#------------------------------------------------------------------------------
#$Date: 2019-05-28 05:36:33 +0300 (Tue, 28 May 2019) $
#$Revision: 215561 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/84/7058426.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_7058426
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         'C18 H12 Cu Mo4 N4 O13'
_chemical_formula_sum            'C18 H12 Cu Mo4 N4 O13'
_chemical_formula_weight         939.62
_chemical_name_systematic
;
 ? 
;
_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_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                78.004(7)
_cell_angle_beta                 88.814(7)
_cell_angle_gamma                84.759(7)
_cell_formula_units_Z            2
_cell_length_a                   10.247(4)
_cell_length_b                   10.682(4)
_cell_length_c                   11.424(5)
_cell_measurement_reflns_used    1300
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.546
_cell_measurement_theta_min      2.382
_cell_volume                     1218.0(8)
_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 0.997
_diffrn_measured_fraction_theta_max 0.981
_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  0.0390
_diffrn_reflns_av_unetI/netI     0.0818
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6732
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.784
_diffrn_reflns_theta_min         1.822
_exptl_absorpt_coefficient_mu    2.938
_exptl_absorpt_correction_T_max  0.683
_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    2.562
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             898
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.566
_refine_diff_density_min         -1.002
_refine_diff_density_rms         0.205
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         4577
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.0963
_refine_ls_R_factor_gt           0.0490
_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)+(0.0609P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1069
_refine_ls_wR_factor_ref         0.1284
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2864
_reflns_number_total             4577
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9nj02224d2.cif
_cod_data_source_block           f
_cod_original_cell_volume        1218.1(8)
_cod_database_code               7058426
_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:
 C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C12(H12), C13(H13), C14(H14),
 C18(H18), C19(H19), C20(H20), C25(H25)
;
_olex2_submission_special_instructions 'No special instructions were received'
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
Mo1 Mo 0.56442(7) 0.23247(7) 0.58556(7) 0.0211(2) Uani 1 1 d .
Cu1 Cu 0.81075(11) 0.15463(11) 0.81477(11) 0.0268(3) Uani 1 1 d .
O1 O 0.3255(6) 0.5757(6) 0.6951(6) 0.0270(15) Uani 1 1 d .
N1 N 0.7286(7) 0.0208(7) 0.9338(6) 0.0215(17) Uani 1 1 d .
C1 C 0.9574(9) 0.0761(9) 1.1690(9) 0.026(2) Uani 1 1 d .
Mo2 Mo 0.35315(7) 0.47396(7) 0.59394(7) 0.0210(2) Uani 1 1 d .
O2 O 0.4593(6) 0.3961(6) 0.4536(5) 0.0241(14) Uani 1 1 d .
N2 N 0.9091(7) 0.1675(7) 0.9602(7) 0.0218(17) Uani 1 1 d .
C2 C 1.0234(9) 0.3532(9) 0.8655(10) 0.032(2) Uani 1 1 d .
H2 H 0.9801 0.3571 0.7939 0.038 Uiso 1 1 calc R
Mo3 Mo 0.67587(8) 0.48289(7) 0.69267(7) 0.0219(2) Uani 1 1 d .
O3 O 0.7030(6) 0.4029(5) 0.5489(5) 0.0228(14) Uani 1 1 d .
C3 C 1.1106(10) 0.4401(9) 0.8727(10) 0.036(3) Uani 1 1 d .
H3 H 1.1267 0.5038 0.8064 0.044 Uiso 1 1 calc R
Mo4 Mo 0.46550(8) 0.72896(8) 0.70383(8) 0.0278(2) Uani 1 1 d .
N4 N 1.0448(8) 0.1566(8) 1.1731(8) 0.032(2) Uani 1 1 d .
C4 C 0.6366(9) -0.0510(9) 0.9065(9) 0.033(2) Uani 1 1 d .
H4 H 0.6044 -0.0346 0.8288 0.039 Uiso 1 1 calc R
C5 C 1.1769(10) 0.4326(10) 0.9823(11) 0.042(3) Uani 1 1 d .
H5 H 1.2363 0.4923 0.9867 0.050 Uiso 1 1 calc R
O6 O 0.7387(6) 0.3486(6) 0.7969(6) 0.0315(16) Uani 1 1 d .
C6 C 0.7799(8) -0.0038(8) 1.0463(8) 0.023(2) Uani 1 1 d .
O7 O 0.6859(6) 0.1549(6) 0.6883(6) 0.0259(15) Uani 1 1 d .
C7 C 0.9984(8) 0.2569(8) 0.9668(9) 0.023(2) Uani 1 1 d .
O8 O 0.4366(6) 0.1403(6) 0.6126(6) 0.0317(16) Uani 1 1 d .
C8 C 0.7335(10) -0.1006(9) 1.1336(9) 0.036(2) Uani 1 1 d .
H8 H 0.7656 -0.1162 1.2113 0.043 Uiso 1 1 calc R
O9 O 0.3675(6) 0.8007(6) 0.5593(6) 0.0289(15) Uani 1 1 d .
O10 O 0.8027(7) 0.5765(6) 0.6631(6) 0.0368(17) Uani 1 1 d .
O11 O 0.2306(6) 0.3765(6) 0.6205(6) 0.0334(16) Uani 1 1 d .
C11 C 0.8826(8) 0.0814(8) 1.0606(8) 0.023(2) Uani 1 1 d .
O12 O 0.5626(6) 0.5715(6) 0.7866(6) 0.0293(15) Uani 1 1 d .
C12 C 0.6395(10) -0.1733(9) 1.1044(9) 0.031(2) Uani 1 1 d .
H12 H 0.6099 -0.2398 1.1618 0.037 Uiso 1 1 calc R
C13 C 0.8522(9) -0.0840(11) 1.4783(10) 0.039(3) Uani 1 1 d .
H13 H 0.7922 -0.0690 1.5371 0.046 Uiso 1 1 calc R
O13 O 0.5924(7) 0.8234(6) 0.6809(7) 0.0421(19) Uani 1 1 d .
N14 N 1.0334(7) -0.1294(7) 1.3000(7) 0.0282(19) Uani 1 1 d .
C14 C 0.5896(10) -0.1473(10) 0.9904(9) 0.038(3) Uani 1 1 d .
H14 H 0.5247 -0.1946 0.9705 0.045 Uiso 1 1 calc R
O14 O 0.3726(7) 0.7804(7) 0.8130(6) 0.0447(19) Uani 1 1 d .
C18 C 0.9412(10) -0.1928(10) 1.4967(10) 0.038(3) Uani 1 1 d .
H18 H 0.9428 -0.2522 1.5690 0.046 Uiso 1 1 calc R
C19 C 0.8565(10) 0.0013(10) 1.3688(10) 0.038(3) Uani 1 1 d .
H19 H 0.7989 0.0752 1.3533 0.046 Uiso 1 1 calc R
O20 O 0.4979(5) 0.3644(5) 0.6799(5) 0.0225(14) Uani 1 1 d .
C20 C 1.0275(10) -0.2112(9) 1.4053(10) 0.035(3) Uani 1 1 d .
H20 H 1.0849 -0.2853 1.4181 0.042 Uiso 1 1 calc R
C21 C 0.9463(9) -0.0238(9) 1.2829(8) 0.024(2) Uani 1 1 d .
C22 C 1.0637(9) 0.2509(9) 1.0747(9) 0.028(2) Uani 1 1 d .
C25 C 1.1557(10) 0.3392(10) 1.0823(10) 0.041(3) Uani 1 1 d .
H25 H 1.2010 0.3347 1.1530 0.049 Uiso 1 1 calc 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
O2 Mo1 O3 73.0(2) . .
O7 Mo1 O2 157.1(3) . .
O7 Mo1 O3 84.4(2) . .
O7 Mo1 O9 102.3(3) . 2_666
O7 Mo1 O20 96.0(3) . .
O8 Mo1 O2 96.5(3) . .
O8 Mo1 O3 166.0(3) . .
O8 Mo1 O7 105.2(3) . .
O8 Mo1 O9 103.3(3) . 2_666
O8 Mo1 O20 97.3(3) . .
O9 Mo1 O2 79.2(2) 2_666 .
O9 Mo1 O3 84.1(2) 2_666 .
O9 Mo1 O20 147.5(3) 2_666 .
O20 Mo1 O2 73.7(2) . .
O20 Mo1 O3 71.2(2) . .
N1 Cu1 N2 81.1(3) . .
N1 Cu1 O6 119.3(3) . .
N1 Cu1 N14 128.0(3) . 2_757
N2 Cu1 O6 89.1(3) . .
N2 Cu1 N14 99.9(3) . 2_757
O7 Cu1 N1 94.5(3) . .
O7 Cu1 N2 169.1(3) . .
O7 Cu1 O6 84.3(2) . .
O7 Cu1 N14 90.7(3) . 2_757
N14 Cu1 O6 112.7(3) 2_757 .
Mo2 O1 Mo4 120.6(3) . .
C4 N1 Cu1 124.0(6) . .
C4 N1 C6 120.2(8) . .
C6 N1 Cu1 115.5(6) . .
N4 C1 C11 121.5(9) . .
N4 C1 C21 114.2(9) . .
C11 C1 C21 124.2(8) . .
O1 Mo2 O2 79.9(2) . 2_666
O1 Mo2 O2 155.3(3) . .
O1 Mo2 O3 97.5(3) . 2_666
O1 Mo2 O20 96.9(3) . .
O2 Mo2 O2 75.4(2) . 2_666
O3 Mo2 O2 76.8(2) 2_666 2_666
O3 Mo2 O2 77.7(2) 2_666 .
O3 Mo2 O20 146.8(2) 2_666 .
O11 Mo2 O1 104.5(3) . .
O11 Mo2 O2 175.4(3) . 2_666
O11 Mo2 O2 100.2(3) . .
O11 Mo2 O3 103.6(3) . 2_666
O11 Mo2 O20 101.5(3) . .
O20 Mo2 O2 76.7(2) . .
O20 Mo2 O2 76.6(2) . 2_666
Mo1 O2 Mo2 96.9(2) . 2_666
Mo1 O2 Mo3 164.3(3) . 2_666
Mo2 O2 Mo1 93.1(2) . .
Mo2 O2 Mo2 104.6(2) . 2_666
Mo2 O2 Mo3 92.3(2) . 2_666
Mo3 O2 Mo2 96.0(2) 2_666 2_666
C7 N2 Cu1 126.1(6) . .
C11 N2 Cu1 115.2(6) . .
C11 N2 C7 118.7(8) . .
C3 C2 C7 120.1(10) . .
O2 Mo3 O20 73.2(2) 2_666 .
O3 Mo3 O2 73.7(2) . 2_666
O3 Mo3 O20 72.1(2) . .
O6 Mo3 O2 158.4(3) . 2_666
O6 Mo3 O3 96.1(3) . .
O6 Mo3 O12 102.6(3) . .
O6 Mo3 O20 85.6(3) . .
O10 Mo3 O2 95.8(3) . 2_666
O10 Mo3 O3 95.8(3) . .
O10 Mo3 O6 104.4(3) . .
O10 Mo3 O12 103.1(3) . .
O10 Mo3 O20 165.3(3) . .
O12 Mo3 O2 80.0(2) . 2_666
O12 Mo3 O3 149.0(3) . .
O12 Mo3 O20 84.9(2) . .
Mo2 O3 Mo1 109.9(3) 2_666 .
Mo2 O3 Mo3 110.0(3) 2_666 .
Mo3 O3 Mo1 103.8(3) . .
C2 C3 C5 119.4(10) . .
O9 Mo4 O1 77.0(2) . .
O9 Mo4 O12 141.8(3) . .
O12 Mo4 O1 77.2(2) . .
O13 Mo4 O1 163.9(3) . .
O13 Mo4 O9 99.3(3) . .
O13 Mo4 O12 97.8(3) . .
O13 Mo4 O14 105.3(4) . .
O14 Mo4 O1 90.8(3) . .
O14 Mo4 O9 103.7(3) . .
O14 Mo4 O12 104.3(3) . .
C1 N4 C22 119.3(9) . .
N1 C4 C14 121.6(9) . .
C25 C5 C3 121.9(9) . .
Mo3 O6 Cu1 142.7(4) . .
N1 C6 C8 119.4(8) . .
N1 C6 C11 113.5(8) . .
C8 C6 C11 127.1(9) . .
Mo1 O7 Cu1 151.7(3) . .
N2 C7 C2 120.5(9) . .
N2 C7 C22 119.6(9) . .
C22 C7 C2 119.9(8) . .
C12 C8 C6 119.6(10) . .
Mo1 O9 Mo4 118.2(3) 2_666 .
C1 C11 C6 126.1(9) . .
N2 C11 C1 119.2(8) . .
N2 C11 C6 114.6(8) . .
Mo3 O12 Mo4 116.8(3) . .
C14 C12 C8 119.9(10) . .
C19 C13 C18 117.4(9) . .
C20 N14 Cu1 119.1(6) . 2_757
C20 N14 C21 116.5(8) . .
C21 N14 Cu1 123.7(6) . 2_757
C4 C14 C12 119.1(9) . .
C20 C18 C13 118.8(10) . .
C21 C19 C13 120.0(10) . .
Mo1 O20 Mo3 105.0(2) . .
Mo2 O20 Mo1 109.3(3) . .
Mo2 O20 Mo3 110.7(3) . .
N14 C20 C18 124.3(9) . .
N14 C21 C1 117.8(8) . .
N14 C21 C19 123.0(9) . .
C19 C21 C1 119.0(8) . .
N4 C22 C7 121.3(8) . .
N4 C22 C25 118.3(9) . .
C7 C22 C25 120.3(10) . .
C5 C25 C22 118.3(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 O2 2.262(6) .
Mo1 O3 2.374(6) .
Mo1 O7 1.756(6) .
Mo1 O8 1.695(6) .
Mo1 O9 1.872(6) 2_666
Mo1 O20 2.009(6) .
Cu1 N1 1.991(7) .
Cu1 N2 1.996(7) .
Cu1 O6 2.105(6) .
Cu1 O7 1.949(6) .
Cu1 N14 2.080(8) 2_757
O1 Mo2 1.747(6) .
O1 Mo4 2.291(6) .
N1 C4 1.348(11) .
N1 C6 1.364(11) .
C1 N4 1.305(12) .
C1 C11 1.458(13) .
C1 C21 1.511(13) .
Mo2 O2 2.459(6) 2_666
Mo2 O2 2.182(6) .
Mo2 O3 1.932(6) 2_666
Mo2 O11 1.687(6) .
Mo2 O20 1.949(6) .
O2 Mo2 2.459(6) 2_666
O2 Mo3 2.291(6) 2_666
N2 C7 1.396(11) .
N2 C11 1.352(11) .
C2 C3 1.362(13) .
C2 C7 1.415(13) .
Mo3 O2 2.291(6) 2_666
Mo3 O3 2.007(6) .
Mo3 O6 1.744(6) .
Mo3 O10 1.697(6) .
Mo3 O12 1.888(6) .
Mo3 O20 2.337(6) .
O3 Mo2 1.932(6) 2_666
C3 C5 1.421(15) .
Mo4 O9 1.930(6) .
Mo4 O12 1.946(6) .
Mo4 O13 1.701(7) .
Mo4 O14 1.704(7) .
N4 C22 1.368(12) .
C4 C14 1.368(13) .
C5 C25 1.380(15) .
C6 C8 1.390(13) .
C6 C11 1.485(12) .
C7 C22 1.402(13) .
C8 C12 1.378(13) .
O9 Mo1 1.872(6) 2_666
C12 C14 1.373(14) .
C13 C18 1.393(14) .
C13 C19 1.389(15) .
N14 Cu1 2.080(8) 2_757
N14 C20 1.335(12) .
N14 C21 1.356(11) .
C18 C20 1.388(14) .
C19 C21 1.381(13) .
C22 C25 1.409(13) .
