# 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_fme
_database_code_depnum_ccdc_archive 'CCDC 2289960'
loop_
_audit_author_name
_audit_author_address
'Akiko Asano'
;Faculty of Pharmacy, Osaka Medical and Pharmaceutical University
Japan
;
_audit_update_record             
;
2023-08-22 deposited with the CCDC.	2023-12-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 cyclo(Phe(Me)-Oxz-D-Val-Thz-Ile-Oxz-D-Val-Thz).MeCN
;
_chemical_name_common            Phe(Me)ASC
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H52 N8 O6 S2, C2 H3 N'
_chemical_formula_sum            'C42 H55 N9 O6 S2'
_chemical_formula_weight         846.07

_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           orthorhombic
_symmetry_space_group_name_H-M   P212121

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

_cell_length_a                   15.6599(13)
_cell_length_b                   16.5029(14)
_cell_length_c                   17.2608(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4460.8(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    240(2)
_cell_measurement_reflns_used    5998
_cell_measurement_theta_min      2.47
_cell_measurement_theta_max      25.85

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1800
_exptl_absorpt_coefficient_mu    0.175
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.889
_exptl_absorpt_correction_T_max  1.0
_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         337
_diffrn_standards_interval_count 36244
_diffrn_standards_interval_time  480
_diffrn_standards_decay_%        0.0
_diffrn_reflns_number            36244
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_sigmaI/netI    0.0329
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.71
_diffrn_reflns_theta_max         26.37
_reflns_number_total             9137
_reflns_number_gt                8537
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'SMART (Bruker, 1998)'
_computing_cell_refinement       'SAINTPLUS (Bruker, 1998)'
_computing_data_reduction        'SAINTPLUS (Bruker, 1998)'
_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)+(0.0946P)²+1.5174P] 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 H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(9)
_refine_ls_number_reflns         9137
_refine_ls_number_parameters     533
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0681
_refine_ls_wR_factor_ref         0.1749
_refine_ls_wR_factor_gt          0.1719
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_restrained_S_all      1.098
_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
N10 N 0.47465(17) 0.34963(17) 0.15821(16) 0.0434(6) Uani 1 1 d . . .
H10 H 0.5006 0.3874 0.1843 0.052 Uiso 1 1 calc R . .
C10 C 0.3884(2) 0.3248(2) 0.1804(2) 0.0450(7) Uani 1 1 d . . .
H10A H 0.3850 0.2649 0.1787 0.054 Uiso 1 1 calc R . .
C11 C 0.3724(3) 0.3531(3) 0.2641(2) 0.0576(9) Uani 1 1 d . . .
H11A H 0.4106 0.3232 0.2989 0.069 Uiso 1 1 calc R . .
H11B H 0.3869 0.4107 0.2682 0.069 Uiso 1 1 calc R . .
C12 C 0.2817(2) 0.3412(2) 0.2906(2) 0.0525(8) Uani 1 1 d . . .
C13 C 0.2415(3) 0.4025(3) 0.3309(3) 0.0714(12) Uani 1 1 d . . .
H13 H 0.2699 0.4520 0.3386 0.086 Uiso 1 1 calc R . .
C14 C 0.1602(3) 0.3921(3) 0.3599(3) 0.0791(14) Uani 1 1 d . . .
H14 H 0.1351 0.4340 0.3890 0.095 Uiso 1 1 calc R . .
C15 C 0.1148(3) 0.3217(3) 0.3473(3) 0.0696(12) Uani 1 1 d . . .
C16 C 0.1545(3) 0.2611(3) 0.3062(3) 0.0626(10) Uani 1 1 d . . .
H16 H 0.1250 0.2125 0.2968 0.075 Uiso 1 1 calc R . .
C17 C 0.2369(3) 0.2700(2) 0.2783(2) 0.0591(10) Uani 1 1 d . . .
H17 H 0.2627 0.2273 0.2508 0.071 Uiso 1 1 calc R . .
C18 C 0.0244(3) 0.3089(4) 0.3802(4) 0.1024(19) Uani 1 1 d . . .
H18A H 0.0036 0.2559 0.3650 0.154 Uiso 1 1 calc R . .
H18B H -0.0134 0.3504 0.3600 0.154 Uiso 1 1 calc R . .
H18C H 0.0262 0.3125 0.4362 0.154 Uiso 1 1 calc R . .
N20 N 0.27784(18) 0.31708(17) 0.07899(17) 0.0450(6) Uani 1 1 d . . .
C20 C 0.2342(2) 0.3750(2) 0.0295(2) 0.0490(8) Uani 1 1 d . . .
H20 H 0.1727 0.3614 0.0267 0.059 Uiso 1 1 calc R . .
C21 C 0.2460(3) 0.4576(2) 0.0713(3) 0.0570(9) Uani 1 1 d . . .
H21 H 0.2601 0.5008 0.0336 0.068 Uiso 1 1 calc R . .
C22 C 0.1704(3) 0.4822(3) 0.1213(4) 0.0895(16) Uani 1 1 d . . .
H22A H 0.1823 0.5338 0.1458 0.134 Uiso 1 1 calc R . .
H22B H 0.1607 0.4414 0.1607 0.134 Uiso 1 1 calc R . .
H22C H 0.1198 0.4872 0.0891 0.134 Uiso 1 1 calc R . .
O22 O 0.31865(16) 0.44101(14) 0.12188(15) 0.0507(6) Uani 1 1 d . . .
C23 C 0.3248(2) 0.35884(19) 0.12417(19) 0.0423(7) Uani 1 1 d . . .
C24 C 0.2720(2) 0.3794(2) -0.0527(2) 0.0496(8) Uani 1 1 d . . .
O24 O 0.2375(2) 0.41928(19) -0.10123(18) 0.0697(8) Uani 1 1 d . . .
N30 N 0.34751(19) 0.34105(17) -0.06188(17) 0.0477(6) Uani 1 1 d . . .
H30 H 0.3620 0.3022 -0.0305 0.057 Uiso 1 1 calc R . .
C30 C 0.4043(2) 0.3647(2) -0.1239(2) 0.0521(8) Uani 1 1 d . . .
H30A H 0.3712 0.4017 -0.1576 0.063 Uiso 1 1 calc R . .
C31 C 0.4325(3) 0.2938(3) -0.1760(2) 0.0660(11) Uani 1 1 d . . .
H31 H 0.4738 0.3156 -0.2141 0.079 Uiso 1 1 calc R . .
C32 C 0.3568(3) 0.2618(4) -0.2207(3) 0.0845(15) Uani 1 1 d . . .
H32A H 0.3747 0.2167 -0.2529 0.127 Uiso 1 1 calc R . .
H32B H 0.3339 0.3046 -0.2533 0.127 Uiso 1 1 calc R . .
H32C H 0.3131 0.2438 -0.1848 0.127 Uiso 1 1 calc R . .
C33 C 0.4781(3) 0.2257(3) -0.1308(3) 0.0758(13) Uani 1 1 d . . .
H33A H 0.5258 0.2484 -0.1021 0.114 Uiso 1 1 calc R . .
H33B H 0.4990 0.1852 -0.1668 0.114 Uiso 1 1 calc R . .
H33C H 0.4383 0.2008 -0.0949 0.114 Uiso 1 1 calc R . .
N40 N 0.46908(18) 0.45602(17) -0.02659(15) 0.0428(6) Uani 1 1 d . . .
C40 C 0.5420(2) 0.5016(2) -0.01360(19) 0.0419(7) Uani 1 1 d . . .
C41 C 0.6034(2) 0.4958(2) -0.0680(2) 0.0520(8) Uani 1 1 d . . .
H41 H 0.6557 0.5238 -0.0672 0.062 Uiso 1 1 calc R . .
S42 S 0.57181(7) 0.42985(7) -0.13887(5) 0.0620(3) Uani 1 1 d . . .
C43 C 0.4759(2) 0.4148(2) -0.09008(19) 0.0461(7) Uani 1 1 d . . .
C44 C 0.5508(2) 0.55555(19) 0.05450(19) 0.0430(7) Uani 1 1 d . . .
O44 O 0.61465(16) 0.59550(16) 0.06493(16) 0.0569(6) Uani 1 1 d . . .
N50 N 0.48160(16) 0.55915(16) 0.10210(16) 0.0410(6) Uani 1 1 d . . .
H50 H 0.4381 0.5275 0.0941 0.049 Uiso 1 1 calc R . .
C50 C 0.4806(2) 0.61614(19) 0.1665(2) 0.0426(7) Uani 1 1 d . . .
H50A H 0.5064 0.6673 0.1478 0.051 Uiso 1 1 calc R . .
C51 C 0.3891(2) 0.6355(2) 0.1922(2) 0.0478(8) Uani 1 1 d . . .
H51 H 0.3602 0.5836 0.2037 0.057 Uiso 1 1 calc R . .
C52 C 0.3402(3) 0.6768(2) 0.1269(3) 0.0623(10) Uani 1 1 d . . .
H52A H 0.3447 0.6431 0.0803 0.075 Uiso 1 1 calc R . .
H52B H 0.2798 0.6795 0.1412 0.075 Uiso 1 1 calc R . .
C53 C 0.3903(3) 0.6858(3) 0.2670(3) 0.0738(13) Uani 1 1 d . . .
H53A H 0.4226 0.6573 0.3064 0.111 Uiso 1 1 calc R . .
H53B H 0.3322 0.6941 0.2849 0.111 Uiso 1 1 calc R . .
H53C H 0.4168 0.7379 0.2569 0.111 Uiso 1 1 calc R . .
N60 N 0.60541(18) 0.61798(17) 0.25347(17) 0.0467(7) Uani 1 1 d . . .
C60 C 0.6428(2) 0.5617(2) 0.3097(2) 0.0518(8) Uani 1 1 d . . .
H60 H 0.6639 0.5922 0.3552 0.062 Uiso 1 1 calc R . .
C61 C 0.5664(2) 0.5068(3) 0.3342(2) 0.0561(9) Uani 1 1 d . . .
H61 H 0.5844 0.4498 0.3408 0.067 Uiso 1 1 calc R . .
C62 C 0.5204(3) 0.5377(4) 0.4050(3) 0.0804(14) Uani 1 1 d . . .
H62A H 0.4741 0.5011 0.4179 0.121 Uiso 1 1 calc R . .
H62B H 0.4975 0.5912 0.3945 0.121 Uiso 1 1 calc R . .
H62C H 0.5601 0.5407 0.4481 0.121 Uiso 1 1 calc R . .
O62 O 0.51035(15) 0.51641(14) 0.26621(14) 0.0484(5) Uani 1 1 d . . .
C63 C 0.5361(2) 0.58483(19) 0.23139(19) 0.0414(7) Uani 1 1 d . . .
C64 C 0.7150(2) 0.5108(2) 0.2758(2) 0.0513(8) Uani 1 1 d . . .
O64 O 0.7517(2) 0.4619(2) 0.31640(17) 0.0738(9) Uani 1 1 d . . .
N70 N 0.73310(19) 0.52283(19) 0.20103(17) 0.0506(7) Uani 1 1 d . . .
H70 H 0.7152 0.5669 0.1787 0.061 Uiso 1 1 calc R . .
C70 C 0.7821(2) 0.4642(2) 0.1557(2) 0.0487(8) Uani 1 1 d . . .
H70A H 0.8107 0.4285 0.1937 0.058 Uiso 1 1 calc R . .
C71 C 0.8535(2) 0.5019(2) 0.1064(2) 0.0541(9) Uani 1 1 d . . .
H71 H 0.8766 0.4584 0.0730 0.065 Uiso 1 1 calc R . .
C72 C 0.8215(3) 0.5682(3) 0.0533(2) 0.0627(10) Uani 1 1 d . . .
H72A H 0.7761 0.5472 0.0208 0.094 Uiso 1 1 calc R . .
H72B H 0.8681 0.5872 0.0209 0.094 Uiso 1 1 calc R . .
H72C H 0.7999 0.6129 0.0841 0.094 Uiso 1 1 calc R . .
C73 C 0.9257(3) 0.5311(3) 0.1571(3) 0.0699(11) Uani 1 1 d . . .
H73A H 0.9452 0.4870 0.1898 0.105 Uiso 1 1 calc R . .
H73B H 0.9060 0.5755 0.1892 0.105 Uiso 1 1 calc R . .
H73C H 0.9725 0.5495 0.1247 0.105 Uiso 1 1 calc R . .
N80 N 0.64228(17) 0.39650(17) 0.13379(16) 0.0437(6) Uani 1 1 d . . .
C80 C 0.6044(2) 0.34160(19) 0.08465(19) 0.0427(7) Uani 1 1 d . . .
C81 C 0.6533(2) 0.3133(2) 0.0260(2) 0.0494(8) Uani 1 1 d . . .
H81 H 0.6358 0.2749 -0.0110 0.059 Uiso 1 1 calc R . .
S82 S 0.75200(6) 0.35779(6) 0.02944(6) 0.0540(2) Uani 1 1 d . . .
C83 C 0.7202(2) 0.4113(2) 0.1120(2) 0.0458(7) Uani 1 1 d . . .
O84 O 0.48048(17) 0.26381(16) 0.05618(16) 0.0575(6) Uani 1 1 d . . .
C84 C 0.5140(2) 0.3144(2) 0.09769(19) 0.0443(7) Uani 1 1 d . . .
C54 C 0.3703(4) 0.7602(4) 0.1077(5) 0.119(3) Uani 1 1 d . . .
H54A H 0.3355 0.7824 0.0664 0.179 Uiso 1 1 calc R . .
H54B H 0.4295 0.7581 0.0911 0.179 Uiso 1 1 calc R . .
H54C H 0.3656 0.7944 0.1532 0.179 Uiso 1 1 calc R . .
N1A N 0.4450(7) 0.3629(6) 0.4856(8) 0.201(4) Uani 1 1 d U . .
C1A C 0.3904(6) 0.3210(5) 0.4869(5) 0.118(2) Uani 1 1 d . . .
C2A C 0.3236(4) 0.2681(4) 0.4834(4) 0.0999(18) Uani 1 1 d . . .
H2A1 H 0.3124 0.2467 0.5347 0.150 Uiso 1 1 calc R . .
H2A2 H 0.3377 0.2240 0.4486 0.150 Uiso 1 1 calc R . .
H2A3 H 0.2733 0.2961 0.4645 0.150 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
N10 C84 1.345(4) . ?
N10 C10 1.463(4) . ?
N10 H10 0.8700 . ?
C10 C23 1.499(5) . ?
C10 C11 1.540(5) . ?
C10 H10A 0.9900 . ?
C11 C12 1.505(5) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C12 C13 1.380(6) . ?
C12 C17 1.385(5) . ?
C13 C14 1.378(7) . ?
C13 H13 0.9400 . ?
C14 C15 1.379(7) . ?
C14 H14 0.9400 . ?
C15 C16 1.375(6) . ?
C15 C18 1.539(6) . ?
C16 C17 1.385(6) . ?
C16 H16 0.9400 . ?
C17 H17 0.9400 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 H18C 0.9700 . ?
N20 C23 1.274(4) . ?
N20 C20 1.453(5) . ?
C20 C24 1.539(5) . ?
C20 C21 1.552(5) . ?
C20 H20 0.9900 . ?
C21 O22 1.461(5) . ?
C21 C22 1.520(6) . ?
C21 H21 0.9900 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 H22C 0.9700 . ?
O22 C23 1.360(4) . ?
C24 O24 1.195(4) . ?
C24 N30 1.351(5) . ?
N30 C30 1.446(5) . ?
N30 H30 0.8700 . ?
C30 C43 1.510(5) . ?
C30 C31 1.540(6) . ?
C30 H30A 0.9900 . ?
C31 C32 1.511(6) . ?
C31 C33 1.543(7) . ?
C31 H31 0.9900 . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 H32C 0.9700 . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C33 H33C 0.9700 . ?
N40 C43 1.294(4) . ?
N40 C40 1.385(4) . ?
C40 C41 1.349(5) . ?
C40 C44 1.482(5) . ?
C41 S42 1.710(4) . ?
C41 H41 0.9400 . ?
S42 C43 1.740(3) . ?
C44 O44 1.211(4) . ?
C44 N50 1.361(4) . ?
N50 C50 1.456(4) . ?
N50 H50 0.8700 . ?
C50 C63 1.509(5) . ?
C50 C51 1.533(5) . ?
C50 H50A 0.9900 . ?
C51 C52 1.523(6) . ?
C51 C53 1.535(5) . ?
C51 H51 0.9900 . ?
C52 C54 1.493(7) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C53 H53A 0.9700 . ?
C53 H53B 0.9700 . ?
C53 H53C 0.9700 . ?
N60 C63 1.274(4) . ?
N60 C60 1.465(5) . ?
C60 C64 1.526(5) . ?
C60 C61 1.559(5) . ?
C60 H60 0.9900 . ?
C61 O62 1.474(4) . ?
C61 C62 1.507(6) . ?
C61 H61 0.9900 . ?
C62 H62A 0.9700 . ?
C62 H62B 0.9700 . ?
C62 H62C 0.9700 . ?
O62 C63 1.341(4) . ?
C64 O64 1.213(5) . ?
C64 N70 1.336(5) . ?
N70 C70 1.461(4) . ?
N70 H70 0.8700 . ?
C70 C83 1.506(5) . ?
C70 C71 1.537(5) . ?
C70 H70A 0.9900 . ?
C71 C73 1.509(6) . ?
C71 C72 1.513(6) . ?
C71 H71 0.9900 . ?
C72 H72A 0.9700 . ?
C72 H72B 0.9700 . ?
C72 H72C 0.9700 . ?
C73 H73A 0.9700 . ?
C73 H73B 0.9700 . ?
C73 H73C 0.9700 . ?
N80 C83 1.301(4) . ?
N80 C80 1.376(4) . ?
C80 C81 1.353(5) . ?
C80 C84 1.502(5) . ?
C81 S82 1.712(4) . ?
C81 H81 0.9400 . ?
S82 C83 1.749(3) . ?
O84 C84 1.218(4) . ?
C54 H54A 0.9700 . ?
C54 H54B 0.9700 . ?
C54 H54C 0.9700 . ?
N1A C1A 1.101(11) . ?
C1A C2A 1.363(10) . ?
C2A H2A1 0.9700 . ?
C2A H2A2 0.9700 . ?
C2A H2A3 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
C84 N10 C10 120.3(3) . . ?
C84 N10 H10 119.8 . . ?
C10 N10 H10 119.8 . . ?
N10 C10 C23 109.8(3) . . ?
N10 C10 C11 108.0(3) . . ?
C23 C10 C11 112.7(3) . . ?
N10 C10 H10A 108.7 . . ?
C23 C10 H10A 108.7 . . ?
C11 C10 H10A 108.7 . . ?
C12 C11 C10 113.5(3) . . ?
C12 C11 H11A 108.9 . . ?
C10 C11 H11A 108.9 . . ?
C12 C11 H11B 108.9 . . ?
C10 C11 H11B 108.9 . . ?
H11A C11 H11B 107.7 . . ?
C13 C12 C17 117.9(4) . . ?
C13 C12 C11 119.2(4) . . ?
C17 C12 C11 122.8(4) . . ?
C14 C13 C12 120.9(4) . . ?
C14 C13 H13 119.6 . . ?
C12 C13 H13 119.6 . . ?
C13 C14 C15 121.6(4) . . ?
C13 C14 H14 119.2 . . ?
C15 C14 H14 119.2 . . ?
C16 C15 C14 117.4(4) . . ?
C16 C15 C18 120.4(5) . . ?
C14 C15 C18 122.1(5) . . ?
C15 C16 C17 121.6(4) . . ?
C15 C16 H16 119.2 . . ?
C17 C16 H16 119.2 . . ?
C12 C17 C16 120.5(4) . . ?
C12 C17 H17 119.7 . . ?
C16 C17 H17 119.7 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C23 N20 C20 105.9(3) . . ?
N20 C20 C24 113.1(3) . . ?
N20 C20 C21 104.5(3) . . ?
C24 C20 C21 110.0(3) . . ?
N20 C20 H20 109.7 . . ?
C24 C20 H20 109.7 . . ?
C21 C20 H20 109.7 . . ?
O22 C21 C22 108.5(4) . . ?
O22 C21 C20 101.9(3) . . ?
C22 C21 C20 114.0(4) . . ?
O22 C21 H21 110.7 . . ?
C22 C21 H21 110.7 . . ?
C20 C21 H21 110.7 . . ?
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 . . ?
C23 O22 C21 105.0(3) . . ?
N20 C23 O22 118.8(3) . . ?
N20 C23 C10 125.2(3) . . ?
O22 C23 C10 116.1(3) . . ?
O24 C24 N30 124.8(4) . . ?
O24 C24 C20 119.9(3) . . ?
N30 C24 C20 115.0(3) . . ?
C24 N30 C30 120.0(3) . . ?
C24 N30 H30 120.0 . . ?
C30 N30 H30 120.0 . . ?
N30 C30 C43 108.5(3) . . ?
N30 C30 C31 113.8(3) . . ?
C43 C30 C31 115.4(3) . . ?
N30 C30 H30A 106.1 . . ?
C43 C30 H30A 106.1 . . ?
C31 C30 H30A 106.1 . . ?
C32 C31 C30 109.8(4) . . ?
C32 C31 C33 111.6(4) . . ?
C30 C31 C33 113.0(3) . . ?
C32 C31 H31 107.4 . . ?
C30 C31 H31 107.4 . . ?
C33 C31 H31 107.4 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C43 N40 C40 110.8(3) . . ?
C41 C40 N40 115.9(3) . . ?
C41 C40 C44 121.9(3) . . ?
N40 C40 C44 122.1(3) . . ?
C40 C41 S42 109.6(3) . . ?
C40 C41 H41 125.2 . . ?
S42 C41 H41 125.2 . . ?
C41 S42 C43 89.71(17) . . ?
N40 C43 C30 123.7(3) . . ?
N40 C43 S42 113.9(3) . . ?
C30 C43 S42 122.1(2) . . ?
O44 C44 N50 122.9(3) . . ?
O44 C44 C40 121.5(3) . . ?
N50 C44 C40 115.5(3) . . ?
C44 N50 C50 119.8(3) . . ?
C44 N50 H50 120.1 . . ?
C50 N50 H50 120.1 . . ?
N50 C50 C63 109.8(3) . . ?
N50 C50 C51 111.4(3) . . ?
C63 C50 C51 113.2(3) . . ?
N50 C50 H50A 107.3 . . ?
C63 C50 H50A 107.3 . . ?
C51 C50 H50A 107.3 . . ?
C52 C51 C50 110.4(3) . . ?
C52 C51 C53 112.7(3) . . ?
C50 C51 C53 110.2(3) . . ?
C52 C51 H51 107.8 . . ?
C50 C51 H51 107.8 . . ?
C53 C51 H51 107.8 . . ?
C54 C52 C51 114.7(4) . . ?
C54 C52 H52A 108.6 . . ?
C51 C52 H52A 108.6 . . ?
C54 C52 H52B 108.6 . . ?
C51 C52 H52B 108.6 . . ?
H52A C52 H52B 107.6 . . ?
C51 C53 H53A 109.5 . . ?
C51 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C51 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C63 N60 C60 105.4(3) . . ?
N60 C60 C64 113.0(3) . . ?
N60 C60 C61 104.0(3) . . ?
C64 C60 C61 110.7(3) . . ?
N60 C60 H60 109.7 . . ?
C64 C60 H60 109.7 . . ?
C61 C60 H60 109.7 . . ?
O62 C61 C62 109.0(3) . . ?
O62 C61 C60 100.3(3) . . ?
C62 C61 C60 113.0(4) . . ?
O62 C61 H61 111.4 . . ?
C62 C61 H61 111.4 . . ?
C60 C61 H61 111.4 . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C63 O62 C61 105.6(3) . . ?
N60 C63 O62 118.9(3) . . ?
N60 C63 C50 124.5(3) . . ?
O62 C63 C50 116.6(3) . . ?
O64 C64 N70 123.8(4) . . ?
O64 C64 C60 119.7(3) . . ?
N70 C64 C60 116.5(3) . . ?
C64 N70 C70 122.0(3) . . ?
C64 N70 H70 119.0 . . ?
C70 N70 H70 119.0 . . ?
N70 C70 C83 108.3(3) . . ?
N70 C70 C71 114.2(3) . . ?
C83 C70 C71 115.2(3) . . ?
N70 C70 H70A 106.1 . . ?
C83 C70 H70A 106.1 . . ?
C71 C70 H70A 106.1 . . ?
C73 C71 C72 111.6(4) . . ?
C73 C71 C70 110.7(3) . . ?
C72 C71 C70 112.8(3) . . ?
C73 C71 H71 107.1 . . ?
C72 C71 H71 107.1 . . ?
C70 C71 H71 107.1 . . ?
C71 C72 H72A 109.5 . . ?
C71 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
C71 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
C71 C73 H73A 109.5 . . ?
C71 C73 H73B 109.5 . . ?
H73A C73 H73B 109.5 . . ?
C71 C73 H73C 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?
C83 N80 C80 110.5(3) . . ?
C81 C80 N80 116.4(3) . . ?
C81 C80 C84 122.9(3) . . ?
N80 C80 C84 120.8(3) . . ?
C80 C81 S82 109.7(3) . . ?
C80 C81 H81 125.1 . . ?
S82 C81 H81 125.1 . . ?
C81 S82 C83 89.33(17) . . ?
N80 C83 C70 124.6(3) . . ?
N80 C83 S82 114.1(3) . . ?
C70 C83 S82 121.2(2) . . ?
O84 C84 N10 123.8(3) . . ?
O84 C84 C80 121.5(3) . . ?
N10 C84 C80 114.7(3) . . ?
C52 C54 H54A 109.5 . . ?
C52 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C52 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
N1A C1A C2A 176.2(13) . . ?
C1A C2A H2A1 109.5 . . ?
C1A C2A H2A2 109.5 . . ?
H2A1 C2A H2A2 109.5 . . ?
C1A C2A H2A3 109.5 . . ?
H2A1 C2A H2A3 109.5 . . ?
H2A2 C2A H2A3 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
C84 N10 C10 C23 -75.2(4) . . . . ?
C84 N10 C10 C11 161.4(3) . . . . ?
N10 C10 C11 C12 172.3(3) . . . . ?
C23 C10 C11 C12 50.8(4) . . . . ?
C10 C11 C12 C13 -135.9(4) . . . . ?
C10 C11 C12 C17 46.0(5) . . . . ?
C17 C12 C13 C14 1.9(7) . . . . ?
C11 C12 C13 C14 -176.3(5) . . . . ?
C12 C13 C14 C15 -2.6(8) . . . . ?
C13 C14 C15 C16 1.6(8) . . . . ?
C13 C14 C15 C18 179.3(6) . . . . ?
C14 C15 C16 C17 0.0(7) . . . . ?
C18 C15 C16 C17 -177.7(5) . . . . ?
C13 C12 C17 C16 -0.3(6) . . . . ?
C11 C12 C17 C16 177.8(4) . . . . ?
C15 C16 C17 C12 -0.6(7) . . . . ?
C23 N20 C20 C24 103.8(3) . . . . ?
C23 N20 C20 C21 -15.8(3) . . . . ?
N20 C20 C21 O22 19.7(3) . . . . ?
C24 C20 C21 O22 -102.0(3) . . . . ?
N20 C20 C21 C22 -97.0(4) . . . . ?
C24 C20 C21 C22 141.4(4) . . . . ?
C22 C21 O22 C23 104.1(4) . . . . ?
C20 C21 O22 C23 -16.4(3) . . . . ?
C20 N20 C23 O22 5.7(4) . . . . ?
C20 N20 C23 C10 -173.6(3) . . . . ?
C21 O22 C23 N20 7.9(4) . . . . ?
C21 O22 C23 C10 -172.8(3) . . . . ?
N10 C10 C23 N20 115.3(3) . . . . ?
C11 C10 C23 N20 -124.1(3) . . . . ?
N10 C10 C23 O22 -63.9(4) . . . . ?
C11 C10 C23 O22 56.6(4) . . . . ?
N20 C20 C24 O24 173.4(3) . . . . ?
C21 C20 C24 O24 -70.2(4) . . . . ?
N20 C20 C24 N30 -11.6(4) . . . . ?
C21 C20 C24 N30 104.8(3) . . . . ?
O24 C24 N30 C30 18.1(5) . . . . ?
C20 C24 N30 C30 -156.6(3) . . . . ?
C24 N30 C30 C43 103.4(4) . . . . ?
C24 N30 C30 C31 -126.7(4) . . . . ?
N30 C30 C31 C32 67.1(5) . . . . ?
C43 C30 C31 C32 -166.5(4) . . . . ?
N30 C30 C31 C33 -58.2(5) . . . . ?
C43 C30 C31 C33 68.2(5) . . . . ?
C43 N40 C40 C41 1.1(4) . . . . ?
C43 N40 C40 C44 179.0(3) . . . . ?
N40 C40 C41 S42 -1.0(4) . . . . ?
C44 C40 C41 S42 -178.9(2) . . . . ?
C40 C41 S42 C43 0.5(3) . . . . ?
C40 N40 C43 C30 -174.6(3) . . . . ?
C40 N40 C43 S42 -0.6(4) . . . . ?
N30 C30 C43 N40 -25.6(5) . . . . ?
C31 C30 C43 N40 -154.6(3) . . . . ?
N30 C30 C43 S42 161.0(3) . . . . ?
C31 C30 C43 S42 32.0(5) . . . . ?
C41 S42 C43 N40 0.1(3) . . . . ?
C41 S42 C43 C30 174.2(3) . . . . ?
C41 C40 C44 O44 -1.6(5) . . . . ?
N40 C40 C44 O44 -179.5(3) . . . . ?
C41 C40 C44 N50 176.0(3) . . . . ?
N40 C40 C44 N50 -1.8(4) . . . . ?
O44 C44 N50 C50 3.4(5) . . . . ?
C40 C44 N50 C50 -174.2(3) . . . . ?
C44 N50 C50 C63 -76.2(4) . . . . ?
C44 N50 C50 C51 157.4(3) . . . . ?
N50 C50 C51 C52 -62.8(4) . . . . ?
C63 C50 C51 C52 172.7(3) . . . . ?
N50 C50 C51 C53 172.0(3) . . . . ?
C63 C50 C51 C53 47.6(4) . . . . ?
C50 C51 C52 C54 -68.5(5) . . . . ?
C53 C51 C52 C54 55.2(6) . . . . ?
C63 N60 C60 C64 101.5(3) . . . . ?
C63 N60 C60 C61 -18.6(3) . . . . ?
N60 C60 C61 O62 23.4(4) . . . . ?
C64 C60 C61 O62 -98.2(3) . . . . ?
N60 C60 C61 C62 -92.4(4) . . . . ?
C64 C60 C61 C62 145.9(3) . . . . ?
C62 C61 O62 C63 98.5(4) . . . . ?
C60 C61 O62 C63 -20.3(4) . . . . ?
C60 N60 C63 O62 5.9(4) . . . . ?
C60 N60 C63 C50 -172.5(3) . . . . ?
C61 O62 C63 N60 10.5(4) . . . . ?
C61 O62 C63 C50 -170.9(3) . . . . ?
N50 C50 C63 N60 113.1(3) . . . . ?
C51 C50 C63 N60 -121.6(3) . . . . ?
N50 C50 C63 O62 -65.4(3) . . . . ?
C51 C50 C63 O62 59.9(4) . . . . ?
N60 C60 C64 O64 179.7(3) . . . . ?
C61 C60 C64 O64 -64.2(4) . . . . ?
N60 C60 C64 N70 -1.2(4) . . . . ?
C61 C60 C64 N70 115.0(4) . . . . ?
O64 C64 N70 C70 16.9(5) . . . . ?
C60 C64 N70 C70 -162.2(3) . . . . ?
C64 N70 C70 C83 96.7(4) . . . . ?
C64 N70 C70 C71 -133.4(3) . . . . ?
N70 C70 C71 C73 71.3(4) . . . . ?
C83 C70 C71 C73 -162.3(3) . . . . ?
N70 C70 C71 C72 -54.6(4) . . . . ?
C83 C70 C71 C72 71.7(4) . . . . ?
C83 N80 C80 C81 1.0(4) . . . . ?
C83 N80 C80 C84 179.8(3) . . . . ?
N80 C80 C81 S82 -1.2(4) . . . . ?
C84 C80 C81 S82 180.0(2) . . . . ?
C80 C81 S82 C83 0.8(3) . . . . ?
C80 N80 C83 C70 -175.7(3) . . . . ?
C80 N80 C83 S82 -0.3(3) . . . . ?
N70 C70 C83 N80 -26.2(5) . . . . ?
C71 C70 C83 N80 -155.5(3) . . . . ?
N70 C70 C83 S82 158.8(2) . . . . ?
C71 C70 C83 S82 29.5(4) . . . . ?
C81 S82 C83 N80 -0.3(3) . . . . ?
C81 S82 C83 C70 175.2(3) . . . . ?
C10 N10 C84 O84 3.5(5) . . . . ?
C10 N10 C84 C80 -176.1(3) . . . . ?
C81 C80 C84 O84 1.1(5) . . . . ?
N80 C80 C84 O84 -177.6(3) . . . . ?
C81 C80 C84 N10 -179.3(3) . . . . ?
N80 C80 C84 N10 2.0(4) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.532
_refine_diff_density_min         -0.177
_refine_diff_density_rms         0.062
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile'
####################################################################### 
# 
# 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_phe4i
_database_code_depnum_ccdc_archive 'CCDC 2289961'
loop_
_audit_author_name
_audit_author_address
'Akiko Asano'
;Osaka Medical nad Pharmaceutical University
Japan
;
_audit_update_record             
;
2023-08-22 deposited with the CCDC.	2023-12-19 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT971_phe4i               
;
PROBLEM: Check Calcd Resid. Dens. 1.23Ang From I17A 4.29 eA-3
PROBLEM: Check Calcd Resid. Dens. 1.20Ang From I17B 4.11 eA-3
PROBLEM: Check Calcd Resid. Dens. 1.14Ang From I17A 3.87 eA-3
PROBLEM: Check Calcd Resid. Dens. 1.17Ang From I17B 3.76 eA-3
RESPONSE: Residual density resides near the heavy atom.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        Phe(4I)_ASC
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C39 H48 I N8 O6 S2, C39 H49 I N8 O6 S2, C4 H9 N O'
_chemical_formula_sum            'C82 H106 I2 N17 O13 S4'
_chemical_formula_weight         1919.88
_chemical_compound_source        synthesis
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'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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'

_cell_length_a                   13.7742(6)
_cell_length_b                   21.7130(16)
_cell_length_c                   15.1389(6)
_cell_angle_alpha                90
_cell_angle_beta                 91.337(4)
_cell_angle_gamma                90
_cell_volume                     4526.5(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100
_cell_measurement_reflns_used    8857
_cell_measurement_theta_min      3.5250
_cell_measurement_theta_max      73.5900

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_F_000             1982.0
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    6.876
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7101
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   rotating-anode
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single & P200K'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 5.811
_diffrn_reflns_number            26294
_diffrn_reflns_av_unetI/netI     0.0984
_diffrn_reflns_av_R_equivalents  0.0779
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.920
_diffrn_reflns_theta_max         68.251
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.808
_diffrn_reflns_point_group_measured_fraction_full 0.810
_reflns_number_total             13407
_reflns_number_gt                9911
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.572
_reflns_Friedel_fraction_max     0.606
_reflns_Friedel_fraction_full    0.609

_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
_computing_cell_refinement       CrysAlisPro
_computing_data_reduction        CrysAlisPro
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_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 x determined using 2754 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.000(10)
_chemical_absolute_configuration rm
_refine_ls_number_reflns         13407
_refine_ls_number_parameters     1063
_refine_ls_number_restraints     133
_refine_ls_R_factor_all          0.1296
_refine_ls_R_factor_gt           0.1093
_refine_ls_wR_factor_ref         0.3125
_refine_ls_wR_factor_gt          0.2930
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_restrained_S_all      1.166
_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
N1S N 0.7321(18) 0.7257(15) 0.007(2) 0.097(8) Uani 1 1 d . U . . .
O1S O 0.7870(14) 0.7328(11) -0.1293(11) 0.087(6) Uani 1 1 d . U . . .
C1S C 0.752(2) 0.7072(17) -0.0705(19) 0.087(8) Uani 1 1 d . U . . .
C2S C 0.718(3) 0.6364(16) -0.086(3) 0.112(12) Uani 1 1 d . U . . .
H2S1 H 0.689974 0.620629 -0.033310 0.168 Uiso 1 1 calc R U . . .
H2S2 H 0.670093 0.634846 -0.133634 0.168 Uiso 1 1 calc R U . . .
H2S3 H 0.772846 0.611868 -0.101429 0.168 Uiso 1 1 calc R U . . .
C3S C 0.768(2) 0.7895(12) 0.0245(16) 0.067(6) Uani 1 1 d . U . . .
H3S1 H 0.751623 0.801417 0.083363 0.101 Uiso 1 1 calc R U . . .
H3S2 H 0.837287 0.790583 0.018773 0.101 Uiso 1 1 calc R U . . .
H3S3 H 0.738367 0.817420 -0.017173 0.101 Uiso 1 1 calc R U . . .
C4S C 0.684(3) 0.6965(16) 0.079(2) 0.101(11) Uani 1 1 d . U . . .
H4S1 H 0.682062 0.724374 0.127927 0.152 Uiso 1 1 calc R U . . .
H4S2 H 0.619438 0.685382 0.060637 0.152 Uiso 1 1 calc R U . . .
H4S3 H 0.719592 0.660119 0.096095 0.152 Uiso 1 1 calc R U . . .
N11A N 0.7741(9) 0.2820(7) 0.2668(9) 0.032(3) Uani 1 1 d . . . . .
H11A H 0.808903 0.303484 0.231814 0.039 Uiso 1 1 calc R U . . .
C11A C 0.8022(11) 0.2774(8) 0.3612(10) 0.030(3) Uani 1 1 d . . . . .
H11B H 0.792182 0.234430 0.378786 0.036 Uiso 1 1 calc R U . . .
C13A C 0.9082(11) 0.2911(9) 0.3757(11) 0.035(4) Uani 1 1 d . . . . .
H13A H 0.921433 0.332882 0.356664 0.043 Uiso 1 1 calc R U . . .
H13B H 0.946268 0.263332 0.340232 0.043 Uiso 1 1 calc R U . . .
C14A C 0.9382(11) 0.2840(9) 0.4724(12) 0.037(4) Uani 1 1 d . . . . .
C15A C 0.9344(13) 0.2228(8) 0.5064(11) 0.038(4) Uani 1 1 d . . . . .
H15A H 0.916463 0.189769 0.470469 0.046 Uiso 1 1 calc R U . . .
C16A C 0.9589(14) 0.2144(10) 0.5963(12) 0.048(5) Uani 1 1 d . . . . .
H16A H 0.956867 0.174784 0.619680 0.057 Uiso 1 1 calc R U . . .
C17A C 0.9856(13) 0.2621(11) 0.6508(10) 0.044(5) Uani 1 1 d . U . . .
I17A I 1.01251(11) 0.24873(9) 0.78531(8) 0.0656(5) Uani 1 1 d . . . . .
C18A C 0.9914(13) 0.3230(10) 0.6158(13) 0.044(4) Uani 1 1 d . . . . .
H18A H 1.011309 0.355927 0.651160 0.053 Uiso 1 1 calc R U . . .
C19A C 0.9659(12) 0.3318(9) 0.5259(11) 0.037(4) Uani 1 1 d . . . . .
H19A H 0.968011 0.371314 0.502397 0.044 Uiso 1 1 calc R U . . .
N21A N 0.6724(10) 0.2958(6) 0.4682(9) 0.034(3) Uani 1 1 d . . . . .
C21A C 0.6161(12) 0.3499(9) 0.4950(12) 0.037(4) Uani 1 1 d . . . . .
H21A H 0.608579 0.349255 0.559198 0.044 Uiso 1 1 calc R U . . .
C22A C 0.5192(12) 0.3564(9) 0.4510(13) 0.039(4) Uani 1 1 d . . . . .
O22A O 0.4603(9) 0.3945(7) 0.4720(9) 0.051(4) Uani 1 1 d . . . . .
C23A C 0.6789(12) 0.4060(8) 0.4696(11) 0.034(4) Uani 1 1 d . . . . .
H23A H 0.638513 0.438527 0.443072 0.041 Uiso 1 1 calc R U . . .
O23A O 0.7433(8) 0.3783(5) 0.4027(7) 0.031(2) Uani 1 1 d . . . . .
C24A C 0.7404(15) 0.4309(10) 0.5441(13) 0.048(5) Uani 1 1 d . . . . .
H24A H 0.699492 0.448873 0.587616 0.072 Uiso 1 1 calc R U . . .
H24B H 0.777783 0.398131 0.570432 0.072 Uiso 1 1 calc R U . . .
H24C H 0.783446 0.461785 0.521955 0.072 Uiso 1 1 calc R U . . .
C25A C 0.7360(10) 0.3156(7) 0.4143(10) 0.025(3) Uani 1 1 d . . . . .
N31A N 0.5033(9) 0.3165(7) 0.3793(9) 0.032(3) Uani 1 1 d . . . . .
H31A H 0.539512 0.284490 0.374162 0.039 Uiso 1 1 calc R U . . .
C31A C 0.4272(11) 0.3281(7) 0.3134(12) 0.033(4) Uani 1 1 d . . . . .
H31B H 0.392917 0.365022 0.332847 0.040 Uiso 1 1 calc R U . . .
C33A C 0.3510(12) 0.2768(8) 0.3069(13) 0.037(4) Uani 1 1 d . . . . .
H33A H 0.306666 0.285641 0.256951 0.045 Uiso 1 1 calc R U . . .
C34A C 0.2928(14) 0.2768(11) 0.3918(15) 0.053(5) Uani 1 1 d . U . . .
H34A H 0.244690 0.244886 0.388805 0.080 Uiso 1 1 calc R U . . .
H34B H 0.335852 0.269653 0.441587 0.080 Uiso 1 1 calc R U . . .
H34C H 0.261500 0.316002 0.398415 0.080 Uiso 1 1 calc R U . . .
C35A C 0.3969(13) 0.2129(9) 0.2927(13) 0.041(4) Uani 1 1 d . U . . .
H35A H 0.433220 0.213253 0.239332 0.061 Uiso 1 1 calc R U . . .
H35B H 0.439538 0.203242 0.341857 0.061 Uiso 1 1 calc R U . . .
H35C H 0.346642 0.182353 0.288063 0.061 Uiso 1 1 calc R U . . .
N41A N 0.5599(10) 0.3705(8) 0.2245(9) 0.040(3) Uani 1 1 d . . . . .
C41A C 0.5821(14) 0.3841(11) 0.1364(13) 0.049(5) Uani 1 1 d . . . . .
C42A C 0.6744(13) 0.4186(9) 0.1150(12) 0.042(4) Uani 1 1 d . . . . .
O42A O 0.6924(10) 0.4309(7) 0.0389(9) 0.050(3) Uani 1 1 d . . . . .
C43A C 0.5182(14) 0.3653(11) 0.0769(13) 0.053(5) Uani 1 1 d . . . . .
H43A H 0.523817 0.370979 0.016351 0.063 Uiso 1 1 calc R U . . .
S43A S 0.4230(3) 0.3286(3) 0.1254(3) 0.0476(12) Uani 1 1 d . . . . .
C44A C 0.4774(11) 0.3456(9) 0.2289(10) 0.033(4) Uani 1 1 d . . . . .
N51A N 0.7306(11) 0.4314(7) 0.1851(11) 0.040(3) Uani 1 1 d . . . . .
H51A H 0.713573 0.418989 0.236442 0.048 Uiso 1 1 calc R U . . .
C51A C 0.8223(13) 0.4668(10) 0.1767(13) 0.044(4) Uani 1 1 d . . . . .
H51B H 0.811717 0.497074 0.129390 0.053 Uiso 1 1 calc R U . . .
C53A C 0.8463(15) 0.5027(11) 0.2616(16) 0.055(5) Uani 1 1 d . . . . .
H53A H 0.847696 0.473748 0.311341 0.066 Uiso 1 1 calc R U . . .
C54A C 0.9492(14) 0.5307(11) 0.2524(16) 0.055(5) Uani 1 1 d . U . . .
H54A H 0.995206 0.498243 0.243123 0.082 Uiso 1 1 calc R U . . .
H54B H 0.949254 0.558370 0.202916 0.082 Uiso 1 1 calc R U . . .
H54C H 0.966787 0.552765 0.305289 0.082 Uiso 1 1 calc R U . . .
C55A C 0.7690(17) 0.5484(13) 0.2762(18) 0.067(6) Uani 1 1 d . U . . .
H55A H 0.708221 0.526397 0.282465 0.081 Uiso 1 1 calc R U . . .
H55B H 0.762574 0.573694 0.223559 0.081 Uiso 1 1 calc R U . . .
C56A C 0.782(2) 0.5907(14) 0.3552(18) 0.081(8) Uani 1 1 d . U . . .
H56A H 0.728198 0.618341 0.358104 0.122 Uiso 1 1 calc R U . . .
H56B H 0.786630 0.566623 0.408294 0.122 Uiso 1 1 calc R U . . .
H56C H 0.841161 0.614076 0.349195 0.122 Uiso 1 1 calc R U . . .
N61A N 0.9393(10) 0.4249(8) 0.0706(9) 0.039(3) Uani 1 1 d . . . . .
C61A C 0.9958(12) 0.3689(9) 0.0648(9) 0.034(4) Uani 1 1 d . . . . .
H61A H 1.060400 0.377480 0.041901 0.041 Uiso 1 1 calc R U . . .
C62A C 0.9400(15) 0.3226(11) 0.0039(13) 0.050(5) Uani 1 1 d . . . . .
O62A O 0.9750(10) 0.2692(7) -0.0051(8) 0.049(3) Uani 1 1 d . . . . .
C63A C 1.0038(12) 0.3413(11) 0.1598(12) 0.047(5) Uani 1 1 d . . . . .
O63A O 0.9218(8) 0.3754(6) 0.2010(7) 0.038(3) Uani 1 1 d . . . . .
C64A C 1.0959(13) 0.3624(11) 0.2039(11) 0.046(5) Uani 1 1 d . . . . .
H64A H 1.149824 0.341186 0.178780 0.069 Uiso 1 1 calc R U . . .
H64B H 1.103186 0.405900 0.195354 0.069 Uiso 1 1 calc R U . . .
H64C H 1.093789 0.353559 0.265966 0.069 Uiso 1 1 calc R U . . .
C65A C 0.8997(13) 0.4239(8) 0.1474(13) 0.040(4) Uani 1 1 d . . . . .
N71A N 0.8577(11) 0.3422(9) -0.0336(10) 0.047(4) Uani 1 1 d . . . . .
H71A H 0.844344 0.380909 -0.035419 0.056 Uiso 1 1 calc R U . . .
C71A C 0.7891(15) 0.2966(11) -0.0721(12) 0.049(5) Uani 1 1 d . . . . .
H71B H 0.826257 0.262404 -0.096656 0.059 Uiso 1 1 calc R U . . .
C73A C 0.7277(17) 0.3270(13) -0.1479(13) 0.064(7) Uani 1 1 d . . . . .
H73A H 0.670055 0.346754 -0.123752 0.077 Uiso 1 1 calc R U . . .
C74A C 0.697(2) 0.2761(14) -0.2128(14) 0.069(7) Uani 1 1 d . U . . .
H74A H 0.660552 0.245405 -0.182393 0.104 Uiso 1 1 calc R U . . .
H74B H 0.658090 0.293396 -0.259778 0.104 Uiso 1 1 calc R U . . .
H74C H 0.754129 0.257488 -0.236777 0.104 Uiso 1 1 calc R U . . .
C75A C 0.7859(18) 0.3741(14) -0.2014(15) 0.071(7) Uani 1 1 d . U . . .
H75A H 0.806743 0.407164 -0.163455 0.107 Uiso 1 1 calc R U . . .
H75B H 0.841584 0.354218 -0.225583 0.107 Uiso 1 1 calc R U . . .
H75C H 0.745545 0.390126 -0.248584 0.107 Uiso 1 1 calc R U . . .
N81A N 0.7488(11) 0.2833(8) 0.0837(10) 0.044(4) Uani 1 1 d . . . . .
C81A C 0.6838(12) 0.2502(10) 0.1393(11) 0.041(4) Uani 1 1 d . . . . .
C82A C 0.6952(11) 0.2532(9) 0.2352(10) 0.033(3) Uani 1 1 d . . . . .
O82A O 0.6374(8) 0.2265(6) 0.2833(8) 0.038(3) Uani 1 1 d . . . . .
C83A C 0.6150(14) 0.2183(11) 0.0980(14) 0.050(5) Uani 1 1 d . . . . .
H83A H 0.567162 0.195445 0.125359 0.060 Uiso 1 1 calc R U . . .
S83A S 0.6276(4) 0.2256(3) -0.0161(3) 0.0535(13) Uani 1 1 d . . . . .
C84A C 0.7278(13) 0.2724(10) 0.0023(11) 0.047(5) Uani 1 1 d . . . . .
N11B N 0.2720(9) 0.5906(7) 0.7226(8) 0.032(3) Uani 1 1 d . . . . .
H11C H 0.307139 0.567377 0.756518 0.038 Uiso 1 1 calc R U . . .
C11B C 0.2975(12) 0.5985(7) 0.6302(9) 0.028(3) Uani 1 1 d . . . . .
H11D H 0.286135 0.641862 0.615091 0.033 Uiso 1 1 calc R U . . .
C13B C 0.4055(11) 0.5858(8) 0.6186(9) 0.029(3) Uani 1 1 d . . . . .
H13C H 0.443221 0.613345 0.656361 0.034 Uiso 1 1 calc R U . . .
H13D H 0.419878 0.543877 0.636847 0.034 Uiso 1 1 calc R U . . .
C14B C 0.4348(10) 0.5944(8) 0.5245(10) 0.029(3) Uani 1 1 d . . . . .
C15B C 0.4642(11) 0.5463(8) 0.4726(10) 0.032(3) Uani 1 1 d . . . . .
H15B H 0.468992 0.507204 0.497452 0.038 Uiso 1 1 calc R U . . .
C16B C 0.4867(14) 0.5539(10) 0.3854(12) 0.045(5) Uani 1 1 d . . . . .
H16B H 0.505324 0.520082 0.352048 0.054 Uiso 1 1 calc R U . . .
C17B C 0.4817(12) 0.6109(12) 0.3476(12) 0.048(5) Uani 1 1 d . U . . .
I17B I 0.50957(10) 0.62144(8) 0.21233(8) 0.0635(5) Uani 1 1 d . . . . .
C18B C 0.4527(13) 0.6604(9) 0.3962(12) 0.040(4) Uani 1 1 d . . . . .
H18B H 0.448066 0.699119 0.370028 0.048 Uiso 1 1 calc R U . . .
C19B C 0.4303(13) 0.6531(8) 0.4837(11) 0.037(4) Uani 1 1 d . . . . .
H19B H 0.411998 0.687183 0.516565 0.044 Uiso 1 1 calc R U . . .
N21B N 0.1691(10) 0.5824(6) 0.5178(9) 0.032(3) Uani 1 1 d . . . . .
C21B C 0.1148(12) 0.5292(9) 0.4855(11) 0.035(4) Uani 1 1 d . . . . .
H21B H 0.106732 0.532188 0.421150 0.042 Uiso 1 1 calc R U . . .
C22B C 0.0165(12) 0.5255(9) 0.5259(13) 0.041(4) Uani 1 1 d . . . . .
O22B O -0.0425(9) 0.4846(7) 0.4961(8) 0.046(3) Uani 1 1 d . . . . .
C23B C 0.1779(11) 0.4754(9) 0.5077(11) 0.034(4) Uani 1 1 d . . . . .
H23B H 0.138027 0.441606 0.529678 0.041 Uiso 1 1 calc R U . . .
O23B O 0.2419(8) 0.4986(5) 0.5797(7) 0.033(2) Uani 1 1 d . . . . .
C24B C 0.2395(14) 0.4523(11) 0.4317(14) 0.055(6) Uani 1 1 d . . . . .
H24D H 0.197739 0.437198 0.384919 0.083 Uiso 1 1 calc R U . . .
H24E H 0.278414 0.485441 0.410095 0.083 Uiso 1 1 calc R U . . .
H24F H 0.281103 0.419586 0.452531 0.083 Uiso 1 1 calc R U . . .
C25B C 0.2322(11) 0.5606(7) 0.5711(11) 0.029(3) Uani 1 1 d . . . . .
N31B N 0.0004(9) 0.5597(7) 0.5969(9) 0.031(3) Uani 1 1 d . . . . .
H31C H 0.034988 0.592224 0.605485 0.038 Uiso 1 1 calc R U . . .
C31B C -0.0746(12) 0.5442(9) 0.6617(13) 0.039(4) Uani 1 1 d . . . . .
H31D H -0.111986 0.509806 0.636490 0.047 Uiso 1 1 calc R U . . .
C33B C -0.1476(11) 0.5976(8) 0.6752(10) 0.033(4) Uani 1 1 d . . . . .
H33B H -0.191343 0.584848 0.721883 0.040 Uiso 1 1 calc R U . . .
C34B C -0.1021(14) 0.6562(9) 0.7039(12) 0.040(4) Uani 1 1 d . U . . .
H34D H -0.064276 0.649406 0.757136 0.061 Uiso 1 1 calc R U . . .
H34E H -0.060645 0.671068 0.658487 0.061 Uiso 1 1 calc R U . . .
H34F H -0.151691 0.686087 0.714870 0.061 Uiso 1 1 calc R U . . .
C35B C -0.2098(14) 0.6047(11) 0.5897(15) 0.056(6) Uani 1 1 d . U . . .
H35D H -0.237739 0.565663 0.573748 0.084 Uiso 1 1 calc R U . . .
H35E H -0.260778 0.634010 0.599230 0.084 Uiso 1 1 calc R U . . .
H35F H -0.169733 0.618992 0.542846 0.084 Uiso 1 1 calc R U . . .
N41B N 0.0592(10) 0.4952(7) 0.7459(10) 0.035(3) Uani 1 1 d . . . . .
C41B C 0.0835(14) 0.4779(10) 0.8306(14) 0.050(5) Uani 1 1 d . . . . .
C42B C 0.1768(14) 0.4448(10) 0.8491(16) 0.052(5) Uani 1 1 d . . . . .
O42B O 0.1996(11) 0.4292(8) 0.9245(11) 0.061(4) Uani 1 1 d . . . . .
C43B C 0.0186(15) 0.4899(10) 0.8926(13) 0.047(5) Uani 1 1 d . . . . .
H43B H 0.025268 0.478884 0.951766 0.057 Uiso 1 1 calc R U . . .
S43B S -0.0790(3) 0.5286(3) 0.8469(3) 0.0503(12) Uani 1 1 d . . . . .
C44B C -0.0245(12) 0.5202(10) 0.7441(13) 0.043(4) Uani 1 1 d . . . . .
N51B N 0.2329(11) 0.4370(7) 0.7801(11) 0.042(4) Uani 1 1 d . . . . .
H51C H 0.215113 0.452524 0.730009 0.051 Uiso 1 1 calc R U . . .
C51B C 0.3253(13) 0.4024(12) 0.7866(15) 0.056(5) Uani 1 1 d . . . . .
H51D H 0.315706 0.366783 0.825281 0.067 Uiso 1 1 calc R U . . .
C53B C 0.3546(16) 0.3775(11) 0.6914(16) 0.058(6) Uani 1 1 d . . . . .
H53B H 0.365019 0.414001 0.654667 0.070 Uiso 1 1 calc R U . . .
C54B C 0.4552(17) 0.3450(14) 0.702(2) 0.074(8) Uani 1 1 d . U . . .
H54D H 0.499407 0.371322 0.734063 0.112 Uiso 1 1 calc R U . . .
H54E H 0.447647 0.307017 0.733467 0.112 Uiso 1 1 calc R U . . .
H54F H 0.480432 0.336594 0.644529 0.112 Uiso 1 1 calc R U . . .
C55B C 0.2828(19) 0.3374(15) 0.641(2) 0.079(8) Uani 1 1 d . U . . .
H55C H 0.304744 0.331758 0.581002 0.095 Uiso 1 1 calc R U . . .
H55D H 0.220203 0.357856 0.637757 0.095 Uiso 1 1 calc R U . . .
C56B C 0.271(2) 0.2722(16) 0.686(3) 0.097(10) Uani 1 1 d . U . . .
H56D H 0.225092 0.247971 0.652718 0.146 Uiso 1 1 calc R U . . .
H56E H 0.332652 0.251586 0.688529 0.146 Uiso 1 1 calc R U . . .
H56F H 0.248188 0.277660 0.745233 0.146 Uiso 1 1 calc R U . . .
N61B N 0.4413(11) 0.4356(8) 0.9042(10) 0.045(4) Uani 1 1 d . . . . .
C61B C 0.4984(13) 0.4924(11) 0.9209(12) 0.045(5) Uani 1 1 d . . . . .
H61B H 0.562942 0.482114 0.945325 0.054 Uiso 1 1 calc R U . . .
C62B C 0.4470(14) 0.5366(14) 0.9816(12) 0.057(6) Uani 1 1 d . . . . .
O62B O 0.4810(11) 0.5897(8) 1.0001(9) 0.055(4) Uani 1 1 d . . . . .
C63B C 0.5069(13) 0.5217(10) 0.8304(10) 0.040(4) Uani 1 1 d . . . . .
H63B H 0.497220 0.566339 0.834856 0.048 Uiso 1 1 calc R U . . .
O63B O 0.4245(9) 0.4937(6) 0.7814(8) 0.040(3) Uani 1 1 d . . . . .
C64B C 0.6015(14) 0.5084(12) 0.7842(14) 0.053(5) Uani 1 1 d . . . . .
H64D H 0.654517 0.526879 0.816778 0.079 Uiso 1 1 calc R U . . .
H64E H 0.611247 0.464650 0.781104 0.079 Uiso 1 1 calc R U . . .
H64F H 0.598424 0.525140 0.725512 0.079 Uiso 1 1 calc R U . . .
C65B C 0.4010(13) 0.4418(9) 0.8274(11) 0.038(4) Uani 1 1 d . . . . .
N71B N 0.3615(12) 0.5165(9) 1.0136(10) 0.048(4) Uani 1 1 d . . . . .
H71C H 0.346477 0.478225 1.007885 0.058 Uiso 1 1 calc R U . . .
C71B C 0.2944(14) 0.5574(10) 1.0572(12) 0.045(4) Uani 1 1 d . . . . .
H71D H 0.333723 0.590690 1.083228 0.053 Uiso 1 1 calc R U . . .
C73B C 0.2385(16) 0.5277(11) 1.1340(12) 0.052(5) Uani 1 1 d . . . . .
H73B H 0.181574 0.506772 1.108240 0.063 Uiso 1 1 calc R U . . .
C74B C 0.300(2) 0.4797(14) 1.1804(16) 0.077(8) Uani 1 1 d . U . . .
H74D H 0.321334 0.449739 1.138294 0.116 Uiso 1 1 calc R U . . .
H74E H 0.356180 0.499129 1.207594 0.116 Uiso 1 1 calc R U . . .
H74F H 0.263169 0.459731 1.224914 0.116 Uiso 1 1 calc R U . . .
C75B C 0.203(2) 0.5761(15) 1.1947(15) 0.078(8) Uani 1 1 d . U . . .
H75D H 0.164300 0.605262 1.161892 0.117 Uiso 1 1 calc R U . . .
H75E H 0.164492 0.557374 1.239393 0.117 Uiso 1 1 calc R U . . .
H75F H 0.257503 0.596773 1.222072 0.117 Uiso 1 1 calc R U . . .
N81B N 0.2500(11) 0.5826(7) 0.9030(9) 0.038(3) Uani 1 1 d . . . . .
C81B C 0.1826(12) 0.6169(8) 0.8515(10) 0.034(3) Uani 1 1 d . . . . .
C82B C 0.1933(10) 0.6196(7) 0.7553(9) 0.027(3) Uani 1 1 d . . . . .
O82B O 0.1332(8) 0.6474(6) 0.7069(8) 0.036(3) Uani 1 1 d . . . . .
C83B C 0.1144(13) 0.6455(9) 0.8973(12) 0.041(4) Uani 1 1 d . . . . .
H83B H 0.065145 0.669492 0.872019 0.049 Uiso 1 1 calc R U . . .
S83B S 0.1288(3) 0.6329(3) 1.0074(3) 0.0514(13) Uani 1 1 d . . . . .
C84B C 0.2306(13) 0.5866(10) 0.9860(11) 0.043(4) Uani 1 1 d . . . . .


_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
N1S C1S 1.27(4) . ?
N1S C4S 1.44(4) . ?
N1S C3S 1.49(4) . ?
O1S C1S 1.17(3) . ?
C1S C2S 1.62(5) . ?
C2S H2S1 0.9600 . ?
C2S H2S2 0.9600 . ?
C2S H2S3 0.9600 . ?
C3S H3S1 0.9600 . ?
C3S H3S2 0.9600 . ?
C3S H3S3 0.9600 . ?
C4S H4S1 0.9600 . ?
C4S H4S2 0.9600 . ?
C4S H4S3 0.9600 . ?
N11A C82A 1.33(2) . ?
N11A C11A 1.48(2) . ?
N11A H11A 0.8600 . ?
C11A C25A 1.48(2) . ?
C11A C13A 1.50(2) . ?
C11A H11B 0.9800 . ?
C13A C14A 1.52(2) . ?
C13A H13A 0.9700 . ?
C13A H13B 0.9700 . ?
C14A C19A 1.36(3) . ?
C14A C15A 1.43(3) . ?
C15A C16A 1.41(2) . ?
C15A H15A 0.9300 . ?
C16A C17A 1.37(3) . ?
C16A H16A 0.9300 . ?
C17A C18A 1.43(3) . ?
C17A I17A 2.081(16) . ?
C18A C19A 1.41(3) . ?
C18A H18A 0.9300 . ?
C19A H19A 0.9300 . ?
N21A C25A 1.28(2) . ?
N21A C21A 1.47(2) . ?
C21A C22A 1.49(2) . ?
C21A C23A 1.55(3) . ?
C21A H21A 0.9800 . ?
C22A O22A 1.21(2) . ?
C22A N31A 1.40(2) . ?
C23A O23A 1.488(19) . ?
C23A C24A 1.50(2) . ?
C23A H23A 0.9800 . ?
O23A C25A 1.38(2) . ?
C24A H24A 0.9600 . ?
C24A H24B 0.9600 . ?
C24A H24C 0.9600 . ?
N31A C31A 1.45(2) . ?
N31A H31A 0.8600 . ?
C31A C44A 1.52(2) . ?
C31A C33A 1.53(2) . ?
C31A H31B 0.9800 . ?
C33A C34A 1.53(3) . ?
C33A C35A 1.54(3) . ?
C33A H33A 0.9800 . ?
C34A H34A 0.9600 . ?
C34A H34B 0.9600 . ?
C34A H34C 0.9600 . ?
C35A H35A 0.9600 . ?
C35A H35B 0.9600 . ?
C35A H35C 0.9600 . ?
N41A C44A 1.26(2) . ?
N41A C41A 1.41(2) . ?
C41A C43A 1.31(3) . ?
C41A C42A 1.52(3) . ?
C42A O42A 1.21(2) . ?
C42A N51A 1.33(2) . ?
C43A S43A 1.71(2) . ?
C43A H43A 0.9300 . ?
S43A C44A 1.761(16) . ?
N51A C51A 1.49(2) . ?
N51A H51A 0.8600 . ?
C51A C65A 1.49(3) . ?
C51A C53A 1.53(3) . ?
C51A H51B 0.9800 . ?
C53A C55A 1.48(3) . ?
C53A C54A 1.55(3) . ?
C53A H53A 0.9800 . ?
C54A H54A 0.9600 . ?
C54A H54B 0.9600 . ?
C54A H54C 0.9600 . ?
C55A C56A 1.52(3) . ?
C55A H55A 0.9700 . ?
C55A H55B 0.9700 . ?
C56A H56A 0.9600 . ?
C56A H56B 0.9600 . ?
C56A H56C 0.9600 . ?
N61A C65A 1.30(2) . ?
N61A C61A 1.45(2) . ?
C61A C62A 1.55(3) . ?
C61A C63A 1.56(2) . ?
C61A H61A 0.9800 . ?
C62A O62A 1.26(3) . ?
C62A N71A 1.33(3) . ?
C63A C64A 1.49(3) . ?
C63A O63A 1.50(2) . ?
O63A C65A 1.36(2) . ?
C64A H64A 0.9600 . ?
C64A H64B 0.9600 . ?
C64A H64C 0.9600 . ?
N71A C71A 1.48(3) . ?
N71A H71A 0.8600 . ?
C71A C84A 1.52(3) . ?
C71A C73A 1.56(3) . ?
C71A H71B 0.9800 . ?
C73A C74A 1.53(3) . ?
C73A C75A 1.54(4) . ?
C73A H73A 0.9800 . ?
C74A H74A 0.9600 . ?
C74A H74B 0.9600 . ?
C74A H74C 0.9600 . ?
C75A H75A 0.9600 . ?
C75A H75B 0.9600 . ?
C75A H75C 0.9600 . ?
N81A C84A 1.28(2) . ?
N81A C81A 1.44(2) . ?
C81A C83A 1.32(3) . ?
C81A C82A 1.46(2) . ?
C82A O82A 1.24(2) . ?
C83A S83A 1.75(2) . ?
C83A H83A 0.9300 . ?
S83A C84A 1.73(2) . ?
N11B C82B 1.36(2) . ?
N11B C11B 1.460(18) . ?
N11B H11C 0.8600 . ?
C11B C25B 1.50(2) . ?
C11B C13B 1.53(2) . ?
C11B H11D 0.9800 . ?
C13B C14B 1.50(2) . ?
C13B H13C 0.9700 . ?
C13B H13D 0.9700 . ?
C14B C15B 1.37(2) . ?
C14B C19B 1.42(2) . ?
C15B C16B 1.37(2) . ?
C15B H15B 0.9300 . ?
C16B C17B 1.37(3) . ?
C16B H16B 0.9300 . ?
C17B C18B 1.37(3) . ?
C17B I17B 2.104(18) . ?
C18B C19B 1.38(2) . ?
C18B H18B 0.9300 . ?
C19B H19B 0.9300 . ?
N21B C25B 1.26(2) . ?
N21B C21B 1.45(2) . ?
C21B C23B 1.49(3) . ?
C21B C22B 1.50(2) . ?
C21B H21B 0.9800 . ?
C22B O22B 1.28(2) . ?
C22B N31B 1.33(2) . ?
C23B O23B 1.474(19) . ?
C23B C24B 1.53(2) . ?
C23B H23B 0.9800 . ?
O23B C25B 1.36(2) . ?
C24B H24D 0.9600 . ?
C24B H24E 0.9600 . ?
C24B H24F 0.9600 . ?
N31B C31B 1.48(2) . ?
N31B H31C 0.8600 . ?
C31B C44B 1.50(3) . ?
C31B C33B 1.55(2) . ?
C31B H31D 0.9800 . ?
C33B C34B 1.48(2) . ?
C33B C35B 1.54(3) . ?
C33B H33B 0.9800 . ?
C34B H34D 0.9600 . ?
C34B H34E 0.9600 . ?
C34B H34F 0.9600 . ?
C35B H35D 0.9600 . ?
C35B H35E 0.9600 . ?
C35B H35F 0.9600 . ?
N41B C44B 1.27(2) . ?
N41B C41B 1.37(2) . ?
C41B C43B 1.34(3) . ?
C41B C42B 1.49(3) . ?
C42B O42B 1.22(3) . ?
C42B N51B 1.33(3) . ?
C43B S43B 1.72(2) . ?
C43B H43B 0.9300 . ?
S43B C44B 1.754(19) . ?
N51B C51B 1.48(2) . ?
N51B H51C 0.8600 . ?
C51B C65B 1.47(3) . ?
C51B C53B 1.60(3) . ?
C51B H51D 0.9800 . ?
C53B C55B 1.51(4) . ?
C53B C54B 1.56(3) . ?
C53B H53B 0.9800 . ?
C54B H54D 0.9600 . ?
C54B H54E 0.9600 . ?
C54B H54F 0.9600 . ?
C55B C56B 1.58(5) . ?
C55B H55C 0.9700 . ?
C55B H55D 0.9700 . ?
C56B H56D 0.9600 . ?
C56B H56E 0.9600 . ?
C56B H56F 0.9600 . ?
N61B C65B 1.28(2) . ?
N61B C61B 1.48(3) . ?
C61B C62B 1.52(3) . ?
C61B C63B 1.52(3) . ?
C61B H61B 0.9800 . ?
C62B O62B 1.27(3) . ?
C62B N71B 1.36(3) . ?
C63B O63B 1.47(2) . ?
C63B C64B 1.52(3) . ?
C63B H63B 0.9800 . ?
O63B C65B 1.37(2) . ?
C64B H64D 0.9600 . ?
C64B H64E 0.9600 . ?
C64B H64F 0.9600 . ?
N71B C71B 1.45(3) . ?
N71B H71C 0.8600 . ?
C71B C84B 1.51(3) . ?
C71B C73B 1.55(3) . ?
C71B H71D 0.9800 . ?
C73B C75B 1.49(4) . ?
C73B C74B 1.51(3) . ?
C73B H73B 0.9800 . ?
C74B H74D 0.9600 . ?
C74B H74E 0.9600 . ?
C74B H74F 0.9600 . ?
C75B H75D 0.9600 . ?
C75B H75E 0.9600 . ?
C75B H75F 0.9600 . ?
N81B C84B 1.29(2) . ?
N81B C81B 1.41(2) . ?
C81B C83B 1.34(3) . ?
C81B C82B 1.47(2) . ?
C82B O82B 1.248(19) . ?
C83B S83B 1.696(18) . ?
C83B H83B 0.9300 . ?
S83B C84B 1.76(2) . ?

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
C1S N1S C4S 132(3) . . ?
C1S N1S C3S 112(3) . . ?
C4S N1S C3S 115(3) . . ?
O1S C1S N1S 131(4) . . ?
O1S C1S C2S 118(3) . . ?
N1S C1S C2S 112(3) . . ?
C1S C2S H2S1 109.5 . . ?
C1S C2S H2S2 109.5 . . ?
H2S1 C2S H2S2 109.5 . . ?
C1S C2S H2S3 109.5 . . ?
H2S1 C2S H2S3 109.5 . . ?
H2S2 C2S H2S3 109.5 . . ?
N1S C3S H3S1 109.5 . . ?
N1S C3S H3S2 109.5 . . ?
H3S1 C3S H3S2 109.5 . . ?
N1S C3S H3S3 109.5 . . ?
H3S1 C3S H3S3 109.5 . . ?
H3S2 C3S H3S3 109.5 . . ?
N1S C4S H4S1 109.5 . . ?
N1S C4S H4S2 109.5 . . ?
H4S1 C4S H4S2 109.5 . . ?
N1S C4S H4S3 109.5 . . ?
H4S1 C4S H4S3 109.5 . . ?
H4S2 C4S H4S3 109.5 . . ?
C82A N11A C11A 120.6(14) . . ?
C82A N11A H11A 119.7 . . ?
C11A N11A H11A 119.7 . . ?
N11A C11A C25A 109.7(13) . . ?
N11A C11A C13A 111.1(12) . . ?
C25A C11A C13A 114.7(14) . . ?
N11A C11A H11B 107.0 . . ?
C25A C11A H11B 107.0 . . ?
C13A C11A H11B 107.0 . . ?
C11A C13A C14A 111.3(13) . . ?
C11A C13A H13A 109.4 . . ?
C14A C13A H13A 109.4 . . ?
C11A C13A H13B 109.4 . . ?
C14A C13A H13B 109.4 . . ?
H13A C13A H13B 108.0 . . ?
C19A C14A C15A 120.4(16) . . ?
C19A C14A C13A 124.1(17) . . ?
C15A C14A C13A 115.4(16) . . ?
C16A C15A C14A 117.4(17) . . ?
C16A C15A H15A 121.3 . . ?
C14A C15A H15A 121.3 . . ?
C17A C16A C15A 123(2) . . ?
C17A C16A H16A 118.7 . . ?
C15A C16A H16A 118.7 . . ?
C16A C17A C18A 119.6(16) . . ?
C16A C17A I17A 121.5(17) . . ?
C18A C17A I17A 118.9(13) . . ?
C19A C18A C17A 117.9(17) . . ?
C19A C18A H18A 121.0 . . ?
C17A C18A H18A 121.0 . . ?
C14A C19A C18A 122.0(18) . . ?
C14A C19A H19A 119.0 . . ?
C18A C19A H19A 119.0 . . ?
C25A N21A C21A 106.2(14) . . ?
N21A C21A C22A 115.2(15) . . ?
N21A C21A C23A 105.0(13) . . ?
C22A C21A C23A 108.4(15) . . ?
N21A C21A H21A 109.3 . . ?
C22A C21A H21A 109.3 . . ?
C23A C21A H21A 109.3 . . ?
O22A C22A N31A 122.3(16) . . ?
O22A C22A C21A 123.3(18) . . ?
N31A C22A C21A 114.2(15) . . ?
O23A C23A C24A 108.8(13) . . ?
O23A C23A C21A 101.4(12) . . ?
C24A C23A C21A 114.1(15) . . ?
O23A C23A H23A 110.7 . . ?
C24A C23A H23A 110.7 . . ?
C21A C23A H23A 110.7 . . ?
C25A O23A C23A 105.4(12) . . ?
C23A C24A H24A 109.5 . . ?
C23A C24A H24B 109.5 . . ?
H24A C24A H24B 109.5 . . ?
C23A C24A H24C 109.5 . . ?
H24A C24A H24C 109.5 . . ?
H24B C24A H24C 109.5 . . ?
N21A C25A O23A 117.7(13) . . ?
N21A C25A C11A 126.4(15) . . ?
O23A C25A C11A 115.9(13) . . ?
C22A N31A C31A 121.5(14) . . ?
C22A N31A H31A 119.3 . . ?
C31A N31A H31A 119.3 . . ?
N31A C31A C44A 106.6(12) . . ?
N31A C31A C33A 113.7(14) . . ?
C44A C31A C33A 117.0(15) . . ?
N31A C31A H31B 106.3 . . ?
C44A C31A H31B 106.3 . . ?
C33A C31A H31B 106.3 . . ?
C34A C33A C31A 108.5(16) . . ?
C34A C33A C35A 110.1(16) . . ?
C31A C33A C35A 112.3(13) . . ?
C34A C33A H33A 108.6 . . ?
C31A C33A H33A 108.6 . . ?
C35A C33A H33A 108.6 . . ?
C33A C34A H34A 109.5 . . ?
C33A C34A H34B 109.5 . . ?
H34A C34A H34B 109.5 . . ?
C33A C34A H34C 109.5 . . ?
H34A C34A H34C 109.5 . . ?
H34B C34A H34C 109.5 . . ?
C33A C35A H35A 109.5 . . ?
C33A C35A H35B 109.5 . . ?
H35A C35A H35B 109.5 . . ?
C33A C35A H35C 109.5 . . ?
H35A C35A H35C 109.5 . . ?
H35B C35A H35C 109.5 . . ?
C44A N41A C41A 110.9(15) . . ?
C43A C41A N41A 115.4(18) . . ?
C43A C41A C42A 124.1(18) . . ?
N41A C41A C42A 120.5(16) . . ?
O42A C42A N51A 125.7(18) . . ?
O42A C42A C41A 120.1(17) . . ?
N51A C42A C41A 114.1(16) . . ?
C41A C43A S43A 111.0(16) . . ?
C41A C43A H43A 124.5 . . ?
S43A C43A H43A 124.5 . . ?
C43A S43A C44A 88.3(9) . . ?
N41A C44A C31A 125.6(14) . . ?
N41A C44A S43A 114.0(13) . . ?
C31A C44A S43A 120.3(12) . . ?
C42A N51A C51A 121.3(16) . . ?
C42A N51A H51A 119.4 . . ?
C51A N51A H51A 119.4 . . ?
N51A C51A C65A 108.5(17) . . ?
N51A C51A C53A 110.9(15) . . ?
C65A C51A C53A 115.2(16) . . ?
N51A C51A H51B 107.3 . . ?
C65A C51A H51B 107.3 . . ?
C53A C51A H51B 107.3 . . ?
C55A C53A C51A 109.0(19) . . ?
C55A C53A C54A 114(2) . . ?
C51A C53A C54A 107.6(17) . . ?
C55A C53A H53A 108.6 . . ?
C51A C53A H53A 108.6 . . ?
C54A C53A H53A 108.6 . . ?
C53A C54A H54A 109.5 . . ?
C53A C54A H54B 109.5 . . ?
H54A C54A H54B 109.5 . . ?
C53A C54A H54C 109.5 . . ?
H54A C54A H54C 109.5 . . ?
H54B C54A H54C 109.5 . . ?
C53A C55A C56A 117(2) . . ?
C53A C55A H55A 108.1 . . ?
C56A C55A H55A 108.1 . . ?
C53A C55A H55B 108.1 . . ?
C56A C55A H55B 108.1 . . ?
H55A C55A H55B 107.3 . . ?
C55A C56A H56A 109.5 . . ?
C55A C56A H56B 109.5 . . ?
H56A C56A H56B 109.5 . . ?
C55A C56A H56C 109.5 . . ?
H56A C56A H56C 109.5 . . ?
H56B C56A H56C 109.5 . . ?
C65A N61A C61A 106.1(14) . . ?
N61A C61A C62A 108.6(14) . . ?
N61A C61A C63A 107.1(13) . . ?
C62A C61A C63A 108.8(16) . . ?
N61A C61A H61A 110.7 . . ?
C62A C61A H61A 110.7 . . ?
C63A C61A H61A 110.7 . . ?
O62A C62A N71A 124.9(19) . . ?
O62A C62A C61A 118.1(17) . . ?
N71A C62A C61A 116.9(19) . . ?
C64A C63A O63A 107.6(17) . . ?
C64A C63A C61A 109.6(16) . . ?
O63A C63A C61A 99.0(13) . . ?
C65A O63A C63A 107.2(13) . . ?
C63A C64A H64A 109.5 . . ?
C63A C64A H64B 109.5 . . ?
H64A C64A H64B 109.5 . . ?
C63A C64A H64C 109.5 . . ?
H64A C64A H64C 109.5 . . ?
H64B C64A H64C 109.5 . . ?
N61A C65A O63A 117.1(16) . . ?
N61A C65A C51A 125.1(16) . . ?
O63A C65A C51A 117.3(16) . . ?
C62A N71A C71A 119.1(19) . . ?
C62A N71A H71A 120.5 . . ?
C71A N71A H71A 120.5 . . ?
N71A C71A C84A 107.5(15) . . ?
N71A C71A C73A 109.7(18) . . ?
C84A C71A C73A 113.1(17) . . ?
N71A C71A H71B 108.8 . . ?
C84A C71A H71B 108.8 . . ?
C73A C71A H71B 108.8 . . ?
C74A C73A C75A 106(2) . . ?
C74A C73A C71A 108(2) . . ?
C75A C73A C71A 112.9(18) . . ?
C74A C73A H73A 110.0 . . ?
C75A C73A H73A 110.0 . . ?
C71A C73A H73A 110.0 . . ?
C73A C74A H74A 109.5 . . ?
C73A C74A H74B 109.5 . . ?
H74A C74A H74B 109.5 . . ?
C73A C74A H74C 109.5 . . ?
H74A C74A H74C 109.5 . . ?
H74B C74A H74C 109.5 . . ?
C73A C75A H75A 109.5 . . ?
C73A C75A H75B 109.5 . . ?
H75A C75A H75B 109.5 . . ?
C73A C75A H75C 109.5 . . ?
H75A C75A H75C 109.5 . . ?
H75B C75A H75C 109.5 . . ?
C84A N81A C81A 109.9(16) . . ?
C83A C81A N81A 115.9(16) . . ?
C83A C81A C82A 123.7(18) . . ?
N81A C81A C82A 120.4(15) . . ?
O82A C82A N11A 122.6(15) . . ?
O82A C82A C81A 120.7(15) . . ?
N11A C82A C81A 116.5(15) . . ?
C81A C83A S83A 109.5(16) . . ?
C81A C83A H83A 125.3 . . ?
S83A C83A H83A 125.3 . . ?
C84A S83A C83A 89.5(9) . . ?
N81A C84A C71A 122.1(18) . . ?
N81A C84A S83A 115.2(15) . . ?
C71A C84A S83A 122.7(13) . . ?
C82B N11B C11B 120.4(13) . . ?
C82B N11B H11C 119.8 . . ?
C11B N11B H11C 119.8 . . ?
N11B C11B C25B 110.7(13) . . ?
N11B C11B C13B 110.2(11) . . ?
C25B C11B C13B 113.8(13) . . ?
N11B C11B H11D 107.3 . . ?
C25B C11B H11D 107.3 . . ?
C13B C11B H11D 107.3 . . ?
C14B C13B C11B 111.7(11) . . ?
C14B C13B H13C 109.3 . . ?
C11B C13B H13C 109.3 . . ?
C14B C13B H13D 109.3 . . ?
C11B C13B H13D 109.3 . . ?
H13C C13B H13D 107.9 . . ?
C15B C14B C19B 116.4(14) . . ?
C15B C14B C13B 122.5(15) . . ?
C19B C14B C13B 121.1(15) . . ?
C16B C15B C14B 122.3(17) . . ?
C16B C15B H15B 118.8 . . ?
C14B C15B H15B 118.8 . . ?
C17B C16B C15B 120.1(18) . . ?
C17B C16B H16B 119.9 . . ?
C15B C16B H16B 119.9 . . ?
C16B C17B C18B 120.0(17) . . ?
C16B C17B I17B 119.9(16) . . ?
C18B C17B I17B 120.0(15) . . ?
C17B C18B C19B 120.1(17) . . ?
C17B C18B H18B 119.9 . . ?
C19B C18B H18B 119.9 . . ?
C18B C19B C14B 121.0(16) . . ?
C18B C19B H19B 119.5 . . ?
C14B C19B H19B 119.5 . . ?
C25B N21B C21B 105.0(14) . . ?
N21B C21B C23B 104.7(13) . . ?
N21B C21B C22B 111.6(14) . . ?
C23B C21B C22B 113.2(16) . . ?
N21B C21B H21B 109.1 . . ?
C23B C21B H21B 109.1 . . ?
C22B C21B H21B 109.1 . . ?
O22B C22B N31B 123.8(16) . . ?
O22B C22B C21B 117.7(15) . . ?
N31B C22B C21B 118.0(15) . . ?
O23B C23B C21B 103.6(13) . . ?
O23B C23B C24B 109.6(13) . . ?
C21B C23B C24B 114.8(17) . . ?
O23B C23B H23B 109.5 . . ?
C21B C23B H23B 109.5 . . ?
C24B C23B H23B 109.5 . . ?
C25B O23B C23B 102.2(13) . . ?
C23B C24B H24D 109.5 . . ?
C23B C24B H24E 109.5 . . ?
H24D C24B H24E 109.5 . . ?
C23B C24B H24F 109.5 . . ?
H24D C24B H24F 109.5 . . ?
H24E C24B H24F 109.5 . . ?
N21B C25B O23B 119.8(14) . . ?
N21B C25B C11B 124.7(15) . . ?
O23B C25B C11B 115.5(14) . . ?
C22B N31B C31B 122.8(15) . . ?
C22B N31B H31C 118.6 . . ?
C31B N31B H31C 118.6 . . ?
N31B C31B C44B 108.4(13) . . ?
N31B C31B C33B 112.5(15) . . ?
C44B C31B C33B 115.8(15) . . ?
N31B C31B H31D 106.5 . . ?
C44B C31B H31D 106.5 . . ?
C33B C31B H31D 106.5 . . ?
C34B C33B C35B 112.6(16) . . ?
C34B C33B C31B 114.2(14) . . ?
C35B C33B C31B 108.3(14) . . ?
C34B C33B H33B 107.1 . . ?
C35B C33B H33B 107.1 . . ?
C31B C33B H33B 107.1 . . ?
C33B C34B H34D 109.5 . . ?
C33B C34B H34E 109.5 . . ?
H34D C34B H34E 109.5 . . ?
C33B C34B H34F 109.5 . . ?
H34D C34B H34F 109.5 . . ?
H34E C34B H34F 109.5 . . ?
C33B C35B H35D 109.5 . . ?
C33B C35B H35E 109.5 . . ?
H35D C35B H35E 109.5 . . ?
C33B C35B H35F 109.5 . . ?
H35D C35B H35F 109.5 . . ?
H35E C35B H35F 109.5 . . ?
C44B N41B C41B 109.8(15) . . ?
C43B C41B N41B 116.8(17) . . ?
C43B C41B C42B 123.2(18) . . ?
N41B C41B C42B 119.9(18) . . ?
O42B C42B N51B 123.9(18) . . ?
O42B C42B C41B 120.7(19) . . ?
N51B C42B C41B 115.3(19) . . ?
C41B C43B S43B 110.0(14) . . ?
C41B C43B H43B 125.0 . . ?
S43B C43B H43B 125.0 . . ?
C43B S43B C44B 87.7(9) . . ?
N41B C44B C31B 124.3(16) . . ?
N41B C44B S43B 115.5(14) . . ?
C31B C44B S43B 120.2(14) . . ?
C42B N51B C51B 121.9(18) . . ?
C42B N51B H51C 119.1 . . ?
C51B N51B H51C 119.1 . . ?
C65B C51B N51B 109.4(19) . . ?
C65B C51B C53B 112.5(17) . . ?
N51B C51B C53B 110.2(16) . . ?
C65B C51B H51D 108.2 . . ?
N51B C51B H51D 108.2 . . ?
C53B C51B H51D 108.2 . . ?
C55B C53B C54B 111(2) . . ?
C55B C53B C51B 118(2) . . ?
C54B C53B C51B 107.6(18) . . ?
C55B C53B H53B 106.4 . . ?
C54B C53B H53B 106.4 . . ?
C51B C53B H53B 106.4 . . ?
C53B C54B H54D 109.5 . . ?
C53B C54B H54E 109.5 . . ?
H54D C54B H54E 109.5 . . ?
C53B C54B H54F 109.5 . . ?
H54D C54B H54F 109.5 . . ?
H54E C54B H54F 109.5 . . ?
C53B C55B C56B 112(3) . . ?
C53B C55B H55C 109.3 . . ?
C56B C55B H55C 109.3 . . ?
C53B C55B H55D 109.3 . . ?
C56B C55B H55D 109.3 . . ?
H55C C55B H55D 108.0 . . ?
C55B C56B H56D 109.5 . . ?
C55B C56B H56E 109.5 . . ?
H56D C56B H56E 109.5 . . ?
C55B C56B H56F 109.5 . . ?
H56D C56B H56F 109.5 . . ?
H56E C56B H56F 109.5 . . ?
C65B N61B C61B 106.5(16) . . ?
N61B C61B C62B 112.1(16) . . ?
N61B C61B C63B 104.3(15) . . ?
C62B C61B C63B 109.1(17) . . ?
N61B C61B H61B 110.4 . . ?
C62B C61B H61B 110.4 . . ?
C63B C61B H61B 110.4 . . ?
O62B C62B N71B 122(2) . . ?
O62B C62B C61B 122.2(18) . . ?
N71B C62B C61B 116(2) . . ?
O63B C63B C61B 102.0(15) . . ?
O63B C63B C64B 110.3(15) . . ?
C61B C63B C64B 114.8(16) . . ?
O63B C63B H63B 109.8 . . ?
C61B C63B H63B 109.8 . . ?
C64B C63B H63B 109.8 . . ?
C65B O63B C63B 105.8(13) . . ?
C63B C64B H64D 109.5 . . ?
C63B C64B H64E 109.5 . . ?
H64D C64B H64E 109.5 . . ?
C63B C64B H64F 109.5 . . ?
H64D C64B H64F 109.5 . . ?
H64E C64B H64F 109.5 . . ?
N61B C65B O63B 116.4(17) . . ?
N61B C65B C51B 127.3(18) . . ?
O63B C65B C51B 116.1(16) . . ?
C62B N71B C71B 122(2) . . ?
C62B N71B H71C 118.9 . . ?
C71B N71B H71C 118.9 . . ?
N71B C71B C84B 107.4(14) . . ?
N71B C71B C73B 114.8(18) . . ?
C84B C71B C73B 114.7(16) . . ?
N71B C71B H71D 106.5 . . ?
C84B C71B H71D 106.5 . . ?
C73B C71B H71D 106.5 . . ?
C75B C73B C74B 113(2) . . ?
C75B C73B C71B 110(2) . . ?
C74B C73B C71B 110.6(18) . . ?
C75B C73B H73B 107.6 . . ?
C74B C73B H73B 107.6 . . ?
C71B C73B H73B 107.6 . . ?
C73B C74B H74D 109.5 . . ?
C73B C74B H74E 109.5 . . ?
H74D C74B H74E 109.5 . . ?
C73B C74B H74F 109.5 . . ?
H74D C74B H74F 109.5 . . ?
H74E C74B H74F 109.5 . . ?
C73B C75B H75D 109.5 . . ?
C73B C75B H75E 109.5 . . ?
H75D C75B H75E 109.5 . . ?
C73B C75B H75F 109.5 . . ?
H75D C75B H75F 109.5 . . ?
H75E C75B H75F 109.5 . . ?
C84B N81B C81B 110.7(16) . . ?
C83B C81B N81B 114.9(15) . . ?
C83B C81B C82B 125.7(16) . . ?
N81B C81B C82B 119.3(15) . . ?
O82B C82B N11B 122.3(13) . . ?
O82B C82B C81B 121.4(14) . . ?
N11B C82B C81B 116.2(14) . . ?
C81B C83B S83B 111.5(14) . . ?
C81B C83B H83B 124.2 . . ?
S83B C83B H83B 124.2 . . ?
C83B S83B C84B 89.3(9) . . ?
N81B C84B C71B 122.2(17) . . ?
N81B C84B S83B 113.6(15) . . ?
C71B C84B S83B 124.1(13) . . ?

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
C4S N1S C1S O1S 176(4) . . . . ?
C3S N1S C1S O1S -5(5) . . . . ?
C4S N1S C1S C2S -2(5) . . . . ?
C3S N1S C1S C2S 177(3) . . . . ?
C82A N11A C11A C25A -74.3(19) . . . . ?
C82A N11A C11A C13A 157.9(15) . . . . ?
N11A C11A C13A C14A -177.9(15) . . . . ?
C25A C11A C13A C14A 57.1(19) . . . . ?
C11A C13A C14A C19A -112.2(19) . . . . ?
C11A C13A C14A C15A 67(2) . . . . ?
C19A C14A C15A C16A 1(3) . . . . ?
C13A C14A C15A C16A -178.2(15) . . . . ?
C14A C15A C16A C17A 0(3) . . . . ?
C15A C16A C17A C18A -1(3) . . . . ?
C15A C16A C17A I17A 175.9(14) . . . . ?
C16A C17A C18A C19A 2(3) . . . . ?
I17A C17A C18A C19A -175.4(13) . . . . ?
C15A C14A C19A C18A 0(3) . . . . ?
C13A C14A C19A C18A 178.8(15) . . . . ?
C17A C18A C19A C14A -1(3) . . . . ?
C25A N21A C21A C22A 102.2(17) . . . . ?
C25A N21A C21A C23A -17.0(17) . . . . ?
N21A C21A C22A O22A 172.2(18) . . . . ?
C23A C21A C22A O22A -71(2) . . . . ?
N21A C21A C22A N31A -11(2) . . . . ?
C23A C21A C22A N31A 106.2(17) . . . . ?
N21A C21A C23A O23A 20.3(16) . . . . ?
C22A C21A C23A O23A -103.3(15) . . . . ?
N21A C21A C23A C24A -96.5(16) . . . . ?
C22A C21A C23A C24A 139.9(16) . . . . ?
C24A C23A O23A C25A 103.8(15) . . . . ?
C21A C23A O23A C25A -16.7(15) . . . . ?
C21A N21A C25A O23A 6.5(19) . . . . ?
C21A N21A C25A C11A -172.2(15) . . . . ?
C23A O23A C25A N21A 7.4(18) . . . . ?
C23A O23A C25A C11A -173.7(12) . . . . ?
N11A C11A C25A N21A 110.9(18) . . . . ?
C13A C11A C25A N21A -123.3(17) . . . . ?
N11A C11A C25A O23A -67.9(17) . . . . ?
C13A C11A C25A O23A 57.9(18) . . . . ?
O22A C22A N31A C31A 15(3) . . . . ?
C21A C22A N31A C31A -161.5(15) . . . . ?
C22A N31A C31A C44A 110.2(17) . . . . ?
C22A N31A C31A C33A -119.4(17) . . . . ?
N31A C31A C33A C34A 68.4(19) . . . . ?
C44A C31A C33A C34A -166.6(15) . . . . ?
N31A C31A C33A C35A -53(2) . . . . ?
C44A C31A C33A C35A 72(2) . . . . ?
C44A N41A C41A C43A -4(3) . . . . ?
C44A N41A C41A C42A 175.5(18) . . . . ?
C43A C41A C42A O42A 1(3) . . . . ?
N41A C41A C42A O42A -179.1(18) . . . . ?
C43A C41A C42A N51A -178(2) . . . . ?
N41A C41A C42A N51A 2(3) . . . . ?
N41A C41A C43A S43A 0(3) . . . . ?
C42A C41A C43A S43A -179.6(17) . . . . ?
C41A C43A S43A C44A 2.6(19) . . . . ?
C41A N41A C44A C31A -176.2(17) . . . . ?
C41A N41A C44A S43A 6(2) . . . . ?
N31A C31A C44A N41A -27(2) . . . . ?
C33A C31A C44A N41A -155.8(17) . . . . ?
N31A C31A C44A S43A 150.0(12) . . . . ?
C33A C31A C44A S43A 22(2) . . . . ?
C43A S43A C44A N41A -5.4(16) . . . . ?
C43A S43A C44A C31A 177.0(16) . . . . ?
O42A C42A N51A C51A 4(3) . . . . ?
C41A C42A N51A C51A -178.0(17) . . . . ?
C42A N51A C51A C65A -81(2) . . . . ?
C42A N51A C51A C53A 151.5(18) . . . . ?
N51A C51A C53A C55A -63(2) . . . . ?
C65A C51A C53A C55A 173.1(19) . . . . ?
N51A C51A C53A C54A 172.2(17) . . . . ?
C65A C51A C53A C54A 48(2) . . . . ?
C51A C53A C55A C56A -177(2) . . . . ?
C54A C53A C55A C56A -57(3) . . . . ?
C65A N61A C61A C62A 103.9(17) . . . . ?
C65A N61A C61A C63A -13.4(18) . . . . ?
N61A C61A C62A O62A -175.7(16) . . . . ?
C63A C61A C62A O62A -59(2) . . . . ?
N61A C61A C62A N71A 3(2) . . . . ?
C63A C61A C62A N71A 119.3(19) . . . . ?
N61A C61A C63A C64A -94.4(18) . . . . ?
C62A C61A C63A C64A 148.4(17) . . . . ?
N61A C61A C63A O63A 18.0(18) . . . . ?
C62A C61A C63A O63A -99.2(16) . . . . ?
C64A C63A O63A C65A 97.4(17) . . . . ?
C61A C63A O63A C65A -16.6(18) . . . . ?
C61A N61A C65A O63A 2(2) . . . . ?
C61A N61A C65A C51A -169.3(17) . . . . ?
C63A O63A C65A N61A 10(2) . . . . ?
C63A O63A C65A C51A -177.4(16) . . . . ?
N51A C51A C65A N61A 111(2) . . . . ?
C53A C51A C65A N61A -124(2) . . . . ?
N51A C51A C65A O63A -60(2) . . . . ?
C53A C51A C65A O63A 65(2) . . . . ?
O62A C62A N71A C71A 15(3) . . . . ?
C61A C62A N71A C71A -164.0(16) . . . . ?
C62A N71A C71A C84A 84(2) . . . . ?
C62A N71A C71A C73A -152.8(18) . . . . ?
N71A C71A C73A C74A 152.7(19) . . . . ?
C84A C71A C73A C74A -87(2) . . . . ?
N71A C71A C73A C75A 36(3) . . . . ?
C84A C71A C73A C75A 156(2) . . . . ?
C84A N81A C81A C83A -3(3) . . . . ?
C84A N81A C81A C82A 177.6(18) . . . . ?
C11A N11A C82A O82A 7(3) . . . . ?
C11A N11A C82A C81A -168.3(15) . . . . ?
C83A C81A C82A O82A -2(3) . . . . ?
N81A C81A C82A O82A 177.4(17) . . . . ?
C83A C81A C82A N11A 173.2(19) . . . . ?
N81A C81A C82A N11A -7(3) . . . . ?
N81A C81A C83A S83A 1(2) . . . . ?
C82A C81A C83A S83A -179.0(15) . . . . ?
C81A C83A S83A C84A 0.1(17) . . . . ?
C81A N81A C84A C71A -174.8(19) . . . . ?
C81A N81A C84A S83A 3(2) . . . . ?
N71A C71A C84A N81A -11(3) . . . . ?
C73A C71A C84A N81A -133(2) . . . . ?
N71A C71A C84A S83A 171.2(15) . . . . ?
C73A C71A C84A S83A 50(3) . . . . ?
C83A S83A C84A N81A -1.8(17) . . . . ?
C83A S83A C84A C71A 175.7(18) . . . . ?
C82B N11B C11B C25B -77.2(18) . . . . ?
C82B N11B C11B C13B 156.1(14) . . . . ?
N11B C11B C13B C14B -179.1(14) . . . . ?
C25B C11B C13B C14B 55.9(18) . . . . ?
C11B C13B C14B C15B -113.0(17) . . . . ?
C11B C13B C14B C19B 65(2) . . . . ?
C19B C14B C15B C16B -1(2) . . . . ?
C13B C14B C15B C16B 177.0(15) . . . . ?
C14B C15B C16B C17B 1(3) . . . . ?
C15B C16B C17B C18B -1(3) . . . . ?
C15B C16B C17B I17B -177.0(13) . . . . ?
C16B C17B C18B C19B 1(3) . . . . ?
I17B C17B C18B C19B 177.1(14) . . . . ?
C17B C18B C19B C14B -1(3) . . . . ?
C15B C14B C19B C18B 1(2) . . . . ?
C13B C14B C19B C18B -176.8(16) . . . . ?
C25B N21B C21B C23B -17.4(17) . . . . ?
C25B N21B C21B C22B 105.4(17) . . . . ?
N21B C21B C22B O22B 172.8(16) . . . . ?
C23B C21B C22B O22B -69(2) . . . . ?
N21B C21B C22B N31B -15(2) . . . . ?
C23B C21B C22B N31B 103(2) . . . . ?
N21B C21B C23B O23B 21.8(16) . . . . ?
C22B C21B C23B O23B -99.9(15) . . . . ?
N21B C21B C23B C24B -97.7(16) . . . . ?
C22B C21B C23B C24B 140.6(16) . . . . ?
C21B C23B O23B C25B -18.1(15) . . . . ?
C24B C23B O23B C25B 104.9(17) . . . . ?
C21B N21B C25B O23B 6.0(19) . . . . ?
C21B N21B C25B C11B -171.6(14) . . . . ?
C23B O23B C25B N21B 8.3(18) . . . . ?
C23B O23B C25B C11B -173.9(12) . . . . ?
N11B C11B C25B N21B 111.2(18) . . . . ?
C13B C11B C25B N21B -124.1(16) . . . . ?
N11B C11B C25B O23B -66.5(18) . . . . ?
C13B C11B C25B O23B 58.2(17) . . . . ?
O22B C22B N31B C31B 16(3) . . . . ?
C21B C22B N31B C31B -156.1(17) . . . . ?
C22B N31B C31B C44B 106.3(19) . . . . ?
C22B N31B C31B C33B -124.3(18) . . . . ?
N31B C31B C33B C34B -57.4(19) . . . . ?
C44B C31B C33B C34B 68(2) . . . . ?
N31B C31B C33B C35B 68.9(18) . . . . ?
C44B C31B C33B C35B -165.7(15) . . . . ?
C44B N41B C41B C43B 0(3) . . . . ?
C44B N41B C41B C42B 177.2(19) . . . . ?
C43B C41B C42B O42B -3(4) . . . . ?
N41B C41B C42B O42B 180(2) . . . . ?
C43B C41B C42B N51B -180(2) . . . . ?
N41B C41B C42B N51B 3(3) . . . . ?
N41B C41B C43B S43B -3(3) . . . . ?
C42B C41B C43B S43B 179.8(18) . . . . ?
C41B C43B S43B C44B 3.6(17) . . . . ?
C41B N41B C44B C31B -179.4(18) . . . . ?
C41B N41B C44B S43B 3(2) . . . . ?
N31B C31B C44B N41B -25(2) . . . . ?
C33B C31B C44B N41B -152.4(19) . . . . ?
N31B C31B C44B S43B 152.3(13) . . . . ?
C33B C31B C44B S43B 25(2) . . . . ?
C43B S43B C44B N41B -4.1(16) . . . . ?
C43B S43B C44B C31B 178.4(16) . . . . ?
O42B C42B N51B C51B 7(3) . . . . ?
C41B C42B N51B C51B -176.9(19) . . . . ?
C42B N51B C51B C65B -79(2) . . . . ?
C42B N51B C51B C53B 157(2) . . . . ?
C65B C51B C53B C55B -179(2) . . . . ?
N51B C51B C53B C55B -56(3) . . . . ?
C65B C51B C53B C54B 54(3) . . . . ?
N51B C51B C53B C54B 177(2) . . . . ?
C54B C53B C55B C56B 56(3) . . . . ?
C51B C53B C55B C56B -69(3) . . . . ?
C65B N61B C61B C62B 101.5(18) . . . . ?
C65B N61B C61B C63B -16.4(19) . . . . ?
N61B C61B C62B O62B -175.7(16) . . . . ?
C63B C61B C62B O62B -61(2) . . . . ?
N61B C61B C62B N71B 3(2) . . . . ?
C63B C61B C62B N71B 118.1(18) . . . . ?
N61B C61B C63B O63B 21.6(18) . . . . ?
C62B C61B C63B O63B -98.4(18) . . . . ?
N61B C61B C63B C64B -97.6(19) . . . . ?
C62B C61B C63B C64B 142.4(18) . . . . ?
C61B C63B O63B C65B -19.7(18) . . . . ?
C64B C63B O63B C65B 102.7(18) . . . . ?
C61B N61B C65B O63B 4(2) . . . . ?
C61B N61B C65B C51B -169.8(18) . . . . ?
C63B O63B C65B N61B 11(2) . . . . ?
C63B O63B C65B C51B -174.8(16) . . . . ?
N51B C51B C65B N61B 111(2) . . . . ?
C53B C51B C65B N61B -126(2) . . . . ?
N51B C51B C65B O63B -63(2) . . . . ?
C53B C51B C65B O63B 60(2) . . . . ?
O62B C62B N71B C71B 12(3) . . . . ?
C61B C62B N71B C71B -167.1(15) . . . . ?
C62B N71B C71B C84B 86(2) . . . . ?
C62B N71B C71B C73B -145.0(18) . . . . ?
N71B C71B C73B C75B 158.2(19) . . . . ?
C84B C71B C73B C75B -77(2) . . . . ?
N71B C71B C73B C74B 33(3) . . . . ?
C84B C71B C73B C74B 158(2) . . . . ?
C84B N81B C81B C83B 0(2) . . . . ?
C84B N81B C81B C82B 178.5(16) . . . . ?
C11B N11B C82B O82B 9(2) . . . . ?
C11B N11B C82B C81B -170.5(14) . . . . ?
C83B C81B C82B O82B -4(3) . . . . ?
N81B C81B C82B O82B 177.2(15) . . . . ?
C83B C81B C82B N11B 175.3(17) . . . . ?
N81B C81B C82B N11B -3(2) . . . . ?
N81B C81B C83B S83B 0(2) . . . . ?
C82B C81B C83B S83B -178.1(14) . . . . ?
C81B C83B S83B C84B -0.4(15) . . . . ?
C81B N81B C84B C71B -176.4(17) . . . . ?
C81B N81B C84B S83B 0(2) . . . . ?
N71B C71B C84B N81B -12(3) . . . . ?
C73B C71B C84B N81B -141(2) . . . . ?
N71B C71B C84B S83B 172.2(15) . . . . ?
C73B C71B C84B S83B 43(3) . . . . ?
C83B S83B C84B N81B 0.4(16) . . . . ?
C83B S83B C84B C71B 176.5(18) . . . . ?

_refine_diff_density_max         4.104
_refine_diff_density_min         -2.411
_refine_diff_density_rms         0.201



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile'
####################################################################### 
# 
# 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_201219_Phecf3
_database_code_depnum_ccdc_archive 'CCDC 2289965'
loop_
_audit_author_name
_audit_author_address
'Akiko Asano'
;Osaka Medical nad Pharmaceutical University
Japan
;
_audit_update_record             
;
2023-08-22 deposited with the CCDC.	2023-12-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        Phe(4cf3)_ASC
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H47 F3 N8 O6 S2, C3 H6 O'
_chemical_formula_sum            'C43 H53 F3 N8 O7 S2'
_chemical_formula_weight         915.05
_chemical_compound_source        synthesis
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'
F F 0.0727 0.0534 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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'

_cell_length_a                   9.4424(4)
_cell_length_b                   9.8919(4)
_cell_length_c                   12.9370(6)
_cell_angle_alpha                80.097(4)
_cell_angle_beta                 80.867(4)
_cell_angle_gamma                84.776(4)
_cell_volume                     1172.74(9)
_cell_formula_units_Z            1
_cell_measurement_temperature    100
_cell_measurement_reflns_used    4809
_cell_measurement_theta_min      5.4560
_cell_measurement_theta_max      73.0320

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_F_000             482
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    1.607
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.73206
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   CrysAlisPro
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   rotating-anode
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single & P200K'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 5.811
_diffrn_reflns_number            17517
_diffrn_reflns_av_unetI/netI     0.0563
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         4.547
_diffrn_reflns_theta_max         63.685
_diffrn_reflns_theta_full        63.685
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.899
_diffrn_reflns_point_group_measured_fraction_full 0.899
_reflns_number_total             6940
_reflns_number_gt                4779
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.809
_reflns_Friedel_fraction_max     0.804
_reflns_Friedel_fraction_full    0.804

_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
_computing_cell_refinement       CrysAlisPro
_computing_data_reduction        CrysAlisPro
_computing_structure_solution    SHELXT
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_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 x determined using 1688 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.023(15)
_chemical_absolute_configuration rm
_refine_ls_number_reflns         6940
_refine_ls_number_parameters     570
_refine_ls_number_restraints     369
_refine_ls_R_factor_all          0.1541
_refine_ls_R_factor_gt           0.1268
_refine_ls_wR_factor_ref         0.3792
_refine_ls_wR_factor_gt          0.3550
_refine_ls_goodness_of_fit_ref   1.500
_refine_ls_restrained_S_all      1.567
_refine_ls_shift/su_max          0.005
_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
N11 N 0.6255(14) 0.7086(13) 0.3695(8) 0.090(2) Uani 1 1 d . U . . .
H11 H 0.639582 0.621256 0.370695 0.109 Uiso 1 1 calc R U . . .
C11 C 0.5835(18) 0.7637(16) 0.4688(10) 0.092(2) Uani 1 1 d . U . . .
H11A H 0.585618 0.864078 0.455118 0.110 Uiso 1 1 calc R U . . .
C13 C 0.4207(19) 0.7202(17) 0.5158(11) 0.096(2) Uani 1 1 d . U . . .
H13A H 0.356748 0.763519 0.466239 0.115 Uiso 1 1 calc R U . . .
H13B H 0.418199 0.621468 0.520993 0.115 Uiso 1 1 calc R U . . .
C14 C 0.364(2) 0.7604(17) 0.6251(11) 0.097(2) Uani 1 1 d . U . . .
C15 C 0.366(2) 0.6665(18) 0.7151(12) 0.100(2) Uani 1 1 d . U . . .
H15 H 0.407844 0.578041 0.712994 0.120 Uiso 1 1 calc R U . . .
C16 C 0.303(2) 0.7072(18) 0.8094(13) 0.106(2) Uani 1 1 d . U . . .
H16 H 0.300603 0.642129 0.870723 0.127 Uiso 1 1 calc R U . . .
C17 C 0.245(2) 0.834(2) 0.8188(13) 0.113(2) Uani 1 1 d . U . . .
C18 C 0.241(2) 0.932(2) 0.7242(13) 0.107(2) Uani 1 1 d . U . . .
H18 H 0.197452 1.019461 0.728210 0.128 Uiso 1 1 calc R U . . .
C19 C 0.301(2) 0.8979(18) 0.6278(12) 0.101(2) Uani 1 1 d . U . . .
H19 H 0.300682 0.961639 0.565995 0.122 Uiso 1 1 calc R U . . .
C110 C 0.170(3) 0.873(2) 0.9174(16) 0.129(3) Uani 1 1 d . U . . .
F110 F 0.2430(18) 0.8302(17) 0.9931(11) 0.163(3) Uani 1 1 d . U . . .
F111 F 0.0492(18) 0.8236(16) 0.9536(11) 0.159(3) Uani 1 1 d . U . . .
F112 F 0.1284(17) 0.9972(16) 0.9185(10) 0.157(3) Uani 1 1 d . U . . .
N21 N 0.7486(13) 0.5802(11) 0.5537(8) 0.079(3) Uani 1 1 d . . . . .
C21 C 0.8257(17) 0.5644(14) 0.6454(9) 0.082(4) Uani 1 1 d . . . . .
C22 C 0.7598(15) 0.4540(15) 0.7351(9) 0.078(3) Uani 1 1 d . . . . .
O22 O 0.7956(15) 0.4426(15) 0.8212(8) 0.118(4) Uani 1 1 d . . . . .
C23 C 0.811(2) 0.703(2) 0.6792(12) 0.108(5) Uani 1 1 d . . . . .
O23 O 0.7124(12) 0.7834(10) 0.6137(6) 0.093(3) Uani 1 1 d . . . . .
C24 C 0.971(3) 0.770(3) 0.644(3) 0.168(12) Uani 1 1 d . . . . .
H24A H 1.038328 0.718523 0.686299 0.252 Uiso 1 1 calc R U . . .
H24B H 1.003510 0.766112 0.570552 0.252 Uiso 1 1 calc R U . . .
H24C H 0.961613 0.863939 0.655463 0.252 Uiso 1 1 calc R U . . .
C25 C 0.6866(15) 0.7024(15) 0.5466(9) 0.076(3) Uani 1 1 d . . . . .
N31 N 0.6726(13) 0.3716(13) 0.7068(8) 0.085(3) Uani 1 1 d . U . . .
H31 H 0.659478 0.383802 0.641504 0.102 Uiso 1 1 calc R U . . .
C31 C 0.6008(16) 0.2659(14) 0.7780(9) 0.081(3) Uani 1 1 d . U . . .
H31A H 0.606365 0.277689 0.850922 0.098 Uiso 1 1 calc R U . . .
C33 C 0.6671(19) 0.1172(15) 0.7602(11) 0.090(3) Uani 1 1 d . U . . .
H33 H 0.670648 0.109458 0.685257 0.108 Uiso 1 1 calc R U . . .
C34 C 0.815(2) 0.102(2) 0.7855(17) 0.125(6) Uani 1 1 d . U . . .
H34A H 0.869777 0.173315 0.741748 0.188 Uiso 1 1 calc R U . . .
H34B H 0.812753 0.109358 0.858819 0.188 Uiso 1 1 calc R U . . .
H34C H 0.858392 0.013920 0.772569 0.188 Uiso 1 1 calc R U . . .
C35 C 0.576(2) 0.0078(19) 0.8268(13) 0.113(5) Uani 1 1 d . U . . .
H35A H 0.480986 0.020510 0.808290 0.169 Uiso 1 1 calc R U . . .
H35B H 0.617919 -0.081192 0.814142 0.169 Uiso 1 1 calc R U . . .
H35C H 0.572280 0.014246 0.900392 0.169 Uiso 1 1 calc R U . . .
N41 N 0.4034(12) 0.2974(10) 0.6706(7) 0.069(2) Uani 1 1 d . U . . .
C41 C 0.2540(14) 0.3136(13) 0.6790(9) 0.072(3) Uani 1 1 d . U . . .
C42 C 0.1804(15) 0.3287(14) 0.5859(9) 0.077(3) Uani 1 1 d . U . . .
O42 O 0.0494(13) 0.3264(15) 0.5987(8) 0.114(4) Uani 1 1 d . U . . .
C43 C 0.1868(17) 0.3178(14) 0.7796(9) 0.084(3) Uani 1 1 d . U . . .
H43 H 0.087996 0.332454 0.798022 0.101 Uiso 1 1 calc R U . . .
S43 S 0.3056(4) 0.2932(3) 0.8663(2) 0.0890(11) Uani 1 1 d . U . . .
C44 C 0.4464(16) 0.2824(13) 0.7607(8) 0.077(3) Uani 1 1 d . U . . .
N51 N 0.2590(12) 0.3483(11) 0.4892(7) 0.075(3) Uani 1 1 d . U . . .
H51 H 0.350992 0.347410 0.483830 0.090 Uiso 1 1 calc R U . . .
C51 C 0.1942(16) 0.3703(15) 0.3966(9) 0.081(3) Uani 1 1 d . U . . .
H51A H 0.096930 0.338540 0.417976 0.097 Uiso 1 1 calc R U . . .
C53 C 0.176(2) 0.520(2) 0.3530(13) 0.115(5) Uani 1 1 d . U . . .
H53 H 0.149419 0.571112 0.412211 0.138 Uiso 1 1 calc R U . . .
C54 C 0.298(3) 0.559(2) 0.301(2) 0.126(7) Uani 1 1 d . U . . .
H54A H 0.287940 0.655376 0.272197 0.189 Uiso 1 1 calc R U . . .
H54B H 0.369741 0.544621 0.347244 0.189 Uiso 1 1 calc R U . . .
H54C H 0.327294 0.507486 0.243670 0.189 Uiso 1 1 calc R U . . .
C55 C 0.045(3) 0.542(3) 0.281(2) 0.155(9) Uani 1 1 d . U . . .
H55A H 0.075669 0.513740 0.211864 0.187 Uiso 1 1 calc R U . . .
H55B H -0.038104 0.492861 0.316487 0.187 Uiso 1 1 calc R U . . .
C56 C 0.016(3) 0.696(3) 0.272(4) 0.184(13) Uani 1 1 d . U . . .
H56A H -0.060785 0.725447 0.230320 0.276 Uiso 1 1 calc R U . . .
H56B H -0.011661 0.720389 0.341200 0.276 Uiso 1 1 calc R U . . .
H56C H 0.100888 0.741043 0.237704 0.276 Uiso 1 1 calc R U . . .
N61 N 0.394(2) 0.2271(16) 0.3137(9) 0.114(2) Uani 1 1 d . U . . .
C61 C 0.423(2) 0.161(2) 0.2165(11) 0.1175(19) Uani 1 1 d . U . . .
H61 H 0.462698 0.066145 0.235682 0.141 Uiso 1 1 calc R U . . .
C62 C 0.527(3) 0.235(2) 0.1273(11) 0.1205(19) Uani 1 1 d . U . . .
O62 O 0.5420(16) 0.2018(13) 0.0397(7) 0.122(3) Uani 1 1 d . U . . .
C63 C 0.272(2) 0.1554(19) 0.1847(11) 0.117(2) Uani 1 1 d . U . . .
H63 H 0.272257 0.187055 0.108595 0.141 Uiso 1 1 calc R U . . .
O63 O 0.1858(15) 0.2501(12) 0.2478(7) 0.114(2) Uani 1 1 d . U . . .
C64 C 0.212(3) 0.016(2) 0.2190(14) 0.129(3) Uani 1 1 d . U . . .
H64A H 0.266442 -0.048530 0.178718 0.193 Uiso 1 1 calc R U . . .
H64B H 0.216505 -0.013446 0.293095 0.193 Uiso 1 1 calc R U . . .
H64C H 0.113209 0.022499 0.207200 0.193 Uiso 1 1 calc R U . . .
C65 C 0.270(2) 0.2808(19) 0.3193(11) 0.113(2) Uani 1 1 d . U . . .
N71 N 0.606(2) 0.3243(17) 0.1536(9) 0.1237(17) Uani 1 1 d . U . . .
H71 H 0.590892 0.336948 0.218630 0.148 Uiso 1 1 calc R U . . .
C71 C 0.719(3) 0.404(2) 0.0830(11) 0.1258(16) Uani 1 1 d . U . . .
H71A H 0.705694 0.399117 0.010119 0.151 Uiso 1 1 calc R U . . .
C73 C 0.872(3) 0.348(2) 0.0952(12) 0.1268(17) Uani 1 1 d . U . . .
H73 H 0.883813 0.343896 0.169506 0.152 Uiso 1 1 calc R U . . .
C74 C 0.898(3) 0.204(2) 0.0689(12) 0.130(2) Uani 1 1 d . U . . .
H74A H 0.828393 0.145715 0.112916 0.195 Uiso 1 1 calc R U . . .
H74B H 0.889555 0.205418 -0.004291 0.195 Uiso 1 1 calc R U . . .
H74C H 0.992894 0.167994 0.081496 0.195 Uiso 1 1 calc R U . . .
C75 C 0.976(3) 0.440(2) 0.0296(11) 0.129(2) Uani 1 1 d . U . . .
H75A H 0.956737 0.530790 0.047882 0.193 Uiso 1 1 calc R U . . .
H75B H 1.071445 0.406363 0.041849 0.193 Uiso 1 1 calc R U . . .
H75C H 0.968105 0.443788 -0.043939 0.193 Uiso 1 1 calc R U . . .
N81 N 0.681(2) 0.5830(17) 0.1914(9) 0.1270(16) Uani 1 1 d . U . . .
C81 C 0.664(3) 0.729(2) 0.1839(11) 0.1279(16) Uani 1 1 d . U . . .
C82 C 0.641(3) 0.791(2) 0.2803(11) 0.1279(18) Uani 1 1 d . U . . .
O82 O 0.6422(18) 0.9191(14) 0.2740(8) 0.131(2) Uani 1 1 d . U . . .
C83 C 0.656(3) 0.793(2) 0.0837(11) 0.1292(16) Uani 1 1 d . U . . .
H83 H 0.639923 0.887633 0.065546 0.155 Uiso 1 1 calc R U . . .
S83 S 0.6769(7) 0.6838(5) -0.0044(3) 0.1302(15) Uani 1 1 d . U . . .
C84 C 0.688(3) 0.551(2) 0.0976(11) 0.1274(15) Uani 1 1 d . U . . .
O1S O 0.5789(12) 0.3947(12) 0.4287(8) 0.095(3) Uani 1 1 d . U . . .
C1S C 0.666(3) 0.295(3) 0.4321(18) 0.140(6) Uani 1 1 d . U . . .
C3S C 0.827(3) 0.280(4) 0.468(2) 0.175(9) Uani 1 1 d . U . . .
H3S1 H 0.885346 0.210723 0.433606 0.263 Uiso 1 1 calc R U . . .
H3S2 H 0.818984 0.253018 0.543351 0.263 Uiso 1 1 calc R U . . .
H3S3 H 0.870206 0.366031 0.447300 0.263 Uiso 1 1 calc R U . . .
C2S C 0.632(4) 0.149(3) 0.4242(19) 0.159(8) Uani 1 1 d . U . . .
H2S1 H 0.584573 0.151416 0.363414 0.239 Uiso 1 1 calc R U . . .
H2S2 H 0.569983 0.112243 0.487141 0.239 Uiso 1 1 calc R U . . .
H2S3 H 0.719533 0.092078 0.417207 0.239 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
N11 C82 1.29(2) . ?
N11 C11 1.465(14) . ?
N11 H11 0.8600 . ?
C11 C25 1.52(2) . ?
C11 C13 1.63(3) . ?
C11 H11A 0.9800 . ?
C13 C14 1.535(17) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C15 1.36(2) . ?
C14 C19 1.44(2) . ?
C15 C16 1.38(2) . ?
C15 H15 0.9300 . ?
C16 C17 1.34(2) . ?
C16 H16 0.9300 . ?
C17 C18 1.43(3) . ?
C17 C110 1.46(2) . ?
C18 C19 1.37(2) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
C110 F112 1.25(3) . ?
C110 F111 1.27(3) . ?
C110 F110 1.28(3) . ?
N21 C25 1.290(17) . ?
N21 C21 1.468(18) . ?
C21 C23 1.50(2) . ?
C21 C22 1.54(2) . ?
C22 O22 1.200(16) . ?
C22 N31 1.340(19) . ?
C23 O23 1.45(2) . ?
C23 C24 1.67(3) . ?
O23 C25 1.340(16) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
N31 C31 1.415(19) . ?
N31 H31 0.8600 . ?
C31 C44 1.50(2) . ?
C31 C33 1.585(19) . ?
C31 H31A 0.9800 . ?
C33 C34 1.47(3) . ?
C33 C35 1.50(3) . ?
C33 H33 0.9800 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
N41 C44 1.275(16) . ?
N41 C41 1.394(17) . ?
C41 C43 1.360(16) . ?
C41 C42 1.463(19) . ?
C42 O42 1.223(18) . ?
C42 N51 1.342(15) . ?
C43 S43 1.683(16) . ?
C43 H43 0.9300 . ?
S43 C44 1.758(11) . ?
N51 C51 1.405(16) . ?
N51 H51 0.8600 . ?
C51 C53 1.49(3) . ?
C51 C65 1.503(19) . ?
C51 H51A 0.9800 . ?
C53 C54 1.30(3) . ?
C53 C55 1.65(3) . ?
C53 H53 0.9800 . ?
C54 H54A 0.9600 . ?
C54 H54B 0.9600 . ?
C54 H54C 0.9600 . ?
C55 C56 1.52(4) . ?
C55 H55A 0.9700 . ?
C55 H55B 0.9700 . ?
C56 H56A 0.9600 . ?
C56 H56B 0.9600 . ?
C56 H56C 0.9600 . ?
N61 C65 1.24(2) . ?
N61 C61 1.493(18) . ?
C61 C62 1.52(3) . ?
C61 C63 1.55(3) . ?
C61 H61 0.9800 . ?
C62 O62 1.217(18) . ?
C62 N71 1.33(3) . ?
C63 O63 1.456(19) . ?
C63 C64 1.51(3) . ?
C63 H63 0.9800 . ?
O63 C65 1.40(2) . ?
C64 H64A 0.9600 . ?
C64 H64B 0.9600 . ?
C64 H64C 0.9600 . ?
N71 C71 1.47(3) . ?
N71 H71 0.8600 . ?
C71 C84 1.49(3) . ?
C71 C73 1.52(3) . ?
C71 H71A 0.9800 . ?
C73 C75 1.47(3) . ?
C73 C74 1.52(3) . ?
C73 H73 0.9800 . ?
C74 H74A 0.9600 . ?
C74 H74B 0.9600 . ?
C74 H74C 0.9600 . ?
C75 H75A 0.9600 . ?
C75 H75B 0.9600 . ?
C75 H75C 0.9600 . ?
N81 C84 1.30(2) . ?
N81 C81 1.42(3) . ?
C81 C83 1.35(2) . ?
C81 C82 1.46(2) . ?
C82 O82 1.26(2) . ?
C83 S83 1.678(19) . ?
C83 H83 0.9300 . ?
S83 C84 1.705(17) . ?
O1S C1S 1.22(3) . ?
C1S C2S 1.53(4) . ?
C1S C3S 1.65(4) . ?
C3S H3S1 0.9600 . ?
C3S H3S2 0.9600 . ?
C3S H3S3 0.9600 . ?
C2S H2S1 0.9600 . ?
C2S H2S2 0.9600 . ?
C2S H2S3 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
C82 N11 C11 120.1(14) . . ?
C82 N11 H11 120.0 . . ?
C11 N11 H11 120.0 . . ?
N11 C11 C25 109.4(11) . . ?
N11 C11 C13 107.2(13) . . ?
C25 C11 C13 110.5(11) . . ?
N11 C11 H11A 109.9 . . ?
C25 C11 H11A 109.9 . . ?
C13 C11 H11A 109.9 . . ?
C14 C13 C11 113.9(13) . . ?
C14 C13 H13A 108.8 . . ?
C11 C13 H13A 108.8 . . ?
C14 C13 H13B 108.8 . . ?
C11 C13 H13B 108.8 . . ?
H13A C13 H13B 107.7 . . ?
C15 C14 C19 121.5(13) . . ?
C15 C14 C13 120.9(13) . . ?
C19 C14 C13 117.4(13) . . ?
C14 C15 C16 117.6(15) . . ?
C14 C15 H15 121.2 . . ?
C16 C15 H15 121.2 . . ?
C17 C16 C15 124.5(17) . . ?
C17 C16 H16 117.8 . . ?
C15 C16 H16 117.8 . . ?
C16 C17 C18 118.1(14) . . ?
C16 C17 C110 124.2(18) . . ?
C18 C17 C110 117.3(17) . . ?
C19 C18 C17 120.3(16) . . ?
C19 C18 H18 119.9 . . ?
C17 C18 H18 119.9 . . ?
C18 C19 C14 118.0(15) . . ?
C18 C19 H19 121.0 . . ?
C14 C19 H19 121.0 . . ?
F112 C110 F111 96.7(18) . . ?
F112 C110 F110 110(2) . . ?
F111 C110 F110 102.3(19) . . ?
F112 C110 C17 119(2) . . ?
F111 C110 C17 117(2) . . ?
F110 C110 C17 111(2) . . ?
C25 N21 C21 105.5(11) . . ?
N21 C21 C23 105.6(12) . . ?
N21 C21 C22 110.5(12) . . ?
C23 C21 C22 111.5(11) . . ?
O22 C22 N31 125.1(14) . . ?
O22 C22 C21 119.0(14) . . ?
N31 C22 C21 115.7(10) . . ?
O23 C23 C21 104.3(12) . . ?
O23 C23 C24 107.6(19) . . ?
C21 C23 C24 107.4(16) . . ?
C25 O23 C23 105.9(12) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N21 C25 O23 118.1(13) . . ?
N21 C25 C11 125.6(12) . . ?
O23 C25 C11 116.3(12) . . ?
C22 N31 C31 123.9(11) . . ?
C22 N31 H31 118.0 . . ?
C31 N31 H31 118.0 . . ?
N31 C31 C44 106.9(11) . . ?
N31 C31 C33 112.5(11) . . ?
C44 C31 C33 110.1(12) . . ?
N31 C31 H31A 109.1 . . ?
C44 C31 H31A 109.1 . . ?
C33 C31 H31A 109.1 . . ?
C34 C33 C35 111.6(15) . . ?
C34 C33 C31 108.1(14) . . ?
C35 C33 C31 110.9(12) . . ?
C34 C33 H33 108.7 . . ?
C35 C33 H33 108.7 . . ?
C31 C33 H33 108.7 . . ?
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 . . ?
C44 N41 C41 112.2(9) . . ?
C43 C41 N41 113.7(12) . . ?
C43 C41 C42 124.5(13) . . ?
N41 C41 C42 121.7(9) . . ?
O42 C42 N51 122.3(13) . . ?
O42 C42 C41 119.1(10) . . ?
N51 C42 C41 118.6(12) . . ?
C41 C43 S43 111.2(11) . . ?
C41 C43 H43 124.4 . . ?
S43 C43 H43 124.4 . . ?
C43 S43 C44 89.5(6) . . ?
N41 C44 C31 125.0(10) . . ?
N41 C44 S43 113.3(11) . . ?
C31 C44 S43 121.6(8) . . ?
C42 N51 C51 121.5(12) . . ?
C42 N51 H51 119.3 . . ?
C51 N51 H51 119.3 . . ?
N51 C51 C53 111.7(13) . . ?
N51 C51 C65 110.5(12) . . ?
C53 C51 C65 115.3(12) . . ?
N51 C51 H51A 106.2 . . ?
C53 C51 H51A 106.2 . . ?
C65 C51 H51A 106.2 . . ?
C54 C53 C51 108.8(18) . . ?
C54 C53 C55 113.6(17) . . ?
C51 C53 C55 108.2(18) . . ?
C54 C53 H53 108.7 . . ?
C51 C53 H53 108.7 . . ?
C55 C53 H53 108.7 . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C56 C55 C53 100(2) . . ?
C56 C55 H55A 111.8 . . ?
C53 C55 H55A 111.8 . . ?
C56 C55 H55B 111.8 . . ?
C53 C55 H55B 111.8 . . ?
H55A C55 H55B 109.5 . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C65 N61 C61 107.5(16) . . ?
N61 C61 C62 113.8(18) . . ?
N61 C61 C63 104.4(15) . . ?
C62 C61 C63 112.5(14) . . ?
N61 C61 H61 108.7 . . ?
C62 C61 H61 108.7 . . ?
C63 C61 H61 108.7 . . ?
O62 C62 N71 124(2) . . ?
O62 C62 C61 119(2) . . ?
N71 C62 C61 116.6(13) . . ?
O63 C63 C64 107.5(16) . . ?
O63 C63 C61 101.6(13) . . ?
C64 C63 C61 113.0(16) . . ?
O63 C63 H63 111.4 . . ?
C64 C63 H63 111.4 . . ?
C61 C63 H63 111.4 . . ?
C65 O63 C63 107.5(14) . . ?
C63 C64 H64A 109.5 . . ?
C63 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C63 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
N61 C65 O63 116.5(14) . . ?
N61 C65 C51 128.5(17) . . ?
O63 C65 C51 114.9(16) . . ?
C62 N71 C71 127.0(13) . . ?
C62 N71 H71 116.5 . . ?
C71 N71 H71 116.5 . . ?
N71 C71 C84 107.3(15) . . ?
N71 C71 C73 114.5(14) . . ?
C84 C71 C73 114(2) . . ?
N71 C71 H71A 106.8 . . ?
C84 C71 H71A 106.8 . . ?
C73 C71 H71A 106.8 . . ?
C75 C73 C74 111.3(16) . . ?
C75 C73 C71 110.8(15) . . ?
C74 C73 C71 111(2) . . ?
C75 C73 H73 107.9 . . ?
C74 C73 H73 107.9 . . ?
C71 C73 H73 107.9 . . ?
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 . . ?
C84 N81 C81 109.1(13) . . ?
C83 C81 N81 112.5(17) . . ?
C83 C81 C82 127.4(19) . . ?
N81 C81 C82 119.7(14) . . ?
O82 C82 N11 122.8(15) . . ?
O82 C82 C81 120.1(15) . . ?
N11 C82 C81 117.1(18) . . ?
C81 C83 S83 113.0(16) . . ?
C81 C83 H83 123.5 . . ?
S83 C83 H83 123.5 . . ?
C83 S83 C84 88.8(9) . . ?
N81 C84 C71 119.4(14) . . ?
N81 C84 S83 116.5(15) . . ?
C71 C84 S83 123.8(11) . . ?
O1S C1S C2S 125(3) . . ?
O1S C1S C3S 128(2) . . ?
C2S C1S C3S 106(2) . . ?
C1S C3S H3S1 109.5 . . ?
C1S C3S H3S2 109.5 . . ?
H3S1 C3S H3S2 109.5 . . ?
C1S C3S H3S3 109.5 . . ?
H3S1 C3S H3S3 109.5 . . ?
H3S2 C3S H3S3 109.5 . . ?
C1S C2S H2S1 109.5 . . ?
C1S C2S H2S2 109.5 . . ?
H2S1 C2S H2S2 109.5 . . ?
C1S C2S H2S3 109.5 . . ?
H2S1 C2S H2S3 109.5 . . ?
H2S2 C2S H2S3 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
C82 N11 C11 C25 -129.0(18) . . . . ?
C82 N11 C11 C13 111.1(19) . . . . ?
N11 C11 C13 C14 175.4(13) . . . . ?
C25 C11 C13 C14 56.2(16) . . . . ?
C11 C13 C14 C15 -99(2) . . . . ?
C11 C13 C14 C19 85(2) . . . . ?
C19 C14 C15 C16 1(3) . . . . ?
C13 C14 C15 C16 -174.9(18) . . . . ?
C14 C15 C16 C17 -2(3) . . . . ?
C15 C16 C17 C18 4(3) . . . . ?
C15 C16 C17 C110 176(2) . . . . ?
C16 C17 C18 C19 -3(3) . . . . ?
C110 C17 C18 C19 -176(2) . . . . ?
C17 C18 C19 C14 1(3) . . . . ?
C15 C14 C19 C18 0(3) . . . . ?
C13 C14 C19 C18 175.5(17) . . . . ?
C16 C17 C110 F112 176(2) . . . . ?
C18 C17 C110 F112 -12(4) . . . . ?
C16 C17 C110 F111 -69(3) . . . . ?
C18 C17 C110 F111 103(3) . . . . ?
C16 C17 C110 F110 47(3) . . . . ?
C18 C17 C110 F110 -140(2) . . . . ?
C25 N21 C21 C23 -6.8(15) . . . . ?
C25 N21 C21 C22 113.9(12) . . . . ?
N21 C21 C22 O22 -168.9(13) . . . . ?
C23 C21 C22 O22 -51.8(19) . . . . ?
N21 C21 C22 N31 15.3(16) . . . . ?
C23 C21 C22 N31 132.4(14) . . . . ?
N21 C21 C23 O23 6.9(15) . . . . ?
C22 C21 C23 O23 -113.1(13) . . . . ?
N21 C21 C23 C24 -107.1(18) . . . . ?
C22 C21 C23 C24 132.9(18) . . . . ?
C21 C23 O23 C25 -4.7(15) . . . . ?
C24 C23 O23 C25 109.2(14) . . . . ?
C21 N21 C25 O23 4.2(16) . . . . ?
C21 N21 C25 C11 -174.8(12) . . . . ?
C23 O23 C25 N21 0.4(16) . . . . ?
C23 O23 C25 C11 179.5(12) . . . . ?
N11 C11 C25 N21 -33(2) . . . . ?
C13 C11 C25 N21 84.6(15) . . . . ?
N11 C11 C25 O23 147.7(12) . . . . ?
C13 C11 C25 O23 -94.5(14) . . . . ?
O22 C22 N31 C31 5(2) . . . . ?
C21 C22 N31 C31 -179.1(12) . . . . ?
C22 N31 C31 C44 131.3(13) . . . . ?
C22 N31 C31 C33 -107.7(14) . . . . ?
N31 C31 C33 C34 65.0(17) . . . . ?
C44 C31 C33 C34 -175.9(13) . . . . ?
N31 C31 C33 C35 -172.4(12) . . . . ?
C44 C31 C33 C35 -53.3(15) . . . . ?
C44 N41 C41 C43 3.5(16) . . . . ?
C44 N41 C41 C42 -178.3(12) . . . . ?
C43 C41 C42 O42 -10(2) . . . . ?
N41 C41 C42 O42 171.5(13) . . . . ?
C43 C41 C42 N51 167.7(13) . . . . ?
N41 C41 C42 N51 -10.3(18) . . . . ?
N41 C41 C43 S43 -3.1(15) . . . . ?
C42 C41 C43 S43 178.7(11) . . . . ?
C41 C43 S43 C44 1.6(11) . . . . ?
C41 N41 C44 C31 -178.5(12) . . . . ?
C41 N41 C44 S43 -2.2(14) . . . . ?
N31 C31 C44 N41 49.1(16) . . . . ?
C33 C31 C44 N41 -73.4(16) . . . . ?
N31 C31 C44 S43 -127.0(10) . . . . ?
C33 C31 C44 S43 110.6(11) . . . . ?
C43 S43 C44 N41 0.4(11) . . . . ?
C43 S43 C44 C31 176.9(12) . . . . ?
O42 C42 N51 C51 1(2) . . . . ?
C41 C42 N51 C51 -176.8(11) . . . . ?
C42 N51 C51 C53 97.6(16) . . . . ?
C42 N51 C51 C65 -132.7(15) . . . . ?
N51 C51 C53 C54 79.9(17) . . . . ?
C65 C51 C53 C54 -47(2) . . . . ?
N51 C51 C53 C55 -156.3(15) . . . . ?
C65 C51 C53 C55 76(2) . . . . ?
C54 C53 C55 C56 -75(3) . . . . ?
C51 C53 C55 C56 164(2) . . . . ?
C65 N61 C61 C62 108(2) . . . . ?
C65 N61 C61 C63 -15(2) . . . . ?
N61 C61 C62 O62 -169.6(16) . . . . ?
C63 C61 C62 O62 -51(2) . . . . ?
N61 C61 C62 N71 17(2) . . . . ?
C63 C61 C62 N71 135.4(17) . . . . ?
N61 C61 C63 O63 14.7(16) . . . . ?
C62 C61 C63 O63 -109.2(15) . . . . ?
N61 C61 C63 C64 -100.2(15) . . . . ?
C62 C61 C63 C64 136.0(15) . . . . ?
C64 C63 O63 C65 108.5(17) . . . . ?
C61 C63 O63 C65 -10.3(17) . . . . ?
C61 N61 C65 O63 9(2) . . . . ?
C61 N61 C65 C51 -174.2(18) . . . . ?
C63 O63 C65 N61 1(2) . . . . ?
C63 O63 C65 C51 -176.0(14) . . . . ?
N51 C51 C65 N61 -22(3) . . . . ?
C53 C51 C65 N61 106(2) . . . . ?
N51 C51 C65 O63 154.7(14) . . . . ?
C53 C51 C65 O63 -77(2) . . . . ?
O62 C62 N71 C71 4(3) . . . . ?
C61 C62 N71 C71 177.0(15) . . . . ?
C62 N71 C71 C84 129.9(19) . . . . ?
C62 N71 C71 C73 -102(2) . . . . ?
N71 C71 C73 C75 -174.7(14) . . . . ?
C84 C71 C73 C75 -50.5(17) . . . . ?
N71 C71 C73 C74 61.2(17) . . . . ?
C84 C71 C73 C74 -174.6(13) . . . . ?
C84 N81 C81 C83 2(3) . . . . ?
C84 N81 C81 C82 175(2) . . . . ?
C11 N11 C82 O82 10(3) . . . . ?
C11 N11 C82 C81 -171.7(19) . . . . ?
C83 C81 C82 O82 -15(4) . . . . ?
N81 C81 C82 O82 172(2) . . . . ?
C83 C81 C82 N11 166(3) . . . . ?
N81 C81 C82 N11 -6(4) . . . . ?
N81 C81 C83 S83 -3(3) . . . . ?
C82 C81 C83 S83 -176(2) . . . . ?
C81 C83 S83 C84 3(2) . . . . ?
C81 N81 C84 C71 175(2) . . . . ?
C81 N81 C84 S83 0(3) . . . . ?
N71 C71 C84 N81 57(3) . . . . ?
C73 C71 C84 N81 -71(3) . . . . ?
N71 C71 C84 S83 -128.4(18) . . . . ?
C73 C71 C84 S83 104(2) . . . . ?
C83 S83 C84 N81 -2(2) . . . . ?
C83 S83 C84 C71 -176(2) . . . . ?

_refine_diff_density_max         0.749
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.106



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetone'
####################################################################### 
# 
# 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_201219_Phetbu
_database_code_depnum_ccdc_archive 'CCDC 2289964'
loop_
_audit_author_name
_audit_author_address
'Akiko Asano'
;Osaka Medical nad Pharmaceutical University
Japan
;
_audit_update_record             
;
2023-08-22 deposited with the CCDC.	2023-12-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        Phe(tbu)_ASC
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C43 H58 N8 O6 S2, C2 H3 N, H2 O'
_chemical_formula_sum            'C45 H63 N9 O7 S2'
_chemical_formula_weight         906.16
_chemical_compound_source        synthesis
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'

_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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'

_cell_length_a                   9.38850(10)
_cell_length_b                   10.0778(2)
_cell_length_c                   13.0183(2)
_cell_angle_alpha                82.6590(10)
_cell_angle_beta                 86.0780(10)
_cell_angle_gamma                80.1310(10)
_cell_volume                     1202.20(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    100
_cell_measurement_reflns_used    13573
_cell_measurement_theta_min      3.4190
_cell_measurement_theta_max      74.2270

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_F_000             484
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    1.473
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.79920
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   CrysAlisPro
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   rotating-anode
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single & P200K'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 5.811
_diffrn_reflns_number            20933
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.427
_diffrn_reflns_theta_max         66.559
_diffrn_reflns_theta_full        66.559
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.908
_diffrn_reflns_point_group_measured_fraction_full 0.908
_reflns_number_total             7685
_reflns_number_gt                7368
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.823
_reflns_Friedel_fraction_max     0.820
_reflns_Friedel_fraction_full    0.820

_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
_computing_cell_refinement       CrysAlisPro
_computing_data_reduction        CrysAlisPro
_computing_structure_solution    SHELXT
_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)+(0.0972P)²+0.2666P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 3119 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.010(7)
_chemical_absolute_configuration rm
_refine_ls_number_reflns         7685
_refine_ls_number_parameters     569
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0462
_refine_ls_wR_factor_ref         0.1343
_refine_ls_wR_factor_gt          0.1315
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.051
_refine_ls_shift/su_max          0.008
_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
N11 N 0.5998(5) 0.7440(4) 0.3617(3) 0.0429(9) Uani 1 1 d . . . . .
H11 H 0.587136 0.662745 0.356035 0.052 Uiso 1 1 calc R U . . .
C11 C 0.5594(5) 0.7971(5) 0.4599(3) 0.0398(10) Uani 1 1 d . . . . .
H11A H 0.568078 0.893482 0.451631 0.048 Uiso 1 1 calc R U . . .
C13 C 0.4001(6) 0.7831(6) 0.4908(4) 0.0510(12) Uani 1 1 d . . . . .
H13A H 0.337755 0.848822 0.445688 0.061 Uiso 1 1 calc R U . . .
H13B H 0.385155 0.693490 0.478827 0.061 Uiso 1 1 calc R U . . .
C14 C 0.3545(5) 0.8032(5) 0.6019(4) 0.0402(10) Uani 1 1 d . . . . .
C15 C 0.3096(5) 0.9293(5) 0.6335(4) 0.0426(10) Uani 1 1 d . . . . .
H15 H 0.306625 1.006108 0.585279 0.051 Uiso 1 1 calc R U . . .
C16 C 0.2684(5) 0.9438(4) 0.7372(4) 0.0403(10) Uani 1 1 d . . . . .
H16 H 0.238016 1.030246 0.756520 0.048 Uiso 1 1 calc R U . . .
C17 C 0.2716(4) 0.8331(4) 0.8114(3) 0.0324(8) Uani 1 1 d . . . . .
C18 C 0.3166(5) 0.7062(4) 0.7785(4) 0.0394(10) Uani 1 1 d . . . . .
H18 H 0.320774 0.629260 0.826749 0.047 Uiso 1 1 calc R U . . .
C19 C 0.3558(5) 0.6914(5) 0.6749(4) 0.0427(10) Uani 1 1 d . . . . .
H19 H 0.383178 0.604998 0.654873 0.051 Uiso 1 1 calc R U . . .
C110 C 0.2235(5) 0.8433(4) 0.9260(4) 0.0376(9) Uani 1 1 d . . . . .
C111 C 0.3431(6) 0.7651(5) 0.9962(4) 0.0495(12) Uani 1 1 d . . . . .
H11B H 0.430323 0.802826 0.980193 0.074 Uiso 1 1 calc R U . . .
H11C H 0.312880 0.772175 1.067462 0.074 Uiso 1 1 calc R U . . .
H11D H 0.360782 0.671343 0.984535 0.074 Uiso 1 1 calc R U . . .
C112 C 0.0850(6) 0.7843(6) 0.9507(4) 0.0523(12) Uani 1 1 d . . . . .
H11E H 0.101140 0.691691 0.936254 0.078 Uiso 1 1 calc R U . . .
H11F H 0.056490 0.788031 1.022624 0.078 Uiso 1 1 calc R U . . .
H11G H 0.009748 0.835872 0.908721 0.078 Uiso 1 1 calc R U . . .
C113 C 0.1926(6) 0.9900(5) 0.9501(4) 0.0503(12) Uani 1 1 d . . . . .
H11H H 0.278482 1.030118 0.935181 0.075 Uiso 1 1 calc R U . . .
H11I H 0.116556 1.040019 0.908112 0.075 Uiso 1 1 calc R U . . .
H11J H 0.163298 0.992177 1.022016 0.075 Uiso 1 1 calc R U . . .
N21 N 0.6959(4) 0.5970(3) 0.5596(3) 0.0347(8) Uani 1 1 d . . . . .
C21 C 0.7877(5) 0.5718(4) 0.6500(3) 0.0313(8) Uani 1 1 d . . . . .
H21 H 0.886650 0.535529 0.627031 0.038 Uiso 1 1 calc R U . . .
C22 C 0.7379(4) 0.4727(4) 0.7358(3) 0.0304(8) Uani 1 1 d . . . . .
O22 O 0.7792(3) 0.4668(3) 0.8246(2) 0.0408(7) Uani 1 1 d . . . . .
C23 C 0.7872(5) 0.7130(4) 0.6850(3) 0.0367(9) Uani 1 1 d . . . . .
H23 H 0.734579 0.718829 0.752307 0.044 Uiso 1 1 calc R U . . .
O23 O 0.7053(3) 0.8043(3) 0.6045(2) 0.0366(7) Uani 1 1 d . . . . .
C24 C 0.9331(6) 0.7502(5) 0.6901(5) 0.0521(13) Uani 1 1 d . . . . .
H24A H 0.985557 0.689837 0.742922 0.078 Uiso 1 1 calc R U . . .
H24B H 0.984918 0.742951 0.624368 0.078 Uiso 1 1 calc R U . . .
H24C H 0.922874 0.841679 0.706405 0.078 Uiso 1 1 calc R U . . .
C25 C 0.6588(5) 0.7230(4) 0.5429(3) 0.0315(8) Uani 1 1 d . . . . .
N31 N 0.6506(4) 0.3923(3) 0.7080(2) 0.0300(7) Uani 1 1 d . . . . .
H31 H 0.627718 0.402554 0.644311 0.036 Uiso 1 1 calc R U . . .
C31 C 0.5925(4) 0.2890(4) 0.7787(3) 0.0307(8) Uani 1 1 d . . . . .
H31A H 0.603246 0.306360 0.849916 0.037 Uiso 1 1 calc R U . . .
C33 C 0.6739(5) 0.1452(4) 0.7644(3) 0.0351(9) Uani 1 1 d . . . . .
H33 H 0.664224 0.128383 0.692957 0.042 Uiso 1 1 calc R U . . .
C34 C 0.6088(6) 0.0389(5) 0.8373(4) 0.0455(11) Uani 1 1 d . . . . .
H34A H 0.508129 0.046007 0.824544 0.068 Uiso 1 1 calc R U . . .
H34B H 0.658492 -0.049823 0.825677 0.068 Uiso 1 1 calc R U . . .
H34C H 0.618685 0.053236 0.907807 0.068 Uiso 1 1 calc R U . . .
C35 C 0.8339(5) 0.1378(5) 0.7819(4) 0.0433(10) Uani 1 1 d . . . . .
H35A H 0.872000 0.205953 0.734931 0.065 Uiso 1 1 calc R U . . .
H35B H 0.845375 0.152832 0.852015 0.065 Uiso 1 1 calc R U . . .
H35C H 0.885182 0.049773 0.769886 0.065 Uiso 1 1 calc R U . . .
N41 N 0.3859(4) 0.3111(3) 0.6669(3) 0.0305(7) Uani 1 1 d . . . . .
C41 C 0.2367(4) 0.3287(4) 0.6709(3) 0.0297(8) Uani 1 1 d . . . . .
C42 C 0.1567(4) 0.3414(4) 0.5739(3) 0.0307(8) Uani 1 1 d . . . . .
O42 O 0.0287(3) 0.3286(3) 0.5777(2) 0.0382(7) Uani 1 1 d . . . . .
C43 C 0.1717(5) 0.3372(4) 0.7663(3) 0.0315(8) Uani 1 1 d . . . . .
H43 H 0.072226 0.349232 0.780535 0.038 Uiso 1 1 calc R U . . .
S43 S 0.29837(10) 0.32290(9) 0.85668(7) 0.0327(2) Uani 1 1 d . . . . .
C44 C 0.4326(4) 0.3052(4) 0.7602(3) 0.0292(8) Uani 1 1 d . . . . .
N51 N 0.2351(4) 0.3684(4) 0.4864(3) 0.0365(8) Uani 1 1 d . . . . .
H51 H 0.325355 0.372360 0.490148 0.044 Uiso 1 1 calc R U . . .
C51 C 0.1725(5) 0.3914(5) 0.3843(3) 0.0374(10) Uani 1 1 d . . . . .
H51A H 0.077382 0.362592 0.392225 0.045 Uiso 1 1 calc R U . . .
C53 C 0.1505(5) 0.5436(5) 0.3405(3) 0.0413(10) Uani 1 1 d . . . . .
H53 H 0.242979 0.576339 0.340282 0.050 Uiso 1 1 calc R U . . .
C54 C 0.1013(7) 0.5624(6) 0.2291(4) 0.0576(14) Uani 1 1 d . . . . .
H54A H 0.172029 0.510502 0.186829 0.086 Uiso 1 1 calc R U . . .
H54B H 0.009993 0.531921 0.228332 0.086 Uiso 1 1 calc R U . . .
H54C H 0.091032 0.656639 0.202169 0.086 Uiso 1 1 calc R U . . .
C55 C 0.0401(7) 0.6250(6) 0.4094(5) 0.0581(13) Uani 1 1 d . . . . .
H55A H 0.070700 0.605607 0.480189 0.070 Uiso 1 1 calc R U . . .
H55B H -0.052129 0.594473 0.407846 0.070 Uiso 1 1 calc R U . . .
C56 C 0.0181(7) 0.7786(6) 0.3790(5) 0.0619(15) Uani 1 1 d . . . . .
H56A H -0.052705 0.822099 0.425992 0.093 Uiso 1 1 calc R U . . .
H56B H 0.108095 0.810661 0.382137 0.093 Uiso 1 1 calc R U . . .
H56C H -0.014941 0.799509 0.309671 0.093 Uiso 1 1 calc R U . . .
N61 N 0.4026(4) 0.2914(4) 0.3020(3) 0.0391(8) Uani 1 1 d . . . . .
C61 C 0.4472(5) 0.2038(4) 0.2186(3) 0.0365(9) Uani 1 1 d . . . . .
H61 H 0.511694 0.122561 0.247350 0.044 Uiso 1 1 calc R U . . .
C62 C 0.5274(5) 0.2739(5) 0.1285(3) 0.0366(9) Uani 1 1 d . . . . .
O62 O 0.5238(4) 0.2434(4) 0.0396(2) 0.0496(8) Uani 1 1 d . . . . .
C63 C 0.3062(5) 0.1607(4) 0.1897(3) 0.0357(9) Uani 1 1 d . . . . .
H63 H 0.291026 0.185706 0.115567 0.043 Uiso 1 1 calc R U . . .
O63 O 0.1957(3) 0.2408(3) 0.2512(2) 0.0401(7) Uani 1 1 d . . . . .
C64 C 0.2999(7) 0.0136(5) 0.2195(5) 0.0561(13) Uani 1 1 d . . . . .
H64A H 0.372285 -0.039619 0.179312 0.084 Uiso 1 1 calc R U . . .
H64B H 0.317297 -0.009925 0.291838 0.084 Uiso 1 1 calc R U . . .
H64C H 0.205896 -0.004092 0.206342 0.084 Uiso 1 1 calc R U . . .
C65 C 0.2664(5) 0.3049(4) 0.3123(3) 0.0336(9) Uani 1 1 d . . . . .
N71 N 0.6084(4) 0.3600(4) 0.1541(3) 0.0343(7) Uani 1 1 d . . . . .
H71 H 0.594403 0.384700 0.215352 0.041 Uiso 1 1 calc R U . . .
C71 C 0.7183(4) 0.4148(5) 0.0862(3) 0.0353(9) Uani 1 1 d . . . . .
H71A H 0.697971 0.409555 0.014103 0.042 Uiso 1 1 calc R U . . .
C73 C 0.8702(5) 0.3314(5) 0.1094(3) 0.0387(10) Uani 1 1 d . . . . .
H73 H 0.894006 0.348155 0.178276 0.046 Uiso 1 1 calc R U . . .
C74 C 0.8723(6) 0.1796(5) 0.1123(5) 0.0526(13) Uani 1 1 d . . . . .
H74A H 0.799049 0.151992 0.161551 0.079 Uiso 1 1 calc R U . . .
H74B H 0.853700 0.159584 0.044765 0.079 Uiso 1 1 calc R U . . .
H74C H 0.965476 0.131494 0.132244 0.079 Uiso 1 1 calc R U . . .
C75 C 0.9849(5) 0.3781(6) 0.0322(4) 0.0479(12) Uani 1 1 d . . . . .
H75A H 0.981832 0.473934 0.031492 0.072 Uiso 1 1 calc R U . . .
H75B H 1.078575 0.330964 0.051762 0.072 Uiso 1 1 calc R U . . .
H75C H 0.966798 0.359054 -0.035717 0.072 Uiso 1 1 calc R U . . .
N81 N 0.6808(4) 0.6060(4) 0.1921(3) 0.0343(8) Uani 1 1 d . . . . .
C81 C 0.6873(4) 0.7413(4) 0.1853(3) 0.0338(9) Uani 1 1 d . . . . .
C82 C 0.6559(4) 0.8151(4) 0.2791(3) 0.0343(9) Uani 1 1 d . . . . .
O82 O 0.6776(4) 0.9311(3) 0.2782(3) 0.0438(8) Uani 1 1 d . . . . .
C83 C 0.7212(5) 0.8018(5) 0.0897(4) 0.0406(10) Uani 1 1 d . . . . .
H83 H 0.729370 0.892884 0.073897 0.049 Uiso 1 1 calc R U . . .
S83 S 0.74662(12) 0.68533(11) 0.00270(8) 0.0415(3) Uani 1 1 d . . . . .
C84 C 0.7107(4) 0.5618(4) 0.1018(3) 0.0339(9) Uani 1 1 d . . . . .
OW O 0.5083(5) 0.4768(5) 0.4322(4) 0.0711(12) Uani 1 1 d . . . . .
N1S N 0.7558(9) 0.2762(8) 0.3794(7) 0.1082(19) Uani 1 1 d . U . . .
C1S C 0.8215(11) 0.1877(10) 0.4295(8) 0.1018(18) Uani 1 1 d . U . . .
C2S C 0.9124(12) 0.0890(10) 0.4926(9) 0.109(2) Uani 1 1 d . U . . .
H2S1 H 0.960561 0.020125 0.451782 0.163 Uiso 1 1 calc R U . . .
H2S2 H 0.855433 0.048689 0.548187 0.163 Uiso 1 1 calc R U . . .
H2S3 H 0.983123 0.130888 0.520656 0.163 Uiso 1 1 calc R U . . .
H1W H 0.579405 0.481160 0.470645 0.163 Uiso 1 1 d . U . . .
H2W H 0.507870 0.415100 0.388391 0.163 Uiso 1 1 d . 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
N11 C82 1.342(6) . ?
N11 C11 1.451(5) . ?
N11 H11 0.8600 . ?
C11 C25 1.513(6) . ?
C11 C13 1.548(7) . ?
C11 H11A 0.9800 . ?
C13 C14 1.509(7) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C15 1.375(7) . ?
C14 C19 1.377(7) . ?
C15 C16 1.397(7) . ?
C15 H15 0.9300 . ?
C16 C17 1.377(6) . ?
C16 H16 0.9300 . ?
C17 C18 1.389(6) . ?
C17 C110 1.540(6) . ?
C18 C19 1.393(7) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
C110 C112 1.519(7) . ?
C110 C113 1.525(7) . ?
C110 C111 1.539(6) . ?
C111 H11B 0.9600 . ?
C111 H11C 0.9600 . ?
C111 H11D 0.9600 . ?
C112 H11E 0.9600 . ?
C112 H11F 0.9600 . ?
C112 H11G 0.9600 . ?
C113 H11H 0.9600 . ?
C113 H11I 0.9600 . ?
C113 H11J 0.9600 . ?
N21 C25 1.253(5) . ?
N21 C21 1.477(5) . ?
C21 C22 1.505(6) . ?
C21 C23 1.547(6) . ?
C21 H21 0.9800 . ?
C22 O22 1.234(5) . ?
C22 N31 1.343(5) . ?
C23 O23 1.469(5) . ?
C23 C24 1.488(7) . ?
C23 H23 0.9800 . ?
O23 C25 1.357(5) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
N31 C31 1.452(5) . ?
N31 H31 0.8600 . ?
C31 C44 1.515(5) . ?
C31 C33 1.545(5) . ?
C31 H31A 0.9800 . ?
C33 C34 1.519(7) . ?
C33 C35 1.522(6) . ?
C33 H33 0.9800 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
N41 C44 1.310(5) . ?
N41 C41 1.379(5) . ?
C41 C43 1.352(6) . ?
C41 C42 1.493(5) . ?
C42 O42 1.228(5) . ?
C42 N51 1.337(6) . ?
C43 S43 1.706(4) . ?
C43 H43 0.9300 . ?
S43 C44 1.721(4) . ?
N51 C51 1.465(5) . ?
N51 H51 0.8600 . ?
C51 C65 1.499(6) . ?
C51 C53 1.551(6) . ?
C51 H51A 0.9800 . ?
C53 C55 1.523(7) . ?
C53 C54 1.531(6) . ?
C53 H53 0.9800 . ?
C54 H54A 0.9600 . ?
C54 H54B 0.9600 . ?
C54 H54C 0.9600 . ?
C55 C56 1.530(8) . ?
C55 H55A 0.9700 . ?
C55 H55B 0.9700 . ?
C56 H56A 0.9600 . ?
C56 H56B 0.9600 . ?
C56 H56C 0.9600 . ?
N61 C65 1.263(6) . ?
N61 C61 1.480(6) . ?
C61 C62 1.513(6) . ?
C61 C63 1.546(6) . ?
C61 H61 0.9800 . ?
C62 O62 1.240(5) . ?
C62 N71 1.333(6) . ?
C63 O63 1.460(5) . ?
C63 C64 1.493(7) . ?
C63 H63 0.9800 . ?
O63 C65 1.357(5) . ?
C64 H64A 0.9600 . ?
C64 H64B 0.9600 . ?
C64 H64C 0.9600 . ?
N71 C71 1.449(6) . ?
N71 H71 0.8600 . ?
C71 C84 1.510(6) . ?
C71 C73 1.553(5) . ?
C71 H71A 0.9800 . ?
C73 C75 1.516(7) . ?
C73 C74 1.523(7) . ?
C73 H73 0.9800 . ?
C74 H74A 0.9600 . ?
C74 H74B 0.9600 . ?
C74 H74C 0.9600 . ?
C75 H75A 0.9600 . ?
C75 H75B 0.9600 . ?
C75 H75C 0.9600 . ?
N81 C84 1.306(5) . ?
N81 C81 1.367(6) . ?
C81 C83 1.356(7) . ?
C81 C82 1.497(6) . ?
C82 O82 1.220(6) . ?
C83 S83 1.710(5) . ?
C83 H83 0.9300 . ?
S83 C84 1.732(5) . ?
OW H1W 0.871(4) . ?
OW H2W 0.897(5) . ?
N1S C1S 1.149(11) . ?
C1S C2S 1.410(13) . ?
C2S H2S1 0.9600 . ?
C2S H2S2 0.9600 . ?
C2S H2S3 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
C82 N11 C11 123.4(4) . . ?
C82 N11 H11 118.3 . . ?
C11 N11 H11 118.3 . . ?
N11 C11 C25 110.5(4) . . ?
N11 C11 C13 109.3(4) . . ?
C25 C11 C13 110.7(4) . . ?
N11 C11 H11A 108.8 . . ?
C25 C11 H11A 108.8 . . ?
C13 C11 H11A 108.8 . . ?
C14 C13 C11 114.7(4) . . ?
C14 C13 H13A 108.6 . . ?
C11 C13 H13A 108.6 . . ?
C14 C13 H13B 108.6 . . ?
C11 C13 H13B 108.6 . . ?
H13A C13 H13B 107.6 . . ?
C15 C14 C19 118.2(4) . . ?
C15 C14 C13 122.6(5) . . ?
C19 C14 C13 119.2(4) . . ?
C14 C15 C16 120.9(4) . . ?
C14 C15 H15 119.5 . . ?
C16 C15 H15 119.5 . . ?
C17 C16 C15 121.6(4) . . ?
C17 C16 H16 119.2 . . ?
C15 C16 H16 119.2 . . ?
C16 C17 C18 117.0(4) . . ?
C16 C17 C110 123.6(4) . . ?
C18 C17 C110 119.3(4) . . ?
C17 C18 C19 121.5(4) . . ?
C17 C18 H18 119.3 . . ?
C19 C18 H18 119.3 . . ?
C14 C19 C18 120.8(4) . . ?
C14 C19 H19 119.6 . . ?
C18 C19 H19 119.6 . . ?
C112 C110 C113 107.6(4) . . ?
C112 C110 C111 109.9(4) . . ?
C113 C110 C111 108.3(4) . . ?
C112 C110 C17 109.4(4) . . ?
C113 C110 C17 111.9(4) . . ?
C111 C110 C17 109.8(4) . . ?
C110 C111 H11B 109.5 . . ?
C110 C111 H11C 109.5 . . ?
H11B C111 H11C 109.5 . . ?
C110 C111 H11D 109.5 . . ?
H11B C111 H11D 109.5 . . ?
H11C C111 H11D 109.5 . . ?
C110 C112 H11E 109.5 . . ?
C110 C112 H11F 109.5 . . ?
H11E C112 H11F 109.5 . . ?
C110 C112 H11G 109.5 . . ?
H11E C112 H11G 109.5 . . ?
H11F C112 H11G 109.5 . . ?
C110 C113 H11H 109.5 . . ?
C110 C113 H11I 109.5 . . ?
H11H C113 H11I 109.5 . . ?
C110 C113 H11J 109.5 . . ?
H11H C113 H11J 109.5 . . ?
H11I C113 H11J 109.5 . . ?
C25 N21 C21 106.3(3) . . ?
N21 C21 C22 113.4(3) . . ?
N21 C21 C23 105.4(3) . . ?
C22 C21 C23 112.6(3) . . ?
N21 C21 H21 108.4 . . ?
C22 C21 H21 108.4 . . ?
C23 C21 H21 108.4 . . ?
O22 C22 N31 123.9(4) . . ?
O22 C22 C21 120.5(4) . . ?
N31 C22 C21 115.6(3) . . ?
O23 C23 C24 110.3(4) . . ?
O23 C23 C21 102.4(3) . . ?
C24 C23 C21 114.9(4) . . ?
O23 C23 H23 109.7 . . ?
C24 C23 H23 109.7 . . ?
C21 C23 H23 109.7 . . ?
C25 O23 C23 106.0(3) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N21 C25 O23 119.7(4) . . ?
N21 C25 C11 125.6(4) . . ?
O23 C25 C11 114.7(3) . . ?
C22 N31 C31 124.1(3) . . ?
C22 N31 H31 117.9 . . ?
C31 N31 H31 117.9 . . ?
N31 C31 C44 107.1(3) . . ?
N31 C31 C33 111.7(3) . . ?
C44 C31 C33 112.6(3) . . ?
N31 C31 H31A 108.5 . . ?
C44 C31 H31A 108.5 . . ?
C33 C31 H31A 108.5 . . ?
C34 C33 C35 111.3(4) . . ?
C34 C33 C31 110.7(4) . . ?
C35 C33 C31 109.5(3) . . ?
C34 C33 H33 108.4 . . ?
C35 C33 H33 108.4 . . ?
C31 C33 H33 108.4 . . ?
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 . . ?
C44 N41 C41 110.2(3) . . ?
C43 C41 N41 115.5(3) . . ?
C43 C41 C42 124.0(4) . . ?
N41 C41 C42 120.5(4) . . ?
O42 C42 N51 124.6(4) . . ?
O42 C42 C41 120.7(4) . . ?
N51 C42 C41 114.7(3) . . ?
C41 C43 S43 110.3(3) . . ?
C41 C43 H43 124.9 . . ?
S43 C43 H43 124.9 . . ?
C43 S43 C44 89.50(19) . . ?
N41 C44 C31 121.5(4) . . ?
N41 C44 S43 114.6(3) . . ?
C31 C44 S43 123.8(3) . . ?
C42 N51 C51 122.2(3) . . ?
C42 N51 H51 118.9 . . ?
C51 N51 H51 118.9 . . ?
N51 C51 C65 109.3(3) . . ?
N51 C51 C53 111.6(4) . . ?
C65 C51 C53 111.8(4) . . ?
N51 C51 H51A 108.0 . . ?
C65 C51 H51A 108.0 . . ?
C53 C51 H51A 108.0 . . ?
C55 C53 C54 110.6(4) . . ?
C55 C53 C51 109.9(4) . . ?
C54 C53 C51 110.3(4) . . ?
C55 C53 H53 108.6 . . ?
C54 C53 H53 108.6 . . ?
C51 C53 H53 108.6 . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C53 C55 C56 114.8(5) . . ?
C53 C55 H55A 108.6 . . ?
C56 C55 H55A 108.6 . . ?
C53 C55 H55B 108.6 . . ?
C56 C55 H55B 108.6 . . ?
H55A C55 H55B 107.6 . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C65 N61 C61 106.5(3) . . ?
N61 C61 C62 112.2(4) . . ?
N61 C61 C63 105.1(3) . . ?
C62 C61 C63 114.3(3) . . ?
N61 C61 H61 108.3 . . ?
C62 C61 H61 108.3 . . ?
C63 C61 H61 108.3 . . ?
O62 C62 N71 124.1(4) . . ?
O62 C62 C61 120.6(4) . . ?
N71 C62 C61 115.1(4) . . ?
O63 C63 C64 109.1(4) . . ?
O63 C63 C61 102.4(3) . . ?
C64 C63 C61 113.9(4) . . ?
O63 C63 H63 110.4 . . ?
C64 C63 H63 110.4 . . ?
C61 C63 H63 110.4 . . ?
C65 O63 C63 106.9(3) . . ?
C63 C64 H64A 109.5 . . ?
C63 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C63 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
N61 C65 O63 118.6(4) . . ?
N61 C65 C51 125.6(4) . . ?
O63 C65 C51 115.8(4) . . ?
C62 N71 C71 124.7(3) . . ?
C62 N71 H71 117.7 . . ?
C71 N71 H71 117.7 . . ?
N71 C71 C84 108.3(3) . . ?
N71 C71 C73 110.2(4) . . ?
C84 C71 C73 111.5(3) . . ?
N71 C71 H71A 108.9 . . ?
C84 C71 H71A 108.9 . . ?
C73 C71 H71A 108.9 . . ?
C75 C73 C74 110.7(4) . . ?
C75 C73 C71 111.0(4) . . ?
C74 C73 C71 112.1(4) . . ?
C75 C73 H73 107.6 . . ?
C74 C73 H73 107.6 . . ?
C71 C73 H73 107.6 . . ?
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 . . ?
C84 N81 C81 110.7(4) . . ?
C83 C81 N81 115.9(4) . . ?
C83 C81 C82 123.6(4) . . ?
N81 C81 C82 120.5(4) . . ?
O82 C82 N11 123.8(4) . . ?
O82 C82 C81 121.8(4) . . ?
N11 C82 C81 114.4(4) . . ?
C81 C83 S83 109.8(4) . . ?
C81 C83 H83 125.1 . . ?
S83 C83 H83 125.1 . . ?
C83 S83 C84 89.4(2) . . ?
N81 C84 C71 122.7(4) . . ?
N81 C84 S83 114.2(3) . . ?
C71 C84 S83 123.1(3) . . ?
H1W OW H2W 125.6(6) . . ?
N1S C1S C2S 173.8(11) . . ?
C1S C2S H2S1 109.5 . . ?
C1S C2S H2S2 109.5 . . ?
H2S1 C2S H2S2 109.5 . . ?
C1S C2S H2S3 109.5 . . ?
H2S1 C2S H2S3 109.5 . . ?
H2S2 C2S H2S3 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
C82 N11 C11 C25 -112.0(5) . . . . ?
C82 N11 C11 C13 125.9(5) . . . . ?
N11 C11 C13 C14 166.2(4) . . . . ?
C25 C11 C13 C14 44.3(6) . . . . ?
C11 C13 C14 C15 83.9(6) . . . . ?
C11 C13 C14 C19 -97.0(6) . . . . ?
C19 C14 C15 C16 0.9(7) . . . . ?
C13 C14 C15 C16 -180.0(4) . . . . ?
C14 C15 C16 C17 0.3(7) . . . . ?
C15 C16 C17 C18 -0.5(7) . . . . ?
C15 C16 C17 C110 -178.4(4) . . . . ?
C16 C17 C18 C19 -0.5(6) . . . . ?
C110 C17 C18 C19 177.5(4) . . . . ?
C15 C14 C19 C18 -1.8(7) . . . . ?
C13 C14 C19 C18 179.0(4) . . . . ?
C17 C18 C19 C14 1.7(7) . . . . ?
C16 C17 C110 C112 111.1(5) . . . . ?
C18 C17 C110 C112 -66.7(5) . . . . ?
C16 C17 C110 C113 -8.0(6) . . . . ?
C18 C17 C110 C113 174.2(4) . . . . ?
C16 C17 C110 C111 -128.2(4) . . . . ?
C18 C17 C110 C111 53.9(5) . . . . ?
C25 N21 C21 C22 126.6(4) . . . . ?
C25 N21 C21 C23 3.0(5) . . . . ?
N21 C21 C22 O22 -161.8(4) . . . . ?
C23 C21 C22 O22 -42.3(5) . . . . ?
N21 C21 C22 N31 19.6(5) . . . . ?
C23 C21 C22 N31 139.1(4) . . . . ?
N21 C21 C23 O23 -4.8(4) . . . . ?
C22 C21 C23 O23 -128.8(4) . . . . ?
N21 C21 C23 C24 -124.3(4) . . . . ?
C22 C21 C23 C24 111.7(5) . . . . ?
C24 C23 O23 C25 127.5(4) . . . . ?
C21 C23 O23 C25 4.8(4) . . . . ?
C21 N21 C25 O23 0.2(5) . . . . ?
C21 N21 C25 C11 -177.7(4) . . . . ?
C23 O23 C25 N21 -3.5(5) . . . . ?
C23 O23 C25 C11 174.6(4) . . . . ?
N11 C11 C25 N21 -46.2(6) . . . . ?
C13 C11 C25 N21 75.0(6) . . . . ?
N11 C11 C25 O23 135.9(4) . . . . ?
C13 C11 C25 O23 -102.9(5) . . . . ?
O22 C22 N31 C31 0.6(6) . . . . ?
C21 C22 N31 C31 179.2(3) . . . . ?
C22 N31 C31 C44 133.3(4) . . . . ?
C22 N31 C31 C33 -103.1(4) . . . . ?
N31 C31 C33 C34 -178.6(3) . . . . ?
C44 C31 C33 C34 -58.1(4) . . . . ?
N31 C31 C33 C35 58.3(4) . . . . ?
C44 C31 C33 C35 178.8(4) . . . . ?
C44 N41 C41 C43 0.6(5) . . . . ?
C44 N41 C41 C42 178.7(3) . . . . ?
C43 C41 C42 O42 -17.4(6) . . . . ?
N41 C41 C42 O42 164.6(4) . . . . ?
C43 C41 C42 N51 162.0(4) . . . . ?
N41 C41 C42 N51 -16.0(5) . . . . ?
N41 C41 C43 S43 -0.1(4) . . . . ?
C42 C41 C43 S43 -178.2(3) . . . . ?
C41 C43 S43 C44 -0.3(3) . . . . ?
C41 N41 C44 C31 -178.8(3) . . . . ?
C41 N41 C44 S43 -0.8(4) . . . . ?
N31 C31 C44 N41 51.1(5) . . . . ?
C33 C31 C44 N41 -72.0(5) . . . . ?
N31 C31 C44 S43 -126.7(3) . . . . ?
C33 C31 C44 S43 110.2(4) . . . . ?
C43 S43 C44 N41 0.6(3) . . . . ?
C43 S43 C44 C31 178.6(3) . . . . ?
O42 C42 N51 C51 2.7(6) . . . . ?
C41 C42 N51 C51 -176.7(4) . . . . ?
C42 N51 C51 C65 -130.3(4) . . . . ?
C42 N51 C51 C53 105.5(5) . . . . ?
N51 C51 C53 C55 -64.2(5) . . . . ?
C65 C51 C53 C55 173.1(4) . . . . ?
N51 C51 C53 C54 173.6(4) . . . . ?
C65 C51 C53 C54 50.8(5) . . . . ?
C54 C53 C55 C56 -62.6(6) . . . . ?
C51 C53 C55 C56 175.3(4) . . . . ?
C65 N61 C61 C62 120.2(4) . . . . ?
C65 N61 C61 C63 -4.5(4) . . . . ?
N61 C61 C62 O62 -151.8(4) . . . . ?
C63 C61 C62 O62 -32.2(6) . . . . ?
N61 C61 C62 N71 33.2(5) . . . . ?
C63 C61 C62 N71 152.8(4) . . . . ?
N61 C61 C63 O63 6.3(4) . . . . ?
C62 C61 C63 O63 -117.2(4) . . . . ?
N61 C61 C63 C64 -111.3(4) . . . . ?
C62 C61 C63 C64 125.2(4) . . . . ?
C64 C63 O63 C65 115.0(4) . . . . ?
C61 C63 O63 C65 -6.0(4) . . . . ?
C61 N61 C65 O63 0.7(5) . . . . ?
C61 N61 C65 C51 -176.6(4) . . . . ?
C63 O63 C65 N61 3.7(5) . . . . ?
C63 O63 C65 C51 -178.7(4) . . . . ?
N51 C51 C65 N61 -45.9(6) . . . . ?
C53 C51 C65 N61 78.2(5) . . . . ?
N51 C51 C65 O63 136.7(4) . . . . ?
C53 C51 C65 O63 -99.2(4) . . . . ?
O62 C62 N71 C71 -9.3(7) . . . . ?
C61 C62 N71 C71 165.5(4) . . . . ?
C62 N71 C71 C84 140.7(4) . . . . ?
C62 N71 C71 C73 -97.1(4) . . . . ?
N71 C71 C73 C75 174.3(4) . . . . ?
C84 C71 C73 C75 -65.4(5) . . . . ?
N71 C71 C73 C74 49.9(5) . . . . ?
C84 C71 C73 C74 170.2(4) . . . . ?
C84 N81 C81 C83 0.4(5) . . . . ?
C84 N81 C81 C82 179.5(4) . . . . ?
C11 N11 C82 O82 -0.5(7) . . . . ?
C11 N11 C82 C81 -179.0(4) . . . . ?
C83 C81 C82 O82 -9.9(6) . . . . ?
N81 C81 C82 O82 171.1(4) . . . . ?
C83 C81 C82 N11 168.7(4) . . . . ?
N81 C81 C82 N11 -10.4(5) . . . . ?
N81 C81 C83 S83 0.0(5) . . . . ?
C82 C81 C83 S83 -179.0(3) . . . . ?
C81 C83 S83 C84 -0.4(3) . . . . ?
C81 N81 C84 C71 177.3(3) . . . . ?
C81 N81 C84 S83 -0.7(4) . . . . ?
N71 C71 C84 N81 36.2(5) . . . . ?
C73 C71 C84 N81 -85.2(5) . . . . ?
N71 C71 C84 S83 -146.0(3) . . . . ?
C73 C71 C84 S83 92.6(4) . . . . ?
C83 S83 C84 N81 0.6(3) . . . . ?
C83 S83 C84 C71 -177.4(3) . . . . ?

_refine_diff_density_max         0.860
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.055



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile'
####################################################################### 
# 
# 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_190823_Phe4Br
_database_code_depnum_ccdc_archive 'CCDC 2289962'
loop_
_audit_author_name
_audit_author_address
'Akiko Asano'
;Osaka Medical nad Pharmaceutical University
Japan
;
_audit_update_record             
;
2023-08-22 deposited with the CCDC.	2023-12-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        Phe(4Br)_ASC
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C39 H49 Br N8 O6 S2),C2 H3 N'
_chemical_formula_sum            'C80 H101 Br2 N17 O12 S4'
_chemical_formula_weight         1780.82
_chemical_compound_source        synthesis
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'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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'

_cell_length_a                   15.64800(10)
_cell_length_b                   16.8169(2)
_cell_length_c                   16.1537(2)
_cell_angle_alpha                90
_cell_angle_beta                 95.6830(10)
_cell_angle_gamma                90
_cell_volume                     4229.97(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    100
_cell_measurement_reflns_used    25771
_cell_measurement_theta_min      3.7450
_cell_measurement_theta_max      74.1980

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_F_000             1860.0
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    2.711
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.93514
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   CrysAlisPro
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   rotating-anode
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single & P200K'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 5.811
_diffrn_reflns_number            33721
_diffrn_reflns_av_unetI/netI     0.0571
_diffrn_reflns_av_R_equivalents  0.0838
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.838
_diffrn_reflns_theta_max         68.247
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.891
_diffrn_reflns_point_group_measured_fraction_full 0.893
_reflns_number_total             13808
_reflns_number_gt                12539
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.749
_reflns_Friedel_fraction_max     0.793
_reflns_Friedel_fraction_full    0.796

_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
_computing_cell_refinement       CrysAlisPro
_computing_data_reduction        CrysAlisPro
_computing_structure_solution    'SHELXT (Sheldrik,2015a)'
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_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 x determined using 4679 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.010(12)
_chemical_absolute_configuration rm
_refine_ls_number_reflns         13808
_refine_ls_number_parameters     1037
_refine_ls_number_restraints     43
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_gt           0.0719
_refine_ls_wR_factor_ref         0.2378
_refine_ls_wR_factor_gt          0.1901
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.070
_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
N1S N 0.2880(6) 0.5698(6) 0.1495(6) 0.044(2) Uani 1 1 d . . . . .
C1S C 0.3461(7) 0.5409(6) 0.1855(6) 0.037(2) Uani 1 1 d . . . . .
C2S C 0.4196(8) 0.5042(9) 0.2320(7) 0.058(3) Uani 1 1 d . . . . .
H2S1 H 0.416360 0.512332 0.290441 0.087 Uiso 1 1 calc R U . . .
H2S2 H 0.471391 0.527832 0.216071 0.087 Uiso 1 1 calc R U . . .
H2S3 H 0.419816 0.448265 0.220355 0.087 Uiso 1 1 calc R U . . .
N11A N 0.2070(4) 0.6666(4) 0.6215(4) 0.0270(14) Uani 1 1 d . . . . .
H11A H 0.231922 0.688027 0.581964 0.032 Uiso 1 1 calc R U . . .
C11A C 0.1198(6) 0.6912(6) 0.6372(6) 0.0321(19) Uani 1 1 d . . . . .
H11B H 0.118116 0.697379 0.697348 0.038 Uiso 1 1 calc R U . . .
C13A C 0.0997(6) 0.7726(6) 0.5951(6) 0.036(2) Uani 1 1 d . . . . .
H13A H 0.145360 0.809927 0.612214 0.044 Uiso 1 1 calc R U . . .
H13B H 0.096781 0.766715 0.535159 0.044 Uiso 1 1 calc R U . . .
C14A C 0.0151(6) 0.8044(6) 0.6192(6) 0.0334(19) Uani 1 1 d . . . . .
C15A C -0.0601(6) 0.7923(6) 0.5663(6) 0.038(2) Uani 1 1 d . . . . .
H15A H -0.057409 0.767450 0.515211 0.045 Uiso 1 1 calc R U . . .
C16A C -0.1396(6) 0.8175(6) 0.5900(6) 0.036(2) Uani 1 1 d . . . . .
H16A H -0.189603 0.810669 0.554527 0.043 Uiso 1 1 calc R U . . .
C17A C -0.1423(5) 0.8525(6) 0.6665(6) 0.0318(18) Uani 1 1 d . . . . .
C18A C -0.0687(6) 0.8665(6) 0.7190(6) 0.038(2) Uani 1 1 d . . . . .
H18A H -0.071675 0.892941 0.769150 0.046 Uiso 1 1 calc R U . . .
C19A C 0.0096(6) 0.8406(6) 0.6958(6) 0.038(2) Uani 1 1 d . . . . .
H19A H 0.059108 0.847519 0.731996 0.046 Uiso 1 1 calc R U . . .
Br01 Br -0.24824(6) 0.88745(6) 0.70050(7) 0.0422(3) Uani 1 1 d . . . . .
N21A N 0.0143(4) 0.5860(5) 0.6535(5) 0.0339(17) Uani 1 1 d . . . . .
C21A C -0.0289(6) 0.5232(6) 0.6004(6) 0.038(2) Uani 1 1 d . . . . .
H21A H -0.090119 0.520244 0.608447 0.045 Uiso 1 1 calc R U . . .
C22A C 0.0151(6) 0.4403(7) 0.6153(6) 0.039(2) Uani 1 1 d . . . . .
O22A O -0.0204(4) 0.3825(5) 0.5845(5) 0.0515(19) Uani 1 1 d . . . . .
C23A C -0.0162(7) 0.5498(7) 0.5104(7) 0.044(2) Uani 1 1 d . . . . .
H23A H 0.003914 0.505392 0.478093 0.053 Uiso 1 1 calc R U . . .
O23A O 0.0502(4) 0.6114(5) 0.5237(4) 0.0355(14) Uani 1 1 d . . . . .
C24A C -0.0972(8) 0.5871(10) 0.4658(8) 0.064(4) Uani 1 1 d . . . . .
H24A H -0.141081 0.547275 0.456773 0.096 Uiso 1 1 calc R U . . .
H24B H -0.116906 0.629033 0.499474 0.096 Uiso 1 1 calc R U . . .
H24C H -0.084407 0.608342 0.413301 0.096 Uiso 1 1 calc R U . . .
C25A C 0.0570(5) 0.6264(6) 0.6069(5) 0.034(2) Uani 1 1 d . . . . .
N31A N 0.0919(4) 0.4416(5) 0.6588(5) 0.0320(16) Uani 1 1 d . . . . .
H31A H 0.106051 0.480862 0.691480 0.038 Uiso 1 1 calc R U . . .
C31A C 0.1510(6) 0.3771(6) 0.6512(6) 0.039(2) Uani 1 1 d . . . . .
H31B H 0.119093 0.337006 0.616658 0.047 Uiso 1 1 calc R U . . .
C33A C 0.1816(6) 0.3347(6) 0.7340(7) 0.043(2) Uani 1 1 d . . . . .
H33A H 0.221591 0.292629 0.721397 0.051 Uiso 1 1 calc R U . . .
C34A C 0.2288(8) 0.3894(8) 0.7983(6) 0.052(3) Uani 1 1 d . . . . .
H34A H 0.276776 0.413328 0.775162 0.077 Uiso 1 1 calc R U . . .
H34B H 0.190437 0.430176 0.813614 0.077 Uiso 1 1 calc R U . . .
H34C H 0.248971 0.359076 0.846723 0.077 Uiso 1 1 calc R U . . .
C35A C 0.1052(9) 0.2952(8) 0.7671(9) 0.058(3) Uani 1 1 d . . . . .
H35A H 0.077078 0.261324 0.725022 0.088 Uiso 1 1 calc R U . . .
H35B H 0.124222 0.264066 0.815247 0.088 Uiso 1 1 calc R U . . .
H35C H 0.065688 0.335165 0.782138 0.088 Uiso 1 1 calc R U . . .
N41A N 0.2137(5) 0.4660(5) 0.5498(4) 0.0320(16) Uani 1 1 d . . . . .
C41A C 0.2864(5) 0.4735(6) 0.5078(6) 0.0323(19) Uani 1 1 d . . . . .
C42A C 0.2941(6) 0.5375(5) 0.4455(5) 0.0299(18) Uani 1 1 d . . . . .
O42A O 0.3625(4) 0.5462(4) 0.4133(4) 0.0298(12) Uani 1 1 d . . . . .
C43A C 0.3505(6) 0.4178(6) 0.5258(6) 0.0327(18) Uani 1 1 d . . . . .
H43A H 0.401634 0.414496 0.501096 0.039 Uiso 1 1 calc R U . . .
S43A S 0.31925(14) 0.35582(14) 0.60184(14) 0.0350(5) Uani 1 1 d . . . . .
C44A C 0.2209(6) 0.4060(6) 0.6009(6) 0.0318(18) Uani 1 1 d . . . . .
N51A N 0.2233(5) 0.5825(4) 0.4250(4) 0.0287(15) Uani 1 1 d . . . . .
H51A H 0.178627 0.577244 0.451462 0.034 Uiso 1 1 calc R U . . .
C51A C 0.2239(5) 0.6400(6) 0.3571(5) 0.0304(18) Uani 1 1 d . . . . .
H51B H 0.254813 0.615794 0.313654 0.036 Uiso 1 1 calc R U . . .
C53A C 0.1321(5) 0.6589(6) 0.3185(5) 0.0299(18) Uani 1 1 d . . . . .
H53A H 0.098299 0.678820 0.362080 0.036 Uiso 1 1 calc R U . . .
C54A C 0.1368(6) 0.7238(7) 0.2515(6) 0.039(2) Uani 1 1 d . . . . .
H54A H 0.162668 0.770815 0.276619 0.059 Uiso 1 1 calc R U . . .
H54B H 0.170771 0.704901 0.209217 0.059 Uiso 1 1 calc R U . . .
H54C H 0.079911 0.735970 0.226982 0.059 Uiso 1 1 calc R U . . .
C55A C 0.0912(5) 0.5816(6) 0.2825(6) 0.035(2) Uani 1 1 d . . . . .
H55A H 0.090850 0.542722 0.326734 0.043 Uiso 1 1 calc R U . . .
H55B H 0.126453 0.560675 0.241400 0.043 Uiso 1 1 calc R U . . .
C56A C -0.0012(6) 0.5925(7) 0.2415(7) 0.043(2) Uani 1 1 d . . . . .
H56A H -0.022962 0.542303 0.220323 0.065 Uiso 1 1 calc R U . . .
H56B H -0.036991 0.611959 0.282039 0.065 Uiso 1 1 calc R U . . .
H56C H -0.001360 0.629926 0.196638 0.065 Uiso 1 1 calc R U . . .
N61A N 0.3428(4) 0.7365(5) 0.3601(4) 0.0284(15) Uani 1 1 d . . . . .
C61A C 0.3749(5) 0.8015(5) 0.4152(5) 0.0292(18) Uani 1 1 d . . . . .
H61A H 0.390949 0.847103 0.382196 0.035 Uiso 1 1 calc R U . . .
C62A C 0.4522(5) 0.7749(6) 0.4755(6) 0.0317(19) Uani 1 1 d . . . . .
O62A O 0.4874(4) 0.8227(4) 0.5238(4) 0.0368(15) Uani 1 1 d . . . . .
C63A C 0.2987(5) 0.8238(6) 0.4644(5) 0.0293(17) Uani 1 1 d . . . . .
H63A H 0.317722 0.831901 0.523419 0.035 Uiso 1 1 calc R U . . .
O63A O 0.2452(4) 0.7514(4) 0.4521(3) 0.0291(12) Uani 1 1 d . . . . .
C64A C 0.2484(6) 0.8939(6) 0.4290(6) 0.039(2) Uani 1 1 d . . . . .
H64A H 0.282887 0.941033 0.436786 0.058 Uiso 1 1 calc R U . . .
H64B H 0.232865 0.885615 0.370630 0.058 Uiso 1 1 calc R U . . .
H64C H 0.197414 0.899916 0.456833 0.058 Uiso 1 1 calc R U . . .
C65A C 0.2732(5) 0.7132(5) 0.3881(5) 0.0257(16) Uani 1 1 d . . . . .
N71A N 0.4726(4) 0.6965(5) 0.4736(4) 0.0286(15) Uani 1 1 d . . . . .
H71A H 0.457100 0.668369 0.430264 0.034 Uiso 1 1 calc R U . . .
C71A C 0.5208(5) 0.6607(6) 0.5457(5) 0.0295(17) Uani 1 1 d . . . . .
H71B H 0.545763 0.704280 0.580416 0.035 Uiso 1 1 calc R U . . .
C73A C 0.5973(5) 0.6065(6) 0.5234(5) 0.0337(19) Uani 1 1 d . . . . .
H73A H 0.620316 0.579752 0.574783 0.040 Uiso 1 1 calc R U . . .
C74A C 0.5694(6) 0.5424(7) 0.4609(6) 0.039(2) Uani 1 1 d . . . . .
H74A H 0.524716 0.511054 0.481360 0.058 Uiso 1 1 calc R U . . .
H74B H 0.548175 0.566611 0.409034 0.058 Uiso 1 1 calc R U . . .
H74C H 0.617438 0.508942 0.452506 0.058 Uiso 1 1 calc R U . . .
C75A C 0.6672(7) 0.6587(8) 0.4965(7) 0.049(3) Uani 1 1 d . . . . .
H75A H 0.682290 0.698030 0.538436 0.073 Uiso 1 1 calc R U . . .
H75B H 0.716712 0.626826 0.488612 0.073 Uiso 1 1 calc R U . . .
H75C H 0.647449 0.684495 0.445140 0.073 Uiso 1 1 calc R U . . .
N81A N 0.3782(4) 0.6411(4) 0.5989(4) 0.0264(14) Uani 1 1 d . . . . .
C81A C 0.3392(5) 0.5954(5) 0.6546(5) 0.0275(17) Uani 1 1 d . . . . .
C82A C 0.2476(5) 0.6099(5) 0.6701(5) 0.0258(16) Uani 1 1 d . . . . .
O82A O 0.2146(4) 0.5746(4) 0.7242(4) 0.0333(13) Uani 1 1 d . . . . .
C83A C 0.3888(6) 0.5371(6) 0.6955(6) 0.0334(19) Uani 1 1 d . . . . .
H83A H 0.370741 0.502356 0.735082 0.040 Uiso 1 1 calc R U . . .
S83A S 0.48854(12) 0.53911(13) 0.66188(13) 0.0289(4) Uani 1 1 d . . . . .
C84A C 0.4571(5) 0.6177(5) 0.5959(5) 0.0272(17) Uani 1 1 d . . . . .
N11B N 0.7027(4) 0.3572(5) 0.8666(5) 0.0316(16) Uani 1 1 d . . . . .
H11C H 0.733402 0.332836 0.905840 0.038 Uiso 1 1 calc R U . . .
C11B C 0.6123(5) 0.3333(5) 0.8442(6) 0.0317(19) Uani 1 1 d . . . . .
H11D H 0.601434 0.333119 0.783369 0.038 Uiso 1 1 calc R U . . .
C13B C 0.5972(7) 0.2492(7) 0.8757(7) 0.0444(16) Uani 1 1 d . U . . .
H13C H 0.639728 0.213802 0.855951 0.053 Uiso 1 1 calc R U . . .
H13D H 0.605262 0.249239 0.935979 0.053 Uiso 1 1 calc R U . . .
C14B C 0.5084(7) 0.2174(7) 0.8477(6) 0.0446(13) Uani 1 1 d . U . . .
C15B C 0.4439(7) 0.2116(8) 0.9022(7) 0.0483(14) Uani 1 1 d . U . . .
H15B H 0.455331 0.229210 0.956750 0.058 Uiso 1 1 calc R U . . .
C16B C 0.3636(7) 0.1803(8) 0.8766(7) 0.0494(14) Uani 1 1 d . U . . .
H16B H 0.321235 0.176266 0.912906 0.059 Uiso 1 1 calc R U . . .
C17B C 0.3492(7) 0.1555(8) 0.7960(6) 0.0458(14) Uani 1 1 d . U . . .
C18B C 0.4068(7) 0.1664(8) 0.7411(7) 0.0477(14) Uani 1 1 d . U . . .
H18B H 0.392790 0.152722 0.685647 0.057 Uiso 1 1 calc R U . . .
C19B C 0.4865(7) 0.1976(7) 0.7657(7) 0.0466(14) Uani 1 1 d . U . . .
H19B H 0.525800 0.205313 0.726846 0.056 Uiso 1 1 calc R U . . .
Br02 Br 0.23992(6) 0.10892(7) 0.76196(7) 0.0464(3) Uani 1 1 d . . . . .
N21B N 0.5051(4) 0.4410(4) 0.8345(4) 0.0266(14) Uani 1 1 d . . . . .
C21B C 0.4689(5) 0.4956(6) 0.8933(5) 0.0312(18) Uani 1 1 d . . . . .
H21B H 0.406499 0.499719 0.880435 0.037 Uiso 1 1 calc R U . . .
C22B C 0.5101(5) 0.5785(5) 0.8933(5) 0.0289(17) Uani 1 1 d . . . . .
O22B O 0.4784(4) 0.6334(4) 0.9287(5) 0.0426(16) Uani 1 1 d . . . . .
C23B C 0.4906(6) 0.4564(6) 0.9801(6) 0.037(2) Uani 1 1 d . . . . .
H23B H 0.513679 0.496040 1.020888 0.044 Uiso 1 1 calc R U . . .
O23B O 0.5570(4) 0.3998(4) 0.9629(4) 0.0325(13) Uani 1 1 d . . . . .
C24B C 0.4154(6) 0.4142(8) 1.0105(7) 0.049(3) Uani 1 1 d . . . . .
H24D H 0.372305 0.452373 1.021554 0.074 Uiso 1 1 calc R U . . .
H24E H 0.391910 0.377488 0.968814 0.074 Uiso 1 1 calc R U . . .
H24F H 0.433748 0.385780 1.060675 0.074 Uiso 1 1 calc R U . . .
C25B C 0.5530(6) 0.3948(6) 0.8784(5) 0.0321(18) Uani 1 1 d . . . . .
N31B N 0.5855(4) 0.5842(5) 0.8585(5) 0.0302(15) Uani 1 1 d . . . . .
H31C H 0.597504 0.549724 0.822039 0.036 Uiso 1 1 calc R U . . .
C31B C 0.6467(6) 0.6481(5) 0.8821(6) 0.0311(18) Uani 1 1 d . . . . .
H31D H 0.618296 0.683120 0.919463 0.037 Uiso 1 1 calc R U . . .
C33B C 0.6683(6) 0.7003(6) 0.8091(6) 0.0349(19) Uani 1 1 d . . . . .
H33B H 0.708145 0.741758 0.831330 0.042 Uiso 1 1 calc R U . . .
C34B C 0.7108(6) 0.6551(6) 0.7434(6) 0.038(2) Uani 1 1 d . . . . .
H34D H 0.762114 0.629951 0.768460 0.057 Uiso 1 1 calc R U . . .
H34E H 0.672109 0.615270 0.719115 0.057 Uiso 1 1 calc R U . . .
H34F H 0.725275 0.691222 0.700985 0.057 Uiso 1 1 calc R U . . .
C35B C 0.5868(7) 0.7408(6) 0.7717(6) 0.039(2) Uani 1 1 d . . . . .
H35D H 0.560912 0.769103 0.814377 0.059 Uiso 1 1 calc R U . . .
H35E H 0.600532 0.777476 0.729387 0.059 Uiso 1 1 calc R U . . .
H35F H 0.547366 0.701524 0.747517 0.059 Uiso 1 1 calc R U . . .
N41B N 0.7198(5) 0.5462(4) 0.9758(4) 0.0282(14) Uani 1 1 d . . . . .
C41B C 0.7969(5) 0.5327(5) 1.0223(5) 0.0257(16) Uani 1 1 d . . . . .
C42B C 0.8085(5) 0.4633(5) 1.0784(5) 0.0252(16) Uani 1 1 d . . . . .
O42B O 0.8767(4) 0.4505(4) 1.1217(4) 0.0304(13) Uani 1 1 d . . . . .
C43B C 0.8568(6) 0.5893(5) 1.0162(5) 0.0318(18) Uani 1 1 d . . . . .
H43B H 0.911057 0.588699 1.045453 0.038 Uiso 1 1 calc R U . . .
S43B S 0.82073(13) 0.66158(13) 0.94868(14) 0.0316(5) Uani 1 1 d . . . . .
C44B C 0.7234(6) 0.6133(6) 0.9337(5) 0.0300(17) Uani 1 1 d . . . . .
N51B N 0.7392(4) 0.4171(4) 1.0809(4) 0.0283(15) Uani 1 1 d . . . . .
H51C H 0.692958 0.427219 1.049371 0.034 Uiso 1 1 calc R U . . .
C51B C 0.7431(5) 0.3491(5) 1.1379(5) 0.0256(16) Uani 1 1 d . . . . .
H51D H 0.773500 0.366225 1.190802 0.031 Uiso 1 1 calc R U . . .
C53B C 0.6519(5) 0.3233(5) 1.1550(5) 0.0273(17) Uani 1 1 d . . . . .
H53B H 0.619608 0.311213 1.101411 0.033 Uiso 1 1 calc R U . . .
C54B C 0.6575(6) 0.2468(6) 1.2068(6) 0.036(2) Uani 1 1 d . . . . .
H54D H 0.600858 0.230575 1.217545 0.054 Uiso 1 1 calc R U . . .
H54E H 0.683590 0.205600 1.176672 0.054 Uiso 1 1 calc R U . . .
H54F H 0.691662 0.256227 1.258562 0.054 Uiso 1 1 calc R U . . .
C55B C 0.6041(5) 0.3902(6) 1.1966(5) 0.0319(18) Uani 1 1 d . . . . .
H55C H 0.607074 0.438252 1.163835 0.038 Uiso 1 1 calc R U . . .
H55D H 0.544017 0.375524 1.195559 0.038 Uiso 1 1 calc R U . . .
C56B C 0.6381(8) 0.4083(7) 1.2852(7) 0.050(3) Uani 1 1 d . . . . .
H56D H 0.604910 0.450341 1.306269 0.075 Uiso 1 1 calc R U . . .
H56E H 0.633914 0.361556 1.318696 0.075 Uiso 1 1 calc R U . . .
H56F H 0.697079 0.424392 1.286917 0.075 Uiso 1 1 calc R U . . .
N61B N 0.8665(5) 0.2606(4) 1.1354(4) 0.0273(14) Uani 1 1 d . . . . .
C61B C 0.8976(5) 0.2037(5) 1.0754(5) 0.0279(17) Uani 1 1 d . . . . .
H61B H 0.922652 0.156950 1.104802 0.033 Uiso 1 1 calc R U . . .
C62B C 0.9638(5) 0.2413(5) 1.0213(6) 0.0295(18) Uani 1 1 d . . . . .
O62B O 0.9904(4) 0.2002(4) 0.9689(4) 0.0366(14) Uani 1 1 d . . . . .
C63B C 0.8140(5) 0.1798(5) 1.0207(5) 0.0256(16) Uani 1 1 d . . . . .
H63B H 0.824508 0.173814 0.962237 0.031 Uiso 1 1 calc R U . . .
O63B O 0.7584(3) 0.2492(4) 1.0323(4) 0.0268(12) Uani 1 1 d . . . . .
C64B C 0.7703(6) 0.1068(6) 1.0517(6) 0.0352(19) Uani 1 1 d . . . . .
H64D H 0.805272 0.060787 1.044801 0.053 Uiso 1 1 calc R U . . .
H64E H 0.762627 0.113279 1.109573 0.053 Uiso 1 1 calc R U . . .
H64F H 0.715343 0.099900 1.020498 0.053 Uiso 1 1 calc R U . . .
C65B C 0.7941(5) 0.2833(5) 1.1041(5) 0.0248(16) Uani 1 1 d . . . . .
N71B N 0.9834(5) 0.3183(5) 1.0357(4) 0.0287(15) Uani 1 1 d . . . . .
H71C H 0.971956 0.340820 1.081068 0.034 Uiso 1 1 calc R U . . .
C71B C 1.0241(6) 0.3625(5) 0.9736(5) 0.0296(18) Uani 1 1 d . . . . .
H71D H 1.050118 0.322918 0.939263 0.036 Uiso 1 1 calc R U . . .
C73B C 1.0969(6) 0.4173(5) 1.0081(5) 0.0296(17) Uani 1 1 d . . . . .
H73B H 1.119754 0.442185 0.960034 0.035 Uiso 1 1 calc R U . . .
C74B C 1.1707(5) 0.3700(6) 1.0536(6) 0.035(2) Uani 1 1 d . . . . .
H74D H 1.215500 0.405782 1.074574 0.052 Uiso 1 1 calc R U . . .
H74E H 1.150086 0.341367 1.099043 0.052 Uiso 1 1 calc R U . . .
H74F H 1.192881 0.333065 1.015731 0.052 Uiso 1 1 calc R U . . .
C75B C 1.0700(6) 0.4850(6) 1.0633(6) 0.0334(19) Uani 1 1 d . . . . .
H75D H 1.119453 0.516325 1.082165 0.050 Uiso 1 1 calc R U . . .
H75E H 1.028433 0.517952 1.031992 0.050 Uiso 1 1 calc R U . . .
H75F H 1.045323 0.463192 1.110444 0.050 Uiso 1 1 calc R U . . .
N81B N 0.8759(4) 0.3833(5) 0.9074(4) 0.0287(14) Uani 1 1 d . . . . .
C81B C 0.8309(5) 0.4294(6) 0.8475(5) 0.0306(18) Uani 1 1 d . . . . .
C82B C 0.7364(5) 0.4165(6) 0.8257(6) 0.0312(19) Uani 1 1 d . . . . .
O82B O 0.6960(4) 0.4574(4) 0.7724(4) 0.0335(13) Uani 1 1 d . . . . .
C83B C 0.8763(5) 0.4856(6) 0.8102(6) 0.0342(19) Uani 1 1 d . . . . .
H83B H 0.853978 0.520276 0.768686 0.041 Uiso 1 1 calc R U . . .
S83B S 0.98192(14) 0.48214(14) 0.85224(14) 0.0349(5) Uani 1 1 d . . . . .
C84B C 0.9560(6) 0.4046(5) 0.9167(5) 0.0310(18) Uani 1 1 d . . . . .


_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
N1S C1S 1.139(14) . ?
C1S C2S 1.447(15) . ?
C2S H2S1 0.9600 . ?
C2S H2S2 0.9600 . ?
C2S H2S3 0.9600 . ?
N11A C82A 1.352(11) . ?
N11A C11A 1.472(10) . ?
N11A H11A 0.8600 . ?
C11A C25A 1.515(13) . ?
C11A C13A 1.548(14) . ?
C11A H11B 0.9800 . ?
C13A C14A 1.514(12) . ?
C13A H13A 0.9700 . ?
C13A H13B 0.9700 . ?
C14A C19A 1.390(14) . ?
C14A C15A 1.399(13) . ?
C15A C16A 1.403(14) . ?
C15A H15A 0.9300 . ?
C16A C17A 1.372(14) . ?
C16A H16A 0.9300 . ?
C17A C18A 1.381(12) . ?
C17A Br01 1.891(9) . ?
C18A C19A 1.387(14) . ?
C18A H18A 0.9300 . ?
C19A H19A 0.9300 . ?
N21A C25A 1.255(13) . ?
N21A C21A 1.480(12) . ?
C21A C23A 1.554(15) . ?
C21A C22A 1.563(15) . ?
C21A H21A 0.9800 . ?
C22A O22A 1.203(13) . ?
C22A N31A 1.330(12) . ?
C23A O23A 1.468(13) . ?
C23A C24A 1.529(15) . ?
C23A H23A 0.9800 . ?
O23A C25A 1.361(11) . ?
C24A H24A 0.9600 . ?
C24A H24B 0.9600 . ?
C24A H24C 0.9600 . ?
N31A C31A 1.440(12) . ?
N31A H31A 0.8600 . ?
C31A C44A 1.506(13) . ?
C31A C33A 1.550(15) . ?
C31A H31B 0.9800 . ?
C33A C35A 1.510(15) . ?
C33A C34A 1.522(16) . ?
C33A H33A 0.9800 . ?
C34A H34A 0.9600 . ?
C34A H34B 0.9600 . ?
C34A H34C 0.9600 . ?
C35A H35A 0.9600 . ?
C35A H35B 0.9600 . ?
C35A H35C 0.9600 . ?
N41A C44A 1.301(12) . ?
N41A C41A 1.387(12) . ?
C41A C43A 1.383(13) . ?
C41A C42A 1.485(13) . ?
C42A O42A 1.244(11) . ?
C42A N51A 1.356(12) . ?
C43A S43A 1.719(10) . ?
C43A H43A 0.9300 . ?
S43A C44A 1.754(9) . ?
N51A C51A 1.462(11) . ?
N51A H51A 0.8600 . ?
C51A C65A 1.512(12) . ?
C51A C53A 1.541(11) . ?
C51A H51B 0.9800 . ?
C53A C55A 1.537(13) . ?
C53A C54A 1.545(14) . ?
C53A H53A 0.9800 . ?
C54A H54A 0.9600 . ?
C54A H54B 0.9600 . ?
C54A H54C 0.9600 . ?
C55A C56A 1.541(11) . ?
C55A H55A 0.9700 . ?
C55A H55B 0.9700 . ?
C56A H56A 0.9600 . ?
C56A H56B 0.9600 . ?
C56A H56C 0.9600 . ?
N61A C65A 1.282(11) . ?
N61A C61A 1.468(11) . ?
C61A C62A 1.542(11) . ?
C61A C63A 1.544(12) . ?
C61A H61A 0.9800 . ?
C62A O62A 1.214(11) . ?
C62A N71A 1.357(13) . ?
C63A O63A 1.479(10) . ?
C63A C64A 1.499(13) . ?
C63A H63A 0.9800 . ?
O63A C65A 1.328(11) . ?
C64A H64A 0.9600 . ?
C64A H64B 0.9600 . ?
C64A H64C 0.9600 . ?
N71A C71A 1.454(10) . ?
N71A H71A 0.8600 . ?
C71A C84A 1.528(12) . ?
C71A C73A 1.575(12) . ?
C71A H71B 0.9800 . ?
C73A C75A 1.500(14) . ?
C73A C74A 1.512(14) . ?
C73A H73A 0.9800 . ?
C74A H74A 0.9600 . ?
C74A H74B 0.9600 . ?
C74A H74C 0.9600 . ?
C75A H75A 0.9600 . ?
C75A H75B 0.9600 . ?
C75A H75C 0.9600 . ?
N81A C84A 1.302(11) . ?
N81A C81A 1.371(11) . ?
C81A C83A 1.378(12) . ?
C81A C82A 1.499(10) . ?
C82A O82A 1.214(11) . ?
C83A S83A 1.703(10) . ?
C83A H83A 0.9300 . ?
S83A C84A 1.738(9) . ?
N11B C82B 1.334(13) . ?
N11B C11B 1.480(10) . ?
N11B H11C 0.8600 . ?
C11B C25B 1.529(13) . ?
C11B C13B 1.530(14) . ?
C11B H11D 0.9800 . ?
C13B C14B 1.516(13) . ?
C13B H13C 0.9700 . ?
C13B H13D 0.9700 . ?
C14B C19B 1.375(14) . ?
C14B C15B 1.407(16) . ?
C15B C16B 1.387(14) . ?
C15B H15B 0.9300 . ?
C16B C17B 1.363(15) . ?
C16B H16B 0.9300 . ?
C17B C18B 1.339(16) . ?
C17B Br02 1.912(10) . ?
C18B C19B 1.375(14) . ?
C18B H18B 0.9300 . ?
C19B H19B 0.9300 . ?
N21B C25B 1.250(11) . ?
N21B C21B 1.475(12) . ?
C21B C22B 1.535(12) . ?
C21B C23B 1.556(12) . ?
C21B H21B 0.9800 . ?
C22B O22B 1.218(12) . ?
C22B N31B 1.361(11) . ?
C23B O23B 1.456(12) . ?
C23B C24B 1.498(15) . ?
C23B H23B 0.9800 . ?
O23B C25B 1.363(11) . ?
C24B H24D 0.9600 . ?
C24B H24E 0.9600 . ?
C24B H24F 0.9600 . ?
N31B C31B 1.465(11) . ?
N31B H31C 0.8600 . ?
C31B C44B 1.509(12) . ?
C31B C33B 1.534(12) . ?
C31B H31D 0.9800 . ?
C33B C34B 1.513(14) . ?
C33B C35B 1.518(14) . ?
C33B H33B 0.9800 . ?
C34B H34D 0.9600 . ?
C34B H34E 0.9600 . ?
C34B H34F 0.9600 . ?
C35B H35D 0.9600 . ?
C35B H35E 0.9600 . ?
C35B H35F 0.9600 . ?
N41B C44B 1.321(12) . ?
N41B C41B 1.376(10) . ?
C41B C43B 1.345(13) . ?
C41B C42B 1.478(11) . ?
C42B O42B 1.236(10) . ?
C42B N51B 1.337(11) . ?
C43B S43B 1.693(9) . ?
C43B H43B 0.9300 . ?
S43B C44B 1.722(9) . ?
N51B C51B 1.466(11) . ?
N51B H51C 0.8600 . ?
C51B C65B 1.499(12) . ?
C51B C53B 1.541(11) . ?
C51B H51D 0.9800 . ?
C53B C54B 1.532(12) . ?
C53B C55B 1.542(13) . ?
C53B H53B 0.9800 . ?
C54B H54D 0.9600 . ?
C54B H54E 0.9600 . ?
C54B H54F 0.9600 . ?
C55B C56B 1.507(13) . ?
C55B H55C 0.9700 . ?
C55B H55D 0.9700 . ?
C56B H56D 0.9600 . ?
C56B H56E 0.9600 . ?
C56B H56F 0.9600 . ?
N61B C65B 1.255(11) . ?
N61B C61B 1.479(11) . ?
C61B C62B 1.553(12) . ?
C61B C63B 1.557(10) . ?
C61B H61B 0.9800 . ?
C62B O62B 1.200(11) . ?
C62B N71B 1.346(12) . ?
C63B O63B 1.478(10) . ?
C63B C64B 1.515(12) . ?
C63B H63B 0.9800 . ?
O63B C65B 1.362(10) . ?
C64B H64D 0.9600 . ?
C64B H64E 0.9600 . ?
C64B H64F 0.9600 . ?
N71B C71B 1.446(12) . ?
N71B H71C 0.8600 . ?
C71B C84B 1.513(12) . ?
C71B C73B 1.527(12) . ?
C71B H71D 0.9800 . ?
C73B C74B 1.529(11) . ?
C73B C75B 1.531(12) . ?
C73B H73B 0.9800 . ?
C74B H74D 0.9600 . ?
C74B H74E 0.9600 . ?
C74B H74F 0.9600 . ?
C75B H75D 0.9600 . ?
C75B H75E 0.9600 . ?
C75B H75F 0.9600 . ?
N81B C84B 1.298(12) . ?
N81B C81B 1.378(11) . ?
C81B C83B 1.357(14) . ?
C81B C82B 1.502(11) . ?
C82B O82B 1.228(11) . ?
C83B S83B 1.725(9) . ?
C83B H83B 0.9300 . ?
S83B C84B 1.741(9) . ?

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
N1S C1S C2S 179.4(11) . . ?
C1S C2S H2S1 109.5 . . ?
C1S C2S H2S2 109.5 . . ?
H2S1 C2S H2S2 109.5 . . ?
C1S C2S H2S3 109.5 . . ?
H2S1 C2S H2S3 109.5 . . ?
H2S2 C2S H2S3 109.5 . . ?
C82A N11A C11A 119.2(7) . . ?
C82A N11A H11A 120.4 . . ?
C11A N11A H11A 120.4 . . ?
N11A C11A C25A 109.0(7) . . ?
N11A C11A C13A 108.9(8) . . ?
C25A C11A C13A 113.4(7) . . ?
N11A C11A H11B 108.5 . . ?
C25A C11A H11B 108.5 . . ?
C13A C11A H11B 108.5 . . ?
C14A C13A C11A 110.1(8) . . ?
C14A C13A H13A 109.6 . . ?
C11A C13A H13A 109.6 . . ?
C14A C13A H13B 109.6 . . ?
C11A C13A H13B 109.6 . . ?
H13A C13A H13B 108.1 . . ?
C19A C14A C15A 119.0(9) . . ?
C19A C14A C13A 121.1(8) . . ?
C15A C14A C13A 119.8(8) . . ?
C14A C15A C16A 120.3(9) . . ?
C14A C15A H15A 119.8 . . ?
C16A C15A H15A 119.8 . . ?
C17A C16A C15A 118.8(8) . . ?
C17A C16A H16A 120.6 . . ?
C15A C16A H16A 120.6 . . ?
C16A C17A C18A 121.8(9) . . ?
C16A C17A Br01 120.1(6) . . ?
C18A C17A Br01 118.0(7) . . ?
C17A C18A C19A 119.1(9) . . ?
C17A C18A H18A 120.4 . . ?
C19A C18A H18A 120.4 . . ?
C18A C19A C14A 120.8(9) . . ?
C18A C19A H19A 119.6 . . ?
C14A C19A H19A 119.6 . . ?
C25A N21A C21A 106.2(8) . . ?
N21A C21A C23A 104.1(8) . . ?
N21A C21A C22A 112.2(8) . . ?
C23A C21A C22A 107.7(8) . . ?
N21A C21A H21A 110.9 . . ?
C23A C21A H21A 110.9 . . ?
C22A C21A H21A 110.9 . . ?
O22A C22A N31A 126.0(11) . . ?
O22A C22A C21A 118.6(9) . . ?
N31A C22A C21A 115.4(9) . . ?
O23A C23A C24A 108.7(10) . . ?
O23A C23A C21A 102.8(7) . . ?
C24A C23A C21A 112.4(10) . . ?
O23A C23A H23A 110.9 . . ?
C24A C23A H23A 110.9 . . ?
C21A C23A H23A 110.9 . . ?
C25A O23A C23A 105.1(7) . . ?
C23A C24A H24A 109.5 . . ?
C23A C24A H24B 109.5 . . ?
H24A C24A H24B 109.5 . . ?
C23A C24A H24C 109.5 . . ?
H24A C24A H24C 109.5 . . ?
H24B C24A H24C 109.5 . . ?
N21A C25A O23A 119.8(9) . . ?
N21A C25A C11A 124.2(8) . . ?
O23A C25A C11A 115.9(8) . . ?
C22A N31A C31A 119.8(8) . . ?
C22A N31A H31A 120.1 . . ?
C31A N31A H31A 120.1 . . ?
N31A C31A C44A 108.1(8) . . ?
N31A C31A C33A 114.7(8) . . ?
C44A C31A C33A 115.9(8) . . ?
N31A C31A H31B 105.7 . . ?
C44A C31A H31B 105.7 . . ?
C33A C31A H31B 105.7 . . ?
C35A C33A C34A 111.8(10) . . ?
C35A C33A C31A 108.7(9) . . ?
C34A C33A C31A 113.5(9) . . ?
C35A C33A H33A 107.5 . . ?
C34A C33A H33A 107.5 . . ?
C31A C33A H33A 107.5 . . ?
C33A C34A H34A 109.5 . . ?
C33A C34A H34B 109.5 . . ?
H34A C34A H34B 109.5 . . ?
C33A C34A H34C 109.5 . . ?
H34A C34A H34C 109.5 . . ?
H34B C34A H34C 109.5 . . ?
C33A C35A H35A 109.5 . . ?
C33A C35A H35B 109.5 . . ?
H35A C35A H35B 109.5 . . ?
C33A C35A H35C 109.5 . . ?
H35A C35A H35C 109.5 . . ?
H35B C35A H35C 109.5 . . ?
C44A N41A C41A 110.9(8) . . ?
C43A C41A N41A 116.7(9) . . ?
C43A C41A C42A 121.8(9) . . ?
N41A C41A C42A 121.5(8) . . ?
O42A C42A N51A 123.2(8) . . ?
O42A C42A C41A 120.0(8) . . ?
N51A C42A C41A 116.8(8) . . ?
C41A C43A S43A 108.0(7) . . ?
C41A C43A H43A 126.0 . . ?
S43A C43A H43A 126.0 . . ?
C43A S43A C44A 90.8(4) . . ?
N41A C44A C31A 124.8(9) . . ?
N41A C44A S43A 113.6(7) . . ?
C31A C44A S43A 121.5(7) . . ?
C42A N51A C51A 119.2(7) . . ?
C42A N51A H51A 120.4 . . ?
C51A N51A H51A 120.4 . . ?
N51A C51A C65A 109.4(6) . . ?
N51A C51A C53A 111.4(7) . . ?
C65A C51A C53A 113.0(7) . . ?
N51A C51A H51B 107.6 . . ?
C65A C51A H51B 107.6 . . ?
C53A C51A H51B 107.6 . . ?
C55A C53A C51A 108.4(7) . . ?
C55A C53A C54A 112.2(7) . . ?
C51A C53A C54A 108.8(8) . . ?
C55A C53A H53A 109.1 . . ?
C51A C53A H53A 109.1 . . ?
C54A C53A H53A 109.1 . . ?
C53A C54A H54A 109.5 . . ?
C53A C54A H54B 109.5 . . ?
H54A C54A H54B 109.5 . . ?
C53A C54A H54C 109.5 . . ?
H54A C54A H54C 109.5 . . ?
H54B C54A H54C 109.5 . . ?
C53A C55A C56A 113.6(8) . . ?
C53A C55A H55A 108.8 . . ?
C56A C55A H55A 108.8 . . ?
C53A C55A H55B 108.8 . . ?
C56A C55A H55B 108.8 . . ?
H55A C55A H55B 107.7 . . ?
C55A C56A H56A 109.5 . . ?
C55A C56A H56B 109.5 . . ?
H56A C56A H56B 109.5 . . ?
C55A C56A H56C 109.5 . . ?
H56A C56A H56C 109.5 . . ?
H56B C56A H56C 109.5 . . ?
C65A N61A C61A 105.4(7) . . ?
N61A C61A C62A 111.5(7) . . ?
N61A C61A C63A 104.9(7) . . ?
C62A C61A C63A 110.1(7) . . ?
N61A C61A H61A 110.1 . . ?
C62A C61A H61A 110.1 . . ?
C63A C61A H61A 110.1 . . ?
O62A C62A N71A 124.4(8) . . ?
O62A C62A C61A 119.4(8) . . ?
N71A C62A C61A 116.0(8) . . ?
O63A C63A C64A 109.2(6) . . ?
O63A C63A C61A 100.8(7) . . ?
C64A C63A C61A 113.4(8) . . ?
O63A C63A H63A 111.0 . . ?
C64A C63A H63A 111.0 . . ?
C61A C63A H63A 111.0 . . ?
C65A O63A C63A 106.1(6) . . ?
C63A C64A H64A 109.5 . . ?
C63A C64A H64B 109.5 . . ?
H64A C64A H64B 109.5 . . ?
C63A C64A H64C 109.5 . . ?
H64A C64A H64C 109.5 . . ?
H64B C64A H64C 109.5 . . ?
N61A C65A O63A 119.0(8) . . ?
N61A C65A C51A 123.8(8) . . ?
O63A C65A C51A 117.1(7) . . ?
C62A N71A C71A 119.3(7) . . ?
C62A N71A H71A 120.4 . . ?
C71A N71A H71A 120.4 . . ?
N71A C71A C84A 107.9(6) . . ?
N71A C71A C73A 113.8(7) . . ?
C84A C71A C73A 113.4(8) . . ?
N71A C71A H71B 107.1 . . ?
C84A C71A H71B 107.1 . . ?
C73A C71A H71B 107.1 . . ?
C75A C73A C74A 113.2(8) . . ?
C75A C73A C71A 108.7(9) . . ?
C74A C73A C71A 112.9(7) . . ?
C75A C73A H73A 107.2 . . ?
C74A C73A H73A 107.2 . . ?
C71A C73A H73A 107.2 . . ?
C73A C74A H74A 109.5 . . ?
C73A C74A H74B 109.5 . . ?
H74A C74A H74B 109.5 . . ?
C73A C74A H74C 109.5 . . ?
H74A C74A H74C 109.5 . . ?
H74B C74A H74C 109.5 . . ?
C73A C75A H75A 109.5 . . ?
C73A C75A H75B 109.5 . . ?
H75A C75A H75B 109.5 . . ?
C73A C75A H75C 109.5 . . ?
H75A C75A H75C 109.5 . . ?
H75B C75A H75C 109.5 . . ?
C84A N81A C81A 109.9(7) . . ?
N81A C81A C83A 116.6(8) . . ?
N81A C81A C82A 120.9(8) . . ?
C83A C81A C82A 122.5(8) . . ?
O82A C82A N11A 123.7(7) . . ?
O82A C82A C81A 121.5(8) . . ?
N11A C82A C81A 114.8(8) . . ?
C81A C83A S83A 108.8(7) . . ?
C81A C83A H83A 125.6 . . ?
S83A C83A H83A 125.6 . . ?
C83A S83A C84A 89.9(4) . . ?
N81A C84A C71A 123.2(8) . . ?
N81A C84A S83A 114.8(7) . . ?
C71A C84A S83A 121.7(6) . . ?
C82B N11B C11B 119.8(7) . . ?
C82B N11B H11C 120.1 . . ?
C11B N11B H11C 120.1 . . ?
N11B C11B C25B 109.1(7) . . ?
N11B C11B C13B 110.2(7) . . ?
C25B C11B C13B 112.7(9) . . ?
N11B C11B H11D 108.2 . . ?
C25B C11B H11D 108.2 . . ?
C13B C11B H11D 108.2 . . ?
C14B C13B C11B 113.3(9) . . ?
C14B C13B H13C 108.9 . . ?
C11B C13B H13C 108.9 . . ?
C14B C13B H13D 108.9 . . ?
C11B C13B H13D 108.9 . . ?
H13C C13B H13D 107.7 . . ?
C19B C14B C15B 117.5(9) . . ?
C19B C14B C13B 120.4(10) . . ?
C15B C14B C13B 122.1(9) . . ?
C16B C15B C14B 121.6(10) . . ?
C16B C15B H15B 119.2 . . ?
C14B C15B H15B 119.2 . . ?
C17B C16B C15B 117.4(11) . . ?
C17B C16B H16B 121.3 . . ?
C15B C16B H16B 121.3 . . ?
C18B C17B C16B 122.2(10) . . ?
C18B C17B Br02 120.5(8) . . ?
C16B C17B Br02 117.3(8) . . ?
C17B C18B C19B 120.8(10) . . ?
C17B C18B H18B 119.6 . . ?
C19B C18B H18B 119.6 . . ?
C14B C19B C18B 120.2(11) . . ?
C14B C19B H19B 119.9 . . ?
C18B C19B H19B 119.9 . . ?
C25B N21B C21B 105.6(7) . . ?
N21B C21B C22B 112.1(7) . . ?
N21B C21B C23B 104.7(7) . . ?
C22B C21B C23B 109.3(7) . . ?
N21B C21B H21B 110.2 . . ?
C22B C21B H21B 110.2 . . ?
C23B C21B H21B 110.2 . . ?
O22B C22B N31B 123.4(8) . . ?
O22B C22B C21B 119.9(8) . . ?
N31B C22B C21B 116.5(8) . . ?
O23B C23B C24B 110.6(8) . . ?
O23B C23B C21B 101.6(7) . . ?
C24B C23B C21B 112.8(8) . . ?
O23B C23B H23B 110.5 . . ?
C24B C23B H23B 110.5 . . ?
C21B C23B H23B 110.5 . . ?
C25B O23B C23B 105.6(6) . . ?
C23B C24B H24D 109.5 . . ?
C23B C24B H24E 109.5 . . ?
H24D C24B H24E 109.5 . . ?
C23B C24B H24F 109.5 . . ?
H24D C24B H24F 109.5 . . ?
H24E C24B H24F 109.5 . . ?
N21B C25B O23B 119.7(9) . . ?
N21B C25B C11B 124.5(8) . . ?
O23B C25B C11B 115.8(7) . . ?
C22B N31B C31B 121.0(8) . . ?
C22B N31B H31C 119.5 . . ?
C31B N31B H31C 119.5 . . ?
N31B C31B C44B 108.8(7) . . ?
N31B C31B C33B 114.0(7) . . ?
C44B C31B C33B 115.0(8) . . ?
N31B C31B H31D 106.1 . . ?
C44B C31B H31D 106.1 . . ?
C33B C31B H31D 106.1 . . ?
C34B C33B C35B 110.9(8) . . ?
C34B C33B C31B 113.4(8) . . ?
C35B C33B C31B 108.9(8) . . ?
C34B C33B H33B 107.8 . . ?
C35B C33B H33B 107.8 . . ?
C31B C33B H33B 107.8 . . ?
C33B C34B H34D 109.5 . . ?
C33B C34B H34E 109.5 . . ?
H34D C34B H34E 109.5 . . ?
C33B C34B H34F 109.5 . . ?
H34D C34B H34F 109.5 . . ?
H34E C34B H34F 109.5 . . ?
C33B C35B H35D 109.5 . . ?
C33B C35B H35E 109.5 . . ?
H35D C35B H35E 109.5 . . ?
C33B C35B H35F 109.5 . . ?
H35D C35B H35F 109.5 . . ?
H35E C35B H35F 109.5 . . ?
C44B N41B C41B 110.0(7) . . ?
C43B C41B N41B 115.0(8) . . ?
C43B C41B C42B 124.0(7) . . ?
N41B C41B C42B 120.8(7) . . ?
O42B C42B N51B 122.7(8) . . ?
O42B C42B C41B 122.0(8) . . ?
N51B C42B C41B 115.3(7) . . ?
C41B C43B S43B 111.4(6) . . ?
C41B C43B H43B 124.3 . . ?
S43B C43B H43B 124.3 . . ?
C43B S43B C44B 89.2(4) . . ?
N41B C44B C31B 122.9(8) . . ?
N41B C44B S43B 114.3(6) . . ?
C31B C44B S43B 122.6(7) . . ?
C42B N51B C51B 119.3(6) . . ?
C42B N51B H51C 120.4 . . ?
C51B N51B H51C 120.4 . . ?
N51B C51B C65B 109.7(7) . . ?
N51B C51B C53B 110.6(6) . . ?
C65B C51B C53B 113.1(7) . . ?
N51B C51B H51D 107.7 . . ?
C65B C51B H51D 107.7 . . ?
C53B C51B H51D 107.7 . . ?
C54B C53B C51B 109.3(7) . . ?
C54B C53B C55B 112.3(7) . . ?
C51B C53B C55B 111.7(7) . . ?
C54B C53B H53B 107.8 . . ?
C51B C53B H53B 107.8 . . ?
C55B C53B H53B 107.8 . . ?
C53B C54B H54D 109.5 . . ?
C53B C54B H54E 109.5 . . ?
H54D C54B H54E 109.5 . . ?
C53B C54B H54F 109.5 . . ?
H54D C54B H54F 109.5 . . ?
H54E C54B H54F 109.5 . . ?
C56B C55B C53B 114.8(8) . . ?
C56B C55B H55C 108.6 . . ?
C53B C55B H55C 108.6 . . ?
C56B C55B H55D 108.6 . . ?
C53B C55B H55D 108.6 . . ?
H55C C55B H55D 107.5 . . ?
C55B C56B H56D 109.5 . . ?
C55B C56B H56E 109.5 . . ?
H56D C56B H56E 109.5 . . ?
C55B C56B H56F 109.5 . . ?
H56D C56B H56F 109.5 . . ?
H56E C56B H56F 109.5 . . ?
C65B N61B C61B 105.9(7) . . ?
N61B C61B C62B 112.7(7) . . ?
N61B C61B C63B 103.1(6) . . ?
C62B C61B C63B 110.9(7) . . ?
N61B C61B H61B 110.0 . . ?
C62B C61B H61B 110.0 . . ?
C63B C61B H61B 110.0 . . ?
O62B C62B N71B 125.9(9) . . ?
O62B C62B C61B 117.4(8) . . ?
N71B C62B C61B 116.7(8) . . ?
O63B C63B C64B 108.0(7) . . ?
O63B C63B C61B 101.3(6) . . ?
C64B C63B C61B 113.8(7) . . ?
O63B C63B H63B 111.1 . . ?
C64B C63B H63B 111.1 . . ?
C61B C63B H63B 111.1 . . ?
C65B O63B C63B 104.1(6) . . ?
C63B C64B H64D 109.5 . . ?
C63B C64B H64E 109.5 . . ?
H64D C64B H64E 109.5 . . ?
C63B C64B H64F 109.5 . . ?
H64D C64B H64F 109.5 . . ?
H64E C64B H64F 109.5 . . ?
N61B C65B O63B 119.5(8) . . ?
N61B C65B C51B 124.8(7) . . ?
O63B C65B C51B 115.7(6) . . ?
C62B N71B C71B 119.0(7) . . ?
C62B N71B H71C 120.5 . . ?
C71B N71B H71C 120.5 . . ?
N71B C71B C84B 109.3(7) . . ?
N71B C71B C73B 114.9(7) . . ?
C84B C71B C73B 113.2(7) . . ?
N71B C71B H71D 106.3 . . ?
C84B C71B H71D 106.3 . . ?
C73B C71B H71D 106.3 . . ?
C71B C73B C74B 111.2(7) . . ?
C71B C73B C75B 115.0(7) . . ?
C74B C73B C75B 110.2(7) . . ?
C71B C73B H73B 106.6 . . ?
C74B C73B H73B 106.6 . . ?
C75B C73B H73B 106.6 . . ?
C73B C74B H74D 109.5 . . ?
C73B C74B H74E 109.5 . . ?
H74D C74B H74E 109.5 . . ?
C73B C74B H74F 109.5 . . ?
H74D C74B H74F 109.5 . . ?
H74E C74B H74F 109.5 . . ?
C73B C75B H75D 109.5 . . ?
C73B C75B H75E 109.5 . . ?
H75D C75B H75E 109.5 . . ?
C73B C75B H75F 109.5 . . ?
H75D C75B H75F 109.5 . . ?
H75E C75B H75F 109.5 . . ?
C84B N81B C81B 110.3(8) . . ?
C83B C81B N81B 116.8(8) . . ?
C83B C81B C82B 122.8(8) . . ?
N81B C81B C82B 120.4(8) . . ?
O82B C82B N11B 124.4(7) . . ?
O82B C82B C81B 120.7(9) . . ?
N11B C82B C81B 114.9(8) . . ?
C81B C83B S83B 108.9(7) . . ?
C81B C83B H83B 125.5 . . ?
S83B C83B H83B 125.5 . . ?
C83B S83B C84B 89.4(5) . . ?
N81B C84B C71B 123.7(8) . . ?
N81B C84B S83B 114.6(7) . . ?
C71B C84B S83B 121.5(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
C82A N11A C11A C25A -74.1(9) . . . . ?
C82A N11A C11A C13A 161.7(7) . . . . ?
N11A C11A C13A C14A -172.8(7) . . . . ?
C25A C11A C13A C14A 65.6(10) . . . . ?
C11A C13A C14A C19A 79.0(12) . . . . ?
C11A C13A C14A C15A -96.4(10) . . . . ?
C19A C14A C15A C16A 1.0(15) . . . . ?
C13A C14A C15A C16A 176.4(9) . . . . ?
C14A C15A C16A C17A -1.5(15) . . . . ?
C15A C16A C17A C18A 2.8(15) . . . . ?
C15A C16A C17A Br01 179.8(8) . . . . ?
C16A C17A C18A C19A -3.6(15) . . . . ?
Br01 C17A C18A C19A 179.3(8) . . . . ?
C17A C18A C19A C14A 3.1(16) . . . . ?
C15A C14A C19A C18A -1.8(15) . . . . ?
C13A C14A C19A C18A -177.2(9) . . . . ?
C25A N21A C21A C23A -12.0(10) . . . . ?
C25A N21A C21A C22A 104.1(9) . . . . ?
N21A C21A C22A O22A 170.1(9) . . . . ?
C23A C21A C22A O22A -76.0(11) . . . . ?
N21A C21A C22A N31A -12.7(12) . . . . ?
C23A C21A C22A N31A 101.2(9) . . . . ?
N21A C21A C23A O23A 13.9(9) . . . . ?
C22A C21A C23A O23A -105.3(8) . . . . ?
N21A C21A C23A C24A -102.7(10) . . . . ?
C22A C21A C23A C24A 138.0(10) . . . . ?
C24A C23A O23A C25A 108.2(10) . . . . ?
C21A C23A O23A C25A -11.1(9) . . . . ?
C21A N21A C25A O23A 5.5(11) . . . . ?
C21A N21A C25A C11A -172.4(8) . . . . ?
C23A O23A C25A N21A 4.2(11) . . . . ?
C23A O23A C25A C11A -177.7(8) . . . . ?
N11A C11A C25A N21A 114.6(10) . . . . ?
C13A C11A C25A N21A -123.9(10) . . . . ?
N11A C11A C25A O23A -63.4(10) . . . . ?
C13A C11A C25A O23A 58.1(10) . . . . ?
O22A C22A N31A C31A 19.6(15) . . . . ?
C21A C22A N31A C31A -157.4(8) . . . . ?
C22A N31A C31A C44A 106.2(9) . . . . ?
C22A N31A C31A C33A -122.8(10) . . . . ?
N31A C31A C33A C35A 64.4(12) . . . . ?
C44A C31A C33A C35A -168.5(9) . . . . ?
N31A C31A C33A C34A -60.7(12) . . . . ?
C44A C31A C33A C34A 66.4(12) . . . . ?
C44A N41A C41A C43A 0.9(11) . . . . ?
C44A N41A C41A C42A 179.9(7) . . . . ?
C43A C41A C42A O42A -6.2(12) . . . . ?
N41A C41A C42A O42A 174.9(7) . . . . ?
C43A C41A C42A N51A 171.8(8) . . . . ?
N41A C41A C42A N51A -7.1(12) . . . . ?
N41A C41A C43A S43A -2.4(10) . . . . ?
C42A C41A C43A S43A 178.6(6) . . . . ?
C41A C43A S43A C44A 2.4(7) . . . . ?
C41A N41A C44A C31A -175.0(8) . . . . ?
C41A N41A C44A S43A 1.1(9) . . . . ?
N31A C31A C44A N41A -22.2(12) . . . . ?
C33A C31A C44A N41A -152.5(9) . . . . ?
N31A C31A C44A S43A 162.1(6) . . . . ?
C33A C31A C44A S43A 31.7(11) . . . . ?
C43A S43A C44A N41A -2.1(7) . . . . ?
C43A S43A C44A C31A 174.1(8) . . . . ?
O42A C42A N51A C51A 5.0(12) . . . . ?
C41A C42A N51A C51A -172.9(7) . . . . ?
C42A N51A C51A C65A -78.4(9) . . . . ?
C42A N51A C51A C53A 156.0(7) . . . . ?
N51A C51A C53A C55A -61.4(9) . . . . ?
C65A C51A C53A C55A 175.0(8) . . . . ?
N51A C51A C53A C54A 176.3(7) . . . . ?
C65A C51A C53A C54A 52.7(9) . . . . ?
C51A C53A C55A C56A -179.8(8) . . . . ?
C54A C53A C55A C56A -59.7(11) . . . . ?
C65A N61A C61A C62A 105.0(8) . . . . ?
C65A N61A C61A C63A -14.1(8) . . . . ?
N61A C61A C62A O62A 178.2(8) . . . . ?
C63A C61A C62A O62A -65.8(10) . . . . ?
N61A C61A C62A N71A -5.8(11) . . . . ?
C63A C61A C62A N71A 110.1(9) . . . . ?
N61A C61A C63A O63A 18.9(8) . . . . ?
C62A C61A C63A O63A -101.2(7) . . . . ?
N61A C61A C63A C64A -97.6(8) . . . . ?
C62A C61A C63A C64A 142.3(8) . . . . ?
C64A C63A O63A C65A 102.3(8) . . . . ?
C61A C63A O63A C65A -17.3(8) . . . . ?
C61A N61A C65A O63A 2.9(10) . . . . ?
C61A N61A C65A C51A -171.8(7) . . . . ?
C63A O63A C65A N61A 10.2(9) . . . . ?
C63A O63A C65A C51A -174.7(7) . . . . ?
N51A C51A C65A N61A 116.6(9) . . . . ?
C53A C51A C65A N61A -118.7(9) . . . . ?
N51A C51A C65A O63A -58.3(9) . . . . ?
C53A C51A C65A O63A 66.4(9) . . . . ?
O62A C62A N71A C71A 18.3(13) . . . . ?
C61A C62A N71A C71A -157.4(7) . . . . ?
C62A N71A C71A C84A 99.1(9) . . . . ?
C62A N71A C71A C73A -134.1(8) . . . . ?
N71A C71A C73A C75A 72.0(9) . . . . ?
C84A C71A C73A C75A -164.2(7) . . . . ?
N71A C71A C73A C74A -54.5(11) . . . . ?
C84A C71A C73A C74A 69.4(9) . . . . ?
C84A N81A C81A C83A 0.9(10) . . . . ?
C84A N81A C81A C82A 180.0(7) . . . . ?
C11A N11A C82A O82A 3.7(12) . . . . ?
C11A N11A C82A C81A -174.0(7) . . . . ?
N81A C81A C82A O82A -173.5(8) . . . . ?
C83A C81A C82A O82A 5.5(13) . . . . ?
N81A C81A C82A N11A 4.2(11) . . . . ?
C83A C81A C82A N11A -176.7(8) . . . . ?
N81A C81A C83A S83A -0.7(10) . . . . ?
C82A C81A C83A S83A -179.7(6) . . . . ?
C81A C83A S83A C84A 0.2(7) . . . . ?
C81A N81A C84A C71A -174.5(7) . . . . ?
C81A N81A C84A S83A -0.7(9) . . . . ?
N71A C71A C84A N81A -31.0(11) . . . . ?
C73A C71A C84A N81A -158.0(7) . . . . ?
N71A C71A C84A S83A 155.6(6) . . . . ?
C73A C71A C84A S83A 28.6(9) . . . . ?
C83A S83A C84A N81A 0.3(7) . . . . ?
C83A S83A C84A C71A 174.2(7) . . . . ?
C82B N11B C11B C25B -75.5(10) . . . . ?
C82B N11B C11B C13B 160.3(9) . . . . ?
N11B C11B C13B C14B -174.3(8) . . . . ?
C25B C11B C13B C14B 63.6(11) . . . . ?
C11B C13B C14B C19B 70.5(15) . . . . ?
C11B C13B C14B C15B -105.4(13) . . . . ?
C19B C14B C15B C16B 5.8(19) . . . . ?
C13B C14B C15B C16B -178.1(12) . . . . ?
C14B C15B C16B C17B 0(2) . . . . ?
C15B C16B C17B C18B -5(2) . . . . ?
C15B C16B C17B Br02 177.8(10) . . . . ?
C16B C17B C18B C19B 5(2) . . . . ?
Br02 C17B C18B C19B -177.9(10) . . . . ?
C15B C14B C19B C18B -5.9(19) . . . . ?
C13B C14B C19B C18B 178.0(12) . . . . ?
C17B C18B C19B C14B 1(2) . . . . ?
C25B N21B C21B C22B 105.2(8) . . . . ?
C25B N21B C21B C23B -13.1(9) . . . . ?
N21B C21B C22B O22B 168.8(8) . . . . ?
C23B C21B C22B O22B -75.6(10) . . . . ?
N21B C21B C22B N31B -16.4(10) . . . . ?
C23B C21B C22B N31B 99.1(9) . . . . ?
N21B C21B C23B O23B 16.6(8) . . . . ?
C22B C21B C23B O23B -103.7(8) . . . . ?
N21B C21B C23B C24B -101.8(9) . . . . ?
C22B C21B C23B C24B 137.9(9) . . . . ?
C24B C23B O23B C25B 105.8(9) . . . . ?
C21B C23B O23B C25B -14.2(9) . . . . ?
C21B N21B C25B O23B 4.3(11) . . . . ?
C21B N21B C25B C11B -173.0(8) . . . . ?
C23B O23B C25B N21B 7.2(11) . . . . ?
C23B O23B C25B C11B -175.2(7) . . . . ?
N11B C11B C25B N21B 111.9(9) . . . . ?
C13B C11B C25B N21B -125.4(9) . . . . ?
N11B C11B C25B O23B -65.6(10) . . . . ?
C13B C11B C25B O23B 57.1(10) . . . . ?
O22B C22B N31B C31B 18.7(12) . . . . ?
C21B C22B N31B C31B -155.9(7) . . . . ?
C22B N31B C31B C44B 108.2(9) . . . . ?
C22B N31B C31B C33B -122.0(9) . . . . ?
N31B C31B C33B C34B -62.1(10) . . . . ?
C44B C31B C33B C34B 64.6(10) . . . . ?
N31B C31B C33B C35B 61.9(10) . . . . ?
C44B C31B C33B C35B -171.4(8) . . . . ?
C44B N41B C41B C43B 0.9(11) . . . . ?
C44B N41B C41B C42B 177.0(8) . . . . ?
C43B C41B C42B O42B -3.2(13) . . . . ?
N41B C41B C42B O42B -179.0(8) . . . . ?
C43B C41B C42B N51B 174.6(8) . . . . ?
N41B C41B C42B N51B -1.1(12) . . . . ?
N41B C41B C43B S43B -2.0(10) . . . . ?
C42B C41B C43B S43B -178.0(7) . . . . ?
C41B C43B S43B C44B 1.9(7) . . . . ?
C41B N41B C44B C31B -174.9(8) . . . . ?
C41B N41B C44B S43B 0.6(9) . . . . ?
N31B C31B C44B N41B -23.7(11) . . . . ?
C33B C31B C44B N41B -153.0(8) . . . . ?
N31B C31B C44B S43B 161.2(6) . . . . ?
C33B C31B C44B S43B 31.9(11) . . . . ?
C43B S43B C44B N41B -1.4(7) . . . . ?
C43B S43B C44B C31B 174.1(8) . . . . ?
O42B C42B N51B C51B 1.0(13) . . . . ?
C41B C42B N51B C51B -176.9(7) . . . . ?
C42B N51B C51B C65B -75.2(9) . . . . ?
C42B N51B C51B C53B 159.3(8) . . . . ?
N51B C51B C53B C54B 173.8(7) . . . . ?
C65B C51B C53B C54B 50.3(9) . . . . ?
N51B C51B C53B C55B -61.3(9) . . . . ?
C65B C51B C53B C55B 175.1(6) . . . . ?
C54B C53B C55B C56B 53.2(11) . . . . ?
C51B C53B C55B C56B -70.1(10) . . . . ?
C65B N61B C61B C62B 101.0(8) . . . . ?
C65B N61B C61B C63B -18.6(8) . . . . ?
N61B C61B C62B O62B -177.6(7) . . . . ?
C63B C61B C62B O62B -62.6(10) . . . . ?
N61B C61B C62B N71B -0.1(10) . . . . ?
C63B C61B C62B N71B 114.9(8) . . . . ?
N61B C61B C63B O63B 23.8(8) . . . . ?
C62B C61B C63B O63B -97.1(8) . . . . ?
N61B C61B C63B C64B -91.8(8) . . . . ?
C62B C61B C63B C64B 147.4(8) . . . . ?
C64B C63B O63B C65B 99.0(7) . . . . ?
C61B C63B O63B C65B -20.8(8) . . . . ?
C61B N61B C65B O63B 5.6(10) . . . . ?
C61B N61B C65B C51B -171.8(7) . . . . ?
C63B O63B C65B N61B 10.9(10) . . . . ?
C63B O63B C65B C51B -171.5(7) . . . . ?
N51B C51B C65B N61B 111.0(9) . . . . ?
C53B C51B C65B N61B -124.9(8) . . . . ?
N51B C51B C65B O63B -66.4(8) . . . . ?
C53B C51B C65B O63B 57.7(9) . . . . ?
O62B C62B N71B C71B 14.7(13) . . . . ?
C61B C62B N71B C71B -162.5(7) . . . . ?
C62B N71B C71B C84B 93.5(9) . . . . ?
C62B N71B C71B C73B -137.9(8) . . . . ?
N71B C71B C73B C74B 62.5(10) . . . . ?
C84B C71B C73B C74B -170.9(8) . . . . ?
N71B C71B C73B C75B -63.6(10) . . . . ?
C84B C71B C73B C75B 63.0(10) . . . . ?
C84B N81B C81B C83B 0.6(11) . . . . ?
C84B N81B C81B C82B -179.7(8) . . . . ?
C11B N11B C82B O82B 4.5(14) . . . . ?
C11B N11B C82B C81B -173.7(8) . . . . ?
C83B C81B C82B O82B -0.3(14) . . . . ?
N81B C81B C82B O82B 180.0(8) . . . . ?
C83B C81B C82B N11B 178.0(9) . . . . ?
N81B C81B C82B N11B -1.7(12) . . . . ?
N81B C81B C83B S83B -0.5(11) . . . . ?
C82B C81B C83B S83B 179.8(7) . . . . ?
C81B C83B S83B C84B 0.2(7) . . . . ?
C81B N81B C84B C71B -175.9(8) . . . . ?
C81B N81B C84B S83B -0.4(9) . . . . ?
N71B C71B C84B N81B -21.3(11) . . . . ?
C73B C71B C84B N81B -150.8(8) . . . . ?
N71B C71B C84B S83B 163.5(6) . . . . ?
C73B C71B C84B S83B 34.0(10) . . . . ?
C83B S83B C84B N81B 0.1(7) . . . . ?
C83B S83B C84B C71B 175.7(8) . . . . ?

_refine_diff_density_max         1.929
_refine_diff_density_min         -0.899
_refine_diff_density_rms         0.140



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrilr'
####################################################################### 
# 
# 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_phe4c
_database_code_depnum_ccdc_archive 'CCDC 2289963'
loop_
_audit_author_name
_audit_author_address
'Akiko Asano'
;Osaka Medical nad Pharmaceutical University
Japan
;
_audit_update_record             
;
2023-08-22 deposited with the CCDC.	2023-12-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        Phe(4Cl)_ASC
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C39 H49 Cl N8 O6 S2, 0.5(C2 H3 N)'
_chemical_formula_sum            'C40 H50.50 Cl N8.50 O6 S2'
_chemical_formula_weight         845.96

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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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'

_cell_length_a                   15.6272(2)
_cell_length_b                   16.6962(2)
_cell_length_c                   16.1368(2)
_cell_angle_alpha                90
_cell_angle_beta                 95.4400(10)
_cell_angle_gamma                90
_cell_volume                     4191.37(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    90
_cell_measurement_reflns_used    33823
_cell_measurement_theta_min      2.7580
_cell_measurement_theta_max      74.1060

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_F_000             1788
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    2.205
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.86377
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.20a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      90
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'rotating anode'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 5.881
_diffrn_reflns_number            46819
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.751
_diffrn_reflns_theta_max         74.452
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             16582
_reflns_number_gt                16132
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.897
_reflns_Friedel_fraction_max     0.951
_reflns_Friedel_fraction_full    0.998

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_structure_solution    SHELXT
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_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)+(0.1088P)²+12.0171P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_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 x determined using 7283 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.019(4)
_chemical_absolute_configuration rm
_refine_ls_number_reflns         16582
_refine_ls_number_parameters     1037
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0428
_refine_ls_wR_factor_ref         0.1337
_refine_ls_wR_factor_gt          0.1329
_refine_ls_goodness_of_fit_ref   0.718
_refine_ls_restrained_S_all      0.718
_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
N1C N 0.7179(3) 0.5712(3) 0.8485(3) 0.0345(10) Uani 1 1 d . . . . .
C1C C 0.6619(3) 0.5383(3) 0.8126(3) 0.0262(10) Uani 1 1 d . . . . .
C2C C 0.5907(3) 0.4966(3) 0.7663(3) 0.0339(11) Uani 1 1 d . . . . .
H2C1 H 0.537297 0.516011 0.783535 0.051 Uiso 1 1 calc R U . . .
H2C2 H 0.595480 0.440198 0.777100 0.051 Uiso 1 1 calc R U . . .
H2C3 H 0.592374 0.506278 0.707863 0.051 Uiso 1 1 calc R U . . .
N11A N 0.7963(2) 0.6658(2) 0.3770(2) 0.0189(7) Uani 1 1 d . . . . .
H11A H 0.772138 0.686856 0.417474 0.023 Uiso 1 1 calc R U . . .
C11A C 0.8822(3) 0.6900(3) 0.3610(3) 0.0204(9) Uani 1 1 d . . . . .
H11B H 0.883351 0.696918 0.300807 0.024 Uiso 1 1 calc R U . . .
C13A C 0.9039(3) 0.7710(3) 0.4034(3) 0.0253(9) Uani 1 1 d . . . . .
H13A H 0.859027 0.809474 0.386563 0.030 Uiso 1 1 calc R U . . .
H13B H 0.906197 0.764693 0.463369 0.030 Uiso 1 1 calc R U . . .
C14A C 0.9890(3) 0.8021(3) 0.3803(3) 0.0226(9) Uani 1 1 d . . . . .
C15A C 0.9949(3) 0.8386(3) 0.3038(3) 0.0299(11) Uani 1 1 d . . . . .
H15A H 0.945517 0.845815 0.267756 0.036 Uiso 1 1 calc R U . . .
C16A C 1.0734(3) 0.8644(3) 0.2803(3) 0.0309(11) Uani 1 1 d . . . . .
H16A H 1.076615 0.889036 0.229045 0.037 Uiso 1 1 calc R U . . .
C17A C 1.1470(3) 0.8531(3) 0.3341(3) 0.0255(9) Uani 1 1 d . . . . .
C18A C 1.1427(3) 0.8174(3) 0.4110(3) 0.0265(10) Uani 1 1 d . . . . .
H18A H 1.192222 0.810408 0.447061 0.032 Uiso 1 1 calc R U . . .
C19A C 1.0639(3) 0.7923(3) 0.4336(3) 0.0260(10) Uani 1 1 d . . . . .
H19A H 1.060692 0.768436 0.485296 0.031 Uiso 1 1 calc R U . . .
CL1A Cl 1.24543(8) 0.88586(8) 0.30454(8) 0.0336(3) Uani 1 1 d . . . . .
C25A C 0.9454(3) 0.6251(3) 0.3896(3) 0.0214(9) Uani 1 1 d . . . . .
N21A N 0.9881(2) 0.5828(2) 0.3427(2) 0.0226(8) Uani 1 1 d . . . . .
C21A C 1.0289(3) 0.5191(3) 0.3955(3) 0.0272(10) Uani 1 1 d . . . . .
H21A H 1.090020 0.515137 0.386793 0.033 Uiso 1 1 calc R U . . .
C22A C 0.9858(3) 0.4379(3) 0.3804(3) 0.0277(10) Uani 1 1 d . . . . .
O22A O 1.0192(2) 0.3775(2) 0.4123(3) 0.0399(9) Uani 1 1 d . . . . .
C23A C 1.0191(3) 0.5460(3) 0.4857(3) 0.0300(10) Uani 1 1 d . . . . .
H23A H 0.999018 0.501491 0.518347 0.036 Uiso 1 1 calc R U . . .
O23A O 0.9525(2) 0.6080(2) 0.4728(2) 0.0264(7) Uani 1 1 d . . . . .
C24A C 1.1002(4) 0.5823(4) 0.5291(4) 0.0453(14) Uani 1 1 d . . . . .
H24A H 1.143733 0.541789 0.537547 0.068 Uiso 1 1 calc R U . . .
H24B H 1.120169 0.624491 0.495387 0.068 Uiso 1 1 calc R U . . .
H24C H 1.088098 0.603714 0.581996 0.068 Uiso 1 1 calc R U . . .
N31A N 0.9086(2) 0.4385(2) 0.3359(3) 0.0230(8) Uani 1 1 d . . . . .
H31A H 0.895175 0.477645 0.302499 0.028 Uiso 1 1 calc R U . . .
C31A C 0.8476(3) 0.3738(3) 0.3434(3) 0.0237(9) Uani 1 1 d . . . . .
H31B H 0.878810 0.332555 0.377244 0.028 Uiso 1 1 calc R U . . .
C33A C 0.8160(4) 0.3331(3) 0.2612(3) 0.0301(11) Uani 1 1 d . . . . .
H33A H 0.774297 0.291871 0.273245 0.036 Uiso 1 1 calc R U . . .
C34A C 0.7715(4) 0.3905(3) 0.1965(3) 0.0361(12) Uani 1 1 d . . . . .
H34A H 0.724169 0.416267 0.219470 0.054 Uiso 1 1 calc R U . . .
H34B H 0.811869 0.430283 0.181923 0.054 Uiso 1 1 calc R U . . .
H34C H 0.750729 0.360958 0.147697 0.054 Uiso 1 1 calc R U . . .
C35A C 0.8918(4) 0.2914(3) 0.2259(4) 0.0388(13) Uani 1 1 d . . . . .
H35A H 0.872303 0.265698 0.174350 0.058 Uiso 1 1 calc R U . . .
H35B H 0.935040 0.330243 0.216441 0.058 Uiso 1 1 calc R U . . .
H35C H 0.915533 0.251978 0.264918 0.058 Uiso 1 1 calc R U . . .
C44A C 0.7774(3) 0.4030(3) 0.3941(3) 0.0208(9) Uani 1 1 d . . . . .
N41A N 0.7866(2) 0.4634(2) 0.4466(2) 0.0202(7) Uani 1 1 d . . . . .
C41A C 0.7146(3) 0.4708(3) 0.4899(3) 0.0217(9) Uani 1 1 d . . . . .
C42A C 0.7072(3) 0.5344(3) 0.5524(3) 0.0198(8) Uani 1 1 d . . . . .
O42A O 0.64010(19) 0.5438(2) 0.58571(19) 0.0222(6) Uani 1 1 d . . . . .
C43A C 0.6504(3) 0.4158(3) 0.4704(3) 0.0225(9) Uani 1 1 d . . . . .
H43A H 0.598838 0.413001 0.494702 0.027 Uiso 1 1 calc R U . . .
S43A S 0.68010(7) 0.35340(7) 0.39455(7) 0.0243(2) Uani 1 1 d . . . . .
N51A N 0.7780(2) 0.5795(2) 0.5721(2) 0.0188(7) Uani 1 1 d . . . . .
H51A H 0.822169 0.574338 0.544558 0.023 Uiso 1 1 calc R U . . .
C51A C 0.7793(3) 0.6374(3) 0.6407(3) 0.0195(8) Uani 1 1 d . . . . .
H51B H 0.749441 0.612359 0.684695 0.023 Uiso 1 1 calc R U . . .
C53A C 0.8712(3) 0.6560(3) 0.6783(3) 0.0229(9) Uani 1 1 d . . . . .
H53A H 0.904214 0.676996 0.634359 0.027 Uiso 1 1 calc R U . . .
C54A C 0.8672(3) 0.7200(3) 0.7455(3) 0.0315(11) Uani 1 1 d . . . . .
H54A H 0.840112 0.767282 0.721365 0.047 Uiso 1 1 calc R U . . .
H54B H 0.834453 0.700176 0.788576 0.047 Uiso 1 1 calc R U . . .
H54C H 0.924341 0.732811 0.768749 0.047 Uiso 1 1 calc R U . . .
C55A C 0.9138(3) 0.5786(3) 0.7127(3) 0.0266(10) Uani 1 1 d . . . . .
H55A H 0.878781 0.556100 0.753373 0.032 Uiso 1 1 calc R U . . .
H55B H 0.914568 0.540390 0.667487 0.032 Uiso 1 1 calc R U . . .
C56A C 1.0051(3) 0.5888(3) 0.7532(4) 0.0341(12) Uani 1 1 d . . . . .
H56A H 1.026913 0.537858 0.772925 0.051 Uiso 1 1 calc R U . . .
H56B H 1.040855 0.609638 0.713037 0.051 Uiso 1 1 calc R U . . .
H56C H 1.005008 0.625373 0.799069 0.051 Uiso 1 1 calc R U . . .
C65A C 0.7282(3) 0.7100(3) 0.6122(3) 0.0188(8) Uani 1 1 d . . . . .
N61A N 0.6599(2) 0.7341(2) 0.6418(2) 0.0197(7) Uani 1 1 d . . . . .
C61A C 0.6261(3) 0.8000(3) 0.5873(3) 0.0208(9) Uani 1 1 d . . . . .
H61A H 0.609827 0.845636 0.620618 0.025 Uiso 1 1 calc R U . . .
C62A C 0.5503(3) 0.7734(3) 0.5271(3) 0.0215(9) Uani 1 1 d . . . . .
O62A O 0.5133(2) 0.8233(2) 0.4801(2) 0.0289(7) Uani 1 1 d . . . . .
C63A C 0.7025(3) 0.8227(3) 0.5373(3) 0.0219(9) Uani 1 1 d . . . . .
H63A H 0.682634 0.831319 0.478535 0.026 Uiso 1 1 calc R U . . .
O63A O 0.75733(19) 0.75105(19) 0.54698(18) 0.0196(6) Uani 1 1 d . . . . .
C64A C 0.7544(3) 0.8943(3) 0.5720(3) 0.0290(10) Uani 1 1 d . . . . .
H64A H 0.719453 0.941656 0.566104 0.043 Uiso 1 1 calc R U . . .
H64B H 0.772313 0.885466 0.629788 0.043 Uiso 1 1 calc R U . . .
H64C H 0.804009 0.900990 0.541890 0.043 Uiso 1 1 calc R U . . .
N71A N 0.5298(2) 0.6948(2) 0.5269(2) 0.0203(7) Uani 1 1 d . . . . .
H71A H 0.545130 0.665603 0.569629 0.024 Uiso 1 1 calc R U . . .
C71A C 0.4819(3) 0.6595(3) 0.4542(3) 0.0201(8) Uani 1 1 d . . . . .
H71B H 0.456966 0.703826 0.420121 0.024 Uiso 1 1 calc R U . . .
C73A C 0.4064(3) 0.6060(3) 0.4765(3) 0.0215(9) Uani 1 1 d . . . . .
H73A H 0.381886 0.580681 0.424893 0.026 Uiso 1 1 calc R U . . .
C74A C 0.4341(3) 0.5391(3) 0.5375(3) 0.0270(10) Uani 1 1 d . . . . .
H74A H 0.477937 0.507460 0.515504 0.041 Uiso 1 1 calc R U . . .
H74B H 0.456173 0.561898 0.589829 0.041 Uiso 1 1 calc R U . . .
H74C H 0.385478 0.505795 0.545612 0.041 Uiso 1 1 calc R U . . .
C75A C 0.3367(3) 0.6587(3) 0.5078(3) 0.0322(11) Uani 1 1 d . . . . .
H75A H 0.321204 0.699912 0.467697 0.048 Uiso 1 1 calc R U . . .
H75B H 0.287105 0.626598 0.515588 0.048 Uiso 1 1 calc R U . . .
H75C H 0.357800 0.682702 0.559804 0.048 Uiso 1 1 calc R U . . .
C84A C 0.5443(3) 0.6170(3) 0.4035(3) 0.0193(8) Uani 1 1 d . . . . .
N81A N 0.6239(2) 0.6402(2) 0.4013(2) 0.0186(7) Uani 1 1 d . . . . .
C81A C 0.6630(3) 0.5953(3) 0.3438(3) 0.0197(8) Uani 1 1 d . . . . .
C82A C 0.7539(3) 0.6095(3) 0.3277(3) 0.0188(8) Uani 1 1 d . . . . .
O82A O 0.7868(2) 0.57379(19) 0.27246(19) 0.0209(6) Uani 1 1 d . . . . .
C83A C 0.6135(3) 0.5383(3) 0.3024(3) 0.0216(9) Uani 1 1 d . . . . .
H83A H 0.631408 0.504211 0.261835 0.026 Uiso 1 1 calc R U . . .
S83A S 0.51289(6) 0.53909(6) 0.33651(6) 0.0195(2) Uani 1 1 d . . . . .
N11B N 0.3004(2) 0.3552(2) 0.1299(2) 0.0213(7) Uani 1 1 d . . . . .
H11C H 0.270292 0.330392 0.090506 0.026 Uiso 1 1 calc R U . . .
C11B C 0.3904(3) 0.3332(3) 0.1510(3) 0.0208(9) Uani 1 1 d . . . . .
H11D H 0.401126 0.332239 0.211770 0.025 Uiso 1 1 calc R U . . .
C13B C 0.4062(3) 0.2488(3) 0.1189(3) 0.0256(10) Uani 1 1 d . . . . .
H13C H 0.363124 0.212837 0.137323 0.031 Uiso 1 1 calc R U . . .
H13D H 0.399920 0.249365 0.058508 0.031 Uiso 1 1 calc R U . . .
C14B C 0.4947(3) 0.2176(3) 0.1490(3) 0.0216(9) Uani 1 1 d . . . . .
C15B C 0.5610(4) 0.2160(3) 0.0971(3) 0.0300(10) Uani 1 1 d . . . . .
H15B H 0.551022 0.236054 0.043266 0.036 Uiso 1 1 calc R U . . .
C16B C 0.6419(3) 0.1851(3) 0.1237(3) 0.0318(11) Uani 1 1 d . . . . .
H16B H 0.685649 0.184784 0.088444 0.038 Uiso 1 1 calc R U . . .
C17B C 0.6554(3) 0.1552(3) 0.2029(3) 0.0256(9) Uani 1 1 d . . . . .
C18B C 0.5917(3) 0.1570(3) 0.2568(3) 0.0320(11) Uani 1 1 d . . . . .
H18B H 0.602180 0.137175 0.310693 0.038 Uiso 1 1 calc R U . . .
C19B C 0.5120(3) 0.1888(3) 0.2293(3) 0.0305(11) Uani 1 1 d . . . . .
H19B H 0.469286 0.190860 0.265668 0.037 Uiso 1 1 calc R U . . .
CL2B Cl 0.75500(8) 0.11296(8) 0.23631(9) 0.0373(3) Uani 1 1 d . . . . .
C25B C 0.4481(3) 0.3953(3) 0.1187(3) 0.0187(8) Uani 1 1 d . . . . .
N21B N 0.4966(2) 0.4435(2) 0.1625(2) 0.0191(7) Uani 1 1 d . . . . .
C21B C 0.5305(3) 0.5002(3) 0.1041(3) 0.0200(9) Uani 1 1 d . . . . .
H21B H 0.592804 0.505733 0.116500 0.024 Uiso 1 1 calc R U . . .
C22B C 0.4876(3) 0.5826(3) 0.1052(3) 0.0191(8) Uani 1 1 d . . . . .
O22B O 0.5186(2) 0.6384(2) 0.0692(2) 0.0298(7) Uani 1 1 d . . . . .
C23B C 0.5100(3) 0.4615(3) 0.0176(3) 0.0236(9) Uani 1 1 d . . . . .
H23B H 0.486512 0.501382 -0.023008 0.028 Uiso 1 1 calc R U . . .
O23B O 0.4439(2) 0.40197(19) 0.03372(19) 0.0216(6) Uani 1 1 d . . . . .
C24B C 0.5862(3) 0.4189(3) -0.0138(3) 0.0315(11) Uani 1 1 d . . . . .
H24D H 0.629394 0.457373 -0.024443 0.047 Uiso 1 1 calc R U . . .
H24E H 0.609468 0.381369 0.027437 0.047 Uiso 1 1 calc R U . . .
H24F H 0.567872 0.390777 -0.064331 0.047 Uiso 1 1 calc R U . . .
N31B N 0.4137(2) 0.5869(2) 0.1420(2) 0.0204(7) Uani 1 1 d . . . . .
H31C H 0.402944 0.551923 0.178706 0.024 Uiso 1 1 calc R U . . .
C31B C 0.3519(3) 0.6507(3) 0.1197(3) 0.0215(9) Uani 1 1 d . . . . .
H31D H 0.379872 0.687372 0.083343 0.026 Uiso 1 1 calc R U . . .
C33B C 0.3278(3) 0.7009(3) 0.1937(3) 0.0238(9) Uani 1 1 d . . . . .
H33B H 0.287622 0.742426 0.171520 0.029 Uiso 1 1 calc R U . . .
C34B C 0.4084(3) 0.7435(3) 0.2333(3) 0.0279(10) Uani 1 1 d . . . . .
H34D H 0.434832 0.772693 0.191315 0.042 Uiso 1 1 calc R U . . .
H34E H 0.392679 0.779854 0.275375 0.042 Uiso 1 1 calc R U . . .
H34F H 0.448130 0.704500 0.258074 0.042 Uiso 1 1 calc R U . . .
C35B C 0.2832(3) 0.6535(3) 0.2579(3) 0.0288(10) Uani 1 1 d . . . . .
H35D H 0.233153 0.627657 0.231131 0.043 Uiso 1 1 calc R U . . .
H35E H 0.321976 0.613806 0.282875 0.043 Uiso 1 1 calc R U . . .
H35F H 0.266525 0.689161 0.300175 0.043 Uiso 1 1 calc R U . . .
C44B C 0.2764(3) 0.6144(3) 0.0669(3) 0.0204(8) Uani 1 1 d . . . . .
N41B N 0.2815(2) 0.5483(2) 0.0244(2) 0.0189(7) Uani 1 1 d . . . . .
C41B C 0.2053(3) 0.5351(3) -0.0240(3) 0.0197(8) Uani 1 1 d . . . . .
C42B C 0.1941(3) 0.4650(2) -0.0806(3) 0.0179(8) Uani 1 1 d . . . . .
O42B O 0.1258(2) 0.45165(18) -0.1229(2) 0.0224(6) Uani 1 1 d . . . . .
C43B C 0.1432(3) 0.5912(3) -0.0189(3) 0.0215(9) Uani 1 1 d . . . . .
H43B H 0.089412 0.590421 -0.048985 0.026 Uiso 1 1 calc R U . . .
S43B S 0.17844(7) 0.66324(6) 0.05071(7) 0.0232(2) Uani 1 1 d . . . . .
N51B N 0.2641(2) 0.4180(2) -0.0829(2) 0.0184(7) Uani 1 1 d . . . . .
H51C H 0.310115 0.428157 -0.051096 0.022 Uiso 1 1 calc R U . . .
C51B C 0.2613(3) 0.3500(3) -0.1396(3) 0.0183(8) Uani 1 1 d . . . . .
H51D H 0.231297 0.367399 -0.192656 0.022 Uiso 1 1 calc R U . . .
C53B C 0.3517(3) 0.3236(3) -0.1568(3) 0.0189(8) Uani 1 1 d . . . . .
H53B H 0.383790 0.311177 -0.103190 0.023 Uiso 1 1 calc R U . . .
C54B C 0.3471(3) 0.2474(3) -0.2091(3) 0.0236(9) Uani 1 1 d . . . . .
H54D H 0.404088 0.231334 -0.219501 0.035 Uiso 1 1 calc R U . . .
H54E H 0.320680 0.205523 -0.179631 0.035 Uiso 1 1 calc R U . . .
H54F H 0.313585 0.257243 -0.261075 0.035 Uiso 1 1 calc R U . . .
C55B C 0.3992(3) 0.3911(3) -0.1973(3) 0.0232(9) Uani 1 1 d . . . . .
H55C H 0.397866 0.438450 -0.162571 0.028 Uiso 1 1 calc R U . . .
H55D H 0.458925 0.375587 -0.198167 0.028 Uiso 1 1 calc R U . . .
C56B C 0.3642(4) 0.4133(4) -0.2848(4) 0.0431(14) Uani 1 1 d . . . . .
H56D H 0.398011 0.455886 -0.304826 0.065 Uiso 1 1 calc R U . . .
H56E H 0.366817 0.367466 -0.320496 0.065 Uiso 1 1 calc R U . . .
H56F H 0.305612 0.430479 -0.284816 0.065 Uiso 1 1 calc R U . . .
C65B C 0.2093(3) 0.2834(2) -0.1063(3) 0.0165(8) Uani 1 1 d . . . . .
N61B N 0.1361(2) 0.2605(2) -0.1380(2) 0.0186(7) Uani 1 1 d . . . . .
C61B C 0.1057(3) 0.2031(3) -0.0778(3) 0.0191(8) Uani 1 1 d . . . . .
H61B H 0.081320 0.155733 -0.107052 0.023 Uiso 1 1 calc R U . . .
C62B C 0.0395(3) 0.2405(3) -0.0251(3) 0.0198(9) Uani 1 1 d . . . . .
O62B O 0.0097(2) 0.1995(2) 0.0280(2) 0.0278(7) Uani 1 1 d . . . . .
C63B C 0.1880(3) 0.1800(3) -0.0218(3) 0.0179(8) Uani 1 1 d . . . . .
H63B H 0.176108 0.174755 0.036469 0.021 Uiso 1 1 calc R U . . .
O63B O 0.24319(19) 0.24988(18) -0.03353(18) 0.0186(6) Uani 1 1 d . . . . .
C64B C 0.2320(3) 0.1062(3) -0.0511(3) 0.0229(9) Uani 1 1 d . . . . .
H64D H 0.196797 0.060088 -0.043836 0.034 Uiso 1 1 calc R U . . .
H64E H 0.240718 0.111917 -0.108864 0.034 Uiso 1 1 calc R U . . .
H64F H 0.286574 0.099639 -0.019084 0.034 Uiso 1 1 calc R U . . .
N71B N 0.0179(2) 0.3186(2) -0.0395(2) 0.0190(7) Uani 1 1 d . . . . .
H71C H 0.028820 0.341665 -0.084939 0.023 Uiso 1 1 calc R U . . .
C71B C -0.0238(3) 0.3623(3) 0.0234(3) 0.0183(8) Uani 1 1 d . . . . .
H71D H -0.050390 0.322111 0.057006 0.022 Uiso 1 1 calc R U . . .
C73B C -0.0965(3) 0.4195(3) -0.0107(3) 0.0212(9) Uani 1 1 d . . . . .
H73B H -0.118725 0.444707 0.037721 0.025 Uiso 1 1 calc R U . . .
C74B C -0.1710(3) 0.3725(3) -0.0556(3) 0.0262(10) Uani 1 1 d . . . . .
H74D H -0.187994 0.330418 -0.020072 0.039 Uiso 1 1 calc R U . . .
H74E H -0.218715 0.407790 -0.069282 0.039 Uiso 1 1 calc R U . . .
H74F H -0.153048 0.349632 -0.105788 0.039 Uiso 1 1 calc R U . . .
C75B C -0.0671(3) 0.4867(3) -0.0643(3) 0.0245(9) Uani 1 1 d . . . . .
H75D H -0.020446 0.514931 -0.034357 0.037 Uiso 1 1 calc R U . . .
H75E H -0.048364 0.464781 -0.114516 0.037 Uiso 1 1 calc R U . . .
H75F H -0.114032 0.522938 -0.078010 0.037 Uiso 1 1 calc R U . . .
C85B C 0.0449(3) 0.4039(3) 0.0812(3) 0.0196(8) Uani 1 1 d . . . . .
N81B N 0.1254(2) 0.3825(2) 0.0892(2) 0.0195(7) Uani 1 1 d . . . . .
C81B C 0.1705(3) 0.4273(3) 0.1508(3) 0.0210(9) Uani 1 1 d . . . . .
C82B C 0.2641(3) 0.4143(3) 0.1721(3) 0.0211(9) Uani 1 1 d . . . . .
O82B O 0.3056(2) 0.4549(2) 0.2261(2) 0.0253(7) Uani 1 1 d . . . . .
C83B C 0.1239(3) 0.4825(3) 0.1892(3) 0.0242(9) Uani 1 1 d . . . . .
H83B H 0.145885 0.516600 0.231540 0.029 Uiso 1 1 calc R U . . .
S83B S 0.01937(7) 0.48000(7) 0.14796(7) 0.0243(2) Uani 1 1 d . . . . .


_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
N1C C1C 1.143(7) . ?
C1C C2C 1.457(7) . ?
C2C H2C1 0.9600 . ?
C2C H2C2 0.9600 . ?
C2C H2C3 0.9600 . ?
N11A C82A 1.362(6) . ?
N11A C11A 1.448(5) . ?
N11A H11A 0.8600 . ?
C11A C25A 1.509(6) . ?
C11A C13A 1.539(6) . ?
C11A H11B 0.9800 . ?
C13A C14A 1.507(6) . ?
C13A H13A 0.9700 . ?
C13A H13B 0.9700 . ?
C14A C15A 1.388(7) . ?
C14A C19A 1.394(7) . ?
C15A C16A 1.386(7) . ?
C15A H15A 0.9300 . ?
C16A C17A 1.386(7) . ?
C16A H16A 0.9300 . ?
C17A C18A 1.385(7) . ?
C17A CL1A 1.742(5) . ?
C18A C19A 1.383(7) . ?
C18A H18A 0.9300 . ?
C19A H19A 0.9300 . ?
C25A N21A 1.270(6) . ?
C25A O23A 1.366(6) . ?
N21A C21A 1.471(6) . ?
C21A C22A 1.522(7) . ?
C21A C23A 1.544(7) . ?
C21A H21A 0.9800 . ?
C22A O22A 1.226(6) . ?
C22A N31A 1.345(6) . ?
C23A O23A 1.469(6) . ?
C23A C24A 1.515(8) . ?
C23A H23A 0.9800 . ?
C24A H24A 0.9600 . ?
C24A H24B 0.9600 . ?
C24A H24C 0.9600 . ?
N31A C31A 1.453(6) . ?
N31A H31A 0.8600 . ?
C31A C44A 1.510(6) . ?
C31A C33A 1.530(7) . ?
C31A H31B 0.9800 . ?
C33A C35A 1.529(7) . ?
C33A C34A 1.535(8) . ?
C33A H33A 0.9800 . ?
C34A H34A 0.9600 . ?
C34A H34B 0.9600 . ?
C34A H34C 0.9600 . ?
C35A H35A 0.9600 . ?
C35A H35B 0.9600 . ?
C35A H35C 0.9600 . ?
C44A N41A 1.316(6) . ?
C44A S43A 1.732(5) . ?
N41A C41A 1.385(6) . ?
C41A C43A 1.374(6) . ?
C41A C42A 1.478(6) . ?
C42A O42A 1.233(5) . ?
C42A N51A 1.351(6) . ?
C43A S43A 1.704(5) . ?
C43A H43A 0.9300 . ?
N51A C51A 1.468(6) . ?
N51A H51A 0.8600 . ?
C51A C65A 1.499(6) . ?
C51A C53A 1.537(6) . ?
C51A H51B 0.9800 . ?
C53A C54A 1.528(7) . ?
C53A C55A 1.533(6) . ?
C53A H53A 0.9800 . ?
C54A H54A 0.9600 . ?
C54A H54B 0.9600 . ?
C54A H54C 0.9600 . ?
C55A C56A 1.521(6) . ?
C55A H55A 0.9700 . ?
C55A H55B 0.9700 . ?
C56A H56A 0.9600 . ?
C56A H56B 0.9600 . ?
C56A H56C 0.9600 . ?
C65A N61A 1.275(6) . ?
C65A O63A 1.369(5) . ?
N61A C61A 1.476(6) . ?
C61A C62A 1.525(6) . ?
C61A C63A 1.550(6) . ?
C61A H61A 0.9800 . ?
C62A O62A 1.235(6) . ?
C62A N71A 1.350(6) . ?
C63A O63A 1.471(5) . ?
C63A C64A 1.520(6) . ?
C63A H63A 0.9800 . ?
C64A H64A 0.9600 . ?
C64A H64B 0.9600 . ?
C64A H64C 0.9600 . ?
N71A C71A 1.454(5) . ?
N71A H71A 0.8600 . ?
C71A C84A 1.509(6) . ?
C71A C73A 1.549(6) . ?
C71A H71B 0.9800 . ?
C73A C75A 1.523(6) . ?
C73A C74A 1.524(7) . ?
C73A H73A 0.9800 . ?
C74A H74A 0.9600 . ?
C74A H74B 0.9600 . ?
C74A H74C 0.9600 . ?
C75A H75A 0.9600 . ?
C75A H75B 0.9600 . ?
C75A H75C 0.9600 . ?
C84A N81A 1.307(6) . ?
C84A S83A 1.731(4) . ?
N81A C81A 1.381(6) . ?
C81A C83A 1.362(6) . ?
C81A C82A 1.487(6) . ?
C82A O82A 1.225(6) . ?
C83A S83A 1.714(5) . ?
C83A H83A 0.9300 . ?
N11B C82B 1.354(6) . ?
N11B C11B 1.462(5) . ?
N11B H11C 0.8600 . ?
C11B C25B 1.500(6) . ?
C11B C13B 1.528(6) . ?
C11B H11D 0.9800 . ?
C13B C14B 1.514(6) . ?
C13B H13C 0.9700 . ?
C13B H13D 0.9700 . ?
C14B C19B 1.386(7) . ?
C14B C15B 1.393(7) . ?
C15B C16B 1.395(7) . ?
C15B H15B 0.9300 . ?
C16B C17B 1.370(7) . ?
C16B H16B 0.9300 . ?
C17B C18B 1.383(7) . ?
C17B CL2B 1.747(5) . ?
C18B C19B 1.388(7) . ?
C18B H18B 0.9300 . ?
C19B H19B 0.9300 . ?
C25B N21B 1.274(6) . ?
C25B O23B 1.371(5) . ?
N21B C21B 1.470(6) . ?
C21B C22B 1.531(6) . ?
C21B C23B 1.544(6) . ?
C21B H21B 0.9800 . ?
C22B O22B 1.222(6) . ?
C22B N31B 1.349(6) . ?
C23B O23B 1.474(5) . ?
C23B C24B 1.515(7) . ?
C23B H23B 0.9800 . ?
C24B H24D 0.9600 . ?
C24B H24E 0.9600 . ?
C24B H24F 0.9600 . ?
N31B C31B 1.459(5) . ?
N31B H31C 0.8600 . ?
C31B C44B 1.515(6) . ?
C31B C33B 1.535(6) . ?
C31B H31D 0.9800 . ?
C33B C35B 1.524(7) . ?
C33B C34B 1.531(6) . ?
C33B H33B 0.9800 . ?
C34B H34D 0.9600 . ?
C34B H34E 0.9600 . ?
C34B H34F 0.9600 . ?
C35B H35D 0.9600 . ?
C35B H35E 0.9600 . ?
C35B H35F 0.9600 . ?
C44B N41B 1.305(6) . ?
C44B S43B 1.732(5) . ?
N41B C41B 1.379(6) . ?
C41B C43B 1.357(6) . ?
C41B C42B 1.484(6) . ?
C42B O42B 1.231(5) . ?
C42B N51B 1.349(6) . ?
C43B S43B 1.701(5) . ?
C43B H43B 0.9300 . ?
N51B C51B 1.456(5) . ?
N51B H51C 0.8600 . ?
C51B C65B 1.506(6) . ?
C51B C53B 1.530(6) . ?
C51B H51D 0.9800 . ?
C53B C54B 1.525(6) . ?
C53B C55B 1.530(6) . ?
C53B H53B 0.9800 . ?
C54B H54D 0.9600 . ?
C54B H54E 0.9600 . ?
C54B H54F 0.9600 . ?
C55B C56B 1.511(7) . ?
C55B H55C 0.9700 . ?
C55B H55D 0.9700 . ?
C56B H56D 0.9600 . ?
C56B H56E 0.9600 . ?
C56B H56F 0.9600 . ?
C65B N61B 1.268(6) . ?
C65B O63B 1.362(5) . ?
N61B C61B 1.473(6) . ?
C61B C62B 1.533(6) . ?
C61B C63B 1.548(6) . ?
C61B H61B 0.9800 . ?
C62B O62B 1.223(6) . ?
C62B N71B 1.362(6) . ?
C63B O63B 1.473(5) . ?
C63B C64B 1.509(6) . ?
C63B H63B 0.9800 . ?
C64B H64D 0.9600 . ?
C64B H64E 0.9600 . ?
C64B H64F 0.9600 . ?
N71B C71B 1.453(5) . ?
N71B H71C 0.8600 . ?
C71B C85B 1.523(6) . ?
C71B C73B 1.544(6) . ?
C71B H71D 0.9800 . ?
C73B C75B 1.514(6) . ?
C73B C74B 1.529(6) . ?
C73B H73B 0.9800 . ?
C74B H74D 0.9600 . ?
C74B H74E 0.9600 . ?
C74B H74F 0.9600 . ?
C75B H75D 0.9600 . ?
C75B H75E 0.9600 . ?
C75B H75F 0.9600 . ?
C85B N81B 1.303(6) . ?
C85B S83B 1.737(4) . ?
N81B C81B 1.382(6) . ?
C81B C83B 1.359(7) . ?
C81B C82B 1.486(6) . ?
C82B O82B 1.237(5) . ?
C83B S83B 1.705(5) . ?
C83B H83B 0.9300 . ?

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
N1C C1C C2C 179.6(6) . . ?
C1C C2C H2C1 109.5 . . ?
C1C C2C H2C2 109.5 . . ?
H2C1 C2C H2C2 109.5 . . ?
C1C C2C H2C3 109.5 . . ?
H2C1 C2C H2C3 109.5 . . ?
H2C2 C2C H2C3 109.5 . . ?
C82A N11A C11A 119.8(4) . . ?
C82A N11A H11A 120.1 . . ?
C11A N11A H11A 120.1 . . ?
N11A C11A C25A 109.6(4) . . ?
N11A C11A C13A 109.6(4) . . ?
C25A C11A C13A 112.6(4) . . ?
N11A C11A H11B 108.3 . . ?
C25A C11A H11B 108.3 . . ?
C13A C11A H11B 108.3 . . ?
C14A C13A C11A 110.8(4) . . ?
C14A C13A H13A 109.5 . . ?
C11A C13A H13A 109.5 . . ?
C14A C13A H13B 109.5 . . ?
C11A C13A H13B 109.5 . . ?
H13A C13A H13B 108.1 . . ?
C15A C14A C19A 118.5(4) . . ?
C15A C14A C13A 120.4(4) . . ?
C19A C14A C13A 121.0(4) . . ?
C16A C15A C14A 121.0(5) . . ?
C16A C15A H15A 119.5 . . ?
C14A C15A H15A 119.5 . . ?
C17A C16A C15A 119.3(5) . . ?
C17A C16A H16A 120.3 . . ?
C15A C16A H16A 120.3 . . ?
C16A C17A C18A 120.8(4) . . ?
C16A C17A CL1A 119.2(4) . . ?
C18A C17A CL1A 119.9(4) . . ?
C19A C18A C17A 119.1(5) . . ?
C19A C18A H18A 120.5 . . ?
C17A C18A H18A 120.5 . . ?
C18A C19A C14A 121.3(4) . . ?
C18A C19A H19A 119.4 . . ?
C14A C19A H19A 119.4 . . ?
N21A C25A O23A 118.1(4) . . ?
N21A C25A C11A 125.6(4) . . ?
O23A C25A C11A 116.1(4) . . ?
C25A N21A C21A 106.3(4) . . ?
N21A C21A C22A 113.0(4) . . ?
N21A C21A C23A 105.0(4) . . ?
C22A C21A C23A 109.2(4) . . ?
N21A C21A H21A 109.9 . . ?
C22A C21A H21A 109.9 . . ?
C23A C21A H21A 109.9 . . ?
O22A C22A N31A 123.7(5) . . ?
O22A C22A C21A 120.0(5) . . ?
N31A C22A C21A 116.1(4) . . ?
O23A C23A C24A 109.5(5) . . ?
O23A C23A C21A 101.8(4) . . ?
C24A C23A C21A 113.5(4) . . ?
O23A C23A H23A 110.6 . . ?
C24A C23A H23A 110.6 . . ?
C21A C23A H23A 110.6 . . ?
C25A O23A C23A 106.1(4) . . ?
C23A C24A H24A 109.5 . . ?
C23A C24A H24B 109.5 . . ?
H24A C24A H24B 109.5 . . ?
C23A C24A H24C 109.5 . . ?
H24A C24A H24C 109.5 . . ?
H24B C24A H24C 109.5 . . ?
C22A N31A C31A 120.8(4) . . ?
C22A N31A H31A 119.6 . . ?
C31A N31A H31A 119.6 . . ?
N31A C31A C44A 108.8(4) . . ?
N31A C31A C33A 114.7(4) . . ?
C44A C31A C33A 114.9(4) . . ?
N31A C31A H31B 105.9 . . ?
C44A C31A H31B 105.9 . . ?
C33A C31A H31B 105.9 . . ?
C35A C33A C31A 109.1(5) . . ?
C35A C33A C34A 110.4(4) . . ?
C31A C33A C34A 113.6(4) . . ?
C35A C33A H33A 107.9 . . ?
C31A C33A H33A 107.9 . . ?
C34A C33A H33A 107.9 . . ?
C33A C34A H34A 109.5 . . ?
C33A C34A H34B 109.5 . . ?
H34A C34A H34B 109.5 . . ?
C33A C34A H34C 109.5 . . ?
H34A C34A H34C 109.5 . . ?
H34B C34A H34C 109.5 . . ?
C33A C35A H35A 109.5 . . ?
C33A C35A H35B 109.5 . . ?
H35A C35A H35B 109.5 . . ?
C33A C35A H35C 109.5 . . ?
H35A C35A H35C 109.5 . . ?
H35B C35A H35C 109.5 . . ?
N41A C44A C31A 123.8(4) . . ?
N41A C44A S43A 113.9(3) . . ?
C31A C44A S43A 122.1(3) . . ?
C44A N41A C41A 110.4(4) . . ?
C43A C41A N41A 115.8(4) . . ?
C43A C41A C42A 122.3(4) . . ?
N41A C41A C42A 121.8(4) . . ?
O42A C42A N51A 122.6(4) . . ?
O42A C42A C41A 120.9(4) . . ?
N51A C42A C41A 116.5(4) . . ?
C41A C43A S43A 109.3(3) . . ?
C41A C43A H43A 125.4 . . ?
S43A C43A H43A 125.4 . . ?
C43A S43A C44A 90.6(2) . . ?
C42A N51A C51A 119.8(4) . . ?
C42A N51A H51A 120.1 . . ?
C51A N51A H51A 120.1 . . ?
N51A C51A C65A 109.4(3) . . ?
N51A C51A C53A 112.1(4) . . ?
C65A C51A C53A 114.1(4) . . ?
N51A C51A H51B 106.9 . . ?
C65A C51A H51B 106.9 . . ?
C53A C51A H51B 106.9 . . ?
C54A C53A C55A 112.2(4) . . ?
C54A C53A C51A 108.7(4) . . ?
C55A C53A C51A 109.3(4) . . ?
C54A C53A H53A 108.8 . . ?
C55A C53A H53A 108.8 . . ?
C51A C53A H53A 108.8 . . ?
C53A C54A H54A 109.5 . . ?
C53A C54A H54B 109.5 . . ?
H54A C54A H54B 109.5 . . ?
C53A C54A H54C 109.5 . . ?
H54A C54A H54C 109.5 . . ?
H54B C54A H54C 109.5 . . ?
C56A C55A C53A 114.8(4) . . ?
C56A C55A H55A 108.6 . . ?
C53A C55A H55A 108.6 . . ?
C56A C55A H55B 108.6 . . ?
C53A C55A H55B 108.6 . . ?
H55A C55A H55B 107.6 . . ?
C55A C56A H56A 109.5 . . ?
C55A C56A H56B 109.5 . . ?
H56A C56A H56B 109.5 . . ?
C55A C56A H56C 109.5 . . ?
H56A C56A H56C 109.5 . . ?
H56B C56A H56C 109.5 . . ?
N61A C65A O63A 118.8(4) . . ?
N61A C65A C51A 125.4(4) . . ?
O63A C65A C51A 115.7(4) . . ?
C65A N61A C61A 106.0(4) . . ?
N61A C61A C62A 112.0(4) . . ?
N61A C61A C63A 104.1(3) . . ?
C62A C61A C63A 109.3(4) . . ?
N61A C61A H61A 110.4 . . ?
C62A C61A H61A 110.4 . . ?
C63A C61A H61A 110.4 . . ?
O62A C62A N71A 123.9(4) . . ?
O62A C62A C61A 119.0(4) . . ?
N71A C62A C61A 117.1(4) . . ?
O63A C63A C64A 108.4(4) . . ?
O63A C63A C61A 102.4(3) . . ?
C64A C63A C61A 114.2(4) . . ?
O63A C63A H63A 110.5 . . ?
C64A C63A H63A 110.5 . . ?
C61A C63A H63A 110.5 . . ?
C65A O63A C63A 104.8(3) . . ?
C63A C64A H64A 109.5 . . ?
C63A C64A H64B 109.5 . . ?
H64A C64A H64B 109.5 . . ?
C63A C64A H64C 109.5 . . ?
H64A C64A H64C 109.5 . . ?
H64B C64A H64C 109.5 . . ?
C62A N71A C71A 120.0(4) . . ?
C62A N71A H71A 120.0 . . ?
C71A N71A H71A 120.0 . . ?
N71A C71A C84A 108.6(3) . . ?
N71A C71A C73A 113.0(4) . . ?
C84A C71A C73A 113.6(4) . . ?
N71A C71A H71B 107.1 . . ?
C84A C71A H71B 107.1 . . ?
C73A C71A H71B 107.1 . . ?
C75A C73A C74A 112.2(4) . . ?
C75A C73A C71A 109.2(4) . . ?
C74A C73A C71A 113.4(4) . . ?
C75A C73A H73A 107.2 . . ?
C74A C73A H73A 107.2 . . ?
C71A C73A H73A 107.2 . . ?
C73A C74A H74A 109.5 . . ?
C73A C74A H74B 109.5 . . ?
H74A C74A H74B 109.5 . . ?
C73A C74A H74C 109.5 . . ?
H74A C74A H74C 109.5 . . ?
H74B C74A H74C 109.5 . . ?
C73A C75A H75A 109.5 . . ?
C73A C75A H75B 109.5 . . ?
H75A C75A H75B 109.5 . . ?
C73A C75A H75C 109.5 . . ?
H75A C75A H75C 109.5 . . ?
H75B C75A H75C 109.5 . . ?
N81A C84A C71A 122.6(4) . . ?
N81A C84A S83A 114.9(3) . . ?
C71A C84A S83A 122.2(3) . . ?
C84A N81A C81A 109.8(4) . . ?
C83A C81A N81A 116.3(4) . . ?
C83A C81A C82A 122.3(4) . . ?
N81A C81A C82A 121.4(4) . . ?
O82A C82A N11A 123.1(4) . . ?
O82A C82A C81A 121.5(4) . . ?
N11A C82A C81A 115.3(4) . . ?
C81A C83A S83A 109.4(3) . . ?
C81A C83A H83A 125.3 . . ?
S83A C83A H83A 125.3 . . ?
C83A S83A C84A 89.5(2) . . ?
C82B N11B C11B 120.4(4) . . ?
C82B N11B H11C 119.8 . . ?
C11B N11B H11C 119.8 . . ?
N11B C11B C25B 110.0(3) . . ?
N11B C11B C13B 109.6(4) . . ?
C25B C11B C13B 113.4(4) . . ?
N11B C11B H11D 107.9 . . ?
C25B C11B H11D 107.9 . . ?
C13B C11B H11D 107.9 . . ?
C14B C13B C11B 112.4(4) . . ?
C14B C13B H13C 109.1 . . ?
C11B C13B H13C 109.1 . . ?
C14B C13B H13D 109.1 . . ?
C11B C13B H13D 109.1 . . ?
H13C C13B H13D 107.9 . . ?
C19B C14B C15B 117.7(4) . . ?
C19B C14B C13B 120.7(4) . . ?
C15B C14B C13B 121.5(4) . . ?
C14B C15B C16B 121.8(5) . . ?
C14B C15B H15B 119.1 . . ?
C16B C15B H15B 119.1 . . ?
C17B C16B C15B 118.5(5) . . ?
C17B C16B H16B 120.8 . . ?
C15B C16B H16B 120.8 . . ?
C16B C17B C18B 121.5(5) . . ?
C16B C17B CL2B 119.3(4) . . ?
C18B C17B CL2B 119.2(4) . . ?
C17B C18B C19B 119.0(4) . . ?
C17B C18B H18B 120.5 . . ?
C19B C18B H18B 120.5 . . ?
C14B C19B C18B 121.5(5) . . ?
C14B C19B H19B 119.3 . . ?
C18B C19B H19B 119.3 . . ?
N21B C25B O23B 118.2(4) . . ?
N21B C25B C11B 126.2(4) . . ?
O23B C25B C11B 115.5(4) . . ?
C25B N21B C21B 106.4(4) . . ?
N21B C21B C22B 112.7(3) . . ?
N21B C21B C23B 104.7(3) . . ?
C22B C21B C23B 109.5(4) . . ?
N21B C21B H21B 109.9 . . ?
C22B C21B H21B 109.9 . . ?
C23B C21B H21B 109.9 . . ?
O22B C22B N31B 124.3(4) . . ?
O22B C22B C21B 119.0(4) . . ?
N31B C22B C21B 116.5(4) . . ?
O23B C23B C24B 109.1(4) . . ?
O23B C23B C21B 102.2(3) . . ?
C24B C23B C21B 113.4(4) . . ?
O23B C23B H23B 110.6 . . ?
C24B C23B H23B 110.6 . . ?
C21B C23B H23B 110.6 . . ?
C25B O23B C23B 105.3(3) . . ?
C23B C24B H24D 109.5 . . ?
C23B C24B H24E 109.5 . . ?
H24D C24B H24E 109.5 . . ?
C23B C24B H24F 109.5 . . ?
H24D C24B H24F 109.5 . . ?
H24E C24B H24F 109.5 . . ?
C22B N31B C31B 120.3(4) . . ?
C22B N31B H31C 119.8 . . ?
C31B N31B H31C 119.8 . . ?
N31B C31B C44B 108.0(3) . . ?
N31B C31B C33B 114.4(4) . . ?
C44B C31B C33B 114.9(4) . . ?
N31B C31B H31D 106.3 . . ?
C44B C31B H31D 106.3 . . ?
C33B C31B H31D 106.3 . . ?
C35B C33B C34B 111.6(4) . . ?
C35B C33B C31B 114.0(4) . . ?
C34B C33B C31B 109.0(4) . . ?
C35B C33B H33B 107.3 . . ?
C34B C33B H33B 107.3 . . ?
C31B C33B H33B 107.3 . . ?
C33B C34B H34D 109.5 . . ?
C33B C34B H34E 109.5 . . ?
H34D C34B H34E 109.5 . . ?
C33B C34B H34F 109.5 . . ?
H34D C34B H34F 109.5 . . ?
H34E C34B H34F 109.5 . . ?
C33B C35B H35D 109.5 . . ?
C33B C35B H35E 109.5 . . ?
H35D C35B H35E 109.5 . . ?
C33B C35B H35F 109.5 . . ?
H35D C35B H35F 109.5 . . ?
H35E C35B H35F 109.5 . . ?
N41B C44B C31B 123.4(4) . . ?
N41B C44B S43B 114.6(3) . . ?
C31B C44B S43B 121.8(3) . . ?
C44B N41B C41B 109.9(4) . . ?
C43B C41B N41B 116.0(4) . . ?
C43B C41B C42B 122.6(4) . . ?
N41B C41B C42B 121.3(4) . . ?
O42B C42B N51B 122.8(4) . . ?
O42B C42B C41B 121.9(4) . . ?
N51B C42B C41B 115.3(4) . . ?
C41B C43B S43B 109.9(3) . . ?
C41B C43B H43B 125.1 . . ?
S43B C43B H43B 125.1 . . ?
C43B S43B C44B 89.6(2) . . ?
C42B N51B C51B 119.7(3) . . ?
C42B N51B H51C 120.2 . . ?
C51B N51B H51C 120.2 . . ?
N51B C51B C65B 109.6(3) . . ?
N51B C51B C53B 111.4(3) . . ?
C65B C51B C53B 113.0(4) . . ?
N51B C51B H51D 107.5 . . ?
C65B C51B H51D 107.5 . . ?
C53B C51B H51D 107.5 . . ?
C54B C53B C51B 110.1(3) . . ?
C54B C53B C55B 112.2(4) . . ?
C51B C53B C55B 111.0(4) . . ?
C54B C53B H53B 107.8 . . ?
C51B C53B H53B 107.8 . . ?
C55B C53B H53B 107.8 . . ?
C53B C54B H54D 109.5 . . ?
C53B C54B H54E 109.5 . . ?
H54D C54B H54E 109.5 . . ?
C53B C54B H54F 109.5 . . ?
H54D C54B H54F 109.5 . . ?
H54E C54B H54F 109.5 . . ?
C56B C55B C53B 115.6(4) . . ?
C56B C55B H55C 108.4 . . ?
C53B C55B H55C 108.4 . . ?
C56B C55B H55D 108.4 . . ?
C53B C55B H55D 108.4 . . ?
H55C C55B H55D 107.4 . . ?
C55B C56B H56D 109.5 . . ?
C55B C56B H56E 109.5 . . ?
H56D C56B H56E 109.5 . . ?
C55B C56B H56F 109.5 . . ?
H56D C56B H56F 109.5 . . ?
H56E C56B H56F 109.5 . . ?
N61B C65B O63B 119.1(4) . . ?
N61B C65B C51B 125.2(4) . . ?
O63B C65B C51B 115.6(4) . . ?
C65B N61B C61B 105.4(4) . . ?
N61B C61B C62B 112.2(3) . . ?
N61B C61B C63B 104.2(3) . . ?
C62B C61B C63B 110.1(3) . . ?
N61B C61B H61B 110.1 . . ?
C62B C61B H61B 110.1 . . ?
C63B C61B H61B 110.1 . . ?
O62B C62B N71B 123.4(4) . . ?
O62B C62B C61B 118.9(4) . . ?
N71B C62B C61B 117.7(4) . . ?
O63B C63B C64B 108.5(3) . . ?
O63B C63B C61B 101.0(3) . . ?
C64B C63B C61B 113.5(4) . . ?
O63B C63B H63B 111.1 . . ?
C64B C63B H63B 111.1 . . ?
C61B C63B H63B 111.1 . . ?
C65B O63B C63B 104.6(3) . . ?
C63B C64B H64D 109.5 . . ?
C63B C64B H64E 109.5 . . ?
H64D C64B H64E 109.5 . . ?
C63B C64B H64F 109.5 . . ?
H64D C64B H64F 109.5 . . ?
H64E C64B H64F 109.5 . . ?
C62B N71B C71B 118.9(4) . . ?
C62B N71B H71C 120.6 . . ?
C71B N71B H71C 120.6 . . ?
N71B C71B C85B 108.6(3) . . ?
N71B C71B C73B 115.2(4) . . ?
C85B C71B C73B 112.8(4) . . ?
N71B C71B H71D 106.5 . . ?
C85B C71B H71D 106.5 . . ?
C73B C71B H71D 106.5 . . ?
C75B C73B C74B 111.6(4) . . ?
C75B C73B C71B 114.2(4) . . ?
C74B C73B C71B 110.6(4) . . ?
C75B C73B H73B 106.7 . . ?
C74B C73B H73B 106.7 . . ?
C71B C73B H73B 106.7 . . ?
C73B C74B H74D 109.5 . . ?
C73B C74B H74E 109.5 . . ?
H74D C74B H74E 109.5 . . ?
C73B C74B H74F 109.5 . . ?
H74D C74B H74F 109.5 . . ?
H74E C74B H74F 109.5 . . ?
C73B C75B H75D 109.5 . . ?
C73B C75B H75E 109.5 . . ?
H75D C75B H75E 109.5 . . ?
C73B C75B H75F 109.5 . . ?
H75D C75B H75F 109.5 . . ?
H75E C75B H75F 109.5 . . ?
N81B C85B C71B 123.6(4) . . ?
N81B C85B S83B 114.6(3) . . ?
C71B C85B S83B 121.6(3) . . ?
C85B N81B C81B 110.1(4) . . ?
C83B C81B N81B 115.9(4) . . ?
C83B C81B C82B 123.4(4) . . ?
N81B C81B C82B 120.7(4) . . ?
O82B C82B N11B 122.4(4) . . ?
O82B C82B C81B 121.5(4) . . ?
N11B C82B C81B 116.1(4) . . ?
C81B C83B S83B 109.9(4) . . ?
C81B C83B H83B 125.1 . . ?
S83B C83B H83B 125.1 . . ?
C83B S83B C85B 89.5(2) . . ?

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
C82A N11A C11A C25A -74.7(5) . . . . ?
C82A N11A C11A C13A 161.2(4) . . . . ?
N11A C11A C13A C14A -173.9(4) . . . . ?
C25A C11A C13A C14A 63.8(5) . . . . ?
C11A C13A C14A C15A 78.6(6) . . . . ?
C11A C13A C14A C19A -99.0(5) . . . . ?
C19A C14A C15A C16A 0.3(8) . . . . ?
C13A C14A C15A C16A -177.2(5) . . . . ?
C14A C15A C16A C17A 0.4(8) . . . . ?
C15A C16A C17A C18A -0.9(8) . . . . ?
C15A C16A C17A CL1A -179.8(4) . . . . ?
C16A C17A C18A C19A 0.6(7) . . . . ?
CL1A C17A C18A C19A 179.5(4) . . . . ?
C17A C18A C19A C14A 0.2(7) . . . . ?
C15A C14A C19A C18A -0.6(7) . . . . ?
C13A C14A C19A C18A 177.0(4) . . . . ?
N11A C11A C25A N21A 113.4(5) . . . . ?
C13A C11A C25A N21A -124.4(5) . . . . ?
N11A C11A C25A O23A -62.5(5) . . . . ?
C13A C11A C25A O23A 59.8(5) . . . . ?
O23A C25A N21A C21A 5.4(5) . . . . ?
C11A C25A N21A C21A -170.3(4) . . . . ?
C25A N21A C21A C22A 105.2(5) . . . . ?
C25A N21A C21A C23A -13.7(5) . . . . ?
N21A C21A C22A O22A 170.9(4) . . . . ?
C23A C21A C22A O22A -72.7(6) . . . . ?
N21A C21A C22A N31A -13.3(6) . . . . ?
C23A C21A C22A N31A 103.1(5) . . . . ?
N21A C21A C23A O23A 16.3(5) . . . . ?
C22A C21A C23A O23A -105.1(4) . . . . ?
N21A C21A C23A C24A -101.3(5) . . . . ?
C22A C21A C23A C24A 137.4(5) . . . . ?
N21A C25A O23A C23A 5.9(5) . . . . ?
C11A C25A O23A C23A -178.0(4) . . . . ?
C24A C23A O23A C25A 107.0(5) . . . . ?
C21A C23A O23A C25A -13.4(5) . . . . ?
O22A C22A N31A C31A 19.3(7) . . . . ?
C21A C22A N31A C31A -156.3(4) . . . . ?
C22A N31A C31A C44A 104.9(5) . . . . ?
C22A N31A C31A C33A -124.8(5) . . . . ?
N31A C31A C33A C35A 64.7(5) . . . . ?
C44A C31A C33A C35A -168.1(4) . . . . ?
N31A C31A C33A C34A -58.9(6) . . . . ?
C44A C31A C33A C34A 68.3(5) . . . . ?
N31A C31A C44A N41A -22.6(6) . . . . ?
C33A C31A C44A N41A -152.8(4) . . . . ?
N31A C31A C44A S43A 163.2(3) . . . . ?
C33A C31A C44A S43A 33.0(5) . . . . ?
C31A C44A N41A C41A -173.9(4) . . . . ?
S43A C44A N41A C41A 0.7(5) . . . . ?
C44A N41A C41A C43A 0.1(5) . . . . ?
C44A N41A C41A C42A -179.4(4) . . . . ?
C43A C41A C42A O42A -4.9(7) . . . . ?
N41A C41A C42A O42A 174.4(4) . . . . ?
C43A C41A C42A N51A 173.4(4) . . . . ?
N41A C41A C42A N51A -7.2(6) . . . . ?
N41A C41A C43A S43A -0.8(5) . . . . ?
C42A C41A C43A S43A 178.6(3) . . . . ?
C41A C43A S43A C44A 0.9(4) . . . . ?
N41A C44A S43A C43A -1.0(4) . . . . ?
C31A C44A S43A C43A 173.7(4) . . . . ?
O42A C42A N51A C51A 5.7(6) . . . . ?
C41A C42A N51A C51A -172.7(4) . . . . ?
C42A N51A C51A C65A -76.8(5) . . . . ?
C42A N51A C51A C53A 155.6(4) . . . . ?
N51A C51A C53A C54A 176.8(4) . . . . ?
C65A C51A C53A C54A 51.7(5) . . . . ?
N51A C51A C53A C55A -60.4(5) . . . . ?
C65A C51A C53A C55A 174.5(4) . . . . ?
C54A C53A C55A C56A -58.3(6) . . . . ?
C51A C53A C55A C56A -179.0(4) . . . . ?
N51A C51A C65A N61A 116.7(5) . . . . ?
C53A C51A C65A N61A -116.9(5) . . . . ?
N51A C51A C65A O63A -61.0(5) . . . . ?
C53A C51A C65A O63A 65.5(5) . . . . ?
O63A C65A N61A C61A 5.3(5) . . . . ?
C51A C65A N61A C61A -172.2(4) . . . . ?
C65A N61A C61A C62A 102.6(4) . . . . ?
C65A N61A C61A C63A -15.4(4) . . . . ?
N61A C61A C62A O62A 177.0(4) . . . . ?
C63A C61A C62A O62A -68.2(5) . . . . ?
N61A C61A C62A N71A -5.4(6) . . . . ?
C63A C61A C62A N71A 109.4(4) . . . . ?
N61A C61A C63A O63A 19.2(4) . . . . ?
C62A C61A C63A O63A -100.5(4) . . . . ?
N61A C61A C63A C64A -97.8(4) . . . . ?
C62A C61A C63A C64A 142.5(4) . . . . ?
N61A C65A O63A C63A 7.9(5) . . . . ?
C51A C65A O63A C63A -174.3(3) . . . . ?
C64A C63A O63A C65A 104.8(4) . . . . ?
C61A C63A O63A C65A -16.3(4) . . . . ?
O62A C62A N71A C71A 19.9(7) . . . . ?
C61A C62A N71A C71A -157.6(4) . . . . ?
C62A N71A C71A C84A 99.5(5) . . . . ?
C62A N71A C71A C73A -133.6(4) . . . . ?
N71A C71A C73A C75A 69.9(5) . . . . ?
C84A C71A C73A C75A -165.9(4) . . . . ?
N71A C71A C73A C74A -56.0(5) . . . . ?
C84A C71A C73A C74A 68.2(5) . . . . ?
N71A C71A C84A N81A -30.3(6) . . . . ?
C73A C71A C84A N81A -156.9(4) . . . . ?
N71A C71A C84A S83A 155.7(3) . . . . ?
C73A C71A C84A S83A 29.1(5) . . . . ?
C71A C84A N81A C81A -174.0(4) . . . . ?
S83A C84A N81A C81A 0.4(5) . . . . ?
C84A N81A C81A C83A 0.1(5) . . . . ?
C84A N81A C81A C82A 179.4(4) . . . . ?
C11A N11A C82A O82A 4.6(6) . . . . ?
C11A N11A C82A C81A -173.7(4) . . . . ?
C83A C81A C82A O82A 4.8(6) . . . . ?
N81A C81A C82A O82A -174.5(4) . . . . ?
C83A C81A C82A N11A -176.8(4) . . . . ?
N81A C81A C82A N11A 3.9(6) . . . . ?
N81A C81A C83A S83A -0.5(5) . . . . ?
C82A C81A C83A S83A -179.9(3) . . . . ?
C81A C83A S83A C84A 0.6(3) . . . . ?
N81A C84A S83A C83A -0.6(4) . . . . ?
C71A C84A S83A C83A 173.9(4) . . . . ?
C82B N11B C11B C25B -75.1(5) . . . . ?
C82B N11B C11B C13B 159.6(4) . . . . ?
N11B C11B C13B C14B -171.9(4) . . . . ?
C25B C11B C13B C14B 64.7(5) . . . . ?
C11B C13B C14B C19B 77.8(6) . . . . ?
C11B C13B C14B C15B -102.9(5) . . . . ?
C19B C14B C15B C16B 1.3(8) . . . . ?
C13B C14B C15B C16B -178.0(5) . . . . ?
C14B C15B C16B C17B 0.5(8) . . . . ?
C15B C16B C17B C18B -1.6(8) . . . . ?
C15B C16B C17B CL2B 177.7(4) . . . . ?
C16B C17B C18B C19B 1.0(8) . . . . ?
CL2B C17B C18B C19B -178.4(4) . . . . ?
C15B C14B C19B C18B -2.0(8) . . . . ?
C13B C14B C19B C18B 177.3(5) . . . . ?
C17B C18B C19B C14B 0.9(8) . . . . ?
N11B C11B C25B N21B 111.4(5) . . . . ?
C13B C11B C25B N21B -125.4(5) . . . . ?
N11B C11B C25B O23B -65.3(5) . . . . ?
C13B C11B C25B O23B 57.9(5) . . . . ?
O23B C25B N21B C21B 4.8(5) . . . . ?
C11B C25B N21B C21B -171.8(4) . . . . ?
C25B N21B C21B C22B 104.9(4) . . . . ?
C25B N21B C21B C23B -14.0(4) . . . . ?
N21B C21B C22B O22B 169.0(4) . . . . ?
C23B C21B C22B O22B -74.8(5) . . . . ?
N21B C21B C22B N31B -15.3(5) . . . . ?
C23B C21B C22B N31B 100.8(4) . . . . ?
N21B C21B C23B O23B 17.4(4) . . . . ?
C22B C21B C23B O23B -103.7(4) . . . . ?
N21B C21B C23B C24B -99.9(4) . . . . ?
C22B C21B C23B C24B 139.0(4) . . . . ?
N21B C25B O23B C23B 7.1(5) . . . . ?
C11B C25B O23B C23B -175.9(4) . . . . ?
C24B C23B O23B C25B 105.6(4) . . . . ?
C21B C23B O23B C25B -14.7(4) . . . . ?
O22B C22B N31B C31B 19.1(6) . . . . ?
C21B C22B N31B C31B -156.3(4) . . . . ?
C22B N31B C31B C44B 106.2(4) . . . . ?
C22B N31B C31B C33B -124.5(4) . . . . ?
N31B C31B C33B C35B -62.9(5) . . . . ?
C44B C31B C33B C35B 62.9(5) . . . . ?
N31B C31B C33B C34B 62.5(5) . . . . ?
C44B C31B C33B C34B -171.7(4) . . . . ?
N31B C31B C44B N41B -23.3(6) . . . . ?
C33B C31B C44B N41B -152.3(4) . . . . ?
N31B C31B C44B S43B 162.9(3) . . . . ?
C33B C31B C44B S43B 33.9(5) . . . . ?
C31B C44B N41B C41B -173.7(4) . . . . ?
S43B C44B N41B C41B 0.5(5) . . . . ?
C44B N41B C41B C43B 0.7(6) . . . . ?
C44B N41B C41B C42B 178.3(4) . . . . ?
C43B C41B C42B O42B -4.0(7) . . . . ?
N41B C41B C42B O42B 178.5(4) . . . . ?
C43B C41B C42B N51B 175.2(4) . . . . ?
N41B C41B C42B N51B -2.2(6) . . . . ?
N41B C41B C43B S43B -1.5(5) . . . . ?
C42B C41B C43B S43B -179.1(3) . . . . ?
C41B C43B S43B C44B 1.4(4) . . . . ?
N41B C44B S43B C43B -1.2(4) . . . . ?
C31B C44B S43B C43B 173.2(4) . . . . ?
O42B C42B N51B C51B 2.4(6) . . . . ?
C41B C42B N51B C51B -176.9(4) . . . . ?
C42B N51B C51B C65B -74.9(5) . . . . ?
C42B N51B C51B C53B 159.2(4) . . . . ?
N51B C51B C53B C54B 174.3(4) . . . . ?
C65B C51B C53B C54B 50.3(5) . . . . ?
N51B C51B C53B C55B -60.8(5) . . . . ?
C65B C51B C53B C55B 175.2(3) . . . . ?
C54B C53B C55B C56B 55.7(6) . . . . ?
C51B C53B C55B C56B -68.0(5) . . . . ?
N51B C51B C65B N61B 110.4(5) . . . . ?
C53B C51B C65B N61B -124.7(4) . . . . ?
N51B C51B C65B O63B -65.5(4) . . . . ?
C53B C51B C65B O63B 59.4(5) . . . . ?
O63B C65B N61B C61B 3.8(5) . . . . ?
C51B C65B N61B C61B -172.0(4) . . . . ?
C65B N61B C61B C62B 101.9(4) . . . . ?
C65B N61B C61B C63B -17.2(4) . . . . ?
N61B C61B C62B O62B -179.2(4) . . . . ?
C63B C61B C62B O62B -63.7(5) . . . . ?
N61B C61B C62B N71B -0.1(5) . . . . ?
C63B C61B C62B N71B 115.4(4) . . . . ?
N61B C61B C63B O63B 23.2(4) . . . . ?
C62B C61B C63B O63B -97.3(4) . . . . ?
N61B C61B C63B C64B -92.7(4) . . . . ?
C62B C61B C63B C64B 146.8(4) . . . . ?
N61B C65B O63B C63B 12.2(5) . . . . ?
C51B C65B O63B C63B -171.7(3) . . . . ?
C64B C63B O63B C65B 98.7(4) . . . . ?
C61B C63B O63B C65B -20.9(4) . . . . ?
O62B C62B N71B C71B 16.8(6) . . . . ?
C61B C62B N71B C71B -162.2(4) . . . . ?
C62B N71B C71B C85B 92.1(4) . . . . ?
C62B N71B C71B C73B -140.3(4) . . . . ?
N71B C71B C73B C75B -62.5(5) . . . . ?
C85B C71B C73B C75B 63.0(5) . . . . ?
N71B C71B C73B C74B 64.3(5) . . . . ?
C85B C71B C73B C74B -170.1(4) . . . . ?
N71B C71B C85B N81B -20.5(6) . . . . ?
C73B C71B C85B N81B -149.5(4) . . . . ?
N71B C71B C85B S83B 164.5(3) . . . . ?
C73B C71B C85B S83B 35.5(5) . . . . ?
C71B C85B N81B C81B -175.2(4) . . . . ?
S83B C85B N81B C81B 0.1(5) . . . . ?
C85B N81B C81B C83B -0.1(5) . . . . ?
C85B N81B C81B C82B -179.9(4) . . . . ?
C11B N11B C82B O82B 4.1(7) . . . . ?
C11B N11B C82B C81B -174.9(4) . . . . ?
C83B C81B C82B O82B -1.0(7) . . . . ?
N81B C81B C82B O82B 178.7(4) . . . . ?
C83B C81B C82B N11B 178.0(4) . . . . ?
N81B C81B C82B N11B -2.3(6) . . . . ?
N81B C81B C83B S83B 0.0(5) . . . . ?
C82B C81B C83B S83B 179.8(3) . . . . ?
C81B C83B S83B C85B 0.1(4) . . . . ?
N81B C85B S83B C83B -0.1(4) . . . . ?
C71B C85B S83B C83B 175.3(4) . . . . ?

_refine_diff_density_max         0.769
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.065



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile'
