 
data_01mel003
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C16 H37 N O4 S' 
_chemical_formula_weight          339.53 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0033   0.0016 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'N'  'N'   0.0061   0.0033 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0106   0.0060 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'S'  'S'   0.1246   0.1234 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            Monoclinic
_symmetry_space_group_name_H-M    P2(1)/c
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y-1/2, z-1/2' 
 
_cell_length_a                    21.7299(4) 
_cell_length_b                    21.3998(4) 
_cell_length_c                    17.0880(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  91.318(3) 
_cell_angle_gamma                 90.00 
_cell_volume                      7944.1(3) 
_cell_formula_units_Z             16 
_cell_measurement_temperature     120(2) 
_cell_measurement_reflns_used     22479 
_cell_measurement_theta_min       2.91 
_cell_measurement_theta_max       27.48 
 
_exptl_crystal_description        block 
_exptl_crystal_colour             colourless 
_exptl_crystal_size_max           0.10 
_exptl_crystal_size_mid           0.10 
_exptl_crystal_size_min           0.10 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.136 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              3008 
_exptl_absorpt_coefficient_mu     0.179 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.9823 
_exptl_absorpt_correction_T_max   0.9823 
_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          'Bruker-Nonius FR591 rotating anode' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Bruker-Nonius KappaCCD' 
_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             38718 
_diffrn_reflns_av_R_equivalents   0.0680 
_diffrn_reflns_av_sigmaI/netI     0.0968 
_diffrn_reflns_limit_h_min        -25 
_diffrn_reflns_limit_h_max        25 
_diffrn_reflns_limit_k_min        -25 
_diffrn_reflns_limit_k_max        24 
_diffrn_reflns_limit_l_min        -20 
_diffrn_reflns_limit_l_max        20 
_diffrn_reflns_theta_min          2.94 
_diffrn_reflns_theta_max          25.03 
_reflns_number_total              13981 
_reflns_number_gt                 8004 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'COLLECT (Hooft, 1998)' 
_computing_cell_refinement        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)'  
_computing_data_reduction         
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)'  
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_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. 
; 
 
_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)+(0.1368P)²+1.0999P] 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        0.0000(3) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 
_refine_ls_number_reflns          13981 
_refine_ls_number_parameters      810 
_refine_ls_number_restraints      19 
_refine_ls_R_factor_all           0.1357 
_refine_ls_R_factor_gt            0.0735 
_refine_ls_wR_factor_ref          0.2369 
_refine_ls_wR_factor_gt           0.2027 
_refine_ls_goodness_of_fit_ref    1.021 
_refine_ls_restrained_S_all       1.041 
_refine_ls_shift/su_max           1.146 
_refine_ls_shift/su_mean          0.066 
 
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 0.36857(18) -0.04268(19) 0.6738(2) 0.0332(10) Uani 1 1 d . . . 
H1A H 0.3608 0.0006 0.6916 0.040 Uiso 1 1 calc R . . 
H1B H 0.3283 -0.0640 0.6683 0.040 Uiso 1 1 calc R . . 
C2 C 0.3981(2) -0.0400(2) 0.5934(2) 0.0396(11) Uani 1 1 d . . . 
H2A H 0.4368 -0.0157 0.5971 0.048 Uiso 1 1 calc R . . 
H2B H 0.4083 -0.0828 0.5761 0.048 Uiso 1 1 calc R . . 
C3 C 0.3544(2) -0.0097(2) 0.5337(2) 0.0554(14) Uani 1 1 d . . . 
H3A H 0.3456 0.0338 0.5498 0.066 Uiso 1 1 calc R . . 
H3B H 0.3151 -0.0330 0.5314 0.066 Uiso 1 1 calc R . . 
C4 C 0.3831(3) -0.0095(2) 0.4525(3) 0.0664(16) Uani 1 1 d . . . 
H4A H 0.3546 0.0102 0.4147 0.100 Uiso 1 1 calc R . . 
H4B H 0.3912 -0.0526 0.4363 0.100 Uiso 1 1 calc R . . 
H4C H 0.4218 0.0140 0.4547 0.100 Uiso 1 1 calc R . . 
C5 C 0.41942(18) -0.14303(17) 0.7129(2) 0.0329(10) Uani 1 1 d . . . 
H5A H 0.4416 -0.1639 0.7569 0.039 Uiso 1 1 calc R . . 
H5B H 0.4472 -0.1428 0.6678 0.039 Uiso 1 1 calc R . . 
C6 C 0.3630(2) -0.18175(19) 0.6912(3) 0.0519(13) Uani 1 1 d . . . 
H6A H 0.3451 -0.1667 0.6409 0.062 Uiso 1 1 calc R . . 
H6B H 0.3316 -0.1766 0.7318 0.062 Uiso 1 1 calc R . . 
C7 C 0.3797(2) -0.2510(2) 0.6839(3) 0.0507(13) Uani 1 1 d . . . 
H7A H 0.3454 -0.2731 0.6568 0.061 Uiso 1 1 calc R . . 
H7B H 0.4164 -0.2548 0.6510 0.061 Uiso 1 1 calc R . . 
C8 C 0.3927(3) -0.2819(2) 0.7599(3) 0.0690(16) Uani 1 1 d . . . 
H8A H 0.4035 -0.3257 0.7509 0.104 Uiso 1 1 calc R . . 
H8B H 0.3560 -0.2797 0.7922 0.104 Uiso 1 1 calc R . . 
H8C H 0.4270 -0.2607 0.7868 0.104 Uiso 1 1 calc R . . 
C9 C 0.46912(17) -0.04597(18) 0.7482(2) 0.0309(10) Uani 1 1 d . . . 
H9A H 0.4922 -0.0501 0.6992 0.037 Uiso 1 1 calc R . . 
H9B H 0.4920 -0.0694 0.7894 0.037 Uiso 1 1 calc R . . 
C10 C 0.4680(2) 0.02281(18) 0.7712(3) 0.0404(11) Uani 1 1 d . . . 
H10A H 0.4433 0.0462 0.7316 0.049 Uiso 1 1 calc R . . 
H10B H 0.4473 0.0270 0.8220 0.049 Uiso 1 1 calc R . . 
C11 C 0.5864(2) 0.0311(3) 0.7668(4) 0.084(2) Uani 1 1 d . . . 
H11A H 0.6153 0.0607 0.7913 0.126 Uiso 1 1 calc R . . 
H11B H 0.5939 0.0286 0.7106 0.126 Uiso 1 1 calc R . . 
H11C H 0.5921 -0.0103 0.7906 0.126 Uiso 1 1 calc R . . 
C12 C 0.5283(3) 0.0506(3) 0.7778(5) 0.124(3) Uani 1 1 d U . . 
H12A H 0.5247 0.0880 0.7439 0.149 Uiso 1 1 calc R . . 
H12B H 0.5298 0.0670 0.8320 0.149 Uiso 1 1 calc R . . 
C13 C 0.37033(19) -0.07382(19) 0.8110(2) 0.0356(10) Uani 1 1 d . . . 
H13A H 0.3292 -0.0924 0.8004 0.043 Uiso 1 1 calc R . . 
H13B H 0.3641 -0.0295 0.8255 0.043 Uiso 1 1 calc R . . 
C14 C 0.4004(2) -0.1078(3) 0.8804(3) 0.0572(14) Uani 1 1 d . . . 
H14A H 0.4073 -0.1519 0.8655 0.069 Uiso 1 1 calc R . . 
H14B H 0.4412 -0.0887 0.8915 0.069 Uiso 1 1 calc R . . 
C15 C 0.3650(3) -0.1065(3) 0.9521(3) 0.0662(15) Uani 1 1 d . . . 
H15A H 0.3241 -0.1253 0.9411 0.079 Uiso 1 1 calc R . . 
H15B H 0.3585 -0.0625 0.9675 0.079 Uiso 1 1 calc R . . 
C16 C 0.3950(3) -0.1406(3) 1.0196(3) 0.0727(17) Uani 1 1 d . . . 
H16A H 0.3690 -0.1375 1.0655 0.109 Uiso 1 1 calc R . . 
H16B H 0.4353 -0.1219 1.0317 0.109 Uiso 1 1 calc R . . 
H16C H 0.4004 -0.1847 1.0057 0.109 Uiso 1 1 calc R . . 
C17 C 0.30977(19) 0.30362(18) 0.8920(2) 0.0331(10) Uani 1 1 d . . . 
H17A H 0.3455 0.3130 0.8591 0.040 Uiso 1 1 calc R . . 
H17B H 0.2813 0.2768 0.8609 0.040 Uiso 1 1 calc R . . 
C18 C 0.2772(2) 0.36424(19) 0.9095(2) 0.0431(12) Uani 1 1 d . . . 
H18A H 0.3011 0.3879 0.9496 0.052 Uiso 1 1 calc R . . 
H18B H 0.2360 0.3553 0.9304 0.052 Uiso 1 1 calc R . . 
C19 C 0.2705(3) 0.4035(2) 0.8341(3) 0.0541(13) Uani 1 1 d . . . 
H19A H 0.2521 0.4444 0.8474 0.065 Uiso 1 1 calc R . . 
H19B H 0.3120 0.4117 0.8137 0.065 Uiso 1 1 calc R . . 
C20 C 0.2316(3) 0.3733(2) 0.7705(3) 0.0673(16) Uani 1 1 d . . . 
H20A H 0.2300 0.4005 0.7245 0.101 Uiso 1 1 calc R . . 
H20B H 0.1899 0.3666 0.7894 0.101 Uiso 1 1 calc R . . 
H20C H 0.2497 0.3330 0.7564 0.101 Uiso 1 1 calc R . . 
C21 C 0.28149(18) 0.25479(18) 1.0204(2) 0.0291(9) Uani 1 1 d . . . 
H21A H 0.2989 0.2312 1.0655 0.035 Uiso 1 1 calc R . . 
H21B H 0.2672 0.2956 1.0404 0.035 Uiso 1 1 calc R . . 
C22 C 0.22640(19) 0.2194(2) 0.9880(2) 0.0369(10) Uani 1 1 d . . . 
H22A H 0.2403 0.1800 0.9638 0.044 Uiso 1 1 calc R . . 
H22B H 0.2054 0.2447 0.9470 0.044 Uiso 1 1 calc R . . 
C23 C 0.1817(2) 0.2048(3) 1.0525(3) 0.0659(16) Uani 1 1 d . . . 
H23A H 0.1470 0.1801 1.0301 0.079 Uiso 1 1 calc R . . 
H23B H 0.2029 0.1786 1.0926 0.079 Uiso 1 1 calc R . . 
C24 C 0.1563(3) 0.2620(4) 1.0915(3) 0.101(3) Uani 1 1 d . . . 
H24A H 0.1279 0.2493 1.1323 0.151 Uiso 1 1 calc R . . 
H24B H 0.1343 0.2877 1.0526 0.151 Uiso 1 1 calc R . . 
H24C H 0.1902 0.2862 1.1152 0.151 Uiso 1 1 calc R . . 
C25 C 0.3580(2) 0.20652(19) 0.9309(2) 0.0382(11) Uani 1 1 d . . . 
H25A H 0.3923 0.2169 0.8959 0.046 Uiso 1 1 calc R . . 
H25B H 0.3254 0.1861 0.8985 0.046 Uiso 1 1 calc R . . 
C26 C 0.3812(2) 0.1601(2) 0.9918(2) 0.0450(12) Uani 1 1 d . . . 
H26A H 0.4129 0.1803 1.0259 0.054 Uiso 1 1 calc R . . 
H26B H 0.3468 0.1470 1.0250 0.054 Uiso 1 1 calc R . . 
C27 C 0.4087(2) 0.1033(2) 0.9527(3) 0.0575(14) Uani 1 1 d . . . 
H27A H 0.3776 0.0843 0.9168 0.069 Uiso 1 1 calc R . . 
H27B H 0.4442 0.1163 0.9213 0.069 Uiso 1 1 calc R . . 
C28 C 0.4295(3) 0.0557(2) 1.0126(3) 0.0714(17) Uani 1 1 d . . . 
H28A H 0.4479 0.0199 0.9860 0.107 Uiso 1 1 calc R . . 
H28B H 0.3940 0.0416 1.0423 0.107 Uiso 1 1 calc R . . 
H28C H 0.4600 0.0746 1.0484 0.107 Uiso 1 1 calc R . . 
C29 C 0.3815(2) 0.3018(2) 1.0100(2) 0.0439(12) Uani 1 1 d . . . 
H29A H 0.3616 0.3368 1.0376 0.053 Uiso 1 1 calc R . . 
H29B H 0.3990 0.2733 1.0504 0.053 Uiso 1 1 calc R . . 
C30 C 0.4339(3) 0.3278(3) 0.9628(3) 0.0827(18) Uani 1 1 d U . . 
H30A H 0.4177 0.3560 0.9212 0.099 Uiso 1 1 calc R . . 
H30B H 0.4569 0.2935 0.9380 0.099 Uiso 1 1 calc R . . 
C31 C 0.4795(3) 0.3670(3) 1.0248(5) 0.103(2) Uani 1 1 d . . . 
H31A H 0.5010 0.4020 0.9990 0.123 Uiso 1 1 calc R . . 
H31B H 0.4571 0.3828 1.0706 0.123 Uiso 1 1 calc R . . 
C32 C 0.5190(3) 0.3184(3) 1.0443(5) 0.120(3) Uani 1 1 d . . . 
H32A H 0.5512 0.3335 1.0807 0.179 Uiso 1 1 calc R . . 
H32B H 0.5380 0.3024 0.9968 0.179 Uiso 1 1 calc R . . 
H32C H 0.4959 0.2848 1.0691 0.179 Uiso 1 1 calc R . . 
C33 C 0.8174(2) 0.19500(19) 0.8964(2) 0.0373(10) Uani 1 1 d . . . 
H33A H 0.7943 0.2250 0.8629 0.045 Uiso 1 1 calc R . . 
H33B H 0.8511 0.1778 0.8649 0.045 Uiso 1 1 calc R . . 
C34 C 0.7750(2) 0.1425(2) 0.9165(3) 0.0530(13) Uani 1 1 d . . . 
H34A H 0.7402 0.1590 0.9466 0.064 Uiso 1 1 calc R . . 
H34B H 0.7974 0.1118 0.9498 0.064 Uiso 1 1 calc R . . 
C35 C 0.7501(3) 0.1100(2) 0.8423(3) 0.0585(14) Uani 1 1 d . . . 
H35A H 0.7167 0.0811 0.8568 0.070 Uiso 1 1 calc R . . 
H35B H 0.7322 0.1419 0.8066 0.070 Uiso 1 1 calc R . . 
C36 C 0.7974(3) 0.0744(3) 0.8002(3) 0.0847(19) Uani 1 1 d . . . 
H36A H 0.7788 0.0559 0.7528 0.127 Uiso 1 1 calc R . . 
H36B H 0.8138 0.0411 0.8341 0.127 Uiso 1 1 calc R . . 
H36C H 0.8308 0.1025 0.7857 0.127 Uiso 1 1 calc R . . 
C37 C 0.8846(2) 0.18735(19) 1.0175(2) 0.0379(11) Uani 1 1 d . . . 
H37A H 0.9029 0.2124 1.0608 0.046 Uiso 1 1 calc R . . 
H37B H 0.8567 0.1563 1.0410 0.046 Uiso 1 1 calc R . . 
C38 C 0.9355(2) 0.1526(2) 0.9783(3) 0.0483(12) Uani 1 1 d . . . 
H38A H 0.9629 0.1824 0.9516 0.058 Uiso 1 1 calc R . . 
H38B H 0.9181 0.1233 0.9388 0.058 Uiso 1 1 calc R . . 
C39 C 0.9715(3) 0.1168(3) 1.0415(3) 0.0736(17) Uani 1 1 d . . . 
H39A H 0.9864 0.1470 1.0815 0.088 Uiso 1 1 calc R . . 
H39B H 0.9430 0.0878 1.0673 0.088 Uiso 1 1 calc R . . 
C40 C 1.0220(4) 0.0825(4) 1.0159(5) 0.135(3) Uani 1 1 d . . . 
H40A H 1.0412 0.0605 1.0604 0.203 Uiso 1 1 calc R . . 
H40B H 1.0520 0.1109 0.9928 0.203 Uiso 1 1 calc R . . 
H40C H 1.0081 0.0520 0.9765 0.203 Uiso 1 1 calc R . . 
C41 C 0.79767(18) 0.25782(19) 1.0187(2) 0.0332(10) Uani 1 1 d . . . 
H41A H 0.7746 0.2227 1.0417 0.040 Uiso 1 1 calc R . . 
H41B H 0.8190 0.2801 1.0622 0.040 Uiso 1 1 calc R . . 
C42 C 0.7520(2) 0.3021(2) 0.9806(2) 0.0485(12) Uani 1 1 d . . . 
H42A H 0.7316 0.2814 0.9352 0.058 Uiso 1 1 calc R . . 
H42B H 0.7738 0.3395 0.9615 0.058 Uiso 1 1 calc R . . 
C43 C 0.7039(2) 0.3215(2) 1.0394(3) 0.0497(12) Uani 1 1 d . . . 
H43A H 0.6716 0.3463 1.0118 0.060 Uiso 1 1 calc R . . 
H43B H 0.6841 0.2835 1.0603 0.060 Uiso 1 1 calc R . . 
C44 C 0.7299(2) 0.3599(2) 1.1076(3) 0.0538(13) Uani 1 1 d . . . 
H44A H 0.6968 0.3700 1.1435 0.081 Uiso 1 1 calc R . . 
H44B H 0.7478 0.3986 1.0877 0.081 Uiso 1 1 calc R . . 
H44C H 0.7618 0.3357 1.1355 0.081 Uiso 1 1 calc R . . 
C45 C 0.88472(18) 0.28196(18) 0.9297(2) 0.0300(9) Uani 1 1 d . . . 
H45A H 0.9123 0.2625 0.8913 0.036 Uiso 1 1 calc R . . 
H45B H 0.8569 0.3107 0.9005 0.036 Uiso 1 1 calc R . . 
C46 C 0.9237(2) 0.32022(19) 0.9862(2) 0.0365(10) Uani 1 1 d . . . 
H46A H 0.9563 0.2936 1.0099 0.044 Uiso 1 1 calc R . . 
H46B H 0.8977 0.3360 1.0288 0.044 Uiso 1 1 calc R . . 
C47 C 0.95266(19) 0.37462(18) 0.9443(2) 0.0348(10) Uani 1 1 d . . . 
H47A H 0.9201 0.4044 0.9276 0.042 Uiso 1 1 calc R . . 
H47B H 0.9729 0.3591 0.8967 0.042 Uiso 1 1 calc R . . 
C48 C 0.9997(2) 0.4083(2) 0.9957(3) 0.0527(13) Uani 1 1 d . . . 
H48A H 1.0175 0.4430 0.9664 0.079 Uiso 1 1 calc R . . 
H48B H 1.0324 0.3791 1.0117 0.079 Uiso 1 1 calc R . . 
H48C H 0.9797 0.4246 1.0423 0.079 Uiso 1 1 calc R . . 
C49 C 0.95508(19) 0.5494(2) 0.7532(3) 0.0430(11) Uani 1 1 d . . . 
H49A H 0.9784 0.5721 0.7130 0.052 Uiso 1 1 calc R . . 
H49B H 0.9641 0.5699 0.8041 0.052 Uiso 1 1 calc R . . 
C50 C 0.9787(2) 0.4832(2) 0.7574(3) 0.0551(13) Uani 1 1 d . . . 
H50A H 0.9715 0.4612 0.7071 0.066 Uiso 1 1 calc R . . 
H50B H 0.9585 0.4596 0.7995 0.066 Uiso 1 1 calc R . . 
C51 C 1.0510(4) 0.4912(4) 0.7762(5) 0.132(3) Uani 1 1 d D . . 
H51A H 1.0691 0.5209 0.7387 0.158 Uiso 1 1 calc R . . 
H51B H 1.0574 0.5080 0.8297 0.158 Uiso 1 1 calc R . . 
C52 C 1.0822(6) 0.4273(4) 0.7694(8) 0.261(7) Uani 1 1 d DU . . 
H52A H 1.1262 0.4315 0.7818 0.391 Uiso 1 1 calc R . . 
H52B H 1.0766 0.4114 0.7159 0.391 Uiso 1 1 calc R . . 
H52C H 1.0637 0.3980 0.8062 0.391 Uiso 1 1 calc R . . 
C53 C 0.8712(2) 0.62669(17) 0.7364(2) 0.0346(10) Uani 1 1 d . . . 
H53A H 0.8259 0.6313 0.7334 0.042 Uiso 1 1 calc R . . 
H53B H 0.8855 0.6437 0.7875 0.042 Uiso 1 1 calc R . . 
C54 C 0.8987(2) 0.66595(19) 0.6720(2) 0.0377(11) Uani 1 1 d . . . 
H54A H 0.9436 0.6583 0.6703 0.045 Uiso 1 1 calc R . . 
H54B H 0.8803 0.6535 0.6208 0.045 Uiso 1 1 calc R . . 
C55 C 0.8870(2) 0.73482(18) 0.6859(2) 0.0382(11) Uani 1 1 d . . . 
H55A H 0.9030 0.7465 0.7386 0.046 Uiso 1 1 calc R . . 
H55B H 0.8421 0.7428 0.6841 0.046 Uiso 1 1 calc R . . 
C56 C 0.9178(2) 0.7749(2) 0.6248(3) 0.0505(13) Uani 1 1 d . . . 
H56A H 0.9091 0.8191 0.6349 0.076 Uiso 1 1 calc R . . 
H56B H 0.9018 0.7636 0.5726 0.076 Uiso 1 1 calc R . . 
H56C H 0.9624 0.7679 0.6274 0.076 Uiso 1 1 calc R . . 
C57 C 0.84721(19) 0.52385(19) 0.7934(2) 0.0394(11) Uani 1 1 d . . . 
H57A H 0.8509 0.4782 0.7851 0.047 Uiso 1 1 calc R . . 
H57B H 0.8037 0.5354 0.7827 0.047 Uiso 1 1 calc R . . 
C58 C 0.8625(2) 0.53778(19) 0.8791(2) 0.0384(11) Uani 1 1 d . . . 
H58A H 0.9044 0.5224 0.8924 0.046 Uiso 1 1 calc R . . 
H58B H 0.8618 0.5835 0.8878 0.046 Uiso 1 1 calc R . . 
C59 C 0.8165(2) 0.5066(2) 0.9316(3) 0.0489(12) Uani 1 1 d . . . 
H59A H 0.7757 0.5266 0.9231 0.059 Uiso 1 1 calc R . . 
H59B H 0.8125 0.4621 0.9165 0.059 Uiso 1 1 calc R . . 
C60 C 0.8339(2) 0.5105(2) 1.0166(3) 0.0585(14) Uani 1 1 d . . . 
H60A H 0.8022 0.4901 1.0474 0.088 Uiso 1 1 calc R . . 
H60B H 0.8375 0.5545 1.0321 0.088 Uiso 1 1 calc R . . 
H60C H 0.8734 0.4895 1.0258 0.088 Uiso 1 1 calc R . . 
C61 C 0.87324(19) 0.5292(2) 0.6546(2) 0.0379(11) Uani 1 1 d . . . 
H61A H 0.9032 0.5467 0.6177 0.045 Uiso 1 1 calc R . . 
H61B H 0.8808 0.4836 0.6578 0.045 Uiso 1 1 calc R . . 
C62 C 0.8096(2) 0.5389(2) 0.6201(3) 0.0449(12) Uani 1 1 d . . . 
H62A H 0.7999 0.5841 0.6193 0.054 Uiso 1 1 calc R . . 
H62B H 0.7791 0.5178 0.6531 0.054 Uiso 1 1 calc R . . 
C63 C 0.8053(3) 0.5132(3) 0.5381(3) 0.0735(17) Uani 1 1 d . . . 
H63A H 0.8395 0.5306 0.5077 0.088 Uiso 1 1 calc R . . 
H63B H 0.8109 0.4673 0.5405 0.088 Uiso 1 1 calc R . . 
C64 C 0.7474(3) 0.5266(3) 0.4961(4) 0.099(2) Uani 1 1 d . . . 
H64A H 0.7480 0.5073 0.4441 0.148 Uiso 1 1 calc R . . 
H64B H 0.7424 0.5719 0.4906 0.148 Uiso 1 1 calc R . . 
H64C H 0.7130 0.5095 0.5255 0.148 Uiso 1 1 calc R . . 
N1 N 0.40682(14) -0.07610(14) 0.73609(17) 0.0274(8) Uani 1 1 d . . . 
N2 N 0.33246(15) 0.26669(15) 0.96321(17) 0.0310(8) Uani 1 1 d . . . 
N3 N 0.84604(15) 0.23086(15) 0.96534(17) 0.0317(8) Uani 1 1 d . . . 
N4 N 0.88677(15) 0.55688(15) 0.73416(18) 0.0340(8) Uani 1 1 d . . . 
O1 O 0.46562(13) 0.31004(13) 0.65551(15) 0.0415(8) Uani 1 1 d . . . 
O2 O 0.42324(14) 0.35186(15) 0.77404(16) 0.0502(9) Uani 1 1 d . . . 
O3 O 0.35910(12) 0.29094(13) 0.68492(15) 0.0369(7) Uani 1 1 d . . . 
O4 O 0.43959(14) 0.24242(17) 0.76359(18) 0.0479(9) Uani 1 1 d . . . 
O5 O 0.77753(16) 0.37005(15) 0.65121(17) 0.0598(10) Uani 1 1 d . . . 
O6 O 0.87327(13) 0.36106(13) 0.7231(2) 0.0554(9) Uani 1 1 d . . . 
O7 O 0.77840(14) 0.37905(14) 0.79043(17) 0.0503(8) Uani 1 1 d . . . 
O8 O 0.79696(14) 0.27979(14) 0.73199(18) 0.0419(8) Uani 1 1 d . . . 
O9 O 0.38224(13) 0.14354(13) 0.70375(19) 0.0496(9) Uani 1 1 d . . . 
O10 O 0.29068(13) 0.19980(14) 0.73823(17) 0.0352(7) Uani 1 1 d . . . 
O11 O 0.28603(16) 0.11823(13) 0.64020(16) 0.0514(9) Uani 1 1 d . . . 
O12 O 0.30183(15) 0.09381(14) 0.77591(17) 0.0494(8) Uani 1 1 d . . . 
O13 O 0.88563(13) 0.21115(13) 0.67888(16) 0.0439(8) Uani 1 1 d . . . 
O14 O 0.99487(15) 0.18891(16) 0.66695(17) 0.0599(10) Uani 1 1 d . . . 
O15 O 0.96212(18) 0.28066(17) 0.7346(3) 0.0738(13) Uani 1 1 d . . . 
O16 O 0.94673(14) 0.18001(16) 0.79156(16) 0.0535(9) Uani 1 1 d . . . 
S1 S 0.42153(5) 0.30311(5) 0.71603(5) 0.0328(3) Uani 1 1 d . . . 
S2 S 0.80648(5) 0.35138(5) 0.72367(6) 0.0318(3) Uani 1 1 d . . . 
S3 S 0.31670(5) 0.13464(4) 0.71318(6) 0.0302(3) Uani 1 1 d . . . 
S4 S 0.94748(5) 0.21101(5) 0.71758(6) 0.0384(3) Uani 1 1 d . . . 
H10 H 0.3125(18) 0.2247(18) 0.719(2) 0.027(13) Uiso 1 1 d . . . 
H4 H 0.424(3) 0.210(3) 0.741(3) 0.09(2) Uiso 1 1 d . . . 
H8 H 0.829(3) 0.260(3) 0.709(4) 0.13(3) Uiso 1 1 d . . . 
H15 H 0.932(4) 0.302(4) 0.733(5) 0.17(4) Uiso 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 
C1 N1 1.515(5) . ? 
C1 C2 1.531(5) . ? 
C2 C3 1.522(6) . ? 
C3 C4 1.533(6) . ? 
C5 N1 1.513(5) . ? 
C5 C6 1.519(6) . ? 
C6 C7 1.531(6) . ? 
C7 C8 1.478(6) . ? 
C9 N1 1.509(5) . ? 
C9 C10 1.524(5) . ? 
C10 C12 1.441(8) . ? 
C11 C12 1.347(8) . ? 
C13 N1 1.521(5) . ? 
C13 C14 1.526(6) . ? 
C14 C15 1.463(6) . ? 
C15 C16 1.501(7) . ? 
C17 C18 1.510(6) . ? 
C17 N2 1.523(5) . ? 
C18 C19 1.542(6) . ? 
C19 C20 1.508(6) . ? 
C21 C22 1.511(5) . ? 
C21 N2 1.515(5) . ? 
C22 C23 1.519(6) . ? 
C23 C24 1.504(8) . ? 
C25 N2 1.512(5) . ? 
C25 C26 1.517(6) . ? 
C26 C27 1.516(6) . ? 
C27 C28 1.506(6) . ? 
C29 C30 1.516(6) . ? 
C29 N2 1.517(5) . ? 
C30 C31 1.660(9) . ? 
C31 C32 1.385(8) . ? 
C33 C34 1.498(6) . ? 
C33 N3 1.526(5) . ? 
C34 C35 1.533(6) . ? 
C35 C36 1.479(7) . ? 
C37 C38 1.503(6) . ? 
C37 N3 1.526(5) . ? 
C38 C39 1.526(6) . ? 
C39 C40 1.398(9) . ? 
C41 C42 1.508(6) . ? 
C41 N3 1.521(5) . ? 
C42 C43 1.525(6) . ? 
C43 C44 1.524(6) . ? 
C45 C46 1.510(5) . ? 
C45 N3 1.515(5) . ? 
C46 C47 1.512(5) . ? 
C47 C48 1.515(6) . ? 
C49 C50 1.508(6) . ? 
C49 N4 1.521(5) . ? 
C50 C51 1.605(9) . ? 
C51 C52 1.532(2) . ? 
C53 C54 1.518(5) . ? 
C53 N4 1.532(5) . ? 
C54 C55 1.515(6) . ? 
C55 C56 1.519(6) . ? 
C57 N4 1.517(5) . ? 
C57 C58 1.524(6) . ? 
C58 C59 1.513(6) . ? 
C59 C60 1.495(6) . ? 
C61 C62 1.504(6) . ? 
C61 N4 1.506(5) . ? 
C62 C63 1.507(6) . ? 
C63 C64 1.461(7) . ? 
O1 S1 1.433(3) . ? 
O2 S1 1.439(3) . ? 
O3 S1 1.469(3) . ? 
O4 S1 1.577(3) . ? 
O5 S2 1.433(3) . ? 
O6 S2 1.466(3) . ? 
O7 S2 1.434(3) . ? 
O8 S2 1.553(3) . ? 
O9 S3 1.450(3) . ? 
O10 S3 1.568(3) . ? 
O11 S3 1.444(3) . ? 
O12 S3 1.426(3) . ? 
O13 S4 1.484(3) . ? 
O14 S4 1.440(3) . ? 
O15 S4 1.550(4) . ? 
O16 S4 1.428(3) . ? 
 
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 114.5(3) . . ? 
C3 C2 C1 110.5(4) . . ? 
C2 C3 C4 110.3(4) . . ? 
N1 C5 C6 115.5(3) . . ? 
C5 C6 C7 110.8(4) . . ? 
C8 C7 C6 113.7(4) . . ? 
N1 C9 C10 115.4(3) . . ? 
C12 C10 C9 113.5(4) . . ? 
C11 C12 C10 135.5(6) . . ? 
N1 C13 C14 114.6(3) . . ? 
C15 C14 C13 114.8(4) . . ? 
C14 C15 C16 114.0(5) . . ? 
C18 C17 N2 115.6(3) . . ? 
C17 C18 C19 109.8(3) . . ? 
C20 C19 C18 114.1(4) . . ? 
C22 C21 N2 115.6(3) . . ? 
C21 C22 C23 110.6(3) . . ? 
C24 C23 C22 113.7(5) . . ? 
N2 C25 C26 115.2(3) . . ? 
C27 C26 C25 110.5(3) . . ? 
C28 C27 C26 111.0(4) . . ? 
C30 C29 N2 115.4(3) . . ? 
C29 C30 C31 106.9(4) . . ? 
C32 C31 C30 97.6(6) . . ? 
C34 C33 N3 116.2(3) . . ? 
C33 C34 C35 111.0(4) . . ? 
C36 C35 C34 113.7(5) . . ? 
C38 C37 N3 116.1(3) . . ? 
C37 C38 C39 107.7(4) . . ? 
C40 C39 C38 115.9(5) . . ? 
C42 C41 N3 115.9(3) . . ? 
C41 C42 C43 110.0(3) . . ? 
C44 C43 C42 113.8(4) . . ? 
C46 C45 N3 116.3(3) . . ? 
C45 C46 C47 110.4(3) . . ? 
C46 C47 C48 112.0(3) . . ? 
C50 C49 N4 116.0(4) . . ? 
C49 C50 C51 103.9(4) . . ? 
C52 C51 C50 108.9(8) . . ? 
C54 C53 N4 115.5(3) . . ? 
C55 C54 C53 110.8(3) . . ? 
C54 C55 C56 111.3(4) . . ? 
N4 C57 C58 115.8(3) . . ? 
C59 C58 C57 110.6(4) . . ? 
C60 C59 C58 113.3(4) . . ? 
C62 C61 N4 117.2(3) . . ? 
C61 C62 C63 110.5(4) . . ? 
C64 C63 C62 114.8(5) . . ? 
C9 N1 C5 105.9(3) . . ? 
C9 N1 C1 111.7(3) . . ? 
C5 N1 C1 111.3(3) . . ? 
C9 N1 C13 110.8(3) . . ? 
C5 N1 C13 110.6(3) . . ? 
C1 N1 C13 106.7(3) . . ? 
C25 N2 C21 111.9(3) . . ? 
C25 N2 C29 110.8(3) . . ? 
C21 N2 C29 105.0(3) . . ? 
C25 N2 C17 105.4(3) . . ? 
C21 N2 C17 112.0(3) . . ? 
C29 N2 C17 112.0(3) . . ? 
C45 N3 C41 111.4(3) . . ? 
C45 N3 C37 111.9(3) . . ? 
C41 N3 C37 105.0(3) . . ? 
C45 N3 C33 105.8(3) . . ? 
C41 N3 C33 112.2(3) . . ? 
C37 N3 C33 110.6(3) . . ? 
C61 N4 C57 108.5(3) . . ? 
C61 N4 C49 108.7(3) . . ? 
C57 N4 C49 112.0(3) . . ? 
C61 N4 C53 111.6(3) . . ? 
C57 N4 C53 108.0(3) . . ? 
C49 N4 C53 108.2(3) . . ? 
O1 S1 O2 114.51(17) . . ? 
O1 S1 O3 112.60(16) . . ? 
O2 S1 O3 112.75(18) . . ? 
O1 S1 O4 107.13(18) . . ? 
O2 S1 O4 103.88(19) . . ? 
O3 S1 O4 104.91(17) . . ? 
O5 S2 O7 112.70(19) . . ? 
O5 S2 O6 111.7(2) . . ? 
O7 S2 O6 112.7(2) . . ? 
O5 S2 O8 107.31(19) . . ? 
O7 S2 O8 105.93(18) . . ? 
O6 S2 O8 105.90(17) . . ? 
O12 S3 O11 113.10(18) . . ? 
O12 S3 O9 113.84(19) . . ? 
O11 S3 O9 111.8(2) . . ? 
O12 S3 O10 104.51(18) . . ? 
O11 S3 O10 106.86(17) . . ? 
O9 S3 O10 105.95(17) . . ? 
O16 S4 O14 113.72(19) . . ? 
O16 S4 O13 111.51(19) . . ? 
O14 S4 O13 112.69(18) . . ? 
O16 S4 O15 106.7(2) . . ? 
O14 S4 O15 106.4(2) . . ? 
O13 S4 O15 105.15(18) . . ? 
 
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 
O10 H10 O3  0.79(4) 1.84(4) 2.628(4) 171(4) . 
O4 H4 O9  0.85(6) 1.81(6) 2.649(5) 171(6) . 
O8 H8 O13  0.92(7) 1.70(7) 2.603(4) 168(7) . 
O15 H15 O6  0.81(8) 1.79(8) 2.590(5) 170(9) . 
 
_diffrn_measured_fraction_theta_max    0.996 
_diffrn_reflns_theta_full              25.03 
_diffrn_measured_fraction_theta_full   0.996 
_refine_diff_density_max    1.259 
_refine_diff_density_min   -0.691 
_refine_diff_density_rms    0.068 
