# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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
_database_code_depnum_ccdc_archive 'CCDC 1840247'
_audit_update_record             
;
2018-04-28 deposited with the CCDC.
2018-06-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C13 H13 N5'
_chemical_formula_sum            'C13 H13 N5'
_chemical_formula_weight         239.28

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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_H-M_alt        'P c c n'
_space_group_name_Hall           '-P 2ab 2ac'

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

_cell_length_a                   16.6173(2)
_cell_length_b                   11.17070(10)
_cell_length_c                   12.4074(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2303.15(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8940
_cell_measurement_theta_min      4.7470
_cell_measurement_theta_max      76.4510

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_F_000             1008
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.146
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.070
_exptl_absorpt_coefficient_mu    0.709
_shelx_estimated_absorpt_T_min   0.904
_shelx_estimated_absorpt_T_max   0.952
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.847
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'CrysAlisPro (Rigaku Oxford Diffraction, 2017)'

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 1 -1 0.0445
-1 5 -3 0.0507
4 5 0 0.0430
5 -4 4 0.0645
-1 -5 2 0.0515
-3 -5 0 0.0312
-5 -3 -2 0.0422
-3 -5 2 0.0524
-1 -5 0 0.0325
0 -5 -2 0.0382
3 -3 -5 0.0542
4 5 -4 0.0530
1 5 0 0.0444
-1 1 0 0.0326
1 -1 0 0.0375
2 -2 5 0.0757
-1 0 5 0.0685
2 5 0 0.0398
0 -1 -5 0.0654

_diffrn_ambient_temperature      100(2)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, AtlasS2'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            AtlasS2
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.2558
_diffrn_reflns_number            14762
_diffrn_reflns_av_unetI/netI     0.0133
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         4.770
_diffrn_reflns_theta_max         67.069
_diffrn_reflns_theta_full        67.069
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2060
_reflns_number_gt                1935
_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       'CrysAlisPro (Rigaku OD, 2017)'
_computing_cell_refinement       'CrysAlisPro (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro (Rigaku OD, 2017)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    
'ORTEP-3 for Windows (Farrugia, 2012), DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0472P)²+0.7780P] 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     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2060
_refine_ls_number_parameters     170
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0317
_refine_ls_wR_factor_ref         0.0854
_refine_ls_wR_factor_gt          0.0832
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.035
_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
N1 N 0.40693(5) 0.27917(8) 0.24618(7) 0.0176(2) Uani 1 1 d . . . . .
N3 N 0.46734(5) 0.40600(8) 0.37903(7) 0.0167(2) Uani 1 1 d . . . . .
N5 N 0.38112(5) 0.25305(8) 0.43389(7) 0.0147(2) Uani 1 1 d . . . . .
N8 N 0.32018(5) 0.12751(8) 0.31922(7) 0.0173(2) Uani 1 1 d . . . . .
N41 N 0.44369(6) 0.37361(8) 0.56088(7) 0.0179(2) Uani 1 1 d D . . . .
H4N1 H 0.4729(7) 0.4372(10) 0.5763(11) 0.022 Uiso 1 1 d D U . . .
H4N2 H 0.4226(7) 0.3289(11) 0.6129(9) 0.022 Uiso 1 1 d D U . . .
C2 C 0.45459(6) 0.36783(9) 0.27665(9) 0.0167(2) Uani 1 1 d . . . . .
C4 C 0.43123(6) 0.34695(9) 0.45876(8) 0.0151(2) Uani 1 1 d . . . . .
C6 C 0.33688(6) 0.17444(9) 0.49678(8) 0.0159(2) Uani 1 1 d . . . . .
H6 H 0.3329 0.1732 0.5732 0.019 Uiso 1 1 calc R U . . .
C7 C 0.30018(6) 0.09899(9) 0.42505(8) 0.0157(2) Uani 1 1 d . . . . .
C9 C 0.36848(6) 0.22020(9) 0.32684(8) 0.0154(2) Uani 1 1 d . . . . .
C21 C 0.50045(7) 0.43297(10) 0.18999(9) 0.0208(3) Uani 1 1 d . . . . .
H21A H 0.5063 0.3797 0.1267 0.025 Uiso 1 1 calc R U . . .
H21B H 0.5551 0.4519 0.2169 0.025 Uiso 1 1 calc R U . . .
C22 C 0.45931(7) 0.54867(11) 0.15474(10) 0.0255(3) Uani 1 1 d . . . . .
H22A H 0.4907 0.5862 0.0970 0.038 Uiso 1 1 calc R U . . .
H22B H 0.4558 0.6035 0.2162 0.038 Uiso 1 1 calc R U . . .
H22C H 0.4051 0.5306 0.1284 0.038 Uiso 1 1 calc R U . . .
C71 C 0.24646(6) -0.00186(9) 0.45002(9) 0.0169(2) Uani 1 1 d . . . . .
C72 C 0.22637(6) -0.02887(10) 0.55665(9) 0.0208(3) Uani 1 1 d . . . . .
H72 H 0.2464 0.0196 0.6135 0.025 Uiso 1 1 calc R U . . .
C73 C 0.17743(7) -0.12572(11) 0.58001(10) 0.0248(3) Uani 1 1 d . . . . .
H73 H 0.1646 -0.1439 0.6528 0.030 Uiso 1 1 calc R U . . .
C74 C 0.14699(7) -0.19640(11) 0.49762(10) 0.0246(3) Uani 1 1 d . . . . .
H74 H 0.1137 -0.2631 0.5139 0.029 Uiso 1 1 calc R U . . .
C75 C 0.16542(7) -0.16931(10) 0.39168(10) 0.0246(3) Uani 1 1 d . . . . .
H75 H 0.1442 -0.2170 0.3350 0.029 Uiso 1 1 calc R U . . .
C76 C 0.21486(7) -0.07275(10) 0.36777(9) 0.0209(3) Uani 1 1 d . . . . .
H76 H 0.2273 -0.0548 0.2948 0.025 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
N1 C2 1.3233(14) . ?
N1 C9 1.3579(14) . ?
N3 C4 1.3318(14) . ?
N3 C2 1.3565(14) . ?
N5 C4 1.3745(14) . ?
N5 C6 1.3858(14) . ?
N5 C9 1.3938(13) . ?
N8 C9 1.3135(14) . ?
N8 C7 1.3914(13) . ?
N41 C4 1.3179(14) . ?
N41 H4N1 0.882(9) . ?
N41 H4N2 0.889(8) . ?
C2 C21 1.5054(15) . ?
C6 C7 1.3691(15) . ?
C6 H6 0.9500 . ?
C7 C71 1.4704(15) . ?
C21 C22 1.5261(16) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C71 C76 1.3944(16) . ?
C71 C72 1.3974(15) . ?
C72 C73 1.3841(16) . ?
C72 H72 0.9500 . ?
C73 C74 1.3872(18) . ?
C73 H73 0.9500 . ?
C74 C75 1.3831(17) . ?
C74 H74 0.9500 . ?
C75 C76 1.3880(16) . ?
C75 H75 0.9500 . ?
C76 H76 0.9500 . ?

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
C2 N1 C9 115.73(9) . . ?
C4 N3 C2 118.01(9) . . ?
C4 N5 C6 132.73(9) . . ?
C4 N5 C9 120.41(9) . . ?
C6 N5 C9 106.85(8) . . ?
C9 N8 C7 104.98(9) . . ?
C4 N41 H4N1 118.5(9) . . ?
C4 N41 H4N2 120.7(9) . . ?
H4N1 N41 H4N2 120.8(12) . . ?
N1 C2 N3 126.60(10) . . ?
N1 C2 C21 117.43(9) . . ?
N3 C2 C21 115.97(9) . . ?
N41 C4 N3 122.10(10) . . ?
N41 C4 N5 118.92(9) . . ?
N3 C4 N5 118.95(9) . . ?
C7 C6 N5 105.09(9) . . ?
C7 C6 H6 127.5 . . ?
N5 C6 H6 127.5 . . ?
C6 C7 N8 111.48(9) . . ?
C6 C7 C71 127.23(10) . . ?
N8 C7 C71 121.29(9) . . ?
N8 C9 N1 128.09(9) . . ?
N8 C9 N5 111.60(9) . . ?
N1 C9 N5 120.25(9) . . ?
C2 C21 C22 112.79(9) . . ?
C2 C21 H21A 109.0 . . ?
C22 C21 H21A 109.0 . . ?
C2 C21 H21B 109.0 . . ?
C22 C21 H21B 109.0 . . ?
H21A C21 H21B 107.8 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C76 C71 C72 118.70(10) . . ?
C76 C71 C7 120.63(10) . . ?
C72 C71 C7 120.66(10) . . ?
C73 C72 C71 120.49(11) . . ?
C73 C72 H72 119.8 . . ?
C71 C72 H72 119.8 . . ?
C72 C73 C74 120.32(11) . . ?
C72 C73 H73 119.8 . . ?
C74 C73 H73 119.8 . . ?
C75 C74 C73 119.67(11) . . ?
C75 C74 H74 120.2 . . ?
C73 C74 H74 120.2 . . ?
C74 C75 C76 120.28(11) . . ?
C74 C75 H75 119.9 . . ?
C76 C75 H75 119.9 . . ?
C75 C76 C71 120.52(11) . . ?
C75 C76 H76 119.7 . . ?
C71 C76 H76 119.7 . . ?

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
C9 N1 C2 N3 -1.21(15) . . . . ?
C9 N1 C2 C21 178.07(9) . . . . ?
C4 N3 C2 N1 2.68(16) . . . . ?
C4 N3 C2 C21 -176.60(9) . . . . ?
C2 N3 C4 N41 176.18(9) . . . . ?
C2 N3 C4 N5 -1.96(14) . . . . ?
C6 N5 C4 N41 0.54(17) . . . . ?
C9 N5 C4 N41 -178.11(9) . . . . ?
C6 N5 C4 N3 178.74(10) . . . . ?
C9 N5 C4 N3 0.09(14) . . . . ?
C4 N5 C6 C7 -178.80(10) . . . . ?
C9 N5 C6 C7 -0.02(10) . . . . ?
N5 C6 C7 N8 0.19(11) . . . . ?
N5 C6 C7 C71 179.61(10) . . . . ?
C9 N8 C7 C6 -0.30(12) . . . . ?
C9 N8 C7 C71 -179.75(9) . . . . ?
C7 N8 C9 N1 177.43(10) . . . . ?
C7 N8 C9 N5 0.28(11) . . . . ?
C2 N1 C9 N8 -177.78(10) . . . . ?
C2 N1 C9 N5 -0.84(14) . . . . ?
C4 N5 C9 N8 178.79(9) . . . . ?
C6 N5 C9 N8 -0.17(12) . . . . ?
C4 N5 C9 N1 1.38(14) . . . . ?
C6 N5 C9 N1 -177.58(9) . . . . ?
N1 C2 C21 C22 97.41(12) . . . . ?
N3 C2 C21 C22 -83.24(12) . . . . ?
C6 C7 C71 C76 -178.55(10) . . . . ?
N8 C7 C71 C76 0.81(15) . . . . ?
C6 C7 C71 C72 1.16(16) . . . . ?
N8 C7 C71 C72 -179.48(9) . . . . ?
C76 C71 C72 C73 1.37(16) . . . . ?
C7 C71 C72 C73 -178.35(10) . . . . ?
C71 C72 C73 C74 -0.72(17) . . . . ?
C72 C73 C74 C75 -0.35(17) . . . . ?
C73 C74 C75 C76 0.74(17) . . . . ?
C74 C75 C76 C71 -0.07(17) . . . . ?
C72 C71 C76 C75 -0.98(16) . . . . ?
C7 C71 C76 C75 178.74(10) . . . . ?

_refine_diff_density_max         0.161
_refine_diff_density_min         -0.227
_refine_diff_density_rms         0.042

####################################################################### 
# 
# 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_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1840248'
_audit_update_record             
;
2018-04-28 deposited with the CCDC.
2018-06-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H17 N5'
_chemical_formula_sum            'C15 H17 N5'
_chemical_formula_weight         267.33

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'

_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                   10.7534(2)
_cell_length_b                   11.8995(2)
_cell_length_c                   12.1124(3)
_cell_angle_alpha                71.918(2)
_cell_angle_beta                 68.962(2)
_cell_angle_gamma                78.712(2)
_cell_volume                     1368.93(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    19802
_cell_measurement_theta_min      3.9050
_cell_measurement_theta_max      76.3900

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_F_000             568
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.128
_exptl_crystal_size_mid          0.064
_exptl_crystal_size_min          0.059
_exptl_absorpt_coefficient_mu    0.650
_shelx_estimated_absorpt_T_min   0.921
_shelx_estimated_absorpt_T_max   0.963
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.760
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'CrysAlisPro (Rigaku Oxford Diffraction, 2017)'

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
3 3 -4 0.0276
0 -5 1 0.0291
2 -5 -1 0.0322
-1 5 0 0.0280
-5 -1 -5 0.0497
2 2 5 0.0270
-2 0 -5 0.0379
0 0 -1 0.0291
1 3 5 0.0147
-3 2 5 0.0192

_diffrn_ambient_temperature      100(2)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, AtlasS2'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            AtlasS2
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.2558
_diffrn_reflns_number            32816
_diffrn_reflns_av_unetI/netI     0.0155
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.925
_diffrn_reflns_theta_max         67.058
_diffrn_reflns_theta_full        67.058
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4893
_reflns_number_gt                4530
_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       'CrysAlisPro (Rigaku OD, 2017)'
_computing_cell_refinement       'CrysAlisPro (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro (Rigaku OD, 2017)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    
'ORTEP-3 for Windows (Farrugia, 2012), DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0507P)²+0.5187P] 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     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4893
_refine_ls_number_parameters     377
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0343
_refine_ls_wR_factor_ref         0.0923
_refine_ls_wR_factor_gt          0.0899
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.028
_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
N1 N 0.30681(10) 0.22094(9) 0.92962(9) 0.0195(2) Uani 1 1 d . . . . .
N3 N 0.12771(10) 0.10560(9) 0.96994(9) 0.0176(2) Uani 1 1 d . . . . .
N5 N 0.34787(9) 0.02649(8) 0.89734(9) 0.0156(2) Uani 1 1 d . . . . .
N8 N 0.52497(10) 0.12671(9) 0.84556(9) 0.0175(2) Uani 1 1 d . . . . .
N41 N 0.17237(10) -0.08232(9) 0.93639(10) 0.0193(2) Uani 1 1 d D . . . .
H4N1 H 0.0858(9) -0.0889(13) 0.9634(13) 0.023 Uiso 1 1 d D U . . .
H4N2 H 0.2304(13) -0.1422(10) 0.9190(13) 0.023 Uiso 1 1 d D U . . .
C2 C 0.17911(12) 0.20241(10) 0.96914(11) 0.0184(2) Uani 1 1 d . . . . .
C4 C 0.21284(11) 0.01660(10) 0.93541(10) 0.0158(2) Uani 1 1 d . . . . .
C6 C 0.45968(11) -0.04716(10) 0.85216(10) 0.0164(2) Uani 1 1 d . . . . .
H6 H 0.4618 -0.1248 0.8448 0.020 Uiso 1 1 calc R U . . .
C7 C 0.56583(11) 0.01621(10) 0.82054(10) 0.0161(2) Uani 1 1 d . . . . .
C9 C 0.39391(12) 0.13073(10) 0.89151(10) 0.0160(2) Uani 1 1 d . . . . .
C21 C 0.07719(12) 0.29596(11) 1.01868(12) 0.0216(3) Uani 1 1 d . . . . .
H21A H 0.1233 0.3501 1.0354 0.026 Uiso 1 1 calc R U . . .
H21B H 0.0130 0.2570 1.0975 0.026 Uiso 1 1 calc R U . . .
C22 C -0.00030(12) 0.36906(12) 0.93220(12) 0.0243(3) Uani 1 1 d . . . . .
H22A H -0.0385 0.3144 0.9085 0.029 Uiso 1 1 calc R U . . .
H22B H -0.0757 0.4180 0.9764 0.029 Uiso 1 1 calc R U . . .
C23 C 0.08471(14) 0.44996(13) 0.81690(13) 0.0320(3) Uani 1 1 d . . . . .
H23A H 0.0291 0.4953 0.7660 0.048 Uiso 1 1 calc R U . . .
H23B H 0.1575 0.4020 0.7708 0.048 Uiso 1 1 calc R U . . .
H23C H 0.1224 0.5049 0.8395 0.048 Uiso 1 1 calc R U . . .
C71 C 0.70774(12) -0.02090(10) 0.76544(10) 0.0175(2) Uani 1 1 d . . . . .
C72 C 0.74616(13) -0.11190(12) 0.70629(12) 0.0244(3) Uani 1 1 d . . . . .
H72 H 0.6797 -0.1506 0.7013 0.029 Uiso 1 1 calc R U . . .
C73 C 0.88048(13) -0.14629(12) 0.65477(13) 0.0292(3) Uani 1 1 d . . . . .
H73 H 0.9045 -0.2079 0.6143 0.035 Uiso 1 1 calc R U . . .
C74 C 0.98115(12) -0.09241(12) 0.66097(12) 0.0256(3) Uani 1 1 d . . . . .
C75 C 0.94199(12) -0.00200(11) 0.71994(12) 0.0235(3) Uani 1 1 d . . . . .
H75 H 1.0086 0.0362 0.7254 0.028 Uiso 1 1 calc R U . . .
C76 C 0.80809(12) 0.03391(11) 0.77106(11) 0.0194(2) Uani 1 1 d . . . . .
H76 H 0.7844 0.0964 0.8103 0.023 Uiso 1 1 calc R U . . .
C77 C 1.12646(13) -0.13115(14) 0.60478(15) 0.0358(3) Uani 1 1 d . . . . .
H77A H 1.1814 -0.1002 0.6360 0.054 Uiso 1 1 calc R U . . .
H77B H 1.1523 -0.1003 0.5154 0.054 Uiso 1 1 calc R U . . .
H77C H 1.1402 -0.2181 0.6263 0.054 Uiso 1 1 calc R U . . .
N1A N 0.57458(10) 0.22902(9) 0.32330(9) 0.0178(2) Uani 1 1 d . . . . .
N3A N 0.53324(9) 0.37799(9) 0.43046(9) 0.0162(2) Uani 1 1 d . . . . .
N5A N 0.59221(9) 0.43493(8) 0.21712(9) 0.0144(2) Uani 1 1 d . . . . .
N8A N 0.63878(10) 0.30488(8) 0.10559(9) 0.0162(2) Uani 1 1 d . . . . .
N41A N 0.55275(11) 0.57612(9) 0.32541(9) 0.0198(2) Uani 1 1 d D . . . .
H4N3 H 0.5249(14) 0.5922(13) 0.3968(10) 0.024 Uiso 1 1 d D U . . .
H4N4 H 0.5656(15) 0.6331(11) 0.2562(10) 0.024 Uiso 1 1 d D U . . .
C6A C 0.62490(11) 0.50109(10) 0.09509(10) 0.0148(2) Uani 1 1 d . . . . .
H6A H 0.6276 0.5847 0.0644 0.018 Uiso 1 1 calc R U . . .
C2A C 0.54227(11) 0.26425(10) 0.42406(10) 0.0163(2) Uani 1 1 d . . . . .
C4A C 0.55816(11) 0.46393(10) 0.32621(10) 0.0153(2) Uani 1 1 d . . . . .
C7A C 0.65218(11) 0.41958(10) 0.02906(10) 0.0146(2) Uani 1 1 d . . . . .
C9A C 0.60132(11) 0.31628(10) 0.21791(10) 0.0150(2) Uani 1 1 d . . . . .
C21A C 0.51288(12) 0.16843(10) 0.54298(11) 0.0197(3) Uani 1 1 d . . . . .
H21C H 0.5061 0.2023 0.6102 0.024 Uiso 1 1 calc R U . . .
H21D H 0.5881 0.1051 0.5377 0.024 Uiso 1 1 calc R U . . .
C22A C 0.38314(13) 0.11422(11) 0.57314(12) 0.0253(3) Uani 1 1 d . . . . .
H22C H 0.3832 0.0932 0.5002 0.030 Uiso 1 1 calc R U . . .
H22D H 0.3791 0.0402 0.6400 0.030 Uiso 1 1 calc R U . . .
C23A C 0.26011(15) 0.19847(14) 0.61199(15) 0.0377(4) Uani 1 1 d . . . . .
H23D H 0.1798 0.1631 0.6235 0.057 Uiso 1 1 calc R U . . .
H23E H 0.2665 0.2739 0.5484 0.057 Uiso 1 1 calc R U . . .
H23F H 0.2545 0.2128 0.6891 0.057 Uiso 1 1 calc R U . . .
C71A C 0.69252(11) 0.43796(10) -0.10429(10) 0.0154(2) Uani 1 1 d . . . . .
C72A C 0.73032(12) 0.54644(11) -0.18662(11) 0.0195(2) Uani 1 1 d . . . . .
H72A H 0.7265 0.6125 -0.1568 0.023 Uiso 1 1 calc R U . . .
C73A C 0.77352(13) 0.55839(11) -0.31198(11) 0.0225(3) Uani 1 1 d . . . . .
H73A H 0.7992 0.6329 -0.3668 0.027 Uiso 1 1 calc R U . . .
C74A C 0.78020(12) 0.46388(11) -0.35934(11) 0.0203(3) Uani 1 1 d . . . . .
C75A C 0.73798(13) 0.35715(11) -0.27633(11) 0.0234(3) Uani 1 1 d . . . . .
H75A H 0.7387 0.2919 -0.3062 0.028 Uiso 1 1 calc R U . . .
C76A C 0.69499(13) 0.34405(11) -0.15131(11) 0.0208(3) Uani 1 1 d . . . . .
H76A H 0.6668 0.2701 -0.0967 0.025 Uiso 1 1 calc R U . . .
C77A C 0.82789(14) 0.47513(12) -0.49518(12) 0.0279(3) Uani 1 1 d . . . . .
H77D H 0.8754 0.3997 -0.5109 0.042 Uiso 1 1 calc R U . . .
H77E H 0.8884 0.5380 -0.5378 0.042 Uiso 1 1 calc R U . . .
H77F H 0.7508 0.4950 -0.5251 0.042 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
N1 C2 1.3207(16) . ?
N1 C9 1.3587(15) . ?
N3 C4 1.3249(15) . ?
N3 C2 1.3679(16) . ?
N5 C4 1.3738(15) . ?
N5 C6 1.3878(15) . ?
N5 C9 1.3963(15) . ?
N8 C9 1.3134(15) . ?
N8 C7 1.3927(15) . ?
N41 C4 1.3280(16) . ?
N41 H4N1 0.880(9) . ?
N41 H4N2 0.875(9) . ?
C2 C21 1.5052(16) . ?
C6 C7 1.3646(16) . ?
C6 H6 0.9500 . ?
C7 C71 1.4687(16) . ?
C21 C22 1.5250(18) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.519(2) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C71 C76 1.3965(17) . ?
C71 C72 1.3966(17) . ?
C72 C73 1.3868(18) . ?
C72 H72 0.9500 . ?
C73 C74 1.3959(19) . ?
C73 H73 0.9500 . ?
C74 C75 1.3888(19) . ?
C74 C77 1.5055(18) . ?
C75 C76 1.3866(18) . ?
C75 H75 0.9500 . ?
C76 H76 0.9500 . ?
C77 H77A 0.9800 . ?
C77 H77B 0.9800 . ?
C77 H77C 0.9800 . ?
N1A C2A 1.3199(15) . ?
N1A C9A 1.3495(15) . ?
N3A C4A 1.3322(15) . ?
N3A C2A 1.3622(15) . ?
N5A C4A 1.3731(15) . ?
N5A C9A 1.3932(14) . ?
N5A C6A 1.3933(14) . ?
N8A C9A 1.3158(15) . ?
N8A C7A 1.3924(15) . ?
N41A C4A 1.3220(15) . ?
N41A H4N3 0.876(9) . ?
N41A H4N4 0.884(9) . ?
C6A C7A 1.3667(16) . ?
C6A H6A 0.9500 . ?
C2A C21A 1.5065(16) . ?
C7A C71A 1.4696(16) . ?
C21A C22A 1.5284(18) . ?
C21A H21C 0.9900 . ?
C21A H21D 0.9900 . ?
C22A C23A 1.518(2) . ?
C22A H22C 0.9900 . ?
C22A H22D 0.9900 . ?
C23A H23D 0.9800 . ?
C23A H23E 0.9800 . ?
C23A H23F 0.9800 . ?
C71A C76A 1.3952(17) . ?
C71A C72A 1.3933(17) . ?
C72A C73A 1.3882(17) . ?
C72A H72A 0.9500 . ?
C73A C74A 1.3922(18) . ?
C73A H73A 0.9500 . ?
C74A C75A 1.3912(18) . ?
C74A C77A 1.5074(17) . ?
C75A C76A 1.3821(17) . ?
C75A H75A 0.9500 . ?
C76A H76A 0.9500 . ?
C77A H77D 0.9800 . ?
C77A H77E 0.9800 . ?
C77A H77F 0.9800 . ?

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
C2 N1 C9 115.12(10) . . ?
C4 N3 C2 117.99(10) . . ?
C4 N5 C6 132.77(10) . . ?
C4 N5 C9 120.12(10) . . ?
C6 N5 C9 106.97(9) . . ?
C9 N8 C7 105.04(9) . . ?
C4 N41 H4N1 117.9(10) . . ?
C4 N41 H4N2 120.6(10) . . ?
H4N1 N41 H4N2 121.1(14) . . ?
N1 C2 N3 126.70(11) . . ?
N1 C2 C21 118.05(11) . . ?
N3 C2 C21 115.25(10) . . ?
N3 C4 N41 122.32(11) . . ?
N3 C4 N5 119.07(10) . . ?
N41 C4 N5 118.61(10) . . ?
C7 C6 N5 104.97(10) . . ?
C7 C6 H6 127.5 . . ?
N5 C6 H6 127.5 . . ?
C6 C7 N8 111.68(10) . . ?
C6 C7 C71 126.93(11) . . ?
N8 C7 C71 121.39(10) . . ?
N8 C9 N1 127.85(11) . . ?
N8 C9 N5 111.34(10) . . ?
N1 C9 N5 120.81(10) . . ?
C2 C21 C22 113.56(10) . . ?
C2 C21 H21A 108.9 . . ?
C22 C21 H21A 108.9 . . ?
C2 C21 H21B 108.9 . . ?
C22 C21 H21B 108.9 . . ?
H21A C21 H21B 107.7 . . ?
C23 C22 C21 113.44(11) . . ?
C23 C22 H22A 108.9 . . ?
C21 C22 H22A 108.9 . . ?
C23 C22 H22B 108.9 . . ?
C21 C22 H22B 108.9 . . ?
H22A C22 H22B 107.7 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C76 C71 C72 118.17(11) . . ?
C76 C71 C7 120.76(11) . . ?
C72 C71 C7 121.07(11) . . ?
C73 C72 C71 120.55(12) . . ?
C73 C72 H72 119.7 . . ?
C71 C72 H72 119.7 . . ?
C72 C73 C74 121.50(12) . . ?
C72 C73 H73 119.2 . . ?
C74 C73 H73 119.2 . . ?
C75 C74 C73 117.54(12) . . ?
C75 C74 C77 121.71(12) . . ?
C73 C74 C77 120.76(13) . . ?
C76 C75 C74 121.58(12) . . ?
C76 C75 H75 119.2 . . ?
C74 C75 H75 119.2 . . ?
C75 C76 C71 120.66(12) . . ?
C75 C76 H76 119.7 . . ?
C71 C76 H76 119.7 . . ?
C74 C77 H77A 109.5 . . ?
C74 C77 H77B 109.5 . . ?
H77A C77 H77B 109.5 . . ?
C74 C77 H77C 109.5 . . ?
H77A C77 H77C 109.5 . . ?
H77B C77 H77C 109.5 . . ?
C2A N1A C9A 115.16(10) . . ?
C4A N3A C2A 118.19(10) . . ?
C4A N5A C9A 119.28(10) . . ?
C4A N5A C6A 133.51(10) . . ?
C9A N5A C6A 107.19(9) . . ?
C9A N8A C7A 105.70(9) . . ?
C4A N41A H4N3 116.9(10) . . ?
C4A N41A H4N4 120.9(10) . . ?
H4N3 N41A H4N4 121.6(14) . . ?
C7A C6A N5A 105.01(9) . . ?
C7A C6A H6A 127.5 . . ?
N5A C6A H6A 127.5 . . ?
N1A C2A N3A 126.38(11) . . ?
N1A C2A C21A 116.23(10) . . ?
N3A C2A C21A 117.40(10) . . ?
N41A C4A N3A 121.47(10) . . ?
N41A C4A N5A 119.35(10) . . ?
N3A C4A N5A 119.17(10) . . ?
C6A C7A N8A 111.19(10) . . ?
C6A C7A C71A 129.38(10) . . ?
N8A C7A C71A 119.42(10) . . ?
N8A C9A N1A 127.31(10) . . ?
N8A C9A N5A 110.89(10) . . ?
N1A C9A N5A 121.81(10) . . ?
C2A C21A C22A 112.30(10) . . ?
C2A C21A H21C 109.1 . . ?
C22A C21A H21C 109.1 . . ?
C2A C21A H21D 109.1 . . ?
C22A C21A H21D 109.1 . . ?
H21C C21A H21D 107.9 . . ?
C23A C22A C21A 112.15(11) . . ?
C23A C22A H22C 109.2 . . ?
C21A C22A H22C 109.2 . . ?
C23A C22A H22D 109.2 . . ?
C21A C22A H22D 109.2 . . ?
H22C C22A H22D 107.9 . . ?
C22A C23A H23D 109.5 . . ?
C22A C23A H23E 109.5 . . ?
H23D C23A H23E 109.5 . . ?
C22A C23A H23F 109.5 . . ?
H23D C23A H23F 109.5 . . ?
H23E C23A H23F 109.5 . . ?
C76A C71A C72A 118.28(11) . . ?
C76A C71A C7A 119.54(10) . . ?
C72A C71A C7A 122.18(10) . . ?
C73A C72A C71A 120.27(11) . . ?
C73A C72A H72A 119.9 . . ?
C71A C72A H72A 119.9 . . ?
C72A C73A C74A 121.65(11) . . ?
C72A C73A H73A 119.2 . . ?
C74A C73A H73A 119.2 . . ?
C73A C74A C75A 117.54(11) . . ?
C73A C74A C77A 122.30(11) . . ?
C75A C74A C77A 120.14(11) . . ?
C76A C75A C74A 121.34(11) . . ?
C76A C75A H75A 119.3 . . ?
C74A C75A H75A 119.3 . . ?
C75A C76A C71A 120.86(11) . . ?
C75A C76A H76A 119.6 . . ?
C71A C76A H76A 119.6 . . ?
C74A C77A H77D 109.5 . . ?
C74A C77A H77E 109.5 . . ?
H77D C77A H77E 109.5 . . ?
C74A C77A H77F 109.5 . . ?
H77D C77A H77F 109.5 . . ?
H77E C77A H77F 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
C9 N1 C2 N3 -3.12(17) . . . . ?
C9 N1 C2 C21 177.02(10) . . . . ?
C4 N3 C2 N1 4.73(18) . . . . ?
C4 N3 C2 C21 -175.41(10) . . . . ?
C2 N3 C4 N41 178.11(11) . . . . ?
C2 N3 C4 N5 -1.79(16) . . . . ?
C6 N5 C4 N3 -177.13(11) . . . . ?
C9 N5 C4 N3 -2.10(16) . . . . ?
C6 N5 C4 N41 2.96(19) . . . . ?
C9 N5 C4 N41 178.00(10) . . . . ?
C4 N5 C6 C7 174.84(11) . . . . ?
C9 N5 C6 C7 -0.67(12) . . . . ?
N5 C6 C7 N8 0.71(13) . . . . ?
N5 C6 C7 C71 -178.63(10) . . . . ?
C9 N8 C7 C6 -0.47(13) . . . . ?
C9 N8 C7 C71 178.92(10) . . . . ?
C7 N8 C9 N1 -179.41(11) . . . . ?
C7 N8 C9 N5 0.02(12) . . . . ?
C2 N1 C9 N8 178.23(11) . . . . ?
C2 N1 C9 N5 -1.15(16) . . . . ?
C4 N5 C9 N8 -175.77(10) . . . . ?
C6 N5 C9 N8 0.42(13) . . . . ?
C4 N5 C9 N1 3.70(16) . . . . ?
C6 N5 C9 N1 179.89(10) . . . . ?
N1 C2 C21 C22 105.99(13) . . . . ?
N3 C2 C21 C22 -73.89(14) . . . . ?
C2 C21 C22 C23 -68.78(14) . . . . ?
C6 C7 C71 C76 -160.61(12) . . . . ?
N8 C7 C71 C76 20.10(16) . . . . ?
C6 C7 C71 C72 19.27(18) . . . . ?
N8 C7 C71 C72 -160.02(11) . . . . ?
C76 C71 C72 C73 -0.02(19) . . . . ?
C7 C71 C72 C73 -179.90(12) . . . . ?
C71 C72 C73 C74 0.5(2) . . . . ?
C72 C73 C74 C75 -0.5(2) . . . . ?
C72 C73 C74 C77 179.84(13) . . . . ?
C73 C74 C75 C76 0.03(19) . . . . ?
C77 C74 C75 C76 179.66(12) . . . . ?
C74 C75 C76 C71 0.47(19) . . . . ?
C72 C71 C76 C75 -0.47(18) . . . . ?
C7 C71 C76 C75 179.42(11) . . . . ?
C4A N5A C6A C7A 178.54(11) . . . . ?
C9A N5A C6A C7A -0.15(11) . . . . ?
C9A N1A C2A N3A 0.36(17) . . . . ?
C9A N1A C2A C21A -179.58(10) . . . . ?
C4A N3A C2A N1A 0.44(17) . . . . ?
C4A N3A C2A C21A -179.62(10) . . . . ?
C2A N3A C4A N41A -179.23(10) . . . . ?
C2A N3A C4A N5A -0.24(15) . . . . ?
C9A N5A C4A N41A 178.31(10) . . . . ?
C6A N5A C4A N41A -0.25(18) . . . . ?
C9A N5A C4A N3A -0.70(15) . . . . ?
C6A N5A C4A N3A -179.27(11) . . . . ?
N5A C6A C7A N8A -0.53(12) . . . . ?
N5A C6A C7A C71A -179.89(10) . . . . ?
C9A N8A C7A C6A 1.03(12) . . . . ?
C9A N8A C7A C71A -179.54(10) . . . . ?
C7A N8A C9A N1A 179.27(11) . . . . ?
C7A N8A C9A N5A -1.12(12) . . . . ?
C2A N1A C9A N8A 178.24(11) . . . . ?
C2A N1A C9A N5A -1.34(16) . . . . ?
C4A N5A C9A N8A -178.09(9) . . . . ?
C6A N5A C9A N8A 0.83(12) . . . . ?
C4A N5A C9A N1A 1.55(16) . . . . ?
C6A N5A C9A N1A -179.53(10) . . . . ?
N1A C2A C21A C22A -68.91(13) . . . . ?
N3A C2A C21A C22A 111.14(12) . . . . ?
C2A C21A C22A C23A -72.27(13) . . . . ?
C6A C7A C71A C76A -169.97(12) . . . . ?
N8A C7A C71A C76A 10.72(16) . . . . ?
C6A C7A C71A C72A 10.78(18) . . . . ?
N8A C7A C71A C72A -168.53(10) . . . . ?
C76A C71A C72A C73A -2.18(17) . . . . ?
C7A C71A C72A C73A 177.08(11) . . . . ?
C71A C72A C73A C74A 0.18(19) . . . . ?
C72A C73A C74A C75A 1.92(18) . . . . ?
C72A C73A C74A C77A -179.51(12) . . . . ?
C73A C74A C75A C76A -2.03(19) . . . . ?
C77A C74A C75A C76A 179.37(12) . . . . ?
C74A C75A C76A C71A 0.05(19) . . . . ?
C72A C71A C76A C75A 2.07(18) . . . . ?
C7A C71A C76A C75A -177.20(11) . . . . ?

_refine_diff_density_max         0.293
_refine_diff_density_min         -0.241
_refine_diff_density_rms         0.041

