# Electronic Supplementary Material (ESI) for Green Chemistry.
# This journal is © The Royal Society of Chemistry 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_shelx
_audit_block_doi                 10.5517/ccdc.csd.cc1m4fz5
_database_code_depnum_ccdc_archive 'CCDC 1493827'
_audit_update_record             
;
2016-07-15 deposited with the CCDC.
2017-06-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H19 N5 O5'
_chemical_formula_sum            'C22 H19 N5 O5'
_chemical_formula_weight         433.42

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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_HALL  '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.7024(3)
_cell_length_b                   9.8685(3)
_cell_length_c                   12.5819(4)
_cell_angle_alpha                80.4210(10)
_cell_angle_beta                 70.6290(10)
_cell_angle_gamma                65.9310(10)
_cell_volume                     1037.01(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4242
_cell_measurement_theta_min      1.72
_cell_measurement_theta_max      26.39

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             452
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9820
_exptl_absorpt_correction_T_max  0.9879
_exptl_absorpt_process_details   '(SADABS; Bruker, 2008)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(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 APEXII area-detector diffractometer'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15154
_diffrn_reflns_av_R_equivalents  0.0207
_diffrn_reflns_av_sigmaI/netI    0.0186
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.72
_diffrn_reflns_theta_max         26.39
_reflns_number_total             4242
_reflns_number_gt                3447
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0498P)²+0.2734P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0057(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4242
_refine_ls_number_parameters     300
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0382
_refine_ls_wR_factor_ref         0.1107
_refine_ls_wR_factor_gt          0.1014
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.025
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1W O 0.69204(19) 0.19541(17) 0.50409(14) 0.0749(4) Uani 1 1 d . . .
H1WA H 0.594(4) 0.192(3) 0.525(2) 0.114(9) Uiso 1 1 d . . .
H1WB H 0.731(4) 0.169(4) 0.563(3) 0.159(14) Uiso 1 1 d . . .
O4 O 0.66815(12) 0.48716(13) 0.47228(8) 0.0504(3) Uani 1 1 d . . .
H4 H 0.6818 0.3999 0.4702 0.076 Uiso 1 1 calc R . .
O3 O 0.63434(12) 0.79295(13) 0.42054(10) 0.0561(3) Uani 1 1 d . . .
N4 N 0.90375(13) 0.66934(14) 0.38120(10) 0.0419(3) Uani 1 1 d . . .
O1 O 0.88446(13) 0.62604(14) 0.12369(9) 0.0579(3) Uani 1 1 d . . .
C10 C 1.01268(16) 0.52385(17) 0.35449(11) 0.0400(3) Uani 1 1 d . . .
C21 C 0.77083(16) 0.59180(17) 0.15685(12) 0.0436(3) Uani 1 1 d . . .
O2 O 0.45048(14) 0.55093(17) 0.12802(10) 0.0693(4) Uani 1 1 d . . .
C16 C 0.76172(16) 0.52947(17) 0.37106(11) 0.0405(3) Uani 1 1 d . . .
N1 N 1.18007(15) 0.86964(14) 0.12367(11) 0.0504(3) Uani 1 1 d . . .
N5 N 0.68020(15) 0.59072(16) 0.09276(10) 0.0501(3) Uani 1 1 d . . .
C17 C 0.75417(16) 0.68288(17) 0.39384(11) 0.0418(3) Uani 1 1 d . . .
C15 C 0.93655(16) 0.43615(17) 0.34495(11) 0.0406(3) Uani 1 1 d . . .
C18 C 0.69701(16) 0.54467(17) 0.27452(11) 0.0419(3) Uani 1 1 d . . .
C11 C 1.17317(17) 0.46763(19) 0.33944(13) 0.0491(4) Uani 1 1 d . . .
H11 H 1.2235 0.5270 0.3461 0.059 Uiso 1 1 calc R . .
N2 N 1.24707(19) 0.89398(19) 0.19310(14) 0.0672(4) Uani 1 1 d . . .
C7 C 1.06127(17) 0.82571(18) 0.18374(14) 0.0496(4) Uani 1 1 d . . .
H7 H 0.9972 0.8008 0.1560 0.059 Uiso 1 1 calc R . .
C14 C 1.02060(19) 0.28978(18) 0.31851(13) 0.0506(4) Uani 1 1 d . . .
H14 H 0.9703 0.2309 0.3110 0.061 Uiso 1 1 calc R . .
C8 C 1.05451(18) 0.82536(17) 0.29308(14) 0.0474(4) Uani 1 1 d . . .
C12 C 1.25612(18) 0.3198(2) 0.31408(14) 0.0564(4) Uani 1 1 d . . .
H12 H 1.3643 0.2789 0.3041 0.068 Uiso 1 1 calc R . .
C9 C 0.94502(19) 0.78873(19) 0.39817(13) 0.0508(4) Uani 1 1 d . . .
H9A H 0.9949 0.7592 0.4581 0.061 Uiso 1 1 calc R . .
H9B H 0.8497 0.8764 0.4212 0.061 Uiso 1 1 calc R . .
C19 C 0.57033(18) 0.52422(19) 0.27559(13) 0.0499(4) Uani 1 1 d . . .
H19 H 0.5030 0.4955 0.3384 0.060 Uiso 1 1 calc R . .
N3 N 1.17094(18) 0.86618(18) 0.29644(13) 0.0631(4) Uani 1 1 d . . .
C13 C 1.1827(2) 0.2310(2) 0.30315(14) 0.0570(4) Uani 1 1 d . . .
H13 H 1.2416 0.1319 0.2855 0.068 Uiso 1 1 calc R . .
C22 C 0.7103(2) 0.6263(2) -0.02755(13) 0.0627(5) Uani 1 1 d . . .
H22A H 0.8149 0.6265 -0.0587 0.094 Uiso 1 1 calc R . .
H22B H 0.6348 0.7225 -0.0398 0.094 Uiso 1 1 calc R . .
H22C H 0.7011 0.5532 -0.0636 0.094 Uiso 1 1 calc R . .
C20 C 0.55280(18) 0.55470(19) 0.15986(13) 0.0499(4) Uani 1 1 d . . .
C1 C 1.23606(18) 0.89126(18) 0.00413(15) 0.0547(4) Uani 1 1 d . . .
C2 C 1.2027(2) 0.8259(2) -0.06720(17) 0.0689(5) Uani 1 1 d . . .
H2 H 1.1453 0.7653 -0.0385 0.083 Uiso 1 1 calc R . .
C6 C 1.3231(2) 0.9801(2) -0.03902(18) 0.0724(5) Uani 1 1 d . . .
H6 H 1.3462 1.0245 0.0090 0.087 Uiso 1 1 calc R . .
C3 C 1.2558(3) 0.8512(2) -0.18302(18) 0.0816(6) Uani 1 1 d . . .
H3 H 1.2324 0.8080 -0.2316 0.098 Uiso 1 1 calc R . .
C4 C 1.3416(3) 0.9383(3) -0.2263(2) 0.0843(7) Uani 1 1 d . . .
H4A H 1.3768 0.9543 -0.3038 0.101 Uiso 1 1 calc R . .
C5 C 1.3754(3) 1.0018(3) -0.1552(2) 0.0868(7) Uani 1 1 d . . .
H5 H 1.4345 1.0608 -0.1848 0.104 Uiso 1 1 calc R . .


_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
O1W H1WA 0.92(3) . ?
O1W H1WB 0.90(4) . ?
O4 C16 1.4092(16) . ?
O4 H4 0.8200 . ?
O3 C17 1.2152(18) . ?
N4 C17 1.3584(17) . ?
N4 C10 1.4066(19) . ?
N4 C9 1.4558(19) . ?
O1 C21 1.2065(17) . ?
C10 C11 1.3795(19) . ?
C10 C15 1.3870(19) . ?
C21 N5 1.3800(18) . ?
C21 C18 1.5035(19) . ?
O2 C20 1.2026(18) . ?
C16 C18 1.5035(19) . ?
C16 C15 1.513(2) . ?
C16 C17 1.556(2) . ?
N1 C7 1.3448(19) . ?
N1 N2 1.348(2) . ?
N1 C1 1.431(2) . ?
N5 C20 1.3905(19) . ?
N5 C22 1.454(2) . ?
C15 C14 1.372(2) . ?
C18 C19 1.3199(19) . ?
C11 C12 1.380(2) . ?
C11 H11 0.9300 . ?
N2 N3 1.312(2) . ?
C7 C8 1.355(2) . ?
C7 H7 0.9300 . ?
C14 C13 1.393(2) . ?
C14 H14 0.9300 . ?
C8 N3 1.3596(19) . ?
C8 C9 1.493(2) . ?
C12 C13 1.381(2) . ?
C12 H12 0.9300 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C19 C20 1.489(2) . ?
C19 H19 0.9300 . ?
C13 H13 0.9300 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C1 C2 1.372(3) . ?
C1 C6 1.385(2) . ?
C2 C3 1.392(3) . ?
C2 H2 0.9300 . ?
C6 C5 1.390(3) . ?
C6 H6 0.9300 . ?
C3 C4 1.362(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.360(4) . ?
C4 H4A 0.9300 . ?
C5 H5 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
H1WA O1W H1WB 110(3) . . ?
C16 O4 H4 109.5 . . ?
C17 N4 C10 111.48(12) . . ?
C17 N4 C9 124.18(13) . . ?
C10 N4 C9 124.29(12) . . ?
C11 C10 C15 121.75(15) . . ?
C11 C10 N4 127.88(13) . . ?
C15 C10 N4 110.37(12) . . ?
O1 C21 N5 126.08(14) . . ?
O1 C21 C18 127.97(13) . . ?
N5 C21 C18 105.94(12) . . ?
O4 C16 C18 111.35(11) . . ?
O4 C16 C15 114.33(11) . . ?
C18 C16 C15 113.34(12) . . ?
O4 C16 C17 104.94(11) . . ?
C18 C16 C17 109.90(11) . . ?
C15 C16 C17 102.14(11) . . ?
C7 N1 N2 110.16(13) . . ?
C7 N1 C1 128.77(14) . . ?
N2 N1 C1 121.07(13) . . ?
C21 N5 C20 110.54(12) . . ?
C21 N5 C22 125.05(13) . . ?
C20 N5 C22 124.38(13) . . ?
O3 C17 N4 126.97(14) . . ?
O3 C17 C16 125.34(12) . . ?
N4 C17 C16 107.67(12) . . ?
C14 C15 C10 120.34(13) . . ?
C14 C15 C16 131.34(13) . . ?
C10 C15 C16 108.30(13) . . ?
C19 C18 C16 128.49(13) . . ?
C19 C18 C21 108.47(12) . . ?
C16 C18 C21 123.03(11) . . ?
C10 C11 C12 117.35(14) . . ?
C10 C11 H11 121.3 . . ?
C12 C11 H11 121.3 . . ?
N3 N2 N1 107.21(12) . . ?
N1 C7 C8 105.53(13) . . ?
N1 C7 H7 127.2 . . ?
C8 C7 H7 127.2 . . ?
C15 C14 C13 118.72(15) . . ?
C15 C14 H14 120.6 . . ?
C13 C14 H14 120.6 . . ?
C7 C8 N3 108.26(14) . . ?
C7 C8 C9 130.13(13) . . ?
N3 C8 C9 121.61(14) . . ?
C11 C12 C13 121.77(15) . . ?
C11 C12 H12 119.1 . . ?
C13 C12 H12 119.1 . . ?
N4 C9 C8 111.35(12) . . ?
N4 C9 H9A 109.4 . . ?
C8 C9 H9A 109.4 . . ?
N4 C9 H9B 109.4 . . ?
C8 C9 H9B 109.4 . . ?
H9A C9 H9B 108.0 . . ?
C18 C19 C20 108.84(13) . . ?
C18 C19 H19 125.6 . . ?
C20 C19 H19 125.6 . . ?
N2 N3 C8 108.83(14) . . ?
C12 C13 C14 120.06(16) . . ?
C12 C13 H13 120.0 . . ?
C14 C13 H13 120.0 . . ?
N5 C22 H22A 109.5 . . ?
N5 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
N5 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O2 C20 N5 125.44(15) . . ?
O2 C20 C19 128.43(15) . . ?
N5 C20 C19 106.13(12) . . ?
C2 C1 C6 120.17(18) . . ?
C2 C1 N1 120.44(15) . . ?
C6 C1 N1 119.38(17) . . ?
C1 C2 C3 119.3(2) . . ?
C1 C2 H2 120.4 . . ?
C3 C2 H2 120.4 . . ?
C1 C6 C5 119.0(2) . . ?
C1 C6 H6 120.5 . . ?
C5 C6 H6 120.5 . . ?
C4 C3 C2 121.0(2) . . ?
C4 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
C5 C4 C3 119.5(2) . . ?
C5 C4 H4A 120.3 . . ?
C3 C4 H4A 120.3 . . ?
C4 C5 C6 121.1(2) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?

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
C17 N4 C10 C11 -177.57(14) . . . . ?
C9 N4 C10 C11 -0.2(2) . . . . ?
C17 N4 C10 C15 1.96(15) . . . . ?
C9 N4 C10 C15 179.38(13) . . . . ?
O1 C21 N5 C20 -176.15(16) . . . . ?
C18 C21 N5 C20 2.92(17) . . . . ?
O1 C21 N5 C22 2.2(3) . . . . ?
C18 C21 N5 C22 -178.70(15) . . . . ?
C10 N4 C17 O3 177.36(13) . . . . ?
C9 N4 C17 O3 -0.1(2) . . . . ?
C10 N4 C17 C16 -1.11(14) . . . . ?
C9 N4 C17 C16 -178.54(12) . . . . ?
O4 C16 C17 O3 -58.97(17) . . . . ?
C18 C16 C17 O3 60.85(17) . . . . ?
C15 C16 C17 O3 -178.55(13) . . . . ?
O4 C16 C17 N4 119.53(12) . . . . ?
C18 C16 C17 N4 -120.64(12) . . . . ?
C15 C16 C17 N4 -0.05(13) . . . . ?
C11 C10 C15 C14 -0.9(2) . . . . ?
N4 C10 C15 C14 179.58(12) . . . . ?
C11 C10 C15 C16 177.65(12) . . . . ?
N4 C10 C15 C16 -1.92(15) . . . . ?
O4 C16 C15 C14 66.71(19) . . . . ?
C18 C16 C15 C14 -62.37(19) . . . . ?
C17 C16 C15 C14 179.46(14) . . . . ?
O4 C16 C15 C10 -111.56(13) . . . . ?
C18 C16 C15 C10 119.35(13) . . . . ?
C17 C16 C15 C10 1.18(13) . . . . ?
O4 C16 C18 C19 0.2(2) . . . . ?
C15 C16 C18 C19 130.82(17) . . . . ?
C17 C16 C18 C19 -115.60(18) . . . . ?
O4 C16 C18 C21 178.64(13) . . . . ?
C15 C16 C18 C21 -50.77(19) . . . . ?
C17 C16 C18 C21 62.80(17) . . . . ?
O1 C21 C18 C19 176.94(17) . . . . ?
N5 C21 C18 C19 -2.10(18) . . . . ?
O1 C21 C18 C16 -1.7(3) . . . . ?
N5 C21 C18 C16 179.21(14) . . . . ?
C15 C10 C11 C12 0.1(2) . . . . ?
N4 C10 C11 C12 179.64(13) . . . . ?
C7 N1 N2 N3 -0.22(19) . . . . ?
C1 N1 N2 N3 179.60(14) . . . . ?
N2 N1 C7 C8 0.86(18) . . . . ?
C1 N1 C7 C8 -178.94(15) . . . . ?
C10 C15 C14 C13 0.9(2) . . . . ?
C16 C15 C14 C13 -177.20(14) . . . . ?
N1 C7 C8 N3 -1.16(18) . . . . ?
N1 C7 C8 C9 178.94(16) . . . . ?
C10 C11 C12 C13 0.5(2) . . . . ?
C17 N4 C9 C8 -119.61(15) . . . . ?
C10 N4 C9 C8 63.29(18) . . . . ?
C7 C8 C9 N4 35.6(2) . . . . ?
N3 C8 C9 N4 -144.30(15) . . . . ?
C16 C18 C19 C20 179.10(15) . . . . ?
C21 C18 C19 C20 0.52(18) . . . . ?
N1 N2 N3 C8 -0.52(19) . . . . ?
C7 C8 N3 N2 1.1(2) . . . . ?
C9 C8 N3 N2 -179.01(15) . . . . ?
C11 C12 C13 C14 -0.4(3) . . . . ?
C15 C14 C13 C12 -0.3(2) . . . . ?
C21 N5 C20 O2 176.94(17) . . . . ?
C22 N5 C20 O2 -1.4(3) . . . . ?
C21 N5 C20 C19 -2.64(18) . . . . ?
C22 N5 C20 C19 178.98(16) . . . . ?
C18 C19 C20 O2 -178.33(18) . . . . ?
C18 C19 C20 N5 1.24(19) . . . . ?
C7 N1 C1 C2 -20.0(3) . . . . ?
N2 N1 C1 C2 160.25(17) . . . . ?
C7 N1 C1 C6 159.42(17) . . . . ?
N2 N1 C1 C6 -20.4(2) . . . . ?
C6 C1 C2 C3 -0.7(3) . . . . ?
N1 C1 C2 C3 178.68(16) . . . . ?
C2 C1 C6 C5 0.1(3) . . . . ?
N1 C1 C6 C5 -179.26(16) . . . . ?
C1 C2 C3 C4 0.7(3) . . . . ?
C2 C3 C4 C5 -0.2(3) . . . . ?
C3 C4 C5 C6 -0.4(3) . . . . ?
C1 C6 C5 C4 0.4(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        26.39
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.237
_refine_diff_density_min         -0.169
_refine_diff_density_rms         0.031
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: DCM / Hexane'
