# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_2001105006
_database_code_depnum_ccdc_archive 'CCDC 2158164'
loop_
_audit_author_name
_audit_author_address
'Yangbin Liu'
;Shenzhen Bay Laboratory, China
China
;
_audit_update_record             
;
2022-03-13 deposited with the CCDC.	2022-04-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C19 H19 N O6'
_chemical_formula_sum            'C19 H19 N O6'
_chemical_formula_weight         357.35

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_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'

_cell_length_a                   8.76190(10)
_cell_length_b                   9.03950(10)
_cell_length_c                   21.2088(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1679.80(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    179.99(10)
_cell_measurement_reflns_used    8629
_cell_measurement_theta_min      6.3880
_cell_measurement_theta_max      76.5620

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_F_000             752
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    0.885
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.85091
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.64a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      179.99(10)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean 10.0000
_diffrn_reflns_number            9198
_diffrn_reflns_av_unetI/netI     0.0189
_diffrn_reflns_av_R_equivalents  0.0196
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         6.434
_diffrn_reflns_theta_max         76.665
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             3354
_reflns_number_gt                3318
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.707
_reflns_Friedel_fraction_max     0.933
_reflns_Friedel_fraction_full    0.998

_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       'CrysAlisPro 1.171.41.64a (Rigaku OD, 2020)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.64a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.64a (Rigaku OD, 2020)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0366P)²+0.3480P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.0133(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 1358 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(9)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         3354
_refine_ls_number_parameters     237
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0266
_refine_ls_R_factor_gt           0.0262
_refine_ls_wR_factor_ref         0.0707
_refine_ls_wR_factor_gt          0.0705
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_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
O18 O 0.80202(14) 0.82723(15) 0.70594(5) 0.0300(3) Uani 1 1 d . . . . .
O20 O 0.54666(14) 0.78419(15) 0.70328(5) 0.0315(3) Uani 1 1 d . . . . .
O13 O 0.27287(14) 0.69176(15) 0.76433(6) 0.0290(3) Uani 1 1 d . . . . .
O15 O 0.27592(16) 0.94082(15) 0.76725(6) 0.0336(3) Uani 1 1 d . . . . .
O16 O 0.20082(15) 0.73403(15) 0.90021(6) 0.0334(3) Uani 1 1 d . . . . .
O11 O 0.42067(15) 0.74094(16) 0.95121(6) 0.0343(3) Uani 1 1 d . . . . .
N9 N 0.68565(15) 0.74492(16) 0.79208(6) 0.0240(3) Uani 1 1 d . . . . .
C17 C 0.66734(19) 0.78424(18) 0.73150(7) 0.0232(3) Uani 1 1 d . . . . .
C21 C 0.88795(18) 0.7866(2) 0.59831(7) 0.0236(3) Uani 1 1 d . . . . .
C1 C 0.55939(18) 0.68477(18) 0.82942(7) 0.0228(3) Uani 1 1 d . . . . .
H1 H 0.517386 0.592984 0.809628 0.027 Uiso 1 1 calc R U . . .
C3 C 0.5109(2) 0.9427(2) 0.86117(8) 0.0267(4) Uani 1 1 d . . . . .
H3 H 0.502101 1.034555 0.839690 0.032 Uiso 1 1 calc R U . . .
C12 C 0.31916(18) 0.82242(19) 0.78601(7) 0.0241(3) Uani 1 1 d . . . . .
C4 C 0.5960(2) 0.9232(2) 0.91224(9) 0.0317(4) Uani 1 1 d . . . . .
H4 H 0.658789 0.998633 0.929559 0.038 Uiso 1 1 calc R U . . .
C10 C 0.3364(2) 0.75469(19) 0.89867(8) 0.0266(3) Uani 1 1 d . . . . .
C25 C 0.9749(2) 0.5490(2) 0.56184(9) 0.0326(4) Uani 1 1 d . . . . .
H25 H 0.976794 0.444349 0.566056 0.039 Uiso 1 1 calc R U . . .
C2 C 0.42929(18) 0.80287(18) 0.84075(7) 0.0224(3) Uani 1 1 d . . . . .
C22 C 0.9680(2) 0.8531(2) 0.54926(8) 0.0281(4) Uani 1 1 d . . . . .
H22 H 0.965201 0.957610 0.544584 0.034 Uiso 1 1 calc R U . . .
C26 C 0.8914(2) 0.6334(2) 0.60411(8) 0.0286(4) Uani 1 1 d . . . . .
H26 H 0.836302 0.586484 0.637113 0.034 Uiso 1 1 calc R U . . .
C19 C 0.7969(2) 0.8829(2) 0.64222(8) 0.0327(4) Uani 1 1 d . . . . .
H19A H 0.838268 0.984811 0.641281 0.039 Uiso 1 1 calc R U . . .
H19B H 0.689570 0.886717 0.627742 0.039 Uiso 1 1 calc R U . . .
C24 C 1.0557(2) 0.6159(2) 0.51356(9) 0.0338(4) Uani 1 1 d . . . . .
H24 H 1.113590 0.557624 0.484968 0.041 Uiso 1 1 calc R U . . .
C8 C 0.8337(2) 0.7418(2) 0.82421(8) 0.0353(4) Uani 1 1 d . . . . .
H8A H 0.864982 0.842418 0.837357 0.042 Uiso 1 1 calc R U . . .
H8B H 0.913663 0.699619 0.796539 0.042 Uiso 1 1 calc R U . . .
C7 C 0.8064(2) 0.6437(2) 0.88098(9) 0.0347(4) Uani 1 1 d . . . . .
H7A H 0.864055 0.680475 0.917921 0.042 Uiso 1 1 calc R U . . .
H7B H 0.838691 0.540884 0.872012 0.042 Uiso 1 1 calc R U . . .
C23 C 1.0517(2) 0.7685(2) 0.50714(9) 0.0357(4) Uani 1 1 d . . . . .
H23 H 1.106217 0.814998 0.473895 0.043 Uiso 1 1 calc R U . . .
C14 C 0.1780(2) 0.6968(3) 0.70883(9) 0.0392(4) Uani 1 1 d . . . . .
H14A H 0.239341 0.728325 0.672602 0.059 Uiso 1 1 calc R U . . .
H14B H 0.094493 0.767141 0.715486 0.059 Uiso 1 1 calc R U . . .
H14C H 0.135780 0.598222 0.700678 0.059 Uiso 1 1 calc R U . . .
C6 C 0.6340(2) 0.6503(2) 0.89357(8) 0.0284(4) Uani 1 1 d . . . . .
H6 H 0.597853 0.551764 0.908937 0.034 Uiso 1 1 calc R U . . .
C5 C 0.5839(2) 0.7711(2) 0.94013(8) 0.0327(4) Uani 1 1 d . . . . .
H5 H 0.643153 0.764313 0.980327 0.039 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
O18 C17 1.356(2) . ?
O18 C19 1.443(2) . ?
O20 C17 1.215(2) . ?
O13 C12 1.331(2) . ?
O13 C14 1.442(2) . ?
O15 C12 1.203(2) . ?
O16 C10 1.203(2) . ?
O11 C10 1.343(2) . ?
O11 C5 1.475(2) . ?
N9 C17 1.343(2) . ?
N9 C1 1.465(2) . ?
N9 C8 1.466(2) . ?
C21 C22 1.391(2) . ?
C21 C26 1.391(3) . ?
C21 C19 1.504(2) . ?
C1 C6 1.541(2) . ?
C1 C2 1.580(2) . ?
C1 H1 1.0000 . ?
C3 C4 1.327(3) . ?
C3 C2 1.516(2) . ?
C3 H3 0.9500 . ?
C12 C2 1.520(2) . ?
C4 C5 1.500(3) . ?
C4 H4 0.9500 . ?
C10 C2 1.537(2) . ?
C25 C24 1.384(3) . ?
C25 C26 1.387(3) . ?
C25 H25 0.9500 . ?
C22 C23 1.386(3) . ?
C22 H22 0.9500 . ?
C26 H26 0.9500 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C24 C23 1.386(3) . ?
C24 H24 0.9500 . ?
C8 C7 1.514(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C7 C6 1.535(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C23 H23 0.9500 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C6 C5 1.536(3) . ?
C6 H6 1.0000 . ?
C5 H5 1.0000 . ?

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
C17 O18 C19 116.59(14) . . ?
C12 O13 C14 115.47(14) . . ?
C10 O11 C5 112.59(13) . . ?
C17 N9 C1 121.69(14) . . ?
C17 N9 C8 123.76(14) . . ?
C1 N9 C8 114.20(13) . . ?
O20 C17 N9 125.12(15) . . ?
O20 C17 O18 124.11(14) . . ?
N9 C17 O18 110.76(14) . . ?
C22 C21 C26 119.05(16) . . ?
C22 C21 C19 118.71(16) . . ?
C26 C21 C19 122.21(16) . . ?
N9 C1 C6 103.41(13) . . ?
N9 C1 C2 112.10(13) . . ?
C6 C1 C2 107.95(13) . . ?
N9 C1 H1 111.0 . . ?
C6 C1 H1 111.0 . . ?
C2 C1 H1 111.0 . . ?
C4 C3 C2 112.80(16) . . ?
C4 C3 H3 123.6 . . ?
C2 C3 H3 123.6 . . ?
O15 C12 O13 125.41(15) . . ?
O15 C12 C2 123.77(15) . . ?
O13 C12 C2 110.75(13) . . ?
C3 C4 C5 113.84(16) . . ?
C3 C4 H4 123.1 . . ?
C5 C4 H4 123.1 . . ?
O16 C10 O11 120.42(15) . . ?
O16 C10 C2 126.08(16) . . ?
O11 C10 C2 113.47(14) . . ?
C24 C25 C26 120.51(18) . . ?
C24 C25 H25 119.7 . . ?
C26 C25 H25 119.7 . . ?
C3 C2 C12 114.89(14) . . ?
C3 C2 C10 104.95(13) . . ?
C12 C2 C10 107.89(13) . . ?
C3 C2 C1 105.46(13) . . ?
C12 C2 C1 114.85(13) . . ?
C10 C2 C1 108.20(13) . . ?
C23 C22 C21 120.67(17) . . ?
C23 C22 H22 119.7 . . ?
C21 C22 H22 119.7 . . ?
C25 C26 C21 120.16(17) . . ?
C25 C26 H26 119.9 . . ?
C21 C26 H26 119.9 . . ?
O18 C19 C21 111.21(14) . . ?
O18 C19 H19A 109.4 . . ?
C21 C19 H19A 109.4 . . ?
O18 C19 H19B 109.4 . . ?
C21 C19 H19B 109.4 . . ?
H19A C19 H19B 108.0 . . ?
C25 C24 C23 119.64(18) . . ?
C25 C24 H24 120.2 . . ?
C23 C24 H24 120.2 . . ?
N9 C8 C7 103.92(15) . . ?
N9 C8 H8A 111.0 . . ?
C7 C8 H8A 111.0 . . ?
N9 C8 H8B 111.0 . . ?
C7 C8 H8B 111.0 . . ?
H8A C8 H8B 109.0 . . ?
C8 C7 C6 105.75(14) . . ?
C8 C7 H7A 110.6 . . ?
C6 C7 H7A 110.6 . . ?
C8 C7 H7B 110.6 . . ?
C6 C7 H7B 110.6 . . ?
H7A C7 H7B 108.7 . . ?
C24 C23 C22 119.96(18) . . ?
C24 C23 H23 120.0 . . ?
C22 C23 H23 120.0 . . ?
O13 C14 H14A 109.5 . . ?
O13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
O13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C7 C6 C5 114.87(16) . . ?
C7 C6 C1 105.75(14) . . ?
C5 C6 C1 107.62(14) . . ?
C7 C6 H6 109.5 . . ?
C5 C6 H6 109.5 . . ?
C1 C6 H6 109.5 . . ?
O11 C5 C4 107.50(15) . . ?
O11 C5 C6 104.35(15) . . ?
C4 C5 C6 112.20(14) . . ?
O11 C5 H5 110.9 . . ?
C4 C5 H5 110.9 . . ?
C6 C5 H5 110.9 . . ?

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 N9 C17 O20 5.3(3) . . . . ?
C8 N9 C17 O20 178.01(18) . . . . ?
C1 N9 C17 O18 -175.92(14) . . . . ?
C8 N9 C17 O18 -3.2(2) . . . . ?
C19 O18 C17 O20 3.3(2) . . . . ?
C19 O18 C17 N9 -175.57(14) . . . . ?
C17 N9 C1 C6 177.69(14) . . . . ?
C8 N9 C1 C6 4.3(2) . . . . ?
C17 N9 C1 C2 -66.28(19) . . . . ?
C8 N9 C1 C2 120.32(16) . . . . ?
C14 O13 C12 O15 8.1(2) . . . . ?
C14 O13 C12 C2 -174.93(14) . . . . ?
C2 C3 C4 C5 -3.7(2) . . . . ?
C5 O11 C10 O16 -179.74(17) . . . . ?
C5 O11 C10 C2 -1.8(2) . . . . ?
C4 C3 C2 C12 174.74(15) . . . . ?
C4 C3 C2 C10 56.42(18) . . . . ?
C4 C3 C2 C1 -57.74(18) . . . . ?
O15 C12 C2 C3 -13.6(2) . . . . ?
O13 C12 C2 C3 169.37(14) . . . . ?
O15 C12 C2 C10 103.07(19) . . . . ?
O13 C12 C2 C10 -73.98(16) . . . . ?
O15 C12 C2 C1 -136.19(17) . . . . ?
O13 C12 C2 C1 46.77(18) . . . . ?
O16 C10 C2 C3 123.93(18) . . . . ?
O11 C10 C2 C3 -53.89(18) . . . . ?
O16 C10 C2 C12 1.0(2) . . . . ?
O11 C10 C2 C12 -176.85(14) . . . . ?
O16 C10 C2 C1 -123.85(18) . . . . ?
O11 C10 C2 C1 58.33(18) . . . . ?
N9 C1 C2 C3 -46.77(17) . . . . ?
C6 C1 C2 C3 66.48(17) . . . . ?
N9 C1 C2 C12 80.77(17) . . . . ?
C6 C1 C2 C12 -165.98(14) . . . . ?
N9 C1 C2 C10 -158.65(13) . . . . ?
C6 C1 C2 C10 -45.40(18) . . . . ?
C26 C21 C22 C23 -0.8(3) . . . . ?
C19 C21 C22 C23 -179.11(17) . . . . ?
C24 C25 C26 C21 0.0(3) . . . . ?
C22 C21 C26 C25 0.7(3) . . . . ?
C19 C21 C26 C25 178.91(17) . . . . ?
C17 O18 C19 C21 -117.24(17) . . . . ?
C22 C21 C19 O18 -144.04(16) . . . . ?
C26 C21 C19 O18 37.7(2) . . . . ?
C26 C25 C24 C23 -0.6(3) . . . . ?
C17 N9 C8 C7 -161.02(16) . . . . ?
C1 N9 C8 C7 12.2(2) . . . . ?
N9 C8 C7 C6 -23.6(2) . . . . ?
C25 C24 C23 C22 0.5(3) . . . . ?
C21 C22 C23 C24 0.2(3) . . . . ?
C8 C7 C6 C5 -91.69(19) . . . . ?
C8 C7 C6 C1 26.8(2) . . . . ?
N9 C1 C6 C7 -18.93(18) . . . . ?
C2 C1 C6 C7 -137.87(15) . . . . ?
N9 C1 C6 C5 104.30(15) . . . . ?
C2 C1 C6 C5 -14.63(19) . . . . ?
C10 O11 C5 C4 56.29(18) . . . . ?
C10 O11 C5 C6 -63.03(18) . . . . ?
C3 C4 C5 O11 -54.1(2) . . . . ?
C3 C4 C5 C6 60.1(2) . . . . ?
C7 C6 C5 O11 -172.03(14) . . . . ?
C1 C6 C5 O11 70.50(17) . . . . ?
C7 C6 C5 C4 71.9(2) . . . . ?
C1 C6 C5 C4 -45.6(2) . . . . ?

_refine_diff_density_max         0.172
_refine_diff_density_min         -0.139
_refine_diff_density_rms         0.030



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: ether dicloromethane'
