# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_d8v19708
_database_code_depnum_ccdc_archive 'CCDC 1978629'
loop_
_audit_author_name
_audit_author_address
'DONG CHEN'
;China Academy of Engineering Physics
China
;
_audit_update_record             
;
2020-01-18 deposited with the CCDC.	2020-03-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            DMA-BTO
_chemical_melting_point          ?
_chemical_formula_moiety         '[NH2(CH3)2+][C2HO2N8-]'
_chemical_formula_sum            'C4 H9 N9 O2'
_chemical_formula_weight         215.20

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      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

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

_cell_length_a                   11.6746(5)
_cell_length_b                   8.8149(3)
_cell_length_c                   18.1710(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1869.99(13)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3691
_cell_measurement_theta_min      5.682
_cell_measurement_theta_max      54.553

_exptl_crystal_description       prismatic
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_F_000             896
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    0.125
_shelx_estimated_absorpt_T_min   0.977
_shelx_estimated_absorpt_T_max   0.986
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5564
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8575
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.841
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             1825
_reflns_number_gt                1516
_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0437P)²+0.4672P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.049(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1825
_refine_ls_number_parameters     151
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0385
_refine_ls_wR_factor_ref         0.1032
_refine_ls_wR_factor_gt          0.0952
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.000
_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
O1 O 0.15622(9) 0.50666(13) 0.49677(7) 0.0480(3) Uani 1 1 d D . . . .
O2 O 0.57016(8) 0.73969(13) 0.49337(6) 0.0430(3) Uani 1 1 d . . . . .
N1 N 0.24435(10) 0.52510(14) 0.44976(7) 0.0368(3) Uani 1 1 d . . . . .
N2 N 0.23948(12) 0.47078(17) 0.38112(8) 0.0501(4) Uani 1 1 d . . . . .
N3 N 0.33705(12) 0.50309(16) 0.35164(8) 0.0505(4) Uani 1 1 d . . . . .
N4 N 0.40580(11) 0.57791(15) 0.39963(7) 0.0403(3) Uani 1 1 d . . . . .
N5 N 0.48373(10) 0.72500(14) 0.53987(7) 0.0335(3) Uani 1 1 d . . . . .
N6 N 0.48994(12) 0.77672(17) 0.60881(7) 0.0468(4) Uani 1 1 d . . . . .
N7 N 0.39233(13) 0.74377(19) 0.63925(8) 0.0551(4) Uani 1 1 d . . . . .
N8 N 0.32326(12) 0.67060(17) 0.59175(7) 0.0479(4) Uani 1 1 d . . . . .
N9 N 0.60598(12) 0.73454(17) 0.33849(7) 0.0411(4) Uani 1 1 d . . . . .
C1 C 0.34616(12) 0.59042(15) 0.46126(8) 0.0320(3) Uani 1 1 d . . . . .
C2 C 0.38200(12) 0.65989(16) 0.52951(8) 0.0329(3) Uani 1 1 d . . . . .
C3 C 0.65034(17) 0.6473(2) 0.27539(10) 0.0621(5) Uani 1 1 d . . . . .
H3A H 0.5878 0.6178 0.2442 0.093 Uiso 1 1 calc R U . . .
H3B H 0.6891 0.5583 0.2929 0.093 Uiso 1 1 calc R U . . .
H3C H 0.7030 0.7090 0.2480 0.093 Uiso 1 1 calc R U . . .
C4 C 0.53866(17) 0.8676(2) 0.31617(11) 0.0614(5) Uani 1 1 d . . . . .
H4A H 0.5860 0.9348 0.2878 0.092 Uiso 1 1 calc R U . . .
H4B H 0.5114 0.9195 0.3592 0.092 Uiso 1 1 calc R U . . .
H4C H 0.4747 0.8354 0.2869 0.092 Uiso 1 1 calc R U . . .
H9A H 0.6659(18) 0.763(2) 0.3652(11) 0.063(6) Uiso 1 1 d . . . . .
H9B H 0.5599(18) 0.677(2) 0.3669(12) 0.069(6) Uiso 1 1 d . . . . .
H1 H 0.1215(19) 0.599(2) 0.4989(13) 0.100(9) Uiso 1 1 d 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
O1 N1 1.3471(16) . ?
O1 H1 0.906(16) . ?
O2 N5 1.3224(15) . ?
N1 N2 1.337(2) . ?
N1 C1 1.3371(18) . ?
N2 N3 1.291(2) . ?
N3 N4 1.3562(18) . ?
N4 C1 1.3233(18) . ?
N5 C2 1.3325(18) . ?
N5 N6 1.3351(18) . ?
N6 N7 1.2997(19) . ?
N7 N8 1.346(2) . ?
N8 C2 1.3260(18) . ?
N9 C4 1.469(2) . ?
N9 C3 1.474(2) . ?
N9 H9A 0.89(2) . ?
N9 H9B 0.90(2) . ?
C1 C2 1.445(2) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?

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 O1 H1 105.1(15) . . ?
N2 N1 C1 109.74(12) . . ?
N2 N1 O1 121.05(12) . . ?
C1 N1 O1 129.18(13) . . ?
N3 N2 N1 105.69(12) . . ?
N2 N3 N4 111.28(13) . . ?
C1 N4 N3 105.86(12) . . ?
O2 N5 C2 129.20(12) . . ?
O2 N5 N6 121.64(12) . . ?
C2 N5 N6 109.15(12) . . ?
N7 N6 N5 105.99(13) . . ?
N6 N7 N8 111.07(13) . . ?
C2 N8 N7 105.74(13) . . ?
C4 N9 C3 112.93(14) . . ?
C4 N9 H9A 110.3(13) . . ?
C3 N9 H9A 107.2(13) . . ?
C4 N9 H9B 106.8(13) . . ?
C3 N9 H9B 111.1(13) . . ?
H9A N9 H9B 108.4(19) . . ?
N4 C1 N1 107.43(13) . . ?
N4 C1 C2 127.54(13) . . ?
N1 C1 C2 125.03(13) . . ?
N8 C2 N5 108.05(13) . . ?
N8 C2 C1 127.77(13) . . ?
N5 C2 C1 124.18(13) . . ?
N9 C3 H3A 109.5 . . ?
N9 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N9 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N9 C4 H4A 109.5 . . ?
N9 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N9 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?

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
C1 N1 N2 N3 -0.05(17) . . . . ?
O1 N1 N2 N3 -178.25(13) . . . . ?
N1 N2 N3 N4 -0.13(18) . . . . ?
N2 N3 N4 C1 0.26(17) . . . . ?
O2 N5 N6 N7 -179.69(13) . . . . ?
C2 N5 N6 N7 -0.46(17) . . . . ?
N5 N6 N7 N8 0.54(19) . . . . ?
N6 N7 N8 C2 -0.41(19) . . . . ?
N3 N4 C1 N1 -0.28(16) . . . . ?
N3 N4 C1 C2 179.25(14) . . . . ?
N2 N1 C1 N4 0.22(16) . . . . ?
O1 N1 C1 N4 178.22(13) . . . . ?
N2 N1 C1 C2 -179.33(13) . . . . ?
O1 N1 C1 C2 -1.3(2) . . . . ?
N7 N8 C2 N5 0.11(17) . . . . ?
N7 N8 C2 C1 179.80(15) . . . . ?
O2 N5 C2 N8 179.37(13) . . . . ?
N6 N5 C2 N8 0.22(16) . . . . ?
O2 N5 C2 C1 -0.3(2) . . . . ?
N6 N5 C2 C1 -179.49(13) . . . . ?
N4 C1 C2 N8 -178.84(14) . . . . ?
N1 C1 C2 N8 0.6(2) . . . . ?
N4 C1 C2 N5 0.8(2) . . . . ?
N1 C1 C2 N5 -179.74(13) . . . . ?

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
N9 H9A N7 0.89(2) 2.65(2) 3.373(2) 139.9(17) 4_566
N9 H9A N8 0.89(2) 2.08(2) 2.956(2) 168.8(19) 4_566
N9 H9B O2 0.90(2) 2.37(2) 2.8456(18) 113.2(15) .
N9 H9B N4 0.90(2) 2.09(2) 2.933(2) 155.9(18) .
O1 H1 O2 0.906(16) 1.554(17) 2.4578(16) 175(2) 4_466
O1 H1 N5 0.906(16) 2.346(18) 3.1770(16) 152(2) 4_466

_refine_diff_density_max         0.148
_refine_diff_density_min         -0.166
_refine_diff_density_rms         0.033

_shelxl_version_number           2013-4


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: DMAC'
####################################################################### 
# 
# 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_mo_d8v19707_0m
_database_code_depnum_ccdc_archive 'CCDC 1978631'
loop_
_audit_author_name
_audit_author_address
'DONG CHEN'
;China Academy of Engineering Physics
China
;
_audit_update_record             
;
2020-01-18 deposited with the CCDC.	2020-03-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            DEA-BTO
_chemical_melting_point          ?
_chemical_formula_moiety         '[NH2(CH3CH2) 2+]2[C2O2N8 2 -]'
_chemical_formula_sum            'C10 H24 N10 O2'
_chemical_formula_weight         316.39

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           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

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

_cell_length_a                   8.3308(10)
_cell_length_b                   12.0024(16)
_cell_length_c                   9.2986(12)
_cell_angle_alpha                90
_cell_angle_beta                 105.393(3)
_cell_angle_gamma                90
_cell_volume                     896.4(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3997
_cell_measurement_theta_min      4.103
_cell_measurement_theta_max      52.620

_exptl_crystal_description       prismatic
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_F_000             340
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.070
_exptl_absorpt_coefficient_mu    0.087
_shelx_estimated_absorpt_T_min   0.984
_shelx_estimated_absorpt_T_max   0.994
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6212
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7344
_diffrn_reflns_av_unetI/netI     0.0192
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.052
_diffrn_reflns_theta_max         25.996
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             924
_reflns_number_gt                776
_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0604P)²+0.2653P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.028(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         924
_refine_ls_number_parameters     88
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0402
_refine_ls_wR_factor_ref         0.1183
_refine_ls_wR_factor_gt          0.1111
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_restrained_S_all      1.083
_refine_ls_shift/su_max          0.000
_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
O1 O 0.67679(15) 0.5000 0.44283(16) 0.0774(6) Uani 1 2 d S T P . .
N1 N 0.79047(18) 0.5000 0.36931(17) 0.0495(5) Uani 1 2 d S T P . .
N2 N 0.7513(2) 0.5000 0.22000(18) 0.0579(5) Uani 1 2 d S T P . .
N3 N 0.8927(2) 0.5000 0.18374(19) 0.0631(6) Uani 1 2 d S T P . .
N4 N 1.02173(19) 0.5000 0.30648(18) 0.0586(5) Uani 1 2 d S T P . .
C1 C 0.9564(2) 0.5000 0.4218(2) 0.0445(5) Uani 1 2 d S T P . .
N5 N 0.3575(2) 0.5000 0.26156(19) 0.0511(5) Uani 1 2 d S T P . .
C2 C 0.3276(3) 0.39731(18) 0.1708(2) 0.0790(6) Uani 1 1 d . . . . .
C3 C 0.3585(5) 0.2970(2) 0.2680(5) 0.1214(11) Uani 1 1 d . . . . .
H5A H 0.296(3) 0.5000 0.327(3) 0.065(7) Uiso 1 2 d S . P . .
H2A H 0.210(3) 0.3968(18) 0.113(3) 0.102(7) Uiso 1 1 d . . . . .
H5B H 0.473(3) 0.5000 0.321(3) 0.062(6) Uiso 1 2 d S . P . .
H2B H 0.406(3) 0.394(2) 0.108(3) 0.108(7) Uiso 1 1 d . . . . .
H3A H 0.478(5) 0.298(3) 0.329(4) 0.149(11) Uiso 1 1 d . . . . .
H3B H 0.346(4) 0.228(3) 0.201(4) 0.164(12) Uiso 1 1 d . . . . .
H3C H 0.290(5) 0.297(4) 0.332(5) 0.185(18) 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
O1 N1 1.307(2) . ?
N1 C1 1.338(2) . ?
N1 N2 1.339(2) . ?
N2 N3 1.309(2) . ?
N3 N4 1.344(2) . ?
N4 C1 1.325(2) . ?
C1 C1 1.443(4) 5_766 ?
N5 C2 1.477(2) 6_565 ?
N5 C2 1.477(2) . ?
N5 H5A 0.89(2) . ?
N5 H5B 0.97(2) . ?
C2 C3 1.487(4) . ?
C2 H2A 0.98(2) . ?
C2 H2B 0.99(2) . ?
C3 H3A 1.00(4) . ?
C3 H3B 1.02(4) . ?
C3 H3C 0.93(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 N1 C1 129.13(16) . . ?
O1 N1 N2 122.09(14) . . ?
C1 N1 N2 108.78(15) . . ?
N3 N2 N1 106.18(15) . . ?
N2 N3 N4 110.66(16) . . ?
C1 N4 N3 106.25(15) . . ?
N4 C1 N1 108.13(16) . . ?
N4 C1 C1 127.67(19) . 5_766 ?
N1 C1 C1 124.2(2) . 5_766 ?
C2 N5 C2 113.1(2) 6_565 . ?
C2 N5 H5A 110.3(7) 6_565 . ?
C2 N5 H5A 110.3(7) . . ?
C2 N5 H5B 108.5(6) 6_565 . ?
C2 N5 H5B 108.5(6) . . ?
H5A N5 H5B 106(2) . . ?
N5 C2 C3 110.7(2) . . ?
N5 C2 H2A 108.0(13) . . ?
C3 C2 H2A 108.3(13) . . ?
N5 C2 H2B 109.8(14) . . ?
C3 C2 H2B 106.9(14) . . ?
H2A C2 H2B 113(2) . . ?
C2 C3 H3A 108.6(18) . . ?
C2 C3 H3B 108.2(19) . . ?
H3A C3 H3B 106(2) . . ?
C2 C3 H3C 110(3) . . ?
H3A C3 H3C 109(3) . . ?
H3B C3 H3C 114(3) . . ?

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
O1 N1 N2 N3 180.000(0) . . . . ?
C1 N1 N2 N3 0.000(0) . . . . ?
N1 N2 N3 N4 0.000(0) . . . . ?
N2 N3 N4 C1 0.000(0) . . . . ?
N3 N4 C1 N1 0.000(0) . . . . ?
N3 N4 C1 C1 180.000(0) . . . 5_766 ?
O1 N1 C1 N4 180.000(0) . . . . ?
N2 N1 C1 N4 0.000(0) . . . . ?
O1 N1 C1 C1 0.000(1) . . . 5_766 ?
N2 N1 C1 C1 180.000(0) . . . 5_766 ?
C2 N5 C2 C3 -179.6(2) 6_565 . . . ?

_refine_diff_density_max         0.221
_refine_diff_density_min         -0.100
_refine_diff_density_rms         0.026

_shelxl_version_number           2013-4


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: DEF'
####################################################################### 
# 
# 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_mo_d8v19308_0m
_database_code_depnum_ccdc_archive 'CCDC 1978633'
loop_
_audit_author_name
_audit_author_address
'DONG CHEN'
;China Academy of Engineering Physics
China
;
_audit_update_record             
;
2020-01-18 deposited with the CCDC.	2020-03-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '[NH(CH3CCH3)OH+] [C2HO2N4-].H2O'
_chemical_formula_sum            'C5 H11 N9 O4'
_chemical_formula_weight         261.23

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      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                   6.8110(5)
_cell_length_b                   7.3961(5)
_cell_length_c                   11.6431(9)
_cell_angle_alpha                73.627(2)
_cell_angle_beta                 82.716(2)
_cell_angle_gamma                83.323(2)
_cell_volume                     556.19(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4209
_cell_measurement_theta_min      5.762
_cell_measurement_theta_max      54.810

_exptl_crystal_description       prismatic
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_F_000             272
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.133
_shelx_estimated_absorpt_T_min   0.976
_shelx_estimated_absorpt_T_max   0.987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6551
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7339
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.881
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             2180
_reflns_number_gt                1758
_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0464P)²+0.1891P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       ?
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2180
_refine_ls_number_parameters     208
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0422
_refine_ls_wR_factor_ref         0.1103
_refine_ls_wR_factor_gt          0.1001
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.075
_refine_ls_shift/su_max          0.000
_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
O1 O 0.7706(3) 0.51003(17) 0.60577(12) 0.0625(5) Uani 1 1 d . . . . .
O2 O 0.8007(3) 1.23025(17) 0.53324(12) 0.0553(4) Uani 1 1 d D . . . .
N1 N 0.7433(2) 0.66422(19) 0.51479(13) 0.0387(4) Uani 1 1 d . . . . .
N2 N 0.7172(3) 0.6576(2) 0.40465(14) 0.0475(4) Uani 1 1 d . . . . .
N3 N 0.6979(3) 0.8326(2) 0.33983(14) 0.0491(4) Uani 1 1 d . . . . .
N4 N 0.7118(2) 0.9515(2) 0.40668(13) 0.0426(4) Uani 1 1 d . . . . .
N5 N 0.7904(2) 1.07596(19) 0.62465(13) 0.0369(4) Uani 1 1 d . . . . .
N6 N 0.8094(3) 1.0765(2) 0.73719(14) 0.0464(4) Uani 1 1 d . . . . .
N7 N 0.7951(3) 0.9030(2) 0.80242(14) 0.0491(4) Uani 1 1 d . . . . .
N8 N 0.7681(2) 0.7911(2) 0.73360(13) 0.0422(4) Uani 1 1 d . . . . .
C1 C 0.7406(3) 0.8438(2) 0.51662(15) 0.0329(4) Uani 1 1 d . . . . .
C2 C 0.7658(2) 0.9012(2) 0.62219(14) 0.0322(4) Uani 1 1 d . . . . .
H2 H 0.794(5) 1.336(4) 0.565(3) 0.125(12) Uiso 1 1 d D . . . .
O3 O 0.4604(2) 0.4254(2) 0.89037(13) 0.0598(4) Uani 1 1 d D . . . .
N9 N 0.6609(2) 0.4347(2) 0.87076(13) 0.0408(4) Uani 1 1 d . . . . .
C3 C 0.7783(3) 0.3113(2) 0.93344(15) 0.0398(5) Uani 1 1 d . . . . .
C4 C 0.9928(4) 0.3343(4) 0.9047(2) 0.0592(6) Uani 1 1 d . . . . .
C5 C 0.7035(5) 0.1496(3) 1.0290(2) 0.0576(6) Uani 1 1 d . . . . .
H5A H 0.776(5) 0.131(4) 1.094(3) 0.096(10) Uiso 1 1 d . . . . .
H5B H 0.722(5) 0.040(5) 1.001(3) 0.110(11) Uiso 1 1 d . . . . .
H5C H 0.570(5) 0.176(4) 1.050(3) 0.088(10) Uiso 1 1 d . . . . .
H4A H 1.017(4) 0.464(4) 0.853(2) 0.080(8) Uiso 1 1 d . . . . .
H4B H 1.061(4) 0.308(4) 0.980(2) 0.079(8) Uiso 1 1 d . . . . .
H4C H 1.049(5) 0.239(4) 0.872(3) 0.098(10) Uiso 1 1 d . . . . .
H9 H 0.710(4) 0.539(4) 0.814(2) 0.074(7) Uiso 1 1 d . . . . .
H3 H 0.409(4) 0.504(3) 0.829(2) 0.084(9) Uiso 1 1 d D . . . .
O4 O 0.3030(3) 0.6498(2) 0.71348(14) 0.0616(5) Uani 1 1 d . . . . .
H4D H 0.303(4) 0.770(5) 0.673(3) 0.088(9) Uiso 1 1 d . . . . .
H4E H 0.283(5) 0.585(5) 0.664(3) 0.111(11) 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
O1 N1 1.3330(18) . ?
O2 N5 1.3247(18) . ?
O2 H2 0.946(18) . ?
N1 N2 1.332(2) . ?
N1 C1 1.332(2) . ?
N2 N3 1.303(2) . ?
N3 N4 1.347(2) . ?
N4 C1 1.328(2) . ?
N5 C2 1.331(2) . ?
N5 N6 1.334(2) . ?
N6 N7 1.301(2) . ?
N7 N8 1.344(2) . ?
N8 C2 1.324(2) . ?
C1 C2 1.444(2) . ?
O3 N9 1.362(2) . ?
O3 H3 0.870(17) . ?
N9 C3 1.268(2) . ?
N9 H9 0.93(3) . ?
C3 C5 1.475(3) . ?
C3 C4 1.476(3) . ?
C4 H4A 0.99(3) . ?
C4 H4B 1.01(3) . ?
C4 H4C 0.91(3) . ?
C5 H5A 0.92(3) . ?
C5 H5B 0.94(4) . ?
C5 H5C 0.93(3) . ?
O4 H4D 0.88(3) . ?
O4 H4E 0.88(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N5 O2 H2 108(2) . . ?
N2 N1 O1 123.11(14) . . ?
N2 N1 C1 109.57(14) . . ?
O1 N1 C1 127.32(15) . . ?
N3 N2 N1 106.16(14) . . ?
N2 N3 N4 110.50(14) . . ?
C1 N4 N3 106.31(14) . . ?
O2 N5 C2 128.10(14) . . ?
O2 N5 N6 122.49(14) . . ?
C2 N5 N6 109.39(14) . . ?
N7 N6 N5 106.10(14) . . ?
N6 N7 N8 110.51(14) . . ?
C2 N8 N7 106.42(14) . . ?
N4 C1 N1 107.47(15) . . ?
N4 C1 C2 128.63(15) . . ?
N1 C1 C2 123.91(15) . . ?
N8 C2 N5 107.58(15) . . ?
N8 C2 C1 126.59(14) . . ?
N5 C2 C1 125.83(15) . . ?
N9 O3 H3 107.3(18) . . ?
C3 N9 O3 121.40(16) . . ?
C3 N9 H9 120.3(16) . . ?
O3 N9 H9 118.2(16) . . ?
N9 C3 C5 121.4(2) . . ?
N9 C3 C4 117.07(18) . . ?
C5 C3 C4 121.6(2) . . ?
C3 C4 H4A 111.3(15) . . ?
C3 C4 H4B 110.8(15) . . ?
H4A C4 H4B 110(2) . . ?
C3 C4 H4C 107.9(19) . . ?
H4A C4 H4C 114(2) . . ?
H4B C4 H4C 103(2) . . ?
C3 C5 H5A 107.7(19) . . ?
C3 C5 H5B 109.8(19) . . ?
H5A C5 H5B 109(3) . . ?
C3 C5 H5C 109.4(17) . . ?
H5A C5 H5C 111(3) . . ?
H5B C5 H5C 110(3) . . ?
H4D O4 H4E 108(3) . . ?

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
O1 N1 N2 N3 -179.25(17) . . . . ?
C1 N1 N2 N3 -0.2(2) . . . . ?
N1 N2 N3 N4 0.2(2) . . . . ?
N2 N3 N4 C1 -0.1(2) . . . . ?
O2 N5 N6 N7 -178.92(16) . . . . ?
C2 N5 N6 N7 -0.4(2) . . . . ?
N5 N6 N7 N8 0.3(2) . . . . ?
N6 N7 N8 C2 -0.1(2) . . . . ?
N3 N4 C1 N1 -0.1(2) . . . . ?
N3 N4 C1 C2 179.80(18) . . . . ?
N2 N1 C1 N4 0.2(2) . . . . ?
O1 N1 C1 N4 179.16(17) . . . . ?
N2 N1 C1 C2 -179.69(16) . . . . ?
O1 N1 C1 C2 -0.7(3) . . . . ?
N7 N8 C2 N5 -0.2(2) . . . . ?
N7 N8 C2 C1 179.99(17) . . . . ?
O2 N5 C2 N8 178.78(17) . . . . ?
N6 N5 C2 N8 0.4(2) . . . . ?
O2 N5 C2 C1 -1.4(3) . . . . ?
N6 N5 C2 C1 -179.81(16) . . . . ?
N4 C1 C2 N8 170.46(18) . . . . ?
N1 C1 C2 N8 -9.7(3) . . . . ?
N4 C1 C2 N5 -9.3(3) . . . . ?
N1 C1 C2 N5 170.52(17) . . . . ?
O3 N9 C3 C5 1.2(3) . . . . ?
O3 N9 C3 C4 179.87(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
O2 H2 O1 0.946(18) 1.481(19) 2.4248(18) 175(3) 1_565
O2 H2 N1 0.946(18) 2.33(2) 3.1371(18) 143(3) 1_565
O2 H2 N2 0.946(18) 2.62(3) 3.112(2) 113(2) 1_565
C4 H4A O4 0.99(3) 2.63(3) 3.448(3) 140(2) 1_655
N9 H9 O1 0.93(3) 2.47(3) 2.989(2) 115.6(19) .
N9 H9 N8 0.93(3) 1.90(3) 2.795(2) 162(2) .
O3 H3 O4 0.870(17) 1.653(18) 2.523(2) 178(3) .
O4 H4D N4 0.88(3) 2.00(3) 2.881(2) 175(3) 2_676
O4 H4E O2 0.88(4) 2.42(3) 2.910(2) 116(3) 2_676
O4 H4E N2 0.88(4) 2.16(4) 2.994(2) 158(3) 2_666

_refine_diff_density_max         0.258
_refine_diff_density_min         -0.189
_refine_diff_density_rms         0.037

_shelxl_version_number           2013-4


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: AC/MT'
