# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_valchg
_database_code_depnum_ccdc_archive 'CCDC 2191404'
loop_
_audit_author_name
_audit_author_address
'Akiko Asano'
;Faculty of Pharmacy, Osaka Medical and Pharmaceutical University
Japan
;
_audit_update_record             
;
2022-07-19 deposited with the CCDC.	2023-01-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 c(Val-Oxz-dval-Thz-Chg-Oxz-dval-Thz)2.DMA 
;
_chemical_name_common            '[Val,Chg]ASC'
_chemical_melting_point          ?
_chemical_formula_moiety         'C37 H52 N8 O6 S2, C4 H9 N O'
_chemical_formula_sum            'C41 H61 N9 O7 S2'
_chemical_formula_weight         856.11
_chemical_compound_source        synthesis
_chemical_absolute_configuration rm

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   12.012(2)
_cell_length_b                   12.909(3)
_cell_length_c                   14.885(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.85(3)
_cell_angle_gamma                90.00
_cell_volume                     2286.5(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    27513
_cell_measurement_theta_min      3.0150
_cell_measurement_theta_max      74.9040

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             916
_exptl_absorpt_coefficient_mu    1.518
_exptl_absorpt_correction_T_min  0.70036
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   CrysAlisPro

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'rotated anode'
_diffrn_radiation_monochromator  conforcal
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single P200'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count 39675
_diffrn_standards_interval_time  210
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            39675
_diffrn_reflns_av_R_equivalents  0.0818
_diffrn_reflns_av_sigmaI/netI    0.0366
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.00
_diffrn_reflns_theta_max         70.07
_reflns_number_total             8579
_reflns_number_gt                8214
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       CrysAlisPro
_computing_cell_refinement       CrysAlisPro
_computing_data_reduction        CrysAlisPro
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1676P)²+2.4145P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack (1983), 4025 Friedel pairs'
# 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack   0.005(18)
_refine_ls_number_reflns         8579
_refine_ls_number_parameters     532
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0644
_refine_ls_wR_factor_ref         0.1754
_refine_ls_wR_factor_gt          0.1733
_refine_ls_goodness_of_fit_ref   0.744
_refine_ls_restrained_S_all      0.744
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1D O 0.2480(3) 0.3683(3) 0.7368(2) 0.0657(8) Uani 1 1 d . . .
N1D N 0.2468(3) 0.1962(4) 0.7637(3) 0.0678(9) Uani 1 1 d . . .
C1D C 0.2116(4) 0.2809(5) 0.7116(3) 0.0689(12) Uani 1 1 d . . .
C2D C 0.1234(4) 0.2617(4) 0.6307(3) 0.0658(11) Uani 1 1 d . . .
H2D1 H 0.1087 0.1872 0.6246 0.099 Uiso 1 1 calc R . .
H2D2 H 0.1504 0.2877 0.5757 0.099 Uiso 1 1 calc R . .
H2D3 H 0.0539 0.2978 0.6394 0.099 Uiso 1 1 calc R . .
C3D C 0.3260(4) 0.2158(4) 0.8449(3) 0.0657(11) Uani 1 1 d . . .
H3D1 H 0.3452 0.1502 0.8765 0.099 Uiso 1 1 calc R . .
H3D2 H 0.2920 0.2629 0.8849 0.099 Uiso 1 1 calc R . .
H3D3 H 0.3944 0.2473 0.8278 0.099 Uiso 1 1 calc R . .
C4D C 0.2112(5) 0.0912(5) 0.7420(5) 0.0838(15) Uani 1 1 d . . .
H4D1 H 0.2473 0.0442 0.7889 0.126 Uiso 1 1 calc R . .
H4D2 H 0.2328 0.0718 0.6832 0.126 Uiso 1 1 calc R . .
H4D3 H 0.1294 0.0864 0.7393 0.126 Uiso 1 1 calc R . .
N11 N 0.1117(3) 0.6512(2) 0.63239(19) 0.0450(6) Uani 1 1 d . . .
H11 H 0.1493 0.6014 0.6635 0.054 Uiso 1 1 calc R . .
C11 C 0.1471(3) 0.6853(3) 0.5488(2) 0.0472(8) Uani 1 1 d . . .
H11A H 0.0831 0.7243 0.5142 0.057 Uiso 1 1 calc R . .
C13 C 0.2508(4) 0.7578(3) 0.5603(3) 0.0576(10) Uani 1 1 d . . .
H13 H 0.2709 0.7713 0.4983 0.069 Uiso 1 1 calc R . .
C14 C 0.2256(5) 0.8615(4) 0.6001(3) 0.0719(13) Uani 1 1 d . . .
H14A H 0.1602 0.8927 0.5634 0.108 Uiso 1 1 calc R . .
H14B H 0.2907 0.9073 0.6004 0.108 Uiso 1 1 calc R . .
H14C H 0.2095 0.8518 0.6624 0.108 Uiso 1 1 calc R . .
C15 C 0.3542(4) 0.7051(4) 0.6163(3) 0.0623(10) Uani 1 1 d . . .
H15A H 0.3684 0.6382 0.5888 0.093 Uiso 1 1 calc R . .
H15B H 0.3392 0.6941 0.6786 0.093 Uiso 1 1 calc R . .
H15C H 0.4204 0.7496 0.6167 0.093 Uiso 1 1 calc R . .
N21 N 0.1779(2) 0.4981(2) 0.52061(17) 0.0375(6) Uani 1 1 d . . .
C21 C 0.2147(3) 0.4384(2) 0.4453(2) 0.0373(6) Uani 1 1 d . . .
H21 H 0.1621 0.3791 0.4295 0.045 Uiso 1 1 calc R . .
C22 C 0.3349(3) 0.3970(3) 0.4697(2) 0.0407(7) Uani 1 1 d . . .
O22 O 0.3873(3) 0.3676(3) 0.41112(17) 0.0630(8) Uani 1 1 d . . .
C23 C 0.1704(3) 0.5924(3) 0.4929(2) 0.0407(7) Uani 1 1 d . . .
O23 O 0.1876(2) 0.61402(19) 0.40800(15) 0.0451(5) Uani 1 1 d . . .
C24 C 0.2065(3) 0.5140(3) 0.3652(2) 0.0402(7) Uani 1 1 d . . .
H24 H 0.2786 0.5153 0.3386 0.048 Uiso 1 1 calc R . .
C25 C 0.1082(4) 0.4936(3) 0.2918(2) 0.0522(9) Uani 1 1 d . . .
H25A H 0.1193 0.4272 0.2624 0.078 Uiso 1 1 calc R . .
H25B H 0.1034 0.5492 0.2467 0.078 Uiso 1 1 calc R . .
H25C H 0.0384 0.4912 0.3191 0.078 Uiso 1 1 calc R . .
N31 N 0.3719(2) 0.3902(2) 0.55883(17) 0.0387(6) Uani 1 1 d . . .
H31 H 0.3254 0.4052 0.5978 0.046 Uiso 1 1 calc R . .
C31 C 0.4870(3) 0.3588(3) 0.5934(2) 0.0357(6) Uani 1 1 d . . .
H31A H 0.5266 0.3404 0.5407 0.043 Uiso 1 1 calc R . .
C33 C 0.4882(3) 0.2649(2) 0.6551(2) 0.0391(7) Uani 1 1 d . . .
H33 H 0.4396 0.2802 0.7029 0.047 Uiso 1 1 calc R . .
C34 C 0.4396(3) 0.1702(3) 0.6011(3) 0.0532(9) Uani 1 1 d . . .
H34A H 0.3637 0.1863 0.5713 0.080 Uiso 1 1 calc R . .
H34B H 0.4363 0.1115 0.6424 0.080 Uiso 1 1 calc R . .
H34C H 0.4877 0.1524 0.5553 0.080 Uiso 1 1 calc R . .
C35 C 0.6065(3) 0.2406(3) 0.7019(2) 0.0440(7) Uani 1 1 d . . .
H35A H 0.6040 0.1798 0.7410 0.066 Uiso 1 1 calc R . .
H35B H 0.6356 0.3001 0.7387 0.066 Uiso 1 1 calc R . .
H35C H 0.6558 0.2264 0.6561 0.066 Uiso 1 1 calc R . .
N41 N 0.5193(2) 0.4875(2) 0.71661(17) 0.0350(5) Uani 1 1 d . . .
C41 C 0.5852(3) 0.5732(2) 0.7437(2) 0.0354(6) Uani 1 1 d . . .
C42 C 0.5702(3) 0.6279(2) 0.8284(2) 0.0359(6) Uani 1 1 d . . .
O42 O 0.6336(2) 0.69825(18) 0.85904(17) 0.0430(5) Uani 1 1 d . . .
C43 C 0.5454(2) 0.4506(2) 0.64123(19) 0.0345(6) Uani 1 1 d . . .
S43 S 0.65124(8) 0.51667(7) 0.59781(5) 0.0460(2) Uani 1 1 d . . .
C44 C 0.6595(3) 0.6004(3) 0.6866(2) 0.0453(7) Uani 1 1 d . . .
H44 H 0.7090 0.6580 0.6951 0.054 Uiso 1 1 calc R . .
N51 N 0.4834(2) 0.5944(2) 0.86927(17) 0.0357(5) Uani 1 1 d . . .
H51 H 0.4406 0.5441 0.8442 0.043 Uiso 1 1 calc R . .
C51 C 0.4595(3) 0.6392(2) 0.9528(2) 0.0351(6) Uani 1 1 d . . .
H51A H 0.5327 0.6585 0.9893 0.042 Uiso 1 1 calc R . .
C53 C 0.3879(3) 0.7394(2) 0.9359(2) 0.0375(6) Uani 1 1 d . . .
H53 H 0.4233 0.7809 0.8906 0.045 Uiso 1 1 calc R . .
C54 C 0.2677(3) 0.7183(3) 0.8929(2) 0.0439(7) Uani 1 1 d . . .
H54A H 0.2276 0.6794 0.9359 0.053 Uiso 1 1 calc R . .
H54B H 0.2682 0.6755 0.8377 0.053 Uiso 1 1 calc R . .
C55 C 0.2073(3) 0.8201(3) 0.8680(3) 0.0501(8) Uani 1 1 d . . .
H55A H 0.2442 0.8559 0.8212 0.060 Uiso 1 1 calc R . .
H55B H 0.1286 0.8055 0.8420 0.060 Uiso 1 1 calc R . .
C56 C 0.2083(3) 0.8903(3) 0.9496(3) 0.0491(8) Uani 1 1 d . . .
H56A H 0.1640 0.8579 0.9935 0.059 Uiso 1 1 calc R . .
H56B H 0.1722 0.9571 0.9300 0.059 Uiso 1 1 calc R . .
C57 C 0.3285(3) 0.9107(3) 0.9962(3) 0.0480(8) Uani 1 1 d . . .
H57A H 0.3700 0.9518 0.9555 0.058 Uiso 1 1 calc R . .
H57B H 0.3258 0.9512 1.0524 0.058 Uiso 1 1 calc R . .
C58 C 0.3903(3) 0.8079(3) 1.0197(2) 0.0436(7) Uani 1 1 d . . .
H58A H 0.4692 0.8224 1.0453 0.052 Uiso 1 1 calc R . .
H58B H 0.3542 0.7709 1.0664 0.052 Uiso 1 1 calc R . .
N61 N 0.3649(2) 0.4725(2) 0.97264(16) 0.0325(5) Uani 1 1 d . . .
C61 C 0.3129(2) 0.4226(2) 1.04473(19) 0.0329(6) Uani 1 1 d . . .
H61 H 0.3464 0.3521 1.0563 0.039 Uiso 1 1 calc R . .
C62 C 0.1860(3) 0.4121(3) 1.0207(2) 0.0373(6) Uani 1 1 d . . .
O62 O 0.1267(2) 0.3934(2) 1.08039(15) 0.0462(6) Uani 1 1 d . . .
C63 C 0.4048(3) 0.5587(2) 1.0047(2) 0.0340(6) Uani 1 1 d . . .
O63 O 0.3960(2) 0.58188(16) 1.09171(14) 0.0388(5) Uani 1 1 d . . .
C64 C 0.3453(3) 0.4907(2) 1.1299(2) 0.0346(6) Uani 1 1 d . . .
H64 H 0.2764 0.5113 1.1563 0.041 Uiso 1 1 calc R . .
C65 C 0.4304(3) 0.4435(3) 1.2018(2) 0.0396(7) Uani 1 1 d . . .
H65A H 0.3976 0.3827 1.2277 0.059 Uiso 1 1 calc R . .
H65B H 0.4521 0.4945 1.2497 0.059 Uiso 1 1 calc R . .
H65C H 0.4969 0.4225 1.1749 0.059 Uiso 1 1 calc R . .
N71 N 0.1459(2) 0.4232(2) 0.93209(18) 0.0411(6) Uani 1 1 d . . .
H71 H 0.1939 0.4328 0.8932 0.049 Uiso 1 1 calc R . .
C71 C 0.0262(3) 0.4199(3) 0.8979(2) 0.0437(7) Uani 1 1 d . . .
H71A H -0.0161 0.4151 0.9512 0.052 Uiso 1 1 calc R . .
C73 C -0.0042(3) 0.3256(3) 0.8378(3) 0.0497(8) Uani 1 1 d . . .
H73 H 0.0440 0.3264 0.7880 0.060 Uiso 1 1 calc R . .
C74 C 0.0213(4) 0.2269(4) 0.8922(3) 0.0608(10) Uani 1 1 d . . .
H74A H 0.1003 0.2269 0.9194 0.091 Uiso 1 1 calc R . .
H74B H 0.0068 0.1668 0.8520 0.091 Uiso 1 1 calc R . .
H74C H -0.0269 0.2232 0.9402 0.091 Uiso 1 1 calc R . .
C75 C -0.1269(3) 0.3277(4) 0.7945(3) 0.0597(10) Uani 1 1 d . . .
H75A H -0.1432 0.2660 0.7565 0.090 Uiso 1 1 calc R . .
H75B H -0.1407 0.3900 0.7570 0.090 Uiso 1 1 calc R . .
H75C H -0.1757 0.3283 0.8422 0.090 Uiso 1 1 calc R . .
N81 N 0.0343(2) 0.5497(3) 0.77658(19) 0.0446(6) Uani 1 1 d . . .
C81 C -0.0107(3) 0.6450(3) 0.7473(2) 0.0472(8) Uani 1 1 d . . .
C82 C 0.0221(3) 0.6940(3) 0.6643(2) 0.0505(8) Uani 1 1 d . . .
O82 O -0.0282(3) 0.7695(3) 0.6290(2) 0.0744(10) Uani 1 1 d . . .
C83 C -0.0053(3) 0.5210(3) 0.8498(2) 0.0448(7) Uani 1 1 d . . .
S83 S -0.10090(8) 0.60573(9) 0.88647(7) 0.0574(3) Uani 1 1 d . . .
C84 C -0.0855(3) 0.6854(4) 0.7992(3) 0.0570(9) Uani 1 1 d . . .
H84 H -0.1236 0.7495 0.7878 0.068 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1D C1D 1.248(7) . ?
N1D C1D 1.374(7) . ?
N1D C4D 1.445(7) . ?
N1D C3D 1.454(6) . ?
C1D C2D 1.511(7) . ?
C2D H2D1 0.9800 . ?
C2D H2D2 0.9800 . ?
C2D H2D3 0.9800 . ?
C3D H3D1 0.9800 . ?
C3D H3D2 0.9800 . ?
C3D H3D3 0.9800 . ?
C4D H4D1 0.9800 . ?
C4D H4D2 0.9800 . ?
C4D H4D3 0.9800 . ?
N11 C82 1.353(5) . ?
N11 C11 1.438(5) . ?
N11 H11 0.8800 . ?
C11 C23 1.509(5) . ?
C11 C13 1.549(6) . ?
C11 H11A 1.0000 . ?
C13 C14 1.511(6) . ?
C13 C15 1.555(7) . ?
C13 H13 1.0000 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
N21 C23 1.284(5) . ?
N21 C21 1.477(4) . ?
C21 C24 1.535(4) . ?
C21 C22 1.535(4) . ?
C21 H21 1.0000 . ?
C22 O22 1.205(4) . ?
C22 N31 1.343(4) . ?
C23 O23 1.337(4) . ?
O23 C24 1.471(4) . ?
C24 C25 1.517(5) . ?
C24 H24 1.0000 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
N31 C31 1.466(4) . ?
N31 H31 0.8800 . ?
C31 C43 1.505(4) . ?
C31 C33 1.520(4) . ?
C31 H31A 1.0000 . ?
C33 C35 1.527(4) . ?
C33 C34 1.533(5) . ?
C33 H33 1.0000 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
N41 C43 1.296(4) . ?
N41 C41 1.388(4) . ?
C41 C44 1.360(5) . ?
C41 C42 1.477(4) . ?
C42 O42 1.233(4) . ?
C42 N51 1.347(4) . ?
C43 S43 1.728(3) . ?
S43 C44 1.700(4) . ?
C44 H44 0.9500 . ?
N51 C51 1.435(4) . ?
N51 H51 0.8800 . ?
C51 C63 1.499(4) . ?
C51 C53 1.554(4) . ?
C51 H51A 1.0000 . ?
C53 C54 1.522(5) . ?
C53 C58 1.527(4) . ?
C53 H53 1.0000 . ?
C54 C55 1.522(5) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C55 C56 1.514(5) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C56 C57 1.537(5) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C57 C58 1.536(5) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
N61 C63 1.278(4) . ?
N61 C61 1.463(4) . ?
C61 C62 1.524(4) . ?
C61 C64 1.547(4) . ?
C61 H61 1.0000 . ?
C62 O62 1.236(4) . ?
C62 N71 1.349(4) . ?
C63 O63 1.348(4) . ?
O63 C64 1.475(4) . ?
C64 C65 1.505(4) . ?
C64 H64 1.0000 . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
N71 C71 1.458(4) . ?
N71 H71 0.8800 . ?
C71 C83 1.511(5) . ?
C71 C73 1.526(5) . ?
C71 H71A 1.0000 . ?
C73 C74 1.518(6) . ?
C73 C75 1.527(5) . ?
C73 H73 1.0000 . ?
C74 H74A 0.9800 . ?
C74 H74B 0.9800 . ?
C74 H74C 0.9800 . ?
C75 H75A 0.9800 . ?
C75 H75B 0.9800 . ?
C75 H75C 0.9800 . ?
N81 C83 1.302(5) . ?
N81 C81 1.389(5) . ?
C81 C84 1.366(5) . ?
C81 C82 1.489(6) . ?
C82 O82 1.227(5) . ?
C83 S83 1.728(4) . ?
S83 C84 1.686(5) . ?
C84 H84 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
C1D N1D C4D 124.2(5) . . ?
C1D N1D C3D 116.6(4) . . ?
C4D N1D C3D 119.2(5) . . ?
O1D C1D N1D 118.7(4) . . ?
O1D C1D C2D 124.5(5) . . ?
N1D C1D C2D 116.6(5) . . ?
C1D C2D H2D1 109.5 . . ?
C1D C2D H2D2 109.5 . . ?
H2D1 C2D H2D2 109.5 . . ?
C1D C2D H2D3 109.5 . . ?
H2D1 C2D H2D3 109.5 . . ?
H2D2 C2D H2D3 109.5 . . ?
N1D C3D H3D1 109.5 . . ?
N1D C3D H3D2 109.5 . . ?
H3D1 C3D H3D2 109.5 . . ?
N1D C3D H3D3 109.5 . . ?
H3D1 C3D H3D3 109.5 . . ?
H3D2 C3D H3D3 109.5 . . ?
N1D C4D H4D1 109.5 . . ?
N1D C4D H4D2 109.5 . . ?
H4D1 C4D H4D2 109.5 . . ?
N1D C4D H4D3 109.5 . . ?
H4D1 C4D H4D3 109.5 . . ?
H4D2 C4D H4D3 109.5 . . ?
C82 N11 C11 121.5(3) . . ?
C82 N11 H11 119.3 . . ?
C11 N11 H11 119.3 . . ?
N11 C11 C23 109.4(3) . . ?
N11 C11 C13 114.7(3) . . ?
C23 C11 C13 109.5(3) . . ?
N11 C11 H11A 107.6 . . ?
C23 C11 H11A 107.6 . . ?
C13 C11 H11A 107.6 . . ?
C14 C13 C11 112.1(4) . . ?
C14 C13 C15 111.5(4) . . ?
C11 C13 C15 111.5(3) . . ?
C14 C13 H13 107.1 . . ?
C11 C13 H13 107.1 . . ?
C15 C13 H13 107.1 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C23 N21 C21 105.4(3) . . ?
N21 C21 C24 105.3(2) . . ?
N21 C21 C22 111.8(2) . . ?
C24 C21 C22 111.3(3) . . ?
N21 C21 H21 109.5 . . ?
C24 C21 H21 109.5 . . ?
C22 C21 H21 109.5 . . ?
O22 C22 N31 124.0(3) . . ?
O22 C22 C21 120.3(3) . . ?
N31 C22 C21 115.5(3) . . ?
N21 C23 O23 119.3(3) . . ?
N21 C23 C11 125.9(3) . . ?
O23 C23 C11 114.8(3) . . ?
C23 O23 C24 106.2(2) . . ?
O23 C24 C25 108.3(3) . . ?
O23 C24 C21 102.6(2) . . ?
C25 C24 C21 114.2(3) . . ?
O23 C24 H24 110.5 . . ?
C25 C24 H24 110.5 . . ?
C21 C24 H24 110.5 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C22 N31 C31 122.3(3) . . ?
C22 N31 H31 118.9 . . ?
C31 N31 H31 118.9 . . ?
N31 C31 C43 107.7(3) . . ?
N31 C31 C33 111.3(3) . . ?
C43 C31 C33 112.2(2) . . ?
N31 C31 H31A 108.5 . . ?
C43 C31 H31A 108.5 . . ?
C33 C31 H31A 108.5 . . ?
C31 C33 C35 111.7(3) . . ?
C31 C33 C34 110.4(3) . . ?
C35 C33 C34 109.9(3) . . ?
C31 C33 H33 108.3 . . ?
C35 C33 H33 108.3 . . ?
C34 C33 H33 108.3 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C43 N41 C41 110.4(3) . . ?
C44 C41 N41 114.9(3) . . ?
C44 C41 C42 125.3(3) . . ?
N41 C41 C42 119.8(3) . . ?
O42 C42 N51 123.1(3) . . ?
O42 C42 C41 121.8(3) . . ?
N51 C42 C41 115.1(3) . . ?
N41 C43 C31 123.1(3) . . ?
N41 C43 S43 114.8(2) . . ?
C31 C43 S43 122.0(2) . . ?
C44 S43 C43 89.48(16) . . ?
C41 C44 S43 110.4(3) . . ?
C41 C44 H44 124.8 . . ?
S43 C44 H44 124.8 . . ?
C42 N51 C51 121.4(3) . . ?
C42 N51 H51 119.3 . . ?
C51 N51 H51 119.3 . . ?
N51 C51 C63 108.7(2) . . ?
N51 C51 C53 111.5(2) . . ?
C63 C51 C53 112.8(3) . . ?
N51 C51 H51A 107.9 . . ?
C63 C51 H51A 107.9 . . ?
C53 C51 H51A 107.9 . . ?
C54 C53 C58 111.0(3) . . ?
C54 C53 C51 113.0(3) . . ?
C58 C53 C51 113.7(3) . . ?
C54 C53 H53 106.1 . . ?
C58 C53 H53 106.1 . . ?
C51 C53 H53 106.1 . . ?
C53 C54 C55 109.9(3) . . ?
C53 C54 H54A 109.7 . . ?
C55 C54 H54A 109.7 . . ?
C53 C54 H54B 109.7 . . ?
C55 C54 H54B 109.7 . . ?
H54A C54 H54B 108.2 . . ?
C56 C55 C54 111.8(3) . . ?
C56 C55 H55A 109.3 . . ?
C54 C55 H55A 109.3 . . ?
C56 C55 H55B 109.3 . . ?
C54 C55 H55B 109.3 . . ?
H55A C55 H55B 107.9 . . ?
C55 C56 C57 111.6(3) . . ?
C55 C56 H56A 109.3 . . ?
C57 C56 H56A 109.3 . . ?
C55 C56 H56B 109.3 . . ?
C57 C56 H56B 109.3 . . ?
H56A C56 H56B 108.0 . . ?
C58 C57 C56 110.5(3) . . ?
C58 C57 H57A 109.6 . . ?
C56 C57 H57A 109.6 . . ?
C58 C57 H57B 109.6 . . ?
C56 C57 H57B 109.6 . . ?
H57A C57 H57B 108.1 . . ?
C53 C58 C57 111.1(3) . . ?
C53 C58 H58A 109.4 . . ?
C57 C58 H58A 109.4 . . ?
C53 C58 H58B 109.4 . . ?
C57 C58 H58B 109.4 . . ?
H58A C58 H58B 108.0 . . ?
C63 N61 C61 106.6(2) . . ?
N61 C61 C62 112.4(2) . . ?
N61 C61 C64 105.4(2) . . ?
C62 C61 C64 112.0(2) . . ?
N61 C61 H61 109.0 . . ?
C62 C61 H61 109.0 . . ?
C64 C61 H61 109.0 . . ?
O62 C62 N71 124.0(3) . . ?
O62 C62 C61 120.3(3) . . ?
N71 C62 C61 115.6(3) . . ?
N61 C63 O63 118.5(3) . . ?
N61 C63 C51 125.4(3) . . ?
O63 C63 C51 116.1(3) . . ?
C63 O63 C64 106.5(2) . . ?
O63 C64 C65 108.7(2) . . ?
O63 C64 C61 102.1(2) . . ?
C65 C64 C61 115.0(3) . . ?
O63 C64 H64 110.2 . . ?
C65 C64 H64 110.2 . . ?
C61 C64 H64 110.2 . . ?
C64 C65 H65A 109.5 . . ?
C64 C65 H65B 109.5 . . ?
H65A C65 H65B 109.5 . . ?
C64 C65 H65C 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
C62 N71 C71 122.8(3) . . ?
C62 N71 H71 118.6 . . ?
C71 N71 H71 118.6 . . ?
N71 C71 C83 108.2(3) . . ?
N71 C71 C73 111.9(3) . . ?
C83 C71 C73 112.7(3) . . ?
N71 C71 H71A 108.0 . . ?
C83 C71 H71A 108.0 . . ?
C73 C71 H71A 108.0 . . ?
C74 C73 C71 110.0(3) . . ?
C74 C73 C75 110.6(3) . . ?
C71 C73 C75 111.9(3) . . ?
C74 C73 H73 108.1 . . ?
C71 C73 H73 108.1 . . ?
C75 C73 H73 108.1 . . ?
C73 C74 H74A 109.5 . . ?
C73 C74 H74B 109.5 . . ?
H74A C74 H74B 109.5 . . ?
C73 C74 H74C 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?
C73 C75 H75A 109.5 . . ?
C73 C75 H75B 109.5 . . ?
H75A C75 H75B 109.5 . . ?
C73 C75 H75C 109.5 . . ?
H75A C75 H75C 109.5 . . ?
H75B C75 H75C 109.5 . . ?
C83 N81 C81 110.1(3) . . ?
C84 C81 N81 114.7(4) . . ?
C84 C81 C82 125.2(4) . . ?
N81 C81 C82 120.0(3) . . ?
O82 C82 N11 122.9(4) . . ?
O82 C82 C81 121.5(4) . . ?
N11 C82 C81 115.6(3) . . ?
N81 C83 C71 123.2(3) . . ?
N81 C83 S83 114.7(3) . . ?
C71 C83 S83 122.1(3) . . ?
C84 S83 C83 89.8(2) . . ?
C81 C84 S83 110.6(3) . . ?
C81 C84 H84 124.7 . . ?
S83 C84 H84 124.7 . . ?

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
C4D N1D C1D O1D -179.9(5) . . . . ?
C3D N1D C1D O1D -0.7(6) . . . . ?
C4D N1D C1D C2D 4.7(7) . . . . ?
C3D N1D C1D C2D -176.0(4) . . . . ?
C82 N11 C11 C23 -134.3(4) . . . . ?
C82 N11 C11 C13 102.2(4) . . . . ?
N11 C11 C13 C14 -67.3(4) . . . . ?
C23 C11 C13 C14 169.2(3) . . . . ?
N11 C11 C13 C15 58.5(4) . . . . ?
C23 C11 C13 C15 -65.0(4) . . . . ?
C23 N21 C21 C24 -9.4(3) . . . . ?
C23 N21 C21 C22 111.6(3) . . . . ?
N21 C21 C22 O22 -163.1(4) . . . . ?
C24 C21 C22 O22 -45.7(5) . . . . ?
N21 C21 C22 N31 21.2(4) . . . . ?
C24 C21 C22 N31 138.6(3) . . . . ?
C21 N21 C23 O23 4.4(4) . . . . ?
C21 N21 C23 C11 -173.4(3) . . . . ?
N11 C11 C23 N21 -11.7(5) . . . . ?
C13 C11 C23 N21 114.8(4) . . . . ?
N11 C11 C23 O23 170.4(3) . . . . ?
C13 C11 C23 O23 -63.0(4) . . . . ?
N21 C23 O23 C24 3.0(4) . . . . ?
C11 C23 O23 C24 -179.0(3) . . . . ?
C23 O23 C24 C25 112.6(3) . . . . ?
C23 O23 C24 C21 -8.5(3) . . . . ?
N21 C21 C24 O23 10.8(3) . . . . ?
C22 C21 C24 O23 -110.5(3) . . . . ?
N21 C21 C24 C25 -106.1(3) . . . . ?
C22 C21 C24 C25 132.6(3) . . . . ?
O22 C22 N31 C31 8.5(6) . . . . ?
C21 C22 N31 C31 -175.9(3) . . . . ?
C22 N31 C31 C43 113.6(3) . . . . ?
C22 N31 C31 C33 -123.0(3) . . . . ?
N31 C31 C33 C35 -172.0(3) . . . . ?
C43 C31 C33 C35 -51.3(4) . . . . ?
N31 C31 C33 C34 65.4(4) . . . . ?
C43 C31 C33 C34 -173.8(3) . . . . ?
C43 N41 C41 C44 1.0(4) . . . . ?
C43 N41 C41 C42 -179.8(3) . . . . ?
C44 C41 C42 O42 -7.5(5) . . . . ?
N41 C41 C42 O42 173.3(3) . . . . ?
C44 C41 C42 N51 173.1(3) . . . . ?
N41 C41 C42 N51 -6.1(4) . . . . ?
C41 N41 C43 C31 -178.7(3) . . . . ?
C41 N41 C43 S43 0.0(3) . . . . ?
N31 C31 C43 N41 68.5(4) . . . . ?
C33 C31 C43 N41 -54.3(4) . . . . ?
N31 C31 C43 S43 -110.1(3) . . . . ?
C33 C31 C43 S43 127.0(3) . . . . ?
N41 C43 S43 C44 -0.7(3) . . . . ?
C31 C43 S43 C44 178.0(3) . . . . ?
N41 C41 C44 S43 -1.5(4) . . . . ?
C42 C41 C44 S43 179.3(2) . . . . ?
C43 S43 C44 C41 1.2(3) . . . . ?
O42 C42 N51 C51 -0.3(5) . . . . ?
C41 C42 N51 C51 179.1(3) . . . . ?
C42 N51 C51 C63 -151.2(3) . . . . ?
C42 N51 C51 C53 83.8(4) . . . . ?
N51 C51 C53 C54 70.2(3) . . . . ?
C63 C51 C53 C54 -52.5(3) . . . . ?
N51 C51 C53 C58 -162.0(3) . . . . ?
C63 C51 C53 C58 75.2(3) . . . . ?
C58 C53 C54 C55 57.7(4) . . . . ?
C51 C53 C54 C55 -173.2(3) . . . . ?
C53 C54 C55 C56 -57.1(4) . . . . ?
C54 C55 C56 C57 55.7(4) . . . . ?
C55 C56 C57 C58 -53.9(4) . . . . ?
C54 C53 C58 C57 -57.3(4) . . . . ?
C51 C53 C58 C57 173.9(3) . . . . ?
C56 C57 C58 C53 54.7(4) . . . . ?
C63 N61 C61 C62 114.6(3) . . . . ?
C63 N61 C61 C64 -7.6(3) . . . . ?
N61 C61 C62 O62 -163.8(3) . . . . ?
C64 C61 C62 O62 -45.4(4) . . . . ?
N61 C61 C62 N71 16.9(4) . . . . ?
C64 C61 C62 N71 135.4(3) . . . . ?
C61 N61 C63 O63 2.6(4) . . . . ?
C61 N61 C63 C51 -176.0(3) . . . . ?
N51 C51 C63 N61 -13.4(4) . . . . ?
C53 C51 C63 N61 110.9(3) . . . . ?
N51 C51 C63 O63 168.0(3) . . . . ?
C53 C51 C63 O63 -67.7(3) . . . . ?
N61 C63 O63 C64 3.9(4) . . . . ?
C51 C63 O63 C64 -177.4(3) . . . . ?
C63 O63 C64 C65 113.9(3) . . . . ?
C63 O63 C64 C61 -8.0(3) . . . . ?
N61 C61 C64 O63 9.4(3) . . . . ?
C62 C61 C64 O63 -113.1(3) . . . . ?
N61 C61 C64 C65 -108.1(3) . . . . ?
C62 C61 C64 C65 129.4(3) . . . . ?
O62 C62 N71 C71 3.5(5) . . . . ?
C61 C62 N71 C71 -177.3(3) . . . . ?
C62 N71 C71 C83 121.7(3) . . . . ?
C62 N71 C71 C73 -113.6(4) . . . . ?
N71 C71 C73 C74 62.2(4) . . . . ?
C83 C71 C73 C74 -175.6(3) . . . . ?
N71 C71 C73 C75 -174.4(3) . . . . ?
C83 C71 C73 C75 -52.2(4) . . . . ?
C83 N81 C81 C84 -1.0(4) . . . . ?
C83 N81 C81 C82 -179.9(3) . . . . ?
C11 N11 C82 O82 -6.5(6) . . . . ?
C11 N11 C82 C81 175.0(3) . . . . ?
C84 C81 C82 O82 -10.1(6) . . . . ?
N81 C81 C82 O82 168.8(4) . . . . ?
C84 C81 C82 N11 168.5(4) . . . . ?
N81 C81 C82 N11 -12.6(5) . . . . ?
C81 N81 C83 C71 179.2(3) . . . . ?
C81 N81 C83 S83 1.1(4) . . . . ?
N71 C71 C83 N81 64.5(4) . . . . ?
C73 C71 C83 N81 -59.7(4) . . . . ?
N71 C71 C83 S83 -117.6(3) . . . . ?
C73 C71 C83 S83 118.2(3) . . . . ?
N81 C83 S83 C84 -0.8(3) . . . . ?
C71 C83 S83 C84 -178.9(3) . . . . ?
N81 C81 C84 S83 0.4(4) . . . . ?
C82 C81 C84 S83 179.3(3) . . . . ?
C83 S83 C84 C81 0.2(3) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        70.07
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.959
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.075
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: N,N-Dimethylacetamide'
####################################################################### 
# 
# 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_valphg
_database_code_depnum_ccdc_archive 'CCDC 2191405'
loop_
_audit_author_name
_audit_author_address
'Akiko Asano'
;Faculty of Pharmacy, Osaka Medical and Pharmaceutical University
Japan
;
_audit_update_record             
;
2022-07-20 deposited with the CCDC.	2023-01-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 cyclo(Val-Oxz-D-Val-Thz-Phg-Oxz-D-Val-Thz).dimethylacetamide
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H47 N8 O6 S2, C4 H9 N O7'
_chemical_formula_sum            'C42 H56 N9 O7 S2'
_chemical_formula_weight         863.08

_chemical_compound_source        synthesis
_chemical_absolute_configuration rm

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'C2   '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'

_cell_length_a                   18.269(6)
_cell_length_b                   12.967(4)
_cell_length_c                   11.641(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 123.754(4)
_cell_angle_gamma                90.00
_cell_volume                     2292.9(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    240(2)
_cell_measurement_reflns_used    3354
_cell_measurement_theta_min      2.31
_cell_measurement_theta_max      27.82

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             918
_exptl_absorpt_coefficient_mu    0.173
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.837
_exptl_absorpt_correction_T_max  1.352
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'


_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      240(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode (M18XCE)'
_diffrn_radiation_monochromator  'conforcal (Bruker Montel)'
_diffrn_measurement_device_type  'CCD (Bruker APEX)'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 8.366
_diffrn_standards_number         101
_diffrn_standards_interval_count 7239
_diffrn_standards_interval_time  840
_diffrn_standards_decay_%        0.15
_diffrn_reflns_number            7239
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_sigmaI/netI    0.0994
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.10
_diffrn_reflns_theta_max         25.02
_reflns_number_total             3907
_reflns_number_gt                3055
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'SMART (Bruker, 1998)'
_computing_cell_refinement       'SAINT-PLUS (Bruker, 1998)'
_computing_data_reduction        'SAINT-PLUS (Bruker, 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0873P)²+6.8483P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack (1983), 1787 Friedel pairs'
# 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack   -0.3(3)
_refine_ls_number_reflns         3907
_refine_ls_number_parameters     330
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1249
_refine_ls_R_factor_gt           0.1071
_refine_ls_wR_factor_ref         0.2780
_refine_ls_wR_factor_gt          0.2655
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_restrained_S_all      1.141
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.003

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N11 N 0.3872(4) 0.3107(5) 0.5914(6) 0.0700(18) Uani 1 1 d . . .
H11 H 0.4092 0.2576 0.5751 0.084 Uiso 1 1 calc R . .
C11 C 0.3040(6) 0.3555(7) 0.4789(10) 0.081(3) Uani 1 1 d . . .
H11A H 0.2714 0.3832 0.5173 0.098 Uiso 1 1 calc R A 1
C12 C 0.321(6) 0.444(7) 0.408(9) 0.10(2) Uani 0.50 1 d P B 1
H12 H 0.3710 0.4229 0.4017 0.121 Uiso 0.50 1 calc PR B 1
C13 C 0.241(2) 0.460(2) 0.263(3) 0.154(12) Uani 0.50 1 d P B 1
H13A H 0.2170 0.3939 0.2194 0.231 Uiso 0.50 1 calc PR B 1
H13B H 0.2584 0.4981 0.2095 0.231 Uiso 0.50 1 calc PR B 1
H13C H 0.1973 0.4991 0.2664 0.231 Uiso 0.50 1 calc PR B 1
C14 C 0.346(2) 0.543(2) 0.489(4) 0.154(14) Uani 0.50 1 d P B 1
H14A H 0.3532 0.5968 0.4386 0.231 Uiso 0.50 1 calc PR B 1
H14B H 0.4004 0.5333 0.5783 0.231 Uiso 0.50 1 calc PR B 1
H14C H 0.2995 0.5621 0.5017 0.231 Uiso 0.50 1 calc PR B 1
C12' C 0.313(6) 0.435(7) 0.406(7) 0.09(2) Uani 0.50 1 d P B 2
C13' C 0.2794(17) 0.5306(14) 0.406(2) 0.086(5) Uani 0.50 1 d P B 2
H13' H 0.2461 0.5381 0.4450 0.103 Uiso 0.50 1 calc PR B 2
C14' C 0.2948(15) 0.6156(15) 0.350(2) 0.094(6) Uani 0.50 1 d P B 2
H14' H 0.2720 0.6805 0.3504 0.113 Uiso 0.50 1 calc PR B 2
C15' C 0.3438(8) 0.6046(9) 0.2925(11) 0.108(4) Uani 1 1 d . B 2
H15' H 0.3542 0.6621 0.2542 0.130 Uiso 1 1 calc R B 2
C16' C 0.3774(15) 0.5087(15) 0.2917(19) 0.093(6) Uani 0.50 1 d P B 2
H16' H 0.4106 0.5013 0.2529 0.112 Uiso 0.50 1 calc PR B 2
C17' C 0.3621(14) 0.4237(16) 0.3482(19) 0.084(5) Uani 0.50 1 d P B 2
H17' H 0.3848 0.3588 0.3476 0.101 Uiso 0.50 1 calc PR B 2
C23 C 0.2497(4) 0.2722(5) 0.3755(7) 0.0520(15) Uani 1 1 d . B .
N21 N 0.2758(3) 0.1811(4) 0.3722(5) 0.0485(12) Uani 1 1 d . . .
C21 C 0.2026(4) 0.1317(5) 0.2500(7) 0.0466(14) Uani 1 1 d . B .
H21 H 0.1878 0.0666 0.2771 0.056 Uiso 1 1 calc R . .
C22 C 0.1238(4) 0.2086(5) 0.1929(8) 0.0560(16) Uani 1 1 d . . .
H22 H 0.0985 0.2239 0.0944 0.067 Uiso 1 1 calc R B .
O22 O 0.1662(3) 0.3003(4) 0.2772(6) 0.0679(14) Uani 1 1 d . B .
C24 C 0.0523(5) 0.1737(8) 0.2126(10) 0.084(3) Uani 1 1 d . B .
H24A H 0.0062 0.2255 0.1755 0.127 Uiso 1 1 calc R . .
H24B H 0.0772 0.1645 0.3104 0.127 Uiso 1 1 calc R . .
H24C H 0.0277 0.1089 0.1646 0.127 Uiso 1 1 calc R . .
C25 C 0.2228(4) 0.1085(5) 0.1406(7) 0.0519(15) Uani 1 1 d . . .
O25 O 0.1642(3) 0.0932(6) 0.0226(5) 0.0860(19) Uani 1 1 d . B .
N31 N 0.3085(4) 0.1031(5) 0.1894(6) 0.0612(15) Uani 1 1 d . B .
H31 H 0.3471 0.1102 0.2776 0.073 Uiso 1 1 calc R . .
C31 C 0.3388(5) 0.0855(7) 0.0983(8) 0.070(2) Uani 1 1 d . . .
H31A H 0.2866 0.0762 0.0029 0.084 Uiso 1 1 calc R B .
C32 C 0.3955(7) -0.0102(8) 0.1385(12) 0.089(3) Uani 1 1 d . B .
H32 H 0.4464 -0.0037 0.2355 0.107 Uiso 1 1 calc R . .
C33 C 0.3411(9) -0.1050(10) 0.1246(14) 0.118(4) Uani 1 1 d . . .
H33A H 0.3780 -0.1660 0.1534 0.177 Uiso 1 1 calc R B .
H33B H 0.2922 -0.1126 0.0291 0.177 Uiso 1 1 calc R . .
H33C H 0.3188 -0.0964 0.1826 0.177 Uiso 1 1 calc R . .
C34 C 0.4288(11) -0.0213(12) 0.0442(16) 0.134(5) Uani 1 1 d . . .
H34A H 0.4654 -0.0823 0.0703 0.200 Uiso 1 1 calc R B .
H34B H 0.4629 0.0391 0.0533 0.200 Uiso 1 1 calc R . .
H34C H 0.3790 -0.0278 -0.0509 0.200 Uiso 1 1 calc R . .
C43 C 0.3878(5) 0.1816(7) 0.1013(7) 0.0626(19) Uani 1 1 d . B .
N41 N 0.4613(4) 0.2094(5) 0.2061(6) 0.0557(13) Uani 1 1 d . . .
C41 C 0.4879(5) 0.3021(6) 0.1787(7) 0.0550(16) Uani 1 1 d . B .
C42 C 0.4324(6) 0.3378(8) 0.0529(9) 0.083(3) Uani 1 1 d . . .
H42 H 0.4409 0.3996 0.0197 0.100 Uiso 1 1 calc R B .
S42 S 0.34552(16) 0.2611(2) -0.0407(2) 0.0960(9) Uani 1 1 d . B .
C44 C 0.5711(5) 0.3500(5) 0.2828(8) 0.0607(18) Uani 1 1 d . . .
O44 O 0.6026(4) 0.4236(5) 0.2548(6) 0.0845(17) Uani 1 1 d . B .
O1 O 0.5000 0.0678(18) 0.5000 0.153(6) Uani 1 2 d S . .
C1 C 0.4775(17) -0.018(2) 0.511(3) 0.108(8) Uani 0.50 1 d P . .
C2 C 0.404(5) -0.047(6) 0.520(9) 0.105(13) Uani 0.50 1 d P . .
H2A H 0.3973 -0.1213 0.5131 0.157 Uiso 0.50 1 calc PR . .
H2B H 0.3506 -0.0150 0.4444 0.157 Uiso 0.50 1 calc PR . .
H2C H 0.4150 -0.0238 0.6071 0.157 Uiso 0.50 1 calc PR . .
N1 N 0.5344(18) -0.093(2) 0.521(3) 0.132(8) Uani 0.50 1 d P . .
C3 C 0.530(3) -0.198(2) 0.549(3) 0.152(18) Uani 0.50 1 d P . .
H3A H 0.4792 -0.2083 0.5540 0.227 Uiso 0.50 1 calc PR . .
H3B H 0.5830 -0.2168 0.6357 0.227 Uiso 0.50 1 calc PR . .
H3C H 0.5239 -0.2397 0.4751 0.227 Uiso 0.50 1 calc PR . .
C4 C 0.610(7) -0.075(8) 0.516(11) 0.15(3) Uani 0.50 1 d P . .
H4A H 0.6177 -0.0010 0.5107 0.225 Uiso 0.50 1 calc PR . .
H4B H 0.6024 -0.1083 0.4354 0.225 Uiso 0.50 1 calc PR . .
H4C H 0.6625 -0.1021 0.5988 0.225 Uiso 0.50 1 calc PR . .


_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
N11 C44 1.321(9) 2_656 ?
N11 C11 1.467(11) . ?
N11 H11 0.8700 . ?
C11 C12' 1.40(7) . ?
C11 C23 1.508(10) . ?
C11 C12 1.54(9) . ?
C11 H11A 0.9900 . ?
C12 C14 1.51(10) . ?
C12 C13 1.51(9) . ?
C12 H12 0.9900 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 H13C 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 H14C 0.9700 . ?
C12' C13' 1.39(9) . ?
C12' C17' 1.39(8) . ?
C13' C14' 1.39(3) . ?
C13' H13' 0.9400 . ?
C14' C15' 1.39(3) . ?
C14' H14' 0.9400 . ?
C15' C16' 1.39(2) . ?
C15' H15' 0.9400 . ?
C16' C17' 1.39(2) . ?
C16' H16' 0.9400 . ?
C17' H17' 0.9400 . ?
C23 N21 1.283(8) . ?
C23 O22 1.353(8) . ?
N21 C21 1.451(8) . ?
C21 C25 1.539(9) . ?
C21 C22 1.564(9) . ?
C21 H21 0.9900 . ?
C22 O22 1.459(8) . ?
C22 C24 1.515(11) . ?
C22 H22 0.9900 . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 H24C 0.9700 . ?
C25 O25 1.199(8) . ?
C25 N31 1.338(8) . ?
N31 C31 1.462(9) . ?
N31 H31 0.8700 . ?
C31 C32 1.515(14) . ?
C31 C43 1.522(12) . ?
C31 H31A 0.9900 . ?
C32 C34 1.528(15) . ?
C32 C33 1.532(15) . ?
C32 H32 0.9900 . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C33 H33C 0.9700 . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C34 H34C 0.9700 . ?
C43 N41 1.265(8) . ?
C43 S42 1.724(8) . ?
N41 C41 1.398(9) . ?
C41 C42 1.318(11) . ?
C41 C44 1.455(11) . ?
C42 S42 1.666(11) . ?
C42 H42 0.9400 . ?
C44 O44 1.247(9) . ?
C44 N11 1.321(9) 2_656 ?
O1 C1 1.22(3) . ?
C1 N1 1.38(3) . ?
C1 C2 1.45(9) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 H2C 0.9700 . ?
N1 C3 1.41(4) . ?
N1 C4 1.44(11) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 H3C 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 H4C 0.9700 . ?

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
C44 N11 C11 120.7(6) 2_656 . ?
C44 N11 H11 119.7 2_656 . ?
C11 N11 H11 119.7 . . ?
C12' C11 N11 115(4) . . ?
C12' C11 C23 107(4) . . ?
N11 C11 C23 108.9(6) . . ?
C12' C11 C12 4(7) . . ?
N11 C11 C12 111(3) . . ?
C23 C11 C12 110(4) . . ?
C12' C11 H11A 108.2 . . ?
N11 C11 H11A 109.0 . . ?
C23 C11 H11A 109.0 . . ?
C12 C11 H11A 109.1 . . ?
C14 C12 C13 110(5) . . ?
C14 C12 C11 112(5) . . ?
C13 C12 C11 110(7) . . ?
C14 C12 H12 108.0 . . ?
C13 C12 H12 108.1 . . ?
C11 C12 H12 108.0 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13' C12' C17' 120(5) . . ?
C13' C12' C11 117(5) . . ?
C17' C12' C11 123(6) . . ?
C12' C13' C14' 120(4) . . ?
C12' C13' H13' 120.0 . . ?
C14' C13' H13' 120.0 . . ?
C15' C14' C13' 120(2) . . ?
C15' C14' H14' 120.0 . . ?
C13' C14' H14' 120.0 . . ?
C14' C15' C16' 120.0(15) . . ?
C14' C15' H15' 120.0 . . ?
C16' C15' H15' 120.0 . . ?
C15' C16' C17' 120(2) . . ?
C15' C16' H16' 120.0 . . ?
C17' C16' H16' 120.0 . . ?
C16' C17' C12' 120(4) . . ?
C16' C17' H17' 120.0 . . ?
C12' C17' H17' 120.0 . . ?
N21 C23 O22 119.1(6) . . ?
N21 C23 C11 126.4(6) . . ?
O22 C23 C11 114.5(6) . . ?
C23 N21 C21 106.3(5) . . ?
N21 C21 C25 112.5(5) . . ?
N21 C21 C22 105.4(5) . . ?
C25 C21 C22 111.1(5) . . ?
N21 C21 H21 109.2 . . ?
C25 C21 H21 109.2 . . ?
C22 C21 H21 109.2 . . ?
O22 C22 C24 108.7(6) . . ?
O22 C22 C21 102.4(5) . . ?
C24 C22 C21 114.4(6) . . ?
O22 C22 H22 110.3 . . ?
C24 C22 H22 110.3 . . ?
C21 C22 H22 110.3 . . ?
C23 O22 C22 106.1(5) . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O25 C25 N31 124.5(6) . . ?
O25 C25 C21 120.6(6) . . ?
N31 C25 C21 114.9(6) . . ?
C25 N31 C31 121.8(6) . . ?
C25 N31 H31 119.1 . . ?
C31 N31 H31 119.1 . . ?
N31 C31 C32 111.9(7) . . ?
N31 C31 C43 108.1(6) . . ?
C32 C31 C43 111.8(6) . . ?
N31 C31 H31A 108.3 . . ?
C32 C31 H31A 108.3 . . ?
C43 C31 H31A 108.3 . . ?
C31 C32 C34 109.3(10) . . ?
C31 C32 C33 109.4(8) . . ?
C34 C32 C33 110.0(9) . . ?
C31 C32 H32 109.3 . . ?
C34 C32 H32 109.3 . . ?
C33 C32 H32 109.3 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N41 C43 C31 123.4(7) . . ?
N41 C43 S42 115.1(6) . . ?
C31 C43 S42 121.5(6) . . ?
C43 N41 C41 110.0(6) . . ?
C42 C41 N41 113.9(8) . . ?
C42 C41 C44 125.3(7) . . ?
N41 C41 C44 120.8(6) . . ?
C41 C42 S42 112.4(7) . . ?
C41 C42 H42 123.8 . . ?
S42 C42 H42 123.8 . . ?
C42 S42 C43 88.5(4) . . ?
O44 C44 N11 121.2(7) . 2_656 ?
O44 C44 C41 121.9(7) . . ?
N11 C44 C41 116.8(6) 2_656 . ?
O1 C1 N1 111.8(19) . . ?
O1 C1 C2 129(4) . . ?
N1 C1 C2 120(4) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 N1 C3 124(3) . . ?
C1 N1 C4 125(4) . . ?
C3 N1 C4 110(5) . . ?
N1 C3 H3A 109.5 . . ?
N1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 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
C44 N11 C11 C12' 89(4) 2_656 . . . ?
C44 N11 C11 C23 -151.5(8) 2_656 . . . ?
C44 N11 C11 C12 87(4) 2_656 . . . ?
C12' C11 C12 C14 120(88) . . . . ?
N11 C11 C12 C14 -80(5) . . . . ?
C23 C11 C12 C14 160(4) . . . . ?
C12' C11 C12 C13 -3(82) . . . . ?
N11 C11 C12 C13 157(4) . . . . ?
C23 C11 C12 C13 37(6) . . . . ?
N11 C11 C12' C13' -120(5) . . . . ?
C23 C11 C12' C13' 119(6) . . . . ?
C12 C11 C12' C13' -99(88) . . . . ?
N11 C11 C12' C17' 53(8) . . . . ?
C23 C11 C12' C17' -68(7) . . . . ?
C12 C11 C12' C17' 73(84) . . . . ?
C17' C12' C13' C14' -0(8) . . . . ?
C11 C12' C13' C14' 173(4) . . . . ?
C12' C13' C14' C15' 0(5) . . . . ?
C13' C14' C15' C16' -0(3) . . . . ?
C14' C15' C16' C17' 0(3) . . . . ?
C15' C16' C17' C12' -0(5) . . . . ?
C13' C12' C17' C16' 0(8) . . . . ?
C11 C12' C17' C16' -172(5) . . . . ?
C12' C11 C23 N21 114(4) . . . . ?
N11 C11 C23 N21 -10.4(12) . . . . ?
C12 C11 C23 N21 111(3) . . . . ?
C12' C11 C23 O22 -65(4) . . . . ?
N11 C11 C23 O22 170.8(7) . . . . ?
C12 C11 C23 O22 -68(3) . . . . ?
O22 C23 N21 C21 2.4(8) . . . . ?
C11 C23 N21 C21 -176.5(8) . . . . ?
C23 N21 C21 C25 114.0(6) . . . . ?
C23 N21 C21 C22 -7.2(7) . . . . ?
N21 C21 C22 O22 9.1(6) . . . . ?
C25 C21 C22 O22 -113.1(6) . . . . ?
N21 C21 C22 C24 -108.3(7) . . . . ?
C25 C21 C22 C24 129.5(7) . . . . ?
N21 C23 O22 C22 3.9(8) . . . . ?
C11 C23 O22 C22 -177.1(7) . . . . ?
C24 C22 O22 C23 113.7(7) . . . . ?
C21 C22 O22 C23 -7.7(7) . . . . ?
N21 C21 C25 O25 -160.6(7) . . . . ?
C22 C21 C25 O25 -42.8(9) . . . . ?
N21 C21 C25 N31 21.9(8) . . . . ?
C22 C21 C25 N31 139.8(6) . . . . ?
O25 C25 N31 C31 5.0(12) . . . . ?
C21 C25 N31 C31 -177.6(6) . . . . ?
C25 N31 C31 C32 -121.8(8) . . . . ?
C25 N31 C31 C43 114.7(7) . . . . ?
N31 C31 C32 C34 -177.3(9) . . . . ?
C43 C31 C32 C34 -55.8(11) . . . . ?
N31 C31 C32 C33 62.2(10) . . . . ?
C43 C31 C32 C33 -176.4(8) . . . . ?
N31 C31 C43 N41 68.7(9) . . . . ?
C32 C31 C43 N41 -54.9(10) . . . . ?
N31 C31 C43 S42 -111.1(7) . . . . ?
C32 C31 C43 S42 125.3(7) . . . . ?
C31 C43 N41 C41 -178.0(6) . . . . ?
S42 C43 N41 C41 1.9(8) . . . . ?
C43 N41 C41 C42 -0.7(9) . . . . ?
C43 N41 C41 C44 -179.4(6) . . . . ?
N41 C41 C42 S42 -0.8(9) . . . . ?
C44 C41 C42 S42 177.8(6) . . . . ?
C41 C42 S42 C43 1.5(7) . . . . ?
N41 C43 S42 C42 -2.0(6) . . . . ?
C31 C43 S42 C42 177.8(6) . . . . ?
C42 C41 C44 O44 -9.5(12) . . . . ?
N41 C41 C44 O44 169.0(7) . . . . ?
C42 C41 C44 N11 171.7(8) . . . 2_656 ?
N41 C41 C44 N11 -9.8(10) . . . 2_656 ?
O1 C1 N1 C3 173(3) . . . . ?
C2 C1 N1 C3 -4(6) . . . . ?
O1 C1 N1 C4 -1(7) . . . . ?
C2 C1 N1 C4 -179(9) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.660
_refine_diff_density_min         -0.691
_refine_diff_density_rms         0.088
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: N,N-Dimethylacetamide'
