#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/03/2230367.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2230367
loop_
_publ_author_name
'Wong, Hon Wee'
'Lo, Kong Mun'
'Ng, Seik Weng'
_publ_section_title
;
 Poly[μ-aqua-aqua{μ-6-ethoxy-2-[(2-isonicotinoylhydrazinylidene)methyl]phenolato-κ³O,N,O'}dioxidosodiumvanadate(V)]
;
_journal_coeditor_code           IM2289
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m799
_journal_paper_doi               10.1107/S1600536811019106
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Na V (C15 H13 N3 O3) O2 (H2 O)2]'
_chemical_formula_moiety         'C15 H17 N3 Na O7 V'
_chemical_formula_sum            'C15 H17 N3 Na O7 V'
_chemical_formula_weight         425.25
_chemical_name_systematic
;
Poly[μ-aqua-aqua{μ-6-ethoxy-2-[(2-
isonicotinoylhydrazinylidene)methyl]phenolato-
κ³O,N,O'}dioxidosodiumvanadate(V)]
;
_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                 106.4902(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.1731(2)
_cell_length_b                   14.6913(2)
_cell_length_c                   13.2277(2)
_cell_measurement_reflns_used    9902
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.35
_cell_measurement_theta_min      2.61
_cell_volume                     3572.69(8)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'X-SEED (Barbour, 2001)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       ω
_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  0.0195
_diffrn_reflns_av_sigmaI/netI    0.0224
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            23057
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.17
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.624
_exptl_absorpt_correction_T_max  0.7885
_exptl_absorpt_correction_T_min  0.7885
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            'Dark brown'
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.563
_refine_diff_density_min         -0.737
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         8084
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0684P)²+2.7411P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1111
_refine_ls_wR_factor_ref         0.1202
_reflns_number_gt                6785
_reflns_number_total             8084
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            im2289.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2230367
_cod_database_fobs_code          2230367
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_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_disorder_assembly
_atom_site_disorder_group
V V1 0.117273(15) 0.64283(2) 0.60824(2) 0.01136(9) Uani d . 1 1 . .
V V2 0.385383(15) 0.35452(2) 0.37870(2) 0.01121(9) Uani d . 1 1 . .
Na Na1 0.26390(4) 0.49475(5) 0.64647(6) 0.01554(16) Uani d . 1 1 . .
Na Na2 0.23922(4) 0.50365(5) 0.33801(6) 0.01598(17) Uani d . 1 1 . .
O O1 0.24513(7) 0.43456(10) 0.81471(11) 0.0192(3) Uani d . 1 1 . .
O O2 0.15035(7) 0.53002(9) 0.67556(10) 0.0146(3) Uani d . 1 1 . .
O O3 0.04859(7) 0.70200(9) 0.48708(10) 0.0156(3) Uani d . 1 1 . .
O O4 0.18565(7) 0.65269(9) 0.55605(11) 0.0158(3) Uani d . 1 1 . .
O O5 0.12649(7) 0.71610(9) 0.70224(11) 0.0189(3) Uani d . 1 1 . .
O O6 0.26740(7) 0.57022(10) 0.17087(11) 0.0196(3) Uani d . 1 1 . .
O O7 0.35533(7) 0.47021(9) 0.31652(10) 0.0146(3) Uani d . 1 1 . .
O O8 0.44973(7) 0.28505(9) 0.49566(10) 0.0160(3) Uani d . 1 1 . .
O O9 0.31480(7) 0.34343(9) 0.42565(11) 0.0155(3) Uani d . 1 1 . .
O O10 0.37743(7) 0.28683(9) 0.27927(11) 0.0177(3) Uani d . 1 1 . .
O O1w 0.19031(7) 0.42958(9) 0.47312(11) 0.0168(3) Uani d . 1 1 . .
H H11 0.1954 0.3728 0.4722 0.025 Uiso calc R 1 1 . .
H H12 0.1460 0.4416 0.4623 0.025 Uiso calc R 1 1 . .
O O2w 0.30731(7) 0.57278(9) 0.50975(11) 0.0170(3) Uani d . 1 1 . .
H H21 0.3523 0.5650 0.5209 0.026 Uiso calc R 1 1 . .
H H22 0.2990 0.6289 0.5098 0.026 Uiso calc R 1 1 . .
O O3w 0.32561(8) 0.35904(10) 0.64240(12) 0.0233(3) Uani d . 1 1 . .
H H31 0.3100 0.3187 0.6754 0.035 Uiso calc R 1 1 . .
H H32 0.3189 0.3426 0.5795 0.035 Uiso calc R 1 1 . .
O O4w 0.16471(8) 0.63013(10) 0.33428(12) 0.0240(3) Uani d . 1 1 . .
H H41 0.1705 0.6492 0.3960 0.036 Uiso calc R 1 1 . .
H H42 0.1758 0.6714 0.2978 0.036 Uiso calc R 1 1 . .
N N1 0.01291(8) 0.58117(10) 0.59125(12) 0.0129(3) Uani d . 1 1 . .
N N2 -0.04650(8) 0.62497(11) 0.52086(12) 0.0131(3) Uani d . 1 1 . .
N N3 -0.16486(9) 0.88260(12) 0.27671(13) 0.0196(3) Uani d . 1 1 . .
N N4 0.49119(8) 0.41490(11) 0.41014(12) 0.0128(3) Uani d . 1 1 . .
N N5 0.54804(8) 0.36662(11) 0.47984(12) 0.0137(3) Uani d . 1 1 . .
N N6 0.65617(9) 0.10161(12) 0.72044(13) 0.0208(4) Uani d . 1 1 . .
C C1 0.31672(12) 0.41932(18) 0.99966(17) 0.0331(5) Uani d . 1 1 . .
H H1A 0.3547 0.3823 1.0472 0.050 Uiso calc R 1 1 . .
H H1B 0.2725 0.4172 1.0227 0.050 Uiso calc R 1 1 . .
H H1C 0.3335 0.4824 1.0010 0.050 Uiso calc R 1 1 . .
C C2 0.30060(11) 0.38249(14) 0.88914(16) 0.0215(4) Uani d . 1 1 . .
H H2A 0.3457 0.3833 0.8669 0.026 Uiso calc R 1 1 . .
H H2B 0.2844 0.3185 0.8884 0.026 Uiso calc R 1 1 . .
C C3 0.17389(10) 0.41942(13) 0.81015(15) 0.0157(4) Uani d . 1 1 . .
C C4 0.14874(11) 0.35585(13) 0.86843(16) 0.0200(4) Uani d . 1 1 . .
H H4 0.1824 0.3210 0.9207 0.024 Uiso calc R 1 1 . .
C C5 0.07381(12) 0.34254(14) 0.85081(16) 0.0225(4) Uani d . 1 1 . .
H H5 0.0570 0.2979 0.8902 0.027 Uiso calc R 1 1 . .
C C6 0.02461(11) 0.39376(14) 0.77681(16) 0.0198(4) Uani d . 1 1 . .
H H6 -0.0261 0.3842 0.7650 0.024 Uiso calc R 1 1 . .
C C7 0.04927(10) 0.46034(13) 0.71855(14) 0.0144(4) Uani d . 1 1 . .
C C8 0.12410(10) 0.47349(12) 0.73408(14) 0.0136(3) Uani d . 1 1 . .
C C9 -0.00366(10) 0.51195(13) 0.64041(14) 0.0146(4) Uani d . 1 1 . .
H H9 -0.0533 0.4942 0.6242 0.018 Uiso calc R 1 1 . .
C C10 -0.02060(9) 0.68851(12) 0.47280(14) 0.0136(3) Uani d . 1 1 . .
C C11 -0.07164(10) 0.75199(13) 0.40071(14) 0.0139(4) Uani d . 1 1 . .
C C12 -0.04406(11) 0.82798(14) 0.36272(16) 0.0207(4) Uani d . 1 1 . .
H H12A 0.0069 0.8367 0.3772 0.025 Uiso calc R 1 1 . .
C C13 -0.09251(11) 0.89082(15) 0.30320(17) 0.0232(4) Uani d . 1 1 . .
H H13 -0.0729 0.9434 0.2796 0.028 Uiso calc R 1 1 . .
C C14 -0.19078(10) 0.80815(14) 0.31169(15) 0.0175(4) Uani d . 1 1 . .
H H14 -0.2420 0.8001 0.2932 0.021 Uiso calc R 1 1 . .
C C15 -0.14690(10) 0.74169(13) 0.37369(15) 0.0162(4) Uani d . 1 1 . .
H H15 -0.1680 0.6902 0.3971 0.019 Uiso calc R 1 1 . .
C C16 0.14547(12) 0.57897(18) 0.0608(2) 0.0364(6) Uani d . 1 1 . .
H H16A 0.1122 0.6113 0.0017 0.055 Uiso calc R 1 1 . .
H H16B 0.1280 0.5845 0.1234 0.055 Uiso calc R 1 1 . .
H H16C 0.1474 0.5146 0.0426 0.055 Uiso calc R 1 1 . .
C C17 0.21980(12) 0.61956(16) 0.08341(18) 0.0295(5) Uani d . 1 1 . .
H H17A 0.2378 0.6147 0.0205 0.035 Uiso calc R 1 1 . .
H H17B 0.2184 0.6847 0.1017 0.035 Uiso calc R 1 1 . .
C C18 0.34010(10) 0.58845(13) 0.19174(15) 0.0171(4) Uani d . 1 1 . .
C C19 0.36960(12) 0.65790(14) 0.14579(17) 0.0227(4) Uani d . 1 1 . .
H H19 0.3387 0.6959 0.0940 0.027 Uiso calc R 1 1 . .
C C20 0.44503(12) 0.67204(14) 0.17573(17) 0.0238(4) Uani d . 1 1 . .
H H20 0.4648 0.7208 0.1454 0.029 Uiso calc R 1 1 . .
C C21 0.49049(11) 0.61638(14) 0.24814(16) 0.0204(4) Uani d . 1 1 . .
H H21A 0.5416 0.6261 0.2674 0.025 Uiso calc R 1 1 . .
C C22 0.46124(10) 0.54448(13) 0.29418(15) 0.0154(4) Uani d . 1 1 . .
C C23 0.38582(10) 0.53105(12) 0.26846(14) 0.0139(4) Uani d . 1 1 . .
C C24 0.51098(10) 0.48724(13) 0.36962(15) 0.0147(4) Uani d . 1 1 . .
H H24 0.5610 0.5034 0.3908 0.018 Uiso calc R 1 1 . .
C C25 0.51939(9) 0.29891(13) 0.51815(14) 0.0140(4) Uani d . 1 1 . .
C C26 0.56794(10) 0.23195(13) 0.58868(14) 0.0153(4) Uani d . 1 1 . .
C C27 0.53878(11) 0.15123(14) 0.61331(16) 0.0215(4) Uani d . 1 1 . .
H H27 0.4882 0.1390 0.5863 0.026 Uiso calc R 1 1 . .
C C28 0.58465(11) 0.08880(15) 0.67801(17) 0.0235(4) Uani d . 1 1 . .
H H28 0.5641 0.0334 0.6932 0.028 Uiso calc R 1 1 . .
C C29 0.68389(11) 0.17940(14) 0.69501(16) 0.0203(4) Uani d . 1 1 . .
H H29 0.7346 0.1897 0.7231 0.024 Uiso calc R 1 1 . .
C C30 0.64247(10) 0.24577(14) 0.62976(15) 0.0184(4) Uani d . 1 1 . .
H H30 0.6647 0.2995 0.6136 0.022 Uiso calc R 1 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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O5 V1 O4 . . 109.68(7) ?
O5 V1 O2 . . 105.72(7) ?
O4 V1 O2 . . 94.20(6) ?
O5 V1 O3 . . 103.57(7) ?
O4 V1 O3 . . 92.75(6) ?
O2 V1 O3 . . 145.51(6) ?
O5 V1 N1 . . 104.86(7) ?
O4 V1 N1 . . 144.96(6) ?
O2 V1 N1 . . 81.87(6) ?
O3 V1 N1 . . 73.30(6) ?
O10 V2 O9 . . 110.28(7) ?
O10 V2 O7 . . 104.46(6) ?
O9 V2 O7 . . 94.06(6) ?
O10 V2 O8 . . 102.31(6) ?
O9 V2 O8 . . 92.93(6) ?
O7 V2 O8 . . 147.93(6) ?
O10 V2 N4 . . 106.09(6) ?
O9 V2 N4 . . 143.14(6) ?
O7 V2 N4 . . 82.42(6) ?
O8 V2 N4 . . 73.42(6) ?
O3w Na1 O2 . . 133.37(6) ?
O3w Na1 O2w . . 95.81(6) ?
O2 Na1 O2w . . 122.09(5) ?
O3w Na1 O1 . . 85.44(5) ?
O2 Na1 O1 . . 64.20(5) ?
O2w Na1 O1 . . 166.33(5) ?
O3w Na1 O1w . . 79.05(5) ?
O2 Na1 O1w . . 85.86(5) ?
O2w Na1 O1w . . 74.23(5) ?
O1 Na1 O1w . . 119.27(5) ?
O3w Na1 N6 . 2_656 109.68(6) ?
O2 Na1 N6 . 2_656 98.88(6) ?
O2w Na1 N6 . 2_656 87.60(6) ?
O1 Na1 N6 . 2_656 79.20(6) ?
O1w Na1 N6 . 2_656 160.75(6) ?
O3w Na1 O4 . . 154.51(6) ?
O2 Na1 O4 . . 59.33(4) ?
O2w Na1 O4 . . 63.93(4) ?
O1 Na1 O4 . . 118.01(5) ?
O1w Na1 O4 . . 80.46(5) ?
N6 Na1 O4 2_656 . 85.94(5) ?
O4w Na2 O7 . . 138.65(6) ?
O4w Na2 O1w . . 90.58(5) ?
O7 Na2 O1w . . 123.51(5) ?
O4w Na2 O2w . . 81.61(5) ?
O7 Na2 O2w . . 85.82(5) ?
O1w Na2 O2w . . 74.38(5) ?
O4w Na2 N3 . 2_545 108.21(6) ?
O7 Na2 N3 . 2_545 99.93(6) ?
O1w Na2 N3 . 2_545 81.90(5) ?
O2w Na2 N3 . 2_545 154.50(6) ?
O4w Na2 O6 . . 87.50(5) ?
O7 Na2 O6 . . 63.23(5) ?
O1w Na2 O6 . . 168.97(5) ?
O2w Na2 O6 . . 116.01(5) ?
N3 Na2 O6 2_545 . 88.39(6) ?
O4w Na2 O9 . . 155.24(6) ?
O7 Na2 O9 . . 59.28(4) ?
O1w Na2 O9 . . 66.21(4) ?
O2w Na2 O9 . . 83.74(5) ?
N3 Na2 O9 2_545 . 78.17(5) ?
O6 Na2 O9 . . 116.93(5) ?
C3 O1 C2 . . 118.43(15) ?
C3 O1 Na1 . . 114.22(11) ?
C2 O1 Na1 . . 121.76(12) ?
C8 O2 V1 . . 133.34(12) ?
C8 O2 Na1 . . 118.35(11) ?
V1 O2 Na1 . . 108.27(6) ?
C10 O3 V1 . . 118.08(11) ?
V1 O4 Na1 . . 98.02(6) ?
C18 O6 C17 . . 115.98(16) ?
C18 O6 Na2 . . 110.26(11) ?
C17 O6 Na2 . . 128.99(13) ?
C23 O7 V2 . . 133.52(12) ?
C23 O7 Na2 . . 118.30(11) ?
V2 O7 Na2 . . 108.17(6) ?
C25 O8 V2 . . 118.22(11) ?
V2 O9 Na2 . . 98.21(6) ?
Na2 O1w Na1 . . 105.05(5) ?
Na2 O1w H11 . . 110.7 ?
Na1 O1w H11 . . 110.7 ?
Na2 O1w H12 . . 110.7 ?
Na1 O1w H12 . . 110.7 ?
H11 O1w H12 . . 108.8 ?
Na1 O2w Na2 . . 106.22(5) ?
Na1 O2w H21 . . 110.5 ?
Na2 O2w H21 . . 110.5 ?
Na1 O2w H22 . . 110.5 ?
Na2 O2w H22 . . 110.5 ?
H21 O2w H22 . . 108.7 ?
Na1 O3w H31 . . 109.5 ?
Na1 O3w H32 . . 109.5 ?
H31 O3w H32 . . 109.5 ?
Na2 O4w H41 . . 109.5 ?
Na2 O4w H42 . . 109.5 ?
H41 O4w H42 . . 109.5 ?
C9 N1 N2 . . 115.09(15) ?
C9 N1 V1 . . 129.24(12) ?
N2 N1 V1 . . 115.57(11) ?
C10 N2 N1 . . 107.54(14) ?
C14 N3 C13 . . 116.31(17) ?
C14 N3 Na2 . 2 125.95(13) ?
C13 N3 Na2 . 2 117.70(13) ?
C24 N4 N5 . . 114.99(15) ?
C24 N4 V2 . . 129.18(12) ?
N5 N4 V2 . . 115.71(11) ?
C25 N5 N4 . . 107.82(14) ?
C28 N6 C29 . . 116.46(17) ?
C28 N6 Na1 . 2_646 123.45(14) ?
C29 N6 Na1 . 2_646 119.90(13) ?
C2 C1 H1A . . 109.5 ?
C2 C1 H1B . . 109.5 ?
H1A C1 H1B . . 109.5 ?
C2 C1 H1C . . 109.5 ?
H1A C1 H1C . . 109.5 ?
H1B C1 H1C . . 109.5 ?
O1 C2 C1 . . 112.30(17) ?
O1 C2 H2A . . 109.1 ?
C1 C2 H2A . . 109.1 ?
O1 C2 H2B . . 109.1 ?
C1 C2 H2B . . 109.1 ?
H2A C2 H2B . . 107.9 ?
O1 C3 C4 . . 125.96(17) ?
O1 C3 C8 . . 113.76(16) ?
C4 C3 C8 . . 120.22(17) ?
C3 C4 C5 . . 120.31(17) ?
C3 C4 H4 . . 119.8 ?
C5 C4 H4 . . 119.8 ?
C6 C5 C4 . . 120.37(18) ?
C6 C5 H5 . . 119.8 ?
C4 C5 H5 . . 119.8 ?
C5 C6 C7 . . 120.06(18) ?
C5 C6 H6 . . 120.0 ?
C7 C6 H6 . . 120.0 ?
C8 C7 C6 . . 120.24(17) ?
C8 C7 C9 . . 121.00(17) ?
C6 C7 C9 . . 118.72(17) ?
O2 C8 C7 . . 122.78(16) ?
O2 C8 C3 . . 118.29(16) ?
C7 C8 C3 . . 118.76(17) ?
N1 C9 C7 . . 123.39(17) ?
N1 C9 H9 . . 118.3 ?
C7 C9 H9 . . 118.3 ?
O3 C10 N2 . . 123.49(16) ?
O3 C10 C11 . . 117.15(16) ?
N2 C10 C11 . . 119.31(16) ?
C12 C11 C15 . . 117.88(17) ?
C12 C11 C10 . . 119.20(16) ?
C15 C11 C10 . . 122.83(17) ?
C13 C12 C11 . . 118.59(18) ?
C13 C12 H12A . . 120.7 ?
C11 C12 H12A . . 120.7 ?
N3 C13 C12 . . 124.57(19) ?
N3 C13 H13 . . 117.7 ?
C12 C13 H13 . . 117.7 ?
N3 C14 C15 . . 123.72(17) ?
N3 C14 H14 . . 118.1 ?
C15 C14 H14 . . 118.1 ?
C11 C15 C14 . . 118.90(18) ?
C11 C15 H15 . . 120.5 ?
C14 C15 H15 . . 120.5 ?
C17 C16 H16A . . 109.5 ?
C17 C16 H16B . . 109.5 ?
H16A C16 H16B . . 109.5 ?
C17 C16 H16C . . 109.5 ?
H16A C16 H16C . . 109.5 ?
H16B C16 H16C . . 109.5 ?
O6 C17 C16 . . 107.99(18) ?
O6 C17 H17A . . 110.1 ?
C16 C17 H17A . . 110.1 ?
O6 C17 H17B . . 110.1 ?
C16 C17 H17B . . 110.1 ?
H17A C17 H17B . . 108.4 ?
O6 C18 C19 . . 125.03(18) ?
O6 C18 C23 . . 114.58(17) ?
C19 C18 C23 . . 120.37(18) ?
C18 C19 C20 . . 120.07(19) ?
C18 C19 H19 . . 120.0 ?
C20 C19 H19 . . 120.0 ?
C21 C20 C19 . . 120.69(19) ?
C21 C20 H20 . . 119.7 ?
C19 C20 H20 . . 119.7 ?
C20 C21 C22 . . 119.78(19) ?
C20 C21 H21A . . 120.1 ?
C22 C21 H21A . . 120.1 ?
C23 C22 C21 . . 120.60(17) ?
C23 C22 C24 . . 121.37(17) ?
C21 C22 C24 . . 118.02(17) ?
O7 C23 C22 . . 122.92(16) ?
O7 C23 C18 . . 118.56(16) ?
C22 C23 C18 . . 118.43(17) ?
N4 C24 C22 . . 123.52(17) ?
N4 C24 H24 . . 118.2 ?
C22 C24 H24 . . 118.2 ?
O8 C25 N5 . . 123.27(16) ?
O8 C25 C26 . . 117.36(16) ?
N5 C25 C26 . . 119.34(16) ?
C27 C26 C30 . . 118.03(17) ?
C27 C26 C25 . . 119.35(17) ?
C30 C26 C25 . . 122.60(17) ?
C26 C27 C28 . . 118.89(18) ?
C26 C27 H27 . . 120.6 ?
C28 C27 H27 . . 120.6 ?
N6 C28 C27 . . 124.10(19) ?
N6 C28 H28 . . 118.0 ?
C27 C28 H28 . . 118.0 ?
N6 C29 C30 . . 123.70(18) ?
N6 C29 H29 . . 118.2 ?
C30 C29 H29 . . 118.2 ?
C26 C30 C29 . . 118.79(18) ?
C26 C30 H30 . . 120.6 ?
C29 C30 H30 . . 120.6 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
V1 O5 . 1.6159(14) ?
V1 O4 . 1.6523(13) ?
V1 O2 . 1.9029(13) ?
V1 O3 . 1.9648(13) ?
V1 N1 . 2.1494(15) ?
V2 O10 . 1.6211(14) ?
V2 O9 . 1.6496(13) ?
V2 O7 . 1.9048(13) ?
V2 O8 . 1.9682(13) ?
V2 N4 . 2.1439(15) ?
Na1 O3w . 2.3268(16) ?
Na1 O2 . 2.3732(14) ?
Na1 O2w . 2.4764(15) ?
Na1 O1 . 2.5136(16) ?
Na1 O1w . 2.5157(15) ?
Na1 N6 2_656 2.5260(18) ?
Na1 O4 . 2.8368(15) ?
Na2 O4w . 2.3357(16) ?
Na2 O7 . 2.3743(15) ?
Na2 O1w . 2.4918(15) ?
Na2 O2w . 2.4925(15) ?
Na2 N3 2_545 2.5040(18) ?
Na2 O6 . 2.6104(16) ?
Na2 O9 . 2.8338(15) ?
O1 C3 . 1.368(2) ?
O1 C2 . 1.446(2) ?
O2 C8 . 1.328(2) ?
O3 C10 . 1.301(2) ?
O6 C18 . 1.368(2) ?
O6 C17 . 1.448(2) ?
O7 C23 . 1.325(2) ?
O8 C25 . 1.299(2) ?
O1w H11 . 0.8400 ?
O1w H12 . 0.8400 ?
O2w H21 . 0.8400 ?
O2w H22 . 0.8400 ?
O3w H31 . 0.8400 ?
O3w H32 . 0.8400 ?
O4w H41 . 0.8400 ?
O4w H42 . 0.8400 ?
N1 C9 . 1.294(2) ?
N1 N2 . 1.406(2) ?
N2 C10 . 1.304(2) ?
N3 C14 . 1.337(3) ?
N3 C13 . 1.336(3) ?
N3 Na2 2 2.5040(18) ?
N4 C24 . 1.295(2) ?
N4 N5 . 1.404(2) ?
N5 C25 . 1.306(2) ?
N6 C28 . 1.339(3) ?
N6 C29 . 1.343(3) ?
N6 Na1 2_646 2.5260(18) ?
C1 C2 . 1.506(3) ?
C1 H1A . 0.9800 ?
C1 H1B . 0.9800 ?
C1 H1C . 0.9800 ?
C2 H2A . 0.9900 ?
C2 H2B . 0.9900 ?
C3 C4 . 1.382(3) ?
C3 C8 . 1.418(2) ?
C4 C5 . 1.402(3) ?
C4 H4 . 0.9500 ?
C5 C6 . 1.375(3) ?
C5 H5 . 0.9500 ?
C6 C7 . 1.408(3) ?
C6 H6 . 0.9500 ?
C7 C8 . 1.404(2) ?
C7 C9 . 1.441(2) ?
C9 H9 . 0.9500 ?
C10 C11 . 1.486(2) ?
C11 C12 . 1.389(3) ?
C11 C15 . 1.393(2) ?
C12 C13 . 1.386(3) ?
C12 H12A . 0.9500 ?
C13 H13 . 0.9500 ?
C14 C15 . 1.394(3) ?
C14 H14 . 0.9500 ?
C15 H15 . 0.9500 ?
C16 C17 . 1.495(3) ?
C16 H16A . 0.9800 ?
C16 H16B . 0.9800 ?
C16 H16C . 0.9800 ?
C17 H17A . 0.9900 ?
C17 H17B . 0.9900 ?
C18 C19 . 1.388(3) ?
C18 C23 . 1.416(3) ?
C19 C20 . 1.402(3) ?
C19 H19 . 0.9500 ?
C20 C21 . 1.368(3) ?
C20 H20 . 0.9500 ?
C21 C22 . 1.412(3) ?
C21 H21A . 0.9500 ?
C22 C23 . 1.402(3) ?
C22 C24 . 1.440(3) ?
C24 H24 . 0.9500 ?
C25 C26 . 1.487(2) ?
C26 C27 . 1.389(3) ?
C26 C30 . 1.392(2) ?
C27 C28 . 1.386(3) ?
C27 H27 . 0.9500 ?
C28 H28 . 0.9500 ?
C29 C30 . 1.392(3) ?
C29 H29 . 0.9500 ?
C30 H30 . 0.9500 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O1w H12 N2 3_566 0.84 2.21 2.894(2) 139 yes
O2w H21 N5 3_666 0.84 2.16 2.879(2) 143 yes
O3w H32 O9 . 0.84 2.01 2.825(2) 162 yes
O3w H31 O10 4_566 0.84 2.23 2.799(2) 126 yes
O4w H41 O4 . 0.84 2.05 2.865(2) 162 yes
O4w H42 O5 4_575 0.84 2.13 2.822(2) 139 yes
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
O3w Na1 O1 C3 . . . . -116.11(13) ?
O2 Na1 O1 C3 . . . . 27.38(12) ?
O2w Na1 O1 C3 . . . . 148.0(2) ?
O1w Na1 O1 C3 . . . . -41.36(14) ?
N6 Na1 O1 C3 2_656 . . . 132.84(13) ?
O4 Na1 O1 C3 . . . . 53.39(13) ?
O3w Na1 O1 C2 . . . . 37.07(14) ?
O2 Na1 O1 C2 . . . . -179.45(15) ?
O2w Na1 O1 C2 . . . . -58.8(3) ?
O1w Na1 O1 C2 . . . . 111.82(14) ?
N6 Na1 O1 C2 2_656 . . . -73.98(14) ?
O4 Na1 O1 C2 . . . . -153.43(13) ?
O5 V1 O2 C8 . . . . 69.85(17) ?
O4 V1 O2 C8 . . . . -178.35(16) ?
O3 V1 O2 C8 . . . . -77.29(19) ?
N1 V1 O2 C8 . . . . -33.38(16) ?
O5 V1 O2 Na1 . . . . -107.86(7) ?
O4 V1 O2 Na1 . . . . 3.95(7) ?
O3 V1 O2 Na1 . . . . 105.01(10) ?
N1 V1 O2 Na1 . . . . 148.91(7) ?
O3w Na1 O2 C8 . . . . 27.16(16) ?
O2w Na1 O2 C8 . . . . 166.35(12) ?
O1 Na1 O2 C8 . . . . -27.53(12) ?
O1w Na1 O2 C8 . . . . 97.88(13) ?
N6 Na1 O2 C8 2_656 . . . -100.90(13) ?
O4 Na1 O2 C8 . . . . 179.23(14) ?
O3w Na1 O2 V1 . . . . -154.74(7) ?
O2w Na1 O2 V1 . . . . -15.55(9) ?
O1 Na1 O2 V1 . . . . 150.57(8) ?
O1w Na1 O2 V1 . . . . -84.02(6) ?
N6 Na1 O2 V1 2_656 . . . 77.20(7) ?
O4 Na1 O2 V1 . . . . -2.67(5) ?
O5 V1 O3 C10 . . . . -89.13(14) ?
O4 V1 O3 C10 . . . . 159.87(13) ?
O2 V1 O3 C10 . . . . 58.37(17) ?
N1 V1 O3 C10 . . . . 12.58(13) ?
O5 V1 O4 Na1 . . . . 105.19(7) ?
O2 V1 O4 Na1 . . . . -3.17(6) ?
O3 V1 O4 Na1 . . . . -149.36(5) ?
N1 V1 O4 Na1 . . . . -85.00(11) ?
O3w Na1 O4 V1 . . . . 130.65(12) ?
O2 Na1 O4 V1 . . . . 2.94(5) ?
O2w Na1 O4 V1 . . . . 170.81(7) ?
O1 Na1 O4 V1 . . . . -24.39(8) ?
O1w Na1 O4 V1 . . . . 93.78(6) ?
N6 Na1 O4 V1 2_656 . . . -99.88(7) ?
O4w Na2 O6 C18 . . . . 118.39(12) ?
O7 Na2 O6 C18 . . . . -31.34(11) ?
O1w Na2 O6 C18 . . . . -161.4(3) ?
O2w Na2 O6 C18 . . . . 38.97(13) ?
N3 Na2 O6 C18 2_545 . . . -133.30(12) ?
O9 Na2 O6 C18 . . . . -57.44(13) ?
O4w Na2 O6 C17 . . . . -35.70(17) ?
O7 Na2 O6 C17 . . . . 174.58(17) ?
O1w Na2 O6 C17 . . . . 44.5(4) ?
O2w Na2 O6 C17 . . . . -115.11(16) ?
N3 Na2 O6 C17 2_545 . . . 72.61(17) ?
O9 Na2 O6 C17 . . . . 148.47(16) ?
O10 V2 O7 C23 . . . . -73.90(17) ?
O9 V2 O7 C23 . . . . 173.94(16) ?
O8 V2 O7 C23 . . . . 71.8(2) ?
N4 V2 O7 C23 . . . . 30.84(16) ?
O10 V2 O7 Na2 . . . . 107.11(7) ?
O9 V2 O7 Na2 . . . . -5.05(7) ?
O8 V2 O7 Na2 . . . . -107.14(10) ?
N4 V2 O7 Na2 . . . . -148.15(7) ?
O4w Na2 O7 C23 . . . . -18.30(17) ?
O1w Na2 O7 C23 . . . . -158.72(12) ?
O2w Na2 O7 C23 . . . . -90.57(13) ?
N3 Na2 O7 C23 2_545 . . . 114.48(13) ?
O6 Na2 O7 C23 . . . . 31.39(12) ?
O9 Na2 O7 C23 . . . . -175.76(14) ?
O4w Na2 O7 V2 . . . . 160.87(7) ?
O1w Na2 O7 V2 . . . . 20.45(9) ?
O2w Na2 O7 V2 . . . . 88.60(6) ?
N3 Na2 O7 V2 2_545 . . . -66.35(7) ?
O6 Na2 O7 V2 . . . . -149.44(8) ?
O9 Na2 O7 V2 . . . . 3.41(5) ?
O10 V2 O8 C25 . . . . 92.32(14) ?
O9 V2 O8 C25 . . . . -156.19(14) ?
O7 V2 O8 C25 . . . . -53.77(18) ?
N4 V2 O8 C25 . . . . -11.03(13) ?
O10 V2 O9 Na2 . . . . -102.99(7) ?
O7 V2 O9 Na2 . . . . 4.06(6) ?
O8 V2 O9 Na2 . . . . 152.74(5) ?
N4 V2 O9 Na2 . . . . 86.83(10) ?
O4w Na2 O9 V2 . . . . -146.59(12) ?
O7 Na2 O9 V2 . . . . -3.78(5) ?
O1w Na2 O9 V2 . . . . -168.28(7) ?
O2w Na2 O9 V2 . . . . -92.62(6) ?
N3 Na2 O9 V2 2_545 . . . 105.45(7) ?
O6 Na2 O9 V2 . . . . 23.42(8) ?
O4w Na2 O1w Na1 . . . . -83.78(6) ?
O7 Na2 O1w Na1 . . . . 71.33(7) ?
O2w Na2 O1w Na1 . . . . -2.65(5) ?
N3 Na2 O1w Na1 2_545 . . . 167.91(6) ?
O6 Na2 O1w Na1 . . . . -163.7(3) ?
O9 Na2 O1w Na1 . . . . 87.32(5) ?
O3w Na1 O1w Na2 . . . . -96.64(6) ?
O2 Na1 O1w Na2 . . . . 127.70(6) ?
O2w Na1 O1w Na2 . . . . 2.67(5) ?
O1 Na1 O1w Na2 . . . . -175.03(5) ?
N6 Na1 O1w Na2 2_656 . . . 22.5(2) ?
O4 Na1 O1w Na2 . . . . 68.12(5) ?
O3w Na1 O2w Na2 . . . . 74.19(6) ?
O2 Na1 O2w Na2 . . . . -77.29(7) ?
O1 Na1 O2w Na2 . . . . 168.8(2) ?
O1w Na1 O2w Na2 . . . . -2.69(5) ?
N6 Na1 O2w Na2 2_656 . . . -176.27(6) ?
O4 Na1 O2w Na2 . . . . -89.62(5) ?
O4w Na2 O2w Na1 . . . . 95.68(6) ?
O7 Na2 O2w Na1 . . . . -123.81(6) ?
O1w Na2 O2w Na1 . . . . 2.71(5) ?
N3 Na2 O2w Na1 2_545 . . . -19.44(16) ?
O6 Na2 O2w Na1 . . . . 178.74(5) ?
O9 Na2 O2w Na1 . . . . -64.29(5) ?
O5 V1 N1 C9 . . . . -87.20(17) ?
O4 V1 N1 C9 . . . . 102.71(18) ?
O2 V1 N1 C9 . . . . 17.00(16) ?
O3 V1 N1 C9 . . . . 172.79(17) ?
O5 V1 N1 N2 . . . . 89.02(13) ?
O4 V1 N1 N2 . . . . -81.06(16) ?
O2 V1 N1 N2 . . . . -166.78(12) ?
O3 V1 N1 N2 . . . . -10.99(11) ?
C9 N1 N2 C10 . . . . -175.67(16) ?
V1 N1 N2 C10 . . . . 7.56(18) ?
O10 V2 N4 C24 . . . . 87.21(17) ?
O9 V2 N4 C24 . . . . -102.38(18) ?
O7 V2 N4 C24 . . . . -15.73(16) ?
O8 V2 N4 C24 . . . . -174.41(18) ?
O10 V2 N4 N5 . . . . -88.64(13) ?
O9 V2 N4 N5 . . . . 81.78(16) ?
O7 V2 N4 N5 . . . . 168.43(13) ?
O8 V2 N4 N5 . . . . 9.74(11) ?
C24 N4 N5 C25 . . . . 176.69(16) ?
V2 N4 N5 C25 . . . . -6.87(18) ?
C3 O1 C2 C1 . . . . -79.2(2) ?
Na1 O1 C2 C1 . . . . 128.68(16) ?
C2 O1 C3 C4 . . . . -2.3(3) ?
Na1 O1 C3 C4 . . . . 151.87(17) ?
C2 O1 C3 C8 . . . . -179.53(16) ?
Na1 O1 C3 C8 . . . . -25.40(19) ?
O1 C3 C4 C5 . . . . -175.34(19) ?
C8 C3 C4 C5 . . . . 1.8(3) ?
C3 C4 C5 C6 . . . . -1.2(3) ?
C4 C5 C6 C7 . . . . -0.3(3) ?
C5 C6 C7 C8 . . . . 1.3(3) ?
C5 C6 C7 C9 . . . . 179.06(19) ?
V1 O2 C8 C7 . . . . 33.3(3) ?
Na1 O2 C8 C7 . . . . -149.21(14) ?
V1 O2 C8 C3 . . . . -151.49(14) ?
Na1 O2 C8 C3 . . . . 26.0(2) ?
C6 C7 C8 O2 . . . . 174.43(17) ?
C9 C7 C8 O2 . . . . -3.2(3) ?
C6 C7 C8 C3 . . . . -0.8(3) ?
C9 C7 C8 C3 . . . . -178.48(17) ?
O1 C3 C8 O2 . . . . 1.3(2) ?
C4 C3 C8 O2 . . . . -176.18(17) ?
O1 C3 C8 C7 . . . . 176.70(16) ?
C4 C3 C8 C7 . . . . -0.7(3) ?
N2 N1 C9 C7 . . . . -177.61(16) ?
V1 N1 C9 C7 . . . . -1.4(3) ?
C8 C7 C9 N1 . . . . -10.3(3) ?
C6 C7 C9 N1 . . . . 172.02(18) ?
V1 O3 C10 N2 . . . . -13.9(2) ?
V1 O3 C10 C11 . . . . 163.67(12) ?
N1 N2 C10 O3 . . . . 3.3(2) ?
N1 N2 C10 C11 . . . . -174.22(15) ?
O3 C10 C11 C12 . . . . -7.8(3) ?
N2 C10 C11 C12 . . . . 169.91(18) ?
O3 C10 C11 C15 . . . . 175.95(17) ?
N2 C10 C11 C15 . . . . -6.4(3) ?
C15 C11 C12 C13 . . . . 2.1(3) ?
C10 C11 C12 C13 . . . . -174.36(18) ?
C14 N3 C13 C12 . . . . 0.4(3) ?
Na2 N3 C13 C12 2 . . . -177.51(17) ?
C11 C12 C13 N3 . . . . -1.9(3) ?
C13 N3 C14 C15 . . . . 0.9(3) ?
Na2 N3 C14 C15 2 . . . 178.59(14) ?
C12 C11 C15 C14 . . . . -1.0(3) ?
C10 C11 C15 C14 . . . . 175.36(17) ?
N3 C14 C15 C11 . . . . -0.6(3) ?
C18 O6 C17 C16 . . . . 169.99(18) ?
Na2 O6 C17 C16 . . . . -37.1(3) ?
C17 O6 C18 C19 . . . . 9.2(3) ?
Na2 O6 C18 C19 . . . . -148.61(17) ?
C17 O6 C18 C23 . . . . -172.29(17) ?
Na2 O6 C18 C23 . . . . 29.91(19) ?
O6 C18 C19 C20 . . . . 177.99(19) ?
C23 C18 C19 C20 . . . . -0.4(3) ?
C18 C19 C20 C21 . . . . 1.8(3) ?
C19 C20 C21 C22 . . . . -0.7(3) ?
C20 C21 C22 C23 . . . . -1.7(3) ?
C20 C21 C22 C24 . . . . 179.70(19) ?
V2 O7 C23 C22 . . . . -31.7(3) ?
Na2 O7 C23 C22 . . . . 147.24(15) ?
V2 O7 C23 C18 . . . . 151.86(14) ?
Na2 O7 C23 C18 . . . . -29.2(2) ?
C21 C22 C23 O7 . . . . -173.52(17) ?
C24 C22 C23 O7 . . . . 5.0(3) ?
C21 C22 C23 C18 . . . . 3.0(3) ?
C24 C22 C23 C18 . . . . -178.50(17) ?
O6 C18 C23 O7 . . . . -3.8(3) ?
C19 C18 C23 O7 . . . . 174.75(18) ?
O6 C18 C23 C22 . . . . 179.53(16) ?
C19 C18 C23 C22 . . . . -1.9(3) ?
N5 N4 C24 C22 . . . . 178.13(17) ?
V2 N4 C24 C22 . . . . 2.3(3) ?
C23 C22 C24 N4 . . . . 7.5(3) ?
C21 C22 C24 N4 . . . . -173.93(18) ?
V2 O8 C25 N5 . . . . 12.0(2) ?
V2 O8 C25 C26 . . . . -166.18(12) ?
N4 N5 C25 O8 . . . . -2.6(2) ?
N4 N5 C25 C26 . . . . 175.49(15) ?
O8 C25 C26 C27 . . . . 10.4(3) ?
N5 C25 C26 C27 . . . . -167.87(18) ?
O8 C25 C26 C30 . . . . -171.11(18) ?
N5 C25 C26 C30 . . . . 10.6(3) ?
C30 C26 C27 C28 . . . . 0.6(3) ?
C25 C26 C27 C28 . . . . 179.18(19) ?
C29 N6 C28 C27 . . . . -1.8(3) ?
Na1 N6 C28 C27 2_646 . . . 173.16(17) ?
C26 C27 C28 N6 . . . . 1.0(3) ?
C28 N6 C29 C30 . . . . 1.0(3) ?
Na1 N6 C29 C30 2_646 . . . -174.16(15) ?
C27 C26 C30 C29 . . . . -1.3(3) ?
C25 C26 C30 C29 . . . . -179.86(18) ?
N6 C29 C30 C26 . . . . 0.5(3) ?
