data_pn137 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C88 H160 N32 O16' _chemical_formula_weight 1922.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P4(1)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z+3/4' '-x, -y, z+1/2' '-x+1/2, y+1/2, -z+1/4' 'y, x, -z' 'y+1/2, -x+1/2, z+3/4' '-y+1/2, x+1/2, z+1/4' '-y, -x, -z+1/2' _cell_length_a 11.949 _cell_length_b 11.949 _cell_length_c 18.656 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2663.8 _cell_formula_units_Z 1 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.198 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 0.691 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator 'osmic mirrors' _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31576 _diffrn_reflns_av_R_equivalents 0.0625 _diffrn_reflns_av_sigmaI/netI 0.0456 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 4.39 _diffrn_reflns_theta_max 72.51 _reflns_number_total 2589 _reflns_number_gt 1858 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXD (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1107P)^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 SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.3(3) _chemical_absolute_configuration ad _refine_ls_number_reflns 2589 _refine_ls_number_parameters 165 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0909 _refine_ls_R_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.1695 _refine_ls_wR_factor_gt 0.1368 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 O1 O 0.59648(13) 0.97678(13) 0.93433(9) 0.0389(5) Uani 1 1 d . . . O2 O 0.55584(14) 1.06491(12) 0.82828(9) 0.0381(5) Uani 1 1 d . . . N1 N 0.53702(15) 0.88167(15) 0.83559(11) 0.0339(5) Uani 1 1 d . . . H1 H 0.5283(3) 0.88502(18) 0.7867(15) 0.041 Uiso 1 1 calc R . . C100 C 0.51922(19) 0.77602(17) 0.87193(14) 0.0332(5) Uani 1 1 d . . . H100 H 0.5838(17) 0.7620(4) 0.9038(8) 0.040 Uiso 1 1 calc R . . C102 C 0.5758(2) 1.17881(18) 0.85453(14) 0.0364(5) Uani 1 1 d . . . C101 C 0.56595(18) 0.97517(19) 0.87147(13) 0.0337(5) Uani 1 1 d . . . N3 N 0.30181(18) 0.9118(2) 0.86273(14) 0.0512(6) Uani 1 1 d . . . N2 N 0.31438(18) 0.8108(2) 0.87348(14) 0.0548(7) Uani 1 1 d . . . N4 N 0.2799(2) 1.0024(3) 0.84939(16) 0.0680(9) Uani 1 1 d . . . C4 C 0.4135(2) 0.77982(19) 0.91769(15) 0.0426(6) Uani 1 1 d . . . H4 H 0.4230(3) 0.8344(15) 0.9545(11) 0.051 Uiso 1 1 calc R . . C5 C 0.4998(2) 1.2064(2) 0.91698(14) 0.0421(6) Uani 1 1 d . . . H5A H 0.5245 1.1666 0.9588 0.063 Uiso 1 1 calc R . . H5B H 0.4245 1.1845 0.9056 0.063 Uiso 1 1 calc R . . H5C H 0.5021 1.2854 0.9261 0.063 Uiso 1 1 calc R . . C6 C 0.69812(19) 1.1935(2) 0.87256(16) 0.0501(7) Uani 1 1 d . . . H6A H 0.7430 1.1699 0.8326 0.075 Uiso 1 1 calc R . . H6B H 0.7163 1.1490 0.9138 0.075 Uiso 1 1 calc R . . H6C H 0.7129 1.2709 0.8827 0.075 Uiso 1 1 calc R . . C7 C 0.5435(3) 1.2484(2) 0.78979(15) 0.0571(8) Uani 1 1 d . . . H7A H 0.4660 1.2364 0.7788 0.086 Uiso 1 1 calc R . . H7B H 0.5885 1.2268 0.7495 0.086 Uiso 1 1 calc R . . H7C H 0.5556 1.3262 0.8001 0.086 Uiso 1 1 calc R . . C8 C 0.5134(2) 0.68225(19) 0.81710(14) 0.0415(6) Uani 1 1 d . . . H8A H 0.4564(10) 0.6987(3) 0.7829(6) 0.050 Uiso 1 1 calc R . . H8B H 0.5830(12) 0.6776(2) 0.7922(5) 0.050 Uiso 1 1 calc R . . C9 C 0.4884(2) 0.5702(2) 0.85254(17) 0.0522(8) Uani 1 1 d . . . H9A H 0.4815(3) 0.5126(13) 0.8157(8) 0.063 Uiso 1 1 calc R . . H9B H 0.5507(14) 0.5497(5) 0.8838(7) 0.063 Uiso 1 1 calc R . . C10 C 0.3819(3) 0.5748(2) 0.89589(17) 0.0610(9) Uani 1 1 d . . . H10A H 0.3703(4) 0.5052(15) 0.9188(5) 0.073 Uiso 1 1 calc R . . H10B H 0.3205(13) 0.5882(3) 0.8650(6) 0.073 Uiso 1 1 calc R . . C11 C 0.3882(3) 0.6675(2) 0.95217(17) 0.0616(9) Uani 1 1 d . . . H11A H 0.3139(16) 0.6721(3) 0.9789(6) 0.074 Uiso 1 1 calc R . . H11B H 0.4492(13) 0.6488(4) 0.9884(8) 0.074 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 O1 0.0440(9) 0.0401(8) 0.0326(10) -0.0024(7) -0.0048(7) -0.0024(7) O2 0.0530(10) 0.0274(8) 0.0340(9) 0.0022(7) 0.0003(8) -0.0058(6) N1 0.0433(10) 0.0302(9) 0.0281(11) -0.0011(8) 0.0021(7) -0.0069(8) C100 0.0386(11) 0.0235(10) 0.0375(14) 0.0043(9) -0.0030(10) -0.0001(8) C102 0.0460(13) 0.0254(10) 0.0378(13) -0.0041(9) 0.0045(10) -0.0059(9) C101 0.0328(10) 0.0311(11) 0.0373(13) -0.0019(9) 0.0022(10) -0.0024(7) N3 0.0398(11) 0.0571(14) 0.0569(16) -0.0082(12) -0.0040(10) 0.0039(10) N2 0.0408(11) 0.0444(12) 0.0791(19) -0.0018(13) 0.0026(13) -0.0046(10) N4 0.0628(16) 0.0647(16) 0.077(2) 0.0012(15) -0.0156(14) 0.0219(14) C4 0.0467(13) 0.0353(12) 0.0458(15) 0.0022(10) 0.0023(12) -0.0043(10) C5 0.0405(12) 0.0408(12) 0.0448(15) -0.0029(10) -0.0035(12) 0.0044(10) C6 0.0377(12) 0.0394(13) 0.073(2) -0.0091(13) 0.0094(13) -0.0065(10) C7 0.091(2) 0.0320(12) 0.0485(16) 0.0021(12) 0.0092(15) -0.0016(13) C8 0.0510(14) 0.0339(13) 0.0396(13) -0.0059(10) -0.0010(11) -0.0005(9) C9 0.0659(18) 0.0303(12) 0.0605(19) 0.0002(12) -0.0116(14) -0.0049(11) C10 0.072(2) 0.0403(15) 0.070(2) 0.0084(15) -0.0068(16) -0.0233(14) C11 0.082(2) 0.0478(16) 0.0550(18) 0.0061(14) 0.0135(17) -0.0180(15) _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 C101 1.228(3) . ? O2 C101 1.347(3) . ? O2 C102 1.466(3) . ? N1 C101 1.348(3) . ? N1 C100 1.449(3) . ? C100 C8 1.519(3) . ? C100 C4 1.526(3) . ? C102 C6 1.510(3) . ? C102 C5 1.514(3) . ? C102 C7 1.516(4) . ? N3 N4 1.141(3) . ? N3 N2 1.233(3) . ? N2 C4 1.490(3) . ? C4 C11 1.519(3) . ? C8 C9 1.523(3) . ? C9 C10 1.509(4) . ? C10 C11 1.528(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 C101 O2 C102 121.65(19) . . ? C101 N1 C100 121.8(2) . . ? N1 C100 C8 109.54(19) . . ? N1 C100 C4 110.95(18) . . ? C8 C100 C4 111.16(19) . . ? O2 C102 C6 109.85(19) . . ? O2 C102 C5 111.19(19) . . ? C6 C102 C5 112.6(2) . . ? O2 C102 C7 101.6(2) . . ? C6 C102 C7 111.1(2) . . ? C5 C102 C7 109.9(2) . . ? O1 C101 O2 125.8(2) . . ? O1 C101 N1 124.3(2) . . ? O2 C101 N1 109.9(2) . . ? N4 N3 N2 172.8(3) . . ? N3 N2 C4 115.5(2) . . ? N2 C4 C11 107.2(2) . . ? N2 C4 C100 110.9(2) . . ? C11 C4 C100 112.0(2) . . ? C9 C8 C100 111.4(2) . . ? C10 C9 C8 111.5(2) . . ? C9 C10 C11 110.7(2) . . ? C4 C11 C10 111.0(2) . . ? 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 C101 N1 C100 C8 -167.5(2) . . . . ? C101 N1 C100 C4 69.4(3) . . . . ? C101 O2 C102 C6 67.5(3) . . . . ? C101 O2 C102 C5 -57.8(3) . . . . ? C101 O2 C102 C7 -174.7(2) . . . . ? C102 O2 C101 O1 -3.3(3) . . . . ? C102 O2 C101 N1 176.48(18) . . . . ? C100 N1 C101 O1 11.8(4) . . . . ? C100 N1 C101 O2 -167.98(18) . . . . ? N4 N3 N2 C4 -175(3) . . . . ? N3 N2 C4 C11 155.2(3) . . . . ? N3 N2 C4 C100 -82.2(3) . . . . ? N1 C100 C4 N2 56.2(2) . . . . ? C8 C100 C4 N2 -66.0(3) . . . . ? N1 C100 C4 C11 175.9(2) . . . . ? C8 C100 C4 C11 53.7(3) . . . . ? N1 C100 C8 C9 -176.9(2) . . . . ? C4 C100 C8 C9 -53.9(3) . . . . ? C100 C8 C9 C10 56.1(3) . . . . ? C8 C9 C10 C11 -56.7(3) . . . . ? N2 C4 C11 C10 67.2(3) . . . . ? C100 C4 C11 C10 -54.7(3) . . . . ? C9 C10 C11 C4 55.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 72.51 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.364 _refine_diff_density_min -0.412 _refine_diff_density_rms 0.101