# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2017

####################################################################### 
# 
# 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_shrv440
_audit_block_doi                 10.5517/ccdc.csd.cc1mhn0s
_database_code_depnum_ccdc_archive 'CCDC 1504585'
_audit_update_record             
;
2016-09-16 deposited with the CCDC.
2017-04-17 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         'C6 H6 N12 O4'
_chemical_formula_sum            'C6 H6 N12 O4'
_chemical_formula_weight         310.23

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   6.5577(7)
_cell_length_b                   31.045(3)
_cell_length_c                   5.8420(6)
_cell_angle_alpha                90
_cell_angle_beta                 95.054(2)
_cell_angle_gamma                90
_cell_volume                     1184.7(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6044
_cell_measurement_theta_min      2.625
_cell_measurement_theta_max      29.908

_exptl_crystal_description       needle
_exptl_crystal_colour            'clear colorless'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.739
_exptl_crystal_F_000             632
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.239
_exptl_crystal_size_mid          0.087
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    0.148
_shelx_estimated_absorpt_T_min   0.966
_shelx_estimated_absorpt_T_max   0.997
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6975
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_process_details   'SADABS v2014/5 (Bruker, 2008)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15752
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.624
_diffrn_reflns_theta_max         29.966
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             3348
_reflns_number_gt                2825
_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 APEX3 v2015.5-2 (Bruker, 2015)'
_computing_cell_refinement       'Bruker APEX3 v2015.5-2 (Bruker, 2015)'
_computing_data_reduction        
;
Bruker SAINT v8.34A (Bruker, 2013), Bruker XPREP v2014/2 (Bruker, 2014)
;
_computing_structure_solution    'Bruker SHELXTL v2014/7 (Bruker, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL v2014/7 (Bruker, 2014)'
_computing_publication_material  'Bruker SHELXTL v2014/7 (Bruker, 2014)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0413P)²+0.4590P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3348
_refine_ls_number_parameters     199
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0353
_refine_ls_wR_factor_ref         0.0909
_refine_ls_wR_factor_gt          0.0862
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.039
_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
N1 N 0.61487(19) 0.28240(4) 0.9436(3) 0.0404(3) Uani 1 1 d . . . . .
N2 N 0.47895(16) 0.30202(3) 0.9790(2) 0.0247(2) Uani 1 1 d . . . . .
N3 N 0.34558(16) 0.32516(3) 1.05854(18) 0.0232(2) Uani 1 1 d . . . . .
C4 C 0.17539(16) 0.33833(3) 0.92187(19) 0.0155(2) Uani 1 1 d . . . . .
C5 C 0.05834(17) 0.32567(3) 0.72161(19) 0.0169(2) Uani 1 1 d . . . . .
N6 N 0.09664(17) 0.28985(3) 0.57804(18) 0.0238(2) Uani 1 1 d . . . . .
O7 O 0.26864(17) 0.27420(3) 0.60138(19) 0.0376(3) Uani 1 1 d . . . . .
O8 O -0.04223(17) 0.27688(4) 0.4431(2) 0.0430(3) Uani 1 1 d . . . . .
C9 C -0.10906(17) 0.35405(4) 0.70705(19) 0.0166(2) Uani 1 1 d . . . . .
N10 N -0.28011(15) 0.35816(3) 0.53146(17) 0.0215(2) Uani 1 1 d . . . . .
O11 O -0.24305(15) 0.35447(4) 0.33142(16) 0.0377(3) Uani 1 1 d . . . . .
O12 O -0.44838(14) 0.36594(4) 0.59661(17) 0.0348(2) Uani 1 1 d . . . . .
N13 N -0.09928(14) 0.38234(3) 0.87548(16) 0.01611(18) Uani 1 1 d . . . . .
N14 N 0.07538(14) 0.37226(3) 1.00584(15) 0.01456(18) Uani 1 1 d . . . . .
C15 C 0.15041(17) 0.39944(3) 1.20059(18) 0.0163(2) Uani 1 1 d . . . . .
H15A H 0.1925 0.3810 1.3348 0.020 Uiso 1 1 calc R U . . .
H15B H 0.0387 0.4185 1.2428 0.020 Uiso 1 1 calc R U . . .
C16 C 0.33177(17) 0.42675(3) 1.14121(18) 0.0161(2) Uani 1 1 d . . . . .
H16A H 0.3891 0.4421 1.2808 0.019 Uiso 1 1 calc R U . . .
H16B H 0.4398 0.4076 1.0903 0.019 Uiso 1 1 calc R U . . .
N17 N 0.27503(14) 0.45813(3) 0.96086(15) 0.01536(18) Uani 1 1 d . . . . .
N18 N 0.25903(15) 0.44684(3) 0.73363(16) 0.0205(2) Uani 1 1 d . . . . .
N19 N 0.22495(16) 0.48223(3) 0.62148(17) 0.0221(2) Uani 1 1 d . . . . .
N20 N 0.21752(15) 0.51711(3) 0.76237(16) 0.0194(2) Uani 1 1 d . . . . .
C21 C 0.24895(16) 0.50117(3) 0.97457(18) 0.0146(2) Uani 1 1 d . . . . .
N22 N 0.26047(15) 0.52394(3) 1.17090(16) 0.01844(19) Uani 1 1 d . . . . .
H22A H 0.2468 0.5521 1.1664 0.022 Uiso 1 1 calc R U . . .
H22B H 0.2817 0.5107 1.3039 0.022 Uiso 1 1 calc R U . . .


_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
N1 N2 1.1140(16) . ?
N2 N3 1.2524(15) . ?
N3 C4 1.3759(15) . ?
C4 N14 1.3554(14) . ?
C4 C5 1.3979(15) . ?
C5 C9 1.4043(16) . ?
C5 N6 1.4285(14) . ?
N6 O8 1.2192(14) . ?
N6 O7 1.2247(15) . ?
C9 N13 1.3162(14) . ?
C9 N10 1.4574(14) . ?
N10 O11 1.2198(14) . ?
N10 O12 1.2227(14) . ?
N13 N14 1.3550(13) . ?
N14 C15 1.4663(13) . ?
C15 C16 1.5251(15) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 N17 1.4590(13) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
N17 C21 1.3503(14) . ?
N17 N18 1.3681(13) . ?
N18 N19 1.2885(15) . ?
N19 N20 1.3636(14) . ?
N20 C21 1.3338(14) . ?
C21 N22 1.3438(14) . ?
N22 H22A 0.8800 . ?
N22 H22B 0.8800 . ?

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
N1 N2 N3 168.22(15) . . ?
N2 N3 C4 120.83(11) . . ?
N14 C4 N3 114.49(10) . . ?
N14 C4 C5 105.89(9) . . ?
N3 C4 C5 139.43(10) . . ?
C4 C5 C9 104.06(9) . . ?
C4 C5 N6 126.75(10) . . ?
C9 C5 N6 129.03(10) . . ?
O8 N6 O7 124.69(11) . . ?
O8 N6 C5 118.48(11) . . ?
O7 N6 C5 116.83(10) . . ?
N13 C9 C5 112.77(10) . . ?
N13 C9 N10 116.85(10) . . ?
C5 C9 N10 130.29(10) . . ?
O11 N10 O12 125.32(11) . . ?
O11 N10 C9 117.40(10) . . ?
O12 N10 C9 117.26(10) . . ?
C9 N13 N14 104.43(9) . . ?
N13 N14 C4 112.83(9) . . ?
N13 N14 C15 120.83(9) . . ?
C4 N14 C15 126.03(9) . . ?
N14 C15 C16 111.01(9) . . ?
N14 C15 H15A 109.4 . . ?
C16 C15 H15A 109.4 . . ?
N14 C15 H15B 109.4 . . ?
C16 C15 H15B 109.4 . . ?
H15A C15 H15B 108.0 . . ?
N17 C16 C15 112.40(9) . . ?
N17 C16 H16A 109.1 . . ?
C15 C16 H16A 109.1 . . ?
N17 C16 H16B 109.1 . . ?
C15 C16 H16B 109.1 . . ?
H16A C16 H16B 107.9 . . ?
C21 N17 N18 108.17(9) . . ?
C21 N17 C16 130.06(9) . . ?
N18 N17 C16 121.50(9) . . ?
N19 N18 N17 105.67(9) . . ?
N18 N19 N20 112.57(9) . . ?
C21 N20 N19 104.82(9) . . ?
N20 C21 N22 126.20(10) . . ?
N20 C21 N17 108.78(9) . . ?
N22 C21 N17 124.98(10) . . ?
C21 N22 H22A 120.0 . . ?
C21 N22 H22B 120.0 . . ?
H22A N22 H22B 120.0 . . ?

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
N1 N2 N3 C4 174.7(6) . . . . ?
N2 N3 C4 N14 -162.10(11) . . . . ?
N2 N3 C4 C5 23.8(2) . . . . ?
N14 C4 C5 C9 -0.99(11) . . . . ?
N3 C4 C5 C9 173.46(13) . . . . ?
N14 C4 C5 N6 -176.81(10) . . . . ?
N3 C4 C5 N6 -2.4(2) . . . . ?
C4 C5 N6 O8 162.72(12) . . . . ?
C9 C5 N6 O8 -12.06(18) . . . . ?
C4 C5 N6 O7 -16.91(17) . . . . ?
C9 C5 N6 O7 168.32(12) . . . . ?
C4 C5 C9 N13 1.21(13) . . . . ?
N6 C5 C9 N13 176.89(11) . . . . ?
C4 C5 C9 N10 177.36(11) . . . . ?
N6 C5 C9 N10 -6.96(19) . . . . ?
N13 C9 N10 O11 136.06(12) . . . . ?
C5 C9 N10 O11 -39.96(17) . . . . ?
N13 C9 N10 O12 -42.43(15) . . . . ?
C5 C9 N10 O12 141.55(13) . . . . ?
C5 C9 N13 N14 -0.89(12) . . . . ?
N10 C9 N13 N14 -177.60(9) . . . . ?
C9 N13 N14 C4 0.21(12) . . . . ?
C9 N13 N14 C15 174.13(9) . . . . ?
N3 C4 N14 N13 -175.51(9) . . . . ?
C5 C4 N14 N13 0.53(12) . . . . ?
N3 C4 N14 C15 10.95(15) . . . . ?
C5 C4 N14 C15 -173.02(9) . . . . ?
N13 N14 C15 C16 -104.27(11) . . . . ?
C4 N14 C15 C16 68.80(13) . . . . ?
N14 C15 C16 N17 65.40(11) . . . . ?
C15 C16 N17 C21 105.22(12) . . . . ?
C15 C16 N17 N18 -81.58(12) . . . . ?
C21 N17 N18 N19 -0.01(12) . . . . ?
C16 N17 N18 N19 -174.53(9) . . . . ?
N17 N18 N19 N20 0.14(13) . . . . ?
N18 N19 N20 C21 -0.22(13) . . . . ?
N19 N20 C21 N22 178.01(10) . . . . ?
N19 N20 C21 N17 0.20(12) . . . . ?
N18 N17 C21 N20 -0.13(12) . . . . ?
C16 N17 C21 N20 173.77(10) . . . . ?
N18 N17 C21 N22 -177.97(10) . . . . ?
C16 N17 C21 N22 -4.07(18) . . . . ?

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
C15 H15B N20 0.99 2.61 3.5598(15) 161.0 3_567
C16 H16A N19 0.99 2.65 3.4170(15) 133.9 1_556
C16 H16B N3 0.99 2.64 3.1930(15) 115.8 .
N22 H22A N13 0.88 2.26 3.0992(14) 160.3 3_567
N22 H22B N19 0.88 2.12 2.9611(14) 160.6 1_556

_refine_diff_density_max         0.381
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.046

# start Validation Reply Form
_vrf_PLAT015_shrv440             
;
PROBLEM: No _shelx_hkl_file record in SHELXL20xy CIF ....     Please Do ! 
RESPONSE: It is our policy to routinely not supply the HKL file unless 
specifically required.
;
####################################################################### 
# 
# 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_shrv444
_audit_block_doi                 10.5517/ccdc.csd.cc1mhn1t
_database_code_depnum_ccdc_archive 'CCDC 1504586'
_audit_update_record             
;
2016-09-16 deposited with the CCDC.
2017-04-17 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         'C6 H4 N13 Na O6'
_chemical_formula_sum            'C6 H4 N13 Na O6'
_chemical_formula_weight         377.21

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'
N N 0.0061 0.0033 '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'
O O 0.0106 0.0060 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   29.426(4)
_cell_length_b                   8.4217(11)
_cell_length_c                   11.1029(14)
_cell_angle_alpha                90
_cell_angle_beta                 100.699(5)
_cell_angle_gamma                90
_cell_volume                     2703.7(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2605
_cell_measurement_theta_min      2.519
_cell_measurement_theta_max      22.479

_exptl_crystal_description       plate
_exptl_crystal_colour            'clear colorless'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.853
_exptl_crystal_F_000             1520
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.288
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.005
_exptl_absorpt_coefficient_mu    0.189
_shelx_estimated_absorpt_T_min   0.948
_shelx_estimated_absorpt_T_max   0.999
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5716
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   'SADABS v2014/5 (Bruker, 2008)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22925
_diffrn_reflns_av_unetI/netI     0.1197
_diffrn_reflns_av_R_equivalents  0.1500
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         0.704
_diffrn_reflns_theta_max         25.366
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4937
_reflns_number_gt                3092
_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 APEX3 v2015.5-2 (Bruker, 2015)'
_computing_cell_refinement       'Bruker APEX3 v2015.5-2 (Bruker, 2015)'
_computing_data_reduction        
;
Bruker SAINT v8.34A (Bruker, 2013), Bruker XPREP v2014/2 (Bruker, 2014)
;
_computing_structure_solution    'Bruker SHELXTL v2014/7 (Bruker, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL v2014/7 (Bruker, 2014)'
_computing_publication_material  'Bruker SHELXTL v2014/7 (Bruker, 2014)'
_refine_special_details          
;
Crystal was a pseudo-merohedral two-component twin 
(1 0 1 0 -1 0 0 0 -1, BASF = 0.401).

Enhanced rigid bond restraints were applied to all atoms 
with default esds.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0771P)²+9.8937P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4937
_refine_ls_number_parameters     470
_refine_ls_number_restraints     408
_refine_ls_R_factor_all          0.1383
_refine_ls_R_factor_gt           0.0765
_refine_ls_wR_factor_ref         0.2025
_refine_ls_wR_factor_gt          0.1766
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.001
_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
N1 N 0.7774(3) 0.7019(9) 1.0285(9) 0.050(2) Uani 1 1 d . U . . .
N2 N 0.8030(3) 0.6307(8) 0.9836(7) 0.0291(17) Uani 1 1 d . U . . .
N3 N 0.8360(2) 0.5808(8) 0.9373(7) 0.0285(17) Uani 1 1 d . U . . .
C4 C 0.8347(3) 0.4320(9) 0.8832(8) 0.0217(17) Uani 1 1 d . U . . .
C5 C 0.8206(3) 0.2774(9) 0.9057(8) 0.0221(17) Uani 1 1 d . U . . .
N6 N 0.7953(2) 0.2370(9) 1.0017(7) 0.0300(17) Uani 1 1 d . U . . .
O7 O 0.7934(2) 0.0963(7) 1.0298(6) 0.0419(17) Uani 1 1 d . U . . .
O8 O 0.7794(2) 0.3465(7) 1.0533(6) 0.0346(15) Uani 1 1 d . U . . .
C9 C 0.8393(3) 0.1845(8) 0.8245(8) 0.0191(16) Uani 1 1 d . U . . .
N10 N 0.8360(3) 0.0140(8) 0.8040(7) 0.0303(17) Uani 1 1 d . U . . .
O11 O 0.8706(2) -0.0496(7) 0.7773(9) 0.055(2) Uani 1 1 d . U . . .
O12 O 0.7994(2) -0.0503(7) 0.8105(7) 0.0476(19) Uani 1 1 d . U . . .
N13 N 0.8619(2) 0.2654(7) 0.7536(7) 0.0191(15) Uani 1 1 d . U . . .
N14 N 0.8573(2) 0.4197(7) 0.7895(6) 0.0164(14) Uani 1 1 d . U . . .
C15 C 0.8815(3) 0.5463(8) 0.7351(8) 0.0203(17) Uani 1 1 d . U . . .
H15A H 0.8672 0.6500 0.7479 0.024 Uiso 1 1 calc R U . . .
H15B H 0.8778 0.5284 0.6457 0.024 Uiso 1 1 calc R U . . .
C16 C 0.9316(3) 0.5515(8) 0.7900(7) 0.0159(16) Uani 1 1 d . U . . .
H16B H 0.9458 0.4478 0.7772 0.019 Uiso 1 1 calc R U . . .
H16A H 0.9469 0.6335 0.7474 0.019 Uiso 1 1 calc R U . . .
N17 N 0.9398(2) 0.5867(7) 0.9198(6) 0.0172(14) Uani 1 1 d . U . . .
N18 N 0.9440(2) 0.7394(7) 0.9627(7) 0.0205(15) Uani 1 1 d . U . . .
N19 N 0.9520(3) 0.7282(8) 1.0795(8) 0.0313(18) Uani 1 1 d . U . . .
N20 N 0.9530(2) 0.5729(7) 1.1193(7) 0.0247(16) Uani 1 1 d . U . . .
C21 C 0.9462(3) 0.4882(8) 1.0158(8) 0.0169(16) Uani 1 1 d . U . . .
N22 N 0.9430(2) 0.3279(7) 0.9876(6) 0.0219(16) Uani 1 1 d . U . . .
N23 N 0.9583(2) 0.2334(7) 1.0810(7) 0.0196(14) Uani 1 1 d . U . . .
O24 O 0.9715(2) 0.2722(6) 1.1876(6) 0.0271(14) Uani 1 1 d . U . . .
O25 O 0.9600(2) 0.0851(6) 1.0513(6) 0.0287(14) Uani 1 1 d . U . . .
Na26 Na 0.96252(13) 0.0211(4) 0.8362(3) 0.0369(10) Uani 1 1 d . U . . .
N27 N 0.7492(3) -0.1048(10) 0.2320(8) 0.045(2) Uani 1 1 d . U . . .
N28 N 0.7173(3) -0.0690(8) 0.1691(7) 0.0317(18) Uani 1 1 d . U . . .
N29 N 0.6786(3) -0.0546(8) 0.1004(8) 0.0317(18) Uani 1 1 d . U . . .
C30 C 0.6706(2) 0.0867(9) 0.0341(8) 0.0196(16) Uani 1 1 d . U . . .
C31 C 0.6790(3) 0.2486(9) 0.0625(8) 0.0176(16) Uani 1 1 d . U . . .
N32 N 0.7002(2) 0.3150(9) 0.1751(7) 0.0268(15) Uani 1 1 d . U . . .
O33 O 0.6954(2) 0.4600(7) 0.1862(6) 0.0386(16) Uani 1 1 d . U . . .
O34 O 0.7197(2) 0.2275(8) 0.2531(6) 0.0360(15) Uani 1 1 d . U . . .
C35 C 0.6560(3) 0.3234(9) -0.0416(8) 0.0208(17) Uani 1 1 d . U . . .
N36 N 0.6529(3) 0.4918(7) -0.0750(7) 0.0255(15) Uani 1 1 d . U . . .
O37 O 0.6886(2) 0.5674(7) -0.0634(8) 0.0457(18) Uani 1 1 d . U . . .
O38 O 0.6152(2) 0.5462(6) -0.1201(6) 0.0306(15) Uani 1 1 d . U . . .
N39 N 0.6351(2) 0.2284(7) -0.1279(7) 0.0181(15) Uani 1 1 d . U . . .
N40 N 0.6452(2) 0.0804(7) -0.0766(7) 0.0180(14) Uani 1 1 d . U . . .
C41 C 0.6230(3) -0.0575(8) -0.1407(8) 0.0174(17) Uani 1 1 d . U . . .
H41B H 0.6377 -0.1550 -0.1017 0.021 Uiso 1 1 calc R U . . .
H41A H 0.6277 -0.0556 -0.2267 0.021 Uiso 1 1 calc R U . . .
C42 C 0.5723(3) -0.0629(8) -0.1398(7) 0.0136(15) Uani 1 1 d . U . . .
H42A H 0.5583 0.0402 -0.1692 0.016 Uiso 1 1 calc R U . . .
H42B H 0.5579 -0.1460 -0.1976 0.016 Uiso 1 1 calc R U . . .
N43 N 0.5620(2) -0.0956(6) -0.0192(6) 0.0127(13) Uani 1 1 d . U . . .
N44 N 0.5520(2) -0.2430(7) 0.0122(6) 0.0141(14) Uani 1 1 d . U . . .
N45 N 0.5388(2) -0.2311(7) 0.1198(6) 0.0155(14) Uani 1 1 d . U . . .
N46 N 0.5401(2) -0.0728(7) 0.1574(6) 0.0193(15) Uani 1 1 d . U . . .
C47 C 0.5541(2) 0.0095(8) 0.0698(7) 0.0106(14) Uani 1 1 d . U . . .
N48 N 0.5611(2) 0.1659(7) 0.0467(6) 0.0161(14) Uani 1 1 d . U . . .
N49 N 0.54492(19) 0.2674(7) 0.1142(6) 0.0125(13) Uani 1 1 d . U . . .
O50 O 0.54537(19) 0.4128(6) 0.0836(5) 0.0226(13) Uani 1 1 d . U . . .
O51 O 0.52822(17) 0.2339(5) 0.2100(5) 0.0157(12) Uani 1 1 d . U . . .
Na52 Na 0.52877(12) 0.4709(3) -0.1366(3) 0.0252(8) Uani 1 1 d . U . . .


_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
N1 N2 1.147(10) . ?
N2 N3 1.254(9) . ?
N3 C4 1.388(10) . ?
C4 N14 1.339(11) . ?
C4 C5 1.402(11) . ?
C5 C9 1.382(12) . ?
C5 N6 1.449(11) . ?
N6 O8 1.225(9) . ?
N6 O7 1.229(9) . ?
C9 N13 1.310(10) . ?
C9 N10 1.454(10) . ?
N10 O12 1.221(9) . ?
N10 O11 1.234(9) . ?
O11 Na26 2.728(8) . ?
N13 N14 1.374(9) . ?
N14 C15 1.472(10) . ?
C15 C16 1.489(11) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 N17 1.446(10) . ?
C16 H16B 0.9900 . ?
C16 H16A 0.9900 . ?
N17 C21 1.336(10) . ?
N17 N18 1.369(8) . ?
N18 N19 1.278(10) . ?
N18 Na26 2.860(8) 1_565 ?
N19 N20 1.379(9) . ?
N20 C21 1.336(10) . ?
N20 Na26 2.501(8) 4_566 ?
C21 N22 1.385(10) . ?
N22 N23 1.318(9) . ?
N23 O24 1.219(9) . ?
N23 O25 1.295(8) . ?
O24 Na26 2.447(7) 4_566 ?
O25 Na26 2.462(7) . ?
O25 Na26 2.549(7) 3_757 ?
Na26 O24 2.447(7) 4_565 ?
Na26 N20 2.501(8) 4_565 ?
Na26 O25 2.549(7) 3_757 ?
Na26 N18 2.860(8) 1_545 ?
Na26 Na26 3.904(7) 3_757 ?
N27 N28 1.104(10) . ?
N28 N29 1.252(10) . ?
N29 C30 1.396(10) . ?
C30 N40 1.316(11) . ?
C30 C31 1.411(11) . ?
C31 C35 1.379(11) . ?
C31 N32 1.406(11) . ?
N32 O34 1.199(9) . ?
N32 O33 1.238(9) . ?
C35 N39 1.311(10) . ?
C35 N36 1.465(10) . ?
N36 O37 1.212(8) . ?
N36 O38 1.220(9) . ?
O38 Na52 2.594(7) . ?
N39 N40 1.379(9) . ?
N40 C41 1.453(9) . ?
C41 C42 1.494(11) . ?
C41 H41B 0.9900 . ?
C41 H41A 0.9900 . ?
C42 N43 1.452(9) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
N43 N44 1.337(8) . ?
N43 C47 1.379(9) . ?
N44 N45 1.326(9) . ?
N44 Na52 2.930(7) 1_545 ?
N45 N46 1.396(8) . ?
N45 Na52 2.865(7) 3_655 ?
N46 C47 1.320(9) . ?
N46 Na52 2.522(7) 4_566 ?
C47 N48 1.365(9) . ?
N48 N49 1.286(9) . ?
N49 O50 1.271(8) . ?
N49 O51 1.282(8) . ?
O50 Na52 2.452(7) . ?
O50 Na52 2.558(6) 3_665 ?
O51 Na52 2.422(6) 4_566 ?
Na52 O51 2.422(6) 4_565 ?
Na52 N46 2.522(7) 4_565 ?
Na52 O50 2.558(6) 3_665 ?
Na52 N45 2.865(7) 3_655 ?
Na52 N44 2.930(7) 1_565 ?
Na52 Na52 3.770(6) 3_665 ?

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
N1 N2 N3 167.3(9) . . ?
N2 N3 C4 121.3(7) . . ?
N14 C4 N3 115.4(7) . . ?
N14 C4 C5 105.8(7) . . ?
N3 C4 C5 138.3(8) . . ?
C9 C5 C4 104.0(7) . . ?
C9 C5 N6 131.9(7) . . ?
C4 C5 N6 123.9(8) . . ?
O8 N6 O7 124.5(8) . . ?
O8 N6 C5 117.5(7) . . ?
O7 N6 C5 117.9(7) . . ?
N13 C9 C5 113.9(7) . . ?
N13 C9 N10 116.4(7) . . ?
C5 C9 N10 129.6(7) . . ?
O12 N10 O11 126.7(7) . . ?
O12 N10 C9 117.6(7) . . ?
O11 N10 C9 115.6(7) . . ?
N10 O11 Na26 132.3(6) . . ?
C9 N13 N14 103.3(7) . . ?
C4 N14 N13 112.8(6) . . ?
C4 N14 C15 127.6(6) . . ?
N13 N14 C15 119.1(6) . . ?
N14 C15 C16 111.8(6) . . ?
N14 C15 H15A 109.3 . . ?
C16 C15 H15A 109.3 . . ?
N14 C15 H15B 109.3 . . ?
C16 C15 H15B 109.3 . . ?
H15A C15 H15B 107.9 . . ?
N17 C16 C15 112.5(7) . . ?
N17 C16 H16B 109.1 . . ?
C15 C16 H16B 109.1 . . ?
N17 C16 H16A 109.1 . . ?
C15 C16 H16A 109.1 . . ?
H16B C16 H16A 107.8 . . ?
C21 N17 N18 108.4(7) . . ?
C21 N17 C16 129.8(6) . . ?
N18 N17 C16 121.8(6) . . ?
N19 N18 N17 105.8(6) . . ?
N19 N18 Na26 122.9(5) . 1_565 ?
N17 N18 Na26 128.4(5) . 1_565 ?
N18 N19 N20 112.6(7) . . ?
C21 N20 N19 103.9(7) . . ?
C21 N20 Na26 129.2(5) . 4_566 ?
N19 N20 Na26 126.9(5) . 4_566 ?
N17 C21 N20 109.4(6) . . ?
N17 C21 N22 115.6(7) . . ?
N20 C21 N22 135.0(7) . . ?
N23 N22 C21 114.3(7) . . ?
O24 N23 O25 119.0(7) . . ?
O24 N23 N22 127.1(6) . . ?
O25 N23 N22 113.9(7) . . ?
N23 O24 Na26 142.2(5) . 4_566 ?
N23 O25 Na26 117.9(5) . . ?
N23 O25 Na26 106.6(4) . 3_757 ?
Na26 O25 Na26 102.3(2) . 3_757 ?
O24 Na26 O25 121.6(2) 4_565 . ?
O24 Na26 N20 65.3(2) 4_565 4_565 ?
O25 Na26 N20 170.1(3) . 4_565 ?
O24 Na26 O25 112.4(2) 4_565 3_757 ?
O25 Na26 O25 77.7(2) . 3_757 ?
N20 Na26 O25 106.9(2) 4_565 3_757 ?
O24 Na26 O11 102.7(3) 4_565 . ?
O25 Na26 O11 94.2(3) . . ?
N20 Na26 O11 76.8(3) 4_565 . ?
O25 Na26 O11 142.9(2) 3_757 . ?
O24 Na26 N18 167.3(3) 4_565 1_545 ?
O25 Na26 N18 70.3(2) . 1_545 ?
N20 Na26 N18 102.3(2) 4_565 1_545 ?
O25 Na26 N18 72.7(2) 3_757 1_545 ?
O11 Na26 N18 70.5(2) . 1_545 ?
O24 Na26 Na26 125.5(2) 4_565 3_757 ?
O25 Na26 Na26 39.65(15) . 3_757 ?
N20 Na26 Na26 144.2(2) 4_565 3_757 ?
O25 Na26 Na26 38.04(15) 3_757 3_757 ?
O11 Na26 Na26 124.6(3) . 3_757 ?
N18 Na26 Na26 66.00(18) 1_545 3_757 ?
N27 N28 N29 169.3(10) . . ?
N28 N29 C30 116.8(7) . . ?
N40 C30 N29 118.0(7) . . ?
N40 C30 C31 107.1(7) . . ?
N29 C30 C31 134.4(8) . . ?
C35 C31 N32 129.1(7) . . ?
C35 C31 C30 102.5(7) . . ?
N32 C31 C30 127.9(8) . . ?
O34 N32 O33 125.7(8) . . ?
O34 N32 C31 118.1(7) . . ?
O33 N32 C31 116.2(7) . . ?
N39 C35 C31 115.1(7) . . ?
N39 C35 N36 114.0(7) . . ?
C31 C35 N36 130.8(7) . . ?
O37 N36 O38 123.4(7) . . ?
O37 N36 C35 118.0(7) . . ?
O38 N36 C35 118.4(6) . . ?
N36 O38 Na52 138.0(5) . . ?
C35 N39 N40 102.4(7) . . ?
C30 N40 N39 113.0(6) . . ?
C30 N40 C41 128.0(6) . . ?
N39 N40 C41 118.5(6) . . ?
N40 C41 C42 112.3(6) . . ?
N40 C41 H41B 109.1 . . ?
C42 C41 H41B 109.1 . . ?
N40 C41 H41A 109.1 . . ?
C42 C41 H41A 109.1 . . ?
H41B C41 H41A 107.9 . . ?
N43 C42 C41 113.0(6) . . ?
N43 C42 H42A 109.0 . . ?
C41 C42 H42A 109.0 . . ?
N43 C42 H42B 109.0 . . ?
C41 C42 H42B 109.0 . . ?
H42A C42 H42B 107.8 . . ?
N44 N43 C47 109.5(6) . . ?
N44 N43 C42 120.7(6) . . ?
C47 N43 C42 129.2(6) . . ?
N45 N44 N43 106.3(5) . . ?
N45 N44 Na52 119.6(4) . 1_545 ?
N43 N44 Na52 131.0(5) . 1_545 ?
N44 N45 N46 110.2(5) . . ?
N44 N45 Na52 109.1(4) . 3_655 ?
N46 N45 Na52 129.3(4) . 3_655 ?
C47 N46 N45 106.0(6) . . ?
C47 N46 Na52 126.9(5) . 4_566 ?
N45 N46 Na52 126.6(5) . 4_566 ?
N46 C47 N48 136.4(7) . . ?
N46 C47 N43 108.0(6) . . ?
N48 C47 N43 115.6(6) . . ?
N49 N48 C47 116.5(6) . . ?
O50 N49 O51 117.3(6) . . ?
O50 N49 N48 117.4(6) . . ?
O51 N49 N48 125.3(6) . . ?
N49 O50 Na52 116.7(4) . . ?
N49 O50 Na52 104.8(4) . 3_665 ?
Na52 O50 Na52 97.6(2) . 3_665 ?
N49 O51 Na52 141.8(4) . 4_566 ?
O51 Na52 O50 122.2(2) 4_565 . ?
O51 Na52 N46 65.7(2) 4_565 4_565 ?
O50 Na52 N46 159.5(2) . 4_565 ?
O51 Na52 O50 122.7(2) 4_565 3_665 ?
O50 Na52 O50 82.4(2) . 3_665 ?
N46 Na52 O50 109.9(2) 4_565 3_665 ?
O51 Na52 O38 95.9(2) 4_565 . ?
O50 Na52 O38 88.1(2) . . ?
N46 Na52 O38 71.8(2) 4_565 . ?
O50 Na52 O38 139.2(2) 3_665 . ?
O51 Na52 N45 68.27(19) 4_565 3_655 ?
O50 Na52 N45 78.8(2) . 3_655 ?
N46 Na52 N45 120.6(2) 4_565 3_655 ?
O50 Na52 N45 67.84(18) 3_665 3_655 ?
O38 Na52 N45 148.4(2) . 3_655 ?
O51 Na52 N44 162.3(2) 4_565 1_565 ?
O50 Na52 N44 67.64(19) . 1_565 ?
N46 Na52 N44 100.1(2) 4_565 1_565 ?
O50 Na52 N44 71.03(19) 3_665 1_565 ?
O38 Na52 N44 68.7(2) . 1_565 ?
N45 Na52 N44 129.4(2) 3_655 1_565 ?
O51 Na52 Na52 135.49(19) 4_565 3_665 ?
O50 Na52 Na52 42.25(14) . 3_665 ?
N46 Na52 Na52 147.1(2) 4_565 3_665 ?
O50 Na52 Na52 40.14(14) 3_665 3_665 ?
O38 Na52 Na52 119.5(2) . 3_665 ?
N45 Na52 Na52 67.56(16) 3_655 3_665 ?
N44 Na52 Na52 62.09(15) 1_565 3_665 ?

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
N1 N2 N3 C4 -174(4) . . . . ?
N2 N3 C4 N14 148.3(8) . . . . ?
N2 N3 C4 C5 -41.4(15) . . . . ?
N14 C4 C5 C9 3.4(9) . . . . ?
N3 C4 C5 C9 -167.5(10) . . . . ?
N14 C4 C5 N6 179.2(7) . . . . ?
N3 C4 C5 N6 8.3(16) . . . . ?
C9 C5 N6 O8 -174.0(9) . . . . ?
C4 C5 N6 O8 11.5(12) . . . . ?
C9 C5 N6 O7 9.6(13) . . . . ?
C4 C5 N6 O7 -164.9(8) . . . . ?
C4 C5 C9 N13 -1.8(10) . . . . ?
N6 C5 C9 N13 -177.1(8) . . . . ?
C4 C5 C9 N10 -179.2(8) . . . . ?
N6 C5 C9 N10 5.5(15) . . . . ?
N13 C9 N10 O12 -140.3(8) . . . . ?
C5 C9 N10 O12 37.0(13) . . . . ?
N13 C9 N10 O11 37.1(11) . . . . ?
C5 C9 N10 O11 -145.5(9) . . . . ?
O12 N10 O11 Na26 -152.9(7) . . . . ?
C9 N10 O11 Na26 30.0(12) . . . . ?
C5 C9 N13 N14 -0.6(9) . . . . ?
N10 C9 N13 N14 177.2(6) . . . . ?
N3 C4 N14 N13 169.2(6) . . . . ?
C5 C4 N14 N13 -4.1(9) . . . . ?
N3 C4 N14 C15 -2.6(11) . . . . ?
C5 C4 N14 C15 -176.0(7) . . . . ?
C9 N13 N14 C4 2.9(8) . . . . ?
C9 N13 N14 C15 175.6(7) . . . . ?
C4 N14 C15 C16 94.0(9) . . . . ?
N13 N14 C15 C16 -77.5(9) . . . . ?
N14 C15 C16 N17 -62.3(8) . . . . ?
C15 C16 N17 C21 93.7(9) . . . . ?
C15 C16 N17 N18 -89.1(8) . . . . ?
C21 N17 N18 N19 -0.9(9) . . . . ?
C16 N17 N18 N19 -178.6(7) . . . . ?
C21 N17 N18 Na26 160.1(5) . . . 1_565 ?
C16 N17 N18 Na26 -17.5(10) . . . 1_565 ?
N17 N18 N19 N20 -0.5(10) . . . . ?
Na26 N18 N19 N20 -162.8(5) 1_565 . . . ?
N18 N19 N20 C21 1.6(9) . . . . ?
N18 N19 N20 Na26 -176.3(6) . . . 4_566 ?
N18 N17 C21 N20 2.0(8) . . . . ?
C16 N17 C21 N20 179.4(8) . . . . ?
N18 N17 C21 N22 -180.0(6) . . . . ?
C16 N17 C21 N22 -2.5(12) . . . . ?
N19 N20 C21 N17 -2.1(8) . . . . ?
Na26 N20 C21 N17 175.7(5) 4_566 . . . ?
N19 N20 C21 N22 -179.7(9) . . . . ?
Na26 N20 C21 N22 -1.8(14) 4_566 . . . ?
N17 C21 N22 N23 167.2(7) . . . . ?
N20 C21 N22 N23 -15.3(13) . . . . ?
C21 N22 N23 O24 5.3(11) . . . . ?
C21 N22 N23 O25 -172.7(6) . . . . ?
O25 N23 O24 Na26 -155.8(6) . . . 4_566 ?
N22 N23 O24 Na26 26.2(13) . . . 4_566 ?
O24 N23 O25 Na26 -157.0(5) . . . . ?
N22 N23 O25 Na26 21.2(8) . . . . ?
O24 N23 O25 Na26 -42.7(8) . . . 3_757 ?
N22 N23 O25 Na26 135.5(5) . . . 3_757 ?
N27 N28 N29 C30 -173(5) . . . . ?
N28 N29 C30 N40 145.2(8) . . . . ?
N28 N29 C30 C31 -43.9(13) . . . . ?
N40 C30 C31 C35 0.1(8) . . . . ?
N29 C30 C31 C35 -171.4(8) . . . . ?
N40 C30 C31 N32 172.6(7) . . . . ?
N29 C30 C31 N32 1.0(14) . . . . ?
C35 C31 N32 O34 -177.8(8) . . . . ?
C30 C31 N32 O34 11.8(11) . . . . ?
C35 C31 N32 O33 5.0(11) . . . . ?
C30 C31 N32 O33 -165.5(7) . . . . ?
N32 C31 C35 N39 -172.4(7) . . . . ?
C30 C31 C35 N39 -0.1(9) . . . . ?
N32 C31 C35 N36 11.3(14) . . . . ?
C30 C31 C35 N36 -176.3(8) . . . . ?
N39 C35 N36 O37 -127.0(8) . . . . ?
C31 C35 N36 O37 49.3(12) . . . . ?
N39 C35 N36 O38 48.5(10) . . . . ?
C31 C35 N36 O38 -135.2(9) . . . . ?
O37 N36 O38 Na52 -166.7(6) . . . . ?
C35 N36 O38 Na52 18.0(12) . . . . ?
C31 C35 N39 N40 0.0(9) . . . . ?
N36 C35 N39 N40 176.9(6) . . . . ?
N29 C30 N40 N39 173.0(7) . . . . ?
C31 C30 N40 N39 -0.1(8) . . . . ?
N29 C30 N40 C41 1.2(11) . . . . ?
C31 C30 N40 C41 -172.0(7) . . . . ?
C35 N39 N40 C30 0.1(8) . . . . ?
C35 N39 N40 C41 172.8(7) . . . . ?
C30 N40 C41 C42 102.3(9) . . . . ?
N39 N40 C41 C42 -69.1(8) . . . . ?
N40 C41 C42 N43 -69.6(8) . . . . ?
C41 C42 N43 N44 -97.3(7) . . . . ?
C41 C42 N43 C47 93.4(9) . . . . ?
C47 N43 N44 N45 -1.2(8) . . . . ?
C42 N43 N44 N45 -172.4(6) . . . . ?
C47 N43 N44 Na52 158.1(5) . . . 1_545 ?
C42 N43 N44 Na52 -13.1(9) . . . 1_545 ?
N43 N44 N45 N46 0.6(8) . . . . ?
Na52 N44 N45 N46 -161.5(4) 1_545 . . . ?
N43 N44 N45 Na52 148.0(4) . . . 3_655 ?
Na52 N44 N45 Na52 -14.1(6) 1_545 . . 3_655 ?
N44 N45 N46 C47 0.2(8) . . . . ?
Na52 N45 N46 C47 -138.7(5) 3_655 . . . ?
N44 N45 N46 Na52 -172.0(5) . . . 4_566 ?
Na52 N45 N46 Na52 49.1(8) 3_655 . . 4_566 ?
N45 N46 C47 N48 177.4(8) . . . . ?
Na52 N46 C47 N48 -10.5(13) 4_566 . . . ?
N45 N46 C47 N43 -0.9(8) . . . . ?
Na52 N46 C47 N43 171.3(4) 4_566 . . . ?
N44 N43 C47 N46 1.3(8) . . . . ?
C42 N43 C47 N46 171.6(7) . . . . ?
N44 N43 C47 N48 -177.3(6) . . . . ?
C42 N43 C47 N48 -7.0(11) . . . . ?
N46 C47 N48 N49 -12.2(13) . . . . ?
N43 C47 N48 N49 166.0(6) . . . . ?
C47 N48 N49 O50 -170.5(6) . . . . ?
C47 N48 N49 O51 9.3(10) . . . . ?
O51 N49 O50 Na52 -142.3(5) . . . . ?
N48 N49 O50 Na52 37.5(7) . . . . ?
O51 N49 O50 Na52 -35.7(6) . . . 3_665 ?
N48 N49 O50 Na52 144.1(5) . . . 3_665 ?
O50 N49 O51 Na52 -159.5(5) . . . 4_566 ?
N48 N49 O51 Na52 20.7(11) . . . 4_566 ?

_refine_diff_density_max         0.562
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.107

# start Validation Reply Form
_vrf_PLAT015_shrv444             
;
PROBLEM: No _shelx_hkl_file record in SHELXL20xy CIF ....     Please Do ! 
RESPONSE: It is our policy to routinely not supply the HKL file unless 
specifically required.
;
