# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_cjl_2a_a
_database_code_depnum_ccdc_archive 'CCDC 1413557'
_audit_update_record             
;
2015-07-17 deposited with the CCDC.
2016-01-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H16 N6 Na O6 V'
_chemical_formula_weight         390.22

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020
'XDISP Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
H H 0.0000 0.0000
'XDISP Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
N N 0.0076 0.0040
'XDISP Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
O O 0.0132 0.0074
'XDISP Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
Na Na 0.0437 0.0302
'XDISP Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
V V 0.3275 0.6267
'XDISP Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.9375(3)
_cell_length_b                   8.7365(4)
_cell_length_c                   12.1972(5)
_cell_angle_alpha                102.684(2)
_cell_angle_beta                 107.187(2)
_cell_angle_gamma                103.796(2)
_cell_volume                     745.41(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9903
_cell_measurement_theta_min      2.76
_cell_measurement_theta_max      40.25

_exptl_crystal_description       tablet
_exptl_crystal_colour            brown/orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.739
_exptl_crystal_F_000             400
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.931
_shelx_estimated_absorpt_T_min   0.904
_shelx_estimated_absorpt_T_max   0.973
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.899
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_process_details   'SADABS 2014/4 Bruker AXS Madison WI USA'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.7749
_diffrn_radiation_type           synchrotron
_diffrn_source                   'Advanced Light Source station 11.3.1'
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       'ω/θ shutterless scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13779
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_av_R_equivalents  0.0192
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.756
_diffrn_reflns_theta_max         40.263
_diffrn_reflns_theta_full        27.706
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             7062
_reflns_number_gt                6412
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX 2'
_computing_cell_refinement       'Bruker SAINT v8.34a'
_computing_data_reduction        'Bruker SAINT v8.34a'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL & local programs'
_refine_special_details          
;
 All non-hydrogen atoms were refinement anisotropically. Hydrogen
 atoms were found in the difference map and refined freely.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0345P)²+0.2437P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     'Intrinsic Phasing'
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7062
_refine_ls_number_parameters     281
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0263
_refine_ls_wR_factor_ref         0.0729
_refine_ls_wR_factor_gt          0.0707
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.47199(2) 0.26312(2) 0.74686(2) 0.00827(3) Uani 1 1 d . . . . .
N1 N 0.43194(9) 0.18753(8) 0.57510(6) 0.00954(10) Uani 1 1 d . . . . .
C1 C 0.54177(11) 0.28489(10) 0.53255(7) 0.01122(12) Uani 1 1 d . . . . .
N2 N 0.67905(10) 0.40894(9) 0.61662(7) 0.01382(12) Uani 1 1 d . . . . .
O1 O 0.67291(9) 0.40465(8) 0.72979(6) 0.01356(10) Uani 1 1 d . . . . .
C2 C 0.50032(12) 0.24684(12) 0.39937(8) 0.01474(14) Uani 1 1 d . . . . .
H2A H 0.569(2) 0.173(2) 0.3720(14) 0.024(4) Uiso 1 1 d . . . . .
H2B H 0.541(2) 0.3479(19) 0.3851(13) 0.017(3) Uiso 1 1 d . . . . .
C3 C 0.29040(13) 0.15594(12) 0.32936(8) 0.01539(14) Uani 1 1 d . . . . .
H3A H 0.267(2) 0.124(2) 0.2461(15) 0.024(4) Uiso 1 1 d . . . . .
H3B H 0.220(2) 0.2312(19) 0.3409(14) 0.019(3) Uiso 1 1 d . . . . .
C4 C 0.21984(12) 0.00396(11) 0.36712(7) 0.01364(13) Uani 1 1 d . . . . .
H4A H 0.271(2) -0.0857(18) 0.3379(13) 0.016(3) Uiso 1 1 d . . . . .
H4B H 0.083(2) -0.0457(18) 0.3306(13) 0.018(3) Uiso 1 1 d . . . . .
C5 C 0.27860(10) 0.05277(9) 0.50174(7) 0.00949(11) Uani 1 1 d . . . . .
N3 N 0.19181(10) -0.02442(8) 0.55854(6) 0.01121(11) Uani 1 1 d . . . . .
O2 O 0.28046(9) 0.05322(7) 0.68346(5) 0.01188(10) Uani 1 1 d . . . . .
N4 N 0.39407(9) 0.30587(8) 0.88527(6) 0.00966(10) Uani 1 1 d . . . . .
C6 C 0.24438(11) 0.36247(9) 0.87264(7) 0.00993(11) Uani 1 1 d . . . . .
N5 N 0.19525(10) 0.41300(9) 0.77952(6) 0.01141(11) Uani 1 1 d . . . . .
O3 O 0.31641(8) 0.39611(8) 0.71586(5) 0.01153(10) Uani 1 1 d . . . . .
C7 C 0.14701(12) 0.36020(11) 0.96071(7) 0.01324(13) Uani 1 1 d . . . . .
H7A H 0.021(2) 0.3477(19) 0.9201(14) 0.021(4) Uiso 1 1 d . . . . .
H7B H 0.205(2) 0.4685(19) 1.0219(14) 0.019(3) Uiso 1 1 d . . . . .
C8 C 0.16789(13) 0.21954(11) 1.01485(8) 0.01549(14) Uani 1 1 d . . . . .
H8A H 0.099(2) 0.1133(19) 0.9526(14) 0.021(4) Uiso 1 1 d . . . . .
H8B H 0.114(2) 0.2242(18) 1.0765(14) 0.018(3) Uiso 1 1 d . . . . .
C9 C 0.37409(12) 0.23133(11) 1.06749(7) 0.01382(13) Uani 1 1 d . . . . .
H9A H 0.442(2) 0.334(2) 1.1366(15) 0.024(4) Uiso 1 1 d . . . . .
H9B H 0.388(2) 0.1375(19) 1.0939(14) 0.018(3) Uiso 1 1 d . . . . .
C10 C 0.45845(11) 0.23823(9) 0.97306(7) 0.01039(12) Uani 1 1 d . . . . .
N6 N 0.59187(10) 0.17833(9) 0.96494(6) 0.01243(11) Uani 1 1 d . . . . .
O4 O 0.63026(8) 0.20086(8) 0.86366(5) 0.01193(10) Uani 1 1 d . . . . .
Na1 Na 1.00402(5) 0.54628(4) 0.65658(3) 0.01121(6) Uani 1 1 d . . . . .
O1W O 0.95338(9) 0.65955(8) 0.50046(6) 0.01267(10) Uani 1 1 d . . . . .
H1WA H 0.861(2) 0.648(2) 0.4521(15) 0.024(4) Uiso 1 1 d . . . . .
H1WB H 1.019(2) 0.752(2) 0.5169(15) 0.028(4) Uiso 1 1 d . . . . .
O2W O 1.16068(10) 0.80897(9) 0.79562(6) 0.01825(13) Uani 1 1 d . . . . .
H2WA H 1.228(3) 0.825(2) 0.8584(18) 0.040(5) Uiso 1 1 d . . . . .
H2WB H 1.207(3) 0.885(2) 0.7761(17) 0.035(5) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
V1 O1 1.8667(6) . ?
V1 O4 1.8740(6) . ?
V1 O3 1.9024(6) . ?
V1 O2 1.9039(6) . ?
V1 N4 1.9550(7) . ?
V1 N1 1.9558(7) . ?
N1 C1 1.3639(10) . ?
N1 C5 1.3706(10) . ?
C1 N2 1.3045(11) . ?
C1 C2 1.5008(11) . ?
N2 O1 1.4039(10) . ?
N2 Na1 2.4197(8) . ?
C2 C3 1.5383(13) . ?
C2 H2A 1.003(16) . ?
C2 H2B 0.938(15) . ?
C3 C4 1.5346(12) . ?
C3 H3A 0.940(16) . ?
C3 H3B 0.975(15) . ?
C4 C5 1.4969(11) . ?
C4 H4A 1.008(15) . ?
C4 H4B 0.983(15) . ?
C5 N3 1.2941(10) . ?
N3 O2 1.4005(9) . ?
N4 C10 1.3622(10) . ?
N4 C6 1.3731(10) . ?
C6 N5 1.2952(10) . ?
C6 C7 1.4981(11) . ?
N5 O3 1.4171(9) . ?
N5 Na1 2.4846(8) 1_455 ?
C7 C8 1.5370(12) . ?
C7 H7A 0.945(16) . ?
C7 H7B 0.971(16) . ?
C8 C9 1.5399(13) . ?
C8 H8A 0.969(16) . ?
C8 H8B 0.968(15) . ?
C9 C10 1.4985(11) . ?
C9 H9A 0.990(17) . ?
C9 H9B 0.962(15) . ?
C10 N6 1.3072(11) . ?
N6 O4 1.3993(9) . ?
Na1 O1W 2.3091(7) . ?
Na1 O2W 2.3179(8) . ?
Na1 N5 2.4846(8) 1_655 ?
Na1 O1W 2.4853(8) 2_766 ?
Na1 Na1 3.7044(7) 2_766 ?
O1W Na1 2.4854(8) 2_766 ?
O1W H1WA 0.762(17) . ?
O1W H1WB 0.790(18) . ?
O2W H2WA 0.75(2) . ?
O2W H2WB 0.795(19) . ?

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
O1 V1 O4 92.21(3) . . ?
O1 V1 O3 94.42(3) . . ?
O4 V1 O3 146.67(3) . . ?
O1 V1 O2 147.22(3) . . ?
O4 V1 O2 94.08(3) . . ?
O3 V1 O2 97.72(3) . . ?
O1 V1 N4 125.33(3) . . ?
O4 V1 N4 74.95(3) . . ?
O3 V1 N4 74.60(3) . . ?
O2 V1 N4 87.31(3) . . ?
O1 V1 N1 74.69(3) . . ?
O4 V1 N1 123.07(3) . . ?
O3 V1 N1 90.14(3) . . ?
O2 V1 N1 74.95(3) . . ?
N4 V1 N1 154.94(3) . . ?
C1 N1 C5 123.43(7) . . ?
C1 N1 V1 118.12(5) . . ?
C5 N1 V1 117.77(5) . . ?
N2 C1 N1 114.16(7) . . ?
N2 C1 C2 125.21(7) . . ?
N1 C1 C2 120.62(7) . . ?
C1 N2 O1 108.94(6) . . ?
C1 N2 Na1 136.98(6) . . ?
O1 N2 Na1 104.76(5) . . ?
N2 O1 V1 122.63(5) . . ?
C1 C2 C3 109.66(7) . . ?
C1 C2 H2A 111.3(9) . . ?
C3 C2 H2A 107.8(9) . . ?
C1 C2 H2B 107.3(9) . . ?
C3 C2 H2B 112.2(9) . . ?
H2A C2 H2B 108.6(13) . . ?
C4 C3 C2 111.82(7) . . ?
C4 C3 H3A 110.3(10) . . ?
C2 C3 H3A 109.1(10) . . ?
C4 C3 H3B 109.9(9) . . ?
C2 C3 H3B 110.4(9) . . ?
H3A C3 H3B 105.0(13) . . ?
C5 C4 C3 109.78(7) . . ?
C5 C4 H4A 110.0(8) . . ?
C3 C4 H4A 110.2(8) . . ?
C5 C4 H4B 109.0(9) . . ?
C3 C4 H4B 112.0(9) . . ?
H4A C4 H4B 105.8(12) . . ?
N3 C5 N1 114.56(7) . . ?
N3 C5 C4 124.27(7) . . ?
N1 C5 C4 121.17(7) . . ?
C5 N3 O2 110.22(6) . . ?
N3 O2 V1 120.77(5) . . ?
C10 N4 C6 123.38(7) . . ?
C10 N4 V1 117.03(5) . . ?
C6 N4 V1 117.32(5) . . ?
N5 C6 N4 114.92(7) . . ?
N5 C6 C7 124.27(7) . . ?
N4 C6 C7 120.80(7) . . ?
C6 N5 O3 109.03(6) . . ?
C6 N5 Na1 151.60(6) . 1_455 ?
O3 N5 Na1 99.15(4) . 1_455 ?
N5 O3 V1 120.43(4) . . ?
C6 C7 C8 109.56(7) . . ?
C6 C7 H7A 108.5(9) . . ?
C8 C7 H7A 112.1(10) . . ?
C6 C7 H7B 106.3(9) . . ?
C8 C7 H7B 112.0(9) . . ?
H7A C7 H7B 108.2(13) . . ?
C7 C8 C9 111.09(7) . . ?
C7 C8 H8A 109.6(9) . . ?
C9 C8 H8A 108.7(9) . . ?
C7 C8 H8B 109.3(9) . . ?
C9 C8 H8B 110.7(9) . . ?
H8A C8 H8B 107.4(13) . . ?
C10 C9 C8 109.50(7) . . ?
C10 C9 H9A 108.7(9) . . ?
C8 C9 H9A 109.0(10) . . ?
C10 C9 H9B 108.3(9) . . ?
C8 C9 H9B 111.9(9) . . ?
H9A C9 H9B 109.4(13) . . ?
N6 C10 N4 114.81(7) . . ?
N6 C10 C9 124.48(7) . . ?
N4 C10 C9 120.68(7) . . ?
C10 N6 O4 108.76(6) . . ?
N6 O4 V1 121.81(5) . . ?
O1W Na1 O2W 90.42(3) . . ?
O1W Na1 N2 96.51(3) . . ?
O2W Na1 N2 120.61(3) . . ?
O1W Na1 N5 148.05(3) . 1_655 ?
O2W Na1 N5 93.59(3) . 1_655 ?
N2 Na1 N5 108.41(3) . 1_655 ?
O1W Na1 O1W 78.88(3) . 2_766 ?
O2W Na1 O1W 140.38(3) . 2_766 ?
N2 Na1 O1W 98.59(3) . 2_766 ?
N5 Na1 O1W 77.93(2) 1_655 2_766 ?
O1W Na1 Na1 41.172(18) . 2_766 ?
O2W Na1 Na1 121.43(2) . 2_766 ?
N2 Na1 Na1 99.84(2) . 2_766 ?
N5 Na1 Na1 112.87(2) 1_655 2_766 ?
O1W Na1 Na1 37.705(15) 2_766 2_766 ?
Na1 O1W Na1 101.12(3) . 2_766 ?
Na1 O1W H1WA 127.9(12) . . ?
Na1 O1W H1WA 86.1(13) 2_766 . ?
Na1 O1W H1WB 114.9(12) . . ?
Na1 O1W H1WB 114.1(13) 2_766 . ?
H1WA O1W H1WB 108.2(17) . . ?
Na1 O2W H2WA 123.6(15) . . ?
Na1 O2W H2WB 121.0(14) . . ?
H2WA O2W H2WB 103.5(19) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C2 H2A N3 1.003(16) 2.591(16) 3.4601(11) 144.9(12) 2_656
C2 H2A O2 1.003(16) 2.609(16) 3.6016(11) 170.1(13) 2_656
C4 H4A N1 1.008(15) 2.726(15) 3.5366(11) 137.7(11) 2_656
C9 H9A O3 0.990(17) 2.530(16) 3.4907(11) 163.5(13) 2_667
O1W H1WA N5 0.762(17) 2.636(17) 3.1253(9) 123.9(15) 2_666
O1W H1WA O3 0.762(17) 2.004(17) 2.7175(9) 155.9(17) 2_666
O1W H1WB N3 0.790(18) 1.960(18) 2.7502(9) 177.2(18) 1_665
O2W H2WA N6 0.75(2) 2.22(2) 2.9603(10) 169(2) 2_767
O2W H2WB O2 0.795(19) 2.121(19) 2.9003(9) 166.5(18) 1_665

_refine_diff_density_max         0.628
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.068



_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_NaO2(cyclicAO)
_database_code_depnum_ccdc_archive 'CCDC 1418830'
_audit_update_record             
;
2015-08-14 deposited with the CCDC.
2016-01-14 downloaded from the CCDC.
;
_audit_creation_date             2015-05-20
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            NaO2(cyclciAO)
_chemical_name_systematic        NaO2(cyclciAO)
_chemical_formula_moiety         'C5 H7 N3 Na O4 V'
_chemical_formula_sum            'C5 H7 N3 Na O4 V'
_chemical_formula_weight         247.07
_chemical_melting_point          ?
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   15.0543(8)
_cell_length_b                   5.5070(3)
_cell_length_c                   10.1794(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.569(3)
_cell_angle_gamma                90.00
_cell_volume                     826.77(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2539
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.10
_cell_measurement_theta_min      3.95
_exptl_absorpt_coefficient_mu    1.242
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6460
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0575 before and 0.0406 after correction.
The Ratio of minimum to maximum transmission is 0.8657.
The λ/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear yellowish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.985
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.47
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8438
_diffrn_reflns_theta_full        31.22
_diffrn_reflns_theta_max         31.22
_diffrn_reflns_theta_min         1.38
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         0
_reflns_number_gt                2162
_reflns_number_total             2662
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max         0.634
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.197
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     131
_refine_ls_number_reflns         2662
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0330
_refine_ls_restrained_S_all      0.963
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0794P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0955
_refine_ls_wR_factor_ref         0.1112
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
V1 V 0.14902(2) 0.66830(6) 0.66087(3) 0.00603(11) Uani 1 d . . .
Na2 Na 0.00188(5) 0.76428(15) 0.38275(8) 0.00870(17) Uani 1 d . . .
N1 N 0.15890(12) 0.3238(3) 0.45102(16) 0.0081(3) Uani 1 d . . .
O2 O 0.25180(10) 0.8100(3) 0.77220(15) 0.0130(3) Uani 1 d . . .
O3 O 0.09607(9) 0.5217(3) 0.76765(13) 0.0085(3) Uani 1 d . . .
O5 O 0.09742(9) 0.4613(2) 0.50175(13) 0.0084(3) Uani 1 d . . .
N6 N 0.25551(11) 0.5282(3) 0.59964(16) 0.0079(3) Uani 1 d . . .
N7 N 0.34151(11) 0.7494(3) 0.76380(17) 0.0118(3) Uani 1 d . . .
C8 C 0.24338(13) 0.3620(3) 0.50215(18) 0.0082(3) Uani 1 d . . .
C9 C 0.34014(13) 0.5983(4) 0.66754(19) 0.0092(3) Uani 1 d . . .
C10 C 0.42176(14) 0.4982(4) 0.6242(2) 0.0138(4) Uani 1 d . . .
H10A H 0.4741 0.4998 0.7006 0.017 Uiso 1 calc . . R
H10B H 0.4370 0.6005 0.5519 0.017 Uiso 1 calc . . R
C11 C 0.40290(14) 0.2381(4) 0.5736(2) 0.0130(4) Uani 1 d . . .
H11A H 0.3925 0.1333 0.6481 0.016 Uiso 1 calc . . R
H11B H 0.4561 0.1745 0.5412 0.016 Uiso 1 calc . . R
C12 C 0.31935(14) 0.2319(4) 0.4594(2) 0.0114(4) Uani 1 d . . .
H12A H 0.3336 0.3105 0.3786 0.014 Uiso 1 calc . . R
H12B H 0.3017 0.0614 0.4368 0.014 Uiso 1 calc . . R
O14 O 0.09051(10) 0.9089(3) 0.60182(14) 0.0111(3) Uani 1 d . . .
H1 H 0.136(2) 0.229(6) 0.393(3) 0.028(8) Uiso 1 d . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
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
V1 Na2 3.2601(9) 3_566 ?
V1 Na2 3.2690(8) . ?
V1 Na2 3.4860(9) 4_576 ?
V1 O2 1.8931(14) . ?
V1 O3 1.6781(15) . ?
V1 O5 2.0054(13) . ?
V1 N6 1.9885(17) . ?
V1 O14 1.6374(14) . ?
Na2 V1 3.4861(9) 4_575 ?
Na2 V1 3.2601(9) 3_566 ?
Na2 Na2 3.8506(11) 2 ?
Na2 Na2 3.5350(16) 3_576 ?
Na2 Na2 3.7720(16) 3_566 ?
Na2 O3 2.4684(15) 3_566 ?
Na2 O3 2.3322(16) 4_575 ?
Na2 O5 2.3709(15) . ?
Na2 O5 2.4218(17) 3_566 ?
Na2 O14 2.4889(16) . ?
Na2 O14 2.2990(16) 3_576 ?
N1 O5 1.374(2) . ?
N1 C8 1.291(3) . ?
N1 H1 0.81(3) . ?
O2 N7 1.410(2) . ?
O3 Na2 2.3321(16) 4_576 ?
O3 Na2 2.4684(15) 3_566 ?
O5 Na2 2.4219(17) 3_566 ?
N6 C8 1.335(2) . ?
N6 C9 1.377(2) . ?
N7 C9 1.282(3) . ?
C8 C12 1.487(3) . ?
C9 C10 1.492(3) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.530(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.532(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
O14 Na2 2.2990(16) 3_576 ?

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
Na2 V1 Na2 69.518(17) 3_566 4_576 ?
Na2 V1 Na2 70.58(2) 3_566 . ?
Na2 V1 Na2 97.80(2) . 4_576 ?
O2 V1 Na2 147.80(5) . 3_566 ?
O2 V1 Na2 141.48(5) . . ?
O2 V1 Na2 96.75(5) . 4_576 ?
O2 V1 O5 148.81(6) . . ?
O2 V1 N6 74.57(6) . . ?
O3 V1 Na2 47.79(5) . 3_566 ?
O3 V1 Na2 108.14(5) . . ?
O3 V1 Na2 35.46(5) . 4_576 ?
O3 V1 O2 104.35(7) . . ?
O3 V1 O5 95.30(6) . . ?
O3 V1 N6 122.27(7) . . ?
O5 V1 Na2 47.79(4) . 3_566 ?
O5 V1 Na2 46.13(4) . . ?
O5 V1 Na2 112.97(4) . 4_576 ?
N6 V1 Na2 103.89(5) . . ?
N6 V1 Na2 104.92(5) . 3_566 ?
N6 V1 Na2 154.34(5) . 4_576 ?
N6 V1 O5 74.48(6) . . ?
O14 V1 Na2 47.93(5) . . ?
O14 V1 Na2 103.44(6) . 3_566 ?
O14 V1 Na2 77.68(6) . 4_576 ?
O14 V1 O2 101.61(7) . . ?
O14 V1 O3 109.67(8) . . ?
O14 V1 O5 94.06(6) . . ?
O14 V1 N6 127.38(7) . . ?
V1 Na2 V1 120.37(2) 3_566 4_575 ?
V1 Na2 V1 99.79(2) . 4_575 ?
V1 Na2 V1 109.42(2) 3_566 . ?
V1 Na2 Na2 68.52(2) . 3_576 ?
V1 Na2 Na2 125.76(3) 4_575 3_566 ?
V1 Na2 Na2 129.46(3) . 2 ?
V1 Na2 Na2 117.23(3) 4_575 3_576 ?
V1 Na2 Na2 121.57(4) 3_566 3_576 ?
V1 Na2 Na2 54.82(2) 3_566 3_566 ?
V1 Na2 Na2 121.01(3) 3_566 2 ?
V1 Na2 Na2 54.600(19) . 3_566 ?
V1 Na2 Na2 52.48(2) 4_575 2 ?
Na2 Na2 Na2 174.87(4) 3_566 2 ?
Na2 Na2 Na2 97.76(4) 3_576 3_566 ?
Na2 Na2 Na2 87.065(18) 3_576 2 ?
O3 Na2 V1 24.67(4) 4_575 4_575 ?
O3 Na2 V1 30.23(3) 3_566 3_566 ?
O3 Na2 V1 130.60(4) 3_566 . ?
O3 Na2 V1 141.09(4) 4_575 3_566 ?
O3 Na2 V1 92.54(4) 3_566 4_575 ?
O3 Na2 V1 98.17(4) 4_575 . ?
O3 Na2 Na2 93.54(5) 4_575 3_576 ?
O3 Na2 Na2 142.72(5) 4_575 3_566 ?
O3 Na2 Na2 95.63(4) 3_566 2 ?
O3 Na2 Na2 143.03(5) 3_566 3_576 ?
O3 Na2 Na2 79.47(4) 3_566 3_566 ?
O3 Na2 Na2 37.90(4) 4_575 2 ?
O3 Na2 O3 111.02(4) 4_575 3_566 ?
O3 Na2 O5 178.90(6) 4_575 3_566 ?
O3 Na2 O5 104.16(6) 4_575 . ?
O3 Na2 O14 91.01(5) 4_575 . ?
O3 Na2 O14 154.98(6) 3_566 . ?
O5 Na2 V1 90.39(4) . 4_575 ?
O5 Na2 V1 37.57(3) . . ?
O5 Na2 V1 83.69(4) . 3_566 ?
O5 Na2 V1 82.74(4) 3_566 . ?
O5 Na2 V1 154.62(4) 3_566 4_575 ?
O5 Na2 V1 37.83(3) 3_566 3_566 ?
O5 Na2 Na2 105.19(5) . 3_576 ?
O5 Na2 Na2 141.62(5) 3_566 2 ?
O5 Na2 Na2 37.62(3) 3_566 3_566 ?
O5 Na2 Na2 87.36(4) 3_566 3_576 ?
O5 Na2 Na2 38.57(4) . 3_566 ?
O5 Na2 Na2 141.62(5) . 2 ?
O5 Na2 O3 67.90(5) 3_566 3_566 ?
O5 Na2 O3 95.37(5) . 3_566 ?
O5 Na2 O5 76.19(6) . 3_566 ?
O5 Na2 O14 66.81(5) . . ?
O5 Na2 O14 90.08(5) 3_566 . ?
O14 Na2 V1 115.63(5) 3_576 4_575 ?
O14 Na2 V1 104.50(4) . 4_575 ?
O14 Na2 V1 99.60(5) 3_576 3_566 ?
O14 Na2 V1 126.13(5) . 3_566 ?
O14 Na2 V1 29.23(3) . . ?
O14 Na2 V1 112.43(4) 3_576 . ?
O14 Na2 Na2 64.17(4) 3_576 2 ?
O14 Na2 Na2 44.53(4) 3_576 3_576 ?
O14 Na2 Na2 118.34(5) 3_576 3_566 ?
O14 Na2 Na2 40.37(4) . 3_576 ?
O14 Na2 Na2 75.72(4) . 3_566 ?
O14 Na2 Na2 109.25(4) . 2 ?
O14 Na2 O3 104.33(6) 3_576 3_566 ?
O14 Na2 O3 94.35(6) 3_576 4_575 ?
O14 Na2 O5 146.03(6) 3_576 . ?
O14 Na2 O5 85.85(6) 3_576 3_566 ?
O14 Na2 O14 84.90(5) 3_576 . ?
O5 N1 H1 114(2) . . ?
C8 N1 O5 116.22(15) . . ?
C8 N1 H1 129(2) . . ?
N7 O2 V1 122.95(12) . . ?
V1 O3 Na2 101.98(6) . 3_566 ?
V1 O3 Na2 119.86(7) . 4_576 ?
Na2 O3 Na2 106.63(6) 4_576 3_566 ?
V1 O5 Na2 94.38(6) . 3_566 ?
V1 O5 Na2 96.30(6) . . ?
Na2 O5 Na2 103.81(6) . 3_566 ?
N1 O5 V1 115.83(10) . . ?
N1 O5 Na2 115.31(11) . 3_566 ?
N1 O5 Na2 125.53(11) . . ?
C8 N6 V1 120.00(13) . . ?
C8 N6 C9 122.67(17) . . ?
C9 N6 V1 117.19(13) . . ?
C9 N7 O2 109.33(15) . . ?
N1 C8 N6 112.84(18) . . ?
N1 C8 C12 123.83(17) . . ?
N6 C8 C12 123.31(17) . . ?
N6 C9 C10 118.83(17) . . ?
N7 C9 N6 115.89(18) . . ?
N7 C9 C10 125.28(17) . . ?
C9 C10 H10A 109.7 . . ?
C9 C10 H10B 109.7 . . ?
C9 C10 C11 109.70(17) . . ?
H10A C10 H10B 108.2 . . ?
C11 C10 H10A 109.7 . . ?
C11 C10 H10B 109.7 . . ?
C10 C11 H11A 109.6 . . ?
C10 C11 H11B 109.6 . . ?
C10 C11 C12 110.20(17) . . ?
H11A C11 H11B 108.1 . . ?
C12 C11 H11A 109.6 . . ?
C12 C11 H11B 109.6 . . ?
C8 C12 C11 109.26(16) . . ?
C8 C12 H12A 109.8 . . ?
C8 C12 H12B 109.8 . . ?
C11 C12 H12A 109.8 . . ?
C11 C12 H12B 109.8 . . ?
H12A C12 H12B 108.3 . . ?
V1 O14 Na2 153.74(9) . 3_576 ?
V1 O14 Na2 102.83(7) . . ?
Na2 O14 Na2 95.10(5) 3_576 . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
V1 Na2 O5 V1 -133.81(5) 3_566 . . . ?
V1 Na2 O5 V1 105.67(5) 4_575 . . . ?
V1 Na2 O5 Na2 -37.71(4) 3_566 . . 3_566 ?
V1 Na2 O5 Na2 -158.24(5) 4_575 . . 3_566 ?
V1 Na2 O5 Na2 96.10(7) . . . 3_566 ?
V1 Na2 O5 N1 -128.13(15) . . . . ?
V1 Na2 O5 N1 -22.46(13) 4_575 . . . ?
V1 Na2 O5 N1 98.06(13) 3_566 . . . ?
V1 Na2 O14 V1 -84.13(7) 4_575 . . . ?
V1 Na2 O14 V1 62.51(9) 3_566 . . . ?
V1 Na2 O14 Na2 115.19(5) 4_575 . . 3_576 ?
V1 Na2 O14 Na2 -98.17(6) 3_566 . . 3_576 ?
V1 Na2 O14 Na2 -160.68(11) . . . 3_576 ?
V1 O2 N7 C9 3.1(2) . . . . ?
V1 N6 C8 N1 4.7(2) . . . . ?
V1 N6 C8 C12 -174.10(14) . . . . ?
V1 N6 C9 N7 -0.4(2) . . . . ?
V1 N6 C9 C10 -179.69(14) . . . . ?
Na2 V1 Na2 V1 -127.22(3) 3_566 . . 4_575 ?
Na2 V1 Na2 V1 167.79(3) 4_576 . . 4_575 ?
Na2 V1 Na2 V1 0.0 3_566 . . 3_566 ?
Na2 V1 Na2 V1 -64.994(17) 4_576 . . 3_566 ?
Na2 V1 Na2 Na2 117.25(4) 3_566 . . 3_576 ?
Na2 V1 Na2 Na2 118.97(4) 4_576 . . 2 ?
Na2 V1 Na2 Na2 -176.03(5) 3_566 . . 2 ?
Na2 V1 Na2 Na2 -64.993(17) 4_576 . . 3_566 ?
Na2 V1 Na2 Na2 52.25(2) 4_576 . . 3_576 ?
Na2 V1 Na2 O3 -25.26(5) 3_566 . . 3_566 ?
Na2 V1 Na2 O3 -152.15(5) 3_566 . . 4_575 ?
Na2 V1 Na2 O3 142.86(5) 4_576 . . 4_575 ?
Na2 V1 Na2 O3 -90.26(6) 4_576 . . 3_566 ?
Na2 V1 Na2 O5 -49.51(6) 3_566 . . . ?
Na2 V1 Na2 O5 27.24(3) 3_566 . . 3_566 ?
Na2 V1 Na2 O5 -114.51(6) 4_576 . . . ?
Na2 V1 Na2 O5 -37.76(3) 4_576 . . 3_566 ?
Na2 V1 Na2 O14 109.68(6) 3_566 . . 3_576 ?
Na2 V1 Na2 O14 44.69(5) 4_576 . . 3_576 ?
Na2 V1 Na2 O14 130.56(8) 3_566 . . . ?
Na2 V1 Na2 O14 65.57(8) 4_576 . . . ?
Na2 V1 O2 N7 152.80(14) 4_576 . . . ?
Na2 V1 O2 N7 -95.61(15) . . . . ?
Na2 V1 O2 N7 91.06(16) 3_566 . . . ?
Na2 V1 O3 Na2 -117.34(9) 3_566 . . 4_576 ?
Na2 V1 O3 Na2 -77.65(7) . . . 4_576 ?
Na2 V1 O3 Na2 117.34(9) 4_576 . . 3_566 ?
Na2 V1 O3 Na2 39.69(7) . . . 3_566 ?
Na2 V1 O5 Na2 -104.44(6) . . . 3_566 ?
Na2 V1 O5 Na2 -26.16(5) 4_576 . . 3_566 ?
Na2 V1 O5 Na2 104.44(6) 3_566 . . . ?
Na2 V1 O5 Na2 78.28(6) 4_576 . . . ?
Na2 V1 O5 N1 -120.90(13) 3_566 . . . ?
Na2 V1 O5 N1 134.67(14) . . . . ?
Na2 V1 O5 N1 -147.06(11) 4_576 . . . ?
Na2 V1 N6 C8 30.83(15) 3_566 . . . ?
Na2 V1 N6 C8 104.47(16) 4_576 . . . ?
Na2 V1 N6 C8 -42.40(15) . . . . ?
Na2 V1 N6 C9 -145.07(13) 3_566 . . . ?
Na2 V1 N6 C9 141.70(13) . . . . ?
Na2 V1 N6 C9 -71.43(19) 4_576 . . . ?
Na2 V1 O14 Na2 -112.59(6) 4_576 . . . ?
Na2 V1 O14 Na2 19.29(18) 4_576 . . 3_576 ?
Na2 V1 O14 Na2 -47.45(7) 3_566 . . . ?
Na2 V1 O14 Na2 131.9(2) . . . 3_576 ?
Na2 V1 O14 Na2 84.43(19) 3_566 . . 3_576 ?
Na2 Na2 O5 V1 -96.10(7) 3_566 . . . ?
Na2 Na2 O5 V1 92.15(8) 2 . . . ?
Na2 Na2 O5 V1 -12.76(7) 3_576 . . . ?
Na2 Na2 O5 Na2 83.34(5) 3_576 . . 3_566 ?
Na2 Na2 O5 Na2 -171.75(6) 2 . . 3_566 ?
Na2 Na2 O5 N1 -35.98(16) 2 . . . ?
Na2 Na2 O5 N1 135.77(15) 3_566 . . . ?
Na2 Na2 O5 N1 -140.89(12) 3_576 . . . ?
Na2 Na2 O14 V1 39.72(6) 3_566 . . . ?
Na2 Na2 O14 V1 160.68(11) 3_576 . . . ?
Na2 Na2 O14 V1 -138.96(6) 2 . . . ?
Na2 Na2 O14 Na2 -120.97(6) 3_566 . . 3_576 ?
Na2 Na2 O14 Na2 60.36(5) 2 . . 3_576 ?
N1 C8 C12 C11 -156.31(19) . . . . ?
O2 V1 Na2 V1 -176.24(8) . . . 3_566 ?
O2 V1 Na2 V1 56.54(8) . . . 4_575 ?
O2 V1 Na2 Na2 -176.24(8) . . . 3_566 ?
O2 V1 Na2 Na2 -59.00(8) . . . 3_576 ?
O2 V1 Na2 Na2 7.72(9) . . . 2 ?
O2 V1 Na2 O3 31.61(9) . . . 4_575 ?
O2 V1 Na2 O3 158.50(9) . . . 3_566 ?
O2 V1 Na2 O5 134.24(10) . . . . ?
O2 V1 Na2 O5 -149.00(8) . . . 3_566 ?
O2 V1 Na2 O14 -45.68(11) . . . . ?
O2 V1 Na2 O14 -66.56(10) . . . 3_576 ?
O2 V1 O3 Na2 -161.30(6) . . . 3_566 ?
O2 V1 O3 Na2 81.36(8) . . . 4_576 ?
O2 V1 O5 Na2 -120.50(12) . . . . ?
O2 V1 O5 Na2 135.06(11) . . . 3_566 ?
O2 V1 O5 N1 14.2(2) . . . . ?
O2 V1 N6 C8 177.44(16) . . . . ?
O2 V1 N6 C9 1.54(14) . . . . ?
O2 V1 O14 Na2 -75.2(2) . . . 3_576 ?
O2 V1 O14 Na2 152.94(7) . . . . ?
O2 N7 C9 N6 -1.5(2) . . . . ?
O2 N7 C9 C10 177.76(18) . . . . ?
O3 V1 Na2 V1 -157.32(5) . . . 4_575 ?
O3 V1 Na2 V1 -30.10(6) . . . 3_566 ?
O3 V1 Na2 Na2 -30.10(6) . . . 3_566 ?
O3 V1 Na2 Na2 153.86(6) . . . 2 ?
O3 V1 Na2 Na2 87.14(6) . . . 3_576 ?
O3 V1 Na2 O3 177.75(5) . . . 4_575 ?
O3 V1 Na2 O3 -55.36(10) . . . 3_566 ?
O3 V1 Na2 O5 -2.86(6) . . . 3_566 ?
O3 V1 Na2 O5 -79.62(8) . . . . ?
O3 V1 Na2 O14 100.46(9) . . . . ?
O3 V1 Na2 O14 79.58(7) . . . 3_576 ?
O3 V1 O2 N7 117.52(15) . . . . ?
O3 V1 O5 Na2 5.72(6) . . . 3_566 ?
O3 V1 O5 Na2 110.16(6) . . . . ?
O3 V1 O5 N1 -115.18(13) . . . . ?
O3 V1 N6 C8 79.98(16) . . . . ?
O3 V1 N6 C9 -95.92(15) . . . . ?
O3 V1 O14 Na2 -97.05(7) . . . . ?
O3 V1 O14 Na2 34.8(2) . . . 3_576 ?
O3 Na2 O5 V1 84.98(6) 4_575 . . . ?
O3 Na2 O5 V1 -161.74(6) 3_566 . . . ?
O3 Na2 O5 Na2 -178.93(6) 4_575 . . 3_566 ?
O3 Na2 O5 Na2 -65.65(6) 3_566 . . 3_566 ?
O3 Na2 O5 N1 -43.16(14) 4_575 . . . ?
O3 Na2 O5 N1 70.12(13) 3_566 . . . ?
O3 Na2 O14 V1 47.33(17) 3_566 . . . ?
O3 Na2 O14 V1 -105.04(8) 4_575 . . . ?
O3 Na2 O14 Na2 -113.35(14) 3_566 . . 3_576 ?
O3 Na2 O14 Na2 94.28(6) 4_575 . . 3_576 ?
O5 V1 Na2 V1 49.51(6) . . . 3_566 ?
O5 V1 Na2 V1 -77.70(6) . . . 4_575 ?
O5 V1 Na2 Na2 166.76(7) . . . 3_576 ?
O5 V1 Na2 Na2 49.51(6) . . . 3_566 ?
O5 V1 Na2 Na2 -126.52(8) . . . 2 ?
O5 V1 Na2 O3 -102.63(7) . . . 4_575 ?
O5 V1 Na2 O3 24.25(8) . . . 3_566 ?
O5 V1 Na2 O5 76.75(8) . . . 3_566 ?
O5 V1 Na2 O14 -179.93(10) . . . . ?
O5 V1 Na2 O14 159.19(8) . . . 3_576 ?
O5 V1 O2 N7 -9.8(2) . . . . ?
O5 V1 O3 Na2 -5.72(6) . . . 3_566 ?
O5 V1 O3 Na2 -123.06(7) . . . 4_576 ?
O5 V1 N6 C8 -6.46(14) . . . . ?
O5 V1 N6 C9 177.64(15) . . . . ?
O5 V1 O14 Na2 0.05(7) . . . . ?
O5 V1 O14 Na2 131.94(19) . . . 3_576 ?
O5 Na2 O5 V1 -96.10(7) 3_566 . . . ?
O5 Na2 O5 Na2 0.0 3_566 . . 3_566 ?
O5 Na2 O5 N1 135.77(15) 3_566 . . . ?
O5 Na2 O14 V1 74.86(8) 3_566 . . . ?
O5 Na2 O14 V1 -0.05(7) . . . . ?
O5 Na2 O14 Na2 -85.82(6) 3_566 . . 3_576 ?
O5 Na2 O14 Na2 -160.73(8) . . . 3_576 ?
O5 N1 C8 N6 1.6(2) . . . . ?
O5 N1 C8 C12 -179.60(16) . . . . ?
N6 V1 Na2 V1 101.19(5) . . . 3_566 ?
N6 V1 Na2 V1 -26.03(5) . . . 4_575 ?
N6 V1 Na2 Na2 -141.57(5) . . . 3_576 ?
N6 V1 Na2 Na2 -74.85(6) . . . 2 ?
N6 V1 Na2 Na2 101.19(5) . . . 3_566 ?
N6 V1 Na2 O3 -50.96(7) . . . 4_575 ?
N6 V1 Na2 O3 75.92(8) . . . 3_566 ?
N6 V1 Na2 O5 128.43(6) . . . 3_566 ?
N6 V1 Na2 O5 51.67(8) . . . . ?
N6 V1 Na2 O14 -128.25(9) . . . . ?
N6 V1 Na2 O14 -149.13(7) . . . 3_576 ?
N6 V1 O2 N7 -2.55(14) . . . . ?
N6 V1 O3 Na2 -80.69(8) . . . 3_566 ?
N6 V1 O3 Na2 161.97(7) . . . 4_576 ?
N6 V1 O5 Na2 -127.78(7) . . . . ?
N6 V1 O5 Na2 127.78(7) . . . 3_566 ?
N6 V1 O5 N1 6.88(12) . . . . ?
N6 V1 O14 Na2 73.59(9) . . . . ?
N6 V1 O14 Na2 -154.53(17) . . . 3_576 ?
N6 C8 C12 C11 22.4(3) . . . . ?
N6 C9 C10 C11 -33.9(2) . . . . ?
N7 C9 C10 C11 146.9(2) . . . . ?
C8 N1 O5 V1 -7.0(2) . . . . ?
C8 N1 O5 Na2 -115.81(15) . . . 3_566 ?
C8 N1 O5 Na2 112.72(16) . . . . ?
C8 N6 C9 N7 -176.17(18) . . . . ?
C8 N6 C9 C10 4.5(3) . . . . ?
C9 N6 C8 N1 -179.60(18) . . . . ?
C9 N6 C8 C12 1.6(3) . . . . ?
C9 C10 C11 C12 56.8(2) . . . . ?
C10 C11 C12 C8 -50.6(2) . . . . ?
O14 V1 Na2 V1 102.23(8) . . . 4_575 ?
O14 V1 Na2 V1 -130.56(8) . . . 3_566 ?
O14 V1 Na2 Na2 53.41(8) . . . 2 ?
O14 V1 Na2 Na2 -13.31(7) . . . 3_576 ?
O14 V1 Na2 Na2 -130.56(8) . . . 3_566 ?
O14 V1 Na2 O3 -155.82(10) . . . 3_566 ?
O14 V1 Na2 O3 77.29(8) . . . 4_575 ?
O14 V1 Na2 O5 -103.32(8) . . . 3_566 ?
O14 V1 Na2 O5 179.93(10) . . . . ?
O14 V1 Na2 O14 -20.88(11) . . . 3_576 ?
O14 V1 O2 N7 -128.44(15) . . . . ?
O14 V1 O3 Na2 -26.82(10) . . . 4_576 ?
O14 V1 O3 Na2 90.52(7) . . . 3_566 ?
O14 V1 O5 Na2 -104.49(7) . . . 3_566 ?
O14 V1 O5 Na2 -0.05(7) . . . . ?
O14 V1 O5 N1 134.61(13) . . . . ?
O14 V1 N6 C8 -89.59(16) . . . . ?
O14 V1 N6 C9 94.51(15) . . . . ?
O14 Na2 O5 V1 -35.98(13) 3_576 . . . ?
O14 Na2 O5 V1 0.04(5) . . . . ?
O14 Na2 O5 Na2 60.11(12) 3_576 . . 3_566 ?
O14 Na2 O5 Na2 96.14(6) . . . 3_566 ?
O14 Na2 O5 N1 -128.09(14) . . . . ?
O14 Na2 O5 N1 -164.12(13) 3_576 . . . ?
O14 Na2 O14 V1 160.69(11) 3_576 . . . ?
O14 Na2 O14 Na2 0.0 3_576 . . 3_576 ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: ethanol, hexane'
