#------------------------------------------------------------------------------
#$Date: 2019-05-28 05:36:33 +0300 (Tue, 28 May 2019) $
#$Revision: 215561 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/84/7058422.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_7058422
loop_
_publ_author_name
'Tian, Aixiang'
'Fu, Yubo'
'Cui, Hongtao'
'Ying, Jun'
'Yang, Mengle'
'Yang, Yan'
'Wang, Xiuli'
_publ_section_title
;
 A series of metal-organic loops templated by [SiMo12O40]4- and
 [β-Mo8O26]4- anions by using double chelate ligands: amperometric
 sensoring and selective photocatalytic properties
;
_journal_name_full               'New Journal of Chemistry'
_journal_paper_doi               10.1039/C9NJ02224D
_journal_year                    2019
_chemical_formula_moiety         'C56 H40 Ag4 N16, Mo12 O40 Si'
_chemical_formula_sum            'C56 H40 Ag4 Mo12 N16 O40 Si'
_chemical_formula_weight         3187.89
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a'
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-05-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-05-16 deposited with the CCDC.    2019-05-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.1326(10)
_cell_length_b                   23.1326(10)
_cell_length_c                   14.8376(8)
_cell_measurement_reflns_used    5181
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.979
_cell_measurement_theta_min      2.400
_cell_volume                     7939.9(6)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22512
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.072
_diffrn_reflns_theta_min         1.630
_exptl_absorpt_coefficient_mu    2.903
_exptl_absorpt_correction_T_max  0.647
_exptl_absorpt_correction_T_min  0.578
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.667
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6056
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.931
_refine_diff_density_min         -1.225
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         3521
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0300
_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)+(0.0277P)²+61.9805P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0682
_refine_ls_wR_factor_ref         0.0747
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2799
_reflns_number_total             3521
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9nj02224d2.cif
_cod_data_source_block           2
_cod_original_cell_volume        7939.9(8)
_cod_database_code               7058422
_shelxl_version_number           2014/6
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C6(H6), C65(H65), C13(H13), C14(H14),
 C15(H15), C20(H20)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y+1/2, z'
'-y+3/4, x+1/4, z+1/4'
'y+1/4, -x+1/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'y+3/4, -x+3/4, z+3/4'
'-x, -y, -z'
'x, y-1/2, -z'
'y-3/4, -x-1/4, -z-1/4'
'-y-1/4, x-1/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'-y+1/4, x+1/4, -z+1/4'
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
Ag1 Ag 0.52564(2) 0.03136(2) 0.29421(4) 0.05368(17) Uani 1 1 d . . .
Si1 Si 0.5000 0.2500 -0.1250 0.0185(6) Uani 1 4 d S T P
O1 O 0.47800(15) 0.11393(15) -0.2020(3) 0.0320(9) Uani 1 1 d . . .
N1 N 0.4588(2) 0.1074(3) 0.3542(4) 0.0536(15) Uani 1 1 d . . .
C1 C 0.4226(3) 0.1689(3) 0.4672(4) 0.0495(17) Uani 1 1 d . . .
H1 H 0.4304 0.1965 0.5112 0.059 Uiso 1 1 calc R . .
Mo5 Mo 0.52588(2) 0.14597(2) -0.29341(4) 0.03065(14) Uani 1 1 d . . .
O2 O 0.44975(16) 0.17323(16) 0.1047(2) 0.0322(9) Uani 1 1 d . . .
N2 N 0.44084(18) 0.02579(19) 0.2231(3) 0.0314(11) Uani 1 1 d . . .
C2 C 0.4380(2) -0.0026(2) 0.1450(4) 0.0346(13) Uani 1 1 d . . .
H2 H 0.4658 -0.0307 0.1336 0.042 Uiso 1 1 calc R . .
Mo3 Mo 0.41530(2) 0.12332(2) -0.11775(3) 0.02881(13) Uani 1 1 d . . .
O3 O 0.37000(15) 0.15680(15) -0.0224(3) 0.0331(9) Uani 1 1 d . . .
C3 C 0.6253(3) -0.0492(3) 0.3645(5) 0.0468(16) Uani 1 1 d . . .
H3 H 0.5981 -0.0774 0.3507 0.056 Uiso 1 1 calc R . .
Mo4 Mo 0.51532(2) 0.14247(2) 0.04216(3) 0.02675(13) Uani 1 1 d . . .
O4 O 0.55716(16) 0.21160(15) 0.0745(3) 0.0324(9) Uani 1 1 d . . .
C4 C 0.3565(2) 0.0493(2) 0.0962(4) 0.0354(13) Uani 1 1 d . . .
H4 H 0.3289 0.0582 0.0527 0.042 Uiso 1 1 calc R . .
C5 C 0.3582(2) 0.1190(2) 0.3783(4) 0.0327(13) Uani 1 1 d . . .
C6 C 0.4671(3) 0.1412(3) 0.4251(5) 0.059(2) Uani 1 1 d . . .
H6 H 0.5045 0.1462 0.4468 0.071 Uiso 1 1 calc R . .
O6 O 0.37648(17) 0.06326(17) -0.1381(3) 0.0418(10) Uani 1 1 d . . .
O7 O 0.46823(14) 0.20234(14) -0.0620(2) 0.0250(8) Uani 1 1 d . . .
C8 C 0.4044(2) 0.0975(2) 0.3267(4) 0.0335(13) Uani 1 1 d . . .
N10 N 0.3680(2) 0.1566(2) 0.4454(3) 0.0438(13) Uani 1 1 d . . .
O10 O 0.46640(15) 0.09306(15) -0.0254(2) 0.0300(8) Uani 1 1 d . . .
O11 O 0.38419(15) 0.17622(15) -0.2007(3) 0.0311(8) Uani 1 1 d . . .
C11 C 0.3996(2) 0.0654(2) 0.2396(4) 0.0294(12) Uani 1 1 d . . .
C65 C 0.6800(3) -0.0671(3) 0.3868(5) 0.0461(16) Uani 1 1 d . . .
H65 H 0.6892 -0.1062 0.3897 0.055 Uiso 1 1 calc R . .
C12 C 0.6486(2) 0.0466(2) 0.3810(4) 0.0326(13) Uani 1 1 d . . .
N13 N 0.6084(2) 0.0060(2) 0.3614(4) 0.0403(12) Uani 1 1 d . . .
C13 C 0.7048(2) 0.0317(3) 0.4020(4) 0.0390(14) Uani 1 1 d . . .
H13 H 0.7319 0.0603 0.4145 0.047 Uiso 1 1 calc R . .
C14 C 0.7208(3) -0.0255(3) 0.4045(4) 0.0420(15) Uani 1 1 d . . .
H14 H 0.7587 -0.0359 0.4179 0.050 Uiso 1 1 calc R . .
C15 C 0.3573(2) 0.0789(2) 0.1770(4) 0.0339(13) Uani 1 1 d . . .
H15 H 0.3300 0.1074 0.1891 0.041 Uiso 1 1 calc R . .
C20 C 0.3964(2) 0.0070(2) 0.0803(4) 0.0367(14) Uani 1 1 d . . .
H20 H 0.3956 -0.0146 0.0275 0.044 Uiso 1 1 calc R . .
O40 O 0.52286(18) 0.09403(18) -0.3734(3) 0.0466(11) Uani 1 1 d . . .
O41 O 0.53975(17) 0.09501(17) 0.1196(3) 0.0381(10) 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'
Si Si 0.0817 0.0704 '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
N1 Ag1 N10 78.79(17) . 12_656
N2 Ag1 N1 70.50(16) . .
N2 Ag1 N10 127.93(16) . 12_656
N2 Ag1 N13 161.50(17) . .
N13 Ag1 N1 123.63(18) . .
N13 Ag1 N10 69.66(16) . 12_656
O7 Si1 O7 109.41(12) 2_655 11_665
O7 Si1 O7 109.41(12) . 12_655
O7 Si1 O7 109.41(12) 2_655 12_655
O7 Si1 O7 109.41(12) . 11_665
O7 Si1 O7 109.6(2) 11_665 12_655
O7 Si1 O7 109.6(2) . 2_655
Mo5 O1 Mo3 149.0(2) . .
C6 N1 Ag1 127.4(5) . .
C6 N1 C8 118.5(6) . .
C8 N1 Ag1 110.5(4) . .
N10 C1 C6 120.2(6) . .
O1 Mo5 O2 159.76(16) . 12_655
O1 Mo5 O3 89.29(15) . 12_655
O1 Mo5 O7 85.84(14) . 12_655
O2 Mo5 O7 74.04(13) 12_655 12_655
O3 Mo5 O2 86.99(16) 12_655 12_655
O3 Mo5 O7 73.22(13) 12_655 12_655
O4 Mo5 O1 86.53(15) 11_665 .
O4 Mo5 O2 89.72(16) 11_665 12_655
O4 Mo5 O3 158.65(16) 11_665 12_655
O4 Mo5 O7 85.59(14) 11_665 12_655
O40 Mo5 O1 101.51(19) . .
O40 Mo5 O2 98.72(19) . 12_655
O40 Mo5 O3 99.62(18) . 12_655
O40 Mo5 O4 101.74(19) . 11_665
O40 Mo5 O7 169.83(16) . 12_655
Mo4 O2 Mo5 120.39(19) . 11_665
C2 N2 Ag1 118.8(4) . .
C2 N2 C11 117.3(5) . .
C11 N2 Ag1 119.9(4) . .
N2 C2 C20 124.0(5) . .
O1 Mo3 O7 85.64(14) . .
O1 Mo3 O10 87.65(15) . .
O3 Mo3 O1 158.85(15) . .
O3 Mo3 O7 73.25(13) . .
O3 Mo3 O10 87.59(16) . .
O6 Mo3 O1 101.09(18) . .
O6 Mo3 O3 100.01(18) . .
O6 Mo3 O7 169.69(17) . .
O6 Mo3 O10 98.86(17) . .
O6 Mo3 O11 102.48(18) . .
O10 Mo3 O7 73.42(13) . .
O11 Mo3 O1 86.37(15) . .
O11 Mo3 O3 90.60(16) . .
O11 Mo3 O7 85.61(14) . .
O11 Mo3 O10 158.56(15) . .
Mo3 O3 Mo5 121.77(19) . 11_665
N13 C3 C65 124.5(6) . .
O2 Mo4 O4 88.22(16) . .
O2 Mo4 O7 74.46(14) . .
O2 Mo4 O11 159.19(15) . 12_655
O4 Mo4 O7 84.68(14) . .
O10 Mo4 O2 90.44(16) . .
O10 Mo4 O4 158.54(16) . .
O10 Mo4 O7 74.34(13) . .
O10 Mo4 O11 89.22(15) . 12_655
O11 Mo4 O4 84.56(15) 12_655 .
O11 Mo4 O7 85.43(14) 12_655 .
O41 Mo4 O2 100.19(18) . .
O41 Mo4 O4 101.66(17) . .
O41 Mo4 O7 171.71(16) . .
O41 Mo4 O10 99.66(17) . .
O41 Mo4 O11 100.38(18) . 12_655
Mo5 O4 Mo4 151.1(2) 12_655 .
C20 C4 C15 119.7(5) . .
C8 C5 C12 125.5(5) . 11_666
N10 C5 C8 120.2(5) . .
N10 C5 C12 114.1(5) . 11_666
N1 C6 C1 122.1(6) . .
Si1 O7 Mo5 124.17(17) . 11_665
Si1 O7 Mo3 124.19(18) . .
Si1 O7 Mo4 124.83(17) . .
Mo5 O7 Mo3 91.76(12) 11_665 .
Mo4 O7 Mo5 91.06(12) . 11_665
Mo4 O7 Mo3 90.84(11) . .
N1 C8 C5 119.2(5) . .
N1 C8 C11 114.7(5) . .
C5 C8 C11 126.1(5) . .
C1 N10 Ag1 126.7(4) . 11_666
C1 N10 C5 118.6(5) . .
C5 N10 Ag1 108.0(4) . 11_666
Mo4 O10 Mo3 121.32(18) . .
Mo3 O11 Mo4 151.8(2) . 11_665
N2 C11 C8 116.2(5) . .
N2 C11 C15 122.2(5) . .
C15 C11 C8 121.4(5) . .
C3 C65 C14 117.9(6) . .
N13 C12 C5 117.2(5) . 12_656
N13 C12 C13 121.4(5) . .
C13 C12 C5 121.2(5) . 12_656
C3 N13 Ag1 121.0(4) . .
C3 N13 C12 117.1(5) . .
C12 N13 Ag1 120.1(4) . .
C14 C13 C12 120.0(5) . .
C65 C14 C13 119.0(6) . .
C4 C15 C11 118.8(5) . .
C4 C20 C2 117.9(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ag1 N1 2.505(5) .
Ag1 N2 2.231(4) .
Ag1 N10 2.550(5) 12_656
Ag1 N13 2.237(5) .
Si1 O7 1.622(3) 11_665
Si1 O7 1.622(3) 12_655
Si1 O7 1.622(3) .
Si1 O7 1.622(3) 2_655
O1 Mo5 1.901(4) .
O1 Mo3 1.927(4) .
N1 C6 1.324(8) .
N1 C8 1.343(7) .
C1 C6 1.364(9) .
C1 N10 1.335(8) .
Mo5 O2 1.940(4) 12_655
Mo5 O3 1.934(4) 12_655
Mo5 O4 1.897(3) 11_665
Mo5 O7 2.344(3) 12_655
Mo5 O40 1.690(4) .
O2 Mo5 1.940(4) 11_665
O2 Mo4 1.915(4) .
N2 C2 1.333(7) .
N2 C11 1.346(7) .
C2 C20 1.377(8) .
Mo3 O3 1.923(4) .
Mo3 O6 1.682(4) .
Mo3 O7 2.350(3) .
Mo3 O10 1.940(4) .
Mo3 O11 1.879(4) .
O3 Mo5 1.934(4) 11_665
C3 C65 1.372(9) .
C3 N13 1.336(8) .
Mo4 O4 1.930(3) .
Mo4 O7 2.344(3) .
Mo4 O10 1.895(4) .
Mo4 O11 1.926(4) 12_655
Mo4 O41 1.686(4) .
O4 Mo5 1.897(3) 12_655
C4 C15 1.380(8) .
C4 C20 1.367(8) .
C5 C8 1.406(8) .
C5 N10 1.342(7) .
C5 C12 1.486(8) 11_666
O7 Mo5 2.344(3) 11_665
C8 C11 1.495(8) .
N10 Ag1 2.550(5) 11_666
O11 Mo4 1.926(4) 11_665
C11 C15 1.383(8) .
C65 C14 1.373(9) .
C12 C5 1.486(8) 12_656
C12 N13 1.352(7) .
C12 C13 1.382(8) .
C13 C14 1.374(8) .
