Supplementary Material (ESI) for Chemical Communications
This jopurnal is (C) The Royal Society of Chemistry

 
data_Compound(1) 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 bis(tetraethylammonium) carbonate hepta-thiourea
; 
_chemical_name_common          ?
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C24 H68 N16 O3 S7' 
_chemical_formula_weight          853.36 
 
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    C2/c 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y, -z+1/2' 
 'x+1/2, y+1/2, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y, z-1/2' 
 '-x+1/2, -y+1/2, -z' 
 'x+1/2, -y+1/2, z-1/2' 
 
_cell_length_a                    25.462(4) 
_cell_length_b                    12.901(2) 
_cell_length_c                    17.355(3) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  124.009(3) 
_cell_angle_gamma                 90.00 
_cell_volume                      4725.8(14) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        block 
_exptl_crystal_colour             colorless 
_exptl_crystal_size_max           0.74 
_exptl_crystal_size_mid           0.71 
_exptl_crystal_size_min           0.61 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.199 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1840 
_exptl_absorpt_coefficient_mu     0.377 
_exptl_absorpt_correction_type    Empirical
_exptl_absorpt_correction_T_min   0.774311 
_exptl_absorpt_correction_T_max   1.000000 
_exptl_absorpt_process_details    ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       293(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_SMART_CCD_1K_area_detector 
_diffrn_measurement_method        Omega_scan 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             14020 
_diffrn_reflns_av_R_equivalents   0.0266 
_diffrn_reflns_av_sigmaI/netI     0.0243 
_diffrn_reflns_limit_h_min        -31 
_diffrn_reflns_limit_h_max        31 
_diffrn_reflns_limit_k_min        -15 
_diffrn_reflns_limit_k_max        8 
_diffrn_reflns_limit_l_min        -21 
_diffrn_reflns_limit_l_max        20 
_diffrn_reflns_theta_min          1.85 
_diffrn_reflns_theta_max          26.09 
_reflns_number_total              4656 
_reflns_number_gt                 3592 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'SMART for Windows NT, Bruker AXS, 1997.' 
_computing_cell_refinement        'SAINT-PLUS, Ver. 5.0, Bruker AXS, 1997.'   
_computing_data_reduction         'SAINT-PLUS, Ver. 5.0, Bruker AXS, 1997.'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'XP-Interactive Molecular Graphics, Ver. 5.1'
_computing_publication_material   'SHELXTL-Bruker AXS, 1998.'   
 
_refine_special_details 
; 
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F^2^, conventional R-factors R are based 
 on F, with F set to zero for negative F^2^. The threshold expression of 
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F^2^ 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/[\s^2^(Fo^2^)+(0.0938P)^2^+3.2263P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.0012(4) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' 
_refine_ls_number_reflns          4656 
_refine_ls_number_parameters      229 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0654 
_refine_ls_R_factor_gt            0.0511 
_refine_ls_wR_factor_ref          0.1636 
_refine_ls_wR_factor_gt           0.1473 
_refine_ls_goodness_of_fit_ref    1.037 
_refine_ls_restrained_S_all       1.037 
_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_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
S1 S 0.10440(3) -0.02087(6) 0.55997(5) 0.0664(2) Uani 1 1 d . . . 
C1 C 0.07229(11) 0.02804(17) 0.45161(16) 0.0469(5) Uani 1 1 d . . . 
N1 N 0.01011(10) 0.03213(17) 0.39020(14) 0.0573(5) Uani 1 1 d . . . 
H1A H -0.0051 0.0563 0.3354 0.069 Uiso 1 1 calc R . . 
H1B H -0.0150 0.0106 0.4052 0.069 Uiso 1 1 calc R . . 
N2 N 0.10775(11) 0.0623(2) 0.42385(16) 0.0668(6) Uani 1 1 d . . . 
H2A H 0.0903 0.0858 0.3683 0.080 Uiso 1 1 calc R . . 
H2B H 0.1484 0.0612 0.4612 0.080 Uiso 1 1 calc R . . 
S2 S -0.06195(5) 0.38336(6) 0.50084(6) 0.0780(3) Uani 1 1 d . . . 
C2 C -0.05783(12) 0.34874(19) 0.40976(16) 0.0512(6) Uani 1 1 d . . . 
N3 N -0.03643(11) 0.41318(17) 0.37434(15) 0.0596(6) Uani 1 1 d . . . 
H3A H -0.0348 0.3941 0.3283 0.071 Uiso 1 1 calc R . . 
H3B H -0.0241 0.4743 0.3973 0.071 Uiso 1 1 calc R . . 
N4 N -0.07619(13) 0.25559(18) 0.37192(17) 0.0684(6) Uani 1 1 d . . . 
H4B H -0.0739 0.2389 0.3259 0.082 Uiso 1 1 calc R . . 
H4C H -0.0904 0.2117 0.3934 0.082 Uiso 1 1 calc R . . 
S3 S 0.23991(3) 0.42573(8) 0.52735(7) 0.0887(3) Uani 1 1 d . . . 
C3 C 0.17008(11) 0.3830(2) 0.43310(19) 0.0583(6) Uani 1 1 d . . . 
N5 N 0.16554(11) 0.2958(2) 0.39078(16) 0.0719(7) Uani 1 1 d . . . 
H5B H 0.1296 0.2766 0.3429 0.086 Uiso 1 1 calc R . . 
H5C H 0.1985 0.2578 0.4110 0.086 Uiso 1 1 calc R . . 
N6 N 0.11785(11) 0.4370(2) 0.3986(2) 0.0796(8) Uani 1 1 d . . . 
H6C H 0.0829 0.4148 0.3506 0.095 Uiso 1 1 calc R . . 
H6D H 0.1186 0.4947 0.4241 0.095 Uiso 1 1 calc R . . 
S4 S 0.0000 -0.39217(7) 0.2500 0.0600(3) Uani 1 2 d S . . 
C4 C 0.0000 -0.2620(3) 0.2500 0.0528(8) Uani 1 2 d S . . 
N7 N 0.02216(13) -0.20902(18) 0.32735(18) 0.0773(7) Uani 1 1 d . . . 
H7D H 0.0218 -0.1424 0.3261 0.093 Uiso 1 1 calc R . . 
H7E H 0.0370 -0.2411 0.3790 0.093 Uiso 1 1 calc R . . 
O1 O 0.04639(7) 0.18617(12) 0.25784(10) 0.0460(4) Uani 1 1 d . . . 
O2 O 0.0000 0.33600(17) 0.2500 0.0477(5) Uani 1 2 d S . . 
C5 C 0.0000 0.2364(2) 0.2500 0.0395(6) Uani 1 2 d S . . 
N8 N 0.31181(11) 0.19643(19) 0.24088(19) 0.0698(6) Uani 1 1 d . . . 
C6 C 0.3254(2) 0.0847(3) 0.2333(3) 0.0995(12) Uani 1 1 d . . . 
H6A H 0.3708 0.0735 0.2742 0.119 Uiso 1 1 calc R . . 
H6B H 0.3132 0.0719 0.1702 0.119 Uiso 1 1 calc R . . 
C7 C 0.2922(2) 0.0054(3) 0.2572(3) 0.1128(15) Uani 1 1 d . . . 
H7A H 0.3036 -0.0632 0.2504 0.169 Uiso 1 1 calc R . . 
H7B H 0.2472 0.0141 0.2160 0.169 Uiso 1 1 calc R . . 
H7C H 0.3049 0.0156 0.3202 0.169 Uiso 1 1 calc R . . 
C8 C 0.3255(2) 0.2240(3) 0.3335(3) 0.0946(11) Uani 1 1 d . . . 
H8A H 0.2973 0.1843 0.3432 0.114 Uiso 1 1 calc R . . 
H8B H 0.3155 0.2967 0.3326 0.114 Uiso 1 1 calc R . . 
C9 C 0.3928(2) 0.2059(4) 0.4157(3) 0.1320(18) Uani 1 1 d . . . 
H9A H 0.3966 0.2258 0.4719 0.198 Uiso 1 1 calc R . . 
H9B H 0.4213 0.2466 0.4085 0.198 Uiso 1 1 calc R . . 
H9C H 0.4032 0.1338 0.4188 0.198 Uiso 1 1 calc R . . 
C10 C 0.35149(17) 0.2587(3) 0.2166(3) 0.0933(11) Uani 1 1 d . . . 
H10A H 0.3957 0.2420 0.2615 0.112 Uiso 1 1 calc R . . 
H10B H 0.3409 0.2360 0.1562 0.112 Uiso 1 1 calc R . . 
C11 C 0.3443(2) 0.3739(3) 0.2140(3) 0.1068(13) Uani 1 1 d . . . 
H11A H 0.3705 0.4052 0.1967 0.160 Uiso 1 1 calc R . . 
H11B H 0.3570 0.3985 0.2743 0.160 Uiso 1 1 calc R . . 
H11C H 0.3008 0.3921 0.1693 0.160 Uiso 1 1 calc R . . 
C12 C 0.24159(15) 0.2196(3) 0.1694(3) 0.0878(10) Uani 1 1 d . . . 
H12A H 0.2170 0.1738 0.1820 0.105 Uiso 1 1 calc R . . 
H12B H 0.2334 0.2900 0.1796 0.105 Uiso 1 1 calc R . . 
C13 C 0.2171(2) 0.2089(5) 0.0683(3) 0.1269(17) Uani 1 1 d . . . 
H13A H 0.1728 0.2256 0.0307 0.190 Uiso 1 1 calc R . . 
H13B H 0.2232 0.1389 0.0559 0.190 Uiso 1 1 calc R . . 
H13C H 0.2398 0.2554 0.0536 0.190 Uiso 1 1 calc R . . 
 
loop_ 
 _atom_site_aniso_label 
 _atom_site_aniso_U_11 
 _atom_site_aniso_U_22 
 _atom_site_aniso_U_33 
 _atom_site_aniso_U_23 
 _atom_site_aniso_U_13 
 _atom_site_aniso_U_12 
S1 0.0570(4) 0.0755(5) 0.0571(4) 0.0257(3) 0.0260(3) 0.0024(3) 
C1 0.0522(13) 0.0387(11) 0.0486(12) 0.0049(9) 0.0274(11) 0.0027(10) 
N1 0.0505(11) 0.0664(14) 0.0522(11) 0.0154(10) 0.0270(9) 0.0009(10) 
N2 0.0518(12) 0.0859(17) 0.0639(13) 0.0257(12) 0.0330(11) 0.0071(11) 
S2 0.1306(7) 0.0627(5) 0.0858(5) -0.0161(4) 0.0883(6) -0.0124(4) 
C2 0.0655(15) 0.0486(13) 0.0499(12) 0.0011(10) 0.0388(12) 0.0055(11) 
N3 0.0856(15) 0.0538(12) 0.0581(12) -0.0043(10) 0.0517(12) -0.0030(11) 
N4 0.1092(19) 0.0556(13) 0.0706(14) -0.0109(11) 0.0688(15) -0.0116(12) 
S3 0.0426(4) 0.0904(6) 0.1012(6) -0.0379(5) 0.0205(4) -0.0070(4) 
C3 0.0434(12) 0.0644(17) 0.0622(15) 0.0013(13) 0.0264(12) -0.0008(11) 
N5 0.0496(12) 0.0735(16) 0.0678(14) -0.0141(13) 0.0175(11) 0.0002(11) 
N6 0.0471(12) 0.0789(17) 0.0898(18) -0.0108(14) 0.0242(12) 0.0066(12) 
S4 0.0885(7) 0.0408(5) 0.0546(5) 0.000 0.0423(5) 0.000 
C4 0.0551(19) 0.0436(17) 0.064(2) 0.000 0.0364(17) 0.000 
N7 0.105(2) 0.0456(12) 0.0770(16) -0.0121(12) 0.0485(15) -0.0046(13) 
O1 0.0449(8) 0.0525(9) 0.0417(8) 0.0022(7) 0.0249(7) 0.0052(7) 
O2 0.0530(12) 0.0439(12) 0.0490(12) 0.000 0.0302(10) 0.000 
C5 0.0410(15) 0.0485(17) 0.0276(12) 0.000 0.0182(11) 0.000 
N8 0.0601(13) 0.0670(15) 0.0914(17) 0.0023(13) 0.0479(13) 0.0044(11) 
C6 0.088(2) 0.078(2) 0.134(3) -0.003(2) 0.063(2) 0.0101(19) 
C7 0.098(3) 0.079(2) 0.130(4) 0.010(2) 0.044(3) -0.010(2) 
C8 0.109(3) 0.090(2) 0.086(2) 0.011(2) 0.056(2) 0.007(2) 
C9 0.104(3) 0.120(4) 0.111(3) 0.039(3) 0.023(3) 0.010(3) 
C10 0.079(2) 0.098(3) 0.120(3) 0.010(2) 0.066(2) -0.0003(19) 
C11 0.120(3) 0.087(3) 0.113(3) 0.014(2) 0.066(3) -0.014(2) 
C12 0.0647(18) 0.104(3) 0.091(2) 0.013(2) 0.0413(18) 0.0073(18) 
C13 0.093(3) 0.184(5) 0.087(3) 0.006(3) 0.040(2) -0.019(3) 
 
_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 
S1 C1 1.698(2) . ? 
C1 N2 1.315(3) . ? 
C1 N1 1.326(3) . ? 
S2 C2 1.701(2) . ? 
C2 N3 1.319(3) . ? 
C2 N4 1.323(3) . ? 
S3 C3 1.699(3) . ? 
C3 N6 1.312(3) . ? 
C3 N5 1.313(4) . ? 
S4 C4 1.679(4) . ? 
C4 N7 1.319(3) . ? 
C4 N7 1.319(3) 2 ? 
O1 C5 1.286(2) . ? 
O2 C5 1.285(4) . ? 
C5 O1 1.286(2) 2 ? 
N8 C8 1.485(4) . ? 
N8 C6 1.506(4) . ? 
N8 C10 1.523(4) . ? 
N8 C12 1.531(4) . ? 
C6 C7 1.525(6) . ? 
C8 C9 1.513(6) . ? 
C10 C11 1.495(5) . ? 
C12 C13 1.506(6) . ? 
 
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 
N2 C1 N1 116.6(2) . . ? 
N2 C1 S1 121.79(19) . . ? 
N1 C1 S1 121.59(18) . . ? 
N3 C2 N4 117.7(2) . . ? 
N3 C2 S2 121.57(19) . . ? 
N4 C2 S2 120.75(19) . . ? 
N6 C3 N5 116.8(2) . . ? 
N6 C3 S3 121.0(2) . . ? 
N5 C3 S3 122.3(2) . . ? 
N7 C4 N7 117.6(3) . 2 ? 
N7 C4 S4 121.21(17) . . ? 
N7 C4 S4 121.21(17) 2 . ? 
O2 C5 O1 120.26(14) . 2 ? 
O2 C5 O1 120.26(14) . . ? 
O1 C5 O1 119.5(3) 2 . ? 
C8 N8 C6 113.4(3) . . ? 
C8 N8 C10 112.5(3) . . ? 
C6 N8 C10 105.1(3) . . ? 
C8 N8 C12 106.9(3) . . ? 
C6 N8 C12 109.8(3) . . ? 
C10 N8 C12 109.1(3) . . ? 
N8 C6 C7 115.3(3) . . ? 
N8 C8 C9 116.1(4) . . ? 
C11 C10 N8 116.4(3) . . ? 
C13 C12 N8 117.4(3) . . ? 
 
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 
C8 N8 C6 C7 55.1(5) . . . . ? 
C10 N8 C6 C7 178.4(4) . . . . ? 
C12 N8 C6 C7 -64.4(4) . . . . ? 
C6 N8 C8 C9 58.1(4) . . . . ? 
C10 N8 C8 C9 -60.9(4) . . . . ? 
C12 N8 C8 C9 179.3(3) . . . . ? 
C8 N8 C10 C11 -59.2(4) . . . . ? 
C6 N8 C10 C11 177.0(4) . . . . ? 
C12 N8 C10 C11 59.3(4) . . . . ? 
C8 N8 C12 C13 173.6(4) . . . . ? 
C6 N8 C12 C13 -62.9(5) . . . . ? 
C10 N8 C12 C13 51.7(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 O1  0.86 2.15 2.913(3) 147.4 2 
N4 H4B O1  0.86 2.05 2.892(3) 165.5 2 
N2 H2A O1  0.86 2.05 2.874(3) 160.1 . 
N2 H2B S3  0.86 2.74 3.480(2) 144.5 7_556 
N5 H5C S3  0.86 2.71 3.486(3) 151.2 7_556 
N3 H3A O2  0.86 2.13 2.958(2) 161.4 . 
N3 H3B S2  0.86 2.64 3.433(2) 154.1 5_566 
N6 H6D S2  0.86 2.89 3.636(3) 146.1 5_566 
N5 H5B O1  0.86 2.13 2.949(3) 159.6 . 
N4 H4C S1  0.86 2.68 3.469(2) 153.5 5_556 
N7 H7E S2  0.86 2.58 3.405(3) 162.3 5_556 
N1 H1B S1  0.86 2.67 3.477(2) 157.9 5_556 
N6 H6C O2  0.86 2.10 2.949(3) 168.8 . 
N7 H7D N1  0.86 2.60 3.367(3) 149.0 . 
 
_diffrn_measured_fraction_theta_max    0.993 
_diffrn_reflns_theta_full              26.09 
_diffrn_measured_fraction_theta_full   0.993 
_refine_diff_density_max    0.573 
_refine_diff_density_min   -0.258 
_refine_diff_density_rms    0.058 

#===END
 
data_Compound(2)
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 bis(tetra-n-propylammonium) oxalate-thiourea (1/4)
; 
_chemical_name_common         ?    
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C30 H72 N10 O4 S4' 
_chemical_formula_weight          765.22 
 
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                    11.8476(7) 
_cell_length_b                    12.0889(7) 
_cell_length_c                    16.3965(10) 
_cell_angle_alpha                 74.4270(10) 
_cell_angle_beta                  87.5210(10) 
_cell_angle_gamma                 89.893(2) 
_cell_volume                      2259.9(2) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        block 
_exptl_crystal_colour             colorless 
_exptl_crystal_size_max           0.70 
_exptl_crystal_size_mid           0.52 
_exptl_crystal_size_min           0.43 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.125 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              836 
_exptl_absorpt_coefficient_mu     0.252 
_exptl_absorpt_correction_type    Empirical
_exptl_absorpt_correction_T_min   0.751004 
_exptl_absorpt_correction_T_max   1.000000 
_exptl_absorpt_process_details    ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       293(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_SMART_CCD_1K_area_detector 
_diffrn_measurement_method        omega_scan 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             12397 
_diffrn_reflns_av_R_equivalents   0.0227 
_diffrn_reflns_av_sigmaI/netI     0.0426 
_diffrn_reflns_limit_h_min        -14 
_diffrn_reflns_limit_h_max        14 
_diffrn_reflns_limit_k_min        -12 
_diffrn_reflns_limit_k_max        14 
_diffrn_reflns_limit_l_min        -19 
_diffrn_reflns_limit_l_max        19 
_diffrn_reflns_theta_min          1.72 
_diffrn_reflns_theta_max          25.00 
_reflns_number_total              7933 
_reflns_number_gt                 4093 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'SMART for Windows NT, Bruker AXS, 1997.' 
_computing_cell_refinement        'SAINT-PLUS, Ver. 5.0, Bruker AXS, 1997.'   
_computing_data_reduction         'SAINT-PLUS, Ver. 5.0, Bruker AXS, 1997.'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'XP-Interactive Molecular Graphics, Ver. 5.1'
_computing_publication_material   'SHELXTL-Bruker AXS, 1998.'   
 
_refine_special_details 
; 
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F^2^, conventional R-factors R are based 
 on F, with F set to zero for negative F^2^. The threshold expression of 
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F^2^ 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/[\s^2^(Fo^2^)+(0.1020P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          7933 
_refine_ls_number_parameters      482 
_refine_ls_number_restraints      36 
_refine_ls_R_factor_all           0.1142 
_refine_ls_R_factor_gt            0.0599 
_refine_ls_wR_factor_ref          0.1927 
_refine_ls_wR_factor_gt           0.1674 
_refine_ls_goodness_of_fit_ref    1.028 
_refine_ls_restrained_S_all       1.032 
_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 0.6170(3) 0.4780(5) 0.2354(4) 0.0863(17) Uani 0.70 1 d PDU A 1 
C2 C 0.7400(3) 0.4458(5) 0.2109(3) 0.0747(13) Uani 0.70 1 d PDU A 1 
O1 O 0.5881(6) 0.5791(5) 0.2329(13) 0.134(3) Uani 0.60 1 d PDU A 1 
O2 O 0.5452(5) 0.4002(5) 0.2678(5) 0.105(2) Uani 0.60 1 d PDU A 1 
O3 O 0.7566(5) 0.3454(5) 0.2048(8) 0.0915(19) Uani 0.60 1 d PDU A 1 
O4 O 0.8223(5) 0.5149(7) 0.1979(9) 0.0764(18) Uani 0.60 1 d PDU A 1 
C1' C 0.6952(10) 0.5148(9) 0.2211(8) 0.137(5) Uani 0.40 1 d PDU B 2 
C2' C 0.6524(11) 0.3906(9) 0.2255(8) 0.159(6) Uani 0.40 1 d PDU B 2 
O1' O 0.7977(10) 0.5422(11) 0.2052(16) 0.098(4) Uani 0.40 1 d PDU B 2 
O2' O 0.6237(10) 0.5899(10) 0.2263(18) 0.129(5) Uani 0.40 1 d PDU B 2 
O3' O 0.5494(12) 0.3722(10) 0.2463(12) 0.153(6) Uani 0.40 1 d PDU B 2 
O4' O 0.7243(9) 0.3231(11) 0.2075(14) 0.122(4) Uani 0.40 1 d PDU B 2 
S1 S 1.14394(8) 0.20640(9) 0.32729(7) 0.0927(3) Uani 1 1 d . . . 
C3 C 1.0269(3) 0.2651(3) 0.2798(2) 0.0757(10) Uani 1 1 d . . . 
N1 N 1.0102(3) 0.3766(3) 0.2567(2) 0.0949(9) Uani 1 1 d . . . 
H1A H 1.0624 0.4251 0.2662 0.114 Uiso 1 1 d R . . 
H1B H 0.9462 0.4043 0.2314 0.095 Uiso 1 1 d R . . 
N2 N 0.9441(3) 0.2004(3) 0.26325(19) 0.0950(9) Uani 1 1 d . . . 
H2A H 0.9500 0.1234 0.2774 0.114 Uiso 1 1 d R . . 
H2B H 0.8823 0.2341 0.2377 0.114 Uiso 1 1 d R . . 
S2 S 0.15233(9) 0.59949(8) 0.28744(6) 0.0885(3) Uiso 1 1 d . . . 
C4 C 0.2889(3) 0.5626(3) 0.2828(2) 0.0748(9) Uani 1 1 d . . . 
N3 N 0.3697(3) 0.6406(3) 0.2570(2) 0.0958(10) Uani 1 1 d . . . 
H3A H 0.3516 0.7155 0.2419 0.115 Uiso 1 1 d R . . 
H3B H 0.4424 0.6196 0.2547 0.115 Uiso 1 1 d R . . 
N4 N 0.3217(3) 0.4545(3) 0.3034(2) 0.1019(10) Uani 1 1 d . . . 
H4A H 0.2698 0.3979 0.3213 0.122 Uiso 1 1 d R . . 
H4B H 0.3954 0.4372 0.3001 0.122 Uiso 1 1 d R . . 
S3 S 0.84699(9) 0.97584(9) 0.17687(8) 0.1029(4) Uani 1 1 d . . . 
C5 C 0.8119(3) 0.8346(3) 0.2057(2) 0.0793(10) Uani 1 1 d . . . 
N5 N 0.7046(3) 0.7992(3) 0.22481(19) 0.0980(9) Uani 1 1 d . . . 
H5A H 0.6492 0.8508 0.2226 0.118 Uiso 1 1 d R . . 
H5B H 0.6879 0.7236 0.2400 0.118 Uiso 1 1 d R . . 
N6 N 0.8876(3) 0.7548(3) 0.20812(17) 0.0870(8) Uani 1 1 d . . . 
H6A H 0.9607 0.7737 0.1944 0.104 Uiso 1 1 d R . . 
H6B H 0.8659 0.6805 0.2238 0.104 Uiso 1 1 d R . . 
S4 S 0.46819(9) -0.04010(10) 0.25469(7) 0.1060(4) Uani 1 1 d . . . 
C6 C 0.5150(3) 0.0939(4) 0.2476(2) 0.0929(11) Uani 1 1 d . . . 
N7 N 0.6180(3) 0.1300(3) 0.2175(2) 0.1129(11) Uani 1 1 d . . . 
H7A H 0.6659 0.0828 0.1995 0.135 Uiso 1 1 d R . . 
H7B H 0.6399 0.2022 0.2150 0.135 Uiso 1 1 d R . . 
N8 N 0.4487(3) 0.1690(3) 0.2710(2) 0.1175(12) Uani 1 1 d . . . 
H8A H 0.3774 0.1498 0.2908 0.141 Uiso 1 1 d R . . 
H8B H 0.4755 0.2400 0.2668 0.141 Uiso 1 1 d R . . 
N9 N 0.2530(2) 0.7558(2) 0.50093(15) 0.0706(7) Uani 1 1 d . . . 
C7 C 0.2764(3) 0.8407(3) 0.5521(2) 0.0844(10) Uani 1 1 d . . . 
H7C H 0.3351 0.8108 0.5903 0.101 Uiso 1 1 d R . . 
H7D H 0.2093 0.8458 0.5859 0.101 Uiso 1 1 d R . . 
C8 C 0.3088(4) 0.9602(3) 0.5007(3) 0.1010(12) Uani 1 1 d . . . 
H8C H 0.2474 0.9940 0.4665 0.121 Uiso 1 1 d R . . 
H8D H 0.3721 0.9555 0.4633 0.121 Uiso 1 1 d R . . 
C9 C 0.3398(4) 1.0348(5) 0.5576(4) 0.1415(19) Uani 1 1 d . . . 
H9A H 0.3608 1.1097 0.5224 0.212 Uiso 1 1 d R . . 
H9B H 0.2762 1.0410 0.5943 0.212 Uiso 1 1 d R . . 
H9C H 0.4023 1.0022 0.5911 0.212 Uiso 1 1 d R . . 
C10 C 0.3594(3) 0.7353(3) 0.4526(2) 0.0791(10) Uani 1 1 d . . . 
H10A H 0.3814 0.8064 0.4126 0.095 Uiso 1 1 d R . . 
H10B H 0.3417 0.6819 0.4208 0.095 Uiso 1 1 d R . . 
C11 C 0.4594(3) 0.6897(4) 0.5049(3) 0.1093(13) Uani 1 1 d . . . 
H11A H 0.4384 0.6203 0.5472 0.131 Uiso 1 1 d R . . 
H11B H 0.4834 0.7451 0.5330 0.131 Uiso 1 1 d R . . 
C12 C 0.5561(4) 0.6655(4) 0.4480(3) 0.1305(17) Uani 1 1 d . . . 
H12A H 0.6198 0.6368 0.4813 0.196 Uiso 1 1 d R . . 
H12B H 0.5320 0.6095 0.4204 0.196 Uiso 1 1 d R . . 
H12C H 0.5773 0.7353 0.4061 0.196 Uiso 1 1 d R . . 
C13 C 0.2127(3) 0.6442(3) 0.5628(2) 0.0858(10) Uani 1 1 d . . . 
H13A H 0.1470 0.6599 0.5940 0.103 Uiso 1 1 d R . . 
H13B H 0.2703 0.6171 0.6025 0.103 Uiso 1 1 d R . . 
C14 C 0.1837(4) 0.5495(3) 0.5234(2) 0.1018(12) Uani 1 1 d . . . 
H14A H 0.2486 0.5335 0.4915 0.122 Uiso 1 1 d R . . 
H14B H 0.1244 0.5749 0.4848 0.122 Uiso 1 1 d R . . 
C15 C 0.1455(4) 0.4406(4) 0.5889(3) 0.1273(16) Uani 1 1 d . . . 
H15A H 0.1277 0.3824 0.5614 0.191 Uiso 1 1 d R . . 
H15B H 0.2052 0.4143 0.6270 0.191 Uiso 1 1 d R . . 
H15C H 0.0797 0.4561 0.6202 0.191 Uiso 1 1 d R . . 
C16 C 0.1663(3) 0.8031(3) 0.43608(19) 0.0746(9) Uani 1 1 d . . . 
H16A H 0.1562 0.7494 0.4031 0.089 Uiso 1 1 d R . . 
H16B H 0.1957 0.8730 0.3983 0.089 Uiso 1 1 d R . . 
C17 C 0.0524(3) 0.8261(4) 0.4710(3) 0.1076(13) Uani 1 1 d . . . 
H17A H 0.0611 0.8784 0.5053 0.129 Uiso 1 1 d R . . 
H17B H 0.0197 0.7561 0.5064 0.129 Uiso 1 1 d R . . 
C18 C -0.0234(4) 0.8772(4) 0.4007(3) 0.1352(17) Uani 1 1 d . . . 
H18A H -0.0955 0.8921 0.4244 0.203 Uiso 1 1 d R . . 
H18B H 0.0089 0.9478 0.3659 0.203 Uiso 1 1 d R . . 
H18C H -0.0329 0.8244 0.3670 0.203 Uiso 1 1 d R . . 
N10 N 0.2419(2) 0.2318(2) 0.04383(14) 0.0682(7) Uani 1 1 d . . . 
C19 C 0.1358(3) 0.2616(3) -0.0064(2) 0.0838(10) Uani 1 1 d . . . 
H19A H 0.1188 0.2004 -0.0312 0.101 Uiso 1 1 d R . . 
H19B H 0.1518 0.3292 -0.0519 0.101 Uiso 1 1 d R . . 
C20 C 0.0313(4) 0.2855(4) 0.0436(3) 0.1118(14) Uani 1 1 d . . . 
H20A H 0.0437 0.3521 0.0635 0.134 Uiso 1 1 d R . . 
H20B H 0.0173 0.2210 0.0920 0.134 Uiso 1 1 d R . . 
C21 C -0.0697(4) 0.3038(5) -0.0113(4) 0.171(2) Uani 1 1 d . . . 
H21A H -0.1352 0.3176 0.0209 0.256 Uiso 1 1 d R . . 
H21B H -0.0557 0.3688 -0.0593 0.256 Uiso 1 1 d R . . 
H21C H -0.0824 0.2367 -0.0306 0.256 Uiso 1 1 d R . . 
C22 C 0.2744(3) 0.3264(3) 0.0827(2) 0.0755(9) Uani 1 1 d . . . 
H22A H 0.3393 0.3024 0.1159 0.091 Uiso 1 1 d R . . 
H22B H 0.2135 0.3366 0.1205 0.091 Uiso 1 1 d R . . 
C23 C 0.3008(4) 0.4412(3) 0.0197(2) 0.0955(12) Uani 1 1 d . . . 
H23A H 0.2348 0.4691 -0.0111 0.115 Uiso 1 1 d R . . 
H23B H 0.3594 0.4317 -0.0201 0.115 Uiso 1 1 d R . . 
C24 C 0.3384(4) 0.5294(4) 0.0657(3) 0.1217(15) Uani 1 1 d . . . 
H24A H 0.3550 0.6015 0.0251 0.183 Uiso 1 1 d R . . 
H24B H 0.2793 0.5394 0.1050 0.183 Uiso 1 1 d R . . 
H24C H 0.4049 0.5018 0.0960 0.183 Uiso 1 1 d R . . 
C25 C 0.3335(3) 0.2124(3) -0.0166(2) 0.0795(10) Uani 1 1 d . . . 
H25A H 0.3408 0.2801 -0.0634 0.095 Uiso 1 1 d R . . 
H25B H 0.3110 0.1504 -0.0388 0.095 Uiso 1 1 d R . . 
C26 C 0.4487(3) 0.1844(3) 0.0203(2) 0.0927(11) Uani 1 1 d . . . 
H26A H 0.4434 0.1158 0.0664 0.111 Uiso 1 1 d R . . 
H26B H 0.4732 0.2461 0.0421 0.111 Uiso 1 1 d R . . 
C27 C 0.5345(4) 0.1681(4) -0.0466(3) 0.1252(17) Uani 1 1 d . . . 
H27A H 0.6068 0.1509 -0.0221 0.188 Uiso 1 1 d R . . 
H27B H 0.5105 0.1057 -0.0678 0.188 Uiso 1 1 d R . . 
H27C H 0.5405 0.2371 -0.0923 0.188 Uiso 1 1 d R . . 
C28 C 0.2222(3) 0.1236(3) 0.11647(19) 0.0736(9) Uani 1 1 d . . . 
H28A H 0.1654 0.1398 0.1552 0.088 Uiso 1 1 d R . . 
H28B H 0.2906 0.1065 0.1464 0.088 Uiso 1 1 d R . . 
C29 C 0.1850(4) 0.0175(3) 0.0922(3) 0.0975(12) Uani 1 1 d . . . 
H29A H 0.2390 0.0015 0.0516 0.117 Uiso 1 1 d R . . 
H29B H 0.1131 0.0304 0.0664 0.117 Uiso 1 1 d R . . 
C30 C 0.1758(3) -0.0838(3) 0.1688(3) 0.1171(15) Uani 1 1 d . . . 
H30D H 0.1527 -0.1508 0.1528 0.176 Uiso 1 1 d R . . 
H30A H 0.2480 -0.0970 0.1940 0.176 Uiso 1 1 d R . . 
H30B H 0.1211 -0.0678 0.2089 0.176 Uiso 1 1 d R . . 
 
loop_ 
 _atom_site_aniso_label 
 _atom_site_aniso_U_11 
 _atom_site_aniso_U_22 
 _atom_site_aniso_U_33 
 _atom_site_aniso_U_23 
 _atom_site_aniso_U_13 
 _atom_site_aniso_U_12 
C1 0.056(3) 0.104(5) 0.078(4) 0.009(4) 0.004(3) 0.011(3) 
C2 0.060(3) 0.093(4) 0.066(3) -0.011(4) -0.012(3) 0.016(3) 
O1 0.038(5) 0.083(4) 0.255(9) -0.008(5) 0.031(6) -0.018(3) 
O2 0.095(4) 0.067(4) 0.147(5) -0.027(4) 0.032(3) 0.022(3) 
O3 0.046(4) 0.092(4) 0.131(5) -0.020(4) 0.002(4) -0.032(3) 
O4 0.075(3) 0.054(4) 0.103(4) -0.026(4) -0.006(3) 0.021(3) 
C1' 0.147(10) 0.142(9) 0.106(12) 0.004(9) -0.052(13) 0.018(7) 
C2' 0.179(11) 0.127(8) 0.157(16) 0.002(9) -0.104(13) 0.008(8) 
O1' 0.116(7) 0.066(6) 0.121(8) -0.039(6) -0.017(7) 0.053(5) 
O2' 0.044(7) 0.115(7) 0.204(11) -0.002(6) 0.022(9) -0.054(4) 
O3' 0.194(9) 0.073(6) 0.223(14) -0.098(7) 0.012(9) 0.057(5) 
O4' 0.049(6) 0.144(7) 0.150(8) 0.000(7) -0.004(6) -0.077(5) 
S1 0.0807(7) 0.0887(7) 0.1034(7) -0.0193(5) 0.0133(5) 0.0047(5) 
C3 0.088(3) 0.069(2) 0.071(2) -0.0240(17) 0.0246(19) -0.0110(19) 
N1 0.093(2) 0.080(2) 0.114(2) -0.0290(18) -0.0115(18) -0.0002(17) 
N2 0.100(2) 0.082(2) 0.101(2) -0.0224(17) 0.0062(18) -0.0107(18) 
C4 0.088(2) 0.065(2) 0.074(2) -0.0232(17) 0.0009(18) -0.0032(19) 
N3 0.090(2) 0.078(2) 0.122(3) -0.0336(18) 0.0064(19) -0.0121(17) 
N4 0.083(2) 0.078(2) 0.135(3) -0.0137(19) -0.0012(19) -0.0017(17) 
S3 0.0773(7) 0.0997(8) 0.1287(9) -0.0263(6) 0.0004(6) -0.0108(5) 
C5 0.074(2) 0.101(3) 0.061(2) -0.0192(18) -0.0065(17) -0.011(2) 
N5 0.077(2) 0.108(2) 0.100(2) -0.0107(18) -0.0095(17) -0.0114(17) 
N6 0.080(2) 0.094(2) 0.084(2) -0.0198(16) 0.0007(16) -0.0025(18) 
S4 0.0729(6) 0.1260(9) 0.1063(8) -0.0080(6) -0.0089(6) -0.0074(6) 
C6 0.068(3) 0.106(3) 0.089(3) 0.002(2) -0.015(2) -0.005(2) 
N7 0.072(2) 0.119(3) 0.134(3) -0.010(2) -0.001(2) -0.0013(19) 
N8 0.078(2) 0.126(3) 0.138(3) -0.019(2) 0.003(2) 0.011(2) 
N9 0.0712(17) 0.0847(19) 0.0509(15) -0.0103(13) 0.0035(13) 0.0041(13) 
C7 0.075(2) 0.115(3) 0.069(2) -0.035(2) -0.0036(18) 0.008(2) 
C8 0.104(3) 0.101(3) 0.102(3) -0.033(2) -0.017(2) 0.001(2) 
C9 0.116(4) 0.168(5) 0.171(5) -0.094(4) -0.029(3) -0.007(3) 
C10 0.082(2) 0.079(2) 0.067(2) -0.0078(16) 0.0174(18) 0.0073(18) 
C11 0.083(3) 0.118(3) 0.117(3) -0.015(3) 0.006(2) 0.012(2) 
C12 0.091(3) 0.124(4) 0.171(5) -0.035(3) 0.025(3) 0.027(3) 
C13 0.083(2) 0.097(3) 0.062(2) 0.0032(19) 0.0061(18) -0.001(2) 
C14 0.111(3) 0.088(3) 0.089(3) 0.006(2) 0.001(2) -0.004(2) 
C15 0.110(4) 0.116(3) 0.125(4) 0.017(3) 0.013(3) -0.020(3) 
C16 0.090(2) 0.074(2) 0.0586(19) -0.0148(16) -0.0104(18) 0.0094(18) 
C17 0.080(3) 0.141(4) 0.112(3) -0.050(3) -0.017(2) 0.025(2) 
C18 0.110(4) 0.126(4) 0.163(5) -0.021(3) -0.046(3) 0.023(3) 
N10 0.0855(19) 0.0654(16) 0.0501(14) -0.0101(12) 0.0004(13) 0.0078(13) 
C19 0.106(3) 0.082(2) 0.063(2) -0.0163(17) -0.019(2) 0.010(2) 
C20 0.096(3) 0.138(4) 0.100(3) -0.027(3) -0.018(3) 0.032(3) 
C21 0.114(4) 0.230(7) 0.170(5) -0.050(5) -0.051(4) 0.062(4) 
C22 0.094(2) 0.071(2) 0.065(2) -0.0233(17) -0.0055(18) 0.0076(18) 
C23 0.128(3) 0.070(2) 0.090(3) -0.022(2) -0.009(2) 0.005(2) 
C24 0.147(4) 0.094(3) 0.132(4) -0.043(3) -0.030(3) 0.001(3) 
C25 0.111(3) 0.069(2) 0.0561(19) -0.0156(15) 0.0186(19) -0.0005(19) 
C26 0.092(3) 0.090(3) 0.093(3) -0.024(2) 0.024(2) 0.002(2) 
C27 0.125(4) 0.109(3) 0.142(4) -0.043(3) 0.055(3) -0.003(3) 
C28 0.079(2) 0.073(2) 0.0585(19) -0.0022(16) 0.0030(16) 0.0074(17) 
C29 0.104(3) 0.076(3) 0.100(3) -0.005(2) 0.006(2) -0.005(2) 
C30 0.084(3) 0.092(3) 0.150(4) 0.013(3) -0.013(3) -0.015(2) 
 
_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 O1 1.259(2) . ? 
C1 O2 1.260(2) . ? 
C1 C2 1.571(2) . ? 
C2 O3 1.259(2) . ? 
C2 O4 1.259(2) . ? 
C1' O2' 1.257(2) . ? 
C1' O1' 1.258(2) . ? 
C1' C2' 1.568(2) . ? 
C2' O4' 1.258(2) . ? 
C2' O3' 1.258(2) . ? 
S1 C3 1.681(4) . ? 
C3 N1 1.315(4) . ? 
C3 N2 1.337(4) . ? 
S2 C4 1.681(4) . ? 
C4 N3 1.319(4) . ? 
C4 N4 1.321(4) . ? 
S3 C5 1.692(4) . ? 
C5 N6 1.310(4) . ? 
C5 N5 1.339(4) . ? 
S4 C6 1.686(4) . ? 
C6 N8 1.321(5) . ? 
C6 N7 1.326(4) . ? 
N9 C16 1.510(4) . ? 
N9 C10 1.515(4) . ? 
N9 C13 1.518(4) . ? 
N9 C7 1.523(4) . ? 
C7 C8 1.505(5) . ? 
C8 C9 1.517(6) . ? 
C10 C11 1.507(5) . ? 
C11 C12 1.523(5) . ? 
C13 C14 1.504(5) . ? 
C14 C15 1.515(5) . ? 
C16 C17 1.498(5) . ? 
C17 C18 1.491(6) . ? 
N10 C25 1.499(4) . ? 
N10 C22 1.508(4) . ? 
N10 C19 1.521(4) . ? 
N10 C28 1.525(4) . ? 
C19 C20 1.525(5) . ? 
C20 C21 1.508(6) . ? 
C22 C23 1.515(5) . ? 
C23 C24 1.538(5) . ? 
C25 C26 1.518(5) . ? 
C26 C27 1.515(5) . ? 
C28 C29 1.513(5) . ? 
C29 C30 1.501(5) . ? 
 
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 O2 116.3(6) . . ? 
O1 C1 C2 123.1(5) . . ? 
O2 C1 C2 120.2(5) . . ? 
O3 C2 O4 118.7(5) . . ? 
O3 C2 C1 118.0(5) . . ? 
O4 C2 C1 123.3(5) . . ? 
O2' C1' O1' 120.1(11) . . ? 
O2' C1' C2' 118.7(12) . . ? 
O1' C1' C2' 120.9(13) . . ? 
O4' C2' O3' 128.6(10) . . ? 
O4' C2' C1' 116.6(12) . . ? 
O3' C2' C1' 114.8(12) . . ? 
N1 C3 N2 115.6(4) . . ? 
N1 C3 S1 122.8(3) . . ? 
N2 C3 S1 121.6(3) . . ? 
N3 C4 N4 116.0(3) . . ? 
N3 C4 S2 121.6(3) . . ? 
N4 C4 S2 122.4(3) . . ? 
N6 C5 N5 116.7(3) . . ? 
N6 C5 S3 121.8(3) . . ? 
N5 C5 S3 121.5(3) . . ? 
N8 C6 N7 116.7(4) . . ? 
N8 C6 S4 120.9(3) . . ? 
N7 C6 S4 122.5(4) . . ? 
C16 N9 C10 106.9(2) . . ? 
C16 N9 C13 111.4(3) . . ? 
C10 N9 C13 109.9(2) . . ? 
C16 N9 C7 110.6(2) . . ? 
C10 N9 C7 110.5(3) . . ? 
C13 N9 C7 107.6(2) . . ? 
C8 C7 N9 115.3(3) . . ? 
C7 C8 C9 111.0(4) . . ? 
C11 C10 N9 116.4(3) . . ? 
C10 C11 C12 110.0(4) . . ? 
C14 C13 N9 115.3(3) . . ? 
C13 C14 C15 112.4(4) . . ? 
C17 C16 N9 115.6(3) . . ? 
C18 C17 C16 110.3(4) . . ? 
C25 N10 C22 111.0(3) . . ? 
C25 N10 C19 106.8(2) . . ? 
C22 N10 C19 111.5(2) . . ? 
C25 N10 C28 110.2(2) . . ? 
C22 N10 C28 107.0(2) . . ? 
C19 N10 C28 110.4(2) . . ? 
N10 C19 C20 115.5(3) . . ? 
C21 C20 C19 110.1(4) . . ? 
N10 C22 C23 114.9(3) . . ? 
C22 C23 C24 110.5(3) . . ? 
N10 C25 C26 115.5(3) . . ? 
C27 C26 C25 110.8(4) . . ? 
C29 C28 N10 116.2(3) . . ? 
C30 C29 C28 110.5(4) . . ? 
 
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 
O1 C1 C2 O3 -170.8(13) . . . . ? 
O2 C1 C2 O3 17.0(11) . . . . ? 
O1 C1 C2 O4 9.8(15) . . . . ? 
O2 C1 C2 O4 -162.4(10) . . . . ? 
O2' C1' C2' O4' 170(2) . . . . ? 
O1' C1' C2' O4' -4(2) . . . . ? 
O2' C1' C2' O3' -10(2) . . . . ? 
O1' C1' C2' O3' 176.4(19) . . . . ? 
C16 N9 C7 C8 -53.5(4) . . . . ? 
C10 N9 C7 C8 64.6(4) . . . . ? 
C13 N9 C7 C8 -175.4(3) . . . . ? 
N9 C7 C8 C9 -175.1(3) . . . . ? 
C16 N9 C10 C11 178.9(3) . . . . ? 
C13 N9 C10 C11 -60.0(4) . . . . ? 
C7 N9 C10 C11 58.5(4) . . . . ? 
N9 C10 C11 C12 175.9(3) . . . . ? 
C16 N9 C13 C14 57.9(4) . . . . ? 
C10 N9 C13 C14 -60.4(4) . . . . ? 
C7 N9 C13 C14 179.2(3) . . . . ? 
N9 C13 C14 C15 179.3(3) . . . . ? 
C10 N9 C16 C17 178.1(3) . . . . ? 
C13 N9 C16 C17 58.0(4) . . . . ? 
C7 N9 C16 C17 -61.5(4) . . . . ? 
N9 C16 C17 C18 177.4(3) . . . . ? 
C25 N10 C19 C20 -179.7(3) . . . . ? 
C22 N10 C19 C20 -58.3(4) . . . . ? 
C28 N10 C19 C20 60.4(4) . . . . ? 
N10 C19 C20 C21 -175.2(4) . . . . ? 
C25 N10 C22 C23 58.1(4) . . . . ? 
C19 N10 C22 C23 -60.9(4) . . . . ? 
C28 N10 C22 C23 178.4(3) . . . . ? 
N10 C22 C23 C24 -177.2(3) . . . . ? 
C22 N10 C25 C26 56.8(3) . . . . ? 
C19 N10 C25 C26 178.5(3) . . . . ? 
C28 N10 C25 C26 -61.6(4) . . . . ? 
N10 C25 C26 C27 -179.3(3) . . . . ? 
C25 N10 C28 C29 -60.9(4) . . . . ? 
C22 N10 C28 C29 178.3(3) . . . . ? 
C19 N10 C28 C29 56.9(4) . . . . ? 
N10 C28 C29 C30 176.4(3) . . . . ? 
 
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 
N8 H8A S1  0.90 2.92 3.745(4) 152.5 1_455 
N4 H4A S1  0.90 2.73 3.592(3) 160.1 1_455 
N1 H1A S2  0.90 2.48 3.342(3) 161.4 1_655 
N5 H5A S4  0.90 2.62 3.497(4) 164.1 1_565 
N7 H7A S3  0.90 2.57 3.431(4) 161.0 1_545 
N1 H1B O4  0.90 1.98 2.826(10) 156.4 . 
N1 H1B O1'  0.90 2.39 3.211(15) 151.2 . 
N1 H1B O3  0.90 2.45 3.208(8) 142.1 . 
N2 H2B O3  0.90 2.00 2.862(9) 160.5 . 
N2 H2B O4'  0.90 2.17 3.047(15) 165.4 . 
N3 H3B O2'  0.90 2.23 3.116(12) 169.8 . 
N3 H3B O1  0.90 1.84 2.733(7) 171.4 . 
N4 H4B O2  0.90 1.92 2.802(6) 167.2 . 
N4 H4B O3'  0.90 2.23 3.068(12) 155.8 . 
N5 H5B O2'  0.90 1.86 2.701(13) 154.8 . 
N5 H5B O1  0.90 2.14 2.968(8) 152.0 . 
N5 H5B O1'  0.90 2.73 3.387(11) 131.2 . 
N6 H6B O1'  0.90 1.96 2.797(12) 154.1 . 
N6 H6B O4  0.90 2.22 3.053(7) 153.4 . 
N7 H7B O4'  0.90 1.75 2.617(10) 161.8 . 
N7 H7B O3  0.90 2.18 3.035(7) 157.4 . 
N7 H7B O3'  0.90 2.48 3.187(9) 135.7 . 
N8 H8B O3'  0.90 1.77 2.656(12) 168.9 . 
N8 H8B O2  0.90 2.11 3.007(7) 174.8 . 
 
_diffrn_measured_fraction_theta_max    0.997 
_diffrn_reflns_theta_full              25.00 
_diffrn_measured_fraction_theta_full   0.997 
_refine_diff_density_max    0.624 
_refine_diff_density_min   -0.529 
_refine_diff_density_rms    0.037 

#===END