 
data_01esp001
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C36 H38 N2 O10 S' 
_chemical_formula_weight          690.74 
 
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' 
 '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' 
 'H'  'H'   0.0000   0.0000 
 '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)
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y+1/2, -z' 
 
_cell_length_a                    7.8231(2) 
_cell_length_b                    12.9445(3) 
_cell_length_c                    17.3686(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  95.6680(10) 
_cell_angle_gamma                 90.00 
_cell_volume                      1750.25(7) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     180(2) 
_cell_measurement_reflns_used     10147
_cell_measurement_theta_min       1.00 
_cell_measurement_theta_max       27.48 
 
_exptl_crystal_description        block 
_exptl_crystal_colour             colourless 
_exptl_crystal_size_max           0.20 
_exptl_crystal_size_mid           0.10 
_exptl_crystal_size_min           0.10 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.311 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              728 
_exptl_absorpt_coefficient_mu     0.152 
_exptl_absorpt_correction_type   multi-scan 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
_exptl_absorpt_process_details    'SORTAV (Blessing, 1997)' 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       180(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             13193 
_diffrn_reflns_av_R_equivalents   0.0762 
_diffrn_reflns_av_sigmaI/netI     0.0679 
_diffrn_reflns_limit_h_min        -9 
_diffrn_reflns_limit_h_max        9 
_diffrn_reflns_limit_k_min        -15 
_diffrn_reflns_limit_k_max        15 
_diffrn_reflns_limit_l_min        -20 
_diffrn_reflns_limit_l_max        20 
_diffrn_reflns_theta_min          2.97 
_diffrn_reflns_theta_max          25.03 
_reflns_number_total              5997 
_reflns_number_gt                 5488 
_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)+(0.0595P)²+0.0000P] 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        0.0147(18) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 
_refine_ls_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.01(6) 
_refine_ls_number_reflns          5997 
_refine_ls_number_parameters      448 
_refine_ls_number_restraints      1 
_refine_ls_R_factor_all           0.0475 
_refine_ls_R_factor_gt            0.0418 
_refine_ls_wR_factor_ref          0.1037 
_refine_ls_wR_factor_gt           0.1006 
_refine_ls_goodness_of_fit_ref    1.027 
_refine_ls_restrained_S_all       1.027 
_refine_ls_shift/su_max           0.007 
_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 0.5026(3) 0.5533(3) 1.04484(15) 0.0367(6) Uani 1 1 d . . . 
H1 H 0.5573 0.4922 1.0295 0.044 Uiso 1 1 calc R . . 
C2 C 0.5090(4) 0.5795(3) 1.12317(18) 0.0498(9) Uani 1 1 d . . . 
H2 H 0.5660 0.5354 1.1612 0.060 Uiso 1 1 calc R . . 
C3 C 0.4323(4) 0.6698(3) 1.14535(18) 0.0506(9) Uani 1 1 d . . . 
H3 H 0.4381 0.6879 1.1985 0.061 Uiso 1 1 calc R . . 
C4 C 0.3488(4) 0.7325(3) 1.09126(19) 0.0529(9) Uani 1 1 d . . . 
H4 H 0.2975 0.7947 1.1067 0.064 Uiso 1 1 calc R . . 
C5 C 0.3383(4) 0.7059(3) 1.01372(17) 0.0430(7) Uani 1 1 d . . . 
H5 H 0.2771 0.7492 0.9764 0.052 Uiso 1 1 calc R . . 
C6 C 0.4164(3) 0.6165(2) 0.98994(14) 0.0299(6) Uani 1 1 d . . . 
C7 C 0.4103(3) 0.5911(2) 0.90493(14) 0.0297(6) Uani 1 1 d . . . 
H7A H 0.4324 0.5165 0.8987 0.036 Uiso 1 1 calc R . . 
H7B H 0.2940 0.6064 0.8796 0.036 Uiso 1 1 calc R . . 
C8 C 0.4967(3) 0.7577(2) 0.84448(16) 0.0316(6) Uani 1 1 d . . . 
H8A H 0.5171 0.8027 0.8899 0.047 Uiso 1 1 calc R . . 
H8B H 0.3756 0.7621 0.8240 0.047 Uiso 1 1 calc R . . 
H8C H 0.5693 0.7799 0.8047 0.047 Uiso 1 1 calc R . . 
C9 C 0.6929(3) 0.6067(2) 0.86256(13) 0.0228(5) Uani 1 1 d . . . 
C10 C 0.8770(3) 0.7613(2) 0.88868(14) 0.0243(5) Uani 1 1 d . . . 
C11 C 0.9375(3) 0.8517(2) 0.85794(16) 0.0327(6) Uani 1 1 d . . . 
H11 H 0.9487 0.8565 0.8041 0.039 Uiso 1 1 calc R . . 
C12 C 0.9815(4) 0.9347(2) 0.90586(19) 0.0448(7) Uani 1 1 d . . . 
H12 H 1.0243 0.9962 0.8848 0.054 Uiso 1 1 calc R . . 
C13 C 0.9635(4) 0.9292(3) 0.98448(19) 0.0475(8) Uani 1 1 d . . . 
H13 H 0.9938 0.9864 1.0172 0.057 Uiso 1 1 calc R . . 
C14 C 0.9017(4) 0.8403(3) 1.01437(17) 0.0433(8) Uani 1 1 d . . . 
H14 H 0.8875 0.8366 1.0680 0.052 Uiso 1 1 calc R . . 
C15 C 0.8592(3) 0.7549(2) 0.96712(15) 0.0320(6) Uani 1 1 d . . . 
H15 H 0.8185 0.6931 0.9885 0.038 Uiso 1 1 calc R . . 
C16 C 0.9353(3) 0.63811(18) 0.78741(13) 0.0202(5) Uani 1 1 d . . . 
C17 C 0.8729(3) 0.55470(19) 0.72935(13) 0.0197(5) Uani 1 1 d . . . 
C18 C 0.9698(3) 0.45422(18) 0.74323(13) 0.0206(5) Uani 1 1 d . . . 
C19 C 0.8904(3) 0.36642(19) 0.76844(13) 0.0232(5) Uani 1 1 d . . . 
H19 H 0.7723 0.3685 0.7769 0.028 Uiso 1 1 calc R . . 
C20 C 0.9826(3) 0.2759(2) 0.78123(14) 0.0286(6) Uani 1 1 d . . . 
H20 H 0.9276 0.2161 0.7988 0.034 Uiso 1 1 calc R . . 
C21 C 1.1552(3) 0.2716(2) 0.76867(15) 0.0312(6) Uani 1 1 d . . . 
H21 H 1.2177 0.2089 0.7770 0.037 Uiso 1 1 calc R . . 
C22 C 1.2357(3) 0.3593(2) 0.74388(15) 0.0325(6) Uani 1 1 d . . . 
H22 H 1.3540 0.3571 0.7358 0.039 Uiso 1 1 calc R . . 
C23 C 1.1433(3) 0.4505(2) 0.73077(14) 0.0262(6) Uani 1 1 d . . . 
H23 H 1.1983 0.5103 0.7133 0.031 Uiso 1 1 calc R . . 
C24 C 0.8374(3) 0.59019(18) 0.64678(13) 0.0199(5) Uani 1 1 d . . . 
H24 H 0.8738 0.5400 0.6078 0.024 Uiso 1 1 calc R . . 
C25 C 0.8559(3) 0.70205(18) 0.62462(13) 0.0182(5) Uani 1 1 d . . . 
H25 H 0.8368 0.7472 0.6697 0.022 Uiso 1 1 calc R . . 
C26 C 1.1333(3) 0.78415(19) 0.64453(14) 0.0217(5) Uani 1 1 d . . . 
C27 C 1.3181(3) 0.7606(2) 0.63792(16) 0.0308(6) Uani 1 1 d . . . 
H27A H 1.3842 0.8250 0.6403 0.046 Uiso 1 1 calc R . . 
H27B H 1.3295 0.7259 0.5885 0.046 Uiso 1 1 calc R . . 
H27C H 1.3620 0.7153 0.6806 0.046 Uiso 1 1 calc R . . 
C28 C 0.7336(3) 0.73329(17) 0.55496(13) 0.0182(5) Uani 1 1 d . . . 
H28 H 0.6126 0.7236 0.5675 0.022 Uiso 1 1 calc R . . 
C29 C 0.6301(3) 0.60864(18) 0.46008(14) 0.0233(5) Uani 1 1 d . . . 
C30 C 0.6749(3) 0.5561(2) 0.38858(15) 0.0335(6) Uani 1 1 d . . . 
H30A H 0.5925 0.5004 0.3750 0.050 Uiso 1 1 calc R . . 
H30B H 0.7909 0.5271 0.3975 0.050 Uiso 1 1 calc R . . 
H30C H 0.6709 0.6061 0.3461 0.050 Uiso 1 1 calc R . . 
C31 C 0.7579(3) 0.84506(17) 0.52999(13) 0.0193(5) Uani 1 1 d . . . 
H31 H 0.8806 0.8553 0.5203 0.023 Uiso 1 1 calc R . . 
C32 C 0.8153(3) 0.99530(18) 0.60641(16) 0.0278(6) Uani 1 1 d . . . 
C33 C 0.7894(4) 1.0444(2) 0.68226(16) 0.0373(7) Uani 1 1 d . . . 
H33A H 0.9013 1.0604 0.7102 0.056 Uiso 1 1 calc R . . 
H33B H 0.7267 0.9968 0.7131 0.056 Uiso 1 1 calc R . . 
H33C H 0.7232 1.1083 0.6732 0.056 Uiso 1 1 calc R . . 
C34 C 0.6444(3) 0.87717(18) 0.45885(13) 0.0211(5) Uani 1 1 d . . . 
H34A H 0.6621 0.9514 0.4485 0.025 Uiso 1 1 calc R . . 
H34B H 0.6757 0.8374 0.4136 0.025 Uiso 1 1 calc R . . 
C35 C 0.3688(3) 0.80668(18) 0.41329(14) 0.0214(5) Uani 1 1 d . . . 
C36 C 0.1873(3) 0.7974(2) 0.43197(15) 0.0274(6) Uani 1 1 d . . . 
H36A H 0.1098 0.8025 0.3842 0.041 Uiso 1 1 calc R . . 
H36B H 0.1619 0.8532 0.4673 0.041 Uiso 1 1 calc R . . 
H36C H 0.1710 0.7306 0.4567 0.041 Uiso 1 1 calc R . . 
N1 N 0.8255(2) 0.67511(15) 0.83871(11) 0.0217(4) Uani 1 1 d . . . 
N2 N 0.5384(3) 0.65113(17) 0.86675(11) 0.0250(5) Uani 1 1 d . . . 
O1 O 0.7284(2) 0.51729(13) 0.87793(10) 0.0298(4) Uani 1 1 d . . . 
O2 O 1.0795(2) 0.67379(13) 0.78434(9) 0.0248(4) Uani 1 1 d . . . 
O3 O 1.03310(19) 0.71004(12) 0.60772(9) 0.0210(4) Uani 1 1 d . . . 
O4 O 1.0786(2) 0.85704(14) 0.67718(10) 0.0281(4) Uani 1 1 d . . . 
O5 O 0.76302(19) 0.66945(12) 0.48994(9) 0.0209(4) Uani 1 1 d . . . 
O6 O 0.4966(2) 0.60181(13) 0.48867(11) 0.0298(4) Uani 1 1 d . . . 
O7 O 0.7233(2) 0.90566(12) 0.59634(9) 0.0210(4) Uani 1 1 d . . . 
O8 O 0.9045(2) 1.02729(14) 0.55946(12) 0.0358(5) Uani 1 1 d . . . 
O9 O 0.46555(19) 0.85889(12) 0.46975(9) 0.0210(4) Uani 1 1 d . . . 
O10 O 0.4253(2) 0.77216(13) 0.35636(10) 0.0266(4) Uani 1 1 d . . . 
S1 S 0.64855(7) 0.55121(4) 0.69156(3) 0.02142(15) 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 
C1 C6 1.380(4) . ? 
C1 C2 1.398(4) . ? 
C2 C3 1.385(5) . ? 
C3 C4 1.359(5) . ? 
C4 C5 1.384(5) . ? 
C5 C6 1.391(4) . ? 
C6 C7 1.509(4) . ? 
C7 N2 1.476(3) . ? 
C8 N2 1.462(4) . ? 
C9 O1 1.213(3) . ? 
C9 N2 1.347(3) . ? 
C9 N1 1.455(3) . ? 
C10 C15 1.386(4) . ? 
C10 C11 1.389(4) . ? 
C10 N1 1.446(3) . ? 
C11 C12 1.381(4) . ? 
C12 C13 1.388(5) . ? 
C13 C14 1.370(5) . ? 
C14 C15 1.397(4) . ? 
C16 O2 1.225(3) . ? 
C16 N1 1.383(3) . ? 
C16 C17 1.524(3) . ? 
C17 C24 1.505(3) . ? 
C17 C18 1.513(3) . ? 
C17 S1 1.813(2) . ? 
C18 C19 1.387(3) . ? 
C18 C23 1.396(3) . ? 
C19 C20 1.383(4) . ? 
C20 C21 1.390(4) . ? 
C21 C22 1.388(4) . ? 
C22 C23 1.391(4) . ? 
C24 C25 1.509(3) . ? 
C24 S1 1.808(2) . ? 
C25 O3 1.449(3) . ? 
C25 C28 1.521(3) . ? 
C26 O4 1.201(3) . ? 
C26 O3 1.358(3) . ? 
C26 C27 1.493(3) . ? 
C28 O5 1.436(3) . ? 
C28 C31 1.528(3) . ? 
C29 O6 1.203(3) . ? 
C29 O5 1.365(3) . ? 
C29 C30 1.488(4) . ? 
C31 O7 1.442(3) . ? 
C31 C34 1.507(3) . ? 
C32 O8 1.198(3) . ? 
C32 O7 1.368(3) . ? 
C32 C33 1.494(4) . ? 
C34 O9 1.450(3) . ? 
C35 O10 1.208(3) . ? 
C35 O9 1.358(3) . ? 
C35 C36 1.492(4) . ? 
 
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 
C6 C1 C2 119.8(3) . . ? 
C3 C2 C1 120.0(3) . . ? 
C4 C3 C2 120.2(3) . . ? 
C3 C4 C5 120.2(3) . . ? 
C4 C5 C6 120.6(3) . . ? 
C1 C6 C5 119.2(3) . . ? 
C1 C6 C7 120.9(2) . . ? 
C5 C6 C7 119.9(2) . . ? 
N2 C7 C6 111.6(2) . . ? 
O1 C9 N2 125.6(2) . . ? 
O1 C9 N1 119.3(2) . . ? 
N2 C9 N1 115.1(2) . . ? 
C15 C10 C11 120.0(3) . . ? 
C15 C10 N1 119.7(2) . . ? 
C11 C10 N1 120.3(2) . . ? 
C12 C11 C10 119.9(3) . . ? 
C11 C12 C13 120.6(3) . . ? 
C14 C13 C12 119.3(3) . . ? 
C13 C14 C15 120.9(3) . . ? 
C10 C15 C14 119.3(3) . . ? 
O2 C16 N1 122.1(2) . . ? 
O2 C16 C17 118.3(2) . . ? 
N1 C16 C17 119.5(2) . . ? 
C24 C17 C18 117.17(19) . . ? 
C24 C17 C16 115.5(2) . . ? 
C18 C17 C16 112.38(18) . . ? 
C24 C17 S1 65.28(12) . . ? 
C18 C17 S1 119.24(17) . . ? 
C16 C17 S1 119.51(16) . . ? 
C19 C18 C23 119.6(2) . . ? 
C19 C18 C17 121.4(2) . . ? 
C23 C18 C17 119.0(2) . . ? 
C20 C19 C18 120.1(2) . . ? 
C19 C20 C21 120.6(2) . . ? 
C22 C21 C20 119.6(2) . . ? 
C21 C22 C23 120.1(2) . . ? 
C22 C23 C18 120.1(2) . . ? 
C17 C24 C25 121.5(2) . . ? 
C17 C24 S1 65.59(12) . . ? 
C25 C24 S1 118.70(16) . . ? 
O3 C25 C24 103.74(17) . . ? 
O3 C25 C28 111.03(17) . . ? 
C24 C25 C28 112.94(19) . . ? 
O4 C26 O3 124.1(2) . . ? 
O4 C26 C27 126.1(2) . . ? 
O3 C26 C27 109.7(2) . . ? 
O5 C28 C25 109.62(18) . . ? 
O5 C28 C31 106.71(17) . . ? 
C25 C28 C31 113.06(18) . . ? 
O6 C29 O5 123.1(2) . . ? 
O6 C29 C30 126.6(2) . . ? 
O5 C29 C30 110.3(2) . . ? 
O7 C31 C34 111.30(18) . . ? 
O7 C31 C28 104.47(17) . . ? 
C34 C31 C28 114.48(19) . . ? 
O8 C32 O7 122.7(2) . . ? 
O8 C32 C33 126.3(2) . . ? 
O7 C32 C33 111.0(2) . . ? 
O9 C34 C31 110.24(18) . . ? 
O10 C35 O9 123.5(2) . . ? 
O10 C35 C36 125.5(2) . . ? 
O9 C35 C36 110.9(2) . . ? 
C16 N1 C10 120.0(2) . . ? 
C16 N1 C9 118.57(19) . . ? 
C10 N1 C9 117.59(19) . . ? 
C9 N2 C8 124.6(2) . . ? 
C9 N2 C7 116.9(2) . . ? 
C8 N2 C7 118.1(2) . . ? 
C26 O3 C25 118.32(17) . . ? 
C29 O5 C28 117.09(18) . . ? 
C32 O7 C31 115.20(19) . . ? 
C35 O9 C34 117.59(18) . . ? 
C24 S1 C17 49.13(10) . . ? 
 
_diffrn_measured_fraction_theta_max    0.997 
_diffrn_reflns_theta_full              25.03 
_diffrn_measured_fraction_theta_full   0.997 
_refine_diff_density_max    0.173 
_refine_diff_density_min   -0.243 
_refine_diff_density_rms    0.040 
