# Electronic Supplementary Material (ESI) for Chemical Science.
# 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).
# 
# 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_stb228-p21c
_database_code_depnum_ccdc_archive 'CCDC 2097424'
loop_
_audit_author_name
_audit_author_address
'Jakob Blahusch'
;Max Planck Institute for Solid State Research
Germany
;
_audit_update_record             
;
2021-07-19 deposited with the CCDC.	2021-11-02 downloaded from the CCDC.
;
_audit_creation_date             2021-07-19
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        1,3-diethyl-alloxazine
_chemical_formula_moiety         'C14 H14 N4 O2'
_chemical_formula_sum            'C14 H14 N4 O2'
_chemical_formula_weight         270.29
_chemical_melting_point          445
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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.3313(5)
_cell_length_b                   5.0391(2)
_cell_length_c                   19.8573(7)
_cell_angle_alpha                90
_cell_angle_beta                 103.665(2)
_cell_angle_gamma                90
_cell_volume                     1296.21(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5435
_cell_measurement_temperature    298.6
_cell_measurement_theta_max      27.73
_cell_measurement_theta_min      2.32
_shelx_estimated_absorpt_T_max   0.996
_shelx_estimated_absorpt_T_min   0.972
_exptl_absorpt_coefficient_mu    0.097
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9161
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1333 before and 0.0510 after correction.
The Ratio of minimum to maximum transmission is 0.9161.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             568
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0505
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            23975
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.408
_diffrn_reflns_theta_min         4.145
_diffrn_ambient_temperature      298.6
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           50.0
_diffrn_source_power             2.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2308
_reflns_number_total             3523
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.197
_refine_diff_density_min         -0.141
_refine_diff_density_rms         0.035
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         3523
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0976
_refine_ls_R_factor_gt           0.0615
_refine_ls_restrained_S_all      1.070
_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)+(0.0598P)²+0.5060P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1510
_refine_ls_wR_factor_ref         0.1684
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C00G(H00F,H00G), C00J(H00J,H00K)
2.b Aromatic/amide H refined with riding coordinates:
 C00A(H00A), C00D(H00D), C00H(H00H), C00I(H00I)
2.c Idealised Me refined as rotating group:
 C00F(H00B,H00C,H00E), C00K(H00L,H00M,H00N)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
O001 O 0.86647(11) 0.4816(3) 0.57980(7) 0.0612(4) Uani 1 1 d . . . . .
O002 O 0.62427(13) -0.0925(3) 0.46410(9) 0.0724(5) Uani 1 1 d . . . . .
N003 N 0.74739(12) 0.5255(3) 0.33439(8) 0.0483(4) Uani 1 1 d . . . . .
N004 N 0.88585(11) 0.7063(3) 0.45628(8) 0.0446(4) Uani 1 1 d . . . . .
N005 N 0.74837(12) 0.1886(3) 0.52191(9) 0.0498(4) Uani 1 1 d . . . . .
N006 N 0.68314(12) 0.2164(3) 0.40020(9) 0.0494(4) Uani 1 1 d . . . . .
C007 C 0.81600(14) 0.3991(4) 0.52480(10) 0.0466(4) Uani 1 1 d . . . . .
C008 C 0.81996(13) 0.5134(4) 0.45708(9) 0.0422(4) Uani 1 1 d . . . . .
C009 C 0.81718(14) 0.7202(4) 0.33228(9) 0.0460(4) Uani 1 1 d . . . . .
C00A C 0.95664(14) 1.0195(4) 0.38961(10) 0.0505(5) Uani 1 1 d . . . . .
H00A H 1.0020 1.0810 0.4296 0.061 Uiso 1 1 calc R U . . .
C00B C 0.88694(13) 0.8121(4) 0.39367(9) 0.0433(4) Uani 1 1 d . . . . .
C00C C 0.75031(13) 0.4221(4) 0.39541(9) 0.0438(4) Uani 1 1 d . . . . .
C00D C 0.95710(16) 1.1289(5) 0.32699(11) 0.0553(5) Uani 1 1 d . . . . .
H00D H 1.0031 1.2652 0.3243 0.066 Uiso 1 1 calc R U . . .
C00E C 0.68135(15) 0.0922(4) 0.46153(11) 0.0526(5) Uani 1 1 d . . . . .
C00F C 0.6628(2) 0.2214(5) 0.61876(13) 0.0716(7) Uani 1 1 d . . . . .
H00B H 0.5951 0.2049 0.5888 0.107 Uiso 1 1 calc R U . . .
H00C H 0.6819 0.4053 0.6235 0.107 Uiso 1 1 calc R U . . .
H00E H 0.6627 0.1492 0.6635 0.107 Uiso 1 1 calc R U . . .
C00G C 0.60513(16) 0.1346(4) 0.33794(11) 0.0575(5) Uani 1 1 d . . . . .
H00F H 0.5903 -0.0529 0.3411 0.069 Uiso 1 1 calc R U . . .
H00G H 0.6323 0.1612 0.2972 0.069 Uiso 1 1 calc R U . . .
C00H C 0.88847(17) 1.0374(5) 0.26610(11) 0.0596(5) Uani 1 1 d . . . . .
H00H H 0.8899 1.1135 0.2237 0.072 Uiso 1 1 calc R U . . .
C00I C 0.82049(17) 0.8395(5) 0.26868(10) 0.0578(5) Uani 1 1 d . . . . .
H00I H 0.7756 0.7820 0.2280 0.069 Uiso 1 1 calc R U . . .
C00J C 0.73923(18) 0.0718(4) 0.58811(12) 0.0604(5) Uani 1 1 d . . . . .
H00J H 0.8062 0.0741 0.6205 0.072 Uiso 1 1 calc R U . . .
H00K H 0.7174 -0.1116 0.5807 0.072 Uiso 1 1 calc R U . . .
C00K C 0.50717(17) 0.2913(5) 0.33055(14) 0.0716(7) Uani 1 1 d . . . . .
H00L H 0.4564 0.2277 0.2912 0.107 Uiso 1 1 calc R U . . .
H00M H 0.5208 0.4755 0.3241 0.107 Uiso 1 1 calc R U . . .
H00N H 0.4818 0.2709 0.3716 0.107 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
O001 C007 1.213(2) . ?
O002 C00E 1.211(2) . ?
N003 C009 1.360(3) . ?
N003 C00C 1.311(2) . ?
N004 C008 1.313(2) . ?
N004 C00B 1.356(2) . ?
N005 C007 1.384(2) . ?
N005 C00E 1.402(3) . ?
N005 C00J 1.471(3) . ?
N006 C00C 1.388(2) . ?
N006 C00E 1.374(3) . ?
N006 C00G 1.474(2) . ?
C007 C008 1.475(3) . ?
C008 C00C 1.427(2) . ?
C009 C00B 1.425(3) . ?
C009 C00I 1.409(3) . ?
C00A H00A 0.9300 . ?
C00A C00B 1.414(3) . ?
C00A C00D 1.361(3) . ?
C00D H00D 0.9300 . ?
C00D C00H 1.410(3) . ?
C00F H00B 0.9600 . ?
C00F H00C 0.9600 . ?
C00F H00E 0.9600 . ?
C00F C00J 1.507(3) . ?
C00G H00F 0.9700 . ?
C00G H00G 0.9700 . ?
C00G C00K 1.503(3) . ?
C00H H00H 0.9300 . ?
C00H C00I 1.356(3) . ?
C00I H00I 0.9300 . ?
C00J H00J 0.9700 . ?
C00J H00K 0.9700 . ?
C00K H00L 0.9600 . ?
C00K H00M 0.9600 . ?
C00K H00N 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
C00C N003 C009 116.38(15) . . ?
C008 N004 C00B 117.03(15) . . ?
C007 N005 C00E 125.32(17) . . ?
C007 N005 C00J 117.39(17) . . ?
C00E N005 C00J 117.05(17) . . ?
C00C N006 C00G 119.36(17) . . ?
C00E N006 C00C 123.18(16) . . ?
C00E N006 C00G 117.36(17) . . ?
O001 C007 N005 121.15(18) . . ?
O001 C007 C008 123.71(18) . . ?
N005 C007 C008 115.13(16) . . ?
N004 C008 C007 117.94(15) . . ?
N004 C008 C00C 121.99(17) . . ?
C00C C008 C007 120.01(17) . . ?
N003 C009 C00B 121.40(17) . . ?
N003 C009 C00I 120.15(17) . . ?
C00I C009 C00B 118.44(19) . . ?
C00B C00A H00A 120.1 . . ?
C00D C00A H00A 120.1 . . ?
C00D C00A C00B 119.76(18) . . ?
N004 C00B C009 120.71(17) . . ?
N004 C00B C00A 119.52(16) . . ?
C00A C00B C009 119.76(17) . . ?
N003 C00C N006 118.78(16) . . ?
N003 C00C C008 122.43(18) . . ?
N006 C00C C008 118.79(17) . . ?
C00A C00D H00D 119.7 . . ?
C00A C00D C00H 120.6(2) . . ?
C00H C00D H00D 119.7 . . ?
O002 C00E N005 120.7(2) . . ?
O002 C00E N006 122.0(2) . . ?
N006 C00E N005 117.33(18) . . ?
H00B C00F H00C 109.5 . . ?
H00B C00F H00E 109.5 . . ?
H00C C00F H00E 109.5 . . ?
C00J C00F H00B 109.5 . . ?
C00J C00F H00C 109.5 . . ?
C00J C00F H00E 109.5 . . ?
N006 C00G H00F 109.4 . . ?
N006 C00G H00G 109.4 . . ?
N006 C00G C00K 111.07(17) . . ?
H00F C00G H00G 108.0 . . ?
C00K C00G H00F 109.4 . . ?
C00K C00G H00G 109.4 . . ?
C00D C00H H00H 119.6 . . ?
C00I C00H C00D 120.8(2) . . ?
C00I C00H H00H 119.6 . . ?
C009 C00I H00I 119.7 . . ?
C00H C00I C009 120.68(19) . . ?
C00H C00I H00I 119.7 . . ?
N005 C00J C00F 111.57(18) . . ?
N005 C00J H00J 109.3 . . ?
N005 C00J H00K 109.3 . . ?
C00F C00J H00J 109.3 . . ?
C00F C00J H00K 109.3 . . ?
H00J C00J H00K 108.0 . . ?
C00G C00K H00L 109.5 . . ?
C00G C00K H00M 109.5 . . ?
C00G C00K H00N 109.5 . . ?
H00L C00K H00M 109.5 . . ?
H00L C00K H00N 109.5 . . ?
H00M C00K H00N 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
O001 C007 C008 N004 3.7(3) . . . . ?
O001 C007 C008 C00C -173.55(18) . . . . ?
N003 C009 C00B N004 0.2(3) . . . . ?
N003 C009 C00B C00A -178.41(16) . . . . ?
N003 C009 C00I C00H 178.77(18) . . . . ?
N004 C008 C00C N003 -0.4(3) . . . . ?
N004 C008 C00C N006 179.69(15) . . . . ?
N005 C007 C008 N004 -177.20(15) . . . . ?
N005 C007 C008 C00C 5.6(2) . . . . ?
C007 N005 C00E O002 -179.54(18) . . . . ?
C007 N005 C00E N006 0.2(3) . . . . ?
C007 N005 C00J C00F 84.9(2) . . . . ?
C007 C008 C00C N003 176.77(16) . . . . ?
C007 C008 C00C N006 -3.2(2) . . . . ?
C008 N004 C00B C009 1.6(2) . . . . ?
C008 N004 C00B C00A -179.71(16) . . . . ?
C009 N003 C00C N006 -177.84(15) . . . . ?
C009 N003 C00C C008 2.2(3) . . . . ?
C00A C00D C00H C00I 0.2(3) . . . . ?
C00B N004 C008 C007 -178.79(15) . . . . ?
C00B N004 C008 C00C -1.6(2) . . . . ?
C00B C009 C00I C00H -0.1(3) . . . . ?
C00B C00A C00D C00H 0.1(3) . . . . ?
C00C N003 C009 C00B -2.1(3) . . . . ?
C00C N003 C009 C00I 179.05(17) . . . . ?
C00C N006 C00E O002 -177.60(17) . . . . ?
C00C N006 C00E N005 2.7(3) . . . . ?
C00C N006 C00G C00K -88.9(2) . . . . ?
C00D C00A C00B N004 -179.11(17) . . . . ?
C00D C00A C00B C009 -0.4(3) . . . . ?
C00D C00H C00I C009 -0.3(3) . . . . ?
C00E N005 C007 O001 174.99(18) . . . . ?
C00E N005 C007 C008 -4.1(3) . . . . ?
C00E N005 C00J C00F -89.8(2) . . . . ?
C00E N006 C00C N003 178.94(16) . . . . ?
C00E N006 C00C C008 -1.1(3) . . . . ?
C00E N006 C00G C00K 87.5(2) . . . . ?
C00G N006 C00C N003 -4.9(3) . . . . ?
C00G N006 C00C C008 175.08(16) . . . . ?
C00G N006 C00E O002 6.1(3) . . . . ?
C00G N006 C00E N005 -173.56(16) . . . . ?
C00I C009 C00B N004 179.08(17) . . . . ?
C00I C009 C00B C00A 0.4(3) . . . . ?
C00J N005 C007 O001 0.8(3) . . . . ?
C00J N005 C007 C008 -178.35(16) . . . . ?
C00J N005 C00E O002 -5.3(3) . . . . ?
C00J N005 C00E N006 174.38(16) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Chloroform'
####################################################################### 
# 
# 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_stb226_p-1
_database_code_depnum_ccdc_archive 'CCDC 2097444'
loop_
_audit_author_name
_audit_author_address
'Jakob Blahusch'
;Max Planck Institute for Solid State Research
Germany
;
_audit_update_record             
;
2021-07-19 deposited with the CCDC.	2021-11-02 downloaded from the CCDC.
;
_audit_creation_date             2021-07-19
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        1,3-diethyl-6,9-diphenylalloxazine
_chemical_formula_moiety         'C26 H22 N4 O2'
_chemical_formula_sum            'C26 H22 N4 O2'
_chemical_formula_weight         422.47
_chemical_melting_point          512
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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.4529(6)
_cell_length_b                   10.7933(6)
_cell_length_c                   13.3520(8)
_cell_angle_alpha                67.316(2)
_cell_angle_beta                 71.863(3)
_cell_angle_gamma                87.153(3)
_cell_volume                     1064.65(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4340
_cell_measurement_temperature    298.7
_cell_measurement_theta_max      32.01
_cell_measurement_theta_min      2.59
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9283
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1302 before and 0.0549 after correction.
The Ratio of minimum to maximum transmission is 0.9283.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             444
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.005
_exptl_crystal_size_min          0.005
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0539
_diffrn_reflns_av_unetI/netI     0.0712
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13350
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.544
_diffrn_ambient_temperature      298.7
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2656
_reflns_number_total             4827
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.214
_refine_diff_density_min         -0.210
_refine_diff_density_rms         0.041
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         4827
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1381
_refine_ls_R_factor_gt           0.0702
_refine_ls_restrained_S_all      1.069
_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)+(0.0563P)²+0.3599P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1419
_refine_ls_wR_factor_ref         0.1691
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C00O(H00A,H00B), C00P(H00C,H00D)
2.b Aromatic/amide H refined with riding coordinates:
 C00F(H00F), C00G(H00G), C00H(H00H), C00J(H00J), C00L(H00L), C00M(H00M),
 C00N(H00N), C00Q(H00Q), C00R(H00R), C00S(H00S), C00T(H00T), C00V(H00V)
2.c Idealised Me refined as rotating group:
 C00U(H00E,H00I,H00K), C00W(H00O,H00P,H00U)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
O001 O 0.9761(3) 0.2964(2) 0.42674(17) 0.0527(6) Uani 1 1 d . . . . .
N002 N 0.6506(3) 0.5463(2) 0.63168(17) 0.0336(5) Uani 1 1 d . . . . .
N003 N 0.7905(2) 0.5167(2) 0.42292(17) 0.0327(5) Uani 1 1 d . . . . .
N004 N 0.9237(3) 0.2286(2) 0.61806(19) 0.0401(6) Uani 1 1 d . . . . .
O005 O 0.8613(3) 0.1536(2) 0.81092(18) 0.0656(7) Uani 1 1 d . . . . .
N006 N 0.7545(3) 0.3468(2) 0.72320(18) 0.0393(6) Uani 1 1 d . . . . .
C007 C 0.6943(3) 0.6202(2) 0.4280(2) 0.0314(6) Uani 1 1 d . . . . .
C008 C 0.7363(3) 0.4438(2) 0.6239(2) 0.0333(6) Uani 1 1 d . . . . .
C009 C 0.6284(3) 0.6366(2) 0.5339(2) 0.0318(6) Uani 1 1 d . . . . .
C00A C 0.8111(3) 0.4312(2) 0.5183(2) 0.0329(6) Uani 1 1 d . . . . .
C00B C 0.5344(3) 0.7491(3) 0.5399(2) 0.0344(6) Uani 1 1 d . . . . .
C00C C 0.6622(3) 0.7120(2) 0.3266(2) 0.0343(6) Uani 1 1 d . . . . .
C00D C 0.4676(3) 0.7720(2) 0.6481(2) 0.0371(6) Uani 1 1 d . . . . .
C00E C 0.7274(3) 0.7004(3) 0.2140(2) 0.0361(6) Uani 1 1 d . . . . .
C00F C 0.7366(3) 0.5772(3) 0.2028(2) 0.0404(7) Uani 1 1 d . . . . .
H00F H 0.7076 0.4977 0.2680 0.049 Uiso 1 1 calc R U . . .
C00G C 0.3040(3) 0.8066(3) 0.6806(2) 0.0446(7) Uani 1 1 d . . . . .
H00G H 0.2375 0.8140 0.6349 0.054 Uiso 1 1 calc R U . . .
C00H C 0.5059(3) 0.8343(3) 0.4412(2) 0.0392(7) Uani 1 1 d . . . . .
H00H H 0.4440 0.9076 0.4428 0.047 Uiso 1 1 calc R U . . .
C00I C 0.9117(3) 0.3158(3) 0.5132(2) 0.0373(6) Uani 1 1 d . . . . .
C00J C 0.5661(3) 0.8156(3) 0.3381(2) 0.0415(7) Uani 1 1 d . . . . .
H00J H 0.5401 0.8757 0.2746 0.050 Uiso 1 1 calc R U . . .
C00K C 0.8472(4) 0.2383(3) 0.7235(3) 0.0438(7) Uani 1 1 d . . . . .
C00L C 0.2397(4) 0.8301(3) 0.7790(3) 0.0521(8) Uani 1 1 d . . . . .
H00L H 0.1300 0.8528 0.7995 0.063 Uiso 1 1 calc R U . . .
C00M C 0.7884(4) 0.5716(3) 0.0958(2) 0.0483(7) Uani 1 1 d . . . . .
H00M H 0.7936 0.4884 0.0897 0.058 Uiso 1 1 calc R U . . .
C00N C 0.5632(4) 0.7616(3) 0.7181(2) 0.0442(7) Uani 1 1 d . . . . .
H00N H 0.6725 0.7380 0.6984 0.053 Uiso 1 1 calc R U . . .
C00O C 1.0164(4) 0.1079(3) 0.6214(3) 0.0472(7) Uani 1 1 d . . . . .
H00A H 1.0716 0.0854 0.6791 0.057 Uiso 1 1 calc R U . . .
H00B H 1.1014 0.1270 0.5479 0.057 Uiso 1 1 calc R U . . .
C00P C 0.6788(4) 0.3613(3) 0.8337(2) 0.0487(8) Uani 1 1 d . . . . .
H00C H 0.6475 0.2726 0.8949 0.058 Uiso 1 1 calc R U . . .
H00D H 0.5782 0.4083 0.8323 0.058 Uiso 1 1 calc R U . . .
C00Q C 0.3360(4) 0.8203(3) 0.8471(3) 0.0551(9) Uani 1 1 d . . . . .
H00Q H 0.2922 0.8367 0.9135 0.066 Uiso 1 1 calc R U . . .
C00R C 0.8324(4) 0.6878(3) -0.0016(3) 0.0569(9) Uani 1 1 d . . . . .
H00R H 0.8655 0.6834 -0.0733 0.068 Uiso 1 1 calc R U . . .
C00S C 0.4983(4) 0.7859(3) 0.8166(3) 0.0545(8) Uani 1 1 d . . . . .
H00S H 0.5641 0.7790 0.8626 0.065 Uiso 1 1 calc R U . . .
C00T C 0.7759(4) 0.8170(3) 0.1139(2) 0.0519(8) Uani 1 1 d . . . . .
H00T H 0.7738 0.9006 0.1191 0.062 Uiso 1 1 calc R U . . .
C00U C 0.8996(4) -0.0102(3) 0.6484(3) 0.0549(8) Uani 1 1 d . . . . .
H00E H 0.8454 0.0119 0.5909 0.082 Uiso 1 1 calc R U . . .
H00I H 0.8171 -0.0305 0.7219 0.082 Uiso 1 1 calc R U . . .
H00K H 0.9621 -0.0872 0.6494 0.082 Uiso 1 1 calc R U . . .
C00V C 0.8269(4) 0.8104(3) 0.0076(3) 0.0625(9) Uani 1 1 d . . . . .
H00V H 0.8578 0.8893 -0.0580 0.075 Uiso 1 1 calc R U . . .
C00W C 0.7965(5) 0.4373(4) 0.8575(3) 0.0742(11) Uani 1 1 d . . . . .
H00O H 0.8365 0.5215 0.7936 0.111 Uiso 1 1 calc R U . . .
H00P H 0.8893 0.3851 0.8694 0.111 Uiso 1 1 calc R U . . .
H00U H 0.7393 0.4540 0.9249 0.111 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
O001 C00I 1.207(3) . ?
N002 C008 1.312(3) . ?
N002 C009 1.358(3) . ?
N003 C007 1.359(3) . ?
N003 C00A 1.311(3) . ?
N004 C00I 1.386(3) . ?
N004 C00K 1.397(4) . ?
N004 C00O 1.479(3) . ?
O005 C00K 1.210(3) . ?
N006 C008 1.385(3) . ?
N006 C00K 1.376(3) . ?
N006 C00P 1.480(3) . ?
C007 C009 1.426(3) . ?
C007 C00C 1.434(3) . ?
C008 C00A 1.412(3) . ?
C009 C00B 1.432(3) . ?
C00A C00I 1.484(4) . ?
C00B C00D 1.490(4) . ?
C00B C00H 1.372(3) . ?
C00C C00E 1.484(4) . ?
C00C C00J 1.378(4) . ?
C00D C00G 1.393(4) . ?
C00D C00N 1.386(4) . ?
C00E C00F 1.391(4) . ?
C00E C00T 1.397(4) . ?
C00F H00F 0.9300 . ?
C00F C00M 1.382(4) . ?
C00G H00G 0.9300 . ?
C00G C00L 1.372(4) . ?
C00H H00H 0.9300 . ?
C00H C00J 1.401(4) . ?
C00J H00J 0.9300 . ?
C00L H00L 0.9300 . ?
C00L C00Q 1.372(4) . ?
C00M H00M 0.9300 . ?
C00M C00R 1.375(4) . ?
C00N H00N 0.9300 . ?
C00N C00S 1.379(4) . ?
C00O H00A 0.9700 . ?
C00O H00B 0.9700 . ?
C00O C00U 1.509(4) . ?
C00P H00C 0.9700 . ?
C00P H00D 0.9700 . ?
C00P C00W 1.498(4) . ?
C00Q H00Q 0.9300 . ?
C00Q C00S 1.380(4) . ?
C00R H00R 0.9300 . ?
C00R C00V 1.373(4) . ?
C00S H00S 0.9300 . ?
C00T H00T 0.9300 . ?
C00T C00V 1.378(4) . ?
C00U H00E 0.9600 . ?
C00U H00I 0.9600 . ?
C00U H00K 0.9600 . ?
C00V H00V 0.9300 . ?
C00W H00O 0.9600 . ?
C00W H00P 0.9600 . ?
C00W H00U 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
C008 N002 C009 116.8(2) . . ?
C00A N003 C007 117.9(2) . . ?
C00I N004 C00K 126.3(2) . . ?
C00I N004 C00O 117.6(2) . . ?
C00K N004 C00O 116.0(2) . . ?
C008 N006 C00P 119.8(2) . . ?
C00K N006 C008 122.6(2) . . ?
C00K N006 C00P 117.5(2) . . ?
N003 C007 C009 119.4(2) . . ?
N003 C007 C00C 119.5(2) . . ?
C009 C007 C00C 121.0(2) . . ?
N002 C008 N006 118.1(2) . . ?
N002 C008 C00A 122.1(2) . . ?
N006 C008 C00A 119.8(2) . . ?
N002 C009 C007 121.5(2) . . ?
N002 C009 C00B 118.1(2) . . ?
C007 C009 C00B 120.5(2) . . ?
N003 C00A C008 122.0(2) . . ?
N003 C00A C00I 117.8(2) . . ?
C008 C00A C00I 120.2(2) . . ?
C009 C00B C00D 122.1(2) . . ?
C00H C00B C009 116.7(2) . . ?
C00H C00B C00D 121.2(2) . . ?
C007 C00C C00E 123.6(2) . . ?
C00J C00C C007 116.1(2) . . ?
C00J C00C C00E 120.3(2) . . ?
C00G C00D C00B 119.6(2) . . ?
C00N C00D C00B 122.4(2) . . ?
C00N C00D C00G 118.0(3) . . ?
C00F C00E C00C 122.6(2) . . ?
C00F C00E C00T 117.7(2) . . ?
C00T C00E C00C 119.6(3) . . ?
C00E C00F H00F 119.7 . . ?
C00M C00F C00E 120.6(3) . . ?
C00M C00F H00F 119.7 . . ?
C00D C00G H00G 119.5 . . ?
C00L C00G C00D 120.9(3) . . ?
C00L C00G H00G 119.5 . . ?
C00B C00H H00H 118.6 . . ?
C00B C00H C00J 122.8(2) . . ?
C00J C00H H00H 118.6 . . ?
O001 C00I N004 121.9(2) . . ?
O001 C00I C00A 124.1(2) . . ?
N004 C00I C00A 114.1(2) . . ?
C00C C00J C00H 122.8(2) . . ?
C00C C00J H00J 118.6 . . ?
C00H C00J H00J 118.6 . . ?
O005 C00K N004 120.9(3) . . ?
O005 C00K N006 122.0(3) . . ?
N006 C00K N004 117.1(2) . . ?
C00G C00L H00L 119.8 . . ?
C00Q C00L C00G 120.4(3) . . ?
C00Q C00L H00L 119.8 . . ?
C00F C00M H00M 119.7 . . ?
C00R C00M C00F 120.6(3) . . ?
C00R C00M H00M 119.7 . . ?
C00D C00N H00N 119.6 . . ?
C00S C00N C00D 120.9(3) . . ?
C00S C00N H00N 119.6 . . ?
N004 C00O H00A 109.5 . . ?
N004 C00O H00B 109.5 . . ?
N004 C00O C00U 110.7(2) . . ?
H00A C00O H00B 108.1 . . ?
C00U C00O H00A 109.5 . . ?
C00U C00O H00B 109.5 . . ?
N006 C00P H00C 109.3 . . ?
N006 C00P H00D 109.3 . . ?
N006 C00P C00W 111.8(3) . . ?
H00C C00P H00D 107.9 . . ?
C00W C00P H00C 109.3 . . ?
C00W C00P H00D 109.3 . . ?
C00L C00Q H00Q 120.2 . . ?
C00L C00Q C00S 119.6(3) . . ?
C00S C00Q H00Q 120.2 . . ?
C00M C00R H00R 120.2 . . ?
C00V C00R C00M 119.6(3) . . ?
C00V C00R H00R 120.2 . . ?
C00N C00S C00Q 120.1(3) . . ?
C00N C00S H00S 119.9 . . ?
C00Q C00S H00S 119.9 . . ?
C00E C00T H00T 119.4 . . ?
C00V C00T C00E 121.2(3) . . ?
C00V C00T H00T 119.4 . . ?
C00O C00U H00E 109.5 . . ?
C00O C00U H00I 109.5 . . ?
C00O C00U H00K 109.5 . . ?
H00E C00U H00I 109.5 . . ?
H00E C00U H00K 109.5 . . ?
H00I C00U H00K 109.5 . . ?
C00R C00V C00T 120.2(3) . . ?
C00R C00V H00V 119.9 . . ?
C00T C00V H00V 119.9 . . ?
C00P C00W H00O 109.5 . . ?
C00P C00W H00P 109.5 . . ?
C00P C00W H00U 109.5 . . ?
H00O C00W H00P 109.5 . . ?
H00O C00W H00U 109.5 . . ?
H00P C00W H00U 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
N002 C008 C00A N003 -4.4(4) . . . . ?
N002 C008 C00A C00I 177.9(2) . . . . ?
N002 C009 C00B C00D 2.5(4) . . . . ?
N002 C009 C00B C00H -176.4(2) . . . . ?
N003 C007 C009 N002 -4.2(4) . . . . ?
N003 C007 C009 C00B 176.6(2) . . . . ?
N003 C007 C00C C00E 0.6(4) . . . . ?
N003 C007 C00C C00J -178.9(2) . . . . ?
N003 C00A C00I O001 0.4(4) . . . . ?
N003 C00A C00I N004 -178.5(2) . . . . ?
N006 C008 C00A N003 176.5(2) . . . . ?
N006 C008 C00A C00I -1.1(4) . . . . ?
C007 N003 C00A C008 0.4(4) . . . . ?
C007 N003 C00A C00I 178.1(2) . . . . ?
C007 C009 C00B C00D -178.2(2) . . . . ?
C007 C009 C00B C00H 2.9(4) . . . . ?
C007 C00C C00E C00F 38.6(4) . . . . ?
C007 C00C C00E C00T -144.0(3) . . . . ?
C007 C00C C00J C00H 1.8(4) . . . . ?
C008 N002 C009 C007 0.4(3) . . . . ?
C008 N002 C009 C00B 179.6(2) . . . . ?
C008 N006 C00K N004 -0.2(4) . . . . ?
C008 N006 C00K O005 -179.5(3) . . . . ?
C008 N006 C00P C00W -90.2(3) . . . . ?
C008 C00A C00I O001 178.2(3) . . . . ?
C008 C00A C00I N004 -0.7(3) . . . . ?
C009 N002 C008 N006 -177.1(2) . . . . ?
C009 N002 C008 C00A 3.8(3) . . . . ?
C009 C007 C00C C00E 179.9(2) . . . . ?
C009 C007 C00C C00J 0.4(4) . . . . ?
C009 C00B C00D C00G -135.0(3) . . . . ?
C009 C00B C00D C00N 45.8(4) . . . . ?
C009 C00B C00H C00J -0.8(4) . . . . ?
C00A N003 C007 C009 3.6(3) . . . . ?
C00A N003 C007 C00C -177.0(2) . . . . ?
C00B C00D C00G C00L -179.1(3) . . . . ?
C00B C00D C00N C00S 178.8(3) . . . . ?
C00B C00H C00J C00C -1.6(4) . . . . ?
C00C C007 C009 N002 176.5(2) . . . . ?
C00C C007 C009 C00B -2.8(4) . . . . ?
C00C C00E C00F C00M 175.9(3) . . . . ?
C00C C00E C00T C00V -175.8(3) . . . . ?
C00D C00B C00H C00J -179.7(2) . . . . ?
C00D C00G C00L C00Q 0.3(4) . . . . ?
C00D C00N C00S C00Q 0.3(4) . . . . ?
C00E C00C C00J C00H -177.8(2) . . . . ?
C00E C00F C00M C00R 0.2(4) . . . . ?
C00E C00T C00V C00R -0.6(5) . . . . ?
C00F C00E C00T C00V 1.7(4) . . . . ?
C00F C00M C00R C00V 0.9(5) . . . . ?
C00G C00D C00N C00S -0.4(4) . . . . ?
C00G C00L C00Q C00S -0.3(5) . . . . ?
C00H C00B C00D C00G 43.9(4) . . . . ?
C00H C00B C00D C00N -135.4(3) . . . . ?
C00I N004 C00K O005 177.4(3) . . . . ?
C00I N004 C00K N006 -1.9(4) . . . . ?
C00I N004 C00O C00U -92.1(3) . . . . ?
C00J C00C C00E C00F -141.9(3) . . . . ?
C00J C00C C00E C00T 35.5(4) . . . . ?
C00K N004 C00I O001 -176.6(3) . . . . ?
C00K N004 C00I C00A 2.3(4) . . . . ?
C00K N004 C00O C00U 83.8(3) . . . . ?
C00K N006 C008 N002 -177.5(2) . . . . ?
C00K N006 C008 C00A 1.6(4) . . . . ?
C00K N006 C00P C00W 87.2(3) . . . . ?
C00L C00Q C00S C00N 0.0(5) . . . . ?
C00M C00R C00V C00T -0.7(5) . . . . ?
C00N C00D C00G C00L 0.1(4) . . . . ?
C00O N004 C00I O001 -1.2(4) . . . . ?
C00O N004 C00I C00A 177.7(2) . . . . ?
C00O N004 C00K O005 1.9(4) . . . . ?
C00O N004 C00K N006 -177.4(2) . . . . ?
C00P N006 C008 N002 -0.3(4) . . . . ?
C00P N006 C008 C00A 178.8(2) . . . . ?
C00P N006 C00K N004 -177.4(2) . . . . ?
C00P N006 C00K O005 3.3(4) . . . . ?
C00T C00E C00F C00M -1.5(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Chloroform'
