 
data_06skc0071p-1
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
1,1,3,3-Tetramethylbutylammonium aniline-2-sulphonate
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C14 H26 N2 O3 S'
_chemical_formula_weight          302.43
 
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
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y, -z'
 
_cell_length_a                    9.300(2)
_cell_length_b                    11.925(3)
_cell_length_c                    15.450(4)
_cell_angle_alpha                 76.199(19)
_cell_angle_beta                  74.813(13)
_cell_angle_gamma                 89.758(17)
_cell_volume                      1602.7(7)
_cell_formula_units_Z             4
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     4166
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        block
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.19
_exptl_crystal_size_mid           0.13
_exptl_crystal_size_min           0.03
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.253
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              656
_exptl_absorpt_coefficient_mu     0.211
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.9610
_exptl_absorpt_correction_T_max   0.9937
_exptl_absorpt_process_details    'SADABS V2.10 (Sheldrick, G.M., 2003)' 
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature           120(2)
_diffrn_radiation_wavelength           0.71073
_diffrn_radiation_type                      MoK\a
_diffrn_radiation_source                  'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator    '10cm confocal mirrors'
_diffrn_measurement_device_type  'Bruker-Nonius 95mm CCD camera on κ-goniostat'
_diffrn_measurement_method          'φ & ω scans'
_diffrn_detector_area_resol_mean   9.091
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             24447
_diffrn_reflns_av_R_equivalents   0.2315
_diffrn_reflns_av_sigmaI/netI     0.3039
_diffrn_reflns_limit_h_min        -12
_diffrn_reflns_limit_h_max        12
_diffrn_reflns_limit_k_min        -15
_diffrn_reflns_limit_k_max        15
_diffrn_reflns_limit_l_min        -19
_diffrn_reflns_limit_l_max        19
_diffrn_reflns_theta_min          2.93
_diffrn_reflns_theta_max          27.47
_reflns_number_total              7102
_reflns_number_gt                 2916
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        
'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
#Although determined using DirAx, the cell is refined in the HKL
#package during data reduction
_computing_data_reduction         
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'  
_computing_structure_solution     ?
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_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.

 Due to the particularly high R-values and Rint it would be inappropriate to
 obtain precise structural data from this structure. The transferable hydrogens
 were located on the electron density map in spite of the high R value.
;
 
_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)+(0.0000P)²+16.8167P] 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_number_reflns          7102
_refine_ls_number_parameters      373
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.3758
_refine_ls_R_factor_gt            0.2106
_refine_ls_wR_factor_ref          0.3708
_refine_ls_wR_factor_gt           0.2966
_refine_ls_goodness_of_fit_ref    1.153
_refine_ls_restrained_S_all       1.153
_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 -0.2139(13) 0.0634(11) 0.6957(10) 0.048(3) Uani 1 1 d . . .
C2 C -0.2458(12) -0.0561(9) 0.7163(9) 0.042(3) Uani 1 1 d . . .
C3 C -0.3116(13) -0.1194(10) 0.8049(9) 0.043(3) Uani 1 1 d . . .
H3 H -0.3268 -0.2011 0.8178 0.052 Uiso 1 1 calc R . .
C4 C -0.3561(12) -0.0616(10) 0.8760(9) 0.047(3) Uani 1 1 d . . .
H4 H -0.4063 -0.1034 0.9370 0.056 Uiso 1 1 calc R . .
C5 C -0.3264(12) 0.0553(11) 0.8567(9) 0.046(3) Uani 1 1 d . . .
H5 H -0.3541 0.0936 0.9054 0.055 Uiso 1 1 calc R . .
C6 C -0.2588(13) 0.1181(11) 0.7700(10) 0.048(3) Uani 1 1 d . . .
H6 H -0.2413 0.1993 0.7588 0.057 Uiso 1 1 calc R . .
N1 N -0.1414(11) 0.1285(8) 0.6078(7) 0.048(3) Uani 1 1 d . . .
H1A H -0.1132 0.0948 0.5617 0.057 Uiso 1 1 calc R . .
H1B H -0.1237 0.2036 0.5980 0.057 Uiso 1 1 calc R . .
O2A O -0.0192(8) -0.1293(7) 0.6077(6) 0.049(2) Uani 1 1 d . . .
O2B O -0.2511(9) -0.2488(7) 0.6686(6) 0.055(2) Uani 1 1 d . . .
O2C O -0.2319(9) -0.0701(7) 0.5485(6) 0.049(2) Uani 1 1 d . . .
S2 S -0.1825(3) -0.1323(3) 0.6284(2) 0.0422(8) Uani 1 1 d . . .
C22 C 0.3077(12) 0.0050(10) 0.6679(8) 0.042(3) Uani 1 1 d . . .
C23 C 0.2999(12) 0.0142(9) 0.7660(8) 0.041(3) Uani 1 1 d . . .
H23A H 0.2705 0.0934 0.7687 0.049 Uiso 1 1 calc R . .
H23B H 0.4037 0.0104 0.7714 0.049 Uiso 1 1 calc R . .
C24 C 0.2028(12) -0.0672(10) 0.8550(8) 0.040(3) Uani 1 1 d . . .
C25 C 0.2597(13) -0.1894(10) 0.8760(9) 0.054(4) Uani 1 1 d . . .
H25A H 0.3667 -0.1837 0.8711 0.081 Uiso 1 1 calc R . .
H25B H 0.2426 -0.2307 0.8315 0.081 Uiso 1 1 calc R . .
H25C H 0.2059 -0.2316 0.9389 0.081 Uiso 1 1 calc R . .
C26 C 0.4310(13) 0.0924(10) 0.5995(8) 0.050(3) Uani 1 1 d . . .
H26A H 0.4285 0.0950 0.5360 0.074 Uiso 1 1 calc R . .
H26B H 0.5285 0.0686 0.6076 0.074 Uiso 1 1 calc R . .
H26C H 0.4145 0.1693 0.6111 0.074 Uiso 1 1 calc R . .
C27 C 0.3326(12) -0.1163(9) 0.6492(9) 0.047(3) Uani 1 1 d . . .
H27A H 0.2444 -0.1682 0.6842 0.071 Uiso 1 1 calc R . .
H27B H 0.4201 -0.1470 0.6686 0.071 Uiso 1 1 calc R . .
H27C H 0.3490 -0.1105 0.5830 0.071 Uiso 1 1 calc R . .
C28 C 0.2021(15) -0.0105(12) 0.9336(9) 0.063(4) Uani 1 1 d . . .
H28A H 0.3048 0.0021 0.9360 0.094 Uiso 1 1 calc R . .
H28B H 0.1446 -0.0610 0.9923 0.094 Uiso 1 1 calc R . .
H28C H 0.1563 0.0639 0.9229 0.094 Uiso 1 1 calc R . .
C29 C 0.0393(12) -0.0785(10) 0.8517(9) 0.052(3) Uani 1 1 d . . .
H29A H -0.0243 -0.1119 0.9142 0.078 Uiso 1 1 calc R . .
H29B H 0.0316 -0.1289 0.8113 0.078 Uiso 1 1 calc R . .
H29C H 0.0068 -0.0019 0.8276 0.078 Uiso 1 1 calc R . .
N21 N 0.1669(9) 0.0421(7) 0.6427(7) 0.042(2) Uani 1 1 d . . .
H21A H 0.0961 -0.0176 0.6663 0.062 Uiso 1 1 calc R . .
H21B H 0.1852 0.0632 0.5800 0.062 Uiso 1 1 calc R . .
H21C H 0.1339 0.1033 0.6664 0.062 Uiso 1 1 calc R . .
C31 C 0.0347(12) 0.5646(9) 0.7110(9) 0.040(3) Uani 1 1 d . . .
C32 C 0.0365(12) 0.4448(10) 0.7408(9) 0.041(3) Uani 1 1 d . . .
C33 C -0.0064(12) 0.3861(11) 0.8343(10) 0.046(3) Uani 1 1 d . . .
H33 H -0.0027 0.3044 0.8516 0.055 Uiso 1 1 calc R . .
C34 C -0.0543(13) 0.4467(10) 0.9018(9) 0.048(3) Uani 1 1 d . . .
H34 H -0.0843 0.4082 0.9656 0.058 Uiso 1 1 calc R . .
C35 C -0.0566(12) 0.5679(10) 0.8720(9) 0.044(3) Uani 1 1 d . . .
H35 H -0.0897 0.6110 0.9171 0.052 Uiso 1 1 calc R . .
C36 C -0.0136(13) 0.6254(10) 0.7814(9) 0.046(3) Uani 1 1 d . . .
H36 H -0.0157 0.7073 0.7647 0.055 Uiso 1 1 calc R . .
N31 N 0.0720(10) 0.6237(8) 0.6198(7) 0.048(3) Uani 1 1 d . . .
H31A H 0.0990 0.5859 0.5762 0.057 Uiso 1 1 calc R . .
H31B H 0.0689 0.6995 0.6047 0.057 Uiso 1 1 calc R . .
O32A O 0.0942(9) 0.2440(6) 0.7069(6) 0.049(2) Uani 1 1 d . . .
O32B O 0.2238(9) 0.4145(7) 0.5908(6) 0.050(2) Uani 1 1 d . . .
O32C O -0.0388(8) 0.3702(7) 0.6140(6) 0.047(2) Uani 1 1 d . . .
S32 S 0.0835(3) 0.3604(3) 0.6567(2) 0.0452(8) Uani 1 1 d . . .
C42 C 0.5993(12) 0.4918(9) 0.6587(8) 0.040(3) Uani 1 1 d . . .
C43 C 0.6110(12) 0.4607(10) 0.7593(8) 0.047(3) Uani 1 1 d . . .
H43A H 0.6545 0.5306 0.7693 0.056 Uiso 1 1 calc R . .
H43B H 0.6855 0.4014 0.7629 0.056 Uiso 1 1 calc R . .
C44 C 0.4703(13) 0.4148(10) 0.8454(9) 0.048(3) Uani 1 1 d . . .
C45 C 0.5343(15) 0.3743(11) 0.9287(9) 0.063(4) Uani 1 1 d . . .
H45A H 0.5897 0.4395 0.9363 0.095 Uiso 1 1 calc R . .
H45B H 0.6017 0.3125 0.9185 0.095 Uiso 1 1 calc R . .
H45C H 0.4526 0.3452 0.9847 0.095 Uiso 1 1 calc R . .
C46 C 0.5779(13) 0.3906(10) 0.6198(10) 0.056(4) Uani 1 1 d . . .
H46A H 0.6034 0.4159 0.5521 0.083 Uiso 1 1 calc R . .
H46B H 0.4736 0.3603 0.6436 0.083 Uiso 1 1 calc R . .
H46C H 0.6430 0.3299 0.6383 0.083 Uiso 1 1 calc R . .
C47 C 0.4898(13) 0.5833(10) 0.6390(9) 0.049(3) Uani 1 1 d . . .
H47A H 0.5058 0.6112 0.5720 0.074 Uiso 1 1 calc R . .
H47B H 0.5056 0.6480 0.6651 0.074 Uiso 1 1 calc R . .
H47C H 0.3875 0.5495 0.6673 0.074 Uiso 1 1 calc R . .
C48 C 0.3786(13) 0.3137(11) 0.8360(9) 0.056(4) Uani 1 1 d . . .
H48A H 0.3050 0.2809 0.8952 0.084 Uiso 1 1 calc R . .
H48B H 0.4453 0.2540 0.8190 0.084 Uiso 1 1 calc R . .
H48C H 0.3270 0.3417 0.7880 0.084 Uiso 1 1 calc R . .
C49 C 0.3698(15) 0.5118(11) 0.8618(10) 0.063(4) Uani 1 1 d . . .
H49A H 0.3127 0.5282 0.8157 0.095 Uiso 1 1 calc R . .
H49B H 0.4306 0.5812 0.8566 0.095 Uiso 1 1 calc R . .
H49C H 0.3009 0.4887 0.9239 0.095 Uiso 1 1 calc R . .
N41 N 0.7527(10) 0.5490(8) 0.6039(7) 0.046(3) Uani 1 1 d . . .
H41A H 0.8240 0.4987 0.6139 0.069 Uiso 1 1 calc R . .
H41B H 0.7684 0.6137 0.6225 0.069 Uiso 1 1 calc R . .
H41C H 0.7575 0.5687 0.5426 0.069 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
C1 N1 1.387(15) . ?
C1 C2 1.399(16) . ?
C1 C6 1.423(17) . ?
C2 C3 1.374(16) . ?
C2 S2 1.784(13) . ?
C3 C4 1.405(17) . ?
C3 H3 0.9500 . ?
C4 C5 1.368(15) . ?
C4 H4 0.9500 . ?
C5 C6 1.354(16) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
N1 H1A 0.8800 . ?
N1 H1B 0.8800 . ?
O2A S2 1.466(8) . ?
O2B S2 1.453(8) . ?
O2C S2 1.463(8) . ?
C22 N21 1.497(12) . ?
C22 C23 1.528(15) . ?
C22 C26 1.539(16) . ?
C22 C27 1.546(15) . ?
C23 C24 1.539(15) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C28 1.522(16) . ?
C24 C25 1.538(16) . ?
C24 C29 1.542(15) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
N21 H21A 0.9100 . ?
N21 H21B 0.9100 . ?
N21 H21C 0.9100 . ?
C31 N31 1.368(14) . ?
C31 C32 1.395(15) . ?
C31 C36 1.424(17) . ?
C32 C33 1.398(16) . ?
C32 S32 1.793(12) . ?
C33 C34 1.387(17) . ?
C33 H33 0.9500 . ?
C34 C35 1.410(15) . ?
C34 H34 0.9500 . ?
C35 C36 1.357(16) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
N31 H31A 0.8800 . ?
N31 H31B 0.8800 . ?
O32A S32 1.436(8) . ?
O32B S32 1.467(8) . ?
O32C S32 1.449(7) . ?
C42 C46 1.506(15) . ?
C42 C47 1.521(14) . ?
C42 N41 1.522(14) . ?
C42 C43 1.541(15) . ?
C43 C44 1.589(17) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 C49 1.511(16) . ?
C44 C45 1.532(16) . ?
C44 C48 1.535(15) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
N41 H41A 0.9100 . ?
N41 H41B 0.9100 . ?
N41 H41C 0.9100 . ?
 
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
N1 C1 C2 123.2(12) . . ?
N1 C1 C6 119.8(11) . . ?
C2 C1 C6 116.9(12) . . ?
C3 C2 C1 121.9(12) . . ?
C3 C2 S2 118.2(9) . . ?
C1 C2 S2 119.6(10) . . ?
C2 C3 C4 119.1(11) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C5 C4 C3 119.4(12) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
C6 C5 C4 121.8(13) . . ?
C6 C5 H5 119.1 . . ?
C4 C5 H5 119.1 . . ?
C5 C6 C1 120.6(12) . . ?
C5 C6 H6 119.7 . . ?
C1 C6 H6 119.7 . . ?
C1 N1 H1A 120.0 . . ?
C1 N1 H1B 120.0 . . ?
H1A N1 H1B 120.0 . . ?
O2B S2 O2C 113.7(5) . . ?
O2B S2 O2A 112.5(5) . . ?
O2C S2 O2A 111.7(5) . . ?
O2B S2 C2 105.2(5) . . ?
O2C S2 C2 106.4(5) . . ?
O2A S2 C2 106.8(5) . . ?
N21 C22 C23 110.8(10) . . ?
N21 C22 C26 104.9(9) . . ?
C23 C22 C26 108.5(9) . . ?
N21 C22 C27 106.1(8) . . ?
C23 C22 C27 116.3(9) . . ?
C26 C22 C27 109.7(10) . . ?
C22 C23 C24 124.8(9) . . ?
C22 C23 H23A 106.1 . . ?
C24 C23 H23A 106.1 . . ?
C22 C23 H23B 106.1 . . ?
C24 C23 H23B 106.1 . . ?
H23A C23 H23B 106.3 . . ?
C28 C24 C25 109.8(10) . . ?
C28 C24 C23 106.6(9) . . ?
C25 C24 C23 113.6(10) . . ?
C28 C24 C29 106.8(10) . . ?
C25 C24 C29 108.3(9) . . ?
C23 C24 C29 111.6(9) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C22 C26 H26A 109.5 . . ?
C22 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C22 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C22 C27 H27A 109.5 . . ?
C22 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C22 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C24 C28 H28A 109.5 . . ?
C24 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C24 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C24 C29 H29A 109.5 . . ?
C24 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C24 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C22 N21 H21A 109.5 . . ?
C22 N21 H21B 109.5 . . ?
H21A N21 H21B 109.5 . . ?
C22 N21 H21C 109.5 . . ?
H21A N21 H21C 109.5 . . ?
H21B N21 H21C 109.5 . . ?
N31 C31 C32 123.7(12) . . ?
N31 C31 C36 120.0(10) . . ?
C32 C31 C36 116.3(11) . . ?
C31 C32 C33 122.6(12) . . ?
C31 C32 S32 119.3(10) . . ?
C33 C32 S32 117.9(9) . . ?
C34 C33 C32 120.2(11) . . ?
C34 C33 H33 119.9 . . ?
C32 C33 H33 119.9 . . ?
C33 C34 C35 117.4(12) . . ?
C33 C34 H34 121.3 . . ?
C35 C34 H34 121.3 . . ?
C36 C35 C34 122.6(12) . . ?
C36 C35 H35 118.7 . . ?
C34 C35 H35 118.7 . . ?
C35 C36 C31 120.8(11) . . ?
C35 C36 H36 119.6 . . ?
C31 C36 H36 119.6 . . ?
C31 N31 H31A 120.0 . . ?
C31 N31 H31B 120.0 . . ?
H31A N31 H31B 120.0 . . ?
O32A S32 O32C 112.3(5) . . ?
O32A S32 O32B 114.3(5) . . ?
O32C S32 O32B 111.8(5) . . ?
O32A S32 C32 106.4(5) . . ?
O32C S32 C32 105.2(5) . . ?
O32B S32 C32 106.0(5) . . ?
C46 C42 C47 110.9(9) . . ?
C46 C42 N41 106.2(10) . . ?
C47 C42 N41 105.2(9) . . ?
C46 C42 C43 115.5(10) . . ?
C47 C42 C43 114.7(10) . . ?
N41 C42 C43 103.1(8) . . ?
C42 C43 C44 122.4(9) . . ?
C42 C43 H43A 106.7 . . ?
C44 C43 H43A 106.7 . . ?
C42 C43 H43B 106.7 . . ?
C44 C43 H43B 106.7 . . ?
H43A C43 H43B 106.6 . . ?
C49 C44 C45 108.4(11) . . ?
C49 C44 C48 109.3(10) . . ?
C45 C44 C48 109.3(10) . . ?
C49 C44 C43 110.6(10) . . ?
C45 C44 C43 105.3(9) . . ?
C48 C44 C43 113.7(11) . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C42 C46 H46A 109.5 . . ?
C42 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C42 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C42 C47 H47A 109.5 . . ?
C42 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C42 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C44 C48 H48A 109.5 . . ?
C44 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C44 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C44 C49 H49A 109.5 . . ?
C44 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C44 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C42 N41 H41A 109.5 . . ?
C42 N41 H41B 109.5 . . ?
H41A N41 H41B 109.5 . . ?
C42 N41 H41C 109.5 . . ?
H41A N41 H41C 109.5 . . ?
H41B N41 H41C 109.5 . . ?
 
loop_
 _geom_hbond_atom_site_label_D
 _geom_hbond_atom_site_label_H
 _geom_hbond_atom_site_label_A
 _geom_hbond_distance_DH
 _geom_hbond_distance_HA
 _geom_hbond_distance_DA
 _geom_hbond_angle_DHA
 _geom_hbond_site_symmetry_A
N1 H1A O2C  0.88 2.34 2.934(12) 125.4 .
N1 H1B O32C  0.88 2.23 3.070(11) 159.2 .
N21 H21A O2A  0.91 2.20 2.918(11) 135.3 .
N21 H21C O32A  0.91 1.93 2.831(12) 171.2 .
N31 H31A O32B  0.88 2.34 2.931(13) 124.7 .
N1 H1A O2A  0.88 2.52 3.270(14) 143.9 2_556
N21 H21B O2C  0.91 1.90 2.793(13) 166.6 2_556
N31 H31B O2A  0.88 2.20 3.038(12) 158.2 1_565
N41 H41A O32C  0.91 1.99 2.880(12) 165.3 1_655
N41 H41B O2B  0.91 1.93 2.818(12) 165.8 1_665
N41 H41C O32B  0.91 1.98 2.884(12) 170.7 2_666
N41 H41C S32  0.91 2.96 3.798(10) 153.8 2_666
 
_diffrn_measured_fraction_theta_max    0.967
_diffrn_reflns_theta_full              27.47
_diffrn_measured_fraction_theta_full   0.967
_refine_diff_density_max    0.486
_refine_diff_density_min   -0.413
_refine_diff_density_rms    0.101
