#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:24:55 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180392 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/61/7206159.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_7206159
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(C17 H19 Mo N4 O4), Mo6 O19, 2(H2 O), 2(HO)'
_chemical_formula_sum            'C34 H44 Mo8 N8 O31'
_chemical_formula_weight         1828.29
_chemical_name_common
;
bis(cis-dioxo(2-oxo-4-diethylaminobenzaldehyde
isonicotinylhydrazonato-O, N,O)molybdenum(VI)) hexamolybdate aqua (1/4)
;
_chemical_name_systematic
;
bis(cis-dioxo(2-oxo-4-diethylaminobenzaldehyde isonicotinylhydrazonato-
O, N,O)molybdenum(VI)) hexamolybdate aqua (1/4)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.231(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.2754(8)
_cell_length_b                   7.9268(5)
_cell_length_c                   29.789(2)
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      15
_cell_volume                     2655.2(3)
_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  0.0344
_diffrn_reflns_av_sigmaI/netI    0.0350
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            23290
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         4.26
_exptl_absorpt_coefficient_mu    1.927
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81092
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.279
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1764
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.783
_refine_diff_density_min         -0.712
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_hydrogen_treatment    costr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         5762
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.175
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0444
_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)+(0.0177P)²+6.4984P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0758
_refine_ls_wR_factor_ref         0.0796
_reflns_number_gt                4641
_reflns_number_total             5762
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0ce00927j.txt
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7206159
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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 0.91978(4) 0.24965(6) 0.137899(13) 0.02978(11) Uani 1 1 d . . .
Mo2 Mo 0.66687(4) 0.60979(6) 0.969707(14) 0.02817(11) Uani 1 1 d . . .
Mo3 Mo 0.61838(4) 0.39699(6) 1.060958(13) 0.02537(11) Uani 1 1 d . . .
Mo4 Mo 0.52441(4) 0.24825(6) 0.961758(14) 0.02748(10) Uani 1 1 d . . .
O1 O 0.9365(3) 0.2747(4) 0.07218(11) 0.0294(8) Uani 1 1 d . . .
O2 O 0.8304(3) 0.1706(5) 0.18598(11) 0.0370(9) Uani 1 1 d . . .
O4 O 1.0557(3) 0.1713(6) 0.15400(13) 0.0496(11) Uani 1 1 d . . .
O3 O 0.9253(3) 0.4611(5) 0.14870(12) 0.0414(9) Uani 1 1 d . . .
O5 O 0.6192(3) 0.2188(4) 1.01922(11) 0.0278(8) Uani 1 1 d . . .
O6 O 0.7096(3) 0.3324(5) 1.10595(11) 0.0326(8) Uani 1 1 d . . .
O7 O 0.7330(3) 0.5112(5) 1.02369(11) 0.0297(8) Uani 1 1 d . . .
O8 O 0.7849(3) 0.6886(5) 0.94500(12) 0.0381(9) Uani 1 1 d . . .
O9 O 0.6540(3) 0.3856(4) 0.94434(11) 0.0300(8) Uani 1 1 d . . .
O10 O 0.5000 0.5000 1.0000 0.0211(10) Uani 1 2 d S . .
O11 O 0.5800(3) 0.6261(4) 1.07890(10) 0.0276(7) Uani 1 1 d . . .
O12 O 0.5349(3) 0.6636(4) 0.92438(10) 0.0276(8) Uani 1 1 d . . .
O13 O 0.6122(3) 0.7936(4) 1.00365(11) 0.0288(8) Uani 1 1 d . . .
O14 O 0.5443(4) 0.0687(4) 0.93356(12) 0.0407(9) Uani 1 1 d . . .
N1 N 0.8356(3) 0.0290(5) 0.10422(13) 0.0260(9) Uani 1 1 d . . .
N2 N 0.8422(3) 0.0207(5) 0.05772(12) 0.0261(9) Uani 1 1 d . . .
N3 N 0.9305(4) 0.2142(6) -0.09336(15) 0.0410(12) Uani 1 1 d . . .
H3 H 0.9365 0.2273 -0.1218 0.049 Uiso 1 1 calc R . .
C1 C 0.8958(4) 0.1534(6) 0.04447(15) 0.0234(10) Uani 1 1 d . . .
C2 C 0.9086(4) 0.1755(6) -0.00430(15) 0.0248(10) Uani 1 1 d . . .
C3 C 0.9873(4) 0.2935(6) -0.01941(16) 0.0301(11) Uani 1 1 d . . .
H31 H 1.0331 0.3599 0.0009 0.036 Uiso 1 1 calc R . .
C4 C 0.9966(5) 0.3109(7) -0.06475(18) 0.0387(13) Uani 1 1 d . . .
H4 H 1.0486 0.3896 -0.0755 0.046 Uiso 1 1 calc R . .
C5 C 0.8555(5) 0.0982(8) -0.07977(17) 0.0390(13) Uani 1 1 d . . .
H5 H 0.8122 0.0318 -0.1009 0.047 Uiso 1 1 calc R . .
C6 C 0.8422(4) 0.0766(7) -0.03516(16) 0.0318(12) Uani 1 1 d . . .
H6 H 0.7893 -0.0033 -0.0255 0.038 Uiso 1 1 calc R . .
C7 C 0.7747(4) -0.0930(6) 0.12151(16) 0.0286(11) Uani 1 1 d . . .
H7 H 0.7455 -0.1783 0.1023 0.034 Uiso 1 1 calc R . .
C8 C 0.7802(5) 0.0254(7) 0.19834(17) 0.0317(11) Uani 1 1 d . . .
C9 C 0.7563(5) 0.0084(8) 0.24250(18) 0.0402(14) Uani 1 1 d . . .
H9 H 0.7790 0.0939 0.2627 0.048 Uiso 1 1 calc R . .
C10 C 0.6984(7) -0.1349(9) 0.2582(2) 0.060(2) Uani 1 1 d . A .
C11 C 0.6650(8) -0.2621(10) 0.2259(2) 0.076(2) Uani 1 1 d . . .
H11 H 0.6241 -0.3571 0.2346 0.091 Uiso 1 1 calc R . .
C12 C 0.6925(6) -0.2456(9) 0.1823(2) 0.0550(17) Uani 1 1 d . . .
H12 H 0.6718 -0.3321 0.1621 0.066 Uiso 1 1 calc R . .
C13 C 0.7508(5) -0.1036(7) 0.16678(16) 0.0343(12) Uani 1 1 d . . .
N4 N 0.6737(7) -0.1478(7) 0.30154(19) 0.092(3) Uani 1 1 d D . .
C14 C 0.7161(7) -0.0191(9) 0.3358(2) 0.064(2) Uani 1 1 d D A .
H14A H 0.7203 -0.0692 0.3656 0.077 Uiso 1 1 calc R . .
H14B H 0.7952 0.0187 0.3298 0.077 Uiso 1 1 calc R . .
C15 C 0.6346(7) 0.1245(12) 0.3342(3) 0.092(3) Uani 1 1 d D . .
H15A H 0.6619 0.2060 0.3565 0.138 Uiso 1 1 calc R A .
H15B H 0.5565 0.0866 0.3402 0.138 Uiso 1 1 calc R . .
H15C H 0.6320 0.1752 0.3049 0.138 Uiso 1 1 calc R . .
C16A C 0.6407(11) -0.3161(15) 0.3226(4) 0.065(5) Uani 0.60(2) 1 d PDU A 1
H16A H 0.6769 -0.4095 0.3075 0.078 Uiso 0.60(2) 1 calc PR A 1
H16B H 0.6670 -0.3191 0.3543 0.078 Uiso 0.60(2) 1 calc PR A 1
C17A C 0.5099(11) -0.325(2) 0.3163(5) 0.099(8) Uani 0.60(2) 1 d PDU A 1
H17A H 0.4832 -0.4294 0.3286 0.149 Uiso 0.60(2) 1 calc PR A 1
H17B H 0.4856 -0.3207 0.2847 0.149 Uiso 0.60(2) 1 calc PR A 1
H17C H 0.4758 -0.2322 0.3314 0.149 Uiso 0.60(2) 1 calc PR A 1
C16B C 0.5591(12) -0.240(2) 0.3121(5) 0.058(7) Uani 0.40(2) 1 d PDU A 2
H16C H 0.5175 -0.1782 0.3341 0.070 Uiso 0.40(2) 1 calc PR A 2
H16D H 0.5066 -0.2537 0.2850 0.070 Uiso 0.40(2) 1 calc PR A 2
C17B C 0.597(2) -0.406(2) 0.3301(8) 0.092(10) Uani 0.40(2) 1 d PDU A 2
H17D H 0.5291 -0.4692 0.3378 0.138 Uiso 0.40(2) 1 calc PR A 2
H17E H 0.6505 -0.3908 0.3565 0.138 Uiso 0.40(2) 1 calc PR A 2
H17F H 0.6376 -0.4666 0.3078 0.138 Uiso 0.40(2) 1 calc PR A 2
O1W O 0.9458(5) 0.2795(7) 0.31454(15) 0.0720(15) Uani 1 1 d U . .
O2W O 0.9233(7) 0.5482(12) 0.2491(3) 0.153(3) Uiso 1 1 d . . .
H11W H 0.9114 0.3730 0.3038 0.229 Uiso 1 1 d . . .
H21W H 0.9301 0.5116 0.2227 0.229 Uiso 1 1 d . . .
H12W H 0.9673 0.2215 0.2911 0.229 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'
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 106.7(2) . . ?
O4 Mo1 O2 100.59(19) . . ?
O3 Mo1 O2 101.18(17) . . ?
O4 Mo1 O1 99.56(17) . . ?
O3 Mo1 O1 94.75(16) . . ?
O2 Mo1 O1 149.40(14) . . ?
O4 Mo1 N1 100.91(18) . . ?
O3 Mo1 N1 151.20(17) . . ?
O2 Mo1 N1 81.24(15) . . ?
O1 Mo1 N1 72.49(14) . . ?
O8 Mo2 O7 104.46(16) . . ?
O8 Mo2 O13 104.19(17) . . ?
O7 Mo2 O13 89.28(14) . . ?
O8 Mo2 O9 102.07(17) . . ?
O7 Mo2 O9 88.05(15) . . ?
O13 Mo2 O9 153.44(14) . . ?
O8 Mo2 O12 101.54(15) . . ?
O7 Mo2 O12 153.90(14) . . ?
O13 Mo2 O12 86.60(14) . . ?
O9 Mo2 O12 84.28(14) . . ?
O8 Mo2 O10 177.08(12) . . ?
O7 Mo2 O10 78.11(10) . . ?
O13 Mo2 O10 77.07(10) . . ?
O9 Mo2 O10 76.51(10) . . ?
O12 Mo2 O10 75.84(9) . . ?
O6 Mo3 O12 104.64(15) . 3_667 ?
O6 Mo3 O5 105.17(16) . . ?
O12 Mo3 O5 90.62(15) 3_667 . ?
O6 Mo3 O11 101.37(15) . . ?
O12 Mo3 O11 86.99(14) 3_667 . ?
O5 Mo3 O11 153.07(13) . . ?
O6 Mo3 O7 101.33(15) . . ?
O12 Mo3 O7 153.72(13) 3_667 . ?
O5 Mo3 O7 86.43(15) . . ?
O11 Mo3 O7 84.01(14) . . ?
O6 Mo3 O10 176.63(13) . . ?
O12 Mo3 O10 77.63(10) 3_667 . ?
O5 Mo3 O10 77.15(9) . . ?
O11 Mo3 O10 76.14(9) . . ?
O7 Mo3 O10 76.26(9) . . ?
O14 Mo4 O11 102.97(16) . 3_667 ?
O14 Mo4 O9 102.29(17) . . ?
O11 Mo4 O9 88.76(14) 3_667 . ?
O14 Mo4 O13 105.16(17) . 3_667 ?
O11 Mo4 O13 87.13(14) 3_667 3_667 ?
O9 Mo4 O13 152.48(14) . 3_667 ?
O14 Mo4 O5 104.58(16) . . ?
O11 Mo4 O5 152.45(14) 3_667 . ?
O9 Mo4 O5 85.83(14) . . ?
O13 Mo4 O5 85.36(14) 3_667 . ?
O14 Mo4 O10 178.74(14) . . ?
O11 Mo4 O10 76.87(10) 3_667 . ?
O9 Mo4 O10 76.47(10) . . ?
O13 Mo4 O10 76.10(10) 3_667 . ?
O5 Mo4 O10 75.60(9) . . ?
C1 O1 Mo1 119.1(3) . . ?
C8 O2 Mo1 137.6(3) . . ?
Mo3 O5 Mo4 117.25(15) . . ?
Mo2 O7 Mo3 115.61(15) . . ?
Mo4 O9 Mo2 116.86(16) . . ?
Mo2 O10 Mo2 179.998(1) . 3_667 ?
Mo2 O10 Mo3 89.989(16) . 3_667 ?
Mo2 O10 Mo3 90.013(16) 3_667 3_667 ?
Mo2 O10 Mo3 90.011(16) . . ?
Mo2 O10 Mo3 89.987(16) 3_667 . ?
Mo3 O10 Mo3 180.0 3_667 . ?
Mo2 O10 Mo4 89.845(17) . 3_667 ?
Mo2 O10 Mo4 90.153(17) 3_667 3_667 ?
Mo3 O10 Mo4 89.960(15) 3_667 3_667 ?
Mo3 O10 Mo4 90.038(16) . 3_667 ?
Mo2 O10 Mo4 90.154(17) . . ?
Mo2 O10 Mo4 89.848(17) 3_667 . ?
Mo3 O10 Mo4 90.039(16) 3_667 . ?
Mo3 O10 Mo4 89.963(16) . . ?
Mo4 O10 Mo4 180.0 3_667 . ?
Mo4 O11 Mo3 116.84(15) 3_667 . ?
Mo3 O12 Mo2 116.41(16) 3_667 . ?
Mo2 O13 Mo4 116.84(16) . 3_667 ?
C7 N1 N2 115.0(4) . . ?
C7 N1 Mo1 128.9(3) . . ?
N2 N1 Mo1 116.0(3) . . ?
C1 N2 N1 109.0(4) . . ?
C4 N3 C5 122.7(5) . . ?
N2 C1 O1 123.3(4) . . ?
N2 C1 C2 118.6(4) . . ?
O1 C1 C2 118.1(4) . . ?
C6 C2 C3 119.6(5) . . ?
C6 C2 C1 119.8(5) . . ?
C3 C2 C1 120.6(4) . . ?
C4 C3 C2 119.0(5) . . ?
N3 C4 C3 119.6(5) . . ?
N3 C5 C6 120.1(5) . . ?
C5 C6 C2 119.0(5) . . ?
N1 C7 C13 124.5(5) . . ?
O2 C8 C9 117.6(5) . . ?
O2 C8 C13 121.3(4) . . ?
C9 C8 C13 121.0(5) . . ?
C8 C9 C10 121.9(5) . . ?
N4 C10 C9 120.9(6) . . ?
N4 C10 C11 122.1(6) . . ?
C9 C10 C11 116.9(5) . . ?
C12 C11 C10 120.5(6) . . ?
C11 C12 C13 122.5(6) . . ?
C7 C13 C12 119.8(5) . . ?
C7 C13 C8 123.1(5) . . ?
C12 C13 C8 117.1(5) . . ?
C10 N4 C14 121.7(5) . . ?
C10 N4 C16A 122.2(7) . . ?
C14 N4 C16A 112.9(7) . . ?
C10 N4 C16B 118.0(8) . . ?
C14 N4 C16B 114.6(8) . . ?
C16A N4 C16B 42.9(8) . . ?
C15 C14 N4 109.9(6) . . ?
C17A C16A N4 105.2(7) . . ?
C17B C16B N4 105.8(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 1.690(4) . ?
Mo1 O3 1.707(4) . ?
Mo1 O2 1.917(3) . ?
Mo1 O1 1.990(3) . ?
Mo1 N1 2.197(4) . ?
Mo2 O8 1.688(3) . ?
Mo2 O7 1.891(3) . ?
Mo2 O13 1.902(3) . ?
Mo2 O9 1.932(4) . ?
Mo2 O12 1.981(3) . ?
Mo2 O10 2.3157(4) . ?
Mo3 O6 1.707(3) . ?
Mo3 O12 1.876(3) 3_667 ?
Mo3 O5 1.882(3) . ?
Mo3 O11 1.951(3) . ?
Mo3 O7 1.983(3) . ?
Mo3 O10 2.3213(4) . ?
Mo4 O14 1.676(3) . ?
Mo4 O11 1.906(3) 3_667 ?
Mo4 O9 1.923(3) . ?
Mo4 O13 1.944(3) 3_667 ?
Mo4 O5 1.964(3) . ?
Mo4 O10 2.3243(4) . ?
O1 C1 1.327(5) . ?
O2 C8 1.346(6) . ?
O10 Mo2 2.3157(4) 3_667 ?
O10 Mo3 2.3212(4) 3_667 ?
O10 Mo4 2.3242(4) 3_667 ?
O11 Mo4 1.906(3) 3_667 ?
O12 Mo3 1.876(3) 3_667 ?
O13 Mo4 1.944(3) 3_667 ?
N1 C7 1.313(6) . ?
N1 N2 1.394(5) . ?
N2 C1 1.289(6) . ?
N3 C4 1.332(7) . ?
N3 C5 1.333(7) . ?
C1 C2 1.481(6) . ?
C2 C6 1.385(7) . ?
C2 C3 1.387(7) . ?
C3 C4 1.369(7) . ?
C5 C6 1.359(7) . ?
C7 C13 1.397(7) . ?
C8 C9 1.369(7) . ?
C8 C13 1.412(7) . ?
C9 C10 1.407(8) . ?
C10 N4 1.346(7) . ?
C10 C11 1.425(9) . ?
C11 C12 1.362(8) . ?
C12 C13 1.399(8) . ?
N4 C14 1.497(7) . ?
N4 C16A 1.531(9) . ?
N4 C16B 1.538(10) . ?
C14 C15 1.462(9) . ?
C16A C17A 1.475(10) . ?
C16B C17B 1.471(11) . ?
