#------------------------------------------------------------------------------
#$Date: 2021-06-14 11:20:14 +0300 (Mon, 14 Jun 2021) $
#$Revision: 266429 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/33/1563390.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_1563390
loop_
_publ_author_name
'Nie, Shanshan'
'Zhang, Yaobin'
'Liu, Bin'
'Li, Zuoxi'
'Hu, Huaiming'
'Xue, Ganglin'
'Fu, Feng'
'Wang, Jiwu'
_publ_section_title
;
 Two inorganic--organic hybrid materials based on polyoxometalate anions
 and methylene blue: Preparations, crystal structures and properties
;
_journal_issue                   12
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              2957
_journal_page_last               2962
_journal_paper_doi               10.1016/j.jssc.2010.08.023
_journal_volume                  183
_journal_year                    2010
_chemical_formula_sum            'C38 H50 Mo6 N8 O21 S2'
_chemical_formula_weight         1594.62
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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                90.0130(10)
_cell_angle_beta                 115.1070(10)
_cell_angle_gamma                100.4740(10)
_cell_formula_units_Z            1
_cell_length_a                   10.3869(8)
_cell_length_b                   11.6818(9)
_cell_length_c                   12.1260(10)
_cell_measurement_temperature    296(2)
_cell_volume                     1305.17(18)
_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 0.981
_diffrn_measured_fraction_theta_max 0.981
_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  0.0148
_diffrn_reflns_av_sigmaI/netI    0.0339
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6580
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    1.561
_exptl_absorpt_correction_T_max  0.869
_exptl_absorpt_correction_T_min  0.799
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadbas
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.029
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             786
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.081
_refine_diff_density_min         -0.618
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constrn
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         4545
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0318
_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)+(0.0423P)²+1.6511P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.0897
_reflns_number_gt                3928
_reflns_number_total             4545
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2010-183-2957.cif
_cod_data_source_block           xb3516
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1563390
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 0.32525(4) 0.37611(3) 0.53922(3) 0.03827(12) Uani 1 1 d . . .
Mo2 Mo 0.36674(4) 0.44535(3) 0.29275(3) 0.04008(12) Uani 1 1 d . . .
Mo3 Mo 0.62231(4) 0.34848(3) 0.51719(4) 0.03977(12) Uani 1 1 d . . .
S1 S 0.42843(12) 0.18315(10) 0.06444(11) 0.0482(3) Uani 1 1 d . . .
O1 O 0.5000 0.5000 0.5000 0.0315(8) Uani 1 2 d S . .
O2 O 0.2518(3) 0.3546(3) 0.3621(3) 0.0439(7) Uani 1 1 d . . .
O3 O 0.2942(3) 0.5778(3) 0.3173(3) 0.0431(7) Uani 1 1 d . . .
O4 O 0.2718(4) 0.4077(3) 0.1415(3) 0.0557(9) Uani 1 1 d . . .
O5 O 0.4938(3) 0.3357(3) 0.3470(3) 0.0436(7) Uani 1 1 d . . .
O6 O 0.7143(4) 0.2403(3) 0.5313(3) 0.0586(9) Uani 1 1 d . . .
O7 O 0.4582(3) 0.2778(2) 0.5450(3) 0.0432(7) Uani 1 1 d . . .
O8 O 0.1985(4) 0.2843(3) 0.5660(3) 0.0530(8) Uani 1 1 d . . .
O9 O 0.4645(3) 0.4428(3) 0.6987(3) 0.0404(7) Uani 1 1 d . . .
O10 O 0.2572(3) 0.5202(3) 0.5147(3) 0.0425(7) Uani 1 1 d . . .
O11 O 1.0566(7) 0.1145(5) 0.8401(6) 0.119(2) Uani 1 1 d . . .
C1 C 0.2774(5) -0.1573(4) 0.0544(4) 0.0438(10) Uani 1 1 d . . .
C2 C 0.2942(5) -0.0394(4) 0.0296(4) 0.0456(10) Uani 1 1 d . . .
H2 H 0.2179 -0.0137 -0.0326 0.055 Uiso 1 1 calc R . .
C3 C 0.4220(5) 0.0387(4) 0.0961(4) 0.0390(9) Uani 1 1 d . . .
C4 C 0.5443(5) 0.0040(4) 0.1907(4) 0.0447(10) Uani 1 1 d . . .
C5 C 0.5249(6) -0.1165(4) 0.2129(5) 0.0527(12) Uani 1 1 d . . .
H5 H 0.6024 -0.1429 0.2728 0.063 Uiso 1 1 calc R . .
C6 C 0.3991(5) -0.1942(4) 0.1507(5) 0.0530(12) Uani 1 1 d . . .
H6 H 0.3908 -0.2714 0.1699 0.064 Uiso 1 1 calc R . .
C7 C 0.6032(4) 0.2510(4) 0.1605(4) 0.0380(9) Uani 1 1 d . . .
C8 C 0.7024(5) 0.1876(4) 0.2466(4) 0.0406(10) Uani 1 1 d . . .
C9 C 0.8426(5) 0.2526(4) 0.3233(4) 0.0482(11) Uani 1 1 d . . .
H9 H 0.9094 0.2142 0.3801 0.058 Uiso 1 1 calc R . .
C10 C 0.8829(5) 0.3685(4) 0.3173(4) 0.0450(10) Uani 1 1 d . . .
H10 H 0.9759 0.4078 0.3696 0.054 Uiso 1 1 calc R . .
C11 C 0.7833(5) 0.4311(4) 0.2309(4) 0.0401(10) Uani 1 1 d . . .
C12 C 0.6434(4) 0.3687(4) 0.1542(4) 0.0402(10) Uani 1 1 d . . .
H12 H 0.5767 0.4078 0.0983 0.048 Uiso 1 1 calc R . .
C13 C 0.9715(5) 0.6105(5) 0.3007(5) 0.0580(13) Uani 1 1 d . . .
H13A H 0.9975 0.5956 0.3846 0.087 Uiso 1 1 calc R . .
H13B H 0.9755 0.6927 0.2927 0.087 Uiso 1 1 calc R . .
H13C H 1.0380 0.5853 0.2748 0.087 Uiso 1 1 calc R . .
C14 C 0.7244(5) 0.6120(4) 0.1381(4) 0.0496(11) Uani 1 1 d . . .
H14A H 0.6947 0.5797 0.0562 0.074 Uiso 1 1 calc R . .
H14B H 0.7726 0.6921 0.1474 0.074 Uiso 1 1 calc R . .
H14C H 0.6407 0.6077 0.1540 0.074 Uiso 1 1 calc R . .
C15 C 0.1258(7) -0.3538(4) 0.0208(5) 0.0704(16) Uani 1 1 d . . .
H15A H 0.1882 -0.3949 0.0037 0.106 Uiso 1 1 calc R . .
H15B H 0.0264 -0.3905 -0.0281 0.106 Uiso 1 1 calc R . .
H15C H 0.1466 -0.3555 0.1058 0.106 Uiso 1 1 calc R . .
C16 C 0.0251(6) -0.1931(5) -0.0992(5) 0.0674(15) Uani 1 1 d . . .
H16A H -0.0240 -0.1602 -0.0593 0.101 Uiso 1 1 calc R . .
H16B H -0.0402 -0.2581 -0.1554 0.101 Uiso 1 1 calc R . .
H16C H 0.0570 -0.1348 -0.1429 0.101 Uiso 1 1 calc R . .
C17 C 0.9308(13) 0.0764(8) 0.7890(10) 0.123(3) Uani 1 1 d . . .
H17 H 0.8754 0.0851 0.8307 0.147 Uiso 1 1 calc R . .
C18 C 0.7061(13) -0.0219(9) 0.6394(13) 0.181(6) Uani 1 1 d . . .
H18A H 0.6835 -0.0076 0.7065 0.272 Uiso 1 1 calc R . .
H18B H 0.6826 -0.1043 0.6164 0.272 Uiso 1 1 calc R . .
H18C H 0.6505 0.0176 0.5712 0.272 Uiso 1 1 calc R . .
C19 C 0.9092(18) 0.0102(11) 0.5934(13) 0.220(8) Uani 1 1 d . . .
H19A H 0.8324 -0.0331 0.5210 0.331 Uiso 1 1 calc R . .
H19B H 0.9878 -0.0309 0.6251 0.331 Uiso 1 1 calc R . .
H19C H 0.9429 0.0860 0.5738 0.331 Uiso 1 1 calc R . .
N1 N 0.1505(5) -0.2327(3) -0.0078(4) 0.0544(10) Uani 1 1 d . . .
N2 N 0.8234(4) 0.5460(3) 0.2242(3) 0.0432(8) Uani 1 1 d . . .
N6 N 0.6730(4) 0.0731(3) 0.2593(3) 0.0469(9) Uani 1 1 d . . .
N7 N 0.8605(6) 0.0218(4) 0.6760(5) 0.0731(14) 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'
Mo Mo -1.6832 0.6857 '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'
S S 0.1246 0.1234 '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'
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 O9 103.68(14) . .
O8 Mo1 O10 103.87(15) . .
O9 Mo1 O10 87.90(13) . .
O8 Mo1 O7 102.84(15) . .
O9 Mo1 O7 87.40(13) . .
O10 Mo1 O7 153.25(12) . .
O8 Mo1 O2 102.81(14) . .
O9 Mo1 O2 153.50(12) . .
O10 Mo1 O2 86.68(13) . .
O7 Mo1 O2 85.88(13) . .
O8 Mo1 O1 178.97(12) . .
O9 Mo1 O1 77.02(8) . .
O10 Mo1 O1 76.86(9) . .
O7 Mo1 O1 76.42(8) . .
O2 Mo1 O1 76.48(8) . .
O4 Mo2 O2 103.70(14) . .
O4 Mo2 O3 103.03(15) . .
O2 Mo2 O3 88.14(13) . .
O4 Mo2 O5 103.71(15) . .
O2 Mo2 O5 87.27(13) . .
O3 Mo2 O5 153.20(12) . .
O4 Mo2 O9 102.47(14) . 2_666
O2 Mo2 O9 153.82(12) . 2_666
O3 Mo2 O9 86.48(13) . 2_666
O5 Mo2 O9 86.09(13) . 2_666
O4 Mo2 O1 178.92(12) . .
O2 Mo2 O1 77.36(8) . .
O3 Mo2 O1 76.72(8) . .
O5 Mo2 O1 76.51(8) . .
O9 Mo2 O1 76.47(8) 2_666 .
O6 Mo3 O5 104.15(16) . .
O6 Mo3 O7 104.13(15) . .
O5 Mo3 O7 87.58(13) . .
O6 Mo3 O3 103.10(16) . 2_666
O5 Mo3 O3 152.73(13) . 2_666
O7 Mo3 O3 86.73(13) . 2_666
O6 Mo3 O10 102.76(15) . 2_666
O5 Mo3 O10 87.18(13) . 2_666
O7 Mo3 O10 153.08(12) . 2_666
O3 Mo3 O10 85.93(13) 2_666 2_666
O6 Mo3 O1 178.86(13) . .
O5 Mo3 O1 76.62(9) . .
O7 Mo3 O1 76.70(9) . .
O3 Mo3 O1 76.11(9) 2_666 .
O10 Mo3 O1 76.39(9) 2_666 .
C7 S1 C3 103.7(2) . .
Mo2 O1 Mo2 180.0 . 2_666
Mo2 O1 Mo3 90.276(14) . 2_666
Mo2 O1 Mo3 89.724(14) 2_666 2_666
Mo2 O1 Mo3 89.724(14) . .
Mo2 O1 Mo3 90.276(14) 2_666 .
Mo3 O1 Mo3 180.0 2_666 .
Mo2 O1 Mo1 90.099(14) . 2_666
Mo2 O1 Mo1 89.901(14) 2_666 2_666
Mo3 O1 Mo1 89.901(14) 2_666 2_666
Mo3 O1 Mo1 90.099(14) . 2_666
Mo2 O1 Mo1 89.901(14) . .
Mo2 O1 Mo1 90.099(14) 2_666 .
Mo3 O1 Mo1 90.099(14) 2_666 .
Mo3 O1 Mo1 89.901(14) . .
Mo1 O1 Mo1 180.000(16) 2_666 .
Mo2 O2 Mo1 116.25(14) . .
Mo2 O3 Mo3 116.89(14) . 2_666
Mo3 O5 Mo2 117.12(14) . .
Mo3 O7 Mo1 116.98(14) . .
Mo1 O9 Mo2 116.40(14) . 2_666
Mo1 O10 Mo3 116.62(14) . 2_666
N1 C1 C2 120.8(4) . .
N1 C1 C6 121.2(4) . .
C2 C1 C6 117.9(4) . .
C3 C2 C1 120.9(4) . .
C2 C3 C4 122.2(4) . .
C2 C3 S1 117.4(3) . .
C4 C3 S1 120.5(3) . .
N6 C4 C5 117.8(4) . .
N6 C4 C3 126.4(4) . .
C5 C4 C3 115.8(4) . .
C6 C5 C4 123.1(4) . .
C5 C6 C1 120.2(4) . .
C12 C7 C8 121.1(4) . .
C12 C7 S1 117.6(3) . .
C8 C7 S1 121.3(3) . .
N6 C8 C9 118.1(4) . .
N6 C8 C7 125.3(4) . .
C9 C8 C7 116.6(4) . .
C10 C9 C8 122.6(4) . .
C9 C10 C11 120.6(4) . .
N2 C11 C12 121.4(4) . .
N2 C11 C10 120.6(4) . .
C12 C11 C10 118.0(4) . .
C7 C12 C11 121.2(4) . .
O11 C17 N7 125.8(10) . .
C1 N1 C15 122.4(4) . .
C1 N1 C16 120.9(4) . .
C15 N1 C16 116.4(4) . .
C11 N2 C14 121.9(4) . .
C11 N2 C13 121.5(4) . .
C14 N2 C13 116.6(4) . .
C4 N6 C8 122.7(4) . .
C19 N7 C17 129.2(10) . .
C19 N7 C18 117.2(10) . .
C17 N7 C18 113.5(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 O8 1.685(3) .
Mo1 O9 1.912(3) .
Mo1 O10 1.916(3) .
Mo1 O7 1.930(3) .
Mo1 O2 1.949(3) .
Mo1 O1 2.3223(4) .
Mo2 O4 1.685(3) .
Mo2 O2 1.910(3) .
Mo2 O3 1.914(3) .
Mo2 O5 1.922(3) .
Mo2 O9 1.950(3) 2_666
Mo2 O1 2.3163(4) .
Mo3 O6 1.684(3) .
Mo3 O5 1.911(3) .
Mo3 O7 1.917(3) .
Mo3 O3 1.942(3) 2_666
Mo3 O10 1.945(3) 2_666
Mo3 O1 2.3202(4) .
S1 C7 1.721(4) .
S1 C3 1.727(4) .
O1 Mo2 2.3163(4) 2_666
O1 Mo3 2.3202(4) 2_666
O1 Mo1 2.3223(4) 2_666
O3 Mo3 1.942(3) 2_666
O9 Mo2 1.950(3) 2_666
O10 Mo3 1.945(3) 2_666
O11 C17 1.179(11) .
C1 N1 1.348(6) .
C1 C2 1.406(6) .
C1 C6 1.447(7) .
C2 C3 1.377(6) .
C3 C4 1.430(6) .
C4 N6 1.339(6) .
C4 C5 1.427(6) .
C5 C6 1.354(7) .
C7 C12 1.375(6) .
C7 C8 1.437(6) .
C8 N6 1.341(5) .
C8 C9 1.418(6) .
C9 C10 1.354(6) .
C10 C11 1.434(6) .
C11 N2 1.344(5) .
C11 C12 1.406(6) .
C13 N2 1.470(6) .
C14 N2 1.456(6) .
C15 N1 1.459(6) .
C16 N1 1.461(7) .
C17 N7 1.342(11) .
C18 N7 1.459(12) .
C19 N7 1.316(10) .
