#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:50:47 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179396 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/93/4329315.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_4329315
loop_
_publ_author_name
'C. Gabriel'
'E. Kioseoglou'
'J. Venetis'
'V. Psycharis'
'C. P. Raptopoulou'
'A. Terzis'
'G. Voyiatzis'
'M. Bertmer'
'C. Mateescu'
'A. Salifoglou'
_publ_section_title
;
 pH-Specific Structural Speciation of the Ternary V(V)-Peroxido-Betaine
 System: A Chemical Reactivity-Structure Correlation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6056
_journal_page_last               6069
_journal_paper_doi               10.1021/ic2025878
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C10 H30 N2 Na2 O18 V2'
_chemical_formula_weight         614.22
_chemical_name_systematic
;
 ?
;
_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                111.9120(10)
_cell_angle_beta                 108.4990(10)
_cell_angle_gamma                94.3550(10)
_cell_formula_units_Z            2
_cell_length_a                   10.8295(2)
_cell_length_b                   10.8893(2)
_cell_length_c                   11.5148(2)
_cell_measurement_reflns_used    15486
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      71.74
_cell_measurement_theta_min      6.96
_cell_volume                     1165.19(4)
_computing_cell_refinement       'Crystal Clear, Rigaku MSC, 2005'
_computing_data_collection       'Crystal Clear, Rigaku MSC, 2005'
_computing_data_reduction        'Crystal Clear, Rigaku MSC, 2005'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.939
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       'θ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_sigmaI/netI    0.0355
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            15676
_diffrn_reflns_theta_full        64.98
_diffrn_reflns_theta_max         64.98
_diffrn_reflns_theta_min         6.97
_exptl_absorpt_coefficient_mu    7.899
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.475
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Crystal Clear, Rigaku MSC, 2005'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.751
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.386
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       0.0067(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     431
_refine_ls_number_reflns         3737
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0296
_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)+(0.0461P)²+0.6746P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0785
_refine_ls_wR_factor_ref         0.0791
_reflns_number_gt                3581
_reflns_number_total             3737
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2025878_si_006.cif
_cod_data_source_block           salv337
_cod_database_code               4329315
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
V1 V 0.34444(4) 0.63415(3) 0.73232(3) 0.00947(13) Uani 1 1 d .
V2 V 0.84178(4) 1.13842(3) 0.71197(3) 0.01050(13) Uani 1 1 d .
Na1 Na 0.5000 0.5000 0.5000 0.0163(3) Uani 1 2 d S
Na2 Na 0.5000 1.0000 0.5000 0.0172(3) Uani 1 2 d S
Na3 Na 0.71575(9) 0.76544(8) 0.50143(9) 0.0189(2) Uani 1 1 d .
O1 O 0.18929(15) 0.58379(14) 0.55563(13) 0.0163(3) Uani 1 1 d .
O2 O 0.26383(15) 0.41731(14) 0.43019(14) 0.0142(3) Uani 1 1 d .
N1 N 0.04651(18) 0.38541(17) 0.18885(16) 0.0112(4) Uani 1 1 d .
C1 C 0.1838(2) 0.4908(2) 0.4451(2) 0.0118(5) Uani 1 1 d .
C2 C 0.0602(2) 0.4801(2) 0.3287(2) 0.0138(5) Uani 1 1 d .
C3 C 0.0331(3) 0.2405(2) 0.1712(2) 0.0232(6) Uani 1 1 d .
C4 C -0.0795(2) 0.3973(2) 0.0932(2) 0.0172(5) Uani 1 1 d .
C5 C 0.1612(2) 0.4266(2) 0.1546(2) 0.0176(5) Uani 1 1 d .
O3 O 0.44510(17) 0.69004(15) 0.64800(15) 0.0226(4) Uani 1 1 d .
O4 O 0.52816(16) 0.69260(16) 0.77799(15) 0.0241(4) Uani 1 1 d .
O5 O 0.26155(17) 0.47491(15) 0.72564(15) 0.0216(4) Uani 1 1 d .
O6 O 0.39205(17) 0.53324(15) 0.83490(15) 0.0205(4) Uani 1 1 d .
O7 O 0.29633(16) 0.76009(14) 0.82015(14) 0.0194(4) Uani 1 1 d .
N11 N 0.69965(19) 0.90247(17) 0.15704(16) 0.0130(4) Uani 1 1 d .
O11 O 0.66427(15) 0.92880(14) 0.40496(14) 0.0139(3) Uani 1 1 d .
O12 O 0.85213(15) 1.09089(14) 0.52673(13) 0.0148(3) Uani 1 1 d .
C11 C 0.7629(2) 1.00305(19) 0.41603(19) 0.0109(4) Uani 1 1 d .
C12 C 0.7940(2) 1.0025(2) 0.2962(2) 0.0127(5) Uani 1 1 d .
C13 C 0.6966(3) 0.7577(2) 0.1385(2) 0.0196(5) Uani 1 1 d .
C14 C 0.5609(2) 0.9267(2) 0.1283(2) 0.0178(5) Uani 1 1 d .
C15 C 0.7526(3) 0.9255(2) 0.0590(2) 0.0198(5) Uani 1 1 d .
O13 O 0.68681(16) 1.19689(15) 0.64215(14) 0.0206(4) Uani 1 1 d .
O14 O 0.70627(17) 1.19537(16) 0.77428(15) 0.0218(4) Uani 1 1 d .
O15 O 0.89341(16) 0.97493(14) 0.69489(14) 0.0177(4) Uani 1 1 d .
O16 O 0.86285(17) 1.03801(15) 0.81734(15) 0.0213(4) Uani 1 1 d .
O17 O 0.97011(16) 1.26254(15) 0.79049(14) 0.0191(4) Uani 1 1 d .
O1W O 0.49368(18) 0.62561(17) 0.36326(17) 0.0174(4) Uani 1 1 d .
O2W O 0.59794(18) 0.88868(17) 0.63702(16) 0.0202(4) Uani 1 1 d .
O3W O 0.9046(2) 0.7673(2) 0.4485(2) 0.0333(5) Uani 1 1 d .
O4W O 0.3539(2) 0.56348(19) 1.07507(19) 0.0264(4) Uani 1 1 d .
H2A H 0.059(3) 0.557(3) 0.326(2) 0.019(7) Uiso 1 1 d .
H2B H -0.016(3) 0.452(2) 0.341(2) 0.019(7) Uiso 1 1 d .
H3A H 0.115(3) 0.231(3) 0.221(3) 0.023(7) Uiso 1 1 d .
H3B H -0.032(3) 0.222(3) 0.202(3) 0.038(9) Uiso 1 1 d .
H3C H 0.006(3) 0.186(3) 0.074(3) 0.022(7) Uiso 1 1 d .
H4A H -0.071(3) 0.492(3) 0.106(2) 0.021(6) Uiso 1 1 d .
H4B H -0.150(3) 0.364(3) 0.109(3) 0.037(8) Uiso 1 1 d .
H4C H -0.087(3) 0.339(3) 0.003(3) 0.026(7) Uiso 1 1 d .
H5A H 0.169(2) 0.524(2) 0.173(2) 0.014(6) Uiso 1 1 d .
H5B H 0.240(3) 0.409(3) 0.208(3) 0.030(8) Uiso 1 1 d .
H5C H 0.135(3) 0.373(2) 0.060(3) 0.022(7) Uiso 1 1 d .
H12A H 0.877(3) 0.980(2) 0.304(2) 0.012(6) Uiso 1 1 d .
H12B H 0.789(2) 1.089(2) 0.295(2) 0.014(6) Uiso 1 1 d .
H13A H 0.653(3) 0.744(3) 0.193(3) 0.021(7) Uiso 1 1 d .
H13B H 0.788(3) 0.747(2) 0.158(3) 0.021(7) Uiso 1 1 d .
H13C H 0.646(3) 0.702(2) 0.048(3) 0.016(6) Uiso 1 1 d .
H14A H 0.569(3) 1.018(3) 0.142(3) 0.029(7) Uiso 1 1 d .
H14B H 0.524(3) 0.904(3) 0.187(3) 0.024(7) Uiso 1 1 d .
H14C H 0.511(3) 0.874(2) 0.038(3) 0.017(6) Uiso 1 1 d .
H15A H 0.749(2) 1.016(3) 0.066(2) 0.017(6) Uiso 1 1 d .
H15B H 0.841(3) 0.913(2) 0.080(2) 0.019(7) Uiso 1 1 d .
H15C H 0.698(3) 0.862(3) -0.031(3) 0.022(7) Uiso 1 1 d .
H1W1 H 0.436(3) 0.675(3) 0.361(3) 0.027(8) Uiso 1 1 d .
H2W1 H 0.484(3) 0.594(3) 0.295(3) 0.036(10) Uiso 1 1 d .
H1W2 H 0.549(3) 0.834(3) 0.650(3) 0.033(8) Uiso 1 1 d .
H2W2 H 0.655(3) 0.939(3) 0.706(3) 0.032(8) Uiso 1 1 d .
H1W3 H 0.890(4) 0.695(4) 0.377(4) 0.053(10) Uiso 1 1 d .
H2W3 H 0.978(3) 0.804(3) 0.461(3) 0.037(9) Uiso 1 1 d .
H1W4 H 0.369(4) 0.559(4) 1.009(4) 0.058(11) Uiso 1 1 d .
H2W4 H 0.328(4) 0.636(4) 1.099(3) 0.052(11) 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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.1353 0.1239 '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
O7 V1 O5 109.48(8) . .
O7 V1 O3 110.36(8) . .
O5 V1 O3 139.29(7) . .
O7 V1 O4 106.83(8) . .
O5 V1 O4 126.38(8) . .
O3 V1 O4 46.10(7) . .
O7 V1 O6 106.09(8) . .
O5 V1 O6 45.91(7) . .
O3 V1 O6 126.62(8) . .
O4 V1 O6 86.89(7) . .
O7 V1 O1 95.81(7) . .
O5 V1 O1 83.84(6) . .
O3 V1 O1 84.23(7) . .
O4 V1 O1 129.79(7) . .
O6 V1 O1 129.25(7) . .
O7 V1 Na1 149.45(6) . .
O5 V1 Na1 100.08(5) . .
O3 V1 Na1 39.39(5) . .
O4 V1 Na1 58.31(5) . .
O6 V1 Na1 99.85(5) . .
O1 V1 Na1 79.53(5) . .
O17 V2 O15 110.51(8) . .
O17 V2 O14 108.03(8) . .
O15 V2 O14 124.55(7) . .
O17 V2 O13 110.62(8) . .
O15 V2 O13 138.07(7) . .
O14 V2 O13 46.14(7) . .
O17 V2 O16 105.57(8) . .
O15 V2 O16 46.26(7) . .
O14 V2 O16 85.96(7) . .
O13 V2 O16 126.44(8) . .
O17 V2 O12 94.73(7) . .
O15 V2 O12 84.41(6) . .
O14 V2 O12 130.02(7) . .
O13 V2 O12 84.49(6) . .
O16 V2 O12 130.45(7) . .
O17 V2 Na2 150.65(6) . .
O15 V2 Na2 97.57(5) . .
O14 V2 Na2 59.07(5) . .
O13 V2 Na2 40.58(5) . .
O16 V2 Na2 99.88(5) . .
O12 V2 Na2 79.27(4) . .
O3 Na1 O3 180.0 2_666 .
O3 Na1 O2 79.28(5) 2_666 2_666
O3 Na1 O2 100.72(5) . 2_666
O3 Na1 O2 100.72(5) 2_666 .
O3 Na1 O2 79.28(5) . .
O2 Na1 O2 180.0 2_666 .
O3 Na1 O1W 86.59(6) 2_666 2_666
O3 Na1 O1W 93.41(6) . 2_666
O2 Na1 O1W 99.28(5) 2_666 2_666
O2 Na1 O1W 80.72(5) . 2_666
O3 Na1 O1W 93.41(6) 2_666 .
O3 Na1 O1W 86.59(6) . .
O2 Na1 O1W 80.72(5) 2_666 .
O2 Na1 O1W 99.28(5) . .
O1W Na1 O1W 180.0 2_666 .
O3 Na1 O4 151.08(5) 2_666 .
O3 Na1 O4 28.92(5) . .
O2 Na1 O4 86.56(5) 2_666 .
O2 Na1 O4 93.44(5) . .
O1W Na1 O4 70.86(5) 2_666 .
O1W Na1 O4 109.14(5) . .
O3 Na1 O4 28.92(5) 2_666 2_666
O3 Na1 O4 151.08(5) . 2_666
O2 Na1 O4 93.44(5) 2_666 2_666
O2 Na1 O4 86.56(5) . 2_666
O1W Na1 O4 109.14(5) 2_666 2_666
O1W Na1 O4 70.86(5) . 2_666
O4 Na1 O4 180.0 . 2_666
O3 Na1 V1 150.23(4) 2_666 .
O3 Na1 V1 29.77(4) . .
O2 Na1 V1 118.77(3) 2_666 .
O2 Na1 V1 61.23(3) . .
O1W Na1 V1 68.04(5) 2_666 .
O1W Na1 V1 111.96(5) . .
O4 Na1 V1 32.20(3) . .
O4 Na1 V1 147.80(3) 2_666 .
O3 Na1 V1 29.77(4) 2_666 2_666
O3 Na1 V1 150.23(4) . 2_666
O2 Na1 V1 61.23(3) 2_666 2_666
O2 Na1 V1 118.77(3) . 2_666
O1W Na1 V1 111.96(5) 2_666 2_666
O1W Na1 V1 68.04(5) . 2_666
O4 Na1 V1 147.80(3) . 2_666
O4 Na1 V1 32.20(3) 2_666 2_666
V1 Na1 V1 180.0 . 2_666
O3 Na1 Na3 81.44(4) 2_666 2_666
O3 Na1 Na3 98.56(4) . 2_666
O2 Na1 Na3 138.01(4) 2_666 2_666
O2 Na1 Na3 41.99(4) . 2_666
O1W Na1 Na3 42.46(4) 2_666 2_666
O1W Na1 Na3 137.54(4) . 2_666
O4 Na1 Na3 92.93(3) . 2_666
O4 Na1 Na3 87.07(3) 2_666 2_666
V1 Na1 Na3 69.403(16) . 2_666
V1 Na1 Na3 110.597(16) 2_666 2_666
O3 Na1 Na3 98.56(4) 2_666 .
O3 Na1 Na3 81.44(4) . .
O2 Na1 Na3 41.99(4) 2_666 .
O2 Na1 Na3 138.01(4) . .
O1W Na1 Na3 137.54(4) 2_666 .
O1W Na1 Na3 42.46(4) . .
O4 Na1 Na3 87.07(3) . .
O4 Na1 Na3 92.93(3) 2_666 .
V1 Na1 Na3 110.597(16) . .
V1 Na1 Na3 69.403(16) 2_666 .
Na3 Na1 Na3 180.000(19) 2_666 .
O2W Na2 O2W 180.000(1) 2_676 .
O2W Na2 O11 97.70(5) 2_676 .
O2W Na2 O11 82.30(5) . .
O2W Na2 O11 82.30(5) 2_676 2_676
O2W Na2 O11 97.70(5) . 2_676
O11 Na2 O11 180.0 . 2_676
O2W Na2 O13 89.43(6) 2_676 2_676
O2W Na2 O13 90.57(6) . 2_676
O11 Na2 O13 100.80(5) . 2_676
O11 Na2 O13 79.20(5) 2_676 2_676
O2W Na2 O13 90.57(6) 2_676 .
O2W Na2 O13 89.43(6) . .
O11 Na2 O13 79.20(5) . .
O11 Na2 O13 100.80(5) 2_676 .
O13 Na2 O13 180.0 2_676 .
O2W Na2 V2 116.10(4) 2_676 .
O2W Na2 V2 63.90(4) . .
O11 Na2 V2 62.13(3) . .
O11 Na2 V2 117.87(3) 2_676 .
O13 Na2 V2 149.92(4) 2_676 .
O13 Na2 V2 30.08(4) . .
O2W Na2 V2 63.90(4) 2_676 2_676
O2W Na2 V2 116.10(4) . 2_676
O11 Na2 V2 117.87(3) . 2_676
O11 Na2 V2 62.13(3) 2_676 2_676
O13 Na2 V2 30.08(4) 2_676 2_676
O13 Na2 V2 149.92(4) . 2_676
V2 Na2 V2 180.0 . 2_676
O2W Na2 Na3 41.83(4) 2_676 2_676
O2W Na2 Na3 138.17(4) . 2_676
O11 Na2 Na3 137.52(4) . 2_676
O11 Na2 Na3 42.48(4) 2_676 2_676
O13 Na2 Na3 92.53(4) 2_676 2_676
O13 Na2 Na3 87.47(4) . 2_676
V2 Na2 Na3 116.946(15) . 2_676
V2 Na2 Na3 63.054(14) 2_676 2_676
O2W Na2 Na3 138.17(4) 2_676 .
O2W Na2 Na3 41.83(4) . .
O11 Na2 Na3 42.48(4) . .
O11 Na2 Na3 137.52(4) 2_676 .
O13 Na2 Na3 87.47(4) 2_676 .
O13 Na2 Na3 92.53(4) . .
V2 Na2 Na3 63.054(14) . .
V2 Na2 Na3 116.946(15) 2_676 .
Na3 Na2 Na3 180.0 2_676 .
O3W Na3 O2 97.09(7) . 2_666
O3W Na3 O2W 147.47(7) . .
O2 Na3 O2W 99.59(6) 2_666 .
O3W Na3 O1W 128.86(8) . .
O2 Na3 O1W 81.21(6) 2_666 .
O2W Na3 O1W 81.43(7) . .
O3W Na3 O11 86.72(7) . .
O2 Na3 O11 171.45(6) 2_666 .
O2W Na3 O11 80.81(6) . .
O1W Na3 O11 90.43(6) . .
O3W Na3 O15 73.54(6) . .
O2 Na3 O15 106.48(6) 2_666 .
O2W Na3 O15 75.02(6) . .
O1W Na3 O15 156.09(7) . .
O11 Na3 O15 81.92(5) . .
O3W Na3 Na1 131.55(6) . .
O2 Na3 Na1 42.21(4) 2_666 .
O2W Na3 Na1 77.41(5) . .
O1W Na3 Na1 42.76(4) . .
O11 Na3 Na1 130.44(5) . .
O15 Na3 Na1 132.39(4) . .
O3W Na3 Na2 126.76(6) . .
O2 Na3 Na2 135.90(5) 2_666 .
O2W Na3 Na2 41.03(4) . .
O1W Na3 Na2 74.86(5) . .
O11 Na3 Na2 41.74(4) . .
O15 Na3 Na2 84.57(4) . .
Na1 Na3 Na2 99.02(2) . .
C1 O1 V1 121.84(14) . .
C1 O2 Na3 125.02(13) . 2_666
C1 O2 Na1 124.24(13) . .
Na3 O2 Na1 95.81(6) 2_666 .
C5 N1 C3 110.47(19) . .
C5 N1 C2 111.39(17) . .
C3 N1 C2 111.71(17) . .
C5 N1 C4 108.05(17) . .
C3 N1 C4 108.57(17) . .
C2 N1 C4 106.45(17) . .
O2 C1 O1 126.79(19) . .
O2 C1 C2 122.93(18) . .
O1 C1 C2 110.28(19) . .
N1 C2 C1 116.98(19) . .
N1 C2 H2A 104.6(17) . .
C1 C2 H2A 110.0(17) . .
N1 C2 H2B 106.7(15) . .
C1 C2 H2B 109.7(15) . .
H2A C2 H2B 108(2) . .
N1 C3 H3A 108.0(16) . .
N1 C3 H3B 108.1(19) . .
H3A C3 H3B 111(3) . .
N1 C3 H3C 105.7(15) . .
H3A C3 H3C 113(2) . .
H3B C3 H3C 111(2) . .
N1 C4 H4A 108.5(15) . .
N1 C4 H4B 107.7(18) . .
H4A C4 H4B 114(2) . .
N1 C4 H4C 106.3(16) . .
H4A C4 H4C 111(2) . .
H4B C4 H4C 109(2) . .
N1 C5 H5A 107.4(14) . .
N1 C5 H5B 108.3(17) . .
H5A C5 H5B 113(2) . .
N1 C5 H5C 104.8(15) . .
H5A C5 H5C 110(2) . .
H5B C5 H5C 114(2) . .
O4 O3 V1 67.15(9) . .
O4 O3 Na1 99.09(11) . .
V1 O3 Na1 110.84(7) . .
O3 O4 V1 66.74(9) . .
O3 O4 Na1 52.00(8) . .
V1 O4 Na1 89.49(5) . .
O6 O5 V1 68.00(8) . .
O5 O6 V1 66.10(8) . .
C14 N11 C15 109.15(18) . .
C14 N11 C13 109.52(18) . .
C15 N11 C13 108.55(18) . .
C14 N11 C12 111.39(17) . .
C15 N11 C12 106.14(17) . .
C13 N11 C12 111.97(17) . .
C11 O11 Na2 126.34(13) . .
C11 O11 Na3 114.41(13) . .
Na2 O11 Na3 95.78(5) . .
C11 O12 V2 123.93(14) . .
O11 C11 O12 126.11(19) . .
O11 C11 C12 123.40(18) . .
O12 C11 C12 110.49(18) . .
N11 C12 C11 117.47(18) . .
N11 C12 H12A 105.1(14) . .
C11 C12 H12A 107.9(14) . .
N11 C12 H12B 104.2(14) . .
C11 C12 H12B 107.6(15) . .
H12A C12 H12B 115(2) . .
N11 C13 H13A 105.9(16) . .
N11 C13 H13B 106.4(15) . .
H13A C13 H13B 118(2) . .
N11 C13 H13C 107.7(15) . .
H13A C13 H13C 109(2) . .
H13B C13 H13C 109(2) . .
N11 C14 H14A 105.7(17) . .
N11 C14 H14B 109.1(16) . .
H14A C14 H14B 114(2) . .
N11 C14 H14C 107.6(16) . .
H14A C14 H14C 108(2) . .
H14B C14 H14C 112(2) . .
N11 C15 H15A 109.0(15) . .
N11 C15 H15B 108.5(15) . .
H15A C15 H15B 112(2) . .
N11 C15 H15C 109.2(16) . .
H15A C15 H15C 108(2) . .
H15B C15 H15C 110(2) . .
O14 O13 V2 66.65(9) . .
O14 O13 Na2 98.86(10) . .
V2 O13 Na2 109.34(7) . .
O13 O14 V2 67.21(9) . .
O16 O15 V2 67.75(8) . .
O16 O15 Na3 115.29(11) . .
V2 O15 Na3 113.04(7) . .
O15 O16 V2 65.99(8) . .
Na3 O1W Na1 94.78(6) . .
Na3 O1W H1W1 110.6(19) . .
Na1 O1W H1W1 115(2) . .
Na3 O1W H2W1 113(3) . .
Na1 O1W H2W1 123(3) . .
H1W1 O1W H2W1 101(3) . .
Na2 O2W Na3 97.14(6) . .
Na2 O2W H1W2 121(2) . .
Na3 O2W H1W2 110(2) . .
Na2 O2W H2W2 112(2) . .
Na3 O2W H2W2 104(2) . .
H1W2 O2W H2W2 111(3) . .
Na3 O3W H1W3 108(2) . .
Na3 O3W H2W3 151(2) . .
H1W3 O3W H2W3 101(3) . .
H1W4 O4W H2W4 103(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
V1 O7 1.6071(16) .
V1 O5 1.8545(15) .
V1 O3 1.8742(16) .
V1 O4 1.8799(17) .
V1 O6 1.8807(15) .
V1 O1 2.0301(14) .
V1 Na1 3.5277(4) .
V2 O17 1.6065(15) .
V2 O15 1.8655(15) .
V2 O14 1.8781(17) .
V2 O13 1.8858(16) .
V2 O16 1.8901(15) .
V2 O12 2.0412(14) .
V2 Na2 3.5501(3) .
Na1 O3 2.3954(17) 2_666
Na1 O3 2.3954(17) .
Na1 O2 2.4091(15) 2_666
Na1 O2 2.4091(15) .
Na1 O1W 2.4307(16) 2_666
Na1 O1W 2.4307(16) .
Na1 O4 3.0018(16) .
Na1 O4 3.0018(16) 2_666
Na1 V1 3.5277(4) 2_666
Na1 Na3 3.5677(8) 2_666
Na1 Na3 3.5677(8) .
Na2 O2W 2.3758(16) 2_676
Na2 O2W 2.3758(16) .
Na2 O11 2.4031(16) .
Na2 O11 2.4031(16) 2_676
Na2 O13 2.4473(16) 2_676
Na2 O13 2.4473(16) .
Na2 V2 3.5501(4) 2_676
Na2 Na3 3.5911(9) 2_676
Na2 Na3 3.5911(9) .
Na3 O3W 2.313(2) .
Na3 O2 2.3990(16) 2_666
Na3 O2W 2.414(2) .
Na3 O1W 2.4168(19) .
Na3 O11 2.4375(16) .
Na3 O15 2.5863(16) .
O1 C1 1.276(3) .
O2 C1 1.233(3) .
O2 Na3 2.3990(16) 2_666
N1 C5 1.503(3) .
N1 C3 1.503(3) .
N1 C2 1.504(3) .
N1 C4 1.508(3) .
C1 C2 1.524(3) .
C2 H2A 0.85(3) .
C2 H2B 0.93(3) .
C3 H3A 0.92(3) .
C3 H3B 0.92(3) .
C3 H3C 0.98(3) .
C4 H4A 0.98(3) .
C4 H4B 0.92(3) .
C4 H4C 0.97(3) .
C5 H5A 0.99(2) .
C5 H5B 0.96(3) .
C5 H5C 0.96(3) .
O3 O4 1.470(2) .
O5 O6 1.457(2) .
N11 C14 1.499(3) .
N11 C15 1.506(3) .
N11 C13 1.507(3) .
N11 C12 1.512(2) .
O11 C11 1.232(3) .
O12 C11 1.281(2) .
C11 C12 1.519(3) .
C12 H12A 0.94(3) .
C12 H12B 0.95(2) .
C13 H13A 0.94(3) .
C13 H13B 0.97(3) .
C13 H13C 0.93(3) .
C14 H14A 0.94(3) .
C14 H14B 0.98(3) .
C14 H14C 0.93(3) .
C15 H15A 0.96(3) .
C15 H15B 0.94(3) .
C15 H15C 0.95(3) .
O13 O14 1.475(2) .
O15 O16 1.475(2) .
O1W H1W1 0.85(3) .
O1W H2W1 0.70(3) .
O2W H1W2 0.85(3) .
O2W H2W2 0.79(3) .
O3W H1W3 0.86(4) .
O3W H2W3 0.80(3) .
O4W H1W4 0.82(4) .
O4W H2W4 0.83(4) .
