#------------------------------------------------------------------------------
#$Date: 2016-03-26 17:24:55 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180392 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/61/7206157.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_7206157
loop_
_publ_author_name
'Vrdoljak, Višnja'
'Prugovečki, Biserka'
'Matković-Čalogović, Dubravka'
'Pisk, Jana'
_publ_section_title
;
 Hybrid organic--inorganic compounds based on the Lindqvist
 polyoxomolybdate and dioxomolybdenum(vi) complexes
;
_journal_issue                   13
_journal_name_full               CrystEngComm
_journal_page_first              4382
_journal_paper_doi               10.1039/c0ce00927j
_journal_volume                  13
_journal_year                    2011
_chemical_formula_moiety         '2(C16H15MoN4O5),Mo6O19, 4(C2H3N)'
_chemical_formula_sum            'C40 H42 Mo8 N12 O29'
_chemical_formula_weight         1922.38
_chemical_name_common
;
bis(acetonitrile cis-dioxo(2-oxo-4-methoxybenzaldehyde
isonicotinylhydrazonato-O, N,O')molybdenum(VI)) hexamolybdate
acetonitrile solvate (1/4)
;
_chemical_name_systematic
;
bis(acetonitrile cis-dioxo(2-oxo-4-methoxybenzaldehyde isonicotinylhydrazonato-
O, N,O')molybdenum(VI)) hexamolybdate acetonitrile solvate (1/4)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_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                100.866(3)
_cell_angle_beta                 105.795(3)
_cell_angle_gamma                112.231(3)
_cell_formula_units_Z            1
_cell_length_a                   11.0325(3)
_cell_length_b                   11.0829(4)
_cell_length_c                   14.1157(5)
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      15
_cell_volume                     1452.68(10)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction,2003)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction,2003)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction,2003)'
_computing_molecular_graphics    'PLATON98 (Spek, 1990)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Xcalibur CCD'
_diffrn_measurement_method       CCD
_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  0.0191
_diffrn_reflns_av_sigmaI/netI    0.0180
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20320
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.70
_exptl_absorpt_coefficient_mu    1.767
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.766
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.197
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             934
_exptl_crystal_size_max          0.66
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.416
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     477
_refine_ls_number_reflns         5078
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0201
_refine_ls_R_factor_gt           0.0148
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0214P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0370
_refine_ls_wR_factor_ref         0.0377
_reflns_number_gt                4510
_reflns_number_total             5078
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0ce00927j.txt
_cod_data_source_block           2a
_cod_original_cell_volume        1452.68(8)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7206157
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
Mo3 Mo 0.341687(19) 0.954066(19) 0.835044(13) 0.01454(5) Uani 1 1 d . . .
Mo2 Mo 0.671409(19) 1.178716(18) 0.976756(14) 0.01366(5) Uani 1 1 d . . .
Mo1 Mo 0.242342(19) 0.323544(19) 0.551959(14) 0.01432(5) Uani 1 1 d . . .
Mo4 Mo 0.425516(19) 1.152684(19) 1.070793(14) 0.01447(5) Uani 1 1 d . . .
O11 O 0.78751(15) 1.31167(15) 0.95562(12) 0.0196(3) Uani 1 1 d . . .
O10 O 0.36820(16) 1.25873(15) 1.12412(12) 0.0202(3) Uani 1 1 d . . .
O2 O 0.36169(15) 0.23363(16) 0.57756(11) 0.0189(3) Uani 1 1 d . . .
O4 O 0.35431(15) 0.48150(15) 0.64222(11) 0.0197(3) Uani 1 1 d . . .
O6 O 0.5000 1.0000 1.0000 0.0109(4) Uani 1 2 d S . .
O3 O 0.11750(16) 0.25274(16) 0.60052(11) 0.0206(3) Uani 1 1 d . . .
O5 O 0.73666(17) 0.10711(17) 0.63168(12) 0.0239(4) Uani 1 1 d . . .
O9 O 0.50191(15) 1.10451(15) 0.84533(11) 0.0167(3) Uani 1 1 d . . .
O15 O 0.23460(14) 0.81008(15) 0.88858(11) 0.0164(3) Uani 1 1 d . . .
O13 O 0.43063(15) 0.83678(15) 0.81068(11) 0.0166(3) Uani 1 1 d . . .
O12 O 0.69668(15) 1.02526(15) 0.91994(11) 0.0153(3) Uani 1 1 d . . .
O8 O 0.56793(15) 1.26479(14) 1.03257(11) 0.0162(3) Uani 1 1 d . . .
O7 O 0.30140(15) 1.07403(15) 0.92486(11) 0.0159(3) Uani 1 1 d . . .
N1 N 0.32509(18) 0.35276(18) 0.42557(13) 0.0148(4) Uani 1 1 d . . .
N4 N 0.09650(19) 0.1139(2) 0.40747(15) 0.0210(4) Uani 1 1 d . . .
O1 O 0.12604(15) 0.38855(15) 0.45707(11) 0.0176(3) Uani 1 1 d . . .
O14 O 0.22131(16) 0.91238(16) 0.71615(11) 0.0233(4) Uani 1 1 d . . .
C6 C 0.1042(2) 0.5080(2) 0.23081(17) 0.0179(5) Uani 1 1 d . . .
N2 N 0.25715(18) 0.40000(18) 0.35290(13) 0.0164(4) Uani 1 1 d . . .
C5 C 0.0179(2) 0.5450(2) 0.16688(18) 0.0177(5) Uani 1 1 d . . .
C15 C 0.0248(2) 0.0171(2) 0.33892(18) 0.0190(5) Uani 1 1 d . . .
C10 C 0.5478(2) 0.1742(2) 0.60840(17) 0.0166(5) Uani 1 1 d . . .
C8 C 0.4961(2) 0.2663(2) 0.46689(16) 0.0149(5) Uani 1 1 d . . .
C2 C 0.0683(2) 0.4612(2) 0.30939(16) 0.0150(5) Uani 1 1 d . . .
C14 C 0.7144(3) 0.0709(3) 0.72008(19) 0.0230(5) Uani 1 1 d . . .
N3 N -0.1006(2) 0.53606(19) 0.17955(15) 0.0163(4) Uani 1 1 d . . .
C9 C 0.4680(2) 0.2267(2) 0.55132(16) 0.0152(5) Uani 1 1 d . . .
C11 C 0.6551(2) 0.1596(2) 0.58226(16) 0.0182(5) Uani 1 1 d . . .
C7 C 0.4181(2) 0.3199(2) 0.40487(16) 0.0148(5) Uani 1 1 d . . .
C13 C 0.6060(2) 0.2493(2) 0.44300(17) 0.0176(5) Uani 1 1 d . . .
C3 C -0.0557(2) 0.4540(2) 0.32042(17) 0.0169(5) Uani 1 1 d . . .
N5 N 0.3400(2) 0.4118(2) 0.88167(15) 0.0238(4) Uani 1 1 d . . .
C16 C -0.0665(3) -0.1077(3) 0.2492(2) 0.0255(6) Uani 1 1 d . . .
C12 C 0.6849(2) 0.1979(2) 0.49817(17) 0.0198(5) Uani 1 1 d . . .
C19 C 0.0541(3) 0.1522(3) 1.1052(2) 0.0248(5) Uani 1 1 d . . .
C17 C 0.5629(3) 0.4307(3) 0.8456(2) 0.0218(5) Uani 1 1 d . . .
N6 N 0.0804(2) 0.2947(2) 0.97945(16) 0.0306(5) Uani 1 1 d . . .
C4 C -0.1394(2) 0.4912(2) 0.25339(16) 0.0171(5) Uani 1 1 d . . .
C1 C 0.1576(2) 0.4158(2) 0.37717(16) 0.0158(5) Uani 1 1 d . . .
C18 C 0.4384(2) 0.4205(2) 0.86652(16) 0.0171(5) Uiso 1 1 d . . .
C20 C 0.0697(2) 0.2320(2) 1.03448(18) 0.0204(5) Uiso 1 1 d . . .
H3 H -0.075(2) 0.424(2) 0.3711(19) 0.019(6) Uiso 1 1 d . . .
H5 H 0.034(2) 0.575(2) 0.1210(18) 0.012(6) Uiso 1 1 d . . .
H10 H 0.524(2) 0.146(2) 0.6625(19) 0.022(6) Uiso 1 1 d . . .
H7 H 0.432(2) 0.329(2) 0.3427(18) 0.018(6) Uiso 1 1 d . . .
H4 H -0.220(3) 0.484(2) 0.2552(17) 0.017(6) Uiso 1 1 d . . .
H12 H 0.753(2) 0.184(2) 0.4806(18) 0.021(6) Uiso 1 1 d . . .
H6 H 0.176(2) 0.516(2) 0.2223(17) 0.014(6) Uiso 1 1 d . . .
H14A H 0.622(3) 0.005(2) 0.7014(18) 0.020(6) Uiso 1 1 d . . .
H19C H 0.097(3) 0.090(3) 1.0965(18) 0.025(7) Uiso 1 1 d . . .
H14B H 0.748(2) 0.156(3) 0.7799(19) 0.025(6) Uiso 1 1 d . . .
H14C H 0.776(2) 0.030(2) 0.7378(18) 0.020(6) Uiso 1 1 d . . .
H19A H -0.042(3) 0.104(3) 1.092(2) 0.038(8) Uiso 1 1 d . . .
H19B H 0.099(3) 0.207(3) 1.169(3) 0.058(10) Uiso 1 1 d . . .
H17B H 0.545(3) 0.337(3) 0.816(2) 0.037(8) Uiso 1 1 d . . .
H16B H -0.077(3) -0.088(3) 0.193(2) 0.033(8) Uiso 1 1 d . . .
H16A H -0.167(3) -0.153(3) 0.250(2) 0.048(8) Uiso 1 1 d . . .
H17A H 0.635(3) 0.482(3) 0.904(2) 0.040(8) Uiso 1 1 d . . .
H17C H 0.573(3) 0.478(3) 0.797(2) 0.034(7) Uiso 1 1 d . . .
H16C H -0.030(3) -0.175(3) 0.257(2) 0.053(9) Uiso 1 1 d . . .
H13 H 0.624(2) 0.274(2) 0.3900(18) 0.017(6) Uiso 1 1 d . . .
H31 H -0.148(2) 0.556(2) 0.1440(18) 0.013(7) Uiso 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'
O O 0.0106 0.0060 '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'
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
_geom_angle_publ_flag
O14 Mo3 O9 105.10(7) . . ?
O14 Mo3 O7 103.89(7) . . ?
O9 Mo3 O7 90.33(6) . . ?
O14 Mo3 O13 102.86(7) . . ?
O9 Mo3 O13 89.40(6) . . ?
O7 Mo3 O13 152.35(6) . . ?
O14 Mo3 O15 101.56(7) . . ?
O9 Mo3 O15 153.32(6) . . ?
O7 Mo3 O15 84.37(6) . . ?
O13 Mo3 O15 83.56(6) . . ?
O14 Mo3 O6 176.79(6) . . ?
O9 Mo3 O6 78.03(4) . . ?
O7 Mo3 O6 76.62(4) . . ?
O13 Mo3 O6 76.29(4) . . ?
O15 Mo3 O6 75.30(4) . . ?
O11 Mo2 O15 104.68(7) . 2_677 ?
O11 Mo2 O12 104.73(7) . . ?
O15 Mo2 O12 91.34(6) 2_677 . ?
O11 Mo2 O8 101.31(7) . . ?
O15 Mo2 O8 88.12(6) 2_677 . ?
O12 Mo2 O8 153.20(6) . . ?
O11 Mo2 O9 101.10(7) . . ?
O15 Mo2 O9 153.89(6) 2_677 . ?
O12 Mo2 O9 86.02(6) . . ?
O8 Mo2 O9 82.85(6) . . ?
O11 Mo2 O6 176.04(5) . . ?
O15 Mo2 O6 78.30(5) 2_677 . ?
O12 Mo2 O6 77.62(4) . . ?
O8 Mo2 O6 76.04(4) . . ?
O9 Mo2 O6 75.76(4) . . ?
O4 Mo1 O3 104.34(7) . . ?
O4 Mo1 O2 99.17(7) . . ?
O3 Mo1 O2 104.85(7) . . ?
O4 Mo1 O1 95.90(7) . . ?
O3 Mo1 O1 94.61(7) . . ?
O2 Mo1 O1 151.46(6) . . ?
O4 Mo1 N1 98.18(7) . . ?
O3 Mo1 N1 154.95(7) . . ?
O2 Mo1 N1 81.88(6) . . ?
O1 Mo1 N1 72.05(6) . . ?
O4 Mo1 N4 171.91(7) . . ?
O3 Mo1 N4 83.13(7) . . ?
O2 Mo1 N4 81.62(6) . . ?
O1 Mo1 N4 80.20(6) . . ?
N1 Mo1 N4 73.91(6) . . ?
O10 Mo4 O8 104.86(7) . . ?
O10 Mo4 O13 102.69(7) . 2_677 ?
O8 Mo4 O13 89.08(6) . 2_677 ?
O10 Mo4 O7 104.23(7) . . ?
O8 Mo4 O7 88.23(6) . . ?
O13 Mo4 O7 152.73(6) 2_677 . ?
O10 Mo4 O12 101.96(7) . 2_677 ?
O8 Mo4 O12 153.17(6) . 2_677 ?
O13 Mo4 O12 85.92(6) 2_677 2_677 ?
O7 Mo4 O12 84.34(6) . 2_677 ?
O10 Mo4 O6 177.72(5) . . ?
O8 Mo4 O6 77.35(4) . . ?
O13 Mo4 O6 76.66(4) 2_677 . ?
O7 Mo4 O6 76.27(4) . . ?
O12 Mo4 O6 75.84(4) 2_677 . ?
C9 O2 Mo1 137.62(14) . . ?
Mo2 O6 Mo2 179.998(8) 2_677 . ?
Mo2 O6 Mo3 90.068(7) 2_677 . ?
Mo2 O6 Mo3 89.933(8) . . ?
Mo2 O6 Mo3 89.932(8) 2_677 2_677 ?
Mo2 O6 Mo3 90.068(8) . 2_677 ?
Mo3 O6 Mo3 179.999(10) . 2_677 ?
Mo2 O6 Mo4 90.201(7) 2_677 . ?
Mo2 O6 Mo4 89.801(7) . . ?
Mo3 O6 Mo4 90.002(7) . . ?
Mo3 O6 Mo4 89.999(7) 2_677 . ?
Mo2 O6 Mo4 89.800(7) 2_677 2_677 ?
Mo2 O6 Mo4 90.199(8) . 2_677 ?
Mo3 O6 Mo4 89.999(8) . 2_677 ?
Mo3 O6 Mo4 90.000(7) 2_677 2_677 ?
Mo4 O6 Mo4 180.0 . 2_677 ?
C11 O5 C14 117.43(18) . . ?
Mo3 O9 Mo2 116.26(7) . . ?
Mo2 O15 Mo3 116.24(7) 2_677 . ?
Mo4 O13 Mo3 117.03(7) 2_677 . ?
Mo2 O12 Mo4 116.25(7) . 2_677 ?
Mo4 O8 Mo2 116.60(7) . . ?
Mo3 O7 Mo4 116.65(7) . . ?
C7 N1 N2 115.46(17) . . ?
C7 N1 Mo1 128.60(15) . . ?
N2 N1 Mo1 115.60(13) . . ?
C15 N4 Mo1 177.72(18) . . ?
C1 O1 Mo1 118.99(13) . . ?
C5 C6 C2 119.8(2) . . ?
C1 N2 N1 109.04(17) . . ?
N3 C5 C6 119.8(2) . . ?
N4 C15 C16 179.0(3) . . ?
C11 C10 C9 120.0(2) . . ?
C9 C8 C13 117.6(2) . . ?
C9 C8 C7 123.4(2) . . ?
C13 C8 C7 119.1(2) . . ?
C3 C2 C6 118.7(2) . . ?
C3 C2 C1 120.6(2) . . ?
C6 C2 C1 120.7(2) . . ?
C4 N3 C5 122.4(2) . . ?
O2 C9 C10 117.47(19) . . ?
O2 C9 C8 122.07(19) . . ?
C10 C9 C8 120.4(2) . . ?
O5 C11 C10 124.4(2) . . ?
O5 C11 C12 115.0(2) . . ?
C10 C11 C12 120.6(2) . . ?
N1 C7 C8 124.4(2) . . ?
C12 C13 C8 122.6(2) . . ?
C4 C3 C2 119.1(2) . . ?
C13 C12 C11 118.8(2) . . ?
N3 C4 C3 120.1(2) . . ?
N2 C1 O1 124.3(2) . . ?
N2 C1 C2 118.75(19) . . ?
O1 C1 C2 116.90(19) . . ?
N5 C18 C17 179.2(3) . . ?
N6 C20 C19 179.0(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo3 O14 1.6804(14) . ?
Mo3 O9 1.8614(15) . ?
Mo3 O7 1.9212(14) . ?
Mo3 O13 1.9368(15) . ?
Mo3 O15 2.0069(15) . ?
Mo3 O6 2.3233(2) . ?
Mo2 O11 1.6871(15) . ?
Mo2 O15 1.8560(14) 2_677 ?
Mo2 O12 1.8920(14) . ?
Mo2 O8 1.9658(15) . ?
Mo2 O9 1.9969(14) . ?
Mo2 O6 2.3142(2) . ?
Mo1 O4 1.6970(15) . ?
Mo1 O3 1.6975(15) . ?
Mo1 O2 1.9305(15) . ?
Mo1 O1 2.0216(15) . ?
Mo1 N1 2.2365(17) . ?
Mo1 N4 2.3967(19) . ?
Mo4 O10 1.6840(15) . ?
Mo4 O8 1.8816(15) . ?
Mo4 O13 1.9163(14) 2_677 ?
Mo4 O7 1.9398(14) . ?
Mo4 O12 1.9762(15) 2_677 ?
Mo4 O6 2.32358(19) . ?
O2 C9 1.346(3) . ?
O6 Mo2 2.3142(2) 2_677 ?
O6 Mo3 2.3234(2) 2_677 ?
O6 Mo4 2.3237(2) 2_677 ?
O5 C11 1.357(3) . ?
O5 C14 1.435(3) . ?
O15 Mo2 1.8559(14) 2_677 ?
O13 Mo4 1.9163(14) 2_677 ?
O12 Mo4 1.9762(14) 2_677 ?
N1 C7 1.295(3) . ?
N1 N2 1.403(2) . ?
N4 C15 1.124(3) . ?
O1 C1 1.322(3) . ?
C6 C5 1.363(3) . ?
C6 C2 1.399(3) . ?
N2 C1 1.296(3) . ?
C5 N3 1.337(3) . ?
C15 C16 1.457(3) . ?
C10 C11 1.388(3) . ?
C10 C9 1.393(3) . ?
C8 C9 1.416(3) . ?
C8 C13 1.410(3) . ?
C8 C7 1.426(3) . ?
C2 C3 1.393(3) . ?
C2 C1 1.477(3) . ?
N3 C4 1.339(3) . ?
C11 C12 1.412(3) . ?
C13 C12 1.365(3) . ?
C3 C4 1.370(3) . ?
N5 C18 1.135(3) . ?
C19 C20 1.456(3) . ?
C17 C18 1.449(3) . ?
N6 C20 1.137(3) . ?
