mo3 O4 2.359(3) 3_556
O3 Mo3 1.751(3) 3_556
N3 C3 1.468(5) .
Mo4 O10 1.697(3) .
Mo4 O9 1.885(3) .
Mo4 O13 2.001(3) .
Mo4 O4 2.339(3) .
O4 Mo3 2.359(3) 3_556
O4 Mo1 2.366(3) 3_556
C3 C4 1.506(6) .
C4 N4 1.484(5) .
O11 Mo1 1.905(3) 3_556
