# Supplementary Information (SI) for Organic & Biomolecular Chemistry.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_L3357
_database_code_depnum_ccdc_archive 'CCDC 2361716'
loop_
_audit_author_name
_audit_author_address
'Mikhail Grigoriev'
;IPCE RAS
Russia
;
_audit_update_record             
;
2024-06-10 deposited with the CCDC.	2024-10-14 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         ?
_chemical_formula_sum            'C12 H22 N6 S2'
_chemical_formula_weight         314.47

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   9.7250(3)
_cell_length_b                   9.1469(2)
_cell_length_c                   18.4748(5)
_cell_angle_alpha                90
_cell_angle_beta                 97.306(1)
_cell_angle_gamma                90
_cell_volume                     1630.06(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9951
_cell_measurement_theta_min      2.49
_cell_measurement_theta_max      29.85

_exptl_crystal_description       bulk
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_F_000             672
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.380
_exptl_crystal_size_min          0.340
_exptl_absorpt_coefficient_mu    0.327
_shelx_estimated_absorpt_T_min   0.880
_shelx_estimated_absorpt_T_max   0.897
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.670
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  
'Bruker KAPPA APEX II area-detector diffractometer'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            31725
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.630
_diffrn_reflns_theta_max         29.998
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             4733
_reflns_number_gt                3686
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_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)+(0.0720P)²+1.1165P] 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         4733
_refine_ls_number_parameters     197
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0604
_refine_ls_wR_factor_ref         0.1714
_refine_ls_wR_factor_gt          0.1587
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.001
_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
S1 S -0.15176(6) 0.27717(10) 0.55746(6) 0.0851(3) Uani 1 1 d . . . . .
S2 S 0.68598(5) 0.58630(6) 0.69270(3) 0.04785(17) Uani 1 1 d . . . . .
N1 N 0.12661(19) 0.5423(2) 0.65556(13) 0.0545(5) Uani 1 1 d . . . . .
N2 N -0.00067(18) 0.4832(2) 0.62782(12) 0.0519(5) Uani 1 1 d D . . . .
H2 H -0.073(2) 0.516(3) 0.6392(15) 0.062 Uiso 1 1 d D U . . .
N4 N 0.11883(19) 0.3183(2) 0.56835(14) 0.0602(6) Uani 1 1 d D . . . .
H4 H 0.188(3) 0.373(3) 0.5809(17) 0.072 Uiso 1 1 d D U . . .
N8 N 0.40936(18) 0.3447(2) 0.57491(11) 0.0537(5) Uani 1 1 d . . . . .
N9 N 0.53505(17) 0.4059(2) 0.60395(10) 0.0454(4) Uani 1 1 d D . . . .
H9 H 0.610(2) 0.384(3) 0.5908(14) 0.054 Uiso 1 1 d D U . . .
N11 N 0.41853(19) 0.5234(3) 0.68529(12) 0.0609(6) Uani 1 1 d D . . . .
H11 H 0.352(3) 0.477(3) 0.6630(16) 0.073 Uiso 1 1 d D U . . .
C3 C -0.0019(2) 0.3612(3) 0.58598(13) 0.0473(5) Uani 1 1 d . . . . .
C5 C 0.1493(2) 0.1816(3) 0.53327(13) 0.0490(5) Uani 1 1 d . . . . .
H5 H 0.065306 0.151037 0.501910 0.059 Uiso 1 1 calc R U . . .
C6 C 0.2633(3) 0.2067(4) 0.48464(14) 0.0612(7) Uani 1 1 d . . . . .
H6A H 0.279440 0.114312 0.461382 0.073 Uiso 1 1 calc R U . . .
H6B H 0.226851 0.273765 0.446244 0.073 Uiso 1 1 calc R U . . .
C7 C 0.4025(2) 0.2649(3) 0.51785(12) 0.0482(5) Uani 1 1 d . . . . .
C10 C 0.53738(19) 0.5014(2) 0.65983(11) 0.0384(4) Uani 1 1 d . . . . .
C12 C 0.3902(2) 0.6197(3) 0.74405(13) 0.0501(5) Uani 1 1 d . . . . .
H12 H 0.473510 0.678294 0.758564 0.060 Uiso 1 1 calc R U . . .
C13 C 0.2734(3) 0.7228(3) 0.71939(18) 0.0634(7) Uani 1 1 d . . . . .
H13A H 0.302680 0.783929 0.681254 0.076 Uiso 1 1 calc R U . . .
H13B H 0.261499 0.786466 0.760127 0.076 Uiso 1 1 calc R U . . .
C14 C 0.1327(2) 0.6607(3) 0.69110(14) 0.0497(5) Uani 1 1 d . . . . .
C15 C 0.1858(4) 0.0640(4) 0.58877(19) 0.0792(9) Uani 1 1 d . . . . .
H15A H 0.112184 0.053575 0.618428 0.119 Uiso 1 1 calc R U . . .
H15B H 0.269891 0.089817 0.619078 0.119 Uiso 1 1 calc R U . . .
H15C H 0.198716 -0.026670 0.564382 0.119 Uiso 1 1 calc R U . . .
C16 C 0.5205(3) 0.2274(4) 0.47860(15) 0.0642(7) Uani 1 1 d . . . . .
H16A H 0.578805 0.311642 0.476613 0.096 Uiso 1 1 calc R U . . .
H16B H 0.486582 0.196691 0.429909 0.096 Uiso 1 1 calc R U . . .
H16C H 0.572874 0.149619 0.503710 0.096 Uiso 1 1 calc R U . . .
C17 C 0.3635(4) 0.5274(4) 0.80886(17) 0.0822(9) Uani 1 1 d . . . . .
H17A H 0.441198 0.463919 0.822280 0.123 Uiso 1 1 calc R U . . .
H17B H 0.281485 0.469771 0.796156 0.123 Uiso 1 1 calc R U . . .
H17C H 0.350968 0.589929 0.849234 0.123 Uiso 1 1 calc R U . . .
C18 C 0.0114(3) 0.7494(4) 0.7067(3) 0.0946(13) Uani 1 1 d . . . . .
H18A H -0.054945 0.755073 0.663657 0.142 Uiso 1 1 calc R U . . .
H18B H 0.041695 0.846123 0.721334 0.142 Uiso 1 1 calc R U . . .
H18C H -0.030831 0.704242 0.745324 0.142 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
S1 C3 1.672(2) . ?
S2 C10 1.684(2) . ?
N1 C14 1.264(3) . ?
N1 N2 1.388(2) . ?
N2 C3 1.357(3) . ?
N2 H2 0.819(17) . ?
N4 C3 1.318(3) . ?
N4 C5 1.455(3) . ?
N4 H4 0.845(18) . ?
N8 C7 1.277(3) . ?
N8 N9 1.389(2) . ?
N9 C10 1.350(3) . ?
N9 H9 0.825(17) . ?
N11 C10 1.317(3) . ?
N11 C12 1.452(3) . ?
N11 H11 0.836(18) . ?
C5 C15 1.497(4) . ?
C5 C6 1.531(3) . ?
C5 H5 0.9800 . ?
C6 C7 1.510(3) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C16 1.473(3) . ?
C12 C13 1.501(4) . ?
C12 C17 1.514(4) . ?
C12 H12 0.9800 . ?
C13 C14 1.512(3) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C18 1.490(4) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 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
C14 N1 N2 120.43(19) . . ?
C3 N2 N1 118.28(18) . . ?
C3 N2 H2 120(2) . . ?
N1 N2 H2 121(2) . . ?
C3 N4 C5 127.17(19) . . ?
C3 N4 H4 117(2) . . ?
C5 N4 H4 116(2) . . ?
C7 N8 N9 120.02(18) . . ?
C10 N9 N8 118.98(17) . . ?
C10 N9 H9 117(2) . . ?
N8 N9 H9 124(2) . . ?
C10 N11 C12 128.19(18) . . ?
C10 N11 H11 114(2) . . ?
C12 N11 H11 118(2) . . ?
N4 C3 N2 116.26(18) . . ?
N4 C3 S1 123.59(17) . . ?
N2 C3 S1 120.12(16) . . ?
N4 C5 C15 110.8(2) . . ?
N4 C5 C6 109.6(2) . . ?
C15 C5 C6 112.5(2) . . ?
N4 C5 H5 107.9 . . ?
C15 C5 H5 107.9 . . ?
C6 C5 H5 107.9 . . ?
C7 C6 C5 119.55(19) . . ?
C7 C6 H6A 107.4 . . ?
C5 C6 H6A 107.4 . . ?
C7 C6 H6B 107.4 . . ?
C5 C6 H6B 107.4 . . ?
H6A C6 H6B 107.0 . . ?
N8 C7 C16 125.2(2) . . ?
N8 C7 C6 119.1(2) . . ?
C16 C7 C6 115.6(2) . . ?
N11 C10 N9 116.20(18) . . ?
N11 C10 S2 123.53(16) . . ?
N9 C10 S2 120.27(15) . . ?
N11 C12 C13 111.3(2) . . ?
N11 C12 C17 108.7(2) . . ?
C13 C12 C17 113.0(2) . . ?
N11 C12 H12 107.9 . . ?
C13 C12 H12 107.9 . . ?
C17 C12 H12 107.9 . . ?
C12 C13 C14 119.0(2) . . ?
C12 C13 H13A 107.6 . . ?
C14 C13 H13A 107.6 . . ?
C12 C13 H13B 107.6 . . ?
C14 C13 H13B 107.6 . . ?
H13A C13 H13B 107.0 . . ?
N1 C14 C18 125.5(2) . . ?
N1 C14 C13 118.8(2) . . ?
C18 C14 C13 115.6(2) . . ?
C5 C15 H15A 109.5 . . ?
C5 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C5 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C7 C16 H16A 109.5 . . ?
C7 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C7 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C12 C17 H17A 109.5 . . ?
C12 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C12 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C14 C18 H18A 109.5 . . ?
C14 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C14 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 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
C14 N1 N2 C3 175.7(2) . . . . ?
C7 N8 N9 C10 173.5(2) . . . . ?
C5 N4 C3 N2 170.6(3) . . . . ?
C5 N4 C3 S1 -11.4(4) . . . . ?
N1 N2 C3 N4 -7.4(4) . . . . ?
N1 N2 C3 S1 174.5(2) . . . . ?
C3 N4 C5 C15 -87.8(3) . . . . ?
C3 N4 C5 C6 147.4(3) . . . . ?
N4 C5 C6 C7 58.6(3) . . . . ?
C15 C5 C6 C7 -65.2(3) . . . . ?
N9 N8 C7 C16 1.1(4) . . . . ?
N9 N8 C7 C6 -176.4(2) . . . . ?
C5 C6 C7 N8 -27.6(4) . . . . ?
C5 C6 C7 C16 154.6(3) . . . . ?
C12 N11 C10 N9 -179.5(3) . . . . ?
C12 N11 C10 S2 -0.2(4) . . . . ?
N8 N9 C10 N11 3.4(3) . . . . ?
N8 N9 C10 S2 -175.90(17) . . . . ?
C10 N11 C12 C13 125.7(3) . . . . ?
C10 N11 C12 C17 -109.2(3) . . . . ?
N11 C12 C13 C14 59.6(3) . . . . ?
C17 C12 C13 C14 -63.1(3) . . . . ?
N2 N1 C14 C18 -0.6(5) . . . . ?
N2 N1 C14 C13 -179.0(2) . . . . ?
C12 C13 C14 N1 -34.6(4) . . . . ?
C12 C13 C14 C18 146.9(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N2 H2 S2 0.819(17) 2.732(18) 3.5413(19) 170(3) 1_455 yes
N4 H4 N8 0.845(18) 2.19(3) 2.823(2) 132(3) . yes
N9 H9 S1 0.825(17) 2.655(18) 3.4738(18) 172(3) 1_655 yes
N11 H11 N1 0.836(18) 2.26(3) 2.827(3) 125(3) . yes
N11 H11 N8 0.836(18) 2.16(3) 2.606(3) 114(3) . yes

_refine_diff_density_max         0.630
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.057

####################################################################### 
# 
# 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_L4132_LT
_database_code_depnum_ccdc_archive 'CCDC 2361717'
loop_
_audit_author_name
_audit_author_address
'Mikhail Grigoriev'
;IPCE RAS
Russia
;
_audit_update_record             
;
2024-06-10 deposited with the CCDC.	2024-10-14 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         ?
_chemical_formula_sum            'C21 H40 N10 O S3'
_chemical_formula_weight         544.81

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

_cell_length_a                   12.8167(4)
_cell_length_b                   11.8970(4)
_cell_length_c                   18.1261(6)
_cell_angle_alpha                90
_cell_angle_beta                 90.928(1)
_cell_angle_gamma                90
_cell_volume                     2763.51(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9841
_cell_measurement_theta_min      3.18
_cell_measurement_theta_max      25.06

_exptl_crystal_description       fragment
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_F_000             1168
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    0.303
_shelx_estimated_absorpt_T_min   0.948
_shelx_estimated_absorpt_T_max   0.959
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.917
_exptl_absorpt_correction_T_max  0.959
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  
'Bruker KAPPA APEX II area-detector diffractometer'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            100195
_diffrn_reflns_av_unetI/netI     0.0616
_diffrn_reflns_av_R_equivalents  0.1133
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.425
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             8049
_reflns_number_gt                5621
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_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)+(0.0302P)²+2.0086P] 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         8049
_refine_ls_number_parameters     357
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0490
_refine_ls_wR_factor_ref         0.0980
_refine_ls_wR_factor_gt          0.0867
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.001
_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
S2 S -0.10251(4) 0.64042(4) 0.69764(3) 0.01615(11) Uani 1 1 d . . . . .
S1 S 0.34335(4) 0.47685(4) 0.62340(3) 0.01695(11) Uani 1 1 d . . . . .
S3 S 0.11851(4) 0.97044(4) 0.41204(3) 0.01704(11) Uani 1 1 d . . . . .
O1 O 0.44862(10) 0.75798(12) 0.56448(8) 0.0207(3) Uani 1 1 d D . . . .
N1 N 0.29241(12) 0.57072(13) 0.41911(8) 0.0148(3) Uani 1 1 d . . . . .
N2 N 0.32981(13) 0.56943(14) 0.49105(9) 0.0146(3) Uani 1 1 d . . . . .
H2 H 0.3652(17) 0.6231(19) 0.5116(12) 0.017 Uiso 1 1 d . U . . .
N3 N 0.51003(13) 0.72527(15) 0.68155(10) 0.0235(4) Uani 1 1 d D . . . .
N4 N 0.25275(12) 0.39743(13) 0.49968(9) 0.0126(3) Uani 1 1 d . . . . .
H4 H 0.2424(16) 0.4055(18) 0.4543(12) 0.015 Uiso 1 1 d . U . . .
N8 N 0.05685(12) 0.41257(13) 0.59197(8) 0.0126(3) Uani 1 1 d . . . . .
N9 N -0.02207(12) 0.48189(13) 0.61694(9) 0.0129(3) Uani 1 1 d . . . . .
H9 H -0.0856(17) 0.4704(18) 0.6065(11) 0.016 Uiso 1 1 d . U . . .
N11 N 0.09912(12) 0.57907(13) 0.68589(8) 0.0125(3) Uani 1 1 d . . . . .
H11 H 0.1410(16) 0.5362(18) 0.6648(11) 0.015 Uiso 1 1 d . U . . .
N15 N 0.20007(11) 0.83710(12) 0.60063(8) 0.0119(3) Uani 1 1 d . . . . .
N16 N 0.15330(12) 0.90944(13) 0.54990(8) 0.0129(3) Uani 1 1 d . . . . .
H16 H 0.0920(17) 0.9350(18) 0.5560(11) 0.015 Uiso 1 1 d . U . . .
N18 N 0.28182(12) 0.85822(13) 0.47029(9) 0.0133(3) Uani 1 1 d . . . . .
H18 H 0.3131(16) 0.8354(18) 0.5086(12) 0.016 Uiso 1 1 d . U . . .
C3 C 0.30591(13) 0.47906(16) 0.53329(10) 0.0129(4) Uani 1 1 d . . . . .
C5 C 0.22329(14) 0.29008(15) 0.53265(10) 0.0130(4) Uani 1 1 d . . . . .
H5A H 0.229963 0.295691 0.587569 0.016 Uiso 1 1 calc R U . . .
C6 C 0.11033(14) 0.26432(15) 0.51146(10) 0.0134(4) Uani 1 1 d . . . . .
H6A H 0.104318 0.262379 0.456954 0.016 Uiso 1 1 calc R U . . .
H6B H 0.093178 0.188250 0.529789 0.016 Uiso 1 1 calc R U . . .
C7 C 0.03058(14) 0.34518(15) 0.53985(10) 0.0119(3) Uani 1 1 d . . . . .
C10 C -0.00079(14) 0.56423(15) 0.66686(10) 0.0112(3) Uani 1 1 d . . . . .
C12 C 0.13751(14) 0.65271(15) 0.74501(9) 0.0118(3) Uani 1 1 d . . . . .
H12A H 0.076521 0.688837 0.769258 0.014 Uiso 1 1 calc R U . . .
C13 C 0.20941(14) 0.74485(15) 0.71582(10) 0.0119(3) Uani 1 1 d . . . . .
H13A H 0.239240 0.786694 0.758401 0.014 Uiso 1 1 calc R U . . .
H13B H 0.268015 0.708662 0.689995 0.014 Uiso 1 1 calc R U . . .
C14 C 0.15799(13) 0.82754(15) 0.66403(10) 0.0111(3) Uani 1 1 d . . . . .
C17 C 0.19060(14) 0.90892(15) 0.47933(10) 0.0130(4) Uani 1 1 d . . . . .
C19 C 0.34074(14) 0.85825(16) 0.40144(10) 0.0139(4) Uani 1 1 d . . . . .
H19A H 0.290896 0.870492 0.359193 0.017 Uiso 1 1 calc R U . . .
C20 C 0.39480(14) 0.74366(15) 0.39125(11) 0.0141(4) Uani 1 1 d . . . . .
H20A H 0.444718 0.749845 0.350337 0.017 Uiso 1 1 calc R U . . .
H20B H 0.435296 0.725745 0.436713 0.017 Uiso 1 1 calc R U . . .
C21 C 0.32116(14) 0.64860(15) 0.37498(10) 0.0138(4) Uani 1 1 d . . . . .
C22 C 0.29582(15) 0.19798(16) 0.50519(11) 0.0184(4) Uani 1 1 d . . . . .
H22A H 0.368070 0.216616 0.518840 0.028 Uiso 1 1 calc R U . . .
H22B H 0.289242 0.192044 0.451388 0.028 Uiso 1 1 calc R U . . .
H22C H 0.276748 0.126115 0.527694 0.028 Uiso 1 1 calc R U . . .
C23 C -0.07609(14) 0.34011(16) 0.50528(11) 0.0161(4) Uani 1 1 d . . . . .
H23A H -0.100219 0.416454 0.493987 0.024 Uiso 1 1 calc R U . . .
H23B H -0.124315 0.304468 0.539561 0.024 Uiso 1 1 calc R U . . .
H23C H -0.073622 0.296094 0.459641 0.024 Uiso 1 1 calc R U . . .
C24 C 0.19640(16) 0.58160(17) 0.80191(11) 0.0195(4) Uani 1 1 d . . . . .
H24A H 0.148999 0.525717 0.822692 0.029 Uiso 1 1 calc R U . . .
H24B H 0.223480 0.630178 0.841468 0.029 Uiso 1 1 calc R U . . .
H24C H 0.254572 0.543203 0.778161 0.029 Uiso 1 1 calc R U . . .
C25 C 0.06447(14) 0.89150(16) 0.68976(10) 0.0147(4) Uani 1 1 d . . . . .
H25A H 0.069391 0.969855 0.673501 0.022 Uiso 1 1 calc R U . . .
H25B H 0.061995 0.888922 0.743743 0.022 Uiso 1 1 calc R U . . .
H25C H 0.000937 0.857505 0.668839 0.022 Uiso 1 1 calc R U . . .
C26 C 0.42071(17) 0.95293(17) 0.40210(12) 0.0239(5) Uani 1 1 d . . . . .
H26A H 0.385365 1.024750 0.410447 0.036 Uiso 1 1 calc R U . . .
H26B H 0.456010 0.955158 0.354564 0.036 Uiso 1 1 calc R U . . .
H26C H 0.472227 0.939818 0.441710 0.036 Uiso 1 1 calc R U . . .
C27 C 0.27701(16) 0.64064(18) 0.29789(11) 0.0209(4) Uani 1 1 d . . . . .
H27A H 0.227071 0.578363 0.294992 0.031 Uiso 1 1 calc R U . . .
H27B H 0.333682 0.627285 0.263308 0.031 Uiso 1 1 calc R U . . .
H27C H 0.241485 0.711092 0.285065 0.031 Uiso 1 1 calc R U . . .
C28 C 0.45018(16) 0.77952(18) 0.63123(13) 0.0170(5) Uani 0.870(4) 1 d D . P A 1
H28A H 0.406309 0.838178 0.648124 0.020 Uiso 0.870(4) 1 calc R U P A 1
C29 C 0.57837(18) 0.6367(2) 0.66395(15) 0.0254(6) Uani 0.870(4) 1 d D . P A 1
H29A H 0.571341 0.619018 0.611298 0.038 Uiso 0.870(4) 1 calc R U P A 1
H29B H 0.560897 0.570165 0.693107 0.038 Uiso 0.870(4) 1 calc R U P A 1
H29C H 0.650385 0.659442 0.675195 0.038 Uiso 0.870(4) 1 calc R U P A 1
C30 C 0.4959(2) 0.7539(3) 0.76034(14) 0.0335(7) Uani 0.870(4) 1 d D . P A 1
H30A H 0.447114 0.816986 0.764226 0.050 Uiso 0.870(4) 1 calc R U P A 1
H30B H 0.563328 0.775065 0.782504 0.050 Uiso 0.870(4) 1 calc R U P A 1
H30C H 0.467906 0.688622 0.786386 0.050 Uiso 0.870(4) 1 calc R U P A 1
C28A C 0.4960(12) 0.6960(10) 0.6069(5) 0.028(4) Uiso 0.130(4) 1 d D . P A 2
H28B H 0.523713 0.627114 0.589317 0.034 Uiso 0.130(4) 1 calc R U P A 2
C29A C 0.5003(14) 0.8258(9) 0.7120(8) 0.035(5) Uiso 0.130(4) 1 d D . P A 2
H29D H 0.481591 0.817312 0.763932 0.052 Uiso 0.130(4) 1 calc R U P A 2
H29E H 0.445433 0.868055 0.685850 0.052 Uiso 0.130(4) 1 calc R U P A 2
H29F H 0.566522 0.866484 0.708799 0.052 Uiso 0.130(4) 1 calc R U P A 2
C30A C 0.5892(12) 0.6393(11) 0.7149(8) 0.030(4) Uiso 0.130(4) 1 d D . P A 2
H30D H 0.567272 0.617715 0.764506 0.045 Uiso 0.130(4) 1 calc R U P A 2
H30E H 0.658679 0.673581 0.717865 0.045 Uiso 0.130(4) 1 calc R U P A 2
H30F H 0.591568 0.572380 0.683454 0.045 Uiso 0.130(4) 1 calc R U P A 2


_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
S2 C10 1.6901(18) . ?
S1 C3 1.6952(19) . ?
S3 C17 1.6854(19) . ?
O1 C28A 1.221(8) . ?
O1 C28 1.237(3) . ?
N1 C21 1.282(2) . ?
N1 N2 1.382(2) . ?
N2 C3 1.358(2) . ?
N2 H2 0.86(2) . ?
N3 C29A 1.324(8) . ?
N3 C28 1.347(3) . ?
N3 C28A 1.406(8) . ?
N3 C29 1.410(3) . ?
N3 C30 1.482(3) . ?
N3 C30A 1.557(8) . ?
N4 C3 1.328(2) . ?
N4 C5 1.462(2) . ?
N4 H4 0.84(2) . ?
N8 C7 1.280(2) . ?
N8 N9 1.387(2) . ?
N9 C10 1.358(2) . ?
N9 H9 0.84(2) . ?
N11 C10 1.332(2) . ?
N11 C12 1.463(2) . ?
N11 H11 0.84(2) . ?
N15 C14 1.283(2) . ?
N15 N16 1.388(2) . ?
N16 C17 1.373(2) . ?
N16 H16 0.85(2) . ?
N18 C17 1.328(2) . ?
N18 C19 1.469(2) . ?
N18 H18 0.84(2) . ?
C5 C6 1.523(3) . ?
C5 C22 1.526(3) . ?
C5 H5A 1.0000 . ?
C6 C7 1.501(2) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C23 1.496(2) . ?
C12 C24 1.524(3) . ?
C12 C13 1.532(2) . ?
C12 H12A 1.0000 . ?
C13 C14 1.504(2) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C25 1.500(2) . ?
C19 C26 1.523(3) . ?
C19 C20 1.542(3) . ?
C19 H19A 1.0000 . ?
C20 C21 1.499(3) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C27 1.502(3) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9500 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C28A H28B 0.9500 . ?
C29A H29D 0.9800 . ?
C29A H29E 0.9800 . ?
C29A H29F 0.9800 . ?
C30A H30D 0.9800 . ?
C30A H30E 0.9800 . ?
C30A H30F 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
C21 N1 N2 119.85(16) . . ?
C3 N2 N1 117.57(16) . . ?
C3 N2 H2 117.6(14) . . ?
N1 N2 H2 124.7(14) . . ?
C29A N3 C28A 127.9(7) . . ?
C28 N3 C29 123.63(19) . . ?
C28 N3 C30 117.72(19) . . ?
C29 N3 C30 118.4(2) . . ?
C29A N3 C30A 119.8(7) . . ?
C28A N3 C30A 106.5(6) . . ?
C3 N4 C5 125.80(16) . . ?
C3 N4 H4 116.0(15) . . ?
C5 N4 H4 117.6(15) . . ?
C7 N8 N9 115.39(15) . . ?
C10 N9 N8 120.45(15) . . ?
C10 N9 H9 116.7(14) . . ?
N8 N9 H9 122.4(15) . . ?
C10 N11 C12 125.40(15) . . ?
C10 N11 H11 115.0(14) . . ?
C12 N11 H11 119.2(14) . . ?
C14 N15 N16 117.72(15) . . ?
C17 N16 N15 117.46(15) . . ?
C17 N16 H16 117.3(14) . . ?
N15 N16 H16 121.7(14) . . ?
C17 N18 C19 124.78(16) . . ?
C17 N18 H18 117.0(14) . . ?
C19 N18 H18 117.2(14) . . ?
N4 C3 N2 116.04(16) . . ?
N4 C3 S1 124.44(14) . . ?
N2 C3 S1 119.51(14) . . ?
N4 C5 C6 108.87(15) . . ?
N4 C5 C22 109.34(15) . . ?
C6 C5 C22 110.79(15) . . ?
N4 C5 H5A 109.3 . . ?
C6 C5 H5A 109.3 . . ?
C22 C5 H5A 109.3 . . ?
C7 C6 C5 115.76(15) . . ?
C7 C6 H6A 108.3 . . ?
C5 C6 H6A 108.3 . . ?
C7 C6 H6B 108.3 . . ?
C5 C6 H6B 108.3 . . ?
H6A C6 H6B 107.4 . . ?
N8 C7 C23 124.20(16) . . ?
N8 C7 C6 118.82(16) . . ?
C23 C7 C6 116.97(15) . . ?
N11 C10 N9 116.73(16) . . ?
N11 C10 S2 125.92(14) . . ?
N9 C10 S2 117.33(13) . . ?
N11 C12 C24 108.67(15) . . ?
N11 C12 C13 111.87(14) . . ?
C24 C12 C13 109.68(15) . . ?
N11 C12 H12A 108.9 . . ?
C24 C12 H12A 108.9 . . ?
C13 C12 H12A 108.9 . . ?
C14 C13 C12 115.06(15) . . ?
C14 C13 H13A 108.5 . . ?
C12 C13 H13A 108.5 . . ?
C14 C13 H13B 108.5 . . ?
C12 C13 H13B 108.5 . . ?
H13A C13 H13B 107.5 . . ?
N15 C14 C25 125.67(16) . . ?
N15 C14 C13 115.52(16) . . ?
C25 C14 C13 118.81(15) . . ?
N18 C17 N16 115.95(16) . . ?
N18 C17 S3 125.54(14) . . ?
N16 C17 S3 118.51(14) . . ?
N18 C19 C26 110.41(15) . . ?
N18 C19 C20 109.86(15) . . ?
C26 C19 C20 110.57(15) . . ?
N18 C19 H19A 108.6 . . ?
C26 C19 H19A 108.7 . . ?
C20 C19 H19A 108.6 . . ?
C21 C20 C19 114.08(15) . . ?
C21 C20 H20A 108.7 . . ?
C19 C20 H20A 108.7 . . ?
C21 C20 H20B 108.7 . . ?
C19 C20 H20B 108.7 . . ?
H20A C20 H20B 107.6 . . ?
N1 C21 C20 127.51(18) . . ?
N1 C21 C27 115.28(17) . . ?
C20 C21 C27 117.19(16) . . ?
C5 C22 H22A 109.5 . . ?
C5 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C5 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C7 C23 H23A 109.5 . . ?
C7 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C7 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C12 C24 H24A 109.5 . . ?
C12 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C12 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C14 C25 H25A 109.5 . . ?
C14 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C14 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C19 C26 H26A 109.5 . . ?
C19 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C19 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C21 C27 H27A 109.5 . . ?
C21 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C21 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O1 C28 N3 124.3(2) . . ?
O1 C28 H28A 117.9 . . ?
N3 C28 H28A 117.9 . . ?
N3 C29 H29A 109.5 . . ?
N3 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
N3 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N3 C30 H30A 109.5 . . ?
N3 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
N3 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O1 C28A N3 120.7(8) . . ?
O1 C28A H28B 119.6 . . ?
N3 C28A H28B 119.6 . . ?
N3 C29A H29D 109.5 . . ?
N3 C29A H29E 109.5 . . ?
H29D C29A H29E 109.5 . . ?
N3 C29A H29F 109.5 . . ?
H29D C29A H29F 109.5 . . ?
H29E C29A H29F 109.5 . . ?
N3 C30A H30D 109.5 . . ?
N3 C30A H30E 109.5 . . ?
H30D C30A H30E 109.5 . . ?
N3 C30A H30F 109.5 . . ?
H30D C30A H30F 109.5 . . ?
H30E C30A H30F 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
C21 N1 N2 C3 -173.23(16) . . . . ?
C7 N8 N9 C10 -173.46(16) . . . . ?
C14 N15 N16 C17 -172.05(16) . . . . ?
C5 N4 C3 N2 176.52(16) . . . . ?
C5 N4 C3 S1 -4.0(3) . . . . ?
N1 N2 C3 N4 3.3(2) . . . . ?
N1 N2 C3 S1 -176.21(12) . . . . ?
C3 N4 C5 C6 135.98(18) . . . . ?
C3 N4 C5 C22 -102.9(2) . . . . ?
N4 C5 C6 C7 -63.6(2) . . . . ?
C22 C5 C6 C7 176.09(16) . . . . ?
N9 N8 C7 C23 1.3(3) . . . . ?
N9 N8 C7 C6 -177.82(15) . . . . ?
C5 C6 C7 N8 -15.8(2) . . . . ?
C5 C6 C7 C23 164.99(16) . . . . ?
C12 N11 C10 N9 -171.89(16) . . . . ?
C12 N11 C10 S2 9.7(3) . . . . ?
N8 N9 C10 N11 4.5(2) . . . . ?
N8 N9 C10 S2 -176.90(13) . . . . ?
C10 N11 C12 C24 119.42(19) . . . . ?
C10 N11 C12 C13 -119.33(19) . . . . ?
N11 C12 C13 C14 64.5(2) . . . . ?
C24 C12 C13 C14 -174.84(15) . . . . ?
N16 N15 C14 C25 -2.7(3) . . . . ?
N16 N15 C14 C13 177.78(15) . . . . ?
C12 C13 C14 N15 -123.79(17) . . . . ?
C12 C13 C14 C25 56.6(2) . . . . ?
C19 N18 C17 N16 -173.28(16) . . . . ?
C19 N18 C17 S3 7.2(3) . . . . ?
N15 N16 C17 N18 -14.3(2) . . . . ?
N15 N16 C17 S3 165.28(12) . . . . ?
C17 N18 C19 C26 94.3(2) . . . . ?
C17 N18 C19 C20 -143.48(18) . . . . ?
N18 C19 C20 C21 69.4(2) . . . . ?
C26 C19 C20 C21 -168.51(16) . . . . ?
N2 N1 C21 C20 0.6(3) . . . . ?
N2 N1 C21 C27 179.07(16) . . . . ?
C19 C20 C21 N1 -104.5(2) . . . . ?
C19 C20 C21 C27 77.0(2) . . . . ?
C29 N3 C28 O1 -0.1(3) . . . . ?
C30 N3 C28 O1 -174.5(2) . . . . ?
C29A N3 C28A O1 -18(2) . . . . ?
C30A N3 C28A O1 -170.1(13) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N2 H2 O1 0.86(2) 2.15(2) 3.009(2) 178(2) . yes
N4 H4 N1 0.84(2) 2.17(2) 2.582(2) 110.5(18) . yes
N11 H11 S1 0.84(2) 2.80(2) 3.5602(16) 151.5(18) . yes
N11 H11 N8 0.84(2) 2.24(2) 2.662(2) 111.2(17) . yes
N18 H18 O1 0.84(2) 2.20(2) 2.965(2) 151.4(19) . yes
C12 H12A S2 1.00 2.68 3.1838(18) 111.3 . yes
C20 H20B O1 0.99 2.35 3.208(2) 144.5 . yes
C23 H23A N8 0.98 2.63 3.441(2) 140.6 3_566 yes
C23 H23C N15 0.98 2.50 3.249(2) 132.6 3_566 yes
C25 H25B S1 0.98 2.88 3.710(2) 143.6 2_556 yes

_refine_diff_density_max         0.531
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.072


# start Validation Reply Form
_vrf_PLAT910_L4132_LT            
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min). 11 Note 
RESPONSE: Closed by beamstop.
;
# end Validation Reply Form
