#------------------------------------------------------------------------------
#$Date: 2016-03-26 17:24:55 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180392 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/61/7206156.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_7206156
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(C16 H16 Mo N3 O5), Mo6 O19, C3 H6 O'
_chemical_formula_sum            'C35 H38 Mo8 N6 O30'
_chemical_formula_weight         1790.23
_chemical_name_common
;
bis (acetone cis-dioxo(2-oxobenzaldehyde
isonicotinylhydrazonato-O, N, O) molybdenum(VI)) hexamolybdate acetone
solvate (1/1)
;
_chemical_name_systematic
;
bis (acetone cis-dioxo(2-oxobenzaldehyde isonicotinylhydrazonato-
O, N, O) molybdenum(VI)) hexamolybdate acetone solvate (1/1)
;
_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                92.916(2)
_cell_angle_beta                 95.266(2)
_cell_angle_gamma                114.822(3)
_cell_formula_units_Z            1
_cell_length_a                   10.5322(3)
_cell_length_b                   11.4529(3)
_cell_length_c                   11.6939(3)
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      15
_cell_volume                     1268.60(7)
_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 0.955
_diffrn_measured_fraction_theta_max 0.955
_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  0.0165
_diffrn_reflns_av_sigmaI/netI    0.0199
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16488
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         4.15
_exptl_absorpt_coefficient_mu    2.010
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.86584
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.321
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             855
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.367
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.943
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         5570
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      0.942
_refine_ls_R_factor_all          0.0202
_refine_ls_R_factor_gt           0.0158
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0339P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0394
_refine_ls_wR_factor_ref         0.0401
_reflns_number_gt                4859
_reflns_number_total             5570
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0ce00927j.txt
_cod_data_source_block           1b
_cod_original_cell_volume        1268.60(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7206156
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 0.756549(16) 0.480215(15) 0.210072(13) 0.01133(4) Uani 1 1 d . . .
Mo2 Mo 0.056154(17) 0.825252(15) 0.504983(14) 0.01276(4) Uani 1 1 d . . .
Mo3 Mo -0.165951(17) 0.895785(16) 0.340441(14) 0.01513(4) Uani 1 1 d . . .
Mo4 Mo 0.170821(17) 1.094244(16) 0.379077(14) 0.01489(4) Uani 1 1 d . . .
O1 O 0.59909(13) 0.49448(13) 0.28668(11) 0.0154(3) Uani 1 1 d . . .
O2 O 0.81554(13) 0.37872(13) 0.10884(11) 0.0157(3) Uani 1 1 d . . .
O3 O 0.87876(13) 0.51021(13) 0.32766(11) 0.0156(3) Uani 1 1 d . . .
O4 O 0.80817(14) 0.61579(13) 0.14192(12) 0.0193(3) Uani 1 1 d . . .
O5 O 0.64826(14) 0.28187(13) 0.29720(11) 0.0180(3) Uani 1 1 d . . .
O6 O -0.08602(14) 0.77737(13) 0.37362(12) 0.0180(3) Uani 1 1 d . . .
O7 O 0.0000 1.0000 0.5000 0.0107(4) Uani 1 2 d S . .
O8 O -0.27485(13) 0.84522(13) 0.46047(12) 0.0187(3) Uani 1 1 d . . .
O9 O -0.10419(14) 0.77980(13) 0.59526(12) 0.0196(3) Uani 1 1 d . . .
O10 O 0.09340(14) 0.69566(13) 0.51126(12) 0.0181(3) Uani 1 1 d . . .
O11 O 0.18801(13) 0.93367(13) 0.41544(11) 0.0156(3) Uani 1 1 d . . .
O12 O -0.28146(15) 0.82585(14) 0.22119(12) 0.0248(3) Uani 1 1 d . . .
O13 O 0.16613(13) 0.93559(13) 0.64059(11) 0.0160(3) Uani 1 1 d . . .
O14 O 0.01513(14) 0.99209(14) 0.27506(11) 0.0194(3) Uani 1 1 d . . .
O15 O 0.30129(15) 1.16244(15) 0.29743(13) 0.0248(3) Uani 1 1 d . . .
N1 N 0.55766(15) 0.37985(15) 0.08843(13) 0.0123(3) Uani 1 1 d . . .
N2 N 0.43915(16) 0.38913(15) 0.12428(13) 0.0145(3) Uani 1 1 d . . .
N3 N 0.15287(17) 0.50515(16) 0.37711(14) 0.0176(3) Uani 1 1 d . . .
H3 H 0.0858 0.5183 0.4072 0.021 Uiso 1 1 calc R . .
C1 C 0.47279(19) 0.44937(18) 0.22677(16) 0.0129(4) Uani 1 1 d . . .
C2 C 0.36044(19) 0.46843(18) 0.28169(16) 0.0136(4) Uani 1 1 d . . .
C3 C 0.3894(2) 0.53797(19) 0.38933(16) 0.0167(4) Uani 1 1 d . . .
H31 H 0.4820 0.5734 0.4298 0.020 Uiso 1 1 calc R . .
C4 C 0.2820(2) 0.55495(19) 0.43673(17) 0.0176(4) Uani 1 1 d . . .
H4 H 0.2995 0.6013 0.5105 0.021 Uiso 1 1 calc R . .
C5 C 0.1209(2) 0.43642(19) 0.27404(17) 0.0182(4) Uani 1 1 d . . .
H5 H 0.0272 0.4017 0.2357 0.022 Uiso 1 1 calc R . .
C6 C 0.2237(2) 0.41630(19) 0.22386(17) 0.0165(4) Uani 1 1 d . . .
H6 H 0.2021 0.3676 0.1508 0.020 Uiso 1 1 calc R . .
C7 C 0.54112(19) 0.32702(18) -0.01529(16) 0.0140(4) Uani 1 1 d . . .
H7 H 0.4519 0.2993 -0.0602 0.017 Uiso 1 1 calc R . .
C8 C 0.65131(19) 0.30792(17) -0.06632(16) 0.0132(4) Uani 1 1 d . . .
C9 C 0.7841(2) 0.33704(18) -0.00448(16) 0.0141(4) Uani 1 1 d . . .
C10 C 0.8863(2) 0.3166(2) -0.06001(17) 0.0193(4) Uani 1 1 d . . .
H10 H 0.9764 0.3377 -0.0189 0.023 Uiso 1 1 calc R . .
C11 C 0.8567(2) 0.26573(19) -0.17452(17) 0.0204(4) Uani 1 1 d . . .
H11 H 0.9262 0.2510 -0.2112 0.024 Uiso 1 1 calc R . .
C12 C 0.7251(2) 0.23603(18) -0.23618(17) 0.0179(4) Uani 1 1 d . . .
H12 H 0.7050 0.2014 -0.3147 0.021 Uiso 1 1 calc R . .
C13 C 0.6250(2) 0.25716(18) -0.18245(16) 0.0151(4) Uani 1 1 d . . .
H13 H 0.5358 0.2370 -0.2248 0.018 Uiso 1 1 calc R . .
C14 C 0.5974(2) 0.1636(2) 0.28422(18) 0.0192(4) Uani 1 1 d . . .
C15 C 0.5443(2) 0.0876(2) 0.38346(19) 0.0239(5) Uani 1 1 d . . .
H15A H 0.4435 0.0312 0.3645 0.036 Uiso 1 1 calc R . .
H15B H 0.5589 0.1469 0.4519 0.036 Uiso 1 1 calc R . .
H15C H 0.5958 0.0348 0.3991 0.036 Uiso 1 1 calc R . .
C16 C 0.5857(3) 0.0902(2) 0.1723(2) 0.0374(6) Uani 1 1 d . . .
H16A H 0.6284 0.1508 0.1157 0.056 Uiso 1 1 calc R . .
H16B H 0.4860 0.0366 0.1444 0.056 Uiso 1 1 calc R . .
H16C H 0.6349 0.0347 0.1828 0.056 Uiso 1 1 calc R . .
O16 O 0.9768(5) 0.1536(4) 0.0854(4) 0.0848(18) Uani 0.50 1 d PD A -1
C17 C 0.9820(6) 0.0609(6) 0.0398(5) 0.060(2) Uani 0.50 1 d PDU A -1
C18 C 0.8540(10) -0.0576(9) -0.0038(13) 0.085(4) Uani 0.50 1 d PDU A -1
H18A H 0.7701 -0.0447 0.0097 0.128 Uiso 0.50 1 calc PR A -1
H18B H 0.8544 -0.1303 0.0368 0.128 Uiso 0.50 1 calc PR A -1
H18C H 0.8526 -0.0765 -0.0867 0.128 Uiso 0.50 1 calc PR A -1
C19 C 1.1172(9) 0.0544(12) 0.0260(14) 0.092(5) Uani 0.50 1 d PD A -1
H19A H 1.1956 0.1366 0.0576 0.138 Uiso 0.50 1 calc PR A -1
H19B H 1.1226 0.0383 -0.0562 0.138 Uiso 0.50 1 calc PR A -1
H19C H 1.1229 -0.0159 0.0673 0.138 Uiso 0.50 1 calc PR A -1
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
_geom_angle_publ_flag
O4 Mo1 O3 107.15(6) . . ?
O4 Mo1 O2 99.05(6) . . ?
O3 Mo1 O2 99.15(6) . . ?
O4 Mo1 O1 99.29(6) . . ?
O3 Mo1 O1 100.36(6) . . ?
O2 Mo1 O1 147.85(5) . . ?
O4 Mo1 N1 92.72(6) . . ?
O3 Mo1 N1 159.81(6) . . ?
O2 Mo1 N1 80.73(5) . . ?
O1 Mo1 N1 72.24(5) . . ?
O4 Mo1 O5 171.58(6) . . ?
O3 Mo1 O5 80.06(5) . . ?
O2 Mo1 O5 83.78(5) . . ?
O1 Mo1 O5 74.76(5) . . ?
N1 Mo1 O5 79.86(5) . . ?
O10 Mo2 O11 104.05(6) . . ?
O10 Mo2 O13 103.21(6) . . ?
O11 Mo2 O13 89.15(6) . . ?
O10 Mo2 O6 103.82(6) . . ?
O11 Mo2 O6 88.92(6) . . ?
O13 Mo2 O6 152.55(6) . . ?
O10 Mo2 O9 102.55(6) . . ?
O11 Mo2 O9 153.39(6) . . ?
O13 Mo2 O9 85.19(6) . . ?
O6 Mo2 O9 84.37(6) . . ?
O10 Mo2 O7 178.28(5) . . ?
O11 Mo2 O7 77.67(4) . . ?
O13 Mo2 O7 76.64(4) . . ?
O6 Mo2 O7 76.20(4) . . ?
O9 Mo2 O7 75.73(4) . . ?
O12 Mo3 O8 103.99(7) . . ?
O12 Mo3 O6 104.76(6) . . ?
O8 Mo3 O6 90.70(6) . . ?
O12 Mo3 O13 102.40(6) . 2_576 ?
O8 Mo3 O13 89.73(6) . 2_576 ?
O6 Mo3 O13 151.88(6) . 2_576 ?
O12 Mo3 O14 102.45(7) . . ?
O8 Mo3 O14 153.53(6) . . ?
O6 Mo3 O14 83.62(6) . . ?
O13 Mo3 O14 83.56(6) 2_576 . ?
O12 Mo3 O7 177.28(6) . . ?
O8 Mo3 O7 78.43(4) . . ?
O6 Mo3 O7 76.32(4) . . ?
O13 Mo3 O7 76.23(4) 2_576 . ?
O14 Mo3 O7 75.11(4) . . ?
O15 Mo4 O14 104.77(7) . . ?
O15 Mo4 O9 104.11(7) . 2_576 ?
O14 Mo4 O9 92.98(6) . 2_576 ?
O15 Mo4 O11 102.74(6) . . ?
O14 Mo4 O11 87.56(6) . . ?
O9 Mo4 O11 152.05(6) 2_576 . ?
O15 Mo4 O8 101.68(7) . 2_576 ?
O14 Mo4 O8 152.99(6) . 2_576 ?
O9 Mo4 O8 85.78(6) 2_576 2_576 ?
O11 Mo4 O8 81.35(6) . 2_576 ?
O15 Mo4 O7 176.76(5) . . ?
O14 Mo4 O7 77.96(4) . . ?
O9 Mo4 O7 77.32(4) 2_576 . ?
O11 Mo4 O7 75.48(4) . . ?
O8 Mo4 O7 75.45(4) 2_576 . ?
C1 O1 Mo1 118.21(11) . . ?
C9 O2 Mo1 134.08(12) . . ?
C14 O5 Mo1 146.76(13) . . ?
Mo3 O6 Mo2 117.44(7) . . ?
Mo2 O7 Mo2 180.0 . 2_576 ?
Mo2 O7 Mo3 89.983(6) . 2_576 ?
Mo2 O7 Mo3 90.017(6) 2_576 2_576 ?
Mo2 O7 Mo3 90.017(6) . . ?
Mo2 O7 Mo3 89.983(6) 2_576 . ?
Mo3 O7 Mo3 180.0 2_576 . ?
Mo2 O7 Mo4 90.160(6) . . ?
Mo2 O7 Mo4 89.840(6) 2_576 . ?
Mo3 O7 Mo4 89.967(7) 2_576 . ?
Mo3 O7 Mo4 90.033(7) . . ?
Mo2 O7 Mo4 89.840(6) . 2_576 ?
Mo2 O7 Mo4 90.160(6) 2_576 2_576 ?
Mo3 O7 Mo4 90.033(7) 2_576 2_576 ?
Mo3 O7 Mo4 89.967(7) . 2_576 ?
Mo4 O7 Mo4 180.0 . 2_576 ?
Mo3 O8 Mo4 116.01(6) . 2_576 ?
Mo4 O9 Mo2 116.82(7) 2_576 . ?
Mo2 O11 Mo4 116.50(6) . . ?
Mo2 O13 Mo3 116.55(6) . 2_576 ?
Mo4 O14 Mo3 116.79(7) . . ?
C7 N1 N2 115.57(15) . . ?
C7 N1 Mo1 128.58(12) . . ?
N2 N1 Mo1 115.37(11) . . ?
C1 N2 N1 108.81(15) . . ?
C5 N3 C4 123.23(17) . . ?
N2 C1 O1 125.06(17) . . ?
N2 C1 C2 117.46(16) . . ?
O1 C1 C2 117.47(16) . . ?
C3 C2 C6 119.57(17) . . ?
C3 C2 C1 121.13(17) . . ?
C6 C2 C1 119.30(17) . . ?
C4 C3 C2 119.26(18) . . ?
N3 C4 C3 119.08(18) . . ?
N3 C5 C6 119.79(18) . . ?
C5 C6 C2 119.05(18) . . ?
N1 C7 C8 123.27(17) . . ?
C13 C8 C9 118.54(17) . . ?
C13 C8 C7 118.63(17) . . ?
C9 C8 C7 122.84(17) . . ?
O2 C9 C10 117.75(17) . . ?
O2 C9 C8 122.55(16) . . ?
C10 C9 C8 119.63(17) . . ?
C11 C10 C9 120.43(18) . . ?
C10 C11 C12 120.24(18) . . ?
C13 C12 C11 119.56(18) . . ?
C12 C13 C8 121.60(18) . . ?
O5 C14 C16 122.64(19) . . ?
O5 C14 C15 119.90(19) . . ?
C16 C14 C15 117.46(19) . . ?
O16 C17 C18 122.4(5) . . ?
O16 C17 C19 122.3(5) . . ?
C18 C17 C19 115.3(8) . . ?
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
Mo1 O4 1.6848(14) . ?
Mo1 O3 1.7092(13) . ?
Mo1 O2 1.9339(13) . ?
Mo1 O1 2.0161(12) . ?
Mo1 N1 2.2355(15) . ?
Mo1 O5 2.4027(13) . ?
Mo2 O10 1.6902(13) . ?
Mo2 O11 1.8757(13) . ?
Mo2 O13 1.9191(13) . ?
Mo2 O6 1.9249(13) . ?
Mo2 O9 1.9704(13) . ?
Mo2 O7 2.31474(17) . ?
Mo3 O12 1.6802(14) . ?
Mo3 O8 1.8551(14) . ?
Mo3 O6 1.9107(13) . ?
Mo3 O13 1.9336(13) 2_576 ?
Mo3 O14 2.0064(14) . ?
Mo3 O7 2.32040(18) . ?
Mo4 O15 1.6809(14) . ?
Mo4 O14 1.8481(14) . ?
Mo4 O9 1.8730(13) 2_576 ?
Mo4 O11 1.9850(13) . ?
Mo4 O8 2.0135(14) 2_576 ?
Mo4 O7 2.32235(17) . ?
O1 C1 1.320(2) . ?
O2 C9 1.348(2) . ?
O5 C14 1.225(2) . ?
O7 Mo2 2.31474(16) 2_576 ?
O7 Mo3 2.32040(18) 2_576 ?
O7 Mo4 2.32235(17) 2_576 ?
O8 Mo4 2.0135(14) 2_576 ?
O9 Mo4 1.8730(13) 2_576 ?
O13 Mo3 1.9336(13) 2_576 ?
N1 C7 1.291(2) . ?
N1 N2 1.396(2) . ?
N2 C1 1.293(2) . ?
N3 C5 1.339(3) . ?
N3 C4 1.339(3) . ?
C1 C2 1.484(2) . ?
C2 C3 1.391(3) . ?
C2 C6 1.395(3) . ?
C3 C4 1.384(3) . ?
C5 C6 1.372(3) . ?
C7 C8 1.441(2) . ?
C8 C13 1.405(3) . ?
C8 C9 1.410(3) . ?
C9 C10 1.400(3) . ?
C10 C11 1.386(3) . ?
C11 C12 1.398(3) . ?
C12 C13 1.373(3) . ?
C14 C16 1.486(3) . ?
C14 C15 1.493(3) . ?
O16 C17 1.188(6) . ?
C17 C18 1.479(5) . ?
C17 C19 1.479(5) . ?
