# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
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# 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 
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data_1DiA2
_database_code_depnum_ccdc_archive 'CCDC 2118273'
loop_
_audit_author_name
_audit_author_address
'Nicholas White'
;Australian National University
Australia
;
_audit_update_record             
;
2021-10-27 deposited with the CCDC.	2021-12-02 downloaded from the CCDC.
;
#==============================================================================
# start Validation Reply Form
_vrf_PLAT230_1DiA2               
;
PROBLEM: Hirshfeld Test Diff for    O12      --C13      .        7.6 s.u.  
RESPONSE: These two atoms are part of the dicarboxylate anion,
which appears to be undergoing some side-to-side motion.
;
_vrf_PLAT250_1DiA2               
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....        6.9 Note  
RESPONSE: The diazobenzenedicarboxylate anion shows elongated ellipsoids in one
direction (orthogonal to the hydrogen bonds), which we attribute to either
thermal motion of the anion or disorder over two slightly different positions.
It was not possible to model this by having more than one position for the 
atoms. Instead, DFIX, DANG, SIMU and DELU restraints were used on this anion
in order to give chemically sensible bond lengths.
;

_refine_special_details          
;Initial datasets were collected for this compound using a home source 
diffractometer. These revealed that the crystals were twinned, and that there
are large void spaces containing several poorly-resolved, partial-occupancy 
water molecules. In an effort to make refinement easier, crystals were taken 
from the crystallisation solvent, mounted using a muCHILL cold-mounting device
at 213 K, and immediately submerged in liquid nitrogen and transported
to the Australian Synchrotron in liquid nitrogen in a dry shipper. The crystals
were kept at liquid nitrogen until data collection (at 100 K). Despite these 
precautions, the numerous water molecules in the structure are still poorly 
resolved and mainly have low occupancies.

A suitable two-component twin law was found and implemented within OLEX2, and 
numerous sites for partial occupancy water molecules identified. It was
possible to achive a somewhat stable refinement using stringent ISOR restraints
for these partial occupancy water molecules, although the diffuse nature of the
electron density meant that the water positions and occupancies were little 
more than a best guess. Due to the poor quality  of this attempted refinement, 
it was decided to incorporate the electron density from the ill-defined water 
molecules in the refinement using PLATON SQUEEZE. When this was done, a far 
superior refinement was achieved, although the dicarboxylate anion was still 
poorly-behaved. It was necessary to use DFIX, DANG, SIMU and DELU
restraints to achieve a sensible refinement of this anion. It is possible that 
the problem with this anion is related to positional disorder about a special
position, but it was not possible to model this.,Twin,SQUEEZE
;

_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C29 H32 N8, 2(C14 H8 N2 O4)'
_chemical_formula_sum            'C57 H48 N12 O8'
_chemical_formula_weight         1029.07
_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'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_H-M_alt        'P 42/n'
_space_group_name_Hall           '-P 4bc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x+1/2, z+1/2'
'-x+1/2, -y+1/2, z'
'y+1/2, -x, z+1/2'
'-x, -y, -z'
'y, -x-1/2, -z-1/2'
'x-1/2, y-1/2, -z'
'-y-1/2, x, -z-1/2'

_cell_length_a                   25.440(4)
_cell_length_b                   25.440(4)
_cell_length_c                   7.3400(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4750.4(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    100
_cell_measurement_reflns_used    64383
_cell_measurement_theta_min      0.800
_cell_measurement_theta_max      26.367

_exptl_crystal_description       rod
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02

_exptl_absorpt_correction_type   None

_diffrn_radiation_type           Synchrotron
_diffrn_radiation_source         'MX2 Beamline Australian Synchrotron'
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_measurement_device_type  'Dectris Eiger 16M'
_diffrn_measurement_method       'Omega Scan'

_computing_data_collection       'AS QEGUI'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_publication_material  'OLEX2 (Dolomanov et al., 2009)'

_diffrn_ambient_temperature      100
_diffrn_reflns_number            64383
_diffrn_reflns_av_R_equivalents  0.0517
_diffrn_reflns_av_unetI/netI     0.0216
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.367
_diffrn_reflns_theta_min         0.800
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.981
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4717
_reflns_number_total             4758

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_reflns_threshold_expression     'I > 2σ(I)'
_refine_diff_density_max         0.256
_refine_diff_density_min         -0.256
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         4758
_refine_ls_number_restraints     93
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0556
_refine_ls_restrained_S_all      1.154
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1246P)²+0.8669P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1808
_refine_ls_wR_factor_ref         0.1811
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?


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
O11 O 0.60202(8) 0.55803(8) 0.8138(3) 0.0713(5) Uani 1 1 d D U . . .
O12 O 0.54684(9) 0.62486(8) 0.7940(2) 0.0722(5) Uani 1 1 d D U . . .
N20 N 0.49532(16) 0.51748(14) 0.0325(3) 0.1115(12) Uani 1 1 d D U . . .
C13 C 0.56792(10) 0.58436(10) 0.7319(3) 0.0651(6) Uani 1 1 d D U . . .
C14 C 0.55107(11) 0.56663(11) 0.5426(3) 0.0718(7) Uani 1 1 d D U . . .
C15 C 0.57048(12) 0.51977(12) 0.4733(4) 0.0830(9) Uani 1 1 d D U . . .
H15 H 0.594667 0.500057 0.539282 0.100 Uiso 1 1 calc R U . . .
C16 C 0.55298(14) 0.50256(14) 0.3016(4) 0.0937(10) Uani 1 1 d D U . . .
H16 H 0.565332 0.471004 0.254083 0.112 Uiso 1 1 calc R U . . .
C17 C 0.51737(15) 0.53246(15) 0.2030(3) 0.0977(10) Uani 1 1 d D U . . .
C18 C 0.50062(17) 0.57804(16) 0.2704(3) 0.0935(9) Uani 1 1 d D U . . .
H18 H 0.477255 0.598604 0.203967 0.112 Uiso 1 1 calc R U . . .
C19 C 0.51821(15) 0.59513(14) 0.4421(3) 0.0846(9) Uani 1 1 d D U . . .
H19 H 0.506531 0.627296 0.486711 0.102 Uiso 1 1 calc R U . . .
N1 N 0.64101(7) 0.59769(7) 0.1446(2) 0.0440(4) Uani 1 1 d . . . . .
H1A H 0.627556 0.583165 0.049655 0.053 Uiso 1 1 calc R U . . .
H1B H 0.665326 0.581842 0.204658 0.053 Uiso 1 1 calc R U . . .
N2 N 0.58731(7) 0.66995(7) 0.1108(2) 0.0450(4) Uani 1 1 d . . . . .
H2A H 0.572979 0.656605 0.015285 0.054 Uiso 1 1 calc R U . . .
H2B H 0.577408 0.700270 0.149617 0.054 Uiso 1 1 calc R U . . .
C1 C 0.65119(6) 0.66993(7) 0.3560(2) 0.0317(3) Uani 1 1 d . . . . .
C2 C 0.65772(7) 0.72437(7) 0.3518(2) 0.0327(4) Uani 1 1 d . . . . .
H2 H 0.641951 0.744241 0.260617 0.039 Uiso 1 1 calc R U . . .
C3 C 0.62447(7) 0.64391(8) 0.1977(2) 0.0378(4) Uani 1 1 d . . . . .
C6 C 0.68789(6) 0.74858(6) 0.4848(2) 0.0288(3) Uani 1 1 d . . . . .
H6 H 0.691832 0.784919 0.482286 0.035 Uiso 1 1 calc R U . . .
C7 C 0.71235(6) 0.71996(6) 0.62138(18) 0.0259(3) Uani 1 1 d . . . . .
C8 C 0.70420(7) 0.66535(6) 0.6287(2) 0.0308(3) Uani 1 1 d . . . . .
H8 H 0.719017 0.645554 0.722053 0.037 Uiso 1 1 calc R U . . .
C9 C 0.67385(7) 0.64118(6) 0.4956(2) 0.0345(4) Uani 1 1 d . . . . .
H9 H 0.668661 0.605021 0.500265 0.041 Uiso 1 1 calc R U . . .
C10 C 0.750000 0.750000 0.750000 0.0256(6) Uani 1 4 d S T P . .


_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
O11 C13 1.250(3) . ?
O12 C13 1.248(3) . ?
N20 N20 1.037(7) 5_665 ?
N20 C17 1.424(3) . ?
C13 C14 1.522(2) . ?
C14 C15 1.387(4) . ?
C14 C19 1.330(5) . ?
C15 H15 0.9300 . ?
C15 C16 1.406(4) . ?
C16 H16 0.9300 . ?
C16 C17 1.387(4) . ?
C17 C18 1.331(6) . ?
C18 H18 0.9300 . ?
C18 C19 1.406(3) . ?
C19 H19 0.9300 . ?
N1 H1A 0.8600 . ?
N1 H1B 0.8600 . ?
N1 C3 1.308(3) . ?
N2 H2A 0.8600 . ?
N2 H2B 0.8600 . ?
N2 C3 1.319(3) . ?
C1 C2 1.395(2) . ?
C1 C3 1.500(2) . ?
C1 C9 1.384(2) . ?
C2 H2 0.9300 . ?
C2 C6 1.386(2) . ?
C6 H6 0.9300 . ?
C6 C7 1.387(2) . ?
C7 C8 1.406(2) . ?
C7 C10 1.5468(14) . ?
C8 H8 0.9300 . ?
C8 C9 1.389(2) . ?
C9 H9 0.9300 . ?

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
N20 N20 C17 122.9(6) 5_665 . ?
O11 C13 C14 118.4(2) . . ?
O12 C13 O11 124.4(2) . . ?
O12 C13 C14 117.2(2) . . ?
C15 C14 C13 119.3(3) . . ?
C19 C14 C13 121.4(3) . . ?
C19 C14 C15 119.3(2) . . ?
C14 C15 H15 120.5 . . ?
C14 C15 C16 118.9(3) . . ?
C16 C15 H15 120.5 . . ?
C15 C16 H16 119.9 . . ?
C17 C16 C15 120.2(3) . . ?
C17 C16 H16 119.9 . . ?
C16 C17 N20 124.7(4) . . ?
C18 C17 N20 115.7(4) . . ?
C18 C17 C16 119.5(3) . . ?
C17 C18 H18 120.0 . . ?
C17 C18 C19 120.1(4) . . ?
C19 C18 H18 120.0 . . ?
C14 C19 C18 121.9(4) . . ?
C14 C19 H19 119.1 . . ?
C18 C19 H19 119.1 . . ?
H1A N1 H1B 120.0 . . ?
C3 N1 H1A 120.0 . . ?
C3 N1 H1B 120.0 . . ?
H2A N2 H2B 120.0 . . ?
C3 N2 H2A 120.0 . . ?
C3 N2 H2B 120.0 . . ?
C2 C1 C3 118.36(15) . . ?
C9 C1 C2 119.42(14) . . ?
C9 C1 C3 121.91(15) . . ?
C1 C2 H2 120.3 . . ?
C6 C2 C1 119.45(15) . . ?
C6 C2 H2 120.3 . . ?
N1 C3 N2 122.52(17) . . ?
N1 C3 C1 118.81(17) . . ?
N2 C3 C1 118.55(17) . . ?
C2 C6 H6 119.2 . . ?
C2 C6 C7 121.62(14) . . ?
C7 C6 H6 119.2 . . ?
C6 C7 C8 118.72(14) . . ?
C6 C7 C10 117.38(12) . . ?
C8 C7 C10 123.79(12) . . ?
C7 C8 H8 120.2 . . ?
C9 C8 C7 119.50(15) . . ?
C9 C8 H8 120.2 . . ?
C1 C9 C8 121.21(14) . . ?
C1 C9 H9 119.4 . . ?
C8 C9 H9 119.4 . . ?
C7 C10 C7 111.87(6) 6_577 . ?
C7 C10 C7 104.77(10) 3_665 . ?
C7 C10 C7 104.77(10) 6_577 8_757 ?
C7 C10 C7 111.87(5) 8_757 . ?
C7 C10 C7 111.87(5) 6_577 3_665 ?
C7 C10 C7 111.87(5) 8_757 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
O11 C13 C14 C15 5.4(3) . . . . ?
O11 C13 C14 C19 -174.5(2) . . . . ?
O12 C13 C14 C15 -175.3(2) . . . . ?
O12 C13 C14 C19 4.8(3) . . . . ?
N20 N20 C17 C16 -0.5(6) 5_665 . . . ?
N20 N20 C17 C18 -178.7(4) 5_665 . . . ?
N20 C17 C18 C19 177.1(3) . . . . ?
C13 C14 C15 C16 177.3(2) . . . . ?
C13 C14 C19 C18 -177.2(2) . . . . ?
C14 C15 C16 C17 0.8(4) . . . . ?
C15 C14 C19 C18 2.9(4) . . . . ?
C15 C16 C17 N20 -176.9(2) . . . . ?
C15 C16 C17 C18 1.2(4) . . . . ?
C16 C17 C18 C19 -1.2(4) . . . . ?
C17 C18 C19 C14 -0.9(5) . . . . ?
C19 C14 C15 C16 -2.8(4) . . . . ?
C1 C2 C6 C7 0.7(2) . . . . ?
C2 C1 C3 N1 143.33(17) . . . . ?
C2 C1 C3 N2 -32.7(2) . . . . ?
C2 C1 C9 C8 -1.8(3) . . . . ?
C2 C6 C7 C8 -2.9(2) . . . . ?
C2 C6 C7 C10 173.40(12) . . . . ?
C3 C1 C2 C6 -172.04(15) . . . . ?
C3 C1 C9 C8 171.64(16) . . . . ?
C6 C7 C8 C9 2.7(2) . . . . ?
C6 C7 C10 C7 -172.42(12) . . . 8_757 ?
C6 C7 C10 C7 -51.02(10) . . . 3_665 ?
C6 C7 C10 C7 70.37(8) . . . 6_577 ?
C7 C8 C9 C1 -0.4(3) . . . . ?
C8 C7 C10 C7 3.63(15) . . . 8_757 ?
C8 C7 C10 C7 125.02(16) . . . 3_665 ?
C8 C7 C10 C7 -113.58(18) . . . 6_577 ?
C9 C1 C2 C6 1.7(2) . . . . ?
C9 C1 C3 N1 -30.2(2) . . . . ?
C9 C1 C3 N2 153.82(17) . . . . ?
C10 C7 C8 C9 -173.34(13) . . . . ?

loop_
_platon_missing_refln_index_h
_platon_missing_refln_index_k
_platon_missing_refln_index_l
_platon_missing_refln_theta
0 0 2 5.557

_platon_squeeze_details          
;
TITL 35_sq_sq_sq_sq_sqP 42/n_sq    R = 0.05
CELL   25.4400   25.4400    7.3400     90.00     90.00     90.00
SPGR P42/n
# Solvent Accessible Volume =      2544
# Electrons Found in S.A.V. =      1073
# Note: Atoms in Void are Labelled as Cxxx and Qxxx for all Others
C101 0.958 0.734 0.254 !       5.55 eA-3
C102 0.447 0.271 0.362 !       4.01 eA-3
C103 0.125 0.953 0.082 !       3.47 eA-3
C104 0.869 0.436 0.619 !       2.94 eA-3
C105 0.307 0.490 0.335 !       2.86 eA-3
C106 0.895 0.334 0.134 !       1.93 eA-3
C107 0.442 0.799 0.193 !       1.79 eA-3
C108 0.968 0.274 0.498 !       1.70 eA-3
C109 0.903 0.191 0.478 !       1.55 eA-3
C110 0.059 0.709 0.342 !       1.43 eA-3
Q111 0.368 0.526 0.257 !       1.41 eA-3
C112 0.639 0.409 0.027 !       1.36 eA-3
C113 0.332 0.755 0.737 !       1.20 eA-3
C114 0.835 0.258 0.359 !       1.17 eA-3
C115 0.623 0.392 0.467 !       1.11 eA-3
C116 0.443 0.712 0.161 !       1.10 eA-3
C117 0.979 0.253 0.323 !       1.06 eA-3
C118 0.689 0.268 0.124 !       1.05 eA-3
C119 0.359 0.779 0.072 !       0.89 eA-3
C120 0.198 0.712 0.409 !       0.88 eA-3
C121 0.586 0.297 0.843 !       0.87 eA-3
C122 0.132 0.647 0.157 !       0.86 eA-3
C123 0.391 0.718-0.003 !       0.85 eA-3
C124 0.789 0.196-0.010 !       0.83 eA-3
C125 0.646 0.263 0.535 !       0.78 eA-3
C126 0.890 0.214 0.620 !       0.75 eA-3
Q127 0.117 0.591 0.750 !       0.75 eA-3
C128 0.821 0.297 0.295 !       0.71 eA-3
C129 0.050 0.749 0.065 !       0.68 eA-3
C130 0.867 0.376 0.299 !       0.67 eA-3
C131 0.834 0.270 0.620 !       0.67 eA-3
C132 0.128 0.618 0.637 !       0.66 eA-3
C133 0.327 0.749 0.292 !       0.65 eA-3
C134 0.400 0.758 0.375 !       0.61 eA-3
Q135 0.858 0.985 0.086 !       0.57 eA-3
C136 0.954 0.228 0.153 !       0.57 eA-3
Q137 0.397 0.306 0.342 !       0.57 eA-3
C138 0.320 0.733 0.382 !       0.55 eA-3
C139 0.130 0.790 0.869 !       0.54 eA-3
C140 0.763 0.365 0.785 !       0.54 eA-3
Q141 0.820 1.000 0.087 !       0.54 eA-3
Q142 0.994 0.675 0.491 !       0.52 eA-3
C143 0.180 0.805 0.320 !       0.52 eA-3
C144 0.205 0.978 0.137 !       0.51 eA-3
C145 0.823 0.429 0.407 !       0.51 eA-3
Q146 0.328 0.951 0.067 !       0.50 eA-3
;
_platon_squeeze_special_details  ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.250 0.250 -0.051 1282 537 ' '
2 0.250 0.750 -0.059 1281 537 ' '

_platon_squeeze_void_probe_radius 1.20

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.568(2)
2 0.432(2)

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Water/ethanol'
_chemical_properties_physical    'Rapidly loses 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_1SB2
_database_code_depnum_ccdc_archive 'CCDC 2118274'
loop_
_audit_author_name
_audit_author_address
'Nicholas White'
;Australian National University
Australia
;
_audit_update_record             
;
2021-10-27 deposited with the CCDC.	2021-12-02 downloaded from the CCDC.
;
#==============================================================================
# start Validation Reply Form
_vrf_PLAT230_1SB2                
;
PROBLEM: Hirshfeld Test Diff for    C16      --C17      .        7.5 s.u.  
RESPONSE: These two carbon atoms are part of the stilbenedicarboxylate anion,
which appears to be undergoing some side-to-side motion.
;
_vrf_PLAT250_1SB2                
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....        4.3 Note  
RESPONSE: The stilbenedicarboxylate anion shows elongated ellipsoids in one
direction (orthogonal to the hydrogen bonds), which we attribute to either
thermal motion of the anion or disorder over two slightly different positions.
It was not possible to model this, but nevertheless, the geometry and thermal
ellipsoids of this group refine sensibly without any restraints.
;

_refine_special_details          
;Initial datasets were collected for this compound using a home source 
diffractometer. These revealed that the crystals were twinned, and that there
are large void spaces containing several poorly-resolved, partial-occupancy 
water molecules. In an effort to make refinement easier, crystals were taken 
from the crystallisation solvent, mounted using a muCHILL cold-mounting device
at 213 K, and immediately submerged in liquid nitrogen and transported
to the Australian Synchrotron in liquid nitrogen in a dry shipper. The crystals
were kept at liquid nitrogen until data collection (at 100 K). Despite these 
precautions, the numerous water molecules in the structure are still very 
pooly resolved.

A suitable two-component twin law was found and implemented within OLEX2, and 
numerous sites for partial occupancy water molecules identified. It was
possible to achive a somewhat stable refinement using stringent ISOR restraints
for these partial occupancy water molecules, although the diffuse nature of the
electron density meant that the water positions and occupancies were little 
more than a best guess, and the poor refinement of this part of the molecule
meant that it was necessary to add DFIX, SIMU and DELU restraints to the 
dicarboxylate anion to achieve a sensible refinement. Due to the poor quality 
of this attempted refinement, it was decided to incorporate the electron 
density from the ill-defined water molecules in the refinement using PLATON
SQUEEZE. When this was done, a far superior refinement was achieved, and 
no crystallographic restraints were necessary.,Twin,SQUEEZE
;

_audit_creation_date             2021-08-30
_audit_creation_method           
;
Olex2 1.5-alpha
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6392)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C29 H32 N8, 2(C16 H10 O4)'
_chemical_formula_sum            'C61 H52 N8 O8'
_chemical_formula_weight         1025.10

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'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_H-M_alt        'P 42/n'
_space_group_name_Hall           '-P 4bc'

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x+1/2, z+1/2'
'-x+1/2, -y+1/2, z'
'y+1/2, -x, z+1/2'
'-x, -y, -z'
'y, -x-1/2, -z-1/2'
'x-1/2, y-1/2, -z'
'-y-1/2, x, -z-1/2'

_cell_length_a                   25.779(4)
_cell_length_b                   25.779(4)
_cell_length_c                   7.4300(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4937.7(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    100
_cell_measurement_reflns_used    65639
_cell_measurement_theta_max      26.373
_cell_measurement_theta_min      0.790

_exptl_crystal_description       rod
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02

_exptl_absorpt_correction_type   None

_diffrn_radiation_type           Synchrotron
_diffrn_radiation_source         'MX2 Beamline Australian Synchrotron'
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_measurement_device_type  'Dectris Eiger 16M'
_diffrn_measurement_method       'Omega Scan'

_computing_data_collection       'AS QEGUI'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_publication_material  'OLEX2 (Dolomanov et al., 2009)'

_diffrn_reflns_av_R_equivalents  0.0877
_diffrn_reflns_av_unetI/netI     0.0372
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            65639
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         0.790
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.958
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4745
_reflns_number_total             4846
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_refine_diff_density_max         0.241
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         4846
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0647
_refine_ls_restrained_S_all      1.147
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1432P)²+0.2761P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1922
_refine_ls_wR_factor_ref         0.1934

_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.569(2)
 0.431(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C5(H5), C6(H6), C8(H8),
 C9(H9)
3.b X=CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B)
;

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

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
O11 O 0.36858(8) 0.45062(7) -0.2974(2) 0.0733(5) Uani 1 1 d . . . . .
O12 O 0.43328(8) 0.39319(7) -0.3132(2) 0.0671(5) Uani 1 1 d . . . . .
C13 C 0.40905(10) 0.42921(9) -0.2357(3) 0.0620(6) Uani 1 1 d . . . . .
C14 C 0.42837(10) 0.44670(9) -0.0507(3) 0.0617(6) Uani 1 1 d . . . . .
C15 C 0.47460(12) 0.43217(11) 0.0135(4) 0.0724(7) Uani 1 1 d . . . . .
H15 H 0.495368 0.410081 -0.054276 0.087 Uiso 1 1 calc R U . . .
C16 C 0.49226(11) 0.44959(11) 0.1808(4) 0.0711(7) Uani 1 1 d . . . . .
H16 H 0.524239 0.438408 0.223763 0.085 Uiso 1 1 calc R U . . .
C17 C 0.46298(13) 0.48292(12) 0.2820(3) 0.0807(9) Uani 1 1 d . . . . .
C18 C 0.41439(13) 0.49750(13) 0.2169(4) 0.0825(9) Uani 1 1 d . . . . .
H18 H 0.393050 0.518838 0.285499 0.099 Uiso 1 1 calc R U . . .
C19 C 0.39794(12) 0.48013(13) 0.0499(3) 0.0777(8) Uani 1 1 d . . . . .
H19 H 0.366106 0.491060 0.004817 0.093 Uiso 1 1 calc R U . . .
C20 C 0.47876(15) 0.50362(14) 0.4575(4) 0.0848(9) Uani 1 1 d . . . . .
H20 H 0.454640 0.524823 0.514525 0.102 Uiso 1 1 calc R U . . .
N1 N 0.32617(7) 0.40940(7) 0.3919(2) 0.0504(4) Uani 1 1 d . . . . .
H1A H 0.339696 0.423047 0.486481 0.060 Uiso 1 1 calc R U . . .
H1B H 0.295733 0.418718 0.357254 0.060 Uiso 1 1 calc R U . . .
N2 N 0.39867(6) 0.35909(7) 0.3491(2) 0.0485(4) Uani 1 1 d . . . . .
H2A H 0.412695 0.372401 0.443420 0.058 Uiso 1 1 calc R U . . .
H2B H 0.415124 0.336084 0.287714 0.058 Uiso 1 1 calc R U . . .
C3 C 0.35236(8) 0.37385(7) 0.2990(2) 0.0444(4) Uani 1 1 d . . . . .
C4 C 0.32739(7) 0.34794(6) 0.1424(2) 0.0389(3) Uani 1 1 d . . . . .
C5 C 0.27365(6) 0.34085(6) 0.1461(2) 0.0378(3) Uani 1 1 d . . . . .
H5 H 0.253877 0.356111 0.236423 0.045 Uiso 1 1 calc R U . . .
C6 C 0.25002(6) 0.31108(6) 0.01496(19) 0.0338(3) Uani 1 1 d . . . . .
H6 H 0.214251 0.306487 0.018306 0.041 Uiso 1 1 calc R U . . .
C7 C 0.27884(6) 0.28758(5) -0.12334(18) 0.0317(3) Uani 1 1 d . . . . .
C8 C 0.33222(6) 0.29697(6) -0.1306(2) 0.0377(3) Uani 1 1 d . . . . .
H8 H 0.351865 0.283205 -0.224095 0.045 Uiso 1 1 calc R U . . .
C9 C 0.35621(6) 0.32712(7) 0.0028(2) 0.0404(3) Uani 1 1 d . . . . .
H9 H 0.391742 0.333155 -0.002647 0.048 Uiso 1 1 calc R U . . .
C10 C 0.250000 0.250000 -0.250000 0.0320(6) Uani 1 4 d S T P . .


_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
O11 C13 1.266(3) . ?
O12 C13 1.258(3) . ?
C13 C14 1.530(3) . ?
C14 C15 1.337(4) . ?
C14 C19 1.384(4) . ?
C15 H15 0.9300 . ?
C15 C16 1.397(3) . ?
C16 H16 0.9300 . ?
C16 C17 1.369(5) . ?
C17 C18 1.394(5) . ?
C17 C20 1.467(4) . ?
C18 H18 0.9300 . ?
C18 C19 1.386(3) . ?
C19 H19 0.9300 . ?
C20 C20 1.278(7) 5_666 ?
C20 H20 0.9300 . ?
N1 H1A 0.8600 . ?
N1 H1B 0.8600 . ?
N1 C3 1.331(3) . ?
N2 H2A 0.8600 . ?
N2 H2B 0.8600 . ?
N2 C3 1.307(3) . ?
C3 C4 1.488(2) . ?
C4 C5 1.398(2) . ?
C4 C9 1.384(2) . ?
C5 H5 0.9300 . ?
C5 C6 1.382(2) . ?
C6 H6 0.9300 . ?
C6 C7 1.405(2) . ?
C7 C8 1.398(2) . ?
C7 C10 1.5417(14) . ?
C8 H8 0.9300 . ?
C8 C9 1.403(2) . ?
C9 H9 0.9300 . ?

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
O11 C13 C14 117.7(2) . . ?
O12 C13 O11 124.41(19) . . ?
O12 C13 C14 117.8(2) . . ?
C15 C14 C13 121.9(3) . . ?
C15 C14 C19 119.1(2) . . ?
C19 C14 C13 119.0(2) . . ?
C14 C15 H15 119.4 . . ?
C14 C15 C16 121.2(3) . . ?
C16 C15 H15 119.4 . . ?
C15 C16 H16 119.7 . . ?
C17 C16 C15 120.7(3) . . ?
C17 C16 H16 119.7 . . ?
C16 C17 C18 118.3(2) . . ?
C16 C17 C20 124.3(3) . . ?
C18 C17 C20 117.4(3) . . ?
C17 C18 H18 120.1 . . ?
C19 C18 C17 119.9(3) . . ?
C19 C18 H18 120.1 . . ?
C14 C19 C18 120.7(3) . . ?
C14 C19 H19 119.6 . . ?
C18 C19 H19 119.6 . . ?
C17 C20 H20 115.7 . . ?
C20 C20 C17 128.6(5) 5_666 . ?
C20 C20 H20 115.7 5_666 . ?
H1A N1 H1B 120.0 . . ?
C3 N1 H1A 120.0 . . ?
C3 N1 H1B 120.0 . . ?
H2A N2 H2B 120.0 . . ?
C3 N2 H2A 120.0 . . ?
C3 N2 H2B 120.0 . . ?
N1 C3 C4 119.67(17) . . ?
N2 C3 N1 121.05(16) . . ?
N2 C3 C4 119.16(17) . . ?
C5 C4 C3 118.19(15) . . ?
C9 C4 C3 121.86(15) . . ?
C9 C4 C5 119.73(14) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 C4 119.72(15) . . ?
C6 C5 H5 120.1 . . ?
C5 C6 H6 119.3 . . ?
C5 C6 C7 121.47(14) . . ?
C7 C6 H6 119.3 . . ?
C6 C7 C10 117.53(11) . . ?
C8 C7 C6 118.29(13) . . ?
C8 C7 C10 124.04(12) . . ?
C7 C8 H8 119.9 . . ?
C7 C8 C9 120.16(14) . . ?
C9 C8 H8 119.9 . . ?
C4 C9 C8 120.50(14) . . ?
C4 C9 H9 119.7 . . ?
C8 C9 H9 119.7 . . ?
C7 C10 C7 111.88(5) . 8_655 ?
C7 C10 C7 111.88(5) 8_655 3 ?
C7 C10 C7 104.76(10) . 3 ?
C7 C10 C7 111.88(5) . 6_565 ?
C7 C10 C7 111.88(5) 6_565 3 ?
C7 C10 C7 104.76(10) 8_655 6_565 ?

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
O11 C13 C14 C15 -169.9(2) . . . . ?
O11 C13 C14 C19 7.6(3) . . . . ?
O12 C13 C14 C15 12.8(3) . . . . ?
O12 C13 C14 C19 -169.8(2) . . . . ?
C13 C14 C15 C16 178.3(2) . . . . ?
C13 C14 C19 C18 -179.1(2) . . . . ?
C14 C15 C16 C17 -1.3(4) . . . . ?
C15 C14 C19 C18 -1.5(4) . . . . ?
C15 C16 C17 C18 2.3(4) . . . . ?
C15 C16 C17 C20 -179.2(2) . . . . ?
C16 C17 C18 C19 -2.9(4) . . . . ?
C16 C17 C20 C20 2.5(6) . . . 5_666 ?
C17 C18 C19 C14 2.6(4) . . . . ?
C18 C17 C20 C20 -179.0(4) . . . 5_666 ?
C19 C14 C15 C16 0.8(3) . . . . ?
C20 C17 C18 C19 178.5(3) . . . . ?
N1 C3 C4 C5 -31.0(2) . . . . ?
N1 C3 C4 C9 154.55(17) . . . . ?
N2 C3 C4 C5 145.15(17) . . . . ?
N2 C3 C4 C9 -29.3(2) . . . . ?
C3 C4 C5 C6 -171.56(14) . . . . ?
C3 C4 C9 C8 171.47(16) . . . . ?
C4 C5 C6 C7 -0.1(2) . . . . ?
C5 C4 C9 C8 -2.9(2) . . . . ?
C5 C6 C7 C8 -2.9(2) . . . . ?
C5 C6 C7 C10 173.00(12) . . . . ?
C6 C7 C8 C9 3.0(2) . . . . ?
C6 C7 C10 C7 -171.66(11) . . . 6_565 ?
C6 C7 C10 C7 71.14(8) . . . 8_655 ?
C6 C7 C10 C7 -50.26(9) . . . 3 ?
C7 C8 C9 C4 -0.2(2) . . . . ?
C8 C7 C10 C7 125.42(16) . . . 3 ?
C8 C7 C10 C7 -113.17(17) . . . 8_655 ?
C8 C7 C10 C7 4.02(14) . . . 6_565 ?
C9 C4 C5 C6 3.0(2) . . . . ?
C10 C7 C8 C9 -172.62(12) . . . . ?

loop_
_platon_missing_refln_index_h
_platon_missing_refln_index_k
_platon_missing_refln_index_l
_platon_missing_refln_theta
1 1 0 1.117
2 2 0 2.235
0 0 2 5.489

_platon_squeeze_details          
;
TITL 42_sq_sq_sq_sq_sqP 42/n       R = 0.06
CELL   25.7790   25.7790    7.4300     90.00     90.00     90.00
SPGR P42/n
# Solvent Accessible Volume =      2673
# Electrons Found in S.A.V. =       727
# Note: Atoms in Void are Labelled as Cxxx and Qxxx for all Others
C101 0.265 0.045 0.243 !       4.80 eA-3
C102 0.765 0.945 0.133 !       3.90 eA-3
C103 0.811 0.510 0.339 !       3.05 eA-3
Q104 0.053 0.649 0.154 !       2.90 eA-3
C105 0.826 0.097 0.004 !       1.43 eA-3
C106 0.039 0.862 0.373 !       1.39 eA-3
C107 0.816 0.279-0.001 !       1.11 eA-3
C108 0.055 0.844 0.517 !       1.03 eA-3
C109 0.721 0.305 0.391 !       1.01 eA-3
C110 0.957 0.202 0.081 !       0.93 eA-3
C111 0.118 0.879 0.879 !       0.93 eA-3
C112 0.658 0.102 0.341 !       0.92 eA-3
C113 0.446 0.784 0.806 !       0.87 eA-3
C114 0.299 0.945 0.198 !       0.84 eA-3
C115 0.407 0.798 0.903 !       0.80 eA-3
C116 0.243 0.654 0.859 !       0.79 eA-3
C117 0.510 0.271 0.492 !       0.75 eA-3
C118 0.680 0.225 0.669 !       0.73 eA-3
C119 0.893 0.283 0.030 !       0.73 eA-3
C120 0.733 0.061 0.783 !       0.72 eA-3
C121 0.738 0.172 0.245 !       0.72 eA-3
C122 0.086 0.831 0.044 !       0.72 eA-3
C123 0.207 0.659 0.217 !       0.68 eA-3
C124 0.244 0.539 0.470 !       0.67 eA-3
C125 0.356 0.710 0.885 !       0.65 eA-3
C126 0.645 0.280 0.174 !       0.64 eA-3
C127 0.711 0.203 0.371 !       0.64 eA-3
Q128 0.582 0.089 0.096 !       0.62 eA-3
Q129 0.616 0.414 0.742 !       0.60 eA-3
C130 0.329 0.788 0.558 !       0.59 eA-3
C131 0.298 0.838 0.836 !       0.57 eA-3
C132 0.740 0.306 0.007 !       0.56 eA-3
C133 0.647 0.374 0.746 !       0.56 eA-3
Q134 0.906 0.420 0.338 !       0.56 eA-3
C135 0.547 0.239 0.398 !       0.56 eA-3
Q136 0.093 0.557 0.783 !       0.56 eA-3
Q137 0.909 0.752 0.103 !       0.55 eA-3
C138 0.620 0.084 0.841 !       0.55 eA-3
C139 0.198 0.858 0.216 !       0.54 eA-3
;
_platon_squeeze_special_details  ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.250 0.250 -0.055 1346 370 ' '
2 0.250 0.750 -0.049 1346 370 ' '

_platon_squeeze_void_probe_radius 1.20

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.569(2)
2 0.431(2)

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Water/ethanol'
_chemical_properties_physical    'Rapidly loses solvent'
