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#$Date: 2019-11-28 16:08:21 +0200 (Thu, 28 Nov 2019) $
#$Revision: 244083 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/28/7702877.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_7702877
loop_
_publ_author_name
'Lysenko, Andrey B.'
'Senchyk, Ganna A.'
'Lincke, Jörg'
'Lässig, Daniel'
'Fokin, Andrey A.'
'Butova, Ekaterina D.'
'Schreiner, Peter R.'
'Krautscheid, Harald'
'Domasevitch, Konstantin V.'
_publ_section_title
;
 Metal oxide-organic frameworks (MOOFs), a new series of coordination
 hybrids constructed from molybdenum(VI) oxide and bitopic 1,2,4-triazole
 linkers.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4223
_journal_page_last               4231
_journal_paper_doi               10.1039/b922732f
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C18 H22 Mo2 N6 O6, 0.5(H2 O)'
_chemical_formula_sum            'C18 H23 Mo2 N6 O6.5'
_chemical_formula_weight         619.30
_chemical_name_common
;
Molybdenum(VI) oxide 2:1 complex with 4,9-bis(1,2,4-triazol-4-
yl)diamantane Semihydrate
;
_chemical_name_systematic
;
Molybdenum(VI) oxide 2:1 complex with 4,9-bis(1,2,4-triazol-4-yl)diamantane
Semihydrate
;
_space_group_IT_number           67
_space_group_name_Hall           '-C 2a 2'
_space_group_name_H-M_alt        'C m m a'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      67
_symmetry_space_group_name_H-M   'C m m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.4256(9)
_cell_length_b                   16.6809(16)
_cell_length_c                   10.4993(10)
_cell_measurement_reflns_used    7657
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.85
_cell_measurement_theta_min      3.81
_cell_volume                     2176.2(3)
_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, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0331
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7657
_diffrn_reflns_theta_full        27.85
_diffrn_reflns_theta_max         27.85
_diffrn_reflns_theta_min         3.81
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.204
_exptl_absorpt_correction_T_max  0.8994
_exptl_absorpt_correction_T_min  0.8215
_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    1.890
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1236
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.693
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.919
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     88
_refine_ls_number_reflns         1389
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.919
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0230
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0346P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0524
_refine_ls_wR_factor_ref         0.0530
_reflns_number_gt                1123
_reflns_number_total             1389
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b922732f.txt
_cod_data_source_block           (5)
_cod_original_sg_symbol_Hall     '-C 2b 2'
_cod_original_formula_sum        'C18 H23 Mo2 N6 O6.50'
_cod_database_code               7702877
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z'
'-x, y+1/2, -z'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1, z'
'-x+1/2, y+1, -z'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y-1/2, -z'
'x, -y-1/2, z'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y, -z'
'x+1/2, -y, z'
'-x+1/2, y+1/2, 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
Mo1 Mo 0.14763(2) 0.7500 0.36072(2) 0.01571(9) Uani 1 2 d S
O1 O 0.2500 0.7500 0.5000 0.0187(6) Uani 1 4 d S
O2 O 0.0000 0.7500 0.3044(3) 0.0198(6) Uani 1 4 d S
O3 O 0.19444(14) 0.66892(11) 0.27729(17) 0.0320(4) Uani 1 1 d .
N1 N 0.05539(17) 0.83569(12) 0.50615(19) 0.0241(4) Uani 1 1 d .
N2 N 0.0000 0.90011(16) 0.6754(3) 0.0211(6) Uani 1 2 d S
C1 C 0.0869(2) 0.87409(14) 0.6081(2) 0.0257(5) Uani 1 1 d .
H1 H 0.1590 0.8825 0.6316 0.031 Uiso 1 1 calc R
C2 C 0.0000 0.93904(18) 0.8033(3) 0.0196(6) Uani 1 2 d S
C3 C 0.0000 0.8746(2) 0.9064(4) 0.0306(8) Uani 1 2 d S
H3 H 0.0639 0.8406 0.8975 0.037 Uiso 1 1 d .
C4 C 0.0000 0.91539(19) 1.0387(3) 0.0282(8) Uani 1 2 d S
H4 H 0.0000 0.8740 1.1063 0.034 Uiso 1 2 calc SR
C5 C 0.1009(2) 0.99128(16) 0.8152(2) 0.0300(5) Uani 1 1 d .
H5A H 0.1013 1.0323 0.7483 0.036 Uiso 1 1 calc R
H5B H 0.1656 0.9582 0.8056 0.036 Uiso 1 1 calc R
C6 C 0.1003(2) 1.03165(15) 0.9481(2) 0.0282(5) Uani 1 1 d .
H6 H 0.1654 1.0654 0.9570 0.034 Uiso 1 1 calc R
O4 O -0.2500 0.7500 1.0000 0.098(4) Uani 0.50 4 d SP
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 O3 104.28(14) . 11_575
O3 Mo1 O2 99.58(8) . .
O3 Mo1 O2 99.58(8) 11_575 .
O3 Mo1 O1 99.38(6) . .
O3 Mo1 O1 99.38(6) 11_575 .
O2 Mo1 O1 148.88(8) . .
O3 Mo1 N1 164.51(8) . .
O3 Mo1 N1 90.99(8) 11_575 .
O2 Mo1 N1 74.87(8) . .
O1 Mo1 N1 80.35(5) . .
O3 Mo1 N1 90.99(8) . 11_575
O3 Mo1 N1 164.51(8) 11_575 11_575
O2 Mo1 N1 74.87(8) . 11_575
O1 Mo1 N1 80.35(5) . 11_575
N1 Mo1 N1 73.65(10) . 11_575
Mo1 O1 Mo1 180.0 . 13_566
Mo1 O2 Mo1 144.28(16) 2_565 .
C1 N1 N1 107.40(14) . 12
C1 N1 Mo1 132.39(17) . .
N1 N1 Mo1 118.72(5) 12 .
C1 N2 C1 104.9(3) 12 .
C1 N2 C2 127.31(13) 12 .
C1 N2 C2 127.31(13) . .
N1 C1 N2 110.1(2) . .
N1 C1 H1 124.9 . .
N2 C1 H1 124.9 . .
N2 C2 C3 109.4(2) . .
N2 C2 C5 108.73(17) . .
C3 C2 C5 110.06(19) . .
N2 C2 C5 108.73(17) . 12
C3 C2 C5 110.06(19) . 12
C5 C2 C5 109.8(3) . 12
C2 C3 C4 109.1(3) . .
C2 C3 H3 109.9 . .
C4 C3 H3 109.9 . .
C6 C4 C6 108.7(3) 4_577 9_577
C6 C4 C3 109.56(18) 4_577 .
C6 C4 C3 109.56(18) 9_577 .
C6 C4 H4 109.7 4_577 .
C6 C4 H4 109.7 9_577 .
C3 C4 H4 109.7 . .
C2 C5 C6 108.5(2) . .
C2 C5 H5A 110.0 . .
C6 C5 H5A 110.0 . .
C2 C5 H5B 110.0 . .
C6 C5 H5B 110.0 . .
H5A C5 H5B 108.4 . .
C6 C6 C4 109.62(18) 4_577 9_577
C6 C6 C5 110.1(2) 4_577 .
C4 C6 C5 109.6(2) 9_577 .
C6 C6 H6 109.1 4_577 .
C4 C6 H6 109.1 9_577 .
C5 C6 H6 109.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 O3 1.7132(17) .
Mo1 O3 1.7132(17) 11_575
Mo1 O2 1.9272(9) .
Mo1 O1 1.9382(3) .
Mo1 N1 2.3850(19) .
Mo1 N1 2.3850(19) 11_575
N1 C1 1.308(3) .
N1 N1 1.377(4) 12
N2 C1 1.361(3) 12
N2 C1 1.361(3) .
N2 C2 1.492(4) .
C1 H1 0.9400 .
C2 C3 1.526(5) .
C2 C5 1.532(3) .
C2 C5 1.532(3) 12
C3 C4 1.547(5) .
C3 H3 0.9802 .
C4 C6 1.534(3) 4_577
C4 C6 1.534(3) 9_577
C4 H4 0.9900 .
C5 C6 1.549(3) .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C6 C6 1.518(5) 4_577
C6 C4 1.534(3) 9_577
C6 H6 0.9900 .
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 O2 Mo1 126.81(7) . 2_565
O3 Mo1 O2 Mo1 -126.81(7) 11_575 2_565
O1 Mo1 O2 Mo1 0.0 . 2_565
N1 Mo1 O2 Mo1 -38.38(5) . 2_565
N1 Mo1 O2 Mo1 38.38(5) 11_575 2_565
O3 Mo1 N1 C1 106.0(3) . .
O3 Mo1 N1 C1 -83.7(2) 11_575 .
O2 Mo1 N1 C1 176.7(2) . .
O1 Mo1 N1 C1 15.7(2) . .
N1 Mo1 N1 C1 98.3(2) 11_575 .
O3 Mo1 N1 N1 -58.2(3) . 12
O3 Mo1 N1 N1 112.19(7) 11_575 12
O2 Mo1 N1 N1 12.54(5) . 12
N1 Mo1 N1 N1 -65.78(5) 11_575 12
N1 N1 C1 N2 -0.4(2) 12 .
Mo1 N1 C1 N2 -165.88(18) . .
C1 N2 C1 N1 0.7(4) 12 .
C2 N2 C1 N1 173.4(3) . .
C1 N2 C2 C3 85.6(3) 12 .
C1 N2 C2 C3 -85.6(3) . .
C1 N2 C2 C5 -154.2(3) 12 .
C1 N2 C2 C5 34.6(4) . .
C1 N2 C2 C5 -34.6(4) 12 12
C1 N2 C2 C5 154.2(3) . 12
N2 C2 C3 C4 180.000(2) . .
C5 C2 C3 C4 60.60(17) . .
C5 C2 C3 C4 -60.60(17) 12 .
C2 C3 C4 C6 -59.57(18) . 4_577
C2 C3 C4 C6 59.57(18) . 9_577
N2 C2 C5 C6 179.9(2) . .
C3 C2 C5 C6 -60.3(3) . .
C5 C2 C5 C6 61.0(4) 12 .
C2 C5 C6 C6 59.9(2) . 4_577
C2 C5 C6 C4 -60.8(3) . 9_577
