 
data_03src0209
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C24 H22 N2 O4 S'
_chemical_formula_sum
 'C24 H22 N2 O4 S'
_chemical_formula_weight          434.50
 
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            Triclinic
_symmetry_space_group_name_H-M    P-1
_symmetry_space_group_name_hall   '-P 1'
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y, -z'
 
_cell_length_a                    11.9007(4)
_cell_length_b                    12.8521(4)
_cell_length_c                    14.6202(5)
_cell_angle_alpha                 109.852(2)
_cell_angle_beta                  90.743(2)
_cell_angle_gamma                 92.775(2)
_cell_volume                      2099.76(12)
_cell_formula_units_Z             4
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     25443
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        Prism
_exptl_crystal_colour             'Pale Yellow'
_exptl_crystal_size_max           0.50
_exptl_crystal_size_mid           0.30
_exptl_crystal_size_min           0.10
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.374
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              912
_exptl_absorpt_coefficient_mu     0.189
_exptl_absorpt_correction_type    Multi-scan
_exptl_absorpt_correction_T_min   0.9115
_exptl_absorpt_correction_T_max   0.9814
_exptl_absorpt_process_details    'SORTAV (Blessing, 1997)'
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       120(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   'Bruker Nonius Kappa CCD Area detector'
_diffrn_measurement_method        'φ and ω scans to fill the asymmetric unit'
_diffrn_detector_area_resol_mean  9.091
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             31054
_diffrn_reflns_av_R_equivalents   0.0599
_diffrn_reflns_av_sigmaI/netI     0.0515
_diffrn_reflns_limit_h_min        -14
_diffrn_reflns_limit_h_max        14
_diffrn_reflns_limit_k_min        -15
_diffrn_reflns_limit_k_max        15
_diffrn_reflns_limit_l_min        -17
_diffrn_reflns_limit_l_max        17
_diffrn_reflns_theta_min          2.96
_diffrn_reflns_theta_max          25.02
_reflns_number_total              7393
_reflns_number_gt                 5463
_reflns_threshold_expression      >2σ(I)
 
_computing_data_collection        'COLLECT (Hooft, 1998)'
_computing_cell_refinement        'DENZO (Otwinowski and MInor, 1997)'
_computing_data_reduction         'DENZO, COLLECT, MAXUS (Mackay et al., 1998)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'CAMERON (Watkin, et al., 1993)'
_computing_publication_material   'WINGX (Farrugia, 1998)'
 
_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 > 2σ(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)+(0.0701P)²+0.8725P] 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      SHELXL
_refine_ls_extinction_coef        0.0047(8)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          7393
_refine_ls_number_parameters      560
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0679
_refine_ls_R_factor_gt            0.0432
_refine_ls_wR_factor_ref          0.1202
_refine_ls_wR_factor_gt           0.1078
_refine_ls_goodness_of_fit_ref    0.951
_refine_ls_restrained_S_all       0.951
_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_symmetry_multiplicity
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
C1 C 0.3992(2) 0.7638(2) 0.1428(2) 0.0358(6) Uani 1 1 d . . .
H1A H 0.4576 0.7099 0.1306 0.054 Uiso 1 1 calc R . .
H1B H 0.3255 0.7261 0.1422 0.054 Uiso 1 1 calc R . .
H1C H 0.4140 0.8215 0.2064 0.054 Uiso 1 1 calc R . .
C2 C 0.4292(2) 0.9494(2) -0.13724(17) 0.0306(6) Uani 1 1 d . . .
H2A H 0.4906 0.9147 -0.1787 0.046 Uiso 1 1 calc R . .
H2B H 0.4465 1.0295 -0.1089 0.046 Uiso 1 1 calc R . .
H2C H 0.3590 0.9353 -0.1763 0.046 Uiso 1 1 calc R . .
C3 C 0.16977(18) 1.00165(17) 0.14177(15) 0.0189(5) Uani 1 1 d . . .
C4 C 0.24039(19) 0.91824(18) 0.14194(16) 0.0215(5) Uani 1 1 d . . .
H4 H 0.2313 0.8811 0.1878 0.026 Uiso 1 1 calc R . .
C5 C 0.32359(19) 0.89057(18) 0.07450(17) 0.0223(5) Uani 1 1 d . . .
C6 C 0.33494(19) 0.94316(18) 0.00362(16) 0.0216(5) Uani 1 1 d . . .
C7 C 0.26612(19) 1.02660(18) 0.00469(16) 0.0218(5) Uani 1 1 d . . .
H7 H 0.2740 1.0639 -0.0411 0.026 Uiso 1 1 calc R . .
C8 C 0.18435(18) 1.05461(17) 0.07535(16) 0.0196(5) Uani 1 1 d . . .
C9 C 0.07021(18) 1.03571(18) 0.20526(16) 0.0195(5) Uani 1 1 d . . .
H9 H 0.0141 0.9712 0.1892 0.023 Uiso 1 1 calc R . .
C10 C 0.09786(19) 1.07571(18) 0.31459(16) 0.0209(5) Uani 1 1 d . . .
H10A H 0.0270 1.0849 0.3506 0.025 Uiso 1 1 calc R . .
H10B H 0.1404 1.0193 0.3304 0.025 Uiso 1 1 calc R . .
C11 C 0.16690(18) 1.18486(18) 0.34661(15) 0.0192(5) Uani 1 1 d . . .
C12 C 0.29055(19) 1.18981(19) 0.36582(15) 0.0210(5) Uani 1 1 d . . .
C13 C 0.3461(2) 1.1010(2) 0.37461(17) 0.0267(5) Uani 1 1 d . . .
H13 H 0.3046 1.0340 0.3692 0.032 Uiso 1 1 calc R . .
C14 C 0.4620(2) 1.1095(2) 0.39132(18) 0.0307(6) Uani 1 1 d . . .
H14 H 0.4990 1.0482 0.3973 0.037 Uiso 1 1 calc R . .
C15 C 0.5239(2) 1.2057(2) 0.39926(17) 0.0320(6) Uani 1 1 d . . .
H15 H 0.6032 1.2107 0.4102 0.038 Uiso 1 1 calc R . .
C16 C 0.4693(2) 1.2951(2) 0.39115(19) 0.0332(6) Uani 1 1 d . . .
H16 H 0.5112 1.3619 0.3966 0.040 Uiso 1 1 calc R . .
C17 C 0.3539(2) 1.2873(2) 0.37506(17) 0.0271(6) Uani 1 1 d . . .
H17 H 0.3172 1.3493 0.3702 0.032 Uiso 1 1 calc R . .
C18 C -0.04230(18) 1.20682(18) 0.24320(16) 0.0208(5) Uani 1 1 d . . .
C19 C -0.15269(19) 1.21990(19) 0.22054(17) 0.0250(5) Uani 1 1 d . . .
H19 H -0.1859 1.1735 0.1601 0.030 Uiso 1 1 calc R . .
C20 C -0.21579(19) 1.2991(2) 0.28394(17) 0.0261(5) Uani 1 1 d . . .
H20 H -0.2913 1.3065 0.2664 0.031 Uiso 1 1 calc R . .
C21 C -0.16978(19) 1.36801(19) 0.37324(17) 0.0236(5) Uani 1 1 d . . .
C22 C -0.05780(19) 1.35637(18) 0.39462(17) 0.0235(5) Uani 1 1 d . . .
H22 H -0.0246 1.4041 0.4545 0.028 Uiso 1 1 calc R . .
C23 C 0.00718(19) 1.27788(18) 0.33203(16) 0.0214(5) Uani 1 1 d . . .
C24 C -0.2383(2) 1.4520(2) 0.44490(18) 0.0307(6) Uani 1 1 d . . .
H24A H -0.3147 1.4485 0.4177 0.046 Uiso 1 1 calc R . .
H24B H -0.2032 1.5264 0.4579 0.046 Uiso 1 1 calc R . .
H24C H -0.2417 1.4359 0.5057 0.046 Uiso 1 1 calc R . .
N1 N 0.02085(15) 1.12412(15) 0.17640(13) 0.0204(4) Uani 1 1 d . . .
N2 N 0.12205(15) 1.27712(15) 0.35683(13) 0.0218(4) Uani 1 1 d . . .
O1 O 0.39998(14) 0.81320(13) 0.06845(12) 0.0289(4) Uani 1 1 d . . .
O2 O 0.41697(14) 0.90396(13) -0.06137(11) 0.0281(4) Uani 1 1 d . . .
O3 O 0.13477(14) 1.26490(12) 0.12463(12) 0.0277(4) Uani 1 1 d . . .
O4 O 0.01497(13) 1.12899(13) 0.00291(11) 0.0266(4) Uani 1 1 d . . .
S1 S 0.08533(5) 1.15355(4) 0.08843(4) 0.01981(16) Uani 1 1 d . . .
C25 C 0.4183(2) 0.3021(2) 0.1354(2) 0.0384(7) Uani 1 1 d . . .
H25A H 0.4736 0.2471 0.1067 0.058 Uiso 1 1 calc R . .
H25B H 0.3819 0.3229 0.0841 0.058 Uiso 1 1 calc R . .
H25C H 0.3613 0.2706 0.1678 0.058 Uiso 1 1 calc R . .
C26 C 0.6495(2) 0.6778(2) 0.3526(2) 0.0346(6) Uani 1 1 d . . .
H26A H 0.7296 0.6628 0.3492 0.052 Uiso 1 1 calc R . .
H26B H 0.6293 0.7103 0.4208 0.052 Uiso 1 1 calc R . .
H26C H 0.6347 0.7297 0.3184 0.052 Uiso 1 1 calc R . .
C27 C 0.23515(18) 0.57057(18) 0.29538(16) 0.0189(5) Uani 1 1 d . . .
C28 C 0.29253(19) 0.47615(18) 0.24854(16) 0.0221(5) Uani 1 1 d . . .
H28 H 0.2523 0.4078 0.2147 0.026 Uiso 1 1 calc R . .
C29 C 0.40908(19) 0.48315(18) 0.25189(16) 0.0231(5) Uani 1 1 d . . .
C30 C 0.46965(18) 0.58299(19) 0.30638(16) 0.0214(5) Uani 1 1 d . . .
C31 C 0.41329(19) 0.67608(18) 0.35241(16) 0.0211(5) Uani 1 1 d . . .
H31 H 0.4528 0.7441 0.3884 0.025 Uiso 1 1 calc R . .
C32 C 0.29589(18) 0.66772(18) 0.34466(16) 0.0193(5) Uani 1 1 d . . .
C33 C 0.10872(19) 0.57817(18) 0.30266(16) 0.0205(5) Uani 1 1 d . . .
H33 H 0.0812 0.5345 0.3438 0.025 Uiso 1 1 calc R . .
C34 C 0.03992(18) 0.53834(18) 0.20682(16) 0.0198(5) Uani 1 1 d . . .
H34A H 0.0566 0.4607 0.1701 0.024 Uiso 1 1 calc R . .
H34B H -0.0412 0.5396 0.2211 0.024 Uiso 1 1 calc R . .
C35 C 0.06477(19) 0.60890(18) 0.14431(16) 0.0212(5) Uani 1 1 d . . .
C36 C 0.13316(19) 0.56835(18) 0.05659(16) 0.0226(5) Uani 1 1 d . . .
C37 C 0.1789(2) 0.4653(2) 0.02656(18) 0.0306(6) Uani 1 1 d . . .
H37 H 0.1616 0.4150 0.0600 0.037 Uiso 1 1 calc R . .
C38 C 0.2497(2) 0.4347(2) -0.05182(19) 0.0402(7) Uani 1 1 d . . .
H38 H 0.2805 0.3639 -0.0716 0.048 Uiso 1 1 calc R . .
C39 C 0.2753(2) 0.5064(2) -0.10085(19) 0.0422(7) Uani 1 1 d . . .
H39 H 0.3262 0.4867 -0.1527 0.051 Uiso 1 1 calc R . .
C40 C 0.2269(2) 0.6071(2) -0.07446(19) 0.0416(7) Uani 1 1 d . . .
H40 H 0.2429 0.6559 -0.1096 0.050 Uiso 1 1 calc R . .
C41 C 0.1556(2) 0.6378(2) 0.00231(18) 0.0317(6) Uani 1 1 d . . .
H41 H 0.1213 0.7067 0.0187 0.038 Uiso 1 1 calc R . .
C42 C -0.00298(18) 0.75313(18) 0.34121(17) 0.0208(5) Uani 1 1 d . . .
C43 C -0.0587(2) 0.8171(2) 0.42236(18) 0.0275(6) Uani 1 1 d . . .
H43 H -0.0385 0.8153 0.4849 0.033 Uiso 1 1 calc R . .
C44 C -0.1430(2) 0.8830(2) 0.41301(19) 0.0309(6) Uani 1 1 d . . .
H44 H -0.1794 0.9272 0.4693 0.037 Uiso 1 1 calc R . .
C45 C -0.1753(2) 0.88549(19) 0.32209(19) 0.0286(6) Uani 1 1 d . . .
C46 C -0.1184(2) 0.82175(19) 0.24149(18) 0.0261(5) Uani 1 1 d . . .
H46 H -0.1397 0.8230 0.1790 0.031 Uiso 1 1 calc R . .
C47 C -0.03146(19) 0.75616(18) 0.24907(17) 0.0221(5) Uani 1 1 d . . .
C48 C -0.2671(2) 0.9574(2) 0.3112(2) 0.0433(7) Uani 1 1 d . . .
H48A H -0.2782 0.9483 0.2424 0.065 Uiso 1 1 calc R . .
H48B H -0.2456 1.0351 0.3483 0.065 Uiso 1 1 calc R . .
H48C H -0.3372 0.9355 0.3360 0.065 Uiso 1 1 calc R . .
N3 N 0.09277(15) 0.69705(15) 0.35604(13) 0.0213(4) Uani 1 1 d . . .
N4 N 0.02920(16) 0.70703(15) 0.16535(13) 0.0235(4) Uani 1 1 d . . .
O5 O 0.47403(13) 0.39855(13) 0.20517(12) 0.0307(4) Uani 1 1 d . . .
O6 O 0.58384(13) 0.57680(13) 0.30779(12) 0.0290(4) Uani 1 1 d . . .
O7 O 0.21844(14) 0.81182(14) 0.50137(11) 0.0314(4) Uani 1 1 d . . .
O8 O 0.21964(14) 0.86012(13) 0.35494(13) 0.0323(4) Uani 1 1 d . . .
S2 S 0.20876(5) 0.77439(4) 0.39733(4) 0.02137(16) Uani 1 1 d . . .
 
 
_geom_special_details
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
C1 O1 1.433(3) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 O2 1.424(3) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C8 1.371(3) . ?
C3 C4 1.394(3) . ?
C3 C9 1.503(3) . ?
C4 C5 1.379(3) . ?
C4 H4 0.9500 . ?
C5 O1 1.361(3) . ?
C5 C6 1.421(3) . ?
C6 O2 1.362(3) . ?
C6 C7 1.377(3) . ?
C7 C8 1.397(3) . ?
C7 H7 0.9500 . ?
C8 S1 1.740(2) . ?
C9 N1 1.483(3) . ?
C9 C10 1.529(3) . ?
C9 H9 1.0000 . ?
C10 C11 1.515(3) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 N2 1.287(3) . ?
C11 C12 1.489(3) . ?
C12 C13 1.388(3) . ?
C12 C17 1.396(3) . ?
C13 C14 1.391(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.377(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.386(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.384(3) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
C18 C19 1.383(3) . ?
C18 C23 1.411(3) . ?
C18 N1 1.428(3) . ?
C19 C20 1.382(3) . ?
C19 H19 0.9500 . ?
C20 C21 1.392(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.391(3) . ?
C21 C24 1.506(3) . ?
C22 C23 1.386(3) . ?
C22 H22 0.9500 . ?
C23 N2 1.411(3) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
N1 S1 1.6474(19) . ?
O3 S1 1.4388(16) . ?
O4 S1 1.4295(16) . ?
C25 O5 1.435(3) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 O6 1.427(3) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C32 1.374(3) . ?
C27 C28 1.391(3) . ?
C27 C33 1.515(3) . ?
C28 C29 1.385(3) . ?
C28 H28 0.9500 . ?
C29 O5 1.355(3) . ?
C29 C30 1.415(3) . ?
C30 O6 1.365(3) . ?
C30 C31 1.370(3) . ?
C31 C32 1.396(3) . ?
C31 H31 0.9500 . ?
C32 S2 1.729(2) . ?
C33 N3 1.484(3) . ?
C33 C34 1.529(3) . ?
C33 H33 1.0000 . ?
C34 C35 1.513(3) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 N4 1.287(3) . ?
C35 C36 1.481(3) . ?
C36 C37 1.387(3) . ?
C36 C41 1.400(3) . ?
C37 C38 1.389(4) . ?
C37 H37 0.9500 . ?
C38 C39 1.373(4) . ?
C38 H38 0.9500 . ?
C39 C40 1.376(4) . ?
C39 H39 0.9500 . ?
C40 C41 1.375(4) . ?
C40 H40 0.9500 . ?
C41 H41 0.9500 . ?
C42 C43 1.390(3) . ?
C42 C47 1.399(3) . ?
C42 N3 1.430(3) . ?
C43 C44 1.379(3) . ?
C43 H43 0.9500 . ?
C44 C45 1.390(4) . ?
C44 H44 0.9500 . ?
C45 C46 1.392(3) . ?
C45 C48 1.505(3) . ?
C46 C47 1.393(3) . ?
C46 H46 0.9500 . ?
C47 N4 1.400(3) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
N3 S2 1.6419(19) . ?
O7 S2 1.4323(17) . ?
O8 S2 1.4376(17) . ?
 
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
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O2 C2 H2A 109.5 . . ?
O2 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
O2 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C8 C3 C4 119.8(2) . . ?
C8 C3 C9 114.70(19) . . ?
C4 C3 C9 125.41(19) . . ?
C5 C4 C3 118.9(2) . . ?
C5 C4 H4 120.6 . . ?
C3 C4 H4 120.6 . . ?
O1 C5 C4 124.9(2) . . ?
O1 C5 C6 114.4(2) . . ?
C4 C5 C6 120.7(2) . . ?
O2 C6 C7 125.4(2) . . ?
O2 C6 C5 114.50(19) . . ?
C7 C6 C5 120.1(2) . . ?
C6 C7 C8 117.8(2) . . ?
C6 C7 H7 121.1 . . ?
C8 C7 H7 121.1 . . ?
C3 C8 C7 122.6(2) . . ?
C3 C8 S1 111.23(17) . . ?
C7 C8 S1 126.07(17) . . ?
N1 C9 C3 105.20(17) . . ?
N1 C9 C10 111.10(17) . . ?
C3 C9 C10 114.75(18) . . ?
N1 C9 H9 108.5 . . ?
C3 C9 H9 108.5 . . ?
C10 C9 H9 108.5 . . ?
C11 C10 C9 111.12(17) . . ?
C11 C10 H10A 109.4 . . ?
C9 C10 H10A 109.4 . . ?
C11 C10 H10B 109.4 . . ?
C9 C10 H10B 109.4 . . ?
H10A C10 H10B 108.0 . . ?
N2 C11 C12 116.94(19) . . ?
N2 C11 C10 121.8(2) . . ?
C12 C11 C10 121.30(19) . . ?
C13 C12 C17 118.3(2) . . ?
C13 C12 C11 122.7(2) . . ?
C17 C12 C11 119.0(2) . . ?
C12 C13 C14 120.4(2) . . ?
C12 C13 H13 119.8 . . ?
C14 C13 H13 119.8 . . ?
C15 C14 C13 120.8(2) . . ?
C15 C14 H14 119.6 . . ?
C13 C14 H14 119.6 . . ?
C14 C15 C16 119.3(2) . . ?
C14 C15 H15 120.4 . . ?
C16 C15 H15 120.4 . . ?
C17 C16 C15 120.1(2) . . ?
C17 C16 H16 119.9 . . ?
C15 C16 H16 119.9 . . ?
C16 C17 C12 121.1(2) . . ?
C16 C17 H17 119.5 . . ?
C12 C17 H17 119.5 . . ?
C19 C18 C23 118.9(2) . . ?
C19 C18 N1 120.2(2) . . ?
C23 C18 N1 120.85(19) . . ?
C20 C19 C18 121.4(2) . . ?
C20 C19 H19 119.3 . . ?
C18 C19 H19 119.3 . . ?
C19 C20 C21 120.7(2) . . ?
C19 C20 H20 119.7 . . ?
C21 C20 H20 119.7 . . ?
C20 C21 C22 117.7(2) . . ?
C20 C21 C24 121.5(2) . . ?
C22 C21 C24 120.8(2) . . ?
C23 C22 C21 122.6(2) . . ?
C23 C22 H22 118.7 . . ?
C21 C22 H22 118.7 . . ?
C22 C23 N2 118.61(19) . . ?
C22 C23 C18 118.6(2) . . ?
N2 C23 C18 122.6(2) . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C18 N1 C9 120.90(17) . . ?
C18 N1 S1 118.98(14) . . ?
C9 N1 S1 115.08(14) . . ?
C11 N2 C23 120.12(19) . . ?
C5 O1 C1 117.14(18) . . ?
C6 O2 C2 117.39(18) . . ?
O4 S1 O3 114.70(10) . . ?
O4 S1 N1 112.32(10) . . ?
O3 S1 N1 109.98(10) . . ?
O4 S1 C8 111.79(10) . . ?
O3 S1 C8 112.50(10) . . ?
N1 S1 C8 93.71(10) . . ?
O5 C25 H25A 109.5 . . ?
O5 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
O5 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O6 C26 H26A 109.5 . . ?
O6 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
O6 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C32 C27 C28 119.0(2) . . ?
C32 C27 C33 114.32(19) . . ?
C28 C27 C33 126.64(19) . . ?
C29 C28 C27 119.1(2) . . ?
C29 C28 H28 120.5 . . ?
C27 C28 H28 120.5 . . ?
O5 C29 C28 124.4(2) . . ?
O5 C29 C30 114.72(19) . . ?
C28 C29 C30 120.8(2) . . ?
O6 C30 C31 125.1(2) . . ?
O6 C30 C29 114.8(2) . . ?
C31 C30 C29 120.1(2) . . ?
C30 C31 C32 117.8(2) . . ?
C30 C31 H31 121.1 . . ?
C32 C31 H31 121.1 . . ?
C27 C32 C31 123.1(2) . . ?
C27 C32 S2 111.53(17) . . ?
C31 C32 S2 125.30(17) . . ?
N3 C33 C27 104.54(17) . . ?
N3 C33 C34 110.56(17) . . ?
C27 C33 C34 116.62(18) . . ?
N3 C33 H33 108.3 . . ?
C27 C33 H33 108.3 . . ?
C34 C33 H33 108.3 . . ?
C35 C34 C33 112.51(18) . . ?
C35 C34 H34A 109.1 . . ?
C33 C34 H34A 109.1 . . ?
C35 C34 H34B 109.1 . . ?
C33 C34 H34B 109.1 . . ?
H34A C34 H34B 107.8 . . ?
N4 C35 C36 116.9(2) . . ?
N4 C35 C34 121.9(2) . . ?
C36 C35 C34 121.17(19) . . ?
C37 C36 C41 118.0(2) . . ?
C37 C36 C35 123.1(2) . . ?
C41 C36 C35 118.9(2) . . ?
C38 C37 C36 120.8(2) . . ?
C38 C37 H37 119.6 . . ?
C36 C37 H37 119.6 . . ?
C39 C38 C37 120.2(3) . . ?
C39 C38 H38 119.9 . . ?
C37 C38 H38 119.9 . . ?
C38 C39 C40 119.7(3) . . ?
C38 C39 H39 120.2 . . ?
C40 C39 H39 120.2 . . ?
C41 C40 C39 120.6(3) . . ?
C41 C40 H40 119.7 . . ?
C39 C40 H40 119.7 . . ?
C40 C41 C36 120.6(2) . . ?
C40 C41 H41 119.7 . . ?
C36 C41 H41 119.7 . . ?
C43 C42 C47 120.0(2) . . ?
C43 C42 N3 118.4(2) . . ?
C47 C42 N3 121.1(2) . . ?
C44 C43 C42 120.7(2) . . ?
C44 C43 H43 119.7 . . ?
C42 C43 H43 119.7 . . ?
C43 C44 C45 120.7(2) . . ?
C43 C44 H44 119.7 . . ?
C45 C44 H44 119.7 . . ?
C44 C45 C46 118.1(2) . . ?
C44 C45 C48 121.1(2) . . ?
C46 C45 C48 120.8(2) . . ?
C45 C46 C47 122.4(2) . . ?
C45 C46 H46 118.8 . . ?
C47 C46 H46 118.8 . . ?
C46 C47 C42 118.1(2) . . ?
C46 C47 N4 117.3(2) . . ?
C42 C47 N4 124.3(2) . . ?
C45 C48 H48A 109.5 . . ?
C45 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C45 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C42 N3 C33 123.53(18) . . ?
C42 N3 S2 116.36(14) . . ?
C33 N3 S2 115.42(15) . . ?
C35 N4 C47 122.01(19) . . ?
C29 O5 C25 117.00(18) . . ?
C30 O6 C26 117.06(18) . . ?
O7 S2 O8 115.19(10) . . ?
O7 S2 N3 111.91(10) . . ?
O8 S2 N3 110.16(10) . . ?
O7 S2 C32 111.63(10) . . ?
O8 S2 C32 112.14(11) . . ?
N3 S2 C32 93.88(10) . . ?
 
_diffrn_measured_fraction_theta_max    0.996
_diffrn_reflns_theta_full              25.02
_diffrn_measured_fraction_theta_full   0.996
_refine_diff_density_max    0.461
_refine_diff_density_min   -0.433
_refine_diff_density_rms    0.055
