#------------------------------------------------------------------------------
#$Date: 2016-03-26 17:24:55 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180392 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/61/7206155.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_7206155
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(C15 H13 Mo N4 O4), Mo6 O19, 2(C2 H3 N)'
_chemical_formula_sum            'C34 H32 Mo8 N10 O27'
_chemical_formula_weight         1780.22
_chemical_name_common
;
bis (acetonitrile cis-dioxo(2-oxobenzaldehyde
isonicotinylhydrazonato-O, N, O) molybdenum(VI)) hexamolybdate
acetonitrile solvate (1/2)
;
_chemical_name_systematic
;
bis (acetonitrile cis-dioxo(2-oxobenzaldehyde isonicotinylhydrazonato-O, N, O)
molybdenum(VI)) hexamolybdate acetonitrile solvate (1/2)
;
_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                93.936(3)
_cell_angle_beta                 97.847(3)
_cell_angle_gamma                114.580(3)
_cell_formula_units_Z            1
_cell_length_a                   10.2393(3)
_cell_length_b                   11.7244(4)
_cell_length_c                   11.8311(4)
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      15
_cell_volume                     1267.05(8)
_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 0.952
_diffrn_measured_fraction_theta_max 0.952
_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  0.0150
_diffrn_reflns_av_sigmaI/netI    0.0185
_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       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16243
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         4.16
_exptl_absorpt_coefficient_mu    2.011
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88698
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange-yellow
_exptl_crystal_density_diffrn    2.333
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             858
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.484
_refine_diff_density_min         -0.579
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         5547
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0225
_refine_ls_R_factor_gt           0.0180
_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)+(0.0285P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0441
_refine_ls_wR_factor_ref         0.0449
_reflns_number_gt                4866
_reflns_number_total             5547
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0ce00927j.txt
_cod_data_source_block           1a
_cod_original_cell_volume        1267.05(7)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7206155
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 -0.240096(18) 0.015855(16) 0.293849(14) 0.01499(5) Uani 1 1 d . . .
Mo2 Mo 0.274138(19) 0.367269(17) 0.039502(17) 0.02204(5) Uani 1 1 d . . .
Mo3 Mo 0.433762(19) 0.666756(16) 0.002642(15) 0.01733(5) Uani 1 1 d . . .
Mo4 Mo 0.59321(2) 0.555836(18) 0.195719(15) 0.02223(5) Uani 1 1 d . . .
O1 O -0.07781(15) 0.01824(13) 0.21437(12) 0.0204(3) Uani 1 1 d . . .
O2 O -0.30692(15) 0.09962(14) 0.40205(12) 0.0210(3) Uani 1 1 d . . .
O3 O -0.36945(15) -0.01731(13) 0.17204(12) 0.0202(3) Uani 1 1 d . . .
O4 O -0.27757(17) -0.12006(14) 0.34945(14) 0.0284(4) Uani 1 1 d . . .
O5 O 0.37101(16) 0.25670(13) 0.02379(13) 0.0230(3) Uani 1 1 d . . .
O6 O 0.10941(18) 0.26927(16) 0.06558(17) 0.0368(4) Uani 1 1 d . . .
O7 O 0.39091(18) 0.43160(15) 0.18782(13) 0.0273(3) Uani 1 1 d . . .
O8 O 0.26125(16) 0.52507(14) 0.03367(13) 0.0240(3) Uani 1 1 d . . .
O9 O 0.5000 0.5000 0.0000 0.0144(4) Uani 1 2 d S . .
O10 O 0.37237(16) 0.59201(14) -0.15388(12) 0.0235(3) Uani 1 1 d . . .
O11 O 0.38171(16) 0.78590(14) 0.00405(13) 0.0232(3) Uani 1 1 d . . .
O12 O 0.51460(17) 0.67357(14) 0.16143(12) 0.0239(3) Uani 1 1 d . . .
O13 O 0.75658(16) 0.65029(14) 0.12833(13) 0.0270(3) Uani 1 1 d . . .
O14 O 0.6607(2) 0.59423(17) 0.33732(14) 0.0414(5) Uani 1 1 d . . .
N1 N -0.02950(17) 0.12446(15) 0.41680(14) 0.0164(3) Uani 1 1 d . . .
N2 N 0.09556(18) 0.13234(16) 0.37634(15) 0.0190(4) Uani 1 1 d . . .
N3 N 0.3775(2) 0.02190(17) 0.12007(15) 0.0229(4) Uani 1 1 d . . .
H3 H 0.4423 0.0061 0.0918 0.027 Uiso 1 1 calc R . .
N4 N -0.1465(2) 0.22586(17) 0.23718(15) 0.0231(4) Uani 1 1 d . . .
C1 C 0.0574(2) 0.07315(18) 0.27237(17) 0.0171(4) Uani 1 1 d . . .
C2 C 0.1718(2) 0.06206(19) 0.21530(17) 0.0170(4) Uani 1 1 d . . .
C3 C 0.1337(2) -0.01437(19) 0.10933(17) 0.0191(4) Uani 1 1 d . . .
H3A H 0.0374 -0.0520 0.0705 0.023 Uiso 1 1 calc R . .
C4 C 0.2402(2) -0.0331(2) 0.06337(18) 0.0217(4) Uani 1 1 d . . .
H4 H 0.2166 -0.0839 -0.0070 0.026 Uiso 1 1 calc R . .
C5 C 0.4196(2) 0.1009(2) 0.21934(19) 0.0238(5) Uani 1 1 d . . .
H5 H 0.5175 0.1402 0.2544 0.029 Uiso 1 1 calc R . .
C6 C 0.3176(2) 0.1231(2) 0.26860(19) 0.0220(4) Uani 1 1 d . . .
H6 H 0.3455 0.1784 0.3369 0.026 Uiso 1 1 calc R . .
C7 C -0.0087(2) 0.17512(18) 0.52172(17) 0.0175(4) Uani 1 1 d . . .
H7 H 0.0857 0.2108 0.5644 0.021 Uiso 1 1 calc R . .
C8 C -0.1245(2) 0.17916(18) 0.57622(17) 0.0170(4) Uani 1 1 d . . .
C9 C -0.2674(2) 0.14252(19) 0.51608(17) 0.0179(4) Uani 1 1 d . . .
C10 C -0.3724(2) 0.1539(2) 0.57339(19) 0.0228(4) Uani 1 1 d . . .
H10 H -0.4668 0.1292 0.5336 0.027 Uiso 1 1 calc R . .
C11 C -0.3369(2) 0.2015(2) 0.68908(19) 0.0245(5) Uani 1 1 d . . .
H11 H -0.4076 0.2091 0.7267 0.029 Uiso 1 1 calc R . .
C12 C -0.1962(2) 0.23824(19) 0.74975(18) 0.0234(5) Uani 1 1 d . . .
H12 H -0.1730 0.2700 0.8277 0.028 Uiso 1 1 calc R . .
C13 C -0.0915(2) 0.22754(19) 0.69413(18) 0.0205(4) Uani 1 1 d . . .
H13 H 0.0025 0.2526 0.7350 0.025 Uiso 1 1 calc R . .
C14 C -0.0978(2) 0.3250(2) 0.21474(19) 0.0235(5) Uani 1 1 d . . .
C15 C -0.0321(3) 0.4535(2) 0.1869(3) 0.0392(6) Uani 1 1 d . . .
H15A H -0.0256 0.5120 0.2507 0.059 Uiso 1 1 calc R . .
H15B H -0.0914 0.4607 0.1200 0.059 Uiso 1 1 calc R . .
H15C H 0.0640 0.4728 0.1715 0.059 Uiso 1 1 calc R . .
N5 N 0.0888(5) 0.5189(5) 0.5211(5) 0.0563(10) Uiso 0.50 1 d PD . 1
C16 C 0.1744(6) 0.5066(6) 0.4773(5) 0.0563(10) Uiso 0.50 1 d PD A 1
C17 C 0.2798(7) 0.4891(7) 0.4179(7) 0.0563(10) Uiso 0.50 1 d PD A 1
H17A H 0.2638 0.4020 0.4131 0.084 Uiso 0.50 1 calc PR A 1
H17B H 0.3765 0.5421 0.4595 0.084 Uiso 0.50 1 calc PR A 1
H17C H 0.2694 0.5113 0.3417 0.084 Uiso 0.50 1 calc PR A 1
N5 N 0.4699(8) 0.6486(7) 0.5408(7) 0.0432(17) Uiso 0.262(3) 1 d PD B 2
C16 C 0.3719(9) 0.5658(9) 0.4878(9) 0.0432(17) Uiso 0.262(3) 1 d PD B 2
C17 C 0.2484(10) 0.4620(10) 0.4171(11) 0.0432(17) Uiso 0.262(3) 1 d PD B 2
H17D H 0.1598 0.4644 0.4323 0.065 Uiso 0.262(3) 1 calc PR B 2
H17E H 0.2491 0.3834 0.4343 0.065 Uiso 0.262(3) 1 calc PR B 2
H17F H 0.2539 0.4689 0.3373 0.065 Uiso 0.262(3) 1 calc PR B 2
N5 N 0.3861 0.6574 0.5835 0.051(2) Uiso 0.238(3) 1 d PD C 3
C16 C 0.3211 0.5735 0.5145 0.051(2) Uiso 0.238(3) 1 d PD C 3
C17 C 0.2566 0.4699 0.4198 0.051(2) Uiso 0.238(3) 1 d PD C 3
H17G H 0.1542 0.4239 0.4201 0.076 Uiso 0.238(3) 1 calc PR C 3
H17H H 0.3033 0.4142 0.4285 0.076 Uiso 0.238(3) 1 calc PR C 3
H17I H 0.2697 0.5033 0.3481 0.076 Uiso 0.238(3) 1 calc PR C 3
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 107.25(7) . . ?
O4 Mo1 O2 99.50(7) . . ?
O3 Mo1 O2 101.55(6) . . ?
O4 Mo1 O1 98.47(7) . . ?
O3 Mo1 O1 97.28(6) . . ?
O2 Mo1 O1 148.70(6) . . ?
O4 Mo1 N1 94.32(7) . . ?
O3 Mo1 N1 157.35(6) . . ?
O2 Mo1 N1 81.06(6) . . ?
O1 Mo1 N1 72.21(6) . . ?
O4 Mo1 N4 170.06(7) . . ?
O3 Mo1 N4 82.50(6) . . ?
O2 Mo1 N4 79.96(6) . . ?
O1 Mo1 N4 77.97(6) . . ?
N1 Mo1 N4 75.77(6) . . ?
O6 Mo2 O7 103.90(8) . . ?
O6 Mo2 O8 103.35(7) . . ?
O7 Mo2 O8 89.03(7) . . ?
O6 Mo2 O5 103.19(7) . . ?
O7 Mo2 O5 87.29(7) . . ?
O8 Mo2 O5 153.32(6) . . ?
O6 Mo2 O13 102.95(8) . 2_665 ?
O7 Mo2 O13 153.10(7) . 2_665 ?
O8 Mo2 O13 86.30(7) . 2_665 ?
O5 Mo2 O13 85.15(6) . 2_665 ?
O6 Mo2 O9 178.87(7) . . ?
O7 Mo2 O9 77.12(5) . . ?
O8 Mo2 O9 77.10(4) . . ?
O5 Mo2 O9 76.31(4) . . ?
O13 Mo2 O9 76.01(4) 2_665 . ?
O11 Mo3 O10 102.69(7) . . ?
O11 Mo3 O5 104.02(7) . 2_665 ?
O10 Mo3 O5 88.84(7) . 2_665 ?
O11 Mo3 O12 104.33(7) . . ?
O10 Mo3 O12 152.83(6) . . ?
O5 Mo3 O12 87.31(6) 2_665 . ?
O11 Mo3 O8 102.52(7) . . ?
O10 Mo3 O8 86.85(7) . . ?
O5 Mo3 O8 153.42(6) 2_665 . ?
O12 Mo3 O8 84.69(7) . . ?
O11 Mo3 O9 178.76(5) . . ?
O10 Mo3 O9 76.87(4) . . ?
O5 Mo3 O9 77.15(4) 2_665 . ?
O12 Mo3 O9 76.05(4) . . ?
O8 Mo3 O9 76.32(4) . . ?
O14 Mo4 O13 103.13(9) . . ?
O14 Mo4 O12 104.22(7) . . ?
O13 Mo4 O12 89.57(7) . . ?
O14 Mo4 O10 103.31(7) . 2_665 ?
O13 Mo4 O10 86.87(7) . 2_665 ?
O12 Mo4 O10 152.34(6) . 2_665 ?
O14 Mo4 O7 103.82(9) . . ?
O13 Mo4 O7 152.93(6) . . ?
O12 Mo4 O7 86.32(7) . . ?
O10 Mo4 O7 84.52(6) 2_665 . ?
O14 Mo4 O9 179.19(6) . . ?
O13 Mo4 O9 77.06(5) . . ?
O12 Mo4 O9 76.56(4) . . ?
O10 Mo4 O9 75.91(4) 2_665 . ?
O7 Mo4 O9 75.96(4) . . ?
C1 O1 Mo1 118.72(12) . . ?
C9 O2 Mo1 135.19(13) . . ?
Mo3 O5 Mo2 116.69(7) 2_665 . ?
Mo2 O7 Mo4 116.86(7) . . ?
Mo2 O8 Mo3 116.32(7) . . ?
Mo4 O9 Mo4 180.0 2_665 . ?
Mo4 O9 Mo3 89.875(7) 2_665 2_665 ?
Mo4 O9 Mo3 90.125(7) . 2_665 ?
Mo4 O9 Mo3 90.125(7) 2_665 . ?
Mo4 O9 Mo3 89.875(7) . . ?
Mo3 O9 Mo3 180.0 2_665 . ?
Mo4 O9 Mo2 90.004(8) 2_665 . ?
Mo4 O9 Mo2 89.996(8) . . ?
Mo3 O9 Mo2 89.746(7) 2_665 . ?
Mo3 O9 Mo2 90.254(7) . . ?
Mo4 O9 Mo2 89.996(8) 2_665 2_665 ?
Mo4 O9 Mo2 90.004(8) . 2_665 ?
Mo3 O9 Mo2 90.254(7) 2_665 2_665 ?
Mo3 O9 Mo2 89.746(7) . 2_665 ?
Mo2 O9 Mo2 180.000(12) . 2_665 ?
Mo3 O10 Mo4 117.09(7) . 2_665 ?
Mo4 O12 Mo3 117.38(7) . . ?
Mo4 O13 Mo2 116.91(7) . 2_665 ?
C7 N1 N2 115.77(16) . . ?
C7 N1 Mo1 128.70(13) . . ?
N2 N1 Mo1 115.43(11) . . ?
C1 N2 N1 108.81(16) . . ?
C4 N3 C5 123.01(18) . . ?
C14 N4 Mo1 176.90(18) . . ?
N2 C1 O1 124.73(17) . . ?
N2 C1 C2 118.04(18) . . ?
O1 C1 C2 117.20(17) . . ?
C6 C2 C3 119.40(18) . . ?
C6 C2 C1 120.43(18) . . ?
C3 C2 C1 120.12(18) . . ?
C4 C3 C2 119.1(2) . . ?
N3 C4 C3 119.6(2) . . ?
N3 C5 C6 119.6(2) . . ?
C5 C6 C2 119.1(2) . . ?
N1 C7 C8 123.20(18) . . ?
C9 C8 C13 118.46(18) . . ?
C9 C8 C7 123.11(18) . . ?
C13 C8 C7 118.36(18) . . ?
O2 C9 C10 117.72(19) . . ?
O2 C9 C8 122.27(17) . . ?
C10 C9 C8 119.98(19) . . ?
C11 C10 C9 120.3(2) . . ?
C10 C11 C12 120.4(2) . . ?
C13 C12 C11 119.83(19) . . ?
C12 C13 C8 121.0(2) . . ?
N4 C14 C15 179.0(3) . . ?
C16 N5 N5 133.7(7) . 2_566 ?
N5 C16 C17 178.1(8) . . ?
N5 C16 C17 178.2(13) . . ?
N5 C16 C17 171.960(1) . . ?
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 1.6803(15) . ?
Mo1 O3 1.7192(14) . ?
Mo1 O2 1.9227(13) . ?
Mo1 O1 2.0094(13) . ?
Mo1 N1 2.2343(17) . ?
Mo1 N4 2.4226(18) . ?
Mo2 O6 1.6848(16) . ?
Mo2 O7 1.8902(16) . ?
Mo2 O8 1.9140(14) . ?
Mo2 O5 1.9458(14) . ?
Mo2 O13 1.9503(16) 2_665 ?
Mo2 O9 2.3215(2) . ?
Mo3 O11 1.6894(14) . ?
Mo3 O10 1.8957(14) . ?
Mo3 O5 1.9015(15) 2_665 ?
Mo3 O12 1.9289(14) . ?
Mo3 O8 1.9581(15) . ?
Mo3 O9 2.32034(18) . ?
Mo4 O14 1.6758(16) . ?
Mo4 O13 1.8986(16) . ?
Mo4 O12 1.9052(14) . ?
Mo4 O10 1.9525(14) 2_665 ?
Mo4 O7 1.9594(16) . ?
Mo4 O9 2.3173(2) . ?
O1 C1 1.319(2) . ?
O2 C9 1.351(2) . ?
O5 Mo3 1.9015(14) 2_665 ?
O9 Mo4 2.3173(2) 2_665 ?
O9 Mo3 2.32034(18) 2_665 ?
O9 Mo2 2.3215(2) 2_665 ?
O10 Mo4 1.9525(14) 2_665 ?
O13 Mo2 1.9503(16) 2_665 ?
N1 C7 1.289(2) . ?
N1 N2 1.397(2) . ?
N2 C1 1.293(3) . ?
N3 C4 1.331(3) . ?
N3 C5 1.343(3) . ?
N4 C14 1.125(3) . ?
C1 C2 1.475(3) . ?
C2 C6 1.390(3) . ?
C2 C3 1.396(3) . ?
C3 C4 1.370(3) . ?
C5 C6 1.367(3) . ?
C7 C8 1.441(3) . ?
C8 C9 1.408(3) . ?
C8 C13 1.409(3) . ?
C9 C10 1.392(3) . ?
C10 C11 1.381(3) . ?
C11 C12 1.391(3) . ?
C12 C13 1.376(3) . ?
C14 C15 1.456(3) . ?
N5 C16 1.1303(18) . ?
N5 N5 1.674(10) 2_566 ?
C16 C17 1.4391(19) . ?
N5 C16 1.1300(19) . ?
C16 C17 1.4392(19) . ?
N5 C16 1.1293 . ?
C16 C17 1.4526 . ?
