# Copyright The Royal Society of Chemistry, 1999
# CCDC Number: 207/325 
data_13 
 
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C26 H38 N4 O6' 
_chemical_formula_weight          502.60 
_chemical_melting_point           ? 
_chemical_compound_source         ? 
 
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' 
 
_symmetry_cell_setting            ? 
_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                    8.2588(2) 
_cell_length_b                    13.68780(10) 
_cell_length_c                    24.1712(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  96.5500(10) 
_cell_angle_gamma                 90.00 
_cell_volume                      2714.59(8) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     150(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.33 
_exptl_crystal_size_mid           0.3 
_exptl_crystal_size_min           0.3 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.230 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              1080 
_exptl_absorpt_coefficient_mu     0.088 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       150(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        ? 
_diffrn_measurement_method        ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             27214 
_diffrn_reflns_av_R_equivalents   0.0600 
_diffrn_reflns_av_sigmaI/netI     0.0809 
_diffrn_reflns_limit_h_min        -11 
_diffrn_reflns_limit_h_max        11 
_diffrn_reflns_limit_k_min        -19 
_diffrn_reflns_limit_k_max        17 
_diffrn_reflns_limit_l_min        -34 
_diffrn_reflns_limit_l_max        34 
_diffrn_reflns_theta_min          1.71 
_diffrn_reflns_theta_max          30.50 
_reflns_number_total              13177 
_reflns_number_observed           6055 
_reflns_observed_criterion        >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_refine_special_details 
; 
 Refinement on F^2^ for ALL reflections except for 6551 with very negative F^2^ 
 or flagged by the user for potential systematic errors.  Weighted R-factors 
 wR and all goodnesses 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 observed criterion 
 of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+6.0000P] 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     ? 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.15(183) 
_refine_ls_number_reflns          6626 
_refine_ls_number_parameters      649 
_refine_ls_number_restraints      1 
_refine_ls_R_factor_all           0.1310 
_refine_ls_R_factor_obs           0.0802 
_refine_ls_wR_factor_all          0.2912 
_refine_ls_wR_factor_obs          0.2187 
_refine_ls_goodness_of_fit_all    1.151 
_refine_ls_goodness_of_fit_obs    1.163 
_refine_ls_restrained_S_all       1.188 
_refine_ls_restrained_S_obs       1.163 
_refine_ls_shift/esd_max          0.908 
_refine_ls_shift/esd_mean         0.057 
 
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_thermal_displace_type 
 _atom_site_occupancy 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_group 
O1 O 0.0147(6) 0.2687(5) 0.5243(2) 0.0474(14) Uani 1 d . . 
O2 O 0.5480(6) 0.1596(4) 0.5834(2) 0.0439(13) Uani 1 d . . 
O3 O 0.0202(6) 0.3452(5) 0.6413(2) 0.0504(15) Uani 1 d . . 
O4 O 0.0229(7) 0.1199(5) 0.4853(2) 0.053(2) Uani 1 d . . 
O22 O 0.2320(6) 0.1181(4) 0.3983(2) 0.0451(13) Uani 1 d . . 
O23 O 0.4011(6) 0.4685(4) 0.4940(2) 0.0416(13) Uani 1 d . . 
N1 N 0.3841(7) 0.2927(5) 0.5726(2) 0.041(2) Uani 1 d . . 
N2 N 0.1709(7) 0.2036(5) 0.6443(2) 0.042(2) Uani 1 d . . 
N21 N 0.1693(7) 0.2505(5) 0.4554(2) 0.0362(14) Uani 1 d . . 
N22 N 0.4576(7) 0.3410(5) 0.4372(2) 0.0355(15) Uani 1 d . . 
C1 C 0.1197(9) 0.3552(6) 0.5289(3) 0.040(2) Uani 1 d . . 
H1B H 0.0499(9) 0.4143(6) 0.5314(3) 0.049 Uiso 1 calc R . 
C2 C 0.2361(9) 0.3460(6) 0.5839(3) 0.042(2) Uani 1 d . . 
C3 C 0.4096(9) 0.2088(7) 0.5921(3) 0.040(2) Uani 1 d . . 
C4 C 0.3027(8) 0.1470(6) 0.6242(3) 0.038(2) Uani 1 d . . 
H4A H 0.2496(8) 0.0980(6) 0.5973(3) 0.045 Uiso 1 calc R . 
C5 C 0.1454(9) 0.2884(7) 0.6248(3) 0.043(2) Uani 1 d . . 
C6 C 0.2832(9) 0.4472(6) 0.6087(3) 0.045(2) Uani 1 d . . 
H6A H 0.3419(9) 0.4845(6) 0.5821(3) 0.054 Uiso 1 calc R . 
H6B H 0.1829(9) 0.4838(6) 0.6143(3) 0.054 Uiso 1 calc R . 
C7 C 0.3895(16) 0.4391(7) 0.6635(4) 0.071(3) Uani 1 d . . 
H7A H 0.4817(16) 0.3978(7) 0.6627(4) 0.085 Uiso 1 calc R . 
C8 C 0.3784(36) 0.4746(16) 0.7067(7) 0.193(10) Uani 1 d . . 
H8A H 0.2898(36) 0.5170(16) 0.7113(7) 0.231 Uiso 1 calc R . 
H8B H 0.4579(36) 0.4613(16) 0.7374(7) 0.231 Uiso 1 calc R . 
C9 C 0.6594(10) 0.2083(7) 0.5503(3) 0.052(2) Uani 1 d . . 
H9A H 0.7534(10) 0.1660(7) 0.5469(3) 0.078 Uiso 1 calc R . 
H9B H 0.6965(10) 0.2697(7) 0.5684(3) 0.078 Uiso 1 calc R . 
H9C H 0.6035(10) 0.2223(7) 0.5131(3) 0.078 Uiso 1 calc R . 
C10 C 0.3943(9) 0.0889(7) 0.6718(3) 0.045(2) Uani 1 d . . 
H10A H 0.4807(9) 0.0498(7) 0.6562(3) 0.053 Uiso 1 calc R . 
C11 C 0.2780(9) 0.0174(7) 0.6962(3) 0.046(2) Uani 1 d . . 
H11A H 0.2260(9) -0.0246(7) 0.6665(3) 0.069 Uiso 1 calc R . 
H11B H 0.1943(9) 0.0541(7) 0.7130(3) 0.069 Uiso 1 calc R . 
H11C H 0.3396(9) -0.0231(7) 0.7247(3) 0.069 Uiso 1 calc R . 
C12 C 0.4768(10) 0.1560(8) 0.7160(3) 0.054(2) Uani 1 d . . 
H12A H 0.5348(10) 0.1169(8) 0.7460(3) 0.080 Uiso 1 calc R . 
H12B H 0.3947(10) 0.1965(8) 0.7312(3) 0.080 Uiso 1 calc R . 
H12C H 0.5545(10) 0.1980(8) 0.6995(3) 0.080 Uiso 1 calc R . 
C13 C -0.0780(10) 0.2951(8) 0.6803(3) 0.057(2) Uani 1 d . . 
H13A H -0.1644(10) 0.3389(8) 0.6899(3) 0.085 Uiso 1 calc R . 
H13B H -0.0078(10) 0.2771(8) 0.7142(3) 0.085 Uiso 1 calc R . 
H13C H -0.1270(10) 0.2360(8) 0.6626(3) 0.085 Uiso 1 calc R . 
C14 C 0.0670(9) 0.2021(8) 0.4881(3) 0.047(2) Uani 1 d . . 
C22 C 0.1857(9) 0.3547(6) 0.4703(3) 0.036(2) Uani 1 d . . 
C23 C 0.2738(8) 0.2085(6) 0.4192(3) 0.035(2) Uani 1 d . . 
C24 C 0.4047(8) 0.2548(6) 0.4087(3) 0.038(2) Uani 1 d . . 
C25 C 0.3595(8) 0.3835(6) 0.4666(3) 0.033(2) Uani 1 d . . 
C26 C 0.0693(9) 0.4206(6) 0.4311(3) 0.042(2) Uani 1 d . . 
H26A H -0.0444(9) 0.3995(6) 0.4331(3) 0.050 Uiso 1 calc R . 
H26B H 0.0795(9) 0.4889(6) 0.4446(3) 0.050 Uiso 1 calc R . 
C27 C 0.1032(9) 0.4179(6) 0.3708(3) 0.042(2) Uani 1 d . . 
H27A H 0.0730(9) 0.3602(6) 0.3503(3) 0.050 Uiso 1 calc R . 
C28 C 0.1688(10) 0.4863(8) 0.3451(3) 0.053(2) Uani 1 d . . 
H28A H 0.2010(10) 0.5452(8) 0.3640(3) 0.063 Uiso 1 calc R . 
H28B H 0.1854(10) 0.4781(8) 0.3071(3) 0.063 Uiso 1 calc R . 
C29 C 0.0941(10) 0.1157(8) 0.3555(3) 0.057(2) Uani 1 d . . 
H29A H 0.0743(10) 0.0482(8) 0.3429(3) 0.085 Uiso 1 calc R . 
H29B H 0.1176(10) 0.1562(8) 0.3239(3) 0.085 Uiso 1 calc R . 
H29C H -0.0027(10) 0.1410(8) 0.3706(3) 0.085 Uiso 1 calc R . 
C30 C 0.5078(9) 0.2240(7) 0.3629(3) 0.046(2) Uani 1 d . . 
H30A H 0.4782(9) 0.1551(7) 0.3523(3) 0.056 Uiso 1 calc R . 
C31 C 0.4664(10) 0.2865(8) 0.3126(3) 0.056(2) Uani 1 d . . 
H31A H 0.5322(10) 0.2665(8) 0.2833(3) 0.084 Uiso 1 calc R . 
H31B H 0.4892(10) 0.3550(8) 0.3224(3) 0.084 Uiso 1 calc R . 
H31C H 0.3505(10) 0.2790(8) 0.2993(3) 0.084 Uiso 1 calc R . 
C32 C 0.6895(10) 0.2266(8) 0.3824(4) 0.059(2) Uani 1 d . . 
H32A H 0.7128(10) 0.1850(8) 0.4154(4) 0.088 Uiso 1 calc R . 
H32B H 0.7227(10) 0.2938(8) 0.3918(4) 0.088 Uiso 1 calc R . 
H32C H 0.7501(10) 0.2025(8) 0.3526(4) 0.088 Uiso 1 calc R . 
C33 C 0.5747(9) 0.4911(8) 0.4997(3) 0.055(2) Uani 1 d . . 
H33A H 0.5941(9) 0.5528(8) 0.5200(3) 0.082 Uiso 1 calc R . 
H33B H 0.6113(9) 0.4972(8) 0.4627(3) 0.082 Uiso 1 calc R . 
H33C H 0.6354(9) 0.4385(8) 0.5203(3) 0.082 Uiso 1 calc R . 
O41 O 0.4831(4) -0.0832(3) 0.97809(15) 0.0168(9) Uani 1 d . . 
O42 O -0.0487(4) -0.1869(3) 0.9171(2) 0.0149(8) Uani 1 d . . 
O43 O 0.4895(4) -0.0055(3) 0.8645(2) 0.0187(9) Uani 1 d . . 
O44 O 0.4698(5) -0.2314(3) 1.0173(2) 0.0261(10) Uani 1 d . . 
O62 O 0.2690(4) -0.2270(3) 1.1065(2) 0.0183(9) Uani 1 d . . 
O63 O 0.1032(4) 0.1213(3) 1.00732(15) 0.0148(8) Uani 1 d . . 
N41 N 0.1179(5) -0.0543(3) 0.9300(2) 0.0100(10) Uani 1 d . . 
N42 N 0.3270(5) -0.1413(3) 0.8550(2) 0.0127(10) Uani 1 d . . 
N61 N 0.3306(5) -0.0961(3) 1.0470(2) 0.0088(9) Uani 1 d . . 
C41 C 0.3849(6) 0.0067(4) 0.9741(2) 0.0105(11) Uani 1 d . . 
H41B H 0.4580(6) 0.0645(4) 0.9716(2) 0.013 Uiso 1 calc R . 
C42 C 0.2668(6) -0.0030(4) 0.9182(2) 0.0110(11) Uani 1 d . . 
C43 C 0.0872(5) -0.1379(4) 0.9076(2) 0.0073(10) Uani 1 d . . 
C44 C 0.1919(6) -0.1963(4) 0.8722(2) 0.0113(11) Uani 1 d . . 
H44A H 0.2404(6) -0.2508(4) 0.8962(2) 0.014 Uiso 1 calc R . 
C45 C 0.3589(6) -0.0581(4) 0.8772(2) 0.0118(12) Uani 1 d . . 
C46 C 0.2187(7) 0.0995(4) 0.8943(3) 0.0207(13) Uani 1 d . . 
H46A H 0.1462(7) 0.1317(4) 0.9187(3) 0.025 Uiso 1 calc R . 
H46B H 0.3180(7) 0.1400(4) 0.8944(3) 0.025 Uiso 1 calc R . 
C47 C 0.1334(9) 0.0940(5) 0.8361(3) 0.033(2) Uani 1 d . . 
H47A H 0.1951(9) 0.0710(5) 0.8079(3) 0.040 Uiso 1 calc R . 
C48 C -0.0149(10) 0.1175(6) 0.8212(3) 0.044(2) Uani 1 d . . 
H48A H -0.0810(10) 0.1408(6) 0.8481(3) 0.053 Uiso 1 calc R . 
H48B H -0.0591(10) 0.1117(6) 0.7833(3) 0.053 Uiso 1 calc R . 
C49 C -0.1534(6) -0.1409(4) 0.9547(2) 0.0149(12) Uani 1 d . . 
H49A H -0.2481(6) -0.1827(4) 0.9581(2) 0.022 Uiso 1 calc R . 
H49B H -0.1904(6) -0.0772(4) 0.9398(2) 0.022 Uiso 1 calc R . 
H49C H -0.0917(6) -0.1321(4) 0.9915(2) 0.022 Uiso 1 calc R . 
C50 C 0.0915(7) -0.2448(5) 0.8213(3) 0.0257(14) Uani 1 d . . 
H50A H 0.0041(7) -0.2851(5) 0.8355(3) 0.031 Uiso 1 calc R . 
C51 C 0.0085(9) -0.1675(6) 0.7823(3) 0.041(2) Uani 1 d . . 
H51A H -0.0590(9) -0.1253(6) 0.8031(3) 0.062 Uiso 1 calc R . 
H51B H -0.0603(9) -0.1996(6) 0.7519(3) 0.062 Uiso 1 calc R . 
H51C H 0.0915(9) -0.1279(6) 0.7669(3) 0.062 Uiso 1 calc R . 
C52 C 0.1970(9) -0.3130(6) 0.7908(3) 0.048(2) Uani 1 d . . 
H52A H 0.2483(9) -0.3615(6) 0.8170(3) 0.071 Uiso 1 calc R . 
H52B H 0.2815(9) -0.2750(6) 0.7752(3) 0.071 Uiso 1 calc R . 
H52C H 0.1290(9) -0.3463(6) 0.7607(3) 0.071 Uiso 1 calc R . 
C53 C 0.5940(7) -0.0524(4) 0.8294(3) 0.0227(13) Uani 1 d . . 
H53A H 0.6828(7) -0.0080(4) 0.8227(3) 0.034 Uiso 1 calc R . 
H53B H 0.5313(7) -0.0695(4) 0.7938(3) 0.034 Uiso 1 calc R . 
H53C H 0.6395(7) -0.1119(4) 0.8476(3) 0.034 Uiso 1 calc R . 
C54 C 0.4282(6) -0.1471(4) 1.0148(2) 0.0175(13) Uani 1 d . . 
C62 C 0.3171(6) 0.0069(4) 1.0316(2) 0.0127(11) Uani 1 d . . 
C63 C 0.2285(6) -0.1360(4) 1.0847(2) 0.0115(11) Uani 1 d . . 
C64 C 0.0982(6) -0.0880(4) 1.0960(2) 0.0131(11) Uani 1 d . . 
C65 C 0.1434(6) 0.0393(4) 1.0360(2) 0.0099(11) Uani 1 d . . 
C66 C 0.4362(6) 0.0739(4) 1.0712(2) 0.0163(12) Uani 1 d . . 
H66A H 0.5500(6) 0.0543(4) 1.0677(2) 0.020 Uiso 1 calc R . 
H66B H 0.4229(6) 0.1424(4) 1.0585(2) 0.020 Uiso 1 calc R . 
C67 C 0.4087(7) 0.0688(5) 1.1315(2) 0.0228(13) Uani 1 d . . 
H67A H 0.4325(7) 0.0091(5) 1.1508(2) 0.027 Uiso 1 calc R . 
C68 C 0.3533(9) 0.1423(6) 1.1592(3) 0.041(2) Uani 1 d . . 
H68A H 0.3284(9) 0.2029(6) 1.1410(3) 0.050 Uiso 1 calc R . 
H68B H 0.3383(9) 0.1347(6) 1.1973(3) 0.050 Uiso 1 calc R . 
C69 C 0.4127(7) -0.2304(5) 1.1449(3) 0.0302(15) Uani 1 d . . 
H69A H 0.4315(7) -0.2976(5) 1.1581(3) 0.045 Uiso 1 calc R . 
H69B H 0.3998(7) -0.1875(5) 1.1765(3) 0.045 Uiso 1 calc R . 
H69C H 0.5058(7) -0.2084(5) 1.1264(3) 0.045 Uiso 1 calc R . 
C70 C -0.0035(6) -0.1154(5) 1.1430(3) 0.0232(14) Uani 1 d . . 
H70A H 0.0303(6) -0.1819(5) 1.1570(3) 0.028 Uiso 1 calc R . 
C71 C 0.0324(9) -0.0420(7) 1.1907(3) 0.044(2) Uani 1 d . . 
H71A H 0.1497(9) -0.0413(7) 1.2030(3) 0.066 Uiso 1 calc R . 
H71B H -0.0269(9) -0.0611(7) 1.2219(3) 0.066 Uiso 1 calc R . 
H71C H -0.0025(9) 0.0233(7) 1.1778(3) 0.066 Uiso 1 calc R . 
C72 C -0.1835(8) -0.1177(7) 1.1225(4) 0.046(2) Uani 1 d . . 
H72A H -0.2452(8) -0.1362(7) 1.1532(4) 0.070 Uiso 1 calc R . 
H72B H -0.2034(8) -0.1655(7) 1.0923(4) 0.070 Uiso 1 calc R . 
H72C H -0.2184(8) -0.0528(7) 1.1087(4) 0.070 Uiso 1 calc R . 
C73 C -0.0694(6) 0.1451(4) 1.0004(3) 0.0227(13) Uani 1 d . . 
H73A H -0.0866(6) 0.2062(4) 0.9794(3) 0.034 Uiso 1 calc R . 
H73B H -0.1076(6) 0.1529(4) 1.0371(3) 0.034 Uiso 1 calc R . 
H73C H -0.1303(6) 0.0923(4) 0.9801(3) 0.034 Uiso 1 calc R . 
N62 N 0.0460(5) -0.0011(3) 1.0664(2) 0.0122(10) Uani 1 d . . 
 
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 
O1 0.040(3) 0.075(4) 0.026(2) -0.009(3) 0.002(2) -0.008(3) 
O2 0.034(3) 0.068(4) 0.029(2) 0.001(3) 0.003(2) 0.008(3) 
O3 0.047(3) 0.070(4) 0.036(3) 0.001(3) 0.016(2) 0.005(3) 
O4 0.053(3) 0.063(4) 0.041(3) 0.000(3) 0.001(2) -0.027(3) 
O22 0.049(3) 0.051(4) 0.032(3) 0.000(3) -0.009(2) -0.006(3) 
O23 0.043(3) 0.053(3) 0.028(2) -0.003(2) 0.000(2) -0.002(2) 
N1 0.044(4) 0.062(5) 0.016(3) -0.008(3) -0.005(2) 0.007(3) 
N2 0.043(4) 0.059(5) 0.021(3) -0.004(3) -0.002(2) 0.009(3) 
N21 0.033(3) 0.048(4) 0.027(3) 0.002(3) 0.001(2) -0.004(3) 
N22 0.034(3) 0.052(4) 0.020(3) -0.003(3) -0.002(2) -0.004(3) 
C1 0.038(4) 0.054(5) 0.030(4) -0.004(4) 0.007(3) 0.000(4) 
C2 0.043(4) 0.061(5) 0.022(3) -0.007(3) 0.001(3) 0.001(4) 
C3 0.036(4) 0.066(6) 0.015(3) -0.005(4) -0.005(3) -0.002(4) 
C4 0.038(4) 0.045(5) 0.030(4) -0.008(3) 0.003(3) 0.004(3) 
C5 0.040(4) 0.067(6) 0.022(3) -0.001(4) 0.005(3) 0.013(4) 
C6 0.046(4) 0.060(5) 0.032(4) -0.006(4) 0.011(3) 0.000(4) 
C7 0.137(9) 0.041(6) 0.031(4) -0.021(4) -0.003(5) -0.001(5) 
C8 0.364(31) 0.103(14) 0.095(11) -0.003(11) -0.046(15) -0.030(18) 
C9 0.052(5) 0.075(6) 0.029(4) 0.017(4) 0.008(3) 0.007(4) 
C10 0.038(4) 0.068(6) 0.027(4) 0.004(4) 0.002(3) 0.006(4) 
C11 0.040(4) 0.071(6) 0.026(3) 0.006(4) 0.001(3) -0.001(4) 
C12 0.052(5) 0.074(6) 0.031(4) 0.005(4) -0.014(3) -0.002(4) 
C13 0.050(5) 0.079(7) 0.046(5) 0.004(5) 0.026(4) 0.011(4) 
C14 0.035(4) 0.087(7) 0.018(3) -0.004(4) 0.002(3) -0.009(4) 
C22 0.040(4) 0.042(5) 0.024(3) 0.004(3) -0.004(3) -0.003(3) 
C23 0.030(4) 0.052(5) 0.022(3) 0.005(3) -0.001(3) -0.006(3) 
C24 0.031(4) 0.053(5) 0.027(3) 0.003(3) -0.012(3) 0.003(3) 
C25 0.039(4) 0.043(4) 0.017(3) 0.001(3) -0.004(3) -0.009(3) 
C26 0.035(4) 0.053(5) 0.035(4) 0.002(4) -0.006(3) 0.005(3) 
C27 0.046(4) 0.046(5) 0.028(4) -0.001(4) -0.013(3) 0.011(4) 
C28 0.060(5) 0.071(6) 0.025(4) 0.004(4) -0.004(3) -0.006(5) 
C29 0.050(5) 0.077(7) 0.039(4) 0.003(4) -0.014(4) -0.018(4) 
C30 0.043(4) 0.061(6) 0.036(4) -0.005(4) 0.010(3) -0.002(4) 
C31 0.041(4) 0.093(7) 0.035(4) -0.007(5) 0.008(3) 0.005(4) 
C32 0.040(4) 0.086(7) 0.049(5) 0.006(5) 0.002(4) 0.007(4) 
C33 0.048(5) 0.072(6) 0.043(4) -0.009(4) -0.006(4) -0.020(4) 
O41 0.014(2) 0.015(2) 0.021(2) 0.002(2) 0.002(2) 0.008(2) 
O42 0.008(2) 0.006(2) 0.033(2) -0.007(2) 0.010(2) -0.0074(14) 
O43 0.014(2) 0.014(2) 0.030(2) -0.005(2) 0.011(2) -0.007(2) 
O44 0.031(2) 0.014(2) 0.034(2) -0.005(2) 0.007(2) 0.011(2) 
O62 0.010(2) 0.007(2) 0.038(2) 0.006(2) 0.001(2) -0.0003(15) 
O63 0.017(2) 0.003(2) 0.025(2) 0.000(2) 0.003(2) 0.0082(15) 
N41 0.001(2) 0.012(3) 0.017(2) 0.000(2) 0.003(2) 0.003(2) 
N42 0.008(2) 0.008(3) 0.023(2) 0.004(2) 0.006(2) 0.001(2) 
N61 0.009(2) 0.000(2) 0.018(2) -0.001(2) 0.002(2) 0.003(2) 
C41 0.003(2) 0.007(3) 0.022(3) -0.001(2) -0.001(2) -0.003(2) 
C42 0.005(2) 0.011(3) 0.018(3) -0.002(2) 0.007(2) 0.001(2) 
C43 0.001(2) 0.002(3) 0.019(3) 0.002(2) 0.001(2) 0.000(2) 
C44 0.009(2) 0.007(3) 0.019(3) -0.002(2) 0.005(2) 0.003(2) 
C45 0.004(2) 0.011(3) 0.021(3) 0.004(2) 0.005(2) 0.001(2) 
C46 0.020(3) 0.003(3) 0.040(3) -0.005(3) 0.007(3) -0.002(2) 
C47 0.045(4) 0.023(4) 0.033(4) -0.002(3) 0.007(3) 0.011(3) 
C48 0.050(5) 0.039(5) 0.042(4) -0.004(4) -0.002(3) 0.001(4) 
C49 0.002(2) 0.018(3) 0.026(3) -0.009(3) 0.008(2) 0.000(2) 
C50 0.023(3) 0.027(4) 0.030(3) -0.014(3) 0.013(3) -0.007(3) 
C51 0.045(4) 0.046(5) 0.031(4) -0.006(3) -0.002(3) -0.004(4) 
C52 0.042(4) 0.050(5) 0.054(5) -0.030(4) 0.023(4) -0.022(4) 
C53 0.018(3) 0.019(3) 0.034(3) 0.003(3) 0.012(2) 0.003(2) 
C54 0.007(3) 0.014(3) 0.032(3) -0.005(3) 0.000(2) 0.009(2) 
C62 0.014(3) 0.000(3) 0.025(3) 0.000(2) 0.005(2) -0.002(2) 
C63 0.007(2) 0.000(3) 0.026(3) 0.006(2) -0.001(2) 0.000(2) 
C64 0.008(3) 0.007(3) 0.025(3) 0.004(2) 0.005(2) -0.003(2) 
C65 0.010(2) 0.001(3) 0.017(3) -0.007(2) -0.002(2) 0.000(2) 
C66 0.011(3) 0.008(3) 0.029(3) -0.001(2) -0.001(2) -0.003(2) 
C67 0.021(3) 0.016(3) 0.030(3) 0.002(3) 0.000(2) -0.002(2) 
C68 0.047(4) 0.030(4) 0.047(4) -0.008(4) 0.002(3) -0.009(3) 
C69 0.020(3) 0.027(4) 0.040(4) 0.009(3) -0.008(3) -0.001(3) 
C70 0.012(3) 0.024(3) 0.035(3) 0.018(3) 0.007(2) 0.004(2) 
C71 0.041(4) 0.058(5) 0.035(4) 0.001(4) 0.015(3) -0.006(4) 
C72 0.023(4) 0.059(5) 0.060(5) 0.014(4) 0.018(3) -0.011(3) 
C73 0.014(3) 0.014(3) 0.039(4) -0.001(3) -0.004(2) 0.009(2) 
N62 0.011(2) 0.004(2) 0.022(2) 0.002(2) 0.003(2) 0.004(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 
O1 C14 1.368(10) . ? 
O1 C1 1.464(10) . ? 
O2 C3 1.364(9) . ? 
O2 C9 1.448(9) . ? 
O3 C5 1.387(9) . ? 
O3 C13 1.481(10) . ? 
O4 C14 1.182(11) . ? 
O22 C23 1.366(9) . ? 
O22 C29 1.449(9) . ? 
O23 C25 1.363(9) . ? 
O23 C33 1.458(9) . ? 
N1 C3 1.250(10) . ? 
N1 C2 1.475(10) . ? 
N2 C5 1.261(11) . ? 
N2 C4 1.464(9) . ? 
N21 C14 1.389(10) . ? 
N21 C23 1.418(9) . ? 
N21 C22 1.473(10) . ? 
N22 C25 1.278(9) . ? 
N22 C24 1.410(10) . ? 
C1 C2 1.553(10) . ? 
C1 C22 1.574(9) . ? 
C2 C6 1.543(12) . ? 
C2 C5 1.528(11) . ? 
C3 C4 1.500(11) . ? 
C4 C10 1.528(10) . ? 
C6 C7 1.507(12) . ? 
C7 C8 1.16(2) . ? 
C10 C12 1.511(11) . ? 
C10 C11 1.535(11) . ? 
C22 C25 1.501(10) . ? 
C22 C26 1.559(10) . ? 
C23 C24 1.303(10) . ? 
C24 C30 1.530(10) . ? 
C26 C27 1.514(10) . ? 
C27 C28 1.277(12) . ? 
C30 C31 1.494(12) . ? 
C30 C32 1.521(11) . ? 
O41 C54 1.360(7) . ? 
O41 C41 1.471(6) . ? 
O42 C43 1.349(6) . ? 
O42 C49 1.467(6) . ? 
O43 C45 1.362(6) . ? 
O43 C53 1.430(7) . ? 
O44 C54 1.204(7) . ? 
O62 C63 1.380(6) . ? 
O62 C69 1.420(7) . ? 
O63 C65 1.341(6) . ? 
O63 C73 1.453(6) . ? 
N41 C43 1.279(7) . ? 
N41 C42 1.472(6) . ? 
N42 C45 1.272(7) . ? 
N42 C44 1.447(7) . ? 
N61 C54 1.374(7) . ? 
N61 C63 1.419(7) . ? 
N61 C62 1.459(7) . ? 
C41 C62 1.557(7) . ? 
C41 C42 1.579(7) . ? 
C42 C45 1.517(7) . ? 
C42 C46 1.552(8) . ? 
C43 C44 1.512(7) . ? 
C44 C50 1.554(8) . ? 
C46 C47 1.503(9) . ? 
C47 C48 1.278(11) . ? 
C50 C52 1.522(9) . ? 
C50 C51 1.526(10) . ? 
C62 C65 1.517(7) . ? 
C62 C66 1.584(7) . ? 
C63 C64 1.316(7) . ? 
C64 N62 1.429(7) . ? 
C64 C70 1.535(7) . ? 
C65 N62 1.275(7) . ? 
C66 C67 1.501(8) . ? 
C67 C68 1.320(10) . ? 
C70 C72 1.512(9) . ? 
C70 C71 1.533(10) . ? 
 
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 
C14 O1 C1 111.1(6) . . ? 
C3 O2 C9 117.1(7) . . ? 
C5 O3 C13 113.8(7) . . ? 
C23 O22 C29 115.5(6) . . ? 
C25 O23 C33 114.7(6) . . ? 
C3 N1 C2 119.5(7) . . ? 
C5 N2 C4 117.5(6) . . ? 
C14 N21 C23 127.6(7) . . ? 
C14 N21 C22 111.5(6) . . ? 
C23 N21 C22 119.9(6) . . ? 
C25 N22 C24 118.2(6) . . ? 
O1 C1 C2 107.7(6) . . ? 
O1 C1 C22 101.0(5) . . ? 
C2 C1 C22 121.7(6) . . ? 
N1 C2 C6 109.8(6) . . ? 
N1 C2 C5 110.0(7) . . ? 
C6 C2 C5 109.3(6) . . ? 
N1 C2 C1 109.1(5) . . ? 
C6 C2 C1 111.4(7) . . ? 
C5 C2 C1 107.2(6) . . ? 
N1 C3 O2 120.2(7) . . ? 
N1 C3 C4 128.9(7) . . ? 
O2 C3 C4 110.8(7) . . ? 
N2 C4 C3 112.2(7) . . ? 
N2 C4 C10 110.3(6) . . ? 
C3 C4 C10 114.4(6) . . ? 
N2 C5 O3 120.4(7) . . ? 
N2 C5 C2 130.0(7) . . ? 
O3 C5 C2 109.5(7) . . ? 
C7 C6 C2 111.9(7) . . ? 
C8 C7 C6 131.2(17) . . ? 
C12 C10 C4 111.2(7) . . ? 
C12 C10 C11 111.6(6) . . ? 
C4 C10 C11 110.2(6) . . ? 
O4 C14 O1 123.6(7) . . ? 
O4 C14 N21 128.7(8) . . ? 
O1 C14 N21 107.6(8) . . ? 
N21 C22 C25 107.6(6) . . ? 
N21 C22 C26 112.2(6) . . ? 
C25 C22 C26 109.8(6) . . ? 
N21 C22 C1 101.2(6) . . ? 
C25 C22 C1 118.9(6) . . ? 
C26 C22 C1 107.0(6) . . ? 
C24 C23 O22 123.3(7) . . ? 
C24 C23 N21 120.0(7) . . ? 
O22 C23 N21 116.7(6) . . ? 
C23 C24 N22 121.9(7) . . ? 
C23 C24 C30 123.3(7) . . ? 
N22 C24 C30 114.7(6) . . ? 
N22 C25 O23 121.2(6) . . ? 
N22 C25 C22 125.8(7) . . ? 
O23 C25 C22 112.7(6) . . ? 
C27 C26 C22 113.8(6) . . ? 
C28 C27 C26 125.8(8) . . ? 
C31 C30 C24 109.6(7) . . ? 
C31 C30 C32 111.4(7) . . ? 
C24 C30 C32 112.4(6) . . ? 
C54 O41 C41 111.0(4) . . ? 
C43 O42 C49 116.9(4) . . ? 
C45 O43 C53 116.3(4) . . ? 
C63 O62 C69 115.3(4) . . ? 
C65 O63 C73 115.4(4) . . ? 
C43 N41 C42 118.3(4) . . ? 
C45 N42 C44 118.3(4) . . ? 
C54 N61 C63 126.7(5) . . ? 
C54 N61 C62 112.2(4) . . ? 
C63 N61 C62 120.2(4) . . ? 
O41 C41 C62 101.2(4) . . ? 
O41 C41 C42 105.5(4) . . ? 
C62 C41 C42 120.9(4) . . ? 
N41 C42 C45 112.5(4) . . ? 
N41 C42 C46 108.6(4) . . ? 
C45 C42 C46 109.5(4) . . ? 
N41 C42 C41 108.8(4) . . ? 
C45 C42 C41 107.1(4) . . ? 
C46 C42 C41 110.4(4) . . ? 
N41 C43 O42 120.1(4) . . ? 
N41 C43 C44 127.9(4) . . ? 
O42 C43 C44 111.9(4) . . ? 
N42 C44 C43 113.4(4) . . ? 
N42 C44 C50 110.7(4) . . ? 
C43 C44 C50 112.8(4) . . ? 
N42 C45 O43 120.6(5) . . ? 
N42 C45 C42 128.7(5) . . ? 
O43 C45 C42 110.7(4) . . ? 
C47 C46 C42 112.0(5) . . ? 
C48 C47 C46 125.6(7) . . ? 
C52 C50 C51 111.6(6) . . ? 
C52 C50 C44 111.2(5) . . ? 
C51 C50 C44 110.8(5) . . ? 
O44 C54 O41 122.3(5) . . ? 
O44 C54 N61 129.9(6) . . ? 
O41 C54 N61 107.7(5) . . ? 
N61 C62 C65 108.1(4) . . ? 
N61 C62 C41 101.7(4) . . ? 
C65 C62 C41 120.2(4) . . ? 
N61 C62 C66 112.3(4) . . ? 
C65 C62 C66 108.3(4) . . ? 
C41 C62 C66 106.2(4) . . ? 
C64 C63 O62 122.7(5) . . ? 
C64 C63 N61 120.1(5) . . ? 
O62 C63 N61 117.2(4) . . ? 
C63 C64 N62 121.2(5) . . ? 
C63 C64 C70 124.1(5) . . ? 
N62 C64 C70 114.5(4) . . ? 
N62 C65 O63 121.7(4) . . ? 
N62 C65 C62 125.3(5) . . ? 
O63 C65 C62 112.9(4) . . ? 
C67 C66 C62 114.0(4) . . ? 
C68 C67 C66 123.9(6) . . ? 
C72 C70 C64 111.3(5) . . ? 
C72 C70 C71 111.0(6) . . ? 
C64 C70 C71 108.8(5) . . ? 
C65 N62 C64 118.4(4) . . ? 
 
_refine_diff_density_max    0.620 
_refine_diff_density_min   -0.298 
_refine_diff_density_rms    0.061