Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Jian-Fang Ma' _publ_contact_author_email jianfangma@yahoo.com.cn loop_ _publ_author_name 'Jian-Fang Ma' 'Ying-Ying Liu' 'Ji-Cheng Ma' 'Zhong-Min Su' 'Jin Yang' data_compound-1 _database_code_depnum_ccdc_archive 'CCDC 648889' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H9 Cu O7, 2(H2 O)' _chemical_formula_sum 'C4 H13 Cu O9' _chemical_formula_weight 268.68 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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)/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.067(7) _cell_length_b 14.125(14) _cell_length_c 10.167(10) _cell_angle_alpha 90.00 _cell_angle_beta 93.270(16) _cell_angle_gamma 90.00 _cell_volume 1013.2(17) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2116 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 28.3 _exptl_crystal_description Block _exptl_crystal_colour blue _exptl_crystal_size_max 0.256 _exptl_crystal_size_mid 0.179 _exptl_crystal_size_min 0.154 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.761 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 552 _exptl_absorpt_coefficient_mu 2.182 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.216 _exptl_absorpt_correction_T_max 0.275 _exptl_absorpt_process_details 'SADABS(Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 6117 _diffrn_reflns_av_R_equivalents 0.0230 _diffrn_reflns_av_sigmaI/netI 0.0284 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 28.33 _reflns_number_total 2369 _reflns_number_gt 2116 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97(Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _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^)+(0.0328P)^2^+1.3940P] 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 2369 _refine_ls_number_parameters 157 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0395 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_ref 0.0861 _refine_ls_wR_factor_gt 0.0837 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.107 _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 Cu1 Cu 0.04772(4) 0.28310(2) -0.31196(3) 0.02242(11) Uani 1 1 d . . . C1 C 0.0048(3) 0.37687(17) -0.0855(2) 0.0196(5) Uani 1 1 d . . . C2 C -0.0516(3) 0.45333(16) 0.0111(2) 0.0174(5) Uani 1 1 d . . . H2 H -0.0176 0.4314 0.1009 0.021 Uiso 1 1 calc R . . C3 C -0.2687(3) 0.46695(17) -0.0031(3) 0.0204(5) Uani 1 1 d . . . H3A H -0.3071 0.5127 0.0613 0.024 Uiso 1 1 calc R . . H3B H -0.3042 0.4915 -0.0902 0.024 Uiso 1 1 calc R . . C4 C -0.3699(3) 0.37361(18) 0.0171(3) 0.0210(5) Uani 1 1 d . . . O1 O -0.0107(3) 0.39851(13) -0.20825(17) 0.0247(4) Uani 1 1 d . . . O2 O 0.0564(3) 0.29843(14) -0.0455(2) 0.0334(5) Uani 1 1 d . . . O3 O -0.4406(3) 0.32955(15) -0.0785(2) 0.0337(5) Uani 1 1 d . . . O4 O -0.3695(3) 0.34522(14) 0.13606(19) 0.0299(4) Uani 1 1 d . . . O1W O 0.2119(4) 0.45680(18) -0.6472(3) 0.0471(6) Uani 1 1 d D . . H11 H 0.172(6) 0.505(3) -0.688(4) 0.071 Uiso 1 1 d D . . H12 H 0.131(6) 0.429(3) -0.599(4) 0.071 Uiso 1 1 d D . . O2W O 0.1170(4) 0.0448(2) -0.1317(3) 0.0498(6) Uani 1 1 d D . . H13 H 0.126(7) 0.078(3) -0.199(3) 0.075 Uiso 1 1 d D . . H14 H 0.009(4) 0.041(3) -0.107(5) 0.075 Uiso 1 1 d D . . O3W O -0.2129(3) 0.23352(18) -0.2914(2) 0.0434(6) Uani 1 1 d D . . H15 H -0.280(6) 0.279(3) -0.240(4) 0.065 Uiso 1 1 d D . . H16 H -0.281(6) 0.223(3) -0.376(3) 0.065 Uiso 1 1 d D . . O4W O -0.0596(4) 0.35293(17) -0.5212(2) 0.0414(5) Uani 1 1 d D . . H17 H -0.057(7) 0.298(2) -0.554(4) 0.062 Uiso 1 1 d D . . H18 H -0.156(5) 0.385(3) -0.539(4) 0.062 Uiso 1 1 d D . . O5W O 0.3079(4) 0.33251(19) -0.3377(3) 0.0469(6) Uani 1 1 d D . . H19 H 0.375(6) 0.299(3) -0.403(4) 0.070 Uiso 1 1 d D . . H20 H 0.384(6) 0.335(3) -0.252(3) 0.070 Uiso 1 1 d 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 Cu1 0.02368(18) 0.02153(18) 0.02216(18) -0.00500(12) 0.00221(12) 0.00213(12) C1 0.0169(11) 0.0201(12) 0.0219(12) -0.0029(9) 0.0010(9) -0.0029(9) C2 0.0177(11) 0.0175(12) 0.0174(11) 0.0006(9) 0.0030(9) -0.0006(9) C3 0.0202(11) 0.0176(12) 0.0238(12) 0.0013(9) 0.0048(9) -0.0001(9) C4 0.0164(11) 0.0203(12) 0.0270(13) 0.0001(10) 0.0053(10) 0.0002(9) O1 0.0323(10) 0.0212(9) 0.0211(9) -0.0034(7) 0.0048(7) 0.0018(8) O2 0.0476(13) 0.0217(10) 0.0302(10) -0.0012(8) -0.0038(9) 0.0096(9) O3 0.0370(11) 0.0327(11) 0.0312(11) -0.0049(9) 0.0012(9) -0.0111(9) O4 0.0391(11) 0.0244(10) 0.0267(10) 0.0034(8) 0.0064(8) -0.0082(8) O1W 0.0496(15) 0.0419(14) 0.0499(15) 0.0106(11) 0.0050(12) 0.0073(11) O2W 0.0517(15) 0.0490(15) 0.0482(15) 0.0088(12) -0.0019(13) -0.0026(13) O3W 0.0385(13) 0.0482(15) 0.0436(13) -0.0104(11) 0.0032(10) -0.0024(10) O4W 0.0499(14) 0.0378(13) 0.0357(12) 0.0017(10) -0.0029(10) 0.0077(11) O5W 0.0383(13) 0.0533(16) 0.0491(15) -0.0079(12) 0.0039(11) -0.0001(11) _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 Cu1 O4 1.986(3) 4_665 ? Cu1 O3W 1.992(3) . ? Cu1 O1 1.997(2) . ? Cu1 O5W 1.998(3) . ? Cu1 O4W 2.427(3) . ? C1 O2 1.228(3) . ? C1 O1 1.284(3) . ? C1 C2 1.528(3) . ? C2 C2 1.530(5) 3_565 ? C2 C3 1.545(4) . ? C2 H2 0.9800 . ? C3 C4 1.520(4) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 O3 1.235(3) . ? C4 O4 1.274(3) . ? O4 Cu1 1.986(2) 4_566 ? O1W H11 0.84(3) . ? O1W H12 0.87(3) . ? O2W H13 0.84(3) . ? O2W H14 0.82(3) . ? O3W H15 0.97(3) . ? O3W H16 0.98(3) . ? O4W H17 0.84(3) . ? O4W H18 0.82(3) . ? O5W H19 0.96(3) . ? O5W H20 1.00(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 O4 Cu1 O3W 89.73(11) 4_665 . ? O4 Cu1 O1 163.43(8) 4_665 . ? O3W Cu1 O1 90.66(10) . . ? O4 Cu1 O5W 89.81(11) 4_665 . ? O3W Cu1 O5W 178.49(10) . . ? O1 Cu1 O5W 90.19(10) . . ? O4 Cu1 O4W 102.71(10) 4_665 . ? O3W Cu1 O4W 89.43(11) . . ? O1 Cu1 O4W 93.86(10) . . ? O5W Cu1 O4W 89.27(11) . . ? O2 C1 O1 122.9(2) . . ? O2 C1 C2 120.6(2) . . ? O1 C1 C2 116.5(2) . . ? C1 C2 C2 111.7(2) . 3_565 ? C1 C2 C3 108.77(19) . . ? C2 C2 C3 111.0(2) 3_565 . ? C1 C2 H2 108.4 . . ? C2 C2 H2 108.4 3_565 . ? C3 C2 H2 108.4 . . ? C4 C3 C2 110.6(2) . . ? C4 C3 H3A 109.5 . . ? C2 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 108.1 . . ? O3 C4 O4 124.6(2) . . ? O3 C4 C3 120.2(2) . . ? O4 C4 C3 115.2(2) . . ? C1 O1 Cu1 108.07(17) . . ? C4 O4 Cu1 123.72(17) . 4_566 ? H11 O1W H12 116(4) . . ? H13 O2W H14 114(5) . . ? Cu1 O3W H15 108(3) . . ? Cu1 O3W H16 112(3) . . ? H15 O3W H16 110(4) . . ? Cu1 O4W H17 88(3) . . ? Cu1 O4W H18 128(3) . . ? H17 O4W H18 117(4) . . ? Cu1 O5W H19 114(3) . . ? Cu1 O5W H20 111(3) . . ? H19 O5W H20 111(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 O2 C1 C2 C2 129.0(3) . . . 3_565 ? O1 C1 C2 C2 -53.1(3) . . . 3_565 ? O2 C1 C2 C3 -108.2(3) . . . . ? O1 C1 C2 C3 69.7(3) . . . . ? C1 C2 C3 C4 55.9(3) . . . . ? C2 C2 C3 C4 179.1(2) 3_565 . . . ? C2 C3 C4 O3 -103.5(3) . . . . ? C2 C3 C4 O4 74.5(3) . . . . ? O2 C1 O1 Cu1 3.2(3) . . . . ? C2 C1 O1 Cu1 -174.66(16) . . . . ? O4 Cu1 O1 C1 -11.0(4) 4_665 . . . ? O3W Cu1 O1 C1 80.25(17) . . . . ? O5W Cu1 O1 C1 -101.00(18) . . . . ? O4W Cu1 O1 C1 169.72(16) . . . . ? O3 C4 O4 Cu1 8.4(4) . . . 4_566 ? C3 C4 O4 Cu1 -169.45(16) . . . 4_566 ? 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 O1W H12 O4W 0.87(3) 1.93(3) 2.785(4) 169(4) . _diffrn_measured_fraction_theta_max 0.937 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.562 _refine_diff_density_min -0.513 _refine_diff_density_rms 0.082 #===End data_compound-2 _database_code_depnum_ccdc_archive 'CCDC 648891' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H20 Ni2 O15' _chemical_formula_weight 473.66 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Fdd2 _symmetry_space_group_name_Hall 'F 2 -2d' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/4, y+1/4, z+1/4' 'x+1/4, -y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x+1/4, y+3/4, z+3/4' 'x+1/4, -y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' '-x+3/4, y+1/4, z+3/4' 'x+3/4, -y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+3/4, y+3/4, z+1/4' 'x+3/4, -y+3/4, z+1/4' _cell_length_a 28.016(7) _cell_length_b 28.192(13) _cell_length_c 8.097(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6395(11) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2934 _cell_measurement_theta_min 2.1 _cell_measurement_theta_max 28.7 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.968 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3904 _exptl_absorpt_coefficient_mu 2.435 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.679 _exptl_absorpt_correction_T_max 0.786 _exptl_absorpt_process_details 'SADABS(Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 9730 _diffrn_reflns_av_R_equivalents 0.0347 _diffrn_reflns_av_sigmaI/netI 0.0441 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 28.70 _reflns_number_total 3175 _reflns_number_gt 2934 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97(Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _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^)+(0.0354P)^2^] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.053(14) _refine_ls_number_reflns 3175 _refine_ls_number_parameters 272 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0348 _refine_ls_R_factor_gt 0.0299 _refine_ls_wR_factor_ref 0.0673 _refine_ls_wR_factor_gt 0.0651 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 Ni1 Ni 0.287147(15) 0.354690(15) 0.46257(6) 0.01912(11) Uani 1 1 d . . . Ni2 Ni 0.401535(15) 0.306047(15) 0.51737(5) 0.01613(10) Uani 1 1 d . . . C1 C 0.37060(12) 0.36116(10) 0.2103(4) 0.0145(6) Uani 1 1 d . . . C2 C 0.38202(12) 0.37510(11) 0.0330(4) 0.0166(7) Uani 1 1 d . . . H2A H 0.3712 0.3501 -0.0403 0.020 Uiso 1 1 calc R . . H2B H 0.4164 0.3778 0.0209 0.020 Uiso 1 1 calc R . . C3 C 0.35881(11) 0.42217(11) -0.0204(4) 0.0124(6) Uani 1 1 d . . . H3 H 0.3240 0.4185 -0.0202 0.015 Uiso 1 1 calc R . . C4 C 0.37270(12) 0.46220(12) 0.0978(4) 0.0164(7) Uani 1 1 d . . . C5 C 0.37560(11) 0.43695(11) -0.1963(4) 0.0129(7) Uani 1 1 d . . . H5 H 0.4103 0.4411 -0.1948 0.016 Uiso 1 1 calc R . . C6 C 0.35252(13) 0.48369(11) -0.2468(4) 0.0183(7) Uani 1 1 d . . . H6A H 0.3184 0.4788 -0.2567 0.022 Uiso 1 1 calc R . . H6B H 0.3576 0.5066 -0.1593 0.022 Uiso 1 1 calc R . . C7 C 0.37088(13) 0.50455(12) -0.4078(4) 0.0170(7) Uani 1 1 d . . . C8 C 0.36324(12) 0.39682(12) -0.3166(4) 0.0151(7) Uani 1 1 d . . . O1 O 0.40202(8) 0.33641(9) 0.2825(3) 0.0211(5) Uani 1 1 d . . . O2 O 0.33190(9) 0.37400(9) 0.2697(3) 0.0241(5) Uani 1 1 d . . . O3 O 0.41564(10) 0.46554(10) 0.1372(4) 0.0342(7) Uani 1 1 d . . . O4 O 0.34080(8) 0.49055(8) 0.1439(3) 0.0170(5) Uani 1 1 d . . . O5 O 0.32002(9) 0.39147(9) -0.3504(3) 0.0246(6) Uani 1 1 d . . . O6 O 0.39726(9) 0.37189(9) -0.3690(3) 0.0229(6) Uani 1 1 d . . . O7 O 0.41510(10) 0.50540(12) -0.4320(4) 0.0390(8) Uani 1 1 d . . . O8 O 0.34051(8) 0.52190(8) -0.5040(3) 0.0213(5) Uani 1 1 d . . . O7W O 0.4985(2) 0.5349(3) -0.3067(9) 0.059(2) Uani 0.50 1 d P . . O8W O 0.2426(3) 0.3522(3) -0.0182(10) 0.078(3) Uani 0.50 1 d P . . O1W O 0.25279(10) 0.31257(12) 0.2889(4) 0.0345(7) Uani 1 1 d D . . H1C H 0.2604(19) 0.3065(18) 0.191(4) 0.052 Uiso 1 1 d D . . H1D H 0.2280(14) 0.2955(16) 0.307(7) 0.052 Uiso 1 1 d D . . O2W O 0.23311(12) 0.33465(13) 0.6406(4) 0.0399(8) Uani 1 1 d D . . H2C H 0.2058(13) 0.3241(19) 0.617(7) 0.060 Uiso 1 1 d D . . H2D H 0.242(2) 0.327(2) 0.725(8) 0.060 Uiso 1 1 d . . . O3W O 0.24526(10) 0.41351(11) 0.4140(4) 0.0291(7) Uani 1 1 d D . . H3C H 0.2200(19) 0.4136(18) 0.442(8) 0.044 Uiso 1 1 d . . . H3D H 0.245(2) 0.428(2) 0.319(5) 0.044 Uiso 1 1 d D . . O4W O 0.47734(10) 0.31005(12) 0.5193(4) 0.0308(7) Uani 1 1 d . . . H4C H 0.4929(19) 0.3269(18) 0.467(7) 0.046 Uiso 1 1 d . . . H4D H 0.487(2) 0.307(2) 0.592(7) 0.046 Uiso 1 1 d . . . O5W O 0.32643(9) 0.29540(8) 0.5333(3) 0.0163(5) Uani 1 1 d . . . H5C H 0.3201(15) 0.2815(15) 0.624(6) 0.024 Uiso 1 1 d . . . H5D H 0.3209(15) 0.2768(15) 0.481(6) 0.024 Uiso 1 1 d . . . O6W O 0.24935(11) 0.45521(12) 0.1050(4) 0.0386(8) Uani 1 1 d D . . H6C H 0.2238(13) 0.4724(16) 0.102(7) 0.058 Uiso 1 1 d D . . H6D H 0.2722(15) 0.4720(17) 0.130(7) 0.058 Uiso 1 1 d 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 Ni1 0.0182(2) 0.0218(2) 0.0174(2) -0.00034(18) -0.00062(18) 0.00065(18) Ni2 0.0190(2) 0.0153(2) 0.0142(2) 0.00023(16) 0.00000(16) -0.00010(16) C1 0.0228(17) 0.0089(14) 0.0118(15) -0.0002(13) 0.0008(13) -0.0052(12) C2 0.0241(17) 0.0141(16) 0.0115(15) 0.0033(13) 0.0021(13) 0.0039(13) C3 0.0145(15) 0.0114(14) 0.0114(16) 0.0019(12) -0.0015(12) -0.0005(11) C4 0.0253(19) 0.0136(16) 0.0102(15) 0.0019(13) -0.0010(13) 0.0013(13) C5 0.0161(16) 0.0135(16) 0.0092(16) -0.0005(11) 0.0013(12) -0.0001(12) C6 0.0267(17) 0.0143(15) 0.0140(16) 0.0034(14) 0.0053(13) 0.0039(13) C7 0.0268(19) 0.0097(15) 0.0146(16) 0.0005(13) 0.0031(14) -0.0006(13) C8 0.0247(17) 0.0159(15) 0.0046(16) 0.0036(12) 0.0000(12) 0.0004(13) O1 0.0214(13) 0.0251(13) 0.0167(13) 0.0065(11) 0.0034(10) 0.0032(10) O2 0.0222(12) 0.0271(14) 0.0232(13) 0.0100(11) 0.0067(11) 0.0064(10) O3 0.0193(14) 0.0345(16) 0.0488(18) -0.0269(14) -0.0092(12) 0.0061(12) O4 0.0192(12) 0.0138(12) 0.0179(12) -0.0059(10) 0.0001(9) 0.0007(9) O5 0.0242(14) 0.0262(14) 0.0236(13) -0.0107(11) -0.0081(10) 0.0010(11) O6 0.0275(14) 0.0172(13) 0.0240(14) -0.0066(10) 0.0023(11) -0.0001(10) O7 0.0214(14) 0.061(2) 0.0351(17) 0.0298(15) -0.0003(12) 0.0007(13) O8 0.0227(12) 0.0262(13) 0.0151(13) 0.0075(10) 0.0011(10) 0.0034(10) O7W 0.037(4) 0.095(6) 0.046(4) -0.018(4) -0.006(3) 0.003(4) O8W 0.079(6) 0.111(7) 0.043(5) 0.028(5) -0.011(4) -0.029(5) O1W 0.0302(16) 0.0467(18) 0.0264(16) -0.0061(13) -0.0005(13) -0.0152(13) O2W 0.0287(18) 0.052(2) 0.0387(19) 0.0063(16) 0.0103(14) -0.0019(15) O3W 0.0211(14) 0.0346(16) 0.0317(16) 0.0081(13) 0.0012(12) 0.0073(12) O4W 0.0207(14) 0.0440(17) 0.0278(15) 0.0131(14) -0.0011(13) -0.0078(12) O5W 0.0205(12) 0.0153(13) 0.0131(13) -0.0029(10) 0.0000(10) 0.0001(9) O6W 0.0239(16) 0.050(2) 0.042(2) 0.0051(16) -0.0043(14) 0.0028(14) _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 Ni1 O5 2.054(2) 1_556 ? Ni1 O2 2.076(3) . ? Ni1 O1W 2.077(3) . ? Ni1 O3W 2.069(3) . ? Ni1 O5W 2.082(2) . ? Ni1 O2W 2.166(3) . ? Ni2 O6 2.075(2) 1_556 ? Ni2 O1 2.085(3) . ? Ni2 O8 2.098(2) 15_546 ? Ni2 O4 2.111(2) 15_545 ? Ni2 O4W 2.127(3) . ? Ni2 O5W 2.129(2) . ? C1 O2 1.240(4) . ? C1 O1 1.267(4) . ? C1 C2 1.522(5) . ? C2 C3 1.540(4) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.530(4) . ? C3 C5 1.557(4) . ? C3 H3 0.9800 . ? C4 O3 1.248(4) . ? C4 O4 1.256(4) . ? C5 C6 1.524(4) . ? C5 C8 1.532(4) . ? C5 H5 0.9800 . ? C6 C7 1.520(5) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 O8 1.253(4) . ? C7 O7 1.255(4) . ? C8 O5 1.251(4) . ? C8 O6 1.258(4) . ? O4 Ni2 2.111(2) 11_554 ? O5 Ni1 2.054(2) 1_554 ? O6 Ni2 2.075(2) 1_554 ? O8 Ni2 2.098(2) 11_553 ? O1W H1C 0.84(3) . ? O1W H1D 0.86(3) . ? O2W H2C 0.84(3) . ? O2W H2D 0.76(6) . ? O3W H3C 0.74(5) . ? O3W H3D 0.87(3) . ? O4W H4C 0.77(6) . ? O4W H4D 0.65(6) . ? O5W H5C 0.85(5) . ? O5W H5D 0.69(4) . ? O6W H6C 0.87(3) . ? O6W H6D 0.82(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 O5 Ni1 O2 98.72(11) 1_556 . ? O5 Ni1 O1W 174.77(12) 1_556 . ? O2 Ni1 O1W 85.43(11) . . ? O5 Ni1 O3W 89.43(11) 1_556 . ? O2 Ni1 O3W 89.39(11) . . ? O1W Ni1 O3W 93.81(13) . . ? O5 Ni1 O5W 88.02(10) 1_556 . ? O2 Ni1 O5W 95.64(10) . . ? O1W Ni1 O5W 88.41(12) . . ? O3W Ni1 O5W 174.65(12) . . ? O5 Ni1 O2W 87.38(13) 1_556 . ? O2 Ni1 O2W 172.62(13) . . ? O1W Ni1 O2W 88.72(13) . . ? O3W Ni1 O2W 86.51(13) . . ? O5W Ni1 O2W 88.68(12) . . ? O6 Ni2 O1 92.15(10) 1_556 . ? O6 Ni2 O8 91.45(10) 1_556 15_546 ? O1 Ni2 O8 172.77(10) . 15_546 ? O6 Ni2 O4 176.75(10) 1_556 15_545 ? O1 Ni2 O4 85.80(10) . 15_545 ? O8 Ni2 O4 90.32(10) 15_546 15_545 ? O6 Ni2 O4W 90.40(12) 1_556 . ? O1 Ni2 O4W 88.77(11) . . ? O8 Ni2 O4W 84.93(11) 15_546 . ? O4 Ni2 O4W 87.04(12) 15_545 . ? O6 Ni2 O5W 92.42(10) 1_556 . ? O1 Ni2 O5W 96.86(10) . . ? O8 Ni2 O5W 89.25(10) 15_546 . ? O4 Ni2 O5W 90.33(9) 15_545 . ? O4W Ni2 O5W 173.60(12) . . ? O2 C1 O1 126.1(3) . . ? O2 C1 C2 118.3(3) . . ? O1 C1 C2 115.6(3) . . ? C1 C2 C3 113.5(3) . . ? C1 C2 H2A 108.9 . . ? C3 C2 H2A 108.9 . . ? C1 C2 H2B 108.9 . . ? C3 C2 H2B 108.9 . . ? H2A C2 H2B 107.7 . . ? C4 C3 C2 110.7(3) . . ? C4 C3 C5 107.3(3) . . ? C2 C3 C5 111.1(3) . . ? C4 C3 H3 109.2 . . ? C2 C3 H3 109.2 . . ? C5 C3 H3 109.2 . . ? O3 C4 O4 124.2(3) . . ? O3 C4 C3 117.4(3) . . ? O4 C4 C3 118.3(3) . . ? C6 C5 C8 111.8(3) . . ? C6 C5 C3 110.4(3) . . ? C8 C5 C3 108.4(2) . . ? C6 C5 H5 108.7 . . ? C8 C5 H5 108.7 . . ? C3 C5 H5 108.7 . . ? C7 C6 C5 114.9(3) . . ? C7 C6 H6A 108.5 . . ? C5 C6 H6A 108.5 . . ? C7 C6 H6B 108.5 . . ? C5 C6 H6B 108.5 . . ? H6A C6 H6B 107.5 . . ? O8 C7 O7 124.5(3) . . ? O8 C7 C6 117.0(3) . . ? O7 C7 C6 118.4(3) . . ? O5 C8 O6 126.3(3) . . ? O5 C8 C5 116.5(3) . . ? O6 C8 C5 117.1(3) . . ? C1 O1 Ni2 130.0(2) . . ? C1 O2 Ni1 138.0(2) . . ? C4 O4 Ni2 128.7(2) . 11_554 ? C8 O5 Ni1 131.0(2) . 1_554 ? C8 O6 Ni2 133.9(2) . 1_554 ? C7 O8 Ni2 130.9(2) . 11_553 ? Ni1 O1W H1C 130(4) . . ? Ni1 O1W H1D 125(4) . . ? H1C O1W H1D 105(5) . . ? Ni1 O2W H2C 125(4) . . ? Ni1 O2W H2D 116(5) . . ? H2C O2W H2D 114(6) . . ? Ni1 O3W H3C 119(4) . . ? Ni1 O3W H3D 122(5) . . ? H3C O3W H3D 106(6) . . ? Ni2 O4W H4C 126(4) . . ? Ni2 O4W H4D 115(5) . . ? H4C O4W H4D 110(6) . . ? Ni1 O5W Ni2 113.11(11) . . ? Ni1 O5W H5C 120(3) . . ? Ni2 O5W H5C 109(3) . . ? Ni1 O5W H5D 109(4) . . ? Ni2 O5W H5D 107(4) . . ? H5C O5W H5D 98(4) . . ? H6C O6W H6D 109(5) . . ? 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 O2 C1 C2 C3 29.8(4) . . . . ? O1 C1 C2 C3 -151.3(3) . . . . ? C1 C2 C3 C4 55.5(4) . . . . ? C1 C2 C3 C5 174.6(3) . . . . ? C2 C3 C4 O3 46.0(4) . . . . ? C5 C3 C4 O3 -75.3(4) . . . . ? C2 C3 C4 O4 -136.6(3) . . . . ? C5 C3 C4 O4 102.1(3) . . . . ? C4 C3 C5 C6 -58.6(3) . . . . ? C2 C3 C5 C6 -179.7(3) . . . . ? C4 C3 C5 C8 178.6(3) . . . . ? C2 C3 C5 C8 57.5(3) . . . . ? C8 C5 C6 C7 -66.2(4) . . . . ? C3 C5 C6 C7 173.0(3) . . . . ? C5 C6 C7 O8 138.1(3) . . . . ? C5 C6 C7 O7 -45.3(5) . . . . ? C6 C5 C8 O5 -50.2(4) . . . . ? C3 C5 C8 O5 71.8(4) . . . . ? C6 C5 C8 O6 131.2(3) . . . . ? C3 C5 C8 O6 -106.8(3) . . . . ? O2 C1 O1 Ni2 2.3(5) . . . . ? C2 C1 O1 Ni2 -176.5(2) . . . . ? O6 Ni2 O1 C1 -62.6(3) 1_556 . . . ? O4 Ni2 O1 C1 119.9(3) 15_545 . . . ? O4W Ni2 O1 C1 -153.0(3) . . . . ? O5W Ni2 O1 C1 30.1(3) . . . . ? O1 C1 O2 Ni1 -19.2(6) . . . . ? C2 C1 O2 Ni1 159.6(3) . . . . ? O5 Ni1 O2 C1 83.8(4) 1_556 . . . ? O1W Ni1 O2 C1 -93.0(4) . . . . ? O3W Ni1 O2 C1 173.1(4) . . . . ? O5W Ni1 O2 C1 -5.1(4) . . . . ? O3 C4 O4 Ni2 9.7(5) . . . 11_554 ? C3 C4 O4 Ni2 -167.5(2) . . . 11_554 ? O6 C8 O5 Ni1 -17.3(5) . . . 1_554 ? C5 C8 O5 Ni1 164.2(2) . . . 1_554 ? O5 C8 O6 Ni2 -15.5(5) . . . 1_554 ? C5 C8 O6 Ni2 162.9(2) . . . 1_554 ? O7 C7 O8 Ni2 1.5(5) . . . 11_553 ? C6 C7 O8 Ni2 177.8(2) . . . 11_553 ? O5 Ni1 O5W Ni2 -60.24(13) 1_556 . . . ? O2 Ni1 O5W Ni2 38.33(14) . . . . ? O1W Ni1 O5W Ni2 123.58(14) . . . . ? O2W Ni1 O5W Ni2 -147.67(15) . . . . ? O6 Ni2 O5W Ni1 45.56(14) 1_556 . . . ? O1 Ni2 O5W Ni1 -46.90(14) . . . . ? O8 Ni2 O5W Ni1 136.98(13) 15_546 . . . ? O4 Ni2 O5W Ni1 -132.70(13) 15_545 . . . ? 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 O1W H1C O8W 0.84(3) 2.18(5) 2.740(9) 124(4) . O6W H6D O4 0.82(3) 1.99(3) 2.767(4) 156(6) . O1W H1C O7W 0.84(3) 2.11(3) 2.906(8) 158(5) 15_545 O5W H5D O3 0.69(4) 1.92(4) 2.553(4) 151(5) 15_545 O1W H1D O3 0.86(3) 1.89(3) 2.688(4) 154(5) 16_455 O2W H2C O3 0.84(3) 2.45(4) 3.128(5) 139(5) 16_455 O3W H3C O1 0.74(5) 2.04(5) 2.783(4) 177(6) 16_455 O2W H2D O7W 0.76(6) 2.14(6) 2.870(9) 160(6) 15_546 O5W H5C O7 0.85(5) 1.79(5) 2.578(4) 154(4) 15_546 O2W H2D O8W 0.76(6) 2.20(6) 2.819(9) 139(6) 1_556 O4W H4C O5 0.77(6) 2.40(5) 3.090(4) 149(5) 8 O4W H4D O6W 0.65(6) 2.19(6) 2.820(5) 164(7) 8 O4W H4C O3W 0.77(6) 2.47(6) 3.014(5) 129(5) 8_554 O6W H6C O8 0.87(3) 2.00(4) 2.745(4) 143(5) 10_565 _diffrn_measured_fraction_theta_max 0.936 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.555 _refine_diff_density_min -0.335 _refine_diff_density_rms 0.078 #===End data_compound-3 _database_code_depnum_ccdc_archive 'CCDC 648892' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H6 O6.50 Zn' _chemical_formula_weight 223.46 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pcca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' 'x+1/2, -y, -z+1/2' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' '-x-1/2, y, z-1/2' 'x, -y, z-1/2' _cell_length_a 13.908(2) _cell_length_b 8.4090(10) _cell_length_c 13.042(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1525.3(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1359 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 28.4 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.946 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 3.210 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.411 _exptl_absorpt_correction_T_max 0.479 _exptl_absorpt_process_details 'SADABS(Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8440 _diffrn_reflns_av_R_equivalents 0.1177 _diffrn_reflns_av_sigmaI/netI 0.0678 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 28.41 _reflns_number_total 1811 _reflns_number_gt 1366 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97(Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _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^)+(0.0350P)^2^+3.8092P] 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 1811 _refine_ls_number_parameters 119 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0726 _refine_ls_R_factor_gt 0.0570 _refine_ls_wR_factor_ref 0.1327 _refine_ls_wR_factor_gt 0.1241 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.096 _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 Zn1 Zn 0.2500 0.0000 0.20578(5) 0.0275(2) Uani 1 2 d S . . Zn2 Zn 0.2500 0.5000 0.43079(6) 0.0421(2) Uani 1 2 d S . . C1 C 0.3871(3) 0.0315(6) 0.5806(4) 0.0373(10) Uani 1 1 d . . . C2 C 0.4609(3) 0.0636(5) 0.4962(3) 0.0301(8) Uani 1 1 d . . . H2 H 0.4895 0.1688 0.5067 0.036 Uiso 1 1 calc R . . C3 C 0.4115(3) 0.0586(5) 0.3913(3) 0.0308(9) Uani 1 1 d . . . H3A H 0.4599 0.0688 0.3382 0.037 Uiso 1 1 calc R . . H3B H 0.3807 -0.0441 0.3829 0.037 Uiso 1 1 calc R . . C4 C 0.3371(3) 0.1877(5) 0.3770(3) 0.0267(8) Uani 1 1 d . . . O1 O 0.3758(3) 0.1241(5) 0.6526(2) 0.0452(8) Uani 1 1 d . . . O2 O 0.3381(3) -0.0942(5) 0.5773(3) 0.0582(10) Uani 1 1 d . . . O3 O 0.3368(2) 0.3015(4) 0.4367(2) 0.0410(8) Uani 1 1 d . . . O4 O 0.2796(2) 0.1737(4) 0.3032(2) 0.0392(7) Uani 1 1 d . . . O1W O 0.1430(4) 0.3875(7) 0.4980(6) 0.0508(15) Uani 0.60 1 d P . . O1W' O 0.1769(8) 0.4153(12) 0.5687(8) 0.057(2) Uiso 0.40 1 d P . . O2W O 0.1272(13) 0.372(2) 0.3504(12) 0.105(5) Uiso 0.40 1 d P . . O2W' O 0.2121(7) 0.4617(10) 0.2824(7) 0.089(3) Uiso 0.60 1 d P . . O3W O 0.4652(7) 0.4208(9) 0.6434(5) 0.056(2) Uani 0.50 1 d PD . . H3C H 0.411(4) 0.456(17) 0.668(11) 0.084 Uiso 0.50 1 d PD . . H3D H 0.514(5) 0.459(16) 0.677(10) 0.084 Uiso 0.50 1 d PD . . 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 Zn1 0.0182(3) 0.0411(4) 0.0230(3) 0.000 0.000 0.0021(3) Zn2 0.0435(5) 0.0374(4) 0.0453(5) 0.000 0.000 0.0107(3) C1 0.024(2) 0.049(3) 0.039(2) 0.0032(19) 0.0043(18) 0.0071(18) C2 0.027(2) 0.0299(18) 0.034(2) 0.0016(17) -0.0039(16) 0.0019(16) C3 0.0228(19) 0.040(2) 0.029(2) -0.0048(16) -0.0030(16) 0.0103(17) C4 0.0229(17) 0.0305(19) 0.0266(17) 0.0026(15) -0.0009(15) 0.0023(15) O1 0.0418(18) 0.065(2) 0.0284(15) -0.0046(15) 0.0111(14) 0.0038(17) O2 0.0326(18) 0.057(2) 0.085(3) -0.010(2) 0.0236(19) -0.0117(17) O3 0.0447(18) 0.0368(16) 0.0414(17) -0.0072(13) -0.0131(14) 0.0135(14) O4 0.0360(16) 0.0410(17) 0.0406(16) -0.0049(14) -0.0164(13) 0.0108(14) O1W 0.036(3) 0.033(3) 0.083(4) 0.013(3) 0.014(3) -0.002(2) O3W 0.094(6) 0.042(4) 0.032(4) -0.003(3) -0.021(4) -0.018(4) _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 Zn1 O4 1.979(3) . ? Zn1 O4 1.979(3) 2 ? Zn1 O1 2.152(4) 8 ? Zn1 O1 2.152(4) 7_655 ? Zn1 O2 2.223(4) 7_655 ? Zn1 O2 2.223(4) 8 ? Zn1 C1 2.524(5) 7_655 ? Zn1 C1 2.524(5) 8 ? Zn2 O1W 1.970(5) 2_565 ? Zn2 O1W 1.970(5) . ? Zn2 O2W' 2.032(9) . ? Zn2 O2W' 2.032(9) 2_565 ? Zn2 O3 2.061(3) . ? Zn2 O3 2.061(3) 2_565 ? Zn2 O1W' 2.185(11) 2_565 ? Zn2 O1W' 2.185(11) . ? Zn2 O2W 2.275(17) . ? Zn2 O2W 2.275(17) 2_565 ? C1 O1 1.230(6) . ? C1 O2 1.258(6) . ? C1 C2 1.529(6) . ? C1 Zn1 2.524(5) 7_656 ? C2 C2 1.530(8) 5_656 ? C2 C3 1.531(6) . ? C2 H2 0.9800 . ? C3 C4 1.511(6) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 O3 1.234(5) . ? C4 O4 1.258(5) . ? O1 Zn1 2.152(4) 7_656 ? O2 Zn1 2.223(4) 7_656 ? O1W O1W' 1.062(11) . ? O2W O2W' 1.658(19) . ? O2W' O2W' 1.236(19) 2_565 ? O3W H3C 0.87(2) . ? O3W H3D 0.87(2) . ? 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 O4 Zn1 O4 100.2(2) . 2 ? O4 Zn1 O1 113.32(14) . 8 ? O4 Zn1 O1 91.02(12) 2 8 ? O4 Zn1 O1 91.02(12) . 7_655 ? O4 Zn1 O1 113.32(14) 2 7_655 ? O1 Zn1 O1 142.38(17) 8 7_655 ? O4 Zn1 O2 149.51(13) . 7_655 ? O4 Zn1 O2 96.09(16) 2 7_655 ? O1 Zn1 O2 91.86(14) 8 7_655 ? O1 Zn1 O2 58.76(13) 7_655 7_655 ? O4 Zn1 O2 96.09(16) . 8 ? O4 Zn1 O2 149.51(13) 2 8 ? O1 Zn1 O2 58.76(13) 8 8 ? O1 Zn1 O2 91.86(14) 7_655 8 ? O2 Zn1 O2 82.1(2) 7_655 8 ? O4 Zn1 C1 119.65(14) . 7_655 ? O4 Zn1 C1 109.60(14) 2 7_655 ? O1 Zn1 C1 117.16(15) 8 7_655 ? O1 Zn1 C1 29.13(14) 7_655 7_655 ? O2 Zn1 C1 29.88(14) 7_655 7_655 ? O2 Zn1 C1 83.78(15) 8 7_655 ? O4 Zn1 C1 109.60(14) . 8 ? O4 Zn1 C1 119.65(14) 2 8 ? O1 Zn1 C1 29.13(14) 8 8 ? O1 Zn1 C1 117.16(15) 7_655 8 ? O2 Zn1 C1 83.78(15) 7_655 8 ? O2 Zn1 C1 29.88(14) 8 8 ? C1 Zn1 C1 99.4(2) 7_655 8 ? O1W Zn2 O1W 127.1(5) 2_565 . ? O1W Zn2 O2W' 134.1(3) 2_565 . ? O1W Zn2 O2W' 98.7(4) . . ? O1W Zn2 O2W' 98.7(4) 2_565 2_565 ? O1W Zn2 O2W' 134.1(3) . 2_565 ? O2W' Zn2 O2W' 35.4(5) . 2_565 ? O1W Zn2 O3 85.97(19) 2_565 . ? O1W Zn2 O3 92.1(2) . . ? O2W' Zn2 O3 93.4(3) . . ? O2W' Zn2 O3 90.7(3) 2_565 . ? O1W Zn2 O3 92.1(2) 2_565 2_565 ? O1W Zn2 O3 85.97(19) . 2_565 ? O2W' Zn2 O3 90.7(3) . 2_565 ? O2W' Zn2 O3 93.4(3) 2_565 2_565 ? O3 Zn2 O3 175.68(18) . 2_565 ? O1W Zn2 O1W' 29.0(3) 2_565 2_565 ? O1W Zn2 O1W' 98.1(4) . 2_565 ? O2W' Zn2 O1W' 163.0(4) . 2_565 ? O2W' Zn2 O1W' 127.7(4) 2_565 2_565 ? O3 Zn2 O1W' 87.7(3) . 2_565 ? O3 Zn2 O1W' 88.7(3) 2_565 2_565 ? O1W Zn2 O1W' 98.1(4) 2_565 . ? O1W Zn2 O1W' 29.0(3) . . ? O2W' Zn2 O1W' 127.7(4) . . ? O2W' Zn2 O1W' 163.0(4) 2_565 . ? O3 Zn2 O1W' 88.7(3) . . ? O3 Zn2 O1W' 87.7(3) 2_565 . ? O1W' Zn2 O1W' 69.2(6) 2_565 . ? O1W Zn2 O2W 179.0(5) 2_565 . ? O1W Zn2 O2W 53.9(5) . . ? O2W' Zn2 O2W 44.8(5) . . ? O2W' Zn2 O2W 80.2(5) 2_565 . ? O3 Zn2 O2W 94.3(5) . . ? O3 Zn2 O2W 87.7(5) 2_565 . ? O1W' Zn2 O2W 152.0(5) 2_565 . ? O1W' Zn2 O2W 82.9(5) . . ? O1W Zn2 O2W 53.9(5) 2_565 2_565 ? O1W Zn2 O2W 179.0(5) . 2_565 ? O2W' Zn2 O2W 80.2(5) . 2_565 ? O2W' Zn2 O2W 44.8(5) 2_565 2_565 ? O3 Zn2 O2W 87.7(5) . 2_565 ? O3 Zn2 O2W 94.3(5) 2_565 2_565 ? O1W' Zn2 O2W 82.9(5) 2_565 2_565 ? O1W' Zn2 O2W 152.0(5) . 2_565 ? O2W Zn2 O2W 125.1(8) . 2_565 ? O1 C1 O2 119.3(4) . . ? O1 C1 C2 121.6(4) . . ? O2 C1 C2 119.1(4) . . ? O1 C1 Zn1 58.4(2) . 7_656 ? O2 C1 Zn1 61.7(3) . 7_656 ? C2 C1 Zn1 172.4(3) . 7_656 ? C1 C2 C2 107.9(4) . 5_656 ? C1 C2 C3 109.7(4) . . ? C2 C2 C3 111.0(4) 5_656 . ? C1 C2 H2 109.4 . . ? C2 C2 H2 109.4 5_656 . ? C3 C2 H2 109.4 . . ? C4 C3 C2 113.4(3) . . ? C4 C3 H3A 108.9 . . ? C2 C3 H3A 108.9 . . ? C4 C3 H3B 108.9 . . ? C2 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? O3 C4 O4 123.6(4) . . ? O3 C4 C3 118.8(3) . . ? O4 C4 C3 117.6(4) . . ? C1 O1 Zn1 92.5(3) . 7_656 ? C1 O2 Zn1 88.4(3) . 7_656 ? C4 O3 Zn2 127.3(3) . . ? C4 O4 Zn1 133.8(3) . . ? O1W' O1W Zn2 86.8(7) . . ? O1W O1W' Zn2 64.2(6) . . ? O2W' O2W Zn2 59.8(6) . . ? O2W' O2W' O2W 147.6(7) 2_565 . ? O2W' O2W' Zn2 72.3(3) 2_565 . ? O2W O2W' Zn2 75.4(7) . . ? H3C O3W H3D 112(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 C2 113.5(5) . . . 5_656 ? O2 C1 C2 C2 -65.1(6) . . . 5_656 ? O1 C1 C2 C3 -125.5(5) . . . . ? O2 C1 C2 C3 55.9(5) . . . . ? C1 C2 C3 C4 64.1(5) . . . . ? C2 C2 C3 C4 -176.7(4) 5_656 . . . ? C2 C3 C4 O3 15.3(6) . . . . ? C2 C3 C4 O4 -165.7(4) . . . . ? O2 C1 O1 Zn1 -10.3(5) . . . 7_656 ? C2 C1 O1 Zn1 171.0(4) . . . 7_656 ? O1 C1 O2 Zn1 10.0(5) . . . 7_656 ? C2 C1 O2 Zn1 -171.4(4) . . . 7_656 ? O4 C4 O3 Zn2 -2.9(6) . . . . ? C3 C4 O3 Zn2 176.0(3) . . . . ? O1W Zn2 O3 C4 -150.9(4) 2_565 . . . ? O1W Zn2 O3 C4 82.0(4) . . . . ? O2W' Zn2 O3 C4 -16.9(5) . . . . ? O2W' Zn2 O3 C4 -52.2(5) 2_565 . . . ? O1W' Zn2 O3 C4 -179.9(5) 2_565 . . . ? O1W' Zn2 O3 C4 110.8(5) . . . . ? O2W Zn2 O3 C4 28.1(6) . . . . ? O2W Zn2 O3 C4 -97.0(6) 2_565 . . . ? O3 C4 O4 Zn1 -171.1(3) . . . . ? C3 C4 O4 Zn1 10.0(6) . . . . ? O4 Zn1 O4 C4 54.5(4) 2 . . . ? O1 Zn1 O4 C4 -41.1(4) 8 . . . ? O1 Zn1 O4 C4 168.4(4) 7_655 . . . ? O2 Zn1 O4 C4 175.6(4) 7_655 . . . ? O2 Zn1 O4 C4 -99.6(4) 8 . . . ? C1 Zn1 O4 C4 174.1(4) 7_655 . . . ? C1 Zn1 O4 C4 -72.2(4) 8 . . . ? O1W Zn2 O1W O1W' -3.0(6) 2_565 . . . ? O2W' Zn2 O1W O1W' 177.3(7) . . . . ? O2W' Zn2 O1W O1W' 176.6(7) 2_565 . . . ? O3 Zn2 O1W O1W' 83.5(7) . . . . ? O3 Zn2 O1W O1W' -92.6(7) 2_565 . . . ? O1W' Zn2 O1W O1W' -4.5(9) 2_565 . . . ? O2W Zn2 O1W O1W' 177.3(9) . . . . ? O1W Zn2 O1W' O1W 177.6(5) 2_565 . . . ? O2W' Zn2 O1W' O1W -3.4(9) . . . . ? O2W' Zn2 O1W' O1W -8.4(18) 2_565 . . . ? O3 Zn2 O1W' O1W -96.7(6) . . . . ? O3 Zn2 O1W' O1W 85.8(6) 2_565 . . . ? O1W' Zn2 O1W' O1W 175.3(10) 2_565 . . . ? O2W Zn2 O1W' O1W -2.2(8) . . . . ? O2W Zn2 O1W' O1W -179.4(10) 2_565 . . . ? O2W' Zn2 O2W O2W' -0.5(8) 2_565 . . . ? O3 Zn2 O2W O2W' -90.5(6) . . . . ? O3 Zn2 O2W O2W' 93.3(6) 2_565 . . . ? O1W' Zn2 O2W O2W' 176.3(8) 2_565 . . . ? O1W' Zn2 O2W O2W' -178.7(7) . . . . ? O2W Zn2 O2W O2W' -0.3(4) 2_565 . . . ? Zn2 O2W O2W' O2W' 2(2) . . . 2_565 ? O1W Zn2 O2W' O2W' 1.2(11) 2_565 . . 2_565 ? O1W Zn2 O2W' O2W' -179.1(8) . . . 2_565 ? O3 Zn2 O2W' O2W' -86.5(9) . . . 2_565 ? O3 Zn2 O2W' O2W' 94.9(9) 2_565 . . 2_565 ? O1W' Zn2 O2W' O2W' 7(2) 2_565 . . 2_565 ? O1W' Zn2 O2W' O2W' -177.5(7) . . . 2_565 ? O2W Zn2 O2W' O2W' -179.1(13) . . . 2_565 ? O2W Zn2 O2W' O2W' 0.6(9) 2_565 . . 2_565 ? O1W Zn2 O2W' O2W -179.7(7) 2_565 . . . ? O1W Zn2 O2W' O2W 0.0(7) . . . . ? O2W' Zn2 O2W' O2W 179.1(13) 2_565 . . . ? O3 Zn2 O2W' O2W 92.7(7) . . . . ? O3 Zn2 O2W' O2W -86.0(7) 2_565 . . . ? O1W' Zn2 O2W' O2W -174.0(13) 2_565 . . . ? O1W' Zn2 O2W' O2W 1.7(9) . . . . ? O2W Zn2 O2W' O2W 179.7(4) 2_565 . . . ? _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.209 _refine_diff_density_min -1.002 _refine_diff_density_rms 0.168 #===End data_compound-4 _database_code_depnum_ccdc_archive 'CCDC 648893' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H13 Mn N2 O5' _chemical_formula_weight 344.20 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' Mn Mn 0.3368 0.7283 '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 7.7020(10) _cell_length_b 9.705(2) _cell_length_c 10.387(5) _cell_angle_alpha 79.397(3) _cell_angle_beta 72.326(6) _cell_angle_gamma 68.933(5) _cell_volume 687.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2376 _cell_measurement_theta_min 2.1 _cell_measurement_theta_max 28.3 _exptl_crystal_description Block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.186 _exptl_crystal_size_mid 0.173 _exptl_crystal_size_min 0.120 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.662 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 352 _exptl_absorpt_coefficient_mu 0.986 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.81 _exptl_absorpt_correction_T_max 0.87 _exptl_absorpt_process_details 'SADABS(Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 4232 _diffrn_reflns_av_R_equivalents 0.0178 _diffrn_reflns_av_sigmaI/netI 0.0472 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 3 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 28.25 _reflns_number_total 3057 _reflns_number_gt 2376 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97(Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _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^)+(0.0927P)^2^+0.0840P] 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 3057 _refine_ls_number_parameters 207 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0659 _refine_ls_R_factor_gt 0.0461 _refine_ls_wR_factor_ref 0.1555 _refine_ls_wR_factor_gt 0.1230 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _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 Mn1 Mn 0.24007(7) 0.15636(5) 0.70823(5) 0.0287(2) Uani 1 1 d . . . C1 C 0.5362(6) -0.1679(4) 0.7616(4) 0.0460(10) Uani 1 1 d . . . H1 H 0.5795 -0.1601 0.6675 0.055 Uiso 1 1 calc R . . C2 C 0.6204(6) -0.2976(4) 0.8330(4) 0.0481(10) Uani 1 1 d . . . H2 H 0.7173 -0.3760 0.7881 0.058 Uiso 1 1 calc R . . C3 C 0.5571(6) -0.3072(4) 0.9718(4) 0.0490(10) Uani 1 1 d . . . H3 H 0.6125 -0.3925 1.0223 0.059 Uiso 1 1 calc R . . C4 C 0.4126(6) -0.1914(4) 1.0361(4) 0.0430(9) Uani 1 1 d . . . H4 H 0.3679 -0.1974 1.1301 0.052 Uiso 1 1 calc R . . C5 C 0.3336(5) -0.0640(4) 0.9578(3) 0.0305(7) Uani 1 1 d . . . C6 C 0.1785(5) 0.0669(4) 1.0199(3) 0.0297(7) Uani 1 1 d . . . C7 C 0.1117(6) 0.0774(4) 1.1573(4) 0.0419(9) Uani 1 1 d . . . H7 H 0.1592 -0.0015 1.2168 0.050 Uiso 1 1 calc R . . C8 C -0.0266(6) 0.2063(5) 1.2065(4) 0.0499(10) Uani 1 1 d . . . H8 H -0.0747 0.2142 1.2994 0.060 Uiso 1 1 calc R . . C9 C -0.0928(6) 0.3230(5) 1.1169(4) 0.0504(10) Uani 1 1 d . . . H9 H -0.1824 0.4121 1.1478 0.060 Uiso 1 1 calc R . . C10 C -0.0224(6) 0.3042(4) 0.9802(4) 0.0430(9) Uani 1 1 d . . . H10 H -0.0684 0.3819 0.9191 0.052 Uiso 1 1 calc R . . C11 C -0.1259(5) 0.2985(4) 0.6038(3) 0.0328(7) Uani 1 1 d . . . C12 C -0.2856(5) 0.4411(4) 0.5816(4) 0.0375(8) Uani 1 1 d . . . H12A H -0.2277 0.5130 0.5257 0.045 Uiso 1 1 calc R . . H12B H -0.3572 0.4807 0.6686 0.045 Uiso 1 1 calc R . . C13 C -0.4260(4) 0.4231(3) 0.5146(4) 0.0298(7) Uani 1 1 d . . . H13 H -0.3534 0.3790 0.4285 0.036 Uiso 1 1 calc R . . C14 C -0.5354(4) 0.3237(4) 0.6033(3) 0.0302(7) Uani 1 1 d . . . N1 N 0.3948(4) -0.0532(3) 0.8225(3) 0.0335(6) Uani 1 1 d . . . N2 N 0.1099(4) 0.1782(3) 0.9316(3) 0.0328(6) Uani 1 1 d . . . O1 O -0.0180(4) 0.3086(3) 0.6693(3) 0.0414(6) Uani 1 1 d . . . O2 O -0.1118(4) 0.1834(3) 0.5597(4) 0.0586(9) Uani 1 1 d . . . O3 O -0.5350(4) 0.2151(3) 0.5508(3) 0.0409(6) Uani 1 1 d . . . O4 O -0.6319(4) 0.3505(3) 0.7207(3) 0.0453(7) Uani 1 1 d . . . O1W O 0.2374(5) 0.0130(3) 0.5753(3) 0.0471(7) Uani 1 1 d . . . H1A H 0.137(7) 0.056(5) 0.555(5) 0.054(14) Uiso 1 1 d . . . H1B H 0.315(8) -0.060(6) 0.543(5) 0.075(17) Uiso 1 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 Mn1 0.0268(3) 0.0282(3) 0.0284(3) 0.00289(19) -0.0099(2) -0.0058(2) C1 0.047(2) 0.043(2) 0.040(2) -0.0099(17) -0.0178(17) 0.0023(17) C2 0.047(2) 0.034(2) 0.059(3) -0.0155(18) -0.024(2) 0.0046(17) C3 0.061(3) 0.0265(19) 0.058(3) 0.0089(17) -0.031(2) -0.0065(17) C4 0.050(2) 0.0331(19) 0.041(2) 0.0088(16) -0.0189(17) -0.0071(17) C5 0.0333(17) 0.0255(16) 0.0357(18) 0.0033(13) -0.0156(14) -0.0103(13) C6 0.0311(17) 0.0267(16) 0.0329(17) 0.0036(13) -0.0106(13) -0.0122(13) C7 0.050(2) 0.037(2) 0.034(2) 0.0071(15) -0.0103(17) -0.0139(17) C8 0.053(2) 0.054(2) 0.035(2) -0.0061(18) -0.0031(18) -0.014(2) C9 0.045(2) 0.048(2) 0.045(2) -0.0107(18) -0.0084(18) 0.0005(18) C10 0.046(2) 0.0341(19) 0.039(2) -0.0029(15) -0.0115(17) -0.0009(16) C11 0.0285(17) 0.0302(18) 0.0353(18) 0.0027(14) -0.0123(14) -0.0038(14) C12 0.0366(19) 0.0243(17) 0.056(2) 0.0031(15) -0.0238(17) -0.0083(14) C13 0.0258(16) 0.0256(17) 0.0363(18) 0.0039(13) -0.0114(13) -0.0069(13) C14 0.0234(15) 0.0285(17) 0.0360(18) 0.0060(13) -0.0144(14) -0.0039(13) N1 0.0356(16) 0.0304(15) 0.0322(15) -0.0014(11) -0.0142(12) -0.0044(12) N2 0.0308(15) 0.0318(15) 0.0305(15) 0.0045(11) -0.0090(12) -0.0067(12) O1 0.0359(14) 0.0392(14) 0.0501(16) -0.0077(12) -0.0234(12) -0.0011(11) O2 0.0555(18) 0.0334(15) 0.098(3) -0.0108(15) -0.0520(18) 0.0018(13) O3 0.0361(14) 0.0326(13) 0.0517(16) -0.0060(12) -0.0072(12) -0.0107(11) O4 0.0549(17) 0.0432(15) 0.0341(14) 0.0026(11) -0.0072(12) -0.0181(13) O1W 0.0384(16) 0.0379(16) 0.069(2) -0.0202(14) -0.0246(15) -0.0006(13) _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 Mn1 O1 2.110(2) . ? Mn1 O1W 2.141(3) . ? Mn1 O3 2.156(3) 1_655 ? Mn1 N2 2.247(3) . ? Mn1 N1 2.279(3) . ? Mn1 O4 2.458(3) 1_655 ? C1 N1 1.340(5) . ? C1 C2 1.385(5) . ? C1 H1 0.9300 . ? C2 C3 1.372(6) . ? C2 H2 0.9300 . ? C3 C4 1.369(5) . ? C3 H3 0.9300 . ? C4 C5 1.397(5) . ? C4 H4 0.9300 . ? C5 N1 1.337(4) . ? C5 C6 1.483(5) . ? C6 N2 1.344(4) . ? C6 C7 1.372(5) . ? C7 C8 1.381(5) . ? C7 H7 0.9300 . ? C8 C9 1.375(6) . ? C8 H8 0.9300 . ? C9 C10 1.379(6) . ? C9 H9 0.9300 . ? C10 N2 1.345(4) . ? C10 H10 0.9300 . ? C11 O2 1.241(4) . ? C11 O1 1.261(4) . ? C11 C12 1.521(4) . ? C12 C13 1.524(5) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.508(5) . ? C13 C13 1.562(6) 2_466 ? C13 H13 0.9800 . ? C14 O4 1.238(4) . ? C14 O3 1.272(4) . ? O3 Mn1 2.156(3) 1_455 ? O4 Mn1 2.458(3) 1_455 ? O1W H1A 0.81(5) . ? O1W H1B 0.79(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 Mn1 O1W 88.83(11) . . ? O1 Mn1 O3 104.52(10) . 1_655 ? O1W Mn1 O3 88.56(12) . 1_655 ? O1 Mn1 N2 89.75(10) . . ? O1W Mn1 N2 131.99(12) . . ? O3 Mn1 N2 137.75(11) 1_655 . ? O1 Mn1 N1 149.80(11) . . ? O1W Mn1 N1 86.60(11) . . ? O3 Mn1 N1 105.19(10) 1_655 . ? N2 Mn1 N1 71.69(10) . . ? O1 Mn1 O4 93.93(10) . 1_655 ? O1W Mn1 O4 143.89(11) . 1_655 ? O3 Mn1 O4 55.89(9) 1_655 1_655 ? N2 Mn1 O4 84.07(10) . 1_655 ? N1 Mn1 O4 107.14(10) . 1_655 ? N1 C1 C2 122.7(4) . . ? N1 C1 H1 118.7 . . ? C2 C1 H1 118.7 . . ? C3 C2 C1 118.2(4) . . ? C3 C2 H2 120.9 . . ? C1 C2 H2 120.9 . . ? C4 C3 C2 120.1(3) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 118.7(4) . . ? C3 C4 H4 120.7 . . ? C5 C4 H4 120.7 . . ? N1 C5 C4 121.7(3) . . ? N1 C5 C6 116.4(3) . . ? C4 C5 C6 121.9(3) . . ? N2 C6 C7 121.6(3) . . ? N2 C6 C5 115.2(3) . . ? C7 C6 C5 123.2(3) . . ? C6 C7 C8 119.4(3) . . ? C6 C7 H7 120.3 . . ? C8 C7 H7 120.3 . . ? C9 C8 C7 119.5(4) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? C8 C9 C10 118.1(4) . . ? C8 C9 H9 120.9 . . ? C10 C9 H9 120.9 . . ? N2 C10 C9 122.7(3) . . ? N2 C10 H10 118.6 . . ? C9 C10 H10 118.6 . . ? O2 C11 O1 125.2(3) . . ? O2 C11 C12 119.6(3) . . ? O1 C11 C12 115.2(3) . . ? C11 C12 C13 114.3(3) . . ? C11 C12 H12A 108.7 . . ? C13 C12 H12A 108.7 . . ? C11 C12 H12B 108.7 . . ? C13 C12 H12B 108.7 . . ? H12A C12 H12B 107.6 . . ? C14 C13 C12 111.3(3) . . ? C14 C13 C13 108.6(3) . 2_466 ? C12 C13 C13 110.5(3) . 2_466 ? C14 C13 H13 108.8 . . ? C12 C13 H13 108.8 . . ? C13 C13 H13 108.8 2_466 . ? O4 C14 O3 120.4(3) . . ? O4 C14 C13 121.9(3) . . ? O3 C14 C13 117.6(3) . . ? C5 N1 C1 118.7(3) . . ? C5 N1 Mn1 117.5(2) . . ? C1 N1 Mn1 123.7(2) . . ? C6 N2 C10 118.6(3) . . ? C6 N2 Mn1 119.1(2) . . ? C10 N2 Mn1 122.1(2) . . ? C11 O1 Mn1 131.0(2) . . ? C14 O3 Mn1 98.1(2) . 1_455 ? C14 O4 Mn1 84.9(2) . 1_455 ? Mn1 O1W H1A 103(3) . . ? Mn1 O1W H1B 133(4) . . ? H1A O1W H1B 123(5) . . ? 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 N1 C1 C2 C3 -0.8(7) . . . . ? C1 C2 C3 C4 0.9(7) . . . . ? C2 C3 C4 C5 -0.7(6) . . . . ? C3 C4 C5 N1 0.3(6) . . . . ? C3 C4 C5 C6 -179.2(3) . . . . ? N1 C5 C6 N2 3.8(4) . . . . ? C4 C5 C6 N2 -176.7(3) . . . . ? N1 C5 C6 C7 -174.4(3) . . . . ? C4 C5 C6 C7 5.1(5) . . . . ? N2 C6 C7 C8 -1.3(6) . . . . ? C5 C6 C7 C8 176.9(4) . . . . ? C6 C7 C8 C9 -1.2(6) . . . . ? C7 C8 C9 C10 2.4(7) . . . . ? C8 C9 C10 N2 -1.3(7) . . . . ? O2 C11 C12 C13 4.8(5) . . . . ? O1 C11 C12 C13 -174.3(3) . . . . ? C11 C12 C13 C14 63.9(4) . . . . ? C11 C12 C13 C13 -175.3(3) . . . 2_466 ? C12 C13 C14 O4 56.6(4) . . . . ? C13 C13 C14 O4 -65.2(5) 2_466 . . . ? C12 C13 C14 O3 -127.5(3) . . . . ? C13 C13 C14 O3 110.7(4) 2_466 . . . ? C4 C5 N1 C1 -0.2(5) . . . . ? C6 C5 N1 C1 179.3(3) . . . . ? C4 C5 N1 Mn1 176.6(3) . . . . ? C6 C5 N1 Mn1 -3.9(4) . . . . ? C2 C1 N1 C5 0.5(6) . . . . ? C2 C1 N1 Mn1 -176.1(3) . . . . ? O1 Mn1 N1 C5 -52.5(3) . . . . ? O1W Mn1 N1 C5 -134.3(3) . . . . ? O3 Mn1 N1 C5 138.1(2) 1_655 . . . ? N2 Mn1 N1 C5 2.2(2) . . . . ? O4 Mn1 N1 C5 79.8(3) 1_655 . . . ? O1 Mn1 N1 C1 124.1(3) . . . . ? O1W Mn1 N1 C1 42.3(3) . . . . ? O3 Mn1 N1 C1 -45.3(3) 1_655 . . . ? N2 Mn1 N1 C1 178.8(3) . . . . ? O4 Mn1 N1 C1 -103.6(3) 1_655 . . . ? C7 C6 N2 C10 2.4(5) . . . . ? C5 C6 N2 C10 -175.9(3) . . . . ? C7 C6 N2 Mn1 176.4(3) . . . . ? C5 C6 N2 Mn1 -1.8(4) . . . . ? C9 C10 N2 C6 -1.1(6) . . . . ? C9 C10 N2 Mn1 -175.0(3) . . . . ? O1 Mn1 N2 C6 155.7(3) . . . . ? O1W Mn1 N2 C6 67.5(3) . . . . ? O3 Mn1 N2 C6 -92.7(3) 1_655 . . . ? N1 Mn1 N2 C6 -0.1(2) . . . . ? O4 Mn1 N2 C6 -110.3(3) 1_655 . . . ? O1 Mn1 N2 C10 -30.5(3) . . . . ? O1W Mn1 N2 C10 -118.7(3) . . . . ? O3 Mn1 N2 C10 81.2(3) 1_655 . . . ? N1 Mn1 N2 C10 173.8(3) . . . . ? O4 Mn1 N2 C10 63.5(3) 1_655 . . . ? O2 C11 O1 Mn1 9.3(6) . . . . ? C12 C11 O1 Mn1 -171.7(2) . . . . ? O1W Mn1 O1 C11 6.3(3) . . . . ? O3 Mn1 O1 C11 94.5(3) 1_655 . . . ? N2 Mn1 O1 C11 -125.7(3) . . . . ? N1 Mn1 O1 C11 -74.9(4) . . . . ? O4 Mn1 O1 C11 150.2(3) 1_655 . . . ? O4 C14 O3 Mn1 8.3(3) . . . 1_455 ? C13 C14 O3 Mn1 -167.6(2) . . . 1_455 ? O3 C14 O4 Mn1 -7.3(3) . . . 1_455 ? C13 C14 O4 Mn1 168.5(3) . . . 1_455 ? 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 O1W H1B O3 0.79(5) 1.95(5) 2.733(4) 169(6) 2_556 _diffrn_measured_fraction_theta_max 0.900 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.403 _refine_diff_density_min -0.463 _refine_diff_density_rms 0.107 #===End data_compound-5 _database_code_depnum_ccdc_archive 'CCDC 648894' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H13 Mn N2 O5' _chemical_formula_weight 368.22 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' Mn Mn 0.3368 0.7283 '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 7.655(5) _cell_length_b 9.700(7) _cell_length_c 11.090(6) _cell_angle_alpha 84.068(2) _cell_angle_beta 70.758(2) _cell_angle_gamma 68.703(3) _cell_volume 724.3(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2555 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.224 _exptl_crystal_size_mid 0.189 _exptl_crystal_size_min 0.175 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.689 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 376 _exptl_absorpt_coefficient_mu 0.943 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.79 _exptl_absorpt_correction_T_max 0.81 _exptl_absorpt_process_details 'SADABS(Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 7172 _diffrn_reflns_av_R_equivalents 0.0378 _diffrn_reflns_av_sigmaI/netI 0.0503 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.47 _reflns_number_total 3282 _reflns_number_gt 2555 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97(Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _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^)+(0.0607P)^2^+0.1659P] 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 3282 _refine_ls_number_parameters 225 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0630 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.1198 _refine_ls_wR_factor_gt 0.1102 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.110 _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 Mn1 Mn -0.08169(6) 0.16404(5) 0.80563(4) 0.02374(15) Uani 1 1 d . . . C1 C -0.5338(4) 0.3130(3) 0.9202(3) 0.0268(6) Uani 1 1 d . . . C2 C -0.7143(4) 0.4500(3) 0.9264(3) 0.0291(6) Uani 1 1 d . . . H2A H -0.7061 0.4856 0.8404 0.035 Uiso 1 1 calc R . . H2B H -0.7119 0.5267 0.9749 0.035 Uiso 1 1 calc R . . C3 C -0.9119(4) 0.4261(3) 0.9869(2) 0.0212(5) Uani 1 1 d . . . H3 H -0.9116 0.3756 1.0681 0.025 Uiso 1 1 calc R . . C4 C -0.9420(4) 0.3307(3) 0.9004(3) 0.0247(6) Uani 1 1 d . . . C5 C 0.2718(5) -0.1596(4) 0.7649(3) 0.0358(7) Uani 1 1 d . . . H5 H 0.2269 -0.1633 0.8535 0.043 Uiso 1 1 calc R . . C6 C 0.4335(5) -0.2777(4) 0.6985(3) 0.0418(8) Uani 1 1 d . . . H6 H 0.4939 -0.3585 0.7419 0.050 Uiso 1 1 calc R . . C7 C 0.5025(5) -0.2730(4) 0.5677(3) 0.0413(8) Uani 1 1 d . . . H7 H 0.6114 -0.3505 0.5215 0.050 Uiso 1 1 calc R . . C8 C 0.4081(4) -0.1511(4) 0.5042(3) 0.0330(7) Uani 1 1 d . . . C9 C 0.2440(4) -0.0382(3) 0.5796(2) 0.0249(6) Uani 1 1 d . . . C10 C 0.4733(5) -0.1372(4) 0.3693(3) 0.0394(8) Uani 1 1 d . . . H10 H 0.5808 -0.2129 0.3196 0.047 Uiso 1 1 calc R . . C11 C 0.3813(5) -0.0159(4) 0.3125(3) 0.0397(8) Uani 1 1 d . . . H11 H 0.4270 -0.0090 0.2241 0.048 Uiso 1 1 calc R . . C12 C 0.2149(5) 0.1024(4) 0.3852(3) 0.0324(7) Uani 1 1 d . . . C13 C 0.1450(4) 0.0904(3) 0.5191(3) 0.0250(6) Uani 1 1 d . . . C14 C -0.0994(5) 0.3191(4) 0.5394(3) 0.0406(8) Uani 1 1 d . . . H14 H -0.2076 0.3930 0.5906 0.049 Uiso 1 1 calc R . . C15 C -0.0378(6) 0.3409(4) 0.4083(3) 0.0473(9) Uani 1 1 d . . . H15 H -0.1027 0.4282 0.3735 0.057 Uiso 1 1 calc R . . C16 C 0.1186(5) 0.2327(4) 0.3311(3) 0.0436(8) Uani 1 1 d . . . H16 H 0.1609 0.2455 0.2433 0.052 Uiso 1 1 calc R . . N1 N 0.1776(3) -0.0417(3) 0.7089(2) 0.0276(5) Uani 1 1 d . . . N2 N -0.0114(4) 0.1987(3) 0.5945(2) 0.0273(5) Uani 1 1 d . . . O1 O -0.5560(4) 0.2059(3) 0.9868(3) 0.0609(8) Uani 1 1 d . . . O2 O -0.3703(3) 0.3191(2) 0.8453(2) 0.0335(5) Uani 1 1 d . . . O3 O -0.9803(3) 0.2159(2) 0.9469(2) 0.0350(5) Uani 1 1 d . . . O4 O -0.9365(4) 0.3677(3) 0.7892(2) 0.0414(6) Uani 1 1 d . . . O1W O -0.2009(4) 0.0105(3) 0.9216(2) 0.0399(6) Uani 1 1 d . . . H1B H -0.319(6) 0.062(4) 0.961(3) 0.0599 Uiso 1 1 d . . . H1A H -0.166(7) -0.079(6) 0.960(4) 0.0599 Uiso 1 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 Mn1 0.0184(2) 0.0258(2) 0.0233(2) -0.00340(15) -0.00430(15) -0.00448(17) C1 0.0171(13) 0.0288(15) 0.0307(15) -0.0027(11) -0.0057(10) -0.0045(12) C2 0.0199(14) 0.0233(15) 0.0402(16) -0.0036(12) -0.0061(11) -0.0051(12) C3 0.0173(13) 0.0211(14) 0.0228(13) -0.0003(10) -0.0066(9) -0.0036(11) C4 0.0133(12) 0.0223(14) 0.0326(16) -0.0065(11) -0.0054(10) 0.0006(11) C5 0.0312(17) 0.0402(19) 0.0322(16) 0.0079(13) -0.0065(12) -0.0130(14) C6 0.0295(17) 0.0318(18) 0.058(2) 0.0087(15) -0.0110(14) -0.0078(14) C7 0.0316(18) 0.0303(18) 0.051(2) -0.0096(14) -0.0018(14) -0.0055(14) C8 0.0265(15) 0.0333(17) 0.0384(17) -0.0105(13) -0.0043(12) -0.0118(13) C9 0.0225(14) 0.0272(15) 0.0233(13) -0.0046(10) -0.0014(10) -0.0106(12) C10 0.0273(16) 0.051(2) 0.0339(17) -0.0186(14) 0.0047(12) -0.0141(15) C11 0.0387(18) 0.061(2) 0.0227(15) -0.0091(14) -0.0008(12) -0.0268(17) C12 0.0322(16) 0.0474(19) 0.0248(15) 0.0003(13) -0.0090(11) -0.0221(15) C13 0.0250(14) 0.0288(15) 0.0257(14) 0.0004(11) -0.0076(10) -0.0150(12) C14 0.0366(19) 0.0383(19) 0.0430(19) 0.0059(14) -0.0153(14) -0.0077(15) C15 0.056(2) 0.045(2) 0.050(2) 0.0201(17) -0.0302(18) -0.0202(19) C16 0.047(2) 0.062(2) 0.0330(17) 0.0121(16) -0.0157(15) -0.0316(19) N1 0.0240(12) 0.0299(13) 0.0254(12) 0.0010(9) -0.0040(9) -0.0092(11) N2 0.0260(13) 0.0271(13) 0.0295(12) -0.0001(9) -0.0088(9) -0.0098(10) O1 0.0244(13) 0.0474(16) 0.0791(19) 0.0268(14) 0.0016(11) 0.0006(11) O2 0.0185(10) 0.0303(12) 0.0429(12) -0.0005(9) -0.0038(8) -0.0035(9) O3 0.0391(13) 0.0266(11) 0.0465(13) 0.0003(9) -0.0190(10) -0.0146(10) O4 0.0542(15) 0.0428(14) 0.0269(12) -0.0025(9) -0.0154(10) -0.0137(12) O1W 0.0262(13) 0.0288(13) 0.0535(15) 0.0098(11) -0.0045(10) -0.0067(10) _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 Mn1 O2 2.102(2) . ? Mn1 O1W 2.127(2) . ? Mn1 O3 2.135(2) 1_655 ? Mn1 N2 2.241(3) . ? Mn1 N1 2.288(3) . ? C1 O1 1.241(4) . ? C1 O2 1.272(3) . ? C1 C2 1.517(4) . ? C2 C3 1.532(4) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.521(4) . ? C3 C3 1.544(5) 2_367 ? C3 H3 0.9800 . ? C4 O4 1.240(4) . ? C4 O3 1.269(4) . ? C5 N1 1.328(4) . ? C5 C6 1.389(5) . ? C5 H5 0.9300 . ? C6 C7 1.373(5) . ? C6 H6 0.9300 . ? C7 C8 1.400(5) . ? C7 H7 0.9300 . ? C8 C9 1.405(4) . ? C8 C10 1.422(5) . ? C9 N1 1.355(4) . ? C9 C13 1.433(4) . ? C10 C11 1.347(5) . ? C10 H10 0.9300 . ? C11 C12 1.429(5) . ? C11 H11 0.9300 . ? C12 C16 1.399(5) . ? C12 C13 1.411(4) . ? C13 N2 1.358(4) . ? C14 N2 1.321(4) . ? C14 C15 1.392(5) . ? C14 H14 0.9300 . ? C15 C16 1.365(5) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? O3 Mn1 2.135(2) 1_455 ? O1W H1B 0.85(4) . ? O1W H1A 0.91(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 O2 Mn1 O1W 88.68(10) . . ? O2 Mn1 O3 103.00(9) . 1_655 ? O1W Mn1 O3 94.36(10) . 1_655 ? O2 Mn1 N2 93.11(8) . . ? O1W Mn1 N2 130.07(10) . . ? O3 Mn1 N2 133.23(9) 1_655 . ? O2 Mn1 N1 155.07(9) . . ? O1W Mn1 N1 84.91(10) . . ? O3 Mn1 N1 101.49(10) 1_655 . ? N2 Mn1 N1 73.15(9) . . ? O1 C1 O2 125.6(3) . . ? O1 C1 C2 118.6(3) . . ? O2 C1 C2 115.8(3) . . ? C1 C2 C3 114.5(2) . . ? C1 C2 H2A 108.6 . . ? C3 C2 H2A 108.6 . . ? C1 C2 H2B 108.6 . . ? C3 C2 H2B 108.6 . . ? H2A C2 H2B 107.6 . . ? C4 C3 C2 111.0(2) . . ? C4 C3 C3 108.0(3) . 2_367 ? C2 C3 C3 111.8(3) . 2_367 ? C4 C3 H3 108.7 . . ? C2 C3 H3 108.7 . . ? C3 C3 H3 108.7 2_367 . ? O4 C4 O3 121.2(3) . . ? O4 C4 C3 120.6(3) . . ? O3 C4 C3 118.1(2) . . ? N1 C5 C6 123.7(3) . . ? N1 C5 H5 118.1 . . ? C6 C5 H5 118.1 . . ? C7 C6 C5 118.8(3) . . ? C7 C6 H6 120.6 . . ? C5 C6 H6 120.6 . . ? C6 C7 C8 119.7(3) . . ? C6 C7 H7 120.2 . . ? C8 C7 H7 120.2 . . ? C7 C8 C9 117.3(3) . . ? C7 C8 C10 122.9(3) . . ? C9 C8 C10 119.8(3) . . ? N1 C9 C8 123.1(3) . . ? N1 C9 C13 117.5(2) . . ? C8 C9 C13 119.4(3) . . ? C11 C10 C8 120.8(3) . . ? C11 C10 H10 119.6 . . ? C8 C10 H10 119.6 . . ? C10 C11 C12 121.4(3) . . ? C10 C11 H11 119.3 . . ? C12 C11 H11 119.3 . . ? C16 C12 C13 117.5(3) . . ? C16 C12 C11 123.5(3) . . ? C13 C12 C11 119.0(3) . . ? N2 C13 C12 122.3(3) . . ? N2 C13 C9 118.1(2) . . ? C12 C13 C9 119.6(3) . . ? N2 C14 C15 123.2(3) . . ? N2 C14 H14 118.4 . . ? C15 C14 H14 118.4 . . ? C16 C15 C14 119.3(3) . . ? C16 C15 H15 120.3 . . ? C14 C15 H15 120.3 . . ? C15 C16 C12 119.5(3) . . ? C15 C16 H16 120.2 . . ? C12 C16 H16 120.2 . . ? C5 N1 C9 117.5(3) . . ? C5 N1 Mn1 127.5(2) . . ? C9 N1 Mn1 114.99(19) . . ? C14 N2 C13 118.2(3) . . ? C14 N2 Mn1 125.4(2) . . ? C13 N2 Mn1 116.18(18) . . ? C1 O2 Mn1 130.8(2) . . ? C4 O3 Mn1 101.08(18) . 1_455 ? Mn1 O1W H1B 105(2) . . ? Mn1 O1W H1A 142(3) . . ? H1B O1W H1A 110(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 C3 -15.8(4) . . . . ? O2 C1 C2 C3 164.2(2) . . . . ? C1 C2 C3 C4 -69.9(3) . . . . ? C1 C2 C3 C3 169.4(3) . . . 2_367 ? C2 C3 C4 O4 -56.5(3) . . . . ? C3 C3 C4 O4 66.4(4) 2_367 . . . ? C2 C3 C4 O3 126.2(3) . . . . ? C3 C3 C4 O3 -111.0(3) 2_367 . . . ? N1 C5 C6 C7 0.6(5) . . . . ? C5 C6 C7 C8 -0.6(5) . . . . ? C6 C7 C8 C9 -0.2(5) . . . . ? C6 C7 C8 C10 178.8(3) . . . . ? C7 C8 C9 N1 1.3(4) . . . . ? C10 C8 C9 N1 -177.8(3) . . . . ? C7 C8 C9 C13 178.7(3) . . . . ? C10 C8 C9 C13 -0.4(4) . . . . ? C7 C8 C10 C11 -178.1(3) . . . . ? C9 C8 C10 C11 0.9(5) . . . . ? C8 C10 C11 C12 -0.4(5) . . . . ? C10 C11 C12 C16 177.8(3) . . . . ? C10 C11 C12 C13 -0.7(5) . . . . ? C16 C12 C13 N2 1.0(4) . . . . ? C11 C12 C13 N2 179.5(3) . . . . ? C16 C12 C13 C9 -177.3(3) . . . . ? C11 C12 C13 C9 1.3(4) . . . . ? N1 C9 C13 N2 -1.5(4) . . . . ? C8 C9 C13 N2 -179.1(3) . . . . ? N1 C9 C13 C12 176.9(3) . . . . ? C8 C9 C13 C12 -0.7(4) . . . . ? N2 C14 C15 C16 1.1(6) . . . . ? C14 C15 C16 C12 -0.3(5) . . . . ? C13 C12 C16 C15 -0.6(5) . . . . ? C11 C12 C16 C15 -179.2(3) . . . . ? C6 C5 N1 C9 0.3(5) . . . . ? C6 C5 N1 Mn1 -177.4(2) . . . . ? C8 C9 N1 C5 -1.3(4) . . . . ? C13 C9 N1 C5 -178.8(3) . . . . ? C8 C9 N1 Mn1 176.7(2) . . . . ? C13 C9 N1 Mn1 -0.8(3) . . . . ? O2 Mn1 N1 C5 -121.6(3) . . . . ? O1W Mn1 N1 C5 -45.9(3) . . . . ? O3 Mn1 N1 C5 47.5(3) 1_655 . . . ? N2 Mn1 N1 C5 179.5(3) . . . . ? O2 Mn1 N1 C9 60.6(3) . . . . ? O1W Mn1 N1 C9 136.3(2) . . . . ? O3 Mn1 N1 C9 -130.3(2) 1_655 . . . ? N2 Mn1 N1 C9 1.68(19) . . . . ? C15 C14 N2 C13 -0.8(5) . . . . ? C15 C14 N2 Mn1 173.7(3) . . . . ? C12 C13 N2 C14 -0.2(4) . . . . ? C9 C13 N2 C14 178.1(3) . . . . ? C12 C13 N2 Mn1 -175.3(2) . . . . ? C9 C13 N2 Mn1 3.0(3) . . . . ? O2 Mn1 N2 C14 24.1(3) . . . . ? O1W Mn1 N2 C14 115.0(3) . . . . ? O3 Mn1 N2 C14 -87.1(3) 1_655 . . . ? N1 Mn1 N2 C14 -177.1(3) . . . . ? O2 Mn1 N2 C13 -161.3(2) . . . . ? O1W Mn1 N2 C13 -70.4(2) . . . . ? O3 Mn1 N2 C13 87.6(2) 1_655 . . . ? N1 Mn1 N2 C13 -2.46(19) . . . . ? O1 C1 O2 Mn1 -1.6(5) . . . . ? C2 C1 O2 Mn1 178.48(18) . . . . ? O1W Mn1 O2 C1 5.7(3) . . . . ? O3 Mn1 O2 C1 -88.5(3) 1_655 . . . ? N2 Mn1 O2 C1 135.8(3) . . . . ? N1 Mn1 O2 C1 80.6(3) . . . . ? O4 C4 O3 Mn1 -11.9(3) . . . 1_455 ? C3 C4 O3 Mn1 165.44(19) . . . 1_455 ? 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 O1W H1B O1 0.85(4) 1.79(4) 2.598(4) 158(3) . _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.468 _refine_diff_density_min -0.294 _refine_diff_density_rms 0.089 #===End data_compound-6 _database_code_depnum_ccdc_archive 'CCDC 648895' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H22 N4 O6.5 Zn' _chemical_formula_weight 463.77 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' Zn Zn 0.2839 1.4301 '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 11.268(9) _cell_length_b 13.002(1) _cell_length_c 14.379(1) _cell_angle_alpha 90.00 _cell_angle_beta 101.938(2) _cell_angle_gamma 90.00 _cell_volume 2061.1(30) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3163 _cell_measurement_theta_min 1.9 _cell_measurement_theta_max 27.2 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.184 _exptl_crystal_size_mid 0.121 _exptl_crystal_size_min 0.106 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.495 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 1.236 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.830 _exptl_absorpt_correction_T_max 0.882 _exptl_absorpt_process_details 'SADABS(Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 11905 _diffrn_reflns_av_R_equivalents 0.0456 _diffrn_reflns_av_sigmaI/netI 0.0577 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 27.20 _reflns_number_total 4497 _reflns_number_gt 3193 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97(Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _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^)+(0.0907P)^2^+0.3011P] 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 4497 _refine_ls_number_parameters 295 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0795 _refine_ls_R_factor_gt 0.0550 _refine_ls_wR_factor_ref 0.1623 _refine_ls_wR_factor_gt 0.1463 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.046 _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 Zn1 Zn 0.11982(4) 0.77112(3) 0.68566(3) 0.03620(17) Uani 1 1 d . . . C1 C 0.6928(3) 0.6175(3) 1.0620(3) 0.0408(9) Uani 1 1 d . . . C2 C 0.5797(3) 0.6380(3) 1.0035(3) 0.0430(9) Uani 1 1 d . . . C3 C 0.4778(4) 0.6408(4) 1.0439(4) 0.0600(12) Uani 1 1 d . . . H3 H 0.4024 0.6541 1.0053 0.072 Uiso 1 1 calc R . . C4 C 0.4856(4) 0.6245(4) 1.1392(4) 0.0669(14) Uani 1 1 d . . . H4 H 0.4160 0.6261 1.1645 0.080 Uiso 1 1 calc R . . C5 C 0.5969(5) 0.6057(4) 1.1973(3) 0.0686(15) Uani 1 1 d . . . H5 H 0.6033 0.5959 1.2622 0.082 Uiso 1 1 calc R . . C6 C 0.6988(4) 0.6015(4) 1.1581(3) 0.0561(12) Uani 1 1 d . . . H6 H 0.7736 0.5875 1.1974 0.067 Uiso 1 1 calc R . . C7 C 0.8085(3) 0.6094(3) 1.0259(3) 0.0433(9) Uani 1 1 d . . . H7A H 0.8016 0.6505 0.9688 0.052 Uiso 1 1 calc R . . H7B H 0.8750 0.6367 1.0734 0.052 Uiso 1 1 calc R . . C8 C 0.5667(4) 0.6578(5) 0.8983(3) 0.0678(14) Uani 1 1 d . . . H8A H 0.6387 0.6928 0.8876 0.081 Uiso 1 1 calc R . . H8B H 0.5607 0.5926 0.8650 0.081 Uiso 1 1 calc R . . C9 C 0.8389(3) 0.4642(3) 0.9185(3) 0.0381(8) Uani 1 1 d . . . H9 H 0.8253 0.5032 0.8631 0.046 Uiso 1 1 calc R . . C10 C 0.8779(4) 0.3384(3) 1.0165(3) 0.0485(10) Uani 1 1 d . . . H10 H 0.8959 0.2729 1.0414 0.058 Uiso 1 1 calc R . . C11 C 0.8614(4) 0.4212(3) 1.0676(3) 0.0497(10) Uani 1 1 d . . . H11 H 0.8664 0.4240 1.1329 0.060 Uiso 1 1 calc R . . C12 C 0.3591(4) 0.6930(4) 0.7946(3) 0.0517(10) Uani 1 1 d . . . H12 H 0.3481 0.6290 0.7651 0.062 Uiso 1 1 calc R . . C13 C 0.3311(4) 0.8477(4) 0.8362(3) 0.0570(11) Uani 1 1 d . . . H13 H 0.2951 0.9115 0.8398 0.068 Uiso 1 1 calc R . . C14 C 0.4400(4) 0.8190(4) 0.8853(3) 0.0642(13) Uani 1 1 d . . . H14 H 0.4927 0.8589 0.9292 0.077 Uiso 1 1 calc R . . C15 C 0.0172(4) 0.8974(3) 0.8028(3) 0.0424(9) Uani 1 1 d . . . C16 C -0.0438(3) 0.9169(3) 0.8857(3) 0.0408(9) Uani 1 1 d . . . H16A H -0.1275 0.9366 0.8615 0.049 Uiso 1 1 calc R . . H16B H -0.0439 0.8538 0.9216 0.049 Uiso 1 1 calc R . . C17 C 0.0187(3) 1.0002(3) 0.9510(2) 0.0365(8) Uani 1 1 d . . . H17 H 0.1062 0.9873 0.9622 0.044 Uiso 1 1 calc R . . C18 C -0.0047(4) 1.1085(3) 0.9054(3) 0.0468(10) Uani 1 1 d . . . N1 N 0.8644(3) 0.3633(2) 0.9227(2) 0.0384(7) Uani 1 1 d . . . N2 N 0.8357(3) 0.5009(2) 1.0044(2) 0.0359(7) Uani 1 1 d . . . N3 N 0.2805(3) 0.7663(3) 0.7789(2) 0.0438(8) Uani 1 1 d . . . N4 N 0.4599(3) 0.7202(3) 0.8592(3) 0.0549(10) Uani 1 1 d . . . O1 O 0.0053(3) 0.8067(2) 0.7676(2) 0.0519(7) Uani 1 1 d . . . O2 O 0.0756(3) 0.9649(2) 0.7734(2) 0.0620(8) Uani 1 1 d . . . O3 O -0.1111(3) 1.1275(2) 0.8624(2) 0.0604(8) Uani 1 1 d . . . O4 O 0.0776(4) 1.1718(3) 0.9155(3) 0.0733(10) Uani 1 1 d . . . O1W O 0.8162(4) 0.6622(4) 0.7771(3) 0.0879(12) Uani 1 1 d D . . H1A H 0.791(7) 0.626(5) 0.723(4) 0.132 Uiso 1 1 d D . . H1B H 0.872(5) 0.716(4) 0.779(6) 0.132 Uiso 1 1 d D . . O2W O 0.3150(7) 0.0998(7) 0.9741(7) 0.099(3) Uani 0.50 1 d PD . . H2B H 0.297(8) 0.136(6) 1.013(5) 0.148 Uiso 1 1 d D . . O3W O 0.6613(6) 0.0606(7) 0.9074(6) 0.083(2) Uani 0.50 1 d PD . . H3A H 0.588(3) 0.063(6) 0.902(5) 0.125 Uiso 1 1 d D . . O4W O 0.4265(8) 0.1058(8) 0.8396(8) 0.106(3) Uani 0.50 1 d PD . . H4A H 0.395(8) 0.094(7) 0.893(4) 0.158 Uiso 1 1 d 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 Zn1 0.0443(3) 0.0300(3) 0.0350(3) -0.00177(17) 0.00987(18) -0.00061(18) C1 0.0337(18) 0.038(2) 0.050(2) -0.0087(17) 0.0075(16) 0.0036(15) C2 0.0373(19) 0.045(2) 0.044(2) -0.0064(17) 0.0045(16) 0.0049(17) C3 0.035(2) 0.073(3) 0.069(3) -0.003(2) 0.004(2) 0.009(2) C4 0.054(3) 0.078(4) 0.076(3) 0.002(3) 0.031(2) 0.009(2) C5 0.076(3) 0.084(4) 0.049(3) 0.003(2) 0.022(2) 0.023(3) C6 0.050(2) 0.070(3) 0.046(2) -0.008(2) 0.0026(19) 0.015(2) C7 0.0350(19) 0.035(2) 0.060(3) -0.0094(18) 0.0083(17) -0.0007(15) C8 0.050(2) 0.096(4) 0.054(3) -0.002(3) 0.003(2) 0.028(3) C9 0.0401(19) 0.038(2) 0.036(2) 0.0018(16) 0.0077(15) 0.0012(16) C10 0.060(2) 0.045(2) 0.041(2) 0.0082(18) 0.0120(18) 0.0160(19) C11 0.063(3) 0.053(3) 0.034(2) 0.0038(18) 0.0113(18) 0.017(2) C12 0.053(2) 0.051(3) 0.052(3) -0.006(2) 0.012(2) -0.001(2) C13 0.059(3) 0.049(3) 0.058(3) -0.013(2) 0.000(2) 0.001(2) C14 0.059(3) 0.065(3) 0.064(3) -0.018(3) 0.000(2) -0.009(2) C15 0.049(2) 0.041(2) 0.035(2) -0.0054(17) 0.0042(16) 0.0005(18) C16 0.047(2) 0.039(2) 0.035(2) -0.0025(16) 0.0068(16) 0.0036(17) C17 0.0460(19) 0.035(2) 0.0283(18) 0.0026(14) 0.0078(15) 0.0115(16) C18 0.064(3) 0.044(2) 0.033(2) -0.0059(17) 0.0106(18) 0.006(2) N1 0.0423(16) 0.0355(18) 0.0373(17) 0.0005(13) 0.0079(13) 0.0041(14) N2 0.0319(14) 0.0335(17) 0.0422(17) -0.0064(13) 0.0077(12) 0.0026(12) N3 0.0395(17) 0.044(2) 0.0451(19) -0.0014(15) 0.0016(14) -0.0008(15) N4 0.049(2) 0.060(3) 0.051(2) -0.0056(18) -0.0010(17) 0.0020(17) O1 0.0602(17) 0.0468(17) 0.0518(17) -0.0155(14) 0.0186(14) -0.0013(14) O2 0.089(2) 0.0475(19) 0.0566(19) -0.0075(15) 0.0324(17) -0.0071(17) O3 0.072(2) 0.0501(19) 0.058(2) 0.0118(15) 0.0106(15) 0.0219(15) O4 0.098(3) 0.043(2) 0.074(2) 0.0102(17) 0.0084(19) -0.0132(19) O1W 0.085(3) 0.076(3) 0.109(3) 0.025(2) 0.033(3) -0.005(2) O2W 0.049(4) 0.077(6) 0.141(9) 0.033(5) -0.045(5) -0.029(4) O3W 0.053(4) 0.118(7) 0.076(5) 0.027(5) 0.008(4) 0.006(4) O4W 0.066(5) 0.102(8) 0.143(9) 0.017(7) 0.009(5) 0.012(5) _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 Zn1 O1 1.974(3) . ? Zn1 O3 1.986(3) 2_546 ? Zn1 N1 2.003(3) 2_656 ? Zn1 N3 2.018(3) . ? C1 C6 1.385(6) . ? C1 C2 1.400(5) . ? C1 C7 1.504(5) . ? C2 C3 1.389(6) . ? C2 C8 1.511(6) . ? C3 C4 1.372(7) . ? C3 H3 0.9300 . ? C4 C5 1.377(7) . ? C4 H4 0.9300 . ? C5 C6 1.381(7) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 N2 1.489(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 N4 1.463(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 N2 1.333(5) . ? C9 N1 1.342(5) . ? C9 H9 0.9300 . ? C10 C11 1.338(6) . ? C10 N1 1.365(5) . ? C10 H10 0.9300 . ? C11 N2 1.370(5) . ? C11 H11 0.9300 . ? C12 N3 1.289(6) . ? C12 N4 1.358(6) . ? C12 H12 0.9300 . ? C13 C14 1.336(6) . ? C13 N3 1.390(5) . ? C13 H13 0.9300 . ? C14 N4 1.370(6) . ? C14 H14 0.9300 . ? C15 O2 1.223(5) . ? C15 O1 1.279(5) . ? C15 C16 1.516(5) . ? C16 C17 1.509(5) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C17 1.551(7) 3_577 ? C17 C18 1.552(5) . ? C17 H17 0.9800 . ? C18 O4 1.226(5) . ? C18 O3 1.254(5) . ? N1 Zn1 2.003(3) 2_646 ? O3 Zn1 1.986(3) 2_556 ? O1W H1A 0.90(3) . ? O1W H1B 0.93(3) . ? O2W H2B 0.79(3) . ? O3W H3A 0.81(3) . ? O4W H4A 0.93(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 O1 Zn1 O3 115.88(13) . 2_546 ? O1 Zn1 N1 119.87(13) . 2_656 ? O3 Zn1 N1 107.35(13) 2_546 2_656 ? O1 Zn1 N3 102.62(13) . . ? O3 Zn1 N3 100.06(14) 2_546 . ? N1 Zn1 N3 108.87(13) 2_656 . ? C6 C1 C2 118.6(4) . . ? C6 C1 C7 117.8(3) . . ? C2 C1 C7 123.5(4) . . ? C3 C2 C1 118.8(4) . . ? C3 C2 C8 119.8(4) . . ? C1 C2 C8 121.5(4) . . ? C4 C3 C2 121.7(4) . . ? C4 C3 H3 119.1 . . ? C2 C3 H3 119.1 . . ? C3 C4 C5 119.7(4) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C4 C5 C6 119.3(5) . . ? C4 C5 H5 120.4 . . ? C6 C5 H5 120.4 . . ? C5 C6 C1 121.8(4) . . ? C5 C6 H6 119.1 . . ? C1 C6 H6 119.1 . . ? N2 C7 C1 111.6(3) . . ? N2 C7 H7A 109.3 . . ? C1 C7 H7A 109.3 . . ? N2 C7 H7B 109.3 . . ? C1 C7 H7B 109.3 . . ? H7A C7 H7B 108.0 . . ? N4 C8 C2 112.4(4) . . ? N4 C8 H8A 109.1 . . ? C2 C8 H8A 109.1 . . ? N4 C8 H8B 109.1 . . ? C2 C8 H8B 109.1 . . ? H8A C8 H8B 107.9 . . ? N2 C9 N1 110.8(3) . . ? N2 C9 H9 124.6 . . ? N1 C9 H9 124.6 . . ? C11 C10 N1 110.6(4) . . ? C11 C10 H10 124.7 . . ? N1 C10 H10 124.7 . . ? C10 C11 N2 106.2(3) . . ? C10 C11 H11 126.9 . . ? N2 C11 H11 126.9 . . ? N3 C12 N4 112.0(4) . . ? N3 C12 H12 124.0 . . ? N4 C12 H12 124.0 . . ? C14 C13 N3 108.7(4) . . ? C14 C13 H13 125.6 . . ? N3 C13 H13 125.6 . . ? C13 C14 N4 107.5(4) . . ? C13 C14 H14 126.2 . . ? N4 C14 H14 126.2 . . ? O2 C15 O1 123.0(4) . . ? O2 C15 C16 121.1(4) . . ? O1 C15 C16 115.9(4) . . ? C17 C16 C15 112.3(3) . . ? C17 C16 H16A 109.1 . . ? C15 C16 H16A 109.1 . . ? C17 C16 H16B 109.1 . . ? C15 C16 H16B 109.1 . . ? H16A C16 H16B 107.9 . . ? C16 C17 C17 112.5(4) . 3_577 ? C16 C17 C18 111.8(3) . . ? C17 C17 C18 109.5(4) 3_577 . ? C16 C17 H17 107.6 . . ? C17 C17 H17 107.6 3_577 . ? C18 C17 H17 107.6 . . ? O4 C18 O3 123.2(4) . . ? O4 C18 C17 120.0(4) . . ? O3 C18 C17 116.7(4) . . ? C9 N1 C10 104.9(3) . . ? C9 N1 Zn1 127.1(3) . 2_646 ? C10 N1 Zn1 128.1(3) . 2_646 ? C9 N2 C11 107.5(3) . . ? C9 N2 C7 125.3(3) . . ? C11 N2 C7 127.1(3) . . ? C12 N3 C13 106.0(4) . . ? C12 N3 Zn1 129.0(3) . . ? C13 N3 Zn1 124.9(3) . . ? C12 N4 C14 105.7(4) . . ? C12 N4 C8 128.5(4) . . ? C14 N4 C8 125.7(4) . . ? C15 O1 Zn1 115.1(3) . . ? C18 O3 Zn1 109.3(3) . 2_556 ? H1A O1W H1B 121(7) . . ? 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 C6 C1 C2 C3 -0.5(6) . . . . ? C7 C1 C2 C3 178.1(4) . . . . ? C6 C1 C2 C8 179.1(4) . . . . ? C7 C1 C2 C8 -2.4(7) . . . . ? C1 C2 C3 C4 0.3(7) . . . . ? C8 C2 C3 C4 -179.2(5) . . . . ? C2 C3 C4 C5 0.6(8) . . . . ? C3 C4 C5 C6 -1.3(9) . . . . ? C4 C5 C6 C1 1.2(8) . . . . ? C2 C1 C6 C5 -0.2(7) . . . . ? C7 C1 C6 C5 -178.9(4) . . . . ? C6 C1 C7 N2 84.7(5) . . . . ? C2 C1 C7 N2 -93.9(5) . . . . ? C3 C2 C8 N4 25.1(7) . . . . ? C1 C2 C8 N4 -154.5(4) . . . . ? N1 C10 C11 N2 0.5(5) . . . . ? N3 C13 C14 N4 0.5(6) . . . . ? O2 C15 C16 C17 -26.2(5) . . . . ? O1 C15 C16 C17 152.7(3) . . . . ? C15 C16 C17 C17 -163.8(4) . . . 3_577 ? C15 C16 C17 C18 72.6(4) . . . . ? C16 C17 C18 O4 -139.8(4) . . . . ? C17 C17 C18 O4 94.8(5) 3_577 . . . ? C16 C17 C18 O3 43.0(5) . . . . ? C17 C17 C18 O3 -82.4(5) 3_577 . . . ? N2 C9 N1 C10 -0.4(4) . . . . ? N2 C9 N1 Zn1 -179.9(2) . . . 2_646 ? C11 C10 N1 C9 -0.1(5) . . . . ? C11 C10 N1 Zn1 179.4(3) . . . 2_646 ? N1 C9 N2 C11 0.7(4) . . . . ? N1 C9 N2 C7 -179.2(3) . . . . ? C10 C11 N2 C9 -0.7(5) . . . . ? C10 C11 N2 C7 179.1(3) . . . . ? C1 C7 N2 C9 115.3(4) . . . . ? C1 C7 N2 C11 -64.5(5) . . . . ? N4 C12 N3 C13 0.0(5) . . . . ? N4 C12 N3 Zn1 176.5(3) . . . . ? C14 C13 N3 C12 -0.3(5) . . . . ? C14 C13 N3 Zn1 -177.0(3) . . . . ? O1 Zn1 N3 C12 125.7(4) . . . . ? O3 Zn1 N3 C12 6.1(4) 2_546 . . . ? N1 Zn1 N3 C12 -106.3(4) 2_656 . . . ? O1 Zn1 N3 C13 -58.4(4) . . . . ? O3 Zn1 N3 C13 -178.1(4) 2_546 . . . ? N1 Zn1 N3 C13 69.6(4) 2_656 . . . ? N3 C12 N4 C14 0.3(5) . . . . ? N3 C12 N4 C8 177.5(4) . . . . ? C13 C14 N4 C12 -0.5(6) . . . . ? C13 C14 N4 C8 -177.8(5) . . . . ? C2 C8 N4 C12 -114.4(5) . . . . ? C2 C8 N4 C14 62.3(7) . . . . ? O2 C15 O1 Zn1 15.1(5) . . . . ? C16 C15 O1 Zn1 -163.8(2) . . . . ? O3 Zn1 O1 C15 175.8(3) 2_546 . . . ? N1 Zn1 O1 C15 -52.9(3) 2_656 . . . ? N3 Zn1 O1 C15 67.8(3) . . . . ? O4 C18 O3 Zn1 1.0(5) . . . 2_556 ? C17 C18 O3 Zn1 178.1(2) . . . 2_556 ? 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 O3W H3A O4W 0.81(3) 1.94(4) 2.689(11) 154(8) . O1W H1A O4W 0.90(3) 2.44(7) 2.989(10) 119(6) 2_656 O1W H1B O1 0.93(3) 1.95(3) 2.865(5) 167(7) 1_655 _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.932 _refine_diff_density_min -0.574 _refine_diff_density_rms 0.091 #===End data_compound-7 _database_code_depnum_ccdc_archive 'CCDC 648896' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H12 N2 O5 Zn' _chemical_formula_weight 317.60 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' Zn Zn 0.2839 1.4301 '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 10.758(7) _cell_length_b 7.158(4) _cell_length_c 16.4000(10) _cell_angle_alpha 90.00 _cell_angle_beta 98.9220(10) _cell_angle_gamma 90.00 _cell_volume 1247.6(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2371 _cell_measurement_theta_min 1.9 _cell_measurement_theta_max 28.6 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.218 _exptl_crystal_size_mid 0.154 _exptl_crystal_size_min 0.112 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.691 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 648 _exptl_absorpt_coefficient_mu 1.986 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.702 _exptl_absorpt_correction_T_max 0.806 _exptl_absorpt_process_details 'SADABS(Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 7451 _diffrn_reflns_av_R_equivalents 0.0261 _diffrn_reflns_av_sigmaI/netI 0.0338 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 28.64 _reflns_number_total 2964 _reflns_number_gt 2371 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97(Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _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^)+(0.0671P)^2^] 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 2964 _refine_ls_number_parameters 178 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0497 _refine_ls_R_factor_gt 0.0331 _refine_ls_wR_factor_ref 0.1165 _refine_ls_wR_factor_gt 0.0903 _refine_ls_goodness_of_fit_ref 1.126 _refine_ls_restrained_S_all 1.126 _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 Zn1 Zn 0.11113(3) -0.09267(4) 0.698090(19) 0.02648(14) Uani 1 1 d . . . C1 C 0.0427(3) -0.3819(4) 0.60575(17) 0.0304(7) Uani 1 1 d . . . C2 C -0.0272(3) -0.5125(4) 0.54093(16) 0.0264(6) Uani 1 1 d . . . H2 H -0.1162 -0.4772 0.5312 0.032 Uiso 1 1 calc R . . C3 C -0.0166(3) -0.7147(4) 0.57067(16) 0.0316(6) Uani 1 1 d . . . H3A H -0.0762 -0.7907 0.5345 0.038 Uiso 1 1 calc R . . H3B H 0.0672 -0.7607 0.5672 0.038 Uiso 1 1 calc R . . C4 C -0.0416(3) -0.7361(4) 0.65795(16) 0.0253(6) Uani 1 1 d . . . C5 C 0.3357(3) 0.1355(4) 0.6825(2) 0.0360(7) Uani 1 1 d . . . H5 H 0.3040 0.2358 0.7089 0.043 Uiso 1 1 calc R . . C6 C 0.3556(3) -0.1342(5) 0.6272(2) 0.0411(8) Uani 1 1 d . . . H6 H 0.3391 -0.2559 0.6087 0.049 Uiso 1 1 calc R . . C7 C 0.4592(3) -0.0352(5) 0.6193(2) 0.0449(8) Uani 1 1 d . . . H7 H 0.5266 -0.0748 0.5943 0.054 Uiso 1 1 calc R . . C8 C 0.5309(4) 0.2955(5) 0.6553(2) 0.0478(9) Uani 1 1 d . . . H8A H 0.6173 0.2527 0.6679 0.057 Uiso 1 1 calc R . . H8B H 0.5161 0.3816 0.6985 0.057 Uiso 1 1 calc R . . C9 C 0.5129(3) 0.3980(4) 0.5731(2) 0.0343(7) Uani 1 1 d . . . C10 C 0.4052(3) 0.3845(5) 0.5154(2) 0.0481(9) Uani 1 1 d . . . H10 H 0.3404 0.3058 0.5254 0.058 Uiso 1 1 calc R . . C11 C 0.3925(3) 0.4856(5) 0.4436(2) 0.0444(8) Uani 1 1 d . . . H11 H 0.3190 0.4753 0.4057 0.053 Uiso 1 1 calc R . . N1 N 0.2773(2) -0.0254(4) 0.66722(15) 0.0311(5) Uani 1 1 d . . . N2 N 0.4466(3) 0.1356(4) 0.65511(17) 0.0371(6) Uani 1 1 d . . . O1 O -0.0051(2) -0.2223(3) 0.61248(12) 0.0393(5) Uani 1 1 d . . . O2 O 0.1437(2) -0.4316(3) 0.64713(14) 0.0416(6) Uani 1 1 d . . . O3 O -0.1222(2) -0.6295(3) 0.68199(12) 0.0294(4) Uani 1 1 d . . . O4 O 0.0178(2) -0.8531(3) 0.70497(12) 0.0358(5) Uani 1 1 d . . . O1W O -0.2374(3) -0.0833(5) 0.6816(2) 0.0724(10) Uani 1 1 d D . . H1A H -0.178(5) -0.152(7) 0.662(3) 0.109 Uiso 1 1 d D . . H1B H -0.214(5) 0.015(6) 0.657(3) 0.109 Uiso 1 1 d 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 Zn1 0.0310(2) 0.0300(2) 0.0198(2) -0.00116(12) 0.00833(13) -0.00131(13) C1 0.0461(19) 0.0324(16) 0.0149(13) 0.0010(11) 0.0123(12) -0.0090(13) C2 0.0347(15) 0.0279(14) 0.0182(13) -0.0003(11) 0.0090(11) -0.0039(12) C3 0.0500(18) 0.0269(14) 0.0205(13) -0.0025(11) 0.0129(12) -0.0037(13) C4 0.0349(15) 0.0221(13) 0.0198(12) -0.0047(10) 0.0072(11) -0.0071(11) C5 0.0400(18) 0.0327(16) 0.0373(17) -0.0015(13) 0.0122(14) -0.0008(14) C6 0.0436(19) 0.0367(17) 0.047(2) -0.0067(15) 0.0207(16) -0.0005(15) C7 0.0401(19) 0.0501(19) 0.049(2) -0.0027(17) 0.0223(16) 0.0022(16) C8 0.045(2) 0.053(2) 0.044(2) 0.0104(17) 0.0022(15) -0.0206(17) C9 0.0324(16) 0.0357(17) 0.0355(17) 0.0022(13) 0.0075(13) -0.0049(12) C10 0.0375(19) 0.059(2) 0.046(2) 0.0144(17) -0.0004(15) -0.0191(16) C11 0.0325(18) 0.055(2) 0.0424(19) 0.0093(17) -0.0027(14) -0.0166(16) N1 0.0330(14) 0.0310(13) 0.0319(13) -0.0014(11) 0.0131(10) -0.0013(11) N2 0.0354(15) 0.0422(15) 0.0343(14) 0.0046(12) 0.0075(11) -0.0080(12) O1 0.0644(16) 0.0294(11) 0.0254(11) -0.0054(9) 0.0106(10) -0.0053(11) O2 0.0439(14) 0.0478(14) 0.0324(12) -0.0042(10) 0.0039(10) -0.0102(11) O3 0.0364(12) 0.0326(11) 0.0200(10) 0.0005(8) 0.0068(8) 0.0053(9) O4 0.0509(14) 0.0332(11) 0.0249(11) 0.0015(9) 0.0109(10) 0.0124(10) O1W 0.0465(18) 0.076(2) 0.093(3) 0.0149(18) 0.0042(17) -0.0107(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 Zn1 O1 1.962(2) . ? Zn1 O3 1.9695(19) 2_556 ? Zn1 N1 1.991(3) . ? Zn1 O4 1.999(2) 1_565 ? C1 O2 1.240(4) . ? C1 O1 1.264(4) . ? C1 C2 1.524(4) . ? C2 C3 1.526(4) . ? C2 C2 1.555(5) 3_546 ? C2 H2 0.9800 . ? C3 C4 1.505(4) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 O4 1.245(3) . ? C4 O3 1.263(3) . ? C5 N1 1.317(4) . ? C5 N2 1.339(4) . ? C5 H5 0.9300 . ? C6 C7 1.345(5) . ? C6 N1 1.385(4) . ? C6 H6 0.9300 . ? C7 N2 1.372(4) . ? C7 H7 0.9300 . ? C8 N2 1.460(4) . ? C8 C9 1.521(4) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C11 1.375(4) 3_666 ? C9 C10 1.381(5) . ? C10 C11 1.372(5) . ? C10 H10 0.9300 . ? C11 C9 1.375(4) 3_666 ? C11 H11 0.9300 . ? O3 Zn1 1.9695(19) 2_546 ? O4 Zn1 1.999(2) 1_545 ? O1W H1A 0.91(3) . ? O1W H1B 0.86(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 O1 Zn1 O3 125.75(9) . 2_556 ? O1 Zn1 N1 115.45(10) . . ? O3 Zn1 N1 111.64(10) 2_556 . ? O1 Zn1 O4 100.16(10) . 1_565 ? O3 Zn1 O4 90.67(8) 2_556 1_565 ? N1 Zn1 O4 106.58(10) . 1_565 ? O2 C1 O1 123.0(3) . . ? O2 C1 C2 120.1(3) . . ? O1 C1 C2 116.9(3) . . ? C1 C2 C3 110.8(2) . . ? C1 C2 C2 108.7(3) . 3_546 ? C3 C2 C2 111.5(3) . 3_546 ? C1 C2 H2 108.6 . . ? C3 C2 H2 108.6 . . ? C2 C2 H2 108.6 3_546 . ? C4 C3 C2 112.7(2) . . ? C4 C3 H3A 109.1 . . ? C2 C3 H3A 109.1 . . ? C4 C3 H3B 109.1 . . ? C2 C3 H3B 109.1 . . ? H3A C3 H3B 107.8 . . ? O4 C4 O3 121.6(2) . . ? O4 C4 C3 120.5(3) . . ? O3 C4 C3 117.9(3) . . ? N1 C5 N2 111.1(3) . . ? N1 C5 H5 124.5 . . ? N2 C5 H5 124.5 . . ? C7 C6 N1 108.9(3) . . ? C7 C6 H6 125.6 . . ? N1 C6 H6 125.6 . . ? C6 C7 N2 106.8(3) . . ? C6 C7 H7 126.6 . . ? N2 C7 H7 126.6 . . ? N2 C8 C9 112.5(3) . . ? N2 C8 H8A 109.1 . . ? C9 C8 H8A 109.1 . . ? N2 C8 H8B 109.1 . . ? C9 C8 H8B 109.1 . . ? H8A C8 H8B 107.8 . . ? C11 C9 C10 118.3(3) 3_666 . ? C11 C9 C8 118.2(3) 3_666 . ? C10 C9 C8 123.5(3) . . ? C11 C10 C9 120.8(3) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C10 C11 C9 120.9(3) . 3_666 ? C10 C11 H11 119.6 . . ? C9 C11 H11 119.6 3_666 . ? C5 N1 C6 106.0(3) . . ? C5 N1 Zn1 125.7(2) . . ? C6 N1 Zn1 128.4(2) . . ? C5 N2 C7 107.2(3) . . ? C5 N2 C8 125.8(3) . . ? C7 N2 C8 126.6(3) . . ? C1 O1 Zn1 105.5(2) . . ? C4 O3 Zn1 117.04(18) . 2_546 ? C4 O4 Zn1 139.07(18) . 1_545 ? H1A O1W H1B 90(5) . . ? 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 O2 C1 C2 C3 37.7(3) . . . . ? O1 C1 C2 C3 -144.6(2) . . . . ? O2 C1 C2 C2 -85.1(4) . . . 3_546 ? O1 C1 C2 C2 92.6(4) . . . 3_546 ? C1 C2 C3 C4 46.3(3) . . . . ? C2 C2 C3 C4 167.5(3) 3_546 . . . ? C2 C3 C4 O4 -144.3(3) . . . . ? C2 C3 C4 O3 34.3(4) . . . . ? N1 C6 C7 N2 0.6(4) . . . . ? N2 C8 C9 C11 -161.5(3) . . . 3_666 ? N2 C8 C9 C10 20.4(5) . . . . ? C11 C9 C10 C11 -0.5(7) 3_666 . . . ? C8 C9 C10 C11 177.6(4) . . . . ? C9 C10 C11 C9 0.5(7) . . . 3_666 ? N2 C5 N1 C6 -0.3(4) . . . . ? N2 C5 N1 Zn1 178.9(2) . . . . ? C7 C6 N1 C5 -0.2(4) . . . . ? C7 C6 N1 Zn1 -179.4(2) . . . . ? O1 Zn1 N1 C5 136.4(3) . . . . ? O3 Zn1 N1 C5 -71.3(3) 2_556 . . . ? O4 Zn1 N1 C5 26.2(3) 1_565 . . . ? O1 Zn1 N1 C6 -44.5(3) . . . . ? O3 Zn1 N1 C6 107.8(3) 2_556 . . . ? O4 Zn1 N1 C6 -154.7(3) 1_565 . . . ? N1 C5 N2 C7 0.7(4) . . . . ? N1 C5 N2 C8 174.4(3) . . . . ? C6 C7 N2 C5 -0.7(4) . . . . ? C6 C7 N2 C8 -174.4(3) . . . . ? C9 C8 N2 C5 -95.9(4) . . . . ? C9 C8 N2 C7 76.7(5) . . . . ? O2 C1 O1 Zn1 -0.7(3) . . . . ? C2 C1 O1 Zn1 -178.40(18) . . . . ? O3 Zn1 O1 C1 -78.8(2) 2_556 . . . ? N1 Zn1 O1 C1 69.0(2) . . . . ? O4 Zn1 O1 C1 -177.02(17) 1_565 . . . ? O4 C4 O3 Zn1 20.2(3) . . . 2_546 ? C3 C4 O3 Zn1 -158.3(2) . . . 2_546 ? O3 C4 O4 Zn1 157.4(2) . . . 1_545 ? C3 C4 O4 Zn1 -24.2(5) . . . 1_545 ? 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 O1W H1A O1 0.91(3) 2.20(3) 3.066(4) 160(6) . _diffrn_measured_fraction_theta_max 0.923 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.706 _refine_diff_density_min -0.780 _refine_diff_density_rms 0.308 #===End data_compound-8 _database_code_depnum_ccdc_archive 'CCDC 648897' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H19 N4 O5 Zn' _chemical_formula_weight 388.70 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' Zn Zn 0.2839 1.4301 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.4244(17) _cell_length_b 17.647(4) _cell_length_c 11.247(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.33(3) _cell_angle_gamma 90.00 _cell_volume 1619.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2934 _cell_measurement_theta_min 3.4 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.594 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 804 _exptl_absorpt_coefficient_mu 1.549 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.81 _exptl_absorpt_correction_T_max 0.82 _exptl_absorpt_process_details 'SADABS(Sheldrick, 1996)' _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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15450 _diffrn_reflns_av_R_equivalents 0.0535 _diffrn_reflns_av_sigmaI/netI 0.0443 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.40 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3700 _reflns_number_gt 2861 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97(Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _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^)+(0.0639P)^2^+2.1769P] 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 3700 _refine_ls_number_parameters 277 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0686 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.1316 _refine_ls_wR_factor_gt 0.1214 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.118 _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 Zn1 Zn 0.84017(5) 0.01310(2) 0.75355(3) 0.02072(14) Uani 1 1 d . . . C1' C 0.6903(13) 0.4168(6) -0.0340(9) 0.050(2) Uiso 0.50 1 d PD . . C1 C 0.7968(11) 0.4410(4) -0.0004(6) 0.0336(18) Uani 0.50 1 d PD . . C2' C 0.8562(16) 0.3221(8) -0.0499(13) 0.036(4) Uiso 0.50 1 d P . . C2 C 0.9024(16) 0.3372(7) -0.0309(10) 0.036(2) Uani 0.50 1 d P . . C3 C 0.8828(14) 0.3816(5) -0.1337(8) 0.041(2) Uani 0.50 1 d PD . . C3' C 0.8105(13) 0.3615(6) -0.1529(9) 0.037(2) Uiso 0.50 1 d PD . . C4 C 0.9044(14) 0.3553(6) 0.1806(7) 0.050(3) Uani 0.50 1 d P . . C4' C 0.719(2) 0.3114(9) 0.1213(15) 0.086(4) Uiso 0.50 1 d P . . C5' C 0.8585(15) 0.2898(7) 0.2193(12) 0.048(3) Uiso 0.50 1 d P . . C5 C 0.7880(15) 0.2965(9) 0.2103(10) 0.075(5) Uani 0.50 1 d P . . C6 C 0.7841(13) 0.1191(5) 0.5362(7) 0.0332(18) Uani 0.50 1 d P . . C6' C 0.8944(12) 0.1177(5) 0.5587(8) 0.0322(17) Uani 0.50 1 d P . . C7 C 0.8203(6) 0.2341(3) 0.6093(4) 0.0419(10) Uani 1 1 d . . . C8 C 0.8225(6) 0.1832(2) 0.6974(4) 0.0397(10) Uani 1 1 d . . . H8 H 0.8167 0.1957 0.7765 0.048 Uiso 1 1 calc R . . C9' C 0.7241(13) 0.2215(7) 0.3761(9) 0.061(3) Uani 0.50 1 d P . . C9 C 0.9365(13) 0.2218(6) 0.4157(9) 0.050(2) Uani 0.50 1 d P . . C10' C 0.7908(16) 0.2498(8) 0.3202(12) 0.060(3) Uiso 0.50 1 d P . . C10 C 0.8544(11) 0.2697(5) 0.3453(8) 0.0323(18) Uiso 0.50 1 d P . . C11 C 0.6875(4) -0.0198(2) 0.9349(3) 0.0246(7) Uani 1 1 d . . . C12 C 0.5908(4) -0.0090(2) 1.0318(3) 0.0256(8) Uani 1 1 d . . . H12 H 0.5916 -0.0579 1.0732 0.031 Uiso 1 1 calc R . . C13 C 0.6659(5) 0.0479(3) 1.1295(4) 0.0390(10) Uani 1 1 d . . . H13A H 0.5926 0.0551 1.1828 0.047 Uiso 1 1 calc R . . H13B H 0.6757 0.0961 1.0905 0.047 Uiso 1 1 calc R . . C14 C 0.8340(5) 0.0249(3) 1.2074(4) 0.0349(9) Uani 1 1 d . . . N1 N 0.7768(15) 0.4408(6) -0.1218(10) 0.021(2) Uani 0.50 1 d P . . N1' N 0.7484(15) 0.4290(7) -0.1324(12) 0.019(3) Uiso 0.50 1 d P . . N2' N 0.7788(12) 0.3542(6) 0.0215(9) 0.049(2) Uiso 0.50 1 d P . . N2 N 0.8568(9) 0.3741(4) 0.0486(5) 0.0261(14) Uani 0.50 1 d P . . N3 N 0.8339(4) 0.11129(18) 0.6589(3) 0.0316(7) Uani 1 1 d . . . N4 N 0.8878(11) 0.1910(4) 0.5226(6) 0.0322(15) Uani 0.50 1 d P . . N4' N 0.7771(11) 0.1931(4) 0.5062(7) 0.0373(17) Uani 0.50 1 d P . . O1 O 0.7116(3) 0.03855(17) 0.8756(2) 0.0326(6) Uani 1 1 d . . . O2 O 0.7305(4) -0.08413(17) 0.9139(3) 0.0403(7) Uani 1 1 d . . . O3 O 0.9380(3) 0.00644(18) 1.1489(2) 0.0383(7) Uani 1 1 d . . . O4 O 0.8623(4) 0.0253(3) 1.3197(3) 0.0609(11) Uani 1 1 d . . . O1W O 1.0407(5) -0.1534(2) 0.9974(4) 0.0652(11) Uani 1 1 d D . . H1 H 0.947(6) -0.132(4) 0.966(6) 0.098 Uiso 1 1 d D . . H2 H 1.123(7) -0.121(3) 1.023(6) 0.098 Uiso 1 1 d 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 Zn1 0.0226(2) 0.0227(2) 0.0168(2) -0.00034(16) 0.00476(14) -0.00047(16) C1 0.051(5) 0.031(4) 0.019(3) 0.007(3) 0.011(3) 0.009(4) C2 0.038(6) 0.039(6) 0.029(5) 0.010(5) 0.004(5) 0.013(5) C3 0.058(7) 0.036(5) 0.030(5) 0.009(4) 0.015(4) 0.013(5) C4 0.079(7) 0.050(6) 0.015(4) 0.014(4) 0.000(4) -0.013(5) C5 0.036(6) 0.143(13) 0.045(6) 0.033(8) 0.006(5) 0.010(7) C6 0.046(6) 0.035(5) 0.021(4) 0.004(3) 0.013(4) 0.000(4) C6' 0.038(5) 0.028(4) 0.031(4) 0.007(3) 0.009(4) 0.005(4) C7 0.059(3) 0.033(2) 0.033(2) 0.0039(18) 0.011(2) 0.003(2) C8 0.064(3) 0.030(2) 0.030(2) 0.0017(17) 0.0206(19) 0.007(2) C9' 0.056(7) 0.090(9) 0.038(5) 0.038(5) 0.011(5) -0.012(6) C9 0.060(6) 0.049(6) 0.047(5) 0.020(5) 0.024(5) 0.003(5) C11 0.0185(16) 0.036(2) 0.0182(15) -0.0030(15) 0.0030(12) -0.0016(14) C12 0.0199(17) 0.039(2) 0.0176(15) -0.0030(15) 0.0043(13) 0.0011(15) C13 0.029(2) 0.058(3) 0.031(2) -0.015(2) 0.0094(16) 0.0031(19) C14 0.027(2) 0.055(3) 0.0233(17) -0.0092(18) 0.0058(15) -0.0083(17) N1 0.025(5) 0.016(5) 0.018(4) -0.004(3) 0.000(3) -0.005(4) N2 0.038(4) 0.019(3) 0.017(3) 0.006(2) -0.001(3) -0.006(3) N3 0.047(2) 0.0272(17) 0.0212(15) 0.0032(13) 0.0101(14) 0.0011(14) N4 0.044(5) 0.033(4) 0.023(3) 0.002(3) 0.015(3) 0.002(3) N4' 0.039(4) 0.041(4) 0.032(4) 0.016(3) 0.008(3) -0.006(3) O1 0.0337(15) 0.0415(16) 0.0253(13) 0.0024(12) 0.0122(11) 0.0023(12) O2 0.0454(18) 0.0339(16) 0.0444(17) -0.0141(13) 0.0162(14) 0.0014(13) O3 0.0238(14) 0.069(2) 0.0217(13) -0.0014(13) 0.0041(10) 0.0081(13) O4 0.046(2) 0.116(3) 0.0211(15) -0.0103(17) 0.0077(13) 0.003(2) O1W 0.071(3) 0.038(2) 0.078(3) 0.0094(19) 0.001(2) 0.0004(18) _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 Zn1 O3 1.949(3) 3_757 ? Zn1 O1 1.999(3) . ? Zn1 N1 2.017(11) 2_645 ? Zn1 N1' 2.028(14) 2_645 ? Zn1 N3 2.028(3) . ? C1' C1 0.982(13) . ? C1' N1' 1.333(17) . ? C1' N2' 1.391(14) . ? C1' N1 1.429(16) . ? C1' N2 1.659(12) . ? C1 N1 1.335(13) . ? C1 N2 1.347(10) . ? C1 N1' 1.455(15) . ? C1 N2' 1.564(13) . ? C2' N2' 1.284(18) . ? C2' C3' 1.324(18) . ? C2' N2 1.437(16) . ? C2' C3 1.464(17) . ? C2 N2 1.242(14) . ? C2 N2' 1.351(15) . ? C2 C3 1.372(13) . ? C2 C3' 1.463(14) . ? C3 C3' 0.691(12) . ? C3 N1 1.402(15) . ? C3 N1' 1.411(17) . ? C3' N1' 1.343(17) . ? C3' N1 1.486(15) . ? C4 C5' 1.327(15) . ? C4 N2 1.476(9) . ? C4 C5 1.521(16) . ? C4 N2' 1.840(12) . ? C4' C5 1.057(17) . ? C4' C5' 1.447(19) . ? C4' N2' 1.537(17) . ? C4' N2 1.924(17) . ? C5' C5 0.590(14) . ? C5' C10 1.469(15) . ? C5' C10' 1.559(18) . ? C5 C10' 1.481(15) . ? C5 C10 1.556(12) . ? C6 C6' 0.901(11) . ? C6 N3 1.346(8) . ? C6 N4' 1.347(11) . ? C6 N4 1.569(12) . ? C6' N3 1.351(9) . ? C6' N4 1.353(11) . ? C6' N4' 1.676(12) . ? C7 N4' 1.338(9) . ? C7 N4 1.458(8) . ? C8 N3 1.351(5) . ? C8 H8 0.9300 . ? C9' C10' 1.066(15) . ? C9' C10 1.496(13) . ? C9' N4' 1.506(11) . ? C9' N4 1.945(12) . ? C9 C10 1.245(13) . ? C9 N4 1.468(11) . ? C9 C10' 1.500(16) . ? C9 N4' 1.942(12) . ? C10' C10 0.644(13) . ? C11 O2 1.232(5) . ? C11 O1 1.271(5) . ? C11 C12 1.525(5) . ? C12 C13 1.506(5) . ? C12 C12 1.553(7) 3_657 ? C12 H12 0.9800 . ? C13 C14 1.525(6) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 O4 1.226(5) . ? C14 O3 1.262(5) . ? N1 Zn1 2.017(11) 2_655 ? N1' Zn1 2.028(14) 2_655 ? N2' N2 0.740(9) . ? N4 N4' 0.906(9) . ? O3 Zn1 1.949(3) 3_757 ? O1W H1 0.87(3) . ? O1W H2 0.89(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 O3 Zn1 O1 105.09(11) 3_757 . ? O3 Zn1 N1 121.8(3) 3_757 2_645 ? O1 Zn1 N1 113.4(4) . 2_645 ? O3 Zn1 N1' 113.0(3) 3_757 2_645 ? O1 Zn1 N1' 117.0(4) . 2_645 ? N1 Zn1 N1' 9.0(5) 2_645 2_645 ? O3 Zn1 N3 110.08(14) 3_757 . ? O1 Zn1 N3 102.75(13) . . ? N1 Zn1 N3 102.1(3) 2_645 . ? N1' Zn1 N3 108.4(4) 2_645 . ? C1 C1' N1' 76.2(9) . . ? C1 C1' N2' 80.5(9) . . ? N1' C1' N2' 103.6(10) . . ? C1 C1' N1 64.1(8) . . ? N2' C1' N1 103.7(9) . . ? C1 C1' N2 54.3(7) . . ? N1' C1' N2 96.1(9) . . ? N1 C1' N2 91.0(8) . . ? C1 C1' C3' 84.8(8) . . ? N2' C1' C3' 68.2(6) . . ? N2 C1' C3' 70.9(5) . . ? C1' C1 N1 74.5(9) . . ? C1' C1 N2 89.5(9) . . ? N1 C1 N2 110.9(8) . . ? C1' C1 N1' 62.9(8) . . ? N2 C1 N1' 105.8(8) . . ? C1' C1 N2' 61.3(8) . . ? N1 C1 N2' 99.5(8) . . ? N1' C1 N2' 90.3(8) . . ? C1' C1 C3 87.2(8) . . ? N2 C1 C3 72.2(5) . . ? N2' C1 C3 71.8(5) . . ? N2' C2' C3' 103.4(12) . . ? C3' C2' N2 106.5(11) . . ? N2' C2' C3 105.6(11) . . ? N2 C2' C3 93.9(9) . . ? N2 C2 C3 108.2(9) . . ? N2' C2 C3 107.2(9) . . ? N2 C2 C3' 109.6(9) . . ? N2' C2 C3' 93.3(9) . . ? C3' C3 C2 83.3(14) . . ? C3' C3 N1 83.0(13) . . ? C2 C3 N1 107.0(9) . . ? C3' C3 N1' 70.1(13) . . ? C2 C3 N1' 105.1(9) . . ? C3' C3 C2' 64.6(13) . . ? N1 C3 C2' 105.7(10) . . ? N1' C3 C2' 99.7(10) . . ? C3' C3 C1 92.6(12) . . ? C2 C3 C1 71.0(6) . . ? C2' C3 C1 76.3(7) . . ? C3 C3' N1' 81.0(13) . . ? C3 C3' C2' 87.3(14) . . ? N1' C3' C2' 110.9(11) . . ? C3 C3' N1 69.5(12) . . ? C2' C3' N1 108.7(10) . . ? C3 C3' C2 68.7(13) . . ? N1' C3' C2 103.8(10) . . ? N1 C3' C2 98.3(9) . . ? C3 C3' C1' 95.2(12) . . ? C2' C3' C1' 76.7(8) . . ? C2 C3' C1' 76.5(7) . . ? C5' C4 N2 119.8(9) . . ? N2 C4 C5 110.1(8) . . ? C5' C4 C4' 54.9(8) . . ? N2 C4 C4' 73.5(7) . . ? C5' C4 N2' 99.5(8) . . ? C5 C4 N2' 87.6(7) . . ? C4' C4 N2' 51.0(6) . . ? C5 C4' N2' 127.9(15) . . ? C5' C4' N2' 109.7(12) . . ? C5 C4' C4 61.0(11) . . ? C5' C4' C4 48.6(8) . . ? N2' C4' C4 68.5(8) . . ? C5 C4' N2 107.5(13) . . ? C5' C4' N2 91.0(10) . . ? C4 C4' N2 47.4(5) . . ? C5 C5' C4 98(2) . . ? C4 C5' C4' 76.6(10) . . ? C5 C5' C10 87.2(19) . . ? C4 C5' C10 127.2(10) . . ? C4' C5' C10 126.2(12) . . ? C5 C5' C10' 71.4(18) . . ? C4 C5' C10' 145.3(11) . . ? C4' C5' C10' 107.5(11) . . ? C5' C5 C4' 120(2) . . ? C5' C5 C10' 86.4(18) . . ? C4' C5 C10' 145.2(16) . . ? C5' C5 C4 59.8(19) . . ? C4' C5 C4 81.6(11) . . ? C10' C5 C4 133.2(11) . . ? C5' C5 C10 70.5(17) . . ? C4' C5 C10 168.3(15) . . ? C4 C5 C10 109.0(9) . . ? C6' C6 N3 70.8(8) . . ? C6' C6 N4' 94.3(10) . . ? N3 C6 N4' 109.8(7) . . ? C6' C6 N4 59.3(8) . . ? N3 C6 N4 98.2(6) . . ? C6 C6' N3 70.2(8) . . ? C6 C6' N4 85.8(9) . . ? N3 C6' N4 109.5(7) . . ? C6 C6' N4' 53.3(8) . . ? N3 C6' N4' 92.8(6) . . ? C8 C7 N4' 103.3(5) . . ? C8 C7 N4 102.1(4) . . ? C7 C8 N3 112.5(4) . . ? C7 C8 H8 123.7 . . ? N3 C8 H8 123.7 . . ? C10' C9' N4' 131.0(12) . . ? C10 C9' N4' 110.9(8) . . ? C10' C9' C9 59.2(9) . . ? N4' C9' C9 73.3(6) . . ? C10' C9' N4 105.2(11) . . ? C10 C9' N4 86.9(6) . . ? C9 C9' N4 46.6(4) . . ? C10 C9 N4 123.3(10) . . ? N4 C9 C10' 111.3(9) . . ? C10 C9 C9' 57.5(7) . . ? N4 C9 C9' 74.3(6) . . ? C10 C9 N4' 99.4(8) . . ? C10' C9 N4' 85.0(8) . . ? C9' C9 N4' 48.0(4) . . ? C10 C10' C9' 120(2) . . ? C10 C10' C5 84.4(17) . . ? C9' C10' C5 148.3(14) . . ? C10 C10' C9 54.7(14) . . ? C9' C10' C9 83.1(11) . . ? C5 C10' C9 128.5(11) . . ? C10 C10' C5' 70.0(16) . . ? C9' C10' C5' 169.4(14) . . ? C9 C10' C5' 106.8(10) . . ? C10' C10 C9 100.3(17) . . ? C10' C10 C5' 85.7(16) . . ? C9 C10 C5' 129.4(10) . . ? C9 C10 C9' 77.9(8) . . ? C5' C10 C9' 123.7(9) . . ? C10' C10 C5 71.3(16) . . ? C9 C10 C5 146.7(11) . . ? C9' C10 C5 106.9(8) . . ? O2 C11 O1 123.6(3) . . ? O2 C11 C12 119.2(3) . . ? O1 C11 C12 117.1(3) . . ? C13 C12 C11 113.8(3) . . ? C13 C12 C12 112.8(4) . 3_657 ? C11 C12 C12 109.7(3) . 3_657 ? C13 C12 H12 106.7 . . ? C11 C12 H12 106.7 . . ? C12 C12 H12 106.7 3_657 . ? C12 C13 C14 113.9(4) . . ? C12 C13 H13A 108.8 . . ? C14 C13 H13A 108.8 . . ? C12 C13 H13B 108.8 . . ? C14 C13 H13B 108.8 . . ? H13A C13 H13B 107.7 . . ? O4 C14 O3 123.7(4) . . ? O4 C14 C13 120.5(4) . . ? O3 C14 C13 115.8(3) . . ? C1 N1 C3 100.2(9) . . ? C3 N1 C1' 106.8(9) . . ? C1 N1 C3' 105.0(9) . . ? C1' N1 C3' 92.4(8) . . ? C1 N1 Zn1 131.7(9) . 2_655 ? C3 N1 Zn1 127.5(8) . 2_655 ? C1' N1 Zn1 117.1(8) . 2_655 ? C3' N1 Zn1 120.7(8) . 2_655 ? C1' N1' C3' 103.7(11) . . ? C1' N1' C3 111.9(11) . . ? C3' N1' C1 106.3(10) . . ? C3 N1' C1 94.2(9) . . ? C1' N1' Zn1 121.8(10) . 2_655 ? C3' N1' Zn1 128.9(10) . 2_655 ? C3 N1' Zn1 126.1(9) . 2_655 ? C1 N1' Zn1 122.9(9) . 2_655 ? N2 N2' C2' 86.0(12) . . ? N2 N2' C2 65.5(11) . . ? N2 N2' C1' 97.6(12) . . ? C2' N2' C1' 111.6(10) . . ? C2 N2' C1' 111.5(9) . . ? N2 N2' C4' 110.3(12) . . ? C2' N2' C4' 123.2(11) . . ? C2 N2' C4' 129.4(10) . . ? C1' N2' C4' 118.9(10) . . ? N2 N2' C1 59.4(9) . . ? C2' N2' C1 104.4(9) . . ? C2 N2' C1 92.0(8) . . ? C4' N2' C1 131.2(9) . . ? N2 N2' C4 49.9(9) . . ? C2' N2' C4 110.7(9) . . ? C2 N2' C4 96.1(8) . . ? C1' N2' C4 122.9(8) . . ? C4' N2' C4 60.5(7) . . ? C1 N2' C4 95.0(7) . . ? N2' N2 C1 92.4(11) . . ? C2 N2 C1 108.5(7) . . ? N2' N2 C2' 63.0(10) . . ? C1 N2 C2' 108.3(8) . . ? N2' N2 C4 107.5(11) . . ? C2 N2 C4 123.4(8) . . ? C1 N2 C4 126.1(7) . . ? C2' N2 C4 125.5(8) . . ? N2' N2 C1' 56.2(10) . . ? C2 N2 C1' 101.8(7) . . ? C2' N2 C1' 91.0(7) . . ? C4 N2 C1' 130.3(7) . . ? N2' N2 C4' 48.5(10) . . ? C2 N2 C4' 109.3(9) . . ? C1 N2 C4' 118.3(8) . . ? C2' N2 C4' 94.2(8) . . ? C4 N2 C4' 59.1(7) . . ? C1' N2 C4' 89.2(7) . . ? C6 N3 C8 101.7(5) . . ? C6' N3 C8 105.1(5) . . ? C6 N3 Zn1 125.9(4) . . ? C6' N3 Zn1 122.9(4) . . ? C8 N3 Zn1 128.9(3) . . ? N4' N4 C6' 93.7(9) . . ? N4' N4 C7 64.0(7) . . ? C6' N4 C7 107.0(6) . . ? N4' N4 C9 107.4(9) . . ? C6' N4 C9 126.9(7) . . ? C7 N4 C9 126.1(7) . . ? N4' N4 C6 58.9(7) . . ? C7 N4 C6 92.2(6) . . ? C9 N4 C6 130.9(7) . . ? N4' N4 C9' 48.5(7) . . ? C6' N4 C9' 119.1(7) . . ? C7 N4 C9' 96.3(6) . . ? C9 N4 C9' 59.1(6) . . ? C6 N4 C9' 90.7(6) . . ? N4 N4' C7 78.5(7) . . ? N4 N4' C6 85.9(9) . . ? C7 N4' C6 108.7(6) . . ? N4 N4' C9' 104.7(9) . . ? C7 N4' C9' 127.9(8) . . ? C6 N4' C9' 123.3(8) . . ? N4 N4' C6' 53.6(7) . . ? C7 N4' C6' 96.5(5) . . ? C9' N4' C6' 127.8(8) . . ? N4 N4' C9 46.1(6) . . ? C7 N4' C9 103.8(6) . . ? C6 N4' C9 113.0(7) . . ? C9' N4' C9 58.7(6) . . ? C6' N4' C9 88.1(6) . . ? C11 O1 Zn1 111.2(2) . . ? C14 O3 Zn1 116.4(2) . 3_757 ? H1 O1W H2 113(7) . . ? 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 N1' C1' C1 N1 3.8(11) . . . . ? N2' C1' C1 N1 110.4(8) . . . . ? N2 C1' C1 N1 111.9(7) . . . . ? C3' C1' C1 N1 41.7(7) . . . . ? N1' C1' C1 N2 -108.1(8) . . . . ? N2' C1' C1 N2 -1.5(7) . . . . ? N1 C1' C1 N2 -111.9(7) . . . . ? C3' C1' C1 N2 -70.2(5) . . . . ? N2' C1' C1 N1' 106.7(9) . . . . ? N1 C1' C1 N1' -3.8(11) . . . . ? N2 C1' C1 N1' 108.1(8) . . . . ? C3' C1' C1 N1' 37.9(7) . . . . ? N1' C1' C1 N2' -106.7(9) . . . . ? N1 C1' C1 N2' -110.4(8) . . . . ? N2 C1' C1 N2' 1.5(7) . . . . ? C3' C1' C1 N2' -68.7(6) . . . . ? N1' C1' C1 C3 -35.9(7) . . . . ? N2' C1' C1 C3 70.7(6) . . . . ? N1 C1' C1 C3 -39.7(6) . . . . ? N2 C1' C1 C3 72.2(5) . . . . ? C3' C1' C1 C3 2.0(5) . . . . ? N2 C2 C3 C3' -97.5(15) . . . . ? N2' C2 C3 C3' -63.0(15) . . . . ? N2 C2 C3 N1 -17.0(15) . . . . ? N2' C2 C3 N1 17.5(15) . . . . ? C3' C2 C3 N1 80.6(14) . . . . ? N2 C2 C3 N1' -30.3(15) . . . . ? N2' C2 C3 N1' 4.2(15) . . . . ? C3' C2 C3 N1' 67.2(13) . . . . ? N2 C2 C3 C2' -106(3) . . . . ? N2' C2 C3 C2' -71(3) . . . . ? C3' C2 C3 C2' -8(3) . . . . ? N2 C2 C3 C1 -2.5(9) . . . . ? N2' C2 C3 C1 32.1(10) . . . . ? C3' C2 C3 C1 95.1(12) . . . . ? N2' C2' C3 C3' -89.4(14) . . . . ? N2 C2' C3 C3' -118.5(14) . . . . ? N2' C2' C3 C2 81(3) . . . . ? C3' C2' C3 C2 171(4) . . . . ? N2 C2' C3 C2 52(3) . . . . ? N2' C2' C3 N1 -15.3(13) . . . . ? C3' C2' C3 N1 74.1(14) . . . . ? N2 C2' C3 N1 -44.4(11) . . . . ? N2' C2' C3 N1' -27.0(12) . . . . ? C3' C2' C3 N1' 62.4(13) . . . . ? N2 C2' C3 N1' -56.1(10) . . . . ? N2' C2' C3 C1 10.2(9) . . . . ? C3' C2' C3 C1 99.6(12) . . . . ? N2 C2' C3 C1 -18.9(7) . . . . ? C1' C1 C3 C3' -6.1(15) . . . . ? N1 C1 C3 C3' -75.4(15) . . . . ? N2 C1 C3 C3' 84.3(14) . . . . ? N1' C1 C3 C3' -57.2(14) . . . . ? N2' C1 C3 C3' 54.6(13) . . . . ? C1' C1 C3 C2 -88.1(11) . . . . ? N1 C1 C3 C2 -157.5(14) . . . . ? N2 C1 C3 C2 2.3(8) . . . . ? N1' C1 C3 C2 -139.3(13) . . . . ? N2' C1 C3 C2 -27.5(9) . . . . ? C1' C1 C3 N1 69.4(12) . . . . ? N2 C1 C3 N1 159.7(12) . . . . ? N1' C1 C3 N1 18.2(12) . . . . ? N2' C1 C3 N1 130.0(11) . . . . ? C1' C1 C3 N1' 51.2(11) . . . . ? N1 C1 C3 N1' -18.2(12) . . . . ? N2 C1 C3 N1' 141.5(11) . . . . ? N2' C1 C3 N1' 111.8(10) . . . . ? C1' C1 C3 C2' -69.1(10) . . . . ? N1 C1 C3 C2' -138.5(13) . . . . ? N2 C1 C3 C2' 21.2(7) . . . . ? N1' C1 C3 C2' -120.3(12) . . . . ? N2' C1 C3 C2' -8.5(7) . . . . ? C2 C3 C3' N1' 108.7(9) . . . . ? N1 C3 C3' N1' 0.6(11) . . . . ? C2' C3 C3' N1' 111.7(10) . . . . ? C1 C3 C3' N1' 38.2(8) . . . . ? C2 C3 C3' C2' -3.0(11) . . . . ? N1 C3 C3' C2' -111.1(9) . . . . ? N1' C3 C3' C2' -111.7(10) . . . . ? C1 C3 C3' C2' -73.5(8) . . . . ? C2 C3 C3' N1 108.1(8) . . . . ? N1' C3 C3' N1 -0.6(11) . . . . ? C2' C3 C3' N1 111.1(9) . . . . ? C1 C3 C3' N1 37.6(5) . . . . ? N1 C3 C3' C2 -108.1(8) . . . . ? N1' C3 C3' C2 -108.7(9) . . . . ? C2' C3 C3' C2 3.0(11) . . . . ? C1 C3 C3' C2 -70.5(6) . . . . ? C2 C3 C3' C1' 73.3(7) . . . . ? N1 C3 C3' C1' -34.8(7) . . . . ? N1' C3 C3' C1' -35.3(7) . . . . ? C2' C3 C3' C1' 76.3(9) . . . . ? C1 C3 C3' C1' 2.8(7) . . . . ? N2' C2' C3' C3 98.0(13) . . . . ? N2 C2' C3' C3 66.1(13) . . . . ? N2' C2' C3' N1' 18.7(14) . . . . ? N2 C2' C3' N1' -13.2(13) . . . . ? C3 C2' C3' N1' -79.3(13) . . . . ? N2' C2' C3' N1 30.7(13) . . . . ? N2 C2' C3' N1 -1.2(13) . . . . ? C3 C2' C3' N1 -67.3(12) . . . . ? N2' C2' C3' C2 89(3) . . . . ? N2 C2' C3' C2 57(3) . . . . ? C3 C2' C3' C2 -9(3) . . . . ? N2' C2' C3' C1' 2.0(9) . . . . ? N2 C2' C3' C1' -29.9(8) . . . . ? C3 C2' C3' C1' -96.0(12) . . . . ? N2 C2 C3' C3 92.2(15) . . . . ? N2' C2 C3' C3 121.5(14) . . . . ? N2 C2 C3' N1' 17.8(14) . . . . ? N2' C2 C3' N1' 47.0(12) . . . . ? C3 C2 C3' N1' -74.4(13) . . . . ? N2 C2 C3' C2' -97(3) . . . . ? N2' C2 C3' C2' -68(3) . . . . ? C3 C2 C3' C2' 171(4) . . . . ? N2 C2 C3' N1 28.1(13) . . . . ? N2' C2 C3' N1 57.4(11) . . . . ? C3 C2 C3' N1 -64.1(12) . . . . ? N2 C2 C3' C1' -8.9(10) . . . . ? N2' C2 C3' C1' 20.3(8) . . . . ? C3 C2 C3' C1' -101.1(12) . . . . ? C1 C1' C3' C3 -6.1(15) . . . . ? N1' C1' C3' C3 68.2(15) . . . . ? N2' C1' C3' C3 -87.9(14) . . . . ? N1 C1' C3' C3 52.0(14) . . . . ? N2 C1' C3' C3 -60.0(13) . . . . ? C1 C1' C3' N1' -74.3(11) . . . . ? N2' C1' C3' N1' -156.1(13) . . . . ? N1 C1' C3' N1' -16.2(13) . . . . ? N2 C1' C3' N1' -128.2(11) . . . . ? C1 C1' C3' C2' 79.9(10) . . . . ? N1' C1' C3' C2' 154.2(13) . . . . ? N2' C1' C3' C2' -1.9(8) . . . . ? N1 C1' C3' C2' 137.9(11) . . . . ? N2 C1' C3' C2' 26.0(7) . . . . ? C1 C1' C3' N1 -58.0(10) . . . . ? N1' C1' C3' N1 16.2(13) . . . . ? N2' C1' C3' N1 -139.9(11) . . . . ? N2 C1' C3' N1 -111.9(10) . . . . ? C1 C1' C3' C2 60.5(10) . . . . ? N1' C1' C3' C2 134.8(13) . . . . ? N2' C1' C3' C2 -21.3(9) . . . . ? N1 C1' C3' C2 118.6(11) . . . . ? N2 C1' C3' C2 6.6(7) . . . . ? C5' C4 C4' C5 20.3(13) . . . . ? N2 C4 C4' C5 167.5(15) . . . . ? N2' C4 C4' C5 166.4(16) . . . . ? N2 C4 C4' C5' 147.3(11) . . . . ? C5 C4 C4' C5' -20.3(13) . . . . ? N2' C4 C4' C5' 146.2(12) . . . . ? C5' C4 C4' N2' -146.2(12) . . . . ? N2 C4 C4' N2' 1.1(6) . . . . ? C5 C4 C4' N2' -166.4(16) . . . . ? C5' C4 C4' N2 -147.3(11) . . . . ? C5 C4 C4' N2 -167.5(15) . . . . ? N2' C4 C4' N2 -1.1(6) . . . . ? N2 C4 C5' C5 -70(2) . . . . ? C4' C4 C5' C5 -33(2) . . . . ? N2' C4 C5' C5 -59(2) . . . . ? N2 C4 C5' C4' -36.7(12) . . . . ? C5 C4 C5' C4' 33(2) . . . . ? N2' C4 C5' C4' -26.0(9) . . . . ? N2 C4 C5' C10 -162.2(10) . . . . ? C5 C4 C5' C10 -92(2) . . . . ? C4' C4 C5' C10 -125.5(16) . . . . ? N2' C4 C5' C10 -151.5(11) . . . . ? N2 C4 C5' C10' -138.1(17) . . . . ? C5 C4 C5' C10' -68(3) . . . . ? C4' C4 C5' C10' -101(2) . . . . ? N2' C4 C5' C10' -127.4(18) . . . . ? N2' C4' C5' C5 154(4) . . . . ? C4 C4' C5' C5 121(4) . . . . ? N2 C4' C5' C5 144(3) . . . . ? C5 C4' C5' C4 -121(4) . . . . ? N2' C4' C5' C4 33.4(11) . . . . ? N2 C4' C5' C4 23.5(8) . . . . ? C5 C4' C5' C10 6(3) . . . . ? N2' C4' C5' C10 159.9(11) . . . . ? C4 C4' C5' C10 126.5(15) . . . . ? N2 C4' C5' C10 150.0(11) . . . . ? C5 C4' C5' C10' 24(3) . . . . ? N2' C4' C5' C10' 177.6(10) . . . . ? C4 C4' C5' C10' 144.2(12) . . . . ? N2 C4' C5' C10' 167.6(9) . . . . ? C4 C5' C5 C4' 58(3) . . . . ? C10 C5' C5 C4' -175(2) . . . . ? C10' C5' C5 C4' -156(3) . . . . ? C4 C5' C5 C10' -146.1(10) . . . . ? C4' C5' C5 C10' 156(3) . . . . ? C10 C5' C5 C10' -18.9(9) . . . . ? C4' C5' C5 C4 -58(3) . . . . ? C10 C5' C5 C4 127.2(12) . . . . ? C10' C5' C5 C4 146.1(10) . . . . ? C4 C5' C5 C10 -127.2(12) . . . . ? C4' C5' C5 C10 175(2) . . . . ? C10' C5' C5 C10 18.9(9) . . . . ? N2' C4' C5 C5' -32(4) . . . . ? C4 C4' C5 C5' -48(3) . . . . ? N2 C4' C5 C5' -38(4) . . . . ? C5' C4' C5 C10' -135(6) . . . . ? N2' C4' C5 C10' -167(2) . . . . ? C4 C4' C5 C10' 177(3) . . . . ? N2 C4' C5 C10' -173(2) . . . . ? C5' C4' C5 C4 48(3) . . . . ? N2' C4' C5 C4 16.1(19) . . . . ? N2 C4' C5 C4 9.6(12) . . . . ? C5' C4' C5 C10 -157(12) . . . . ? N2' C4' C5 C10 171(8) . . . . ? C4 C4' C5 C10 155(10) . . . . ? N2 C4' C5 C10 165(9) . . . . ? N2 C4 C5 C5' 120(2) . . . . ? C4' C4 C5 C5' 133(3) . . . . ? N2' C4 C5 C5' 122(2) . . . . ? C5' C4 C5 C4' -133(3) . . . . ? N2 C4 C5 C4' -12.7(15) . . . . ? N2' C4 C5 C4' -10.5(13) . . . . ? C5' C4 C5 C10' 49.8(18) . . . . ? N2 C4 C5 C10' 169.5(15) . . . . ? C4' C4 C5 C10' -178(3) . . . . ? N2' C4 C5 C10' 171.7(17) . . . . ? C5' C4 C5 C10 52.6(18) . . . . ? N2 C4 C5 C10 172.4(9) . . . . ? C4' C4 C5 C10 -174.9(19) . . . . ? N2' C4 C5 C10 174.6(10) . . . . ? N4' C6 C6' N3 109.5(6) . . . . ? N4 C6 C6' N3 112.5(6) . . . . ? N3 C6 C6' N4 -112.5(6) . . . . ? N4' C6 C6' N4 -3.0(7) . . . . ? N3 C6 C6' N4' -109.5(6) . . . . ? N4 C6 C6' N4' 3.0(7) . . . . ? N4' C7 C8 N3 19.5(7) . . . . ? N4 C7 C8 N3 -18.9(6) . . . . ? C10' C9' C9 C10 20.9(11) . . . . ? N4' C9' C9 C10 -146.5(10) . . . . ? N4 C9' C9 C10 -148.8(10) . . . . ? C10' C9' C9 N4 169.7(13) . . . . ? C10 C9' C9 N4 148.8(10) . . . . ? N4' C9' C9 N4 2.2(6) . . . . ? C10 C9' C9 C10' -20.9(11) . . . . ? N4' C9' C9 C10' -167.4(14) . . . . ? N4 C9' C9 C10' -169.7(13) . . . . ? C10' C9' C9 N4' 167.4(14) . . . . ? C10 C9' C9 N4' 146.5(10) . . . . ? N4 C9' C9 N4' -2.2(6) . . . . ? N4' C9' C10' C10 -26(3) . . . . ? C9 C9' C10' C10 -42(2) . . . . ? N4 C9' C10' C10 -34(3) . . . . ? C10 C9' C10' C5 -136(4) . . . . ? N4' C9' C10' C5 -162(2) . . . . ? C9 C9' C10' C5 -178(3) . . . . ? N4 C9' C10' C5 -171(2) . . . . ? C10 C9' C10' C9 42(2) . . . . ? N4' C9' C10' C9 16.0(18) . . . . ? N4 C9' C10' C9 7.8(10) . . . . ? C10 C9' C10' C5' -159(10) . . . . ? N4' C9' C10' C5' 175(7) . . . . ? C9 C9' C10' C5' 159(8) . . . . ? N4 C9' C10' C5' 167(8) . . . . ? C5' C5 C10' C10 48(3) . . . . ? C4' C5 C10' C10 -170(3) . . . . ? C4 C5 C10' C10 7(3) . . . . ? C5' C5 C10' C9' -169(3) . . . . ? C4' C5 C10' C9' -27(5) . . . . ? C4 C5 C10' C9' 149(2) . . . . ? C10 C5 C10' C9' 143(4) . . . . ? C5' C5 C10' C9 13(3) . . . . ? C4' C5 C10' C9 155(3) . . . . ? C4 C5 C10' C9 -28(3) . . . . ? C10 C5 C10' C9 -35.0(13) . . . . ? C4' C5 C10' C5' 143(5) . . . . ? C4 C5 C10' C5' -41.4(17) . . . . ? C10 C5 C10' C5' -48(3) . . . . ? N4 C9 C10' C10 123.9(18) . . . . ? C9' C9 C10' C10 135(2) . . . . ? N4' C9 C10' C10 125.2(17) . . . . ? C10 C9 C10' C9' -135(2) . . . . ? N4 C9 C10' C9' -10.7(13) . . . . ? N4' C9 C10' C9' -9.3(10) . . . . ? C10 C9 C10' C5 44.3(17) . . . . ? N4 C9 C10' C5 168.2(13) . . . . ? C9' C9 C10' C5 179(2) . . . . ? N4' C9 C10' C5 169.5(14) . . . . ? C10 C9 C10' C5' 49.4(15) . . . . ? N4 C9 C10' C5' 173.3(9) . . . . ? C9' C9 C10' C5' -176.1(16) . . . . ? N4' C9 C10' C5' 174.6(9) . . . . ? C5 C5' C10' C10 -128(3) . . . . ? C4 C5' C10' C10 -52(3) . . . . ? C4' C5' C10' C10 -143.6(17) . . . . ? C5 C5' C10' C9' 32(9) . . . . ? C4 C5' C10' C9' 108(8) . . . . ? C4' C5' C10' C9' 17(9) . . . . ? C10 C5' C10' C9' 160(9) . . . . ? C4 C5' C10' C5 76(3) . . . . ? C4' C5' C10' C5 -15(2) . . . . ? C10 C5' C10' C5 128(3) . . . . ? C5 C5' C10' C9 -169(2) . . . . ? C4 C5' C10' C9 -93(2) . . . . ? C4' C5' C10' C9 175.1(11) . . . . ? C10 C5' C10' C9 -41.3(13) . . . . ? C9' C10' C10 C9 55(2) . . . . ? C5 C10' C10 C9 -146.7(10) . . . . ? C5' C10' C10 C9 -129.3(11) . . . . ? C9' C10' C10 C5' -175.9(19) . . . . ? C5 C10' C10 C5' -17.4(9) . . . . ? C9 C10' C10 C5' 129.3(11) . . . . ? C5 C10' C10 C9' 159(2) . . . . ? C9 C10' C10 C9' -55(2) . . . . ? C5' C10' C10 C9' 175.9(19) . . . . ? C9' C10' C10 C5 -159(2) . . . . ? C9 C10' C10 C5 146.7(10) . . . . ? C5' C10' C10 C5 17.4(9) . . . . ? N4 C9 C10 C10' -68(2) . . . . ? C9' C9 C10 C10' -31.0(16) . . . . ? N4' C9 C10 C10' -55.6(18) . . . . ? N4 C9 C10 C5' -160.6(10) . . . . ? C10' C9 C10 C5' -93(2) . . . . ? C9' C9 C10 C5' -123.9(14) . . . . ? N4' C9 C10 C5' -148.4(11) . . . . ? N4 C9 C10 C9' -36.7(11) . . . . ? C10' C9 C10 C9' 31.0(16) . . . . ? N4' C9 C10 C9' -24.5(7) . . . . ? N4 C9 C10 C5 -139.2(16) . . . . ? C10' C9 C10 C5 -71(2) . . . . ? C9' C9 C10 C5 -102.4(19) . . . . ? N4' C9 C10 C5 -127.0(17) . . . . ? C5 C5' C10 C10' 48(3) . . . . ? C4 C5' C10 C10' 145.7(19) . . . . ? C4' C5' C10 C10' 45(2) . . . . ? C5 C5' C10 C9 148(2) . . . . ? C4 C5' C10 C9 -114.6(15) . . . . ? C4' C5' C10 C9 144.3(14) . . . . ? C10' C5' C10 C9 100(2) . . . . ? C5 C5' C10 C9' 45(3) . . . . ? C4 C5' C10 C9' 142.6(13) . . . . ? C4' C5' C10 C9' 41.5(18) . . . . ? C10' C5' C10 C9' -3.0(14) . . . . ? C4 C5' C10 C5 97(3) . . . . ? C4' C5' C10 C5 -3.7(19) . . . . ? C10' C5' C10 C5 -48(3) . . . . ? N4' C9' C10 C10' 159(3) . . . . ? C9 C9' C10 C10' 125(3) . . . . ? N4 C9' C10 C10' 147(3) . . . . ? C10' C9' C10 C9 -125(3) . . . . ? N4' C9' C10 C9 34.4(10) . . . . ? N4 C9' C10 C9 22.2(7) . . . . ? C10' C9' C10 C5' 5(2) . . . . ? N4' C9' C10 C5' 164.0(9) . . . . ? C9 C9' C10 C5' 129.6(12) . . . . ? N4 C9' C10 C5' 151.8(9) . . . . ? C10' C9' C10 C5 21(2) . . . . ? N4' C9' C10 C5 -179.7(10) . . . . ? C9 C9' C10 C5 145.9(11) . . . . ? N4 C9' C10 C5 168.1(8) . . . . ? C5' C5 C10 C10' -128(3) . . . . ? C4' C5 C10 C10' 31(9) . . . . ? C4 C5 C10 C10' -175.0(19) . . . . ? C5' C5 C10 C9 -48(3) . . . . ? C4' C5 C10 C9 111(9) . . . . ? C10' C5 C10 C9 80(2) . . . . ? C4 C5 C10 C9 -95(2) . . . . ? C4' C5 C10 C5' 159(11) . . . . ? C10' C5 C10 C5' 128(3) . . . . ? C4 C5 C10 C5' -46.8(18) . . . . ? C5' C5 C10 C9' -142(2) . . . . ? C4' C5 C10 C9' 17(9) . . . . ? C10' C5 C10 C9' -13.6(15) . . . . ? C4 C5 C10 C9' 171.4(11) . . . . ? O2 C11 C12 C13 125.7(4) . . . . ? O1 C11 C12 C13 -57.8(4) . . . . ? O2 C11 C12 C12 -106.9(5) . . . 3_657 ? O1 C11 C12 C12 69.6(5) . . . 3_657 ? C11 C12 C13 C14 -63.8(5) . . . . ? C12 C12 C13 C14 170.5(4) 3_657 . . . ? C12 C13 C14 O4 -128.5(5) . . . . ? C12 C13 C14 O3 51.9(6) . . . . ? C1' C1 N1 C3 -104.0(11) . . . . ? N2 C1 N1 C3 -20.7(12) . . . . ? N1' C1 N1 C3 -88(5) . . . . ? N2' C1 N1 C3 -47.5(10) . . . . ? N2 C1 N1 C1' 83.3(10) . . . . ? N1' C1 N1 C1' 16(5) . . . . ? N2' C1 N1 C1' 56.4(8) . . . . ? C3 C1 N1 C1' 104.0(11) . . . . ? C1' C1 N1 C3' -76.2(10) . . . . ? N2 C1 N1 C3' 7.1(12) . . . . ? N1' C1 N1 C3' -60(5) . . . . ? N2' C1 N1 C3' -19.8(10) . . . . ? C3 C1 N1 C3' 27.7(6) . . . . ? C1' C1 N1 Zn1 84.9(12) . . . 2_655 ? N2 C1 N1 Zn1 168.2(8) . . . 2_655 ? N1' C1 N1 Zn1 101(5) . . . 2_655 ? N2' C1 N1 Zn1 141.4(9) . . . 2_655 ? C3 C1 N1 Zn1 -171.1(16) . . . 2_655 ? C3' C3 N1 C1 103.1(14) . . . . ? C2 C3 N1 C1 22.3(13) . . . . ? N1' C3 N1 C1 105(5) . . . . ? C2' C3 N1 C1 42.0(12) . . . . ? C3' C3 N1 C1' 60.9(14) . . . . ? C2 C3 N1 C1' -19.9(14) . . . . ? N1' C3 N1 C1' 63(4) . . . . ? C2' C3 N1 C1' -0.1(13) . . . . ? C1 C3 N1 C1' -42.1(7) . . . . ? C2 C3 N1 C3' -80.8(15) . . . . ? N1' C3 N1 C3' 2(5) . . . . ? C2' C3 N1 C3' -61.1(13) . . . . ? C1 C3 N1 C3' -103.1(14) . . . . ? C3' C3 N1 Zn1 -85.3(15) . . . 2_655 ? C2 C3 N1 Zn1 -166.1(9) . . . 2_655 ? N1' C3 N1 Zn1 -83(4) . . . 2_655 ? C2' C3 N1 Zn1 -146.4(9) . . . 2_655 ? C1 C3 N1 Zn1 171.6(15) . . . 2_655 ? N1' C1' N1 C1 -163(5) . . . . ? N2' C1' N1 C1 -72.1(10) . . . . ? N2 C1' N1 C1 -48.9(7) . . . . ? C3' C1' N1 C1 -110.1(10) . . . . ? C1 C1' N1 C3 86.3(11) . . . . ? N1' C1' N1 C3 -77(5) . . . . ? N2' C1' N1 C3 14.2(12) . . . . ? N2 C1' N1 C3 37.4(10) . . . . ? C3' C1' N1 C3 -23.8(6) . . . . ? C1 C1' N1 C3' 110.1(10) . . . . ? N1' C1' N1 C3' -53(5) . . . . ? N2' C1' N1 C3' 38.0(10) . . . . ? N2 C1' N1 C3' 61.2(8) . . . . ? C1 C1' N1 Zn1 -123.4(10) . . . 2_655 ? N1' C1' N1 Zn1 74(5) . . . 2_655 ? N2' C1' N1 Zn1 164.6(7) . . . 2_655 ? N2 C1' N1 Zn1 -172.3(6) . . . 2_655 ? C3' C1' N1 Zn1 126.5(10) . . . 2_655 ? C3 C3' N1 C1 -83.1(14) . . . . ? N1' C3' N1 C1 100(5) . . . . ? C2' C3' N1 C1 -3.5(13) . . . . ? C2 C3' N1 C1 -19.6(11) . . . . ? C1' C3' N1 C1 40.0(7) . . . . ? N1' C3' N1 C3 -177(5) . . . . ? C2' C3' N1 C3 79.6(14) . . . . ? C2 C3' N1 C3 63.5(12) . . . . ? C1' C3' N1 C3 123.1(14) . . . . ? C3 C3' N1 C1' -123.1(14) . . . . ? N1' C3' N1 C1' 60(5) . . . . ? C2' C3' N1 C1' -43.5(11) . . . . ? C2 C3' N1 C1' -59.7(10) . . . . ? C3 C3' N1 Zn1 113.1(14) . . . 2_655 ? N1' C3' N1 Zn1 -64(5) . . . 2_655 ? C2' C3' N1 Zn1 -167.2(9) . . . 2_655 ? C2 C3' N1 Zn1 176.6(8) . . . 2_655 ? C1' C3' N1 Zn1 -123.7(12) . . . 2_655 ? C1 C1' N1' C3' 99.2(11) . . . . ? N2' C1' N1' C3' 22.8(12) . . . . ? N1 C1' N1' C3' 115(5) . . . . ? N2 C1' N1' C3' 48.3(10) . . . . ? C1 C1' N1' C3 70.0(11) . . . . ? N2' C1' N1' C3 -6.4(13) . . . . ? N1 C1' N1' C3 86(5) . . . . ? N2 C1' N1' C3 19.1(11) . . . . ? C3' C1' N1' C3 -29.2(7) . . . . ? N2' C1' N1' C1 -76.4(10) . . . . ? N1 C1' N1' C1 16(5) . . . . ? N2 C1' N1' C1 -50.9(7) . . . . ? C3' C1' N1' C1 -99.2(11) . . . . ? C1 C1' N1' Zn1 -105.2(10) . . . 2_655 ? N2' C1' N1' Zn1 178.4(7) . . . 2_655 ? N1 C1' N1' Zn1 -89(5) . . . 2_655 ? N2 C1' N1' Zn1 -156.0(7) . . . 2_655 ? C3' C1' N1' Zn1 155.6(14) . . . 2_655 ? C3 C3' N1' C1' -110.6(14) . . . . ? C2' C3' N1' C1' -27.0(13) . . . . ? N1 C3' N1' C1' -108(5) . . . . ? C2 C3' N1' C1' -45.3(12) . . . . ? C2' C3' N1' C3 83.6(14) . . . . ? N1 C3' N1' C3 3(5) . . . . ? C2 C3' N1' C3 65.3(12) . . . . ? C1' C3' N1' C3 110.6(14) . . . . ? C3 C3' N1' C1 -68.2(14) . . . . ? C2' C3' N1' C1 15.4(13) . . . . ? N1 C3' N1' C1 -66(5) . . . . ? C2 C3' N1' C1 -2.9(12) . . . . ? C1' C3' N1' C1 42.4(8) . . . . ? C3 C3' N1' Zn1 96.2(14) . . . 2_655 ? C2' C3' N1' Zn1 179.8(9) . . . 2_655 ? N1 C3' N1' Zn1 99(5) . . . 2_655 ? C2 C3' N1' Zn1 161.5(9) . . . 2_655 ? C1' C3' N1' Zn1 -153.2(15) . . . 2_655 ? C3' C3 N1' C1' 78.6(14) . . . . ? C2 C3 N1' C1' 1.6(14) . . . . ? N1 C3 N1' C1' -99(5) . . . . ? C2' C3 N1' C1' 20.2(13) . . . . ? C1 C3 N1' C1' -38.1(8) . . . . ? C2 C3 N1' C3' -77.0(15) . . . . ? N1 C3 N1' C3' -177(5) . . . . ? C2' C3 N1' C3' -58.4(13) . . . . ? C1 C3 N1' C3' -116.7(14) . . . . ? C3' C3 N1' C1 116.7(14) . . . . ? C2 C3 N1' C1 39.7(12) . . . . ? N1 C3 N1' C1 -61(4) . . . . ? C2' C3 N1' C1 58.3(10) . . . . ? C3' C3 N1' Zn1 -106.6(15) . . . 2_655 ? C2 C3 N1' Zn1 176.5(9) . . . 2_655 ? N1 C3 N1' Zn1 76(4) . . . 2_655 ? C2' C3 N1' Zn1 -164.9(8) . . . 2_655 ? C1 C3 N1' Zn1 136.8(12) . . . 2_655 ? N1 C1 N1' C1' -162(5) . . . . ? N2 C1 N1' C1' 81.0(10) . . . . ? N2' C1 N1' C1' 57.2(9) . . . . ? C3 C1 N1' C1' 119.0(11) . . . . ? C1' C1 N1' C3' -92.3(11) . . . . ? N1 C1 N1' C3' 105(5) . . . . ? N2 C1 N1' C3' -11.2(12) . . . . ? N2' C1 N1' C3' -35.1(10) . . . . ? C3 C1 N1' C3' 26.8(6) . . . . ? C1' C1 N1' C3 -119.0(11) . . . . ? N1 C1 N1' C3 79(5) . . . . ? N2 C1 N1' C3 -38.0(10) . . . . ? N2' C1 N1' C3 -61.9(9) . . . . ? C1' C1 N1' Zn1 102.2(12) . . . 2_655 ? N1 C1 N1' Zn1 -60(5) . . . 2_655 ? N2 C1 N1' Zn1 -176.8(7) . . . 2_655 ? N2' C1 N1' Zn1 159.3(8) . . . 2_655 ? C3 C1 N1' Zn1 -138.8(13) . . . 2_655 ? C3' C2' N2' N2 -99.7(12) . . . . ? C3 C2' N2' N2 -70.7(12) . . . . ? C3' C2' N2' C2 -97(3) . . . . ? N2 C2' N2' C2 3(3) . . . . ? C3 C2' N2' C2 -68(3) . . . . ? C3' C2' N2' C1' -3.2(14) . . . . ? N2 C2' N2' C1' 96.6(13) . . . . ? C3 C2' N2' C1' 25.8(13) . . . . ? C3' C2' N2' C4' 148.5(11) . . . . ? N2 C2' N2' C4' -111.8(15) . . . . ? C3 C2' N2' C4' 177.5(11) . . . . ? C3' C2' N2' C1 -42.8(11) . . . . ? N2 C2' N2' C1 56.9(9) . . . . ? C3 C2' N2' C1 -13.8(12) . . . . ? C3' C2' N2' C4 -144.0(8) . . . . ? N2 C2' N2' C4 -44.2(8) . . . . ? C3 C2' N2' C4 -115.0(10) . . . . ? C3 C2 N2' N2 -97.2(13) . . . . ? C3' C2 N2' N2 -122.0(12) . . . . ? N2 C2 N2' C2' -177(3) . . . . ? C3 C2 N2' C2' 86(3) . . . . ? C3' C2 N2' C2' 61(3) . . . . ? N2 C2 N2' C1' 88.6(12) . . . . ? C3 C2 N2' C1' -8.6(16) . . . . ? C3' C2 N2' C1' -33.4(13) . . . . ? N2 C2 N2' C4' -96.9(16) . . . . ? C3 C2 N2' C4' 165.9(12) . . . . ? C3' C2 N2' C4' 141.2(12) . . . . ? N2 C2 N2' C1 54.8(8) . . . . ? C3 C2 N2' C1 -42.4(12) . . . . ? C3' C2 N2' C1 -67.1(9) . . . . ? N2 C2 N2' C4 -40.4(8) . . . . ? C3 C2 N2' C4 -137.6(10) . . . . ? C3' C2 N2' C4 -162.4(8) . . . . ? C1 C1' N2' N2 2.7(12) . . . . ? N1' C1' N2' N2 75.8(13) . . . . ? N1 C1' N2' N2 62.9(13) . . . . ? C3' C1' N2' N2 90.8(11) . . . . ? C1 C1' N2' C2' -86.0(11) . . . . ? N1' C1' N2' C2' -12.9(14) . . . . ? N1 C1' N2' C2' -25.8(13) . . . . ? N2 C1' N2' C2' -88.7(13) . . . . ? C3' C1' N2' C2' 2.1(9) . . . . ? C1 C1' N2' C2 -63.9(12) . . . . ? N1' C1' N2' C2 9.3(14) . . . . ? N1 C1' N2' C2 -3.6(14) . . . . ? N2 C1' N2' C2 -66.6(12) . . . . ? C3' C1' N2' C2 24.3(10) . . . . ? C1 C1' N2' C4' 120.9(11) . . . . ? N1' C1' N2' C4' -165.9(11) . . . . ? N1 C1' N2' C4' -178.8(10) . . . . ? N2 C1' N2' C4' 118.3(16) . . . . ? C3' C1' N2' C4' -150.9(11) . . . . ? N1' C1' N2' C1 73.2(9) . . . . ? N1 C1' N2' C1 60.2(9) . . . . ? N2 C1' N2' C1 -2.7(12) . . . . ? C3' C1' N2' C1 88.1(7) . . . . ? C1 C1' N2' C4 49.2(11) . . . . ? N1' C1' N2' C4 122.4(10) . . . . ? N1 C1' N2' C4 109.4(10) . . . . ? N2 C1' N2' C4 46.5(10) . . . . ? C3' C1' N2' C4 137.3(9) . . . . ? C5 C4' N2' N2 -17(3) . . . . ? C5' C4' N2' N2 -28.6(18) . . . . ? C4 C4' N2' N2 -2.2(13) . . . . ? C5 C4' N2' C2' 82(2) . . . . ? C5' C4' N2' C2' 70.3(16) . . . . ? C4 C4' N2' C2' 96.6(12) . . . . ? N2 C4' N2' C2' 98.9(17) . . . . ? C5 C4' N2' C2 57(3) . . . . ? C5' C4' N2' C2 45.8(19) . . . . ? C4 C4' N2' C2 72.2(14) . . . . ? N2 C4' N2' C2 74.4(15) . . . . ? C5 C4' N2' C1' -129(2) . . . . ? C5' C4' N2' C1' -140.0(12) . . . . ? C4 C4' N2' C1' -113.6(11) . . . . ? N2 C4' N2' C1' -111.4(17) . . . . ? C5 C4' N2' C1 -84(2) . . . . ? C5' C4' N2' C1 -95.1(14) . . . . ? C4 C4' N2' C1 -68.8(12) . . . . ? N2 C4' N2' C1 -66.5(14) . . . . ? C5 C4' N2' C4 -15.1(18) . . . . ? C5' C4' N2' C4 -26.3(9) . . . . ? N2 C4' N2' C4 2.2(13) . . . . ? C1' C1 N2' N2 -176.9(14) . . . . ? N1 C1 N2' N2 116.8(12) . . . . ? N1' C1 N2' N2 124.6(12) . . . . ? C3 C1 N2' N2 86.1(11) . . . . ? C1' C1 N2' C2' 106.7(11) . . . . ? N1 C1 N2' C2' 40.4(11) . . . . ? N2 C1 N2' C2' -76.4(12) . . . . ? N1' C1 N2' C2' 48.2(10) . . . . ? C3 C1 N2' C2' 9.7(8) . . . . ? C1' C1 N2' C2 123.3(11) . . . . ? N1 C1 N2' C2 57.0(10) . . . . ? N2 C1 N2' C2 -59.8(10) . . . . ? N1' C1 N2' C2 64.8(9) . . . . ? C3 C1 N2' C2 26.3(7) . . . . ? N1 C1 N2' C1' -66.3(9) . . . . ? N2 C1 N2' C1' 176.9(14) . . . . ? N1' C1 N2' C1' -58.5(9) . . . . ? C3 C1 N2' C1' -97.0(8) . . . . ? C1' C1 N2' C4' -85.9(14) . . . . ? N1 C1 N2' C4' -152.1(12) . . . . ? N2 C1 N2' C4' 91.1(15) . . . . ? N1' C1 N2' C4' -144.4(13) . . . . ? C3 C1 N2' C4' 177.2(13) . . . . ? C1' C1 N2' C4 -140.4(9) . . . . ? N1 C1 N2' C4 153.3(8) . . . . ? N2 C1 N2' C4 36.5(9) . . . . ? N1' C1 N2' C4 161.1(8) . . . . ? C3 C1 N2' C4 122.6(6) . . . . ? C5' C4 N2' N2 -155.3(15) . . . . ? C5 C4 N2' N2 -174.5(15) . . . . ? C4' C4 N2' N2 177.3(16) . . . . ? C5' C4 N2' C2' -89.8(12) . . . . ? N2 C4 N2' C2' 65.5(13) . . . . ? C5 C4 N2' C2' -109.1(11) . . . . ? C4' C4 N2' C2' -117.3(12) . . . . ? C5' C4 N2' C2 -104.8(11) . . . . ? N2 C4 N2' C2 50.5(11) . . . . ? C5 C4 N2' C2 -124.1(11) . . . . ? C4' C4 N2' C2 -132.3(11) . . . . ? C5' C4 N2' C1' 134.6(11) . . . . ? N2 C4 N2' C1' -70.1(13) . . . . ? C5 C4 N2' C1' 115.4(11) . . . . ? C4' C4 N2' C1' 107.2(12) . . . . ? C5' C4 N2' C4' 27.5(10) . . . . ? N2 C4 N2' C4' -177.3(16) . . . . ? C5 C4 N2' C4' 8.2(10) . . . . ? C5' C4 N2' C1 162.7(9) . . . . ? N2 C4 N2' C1 -42.0(10) . . . . ? C5 C4 N2' C1 143.4(9) . . . . ? C4' C4 N2' C1 135.2(10) . . . . ? C2' N2' N2 C2 1.1(11) . . . . ? C1' N2' N2 C2 -110.2(8) . . . . ? C4' N2' N2 C2 125.1(11) . . . . ? C1 N2' N2 C2 -108.3(7) . . . . ? C4 N2' N2 C2 122.5(9) . . . . ? C2' N2' N2 C1 109.4(9) . . . . ? C2 N2' N2 C1 108.3(7) . . . . ? C1' N2' N2 C1 -1.9(9) . . . . ? C4' N2' N2 C1 -126.6(10) . . . . ? C4 N2' N2 C1 -129.2(10) . . . . ? C2 N2' N2 C2' -1.1(11) . . . . ? C1' N2' N2 C2' -111.3(10) . . . . ? C4' N2' N2 C2' 124.0(13) . . . . ? C1 N2' N2 C2' -109.4(9) . . . . ? C4 N2' N2 C2' 121.5(10) . . . . ? C2' N2' N2 C4 -121.5(10) . . . . ? C2 N2' N2 C4 -122.5(9) . . . . ? C1' N2' N2 C4 127.2(8) . . . . ? C4' N2' N2 C4 2.5(14) . . . . ? C1 N2' N2 C4 129.2(10) . . . . ? C2' N2' N2 C1' 111.3(10) . . . . ? C2 N2' N2 C1' 110.2(8) . . . . ? C4' N2' N2 C1' -124.7(14) . . . . ? C1 N2' N2 C1' 1.9(9) . . . . ? C4 N2' N2 C1' -127.2(8) . . . . ? C2' N2' N2 C4' -124.0(13) . . . . ? C2 N2' N2 C4' -125.1(11) . . . . ? C1' N2' N2 C4' 124.7(14) . . . . ? C1 N2' N2 C4' 126.6(10) . . . . ? C4 N2' N2 C4' -2.5(14) . . . . ? C3 C2 N2 N2' 93.6(13) . . . . ? C3' C2 N2 N2' 64.0(13) . . . . ? N2' C2 N2 C1 -89.8(11) . . . . ? C3 C2 N2 C1 3.8(14) . . . . ? C3' C2 N2 C1 -25.8(14) . . . . ? N2' C2 N2 C2' 3(3) . . . . ? C3 C2 N2 C2' 97(3) . . . . ? C3' C2 N2 C2' 67(3) . . . . ? N2' C2 N2 C4 105.6(13) . . . . ? C3 C2 N2 C4 -160.8(9) . . . . ? C3' C2 N2 C4 169.6(9) . . . . ? N2' C2 N2 C1' -52.8(10) . . . . ? C3 C2 N2 C1' 40.8(13) . . . . ? C3' C2 N2 C1' 11.2(12) . . . . ? N2' C2 N2 C4' 40.5(10) . . . . ? C3 C2 N2 C4' 134.1(11) . . . . ? C3' C2 N2 C4' 104.5(11) . . . . ? C1' C1 N2 N2' 2.7(12) . . . . ? N1 C1 N2 N2' -70.4(13) . . . . ? N1' C1 N2 N2' -58.8(13) . . . . ? C3 C1 N2 N2' -84.5(11) . . . . ? C1' C1 N2 C2 84.7(11) . . . . ? N1 C1 N2 C2 11.6(13) . . . . ? N1' C1 N2 C2 23.2(12) . . . . ? N2' C1 N2 C2 82.0(12) . . . . ? C3 C1 N2 C2 -2.5(9) . . . . ? C1' C1 N2 C2' 65.1(10) . . . . ? N1 C1 N2 C2' -8.1(12) . . . . ? N1' C1 N2 C2' 3.5(11) . . . . ? N2' C1 N2 C2' 62.4(10) . . . . ? C3 C1 N2 C2' -22.2(8) . . . . ? C1' C1 N2 C4 -111.1(10) . . . . ? N1 C1 N2 C4 175.8(9) . . . . ? N1' C1 N2 C4 -172.7(9) . . . . ? N2' C1 N2 C4 -113.8(15) . . . . ? C3 C1 N2 C4 161.7(9) . . . . ? N1 C1 N2 C1' -73.1(10) . . . . ? N1' C1 N2 C1' -61.5(9) . . . . ? N2' C1 N2 C1' -2.7(12) . . . . ? C3 C1 N2 C1' -87.2(8) . . . . ? C1' C1 N2 C4' -40.4(10) . . . . ? N1 C1 N2 C4' -113.5(10) . . . . ? N1' C1 N2 C4' -101.9(9) . . . . ? N2' C1 N2 C4' -43.1(10) . . . . ? C3 C1 N2 C4' -127.6(8) . . . . ? C3' C2' N2 N2' 88.7(13) . . . . ? C3 C2' N2 N2' 114.3(13) . . . . ? N2' C2' N2 C2 -177(3) . . . . ? C3' C2' N2 C2 -88(3) . . . . ? C3 C2' N2 C2 -62(3) . . . . ? N2' C2' N2 C1 -83.2(12) . . . . ? C3' C2' N2 C1 5.5(12) . . . . ? C3 C2' N2 C1 31.1(10) . . . . ? N2' C2' N2 C4 93.0(13) . . . . ? C3' C2' N2 C4 -178.3(9) . . . . ? C3 C2' N2 C4 -152.7(9) . . . . ? N2' C2' N2 C1' -50.7(10) . . . . ? C3' C2' N2 C1' 38.0(10) . . . . ? C3 C2' N2 C1' 63.6(8) . . . . ? N2' C2' N2 C4' 38.5(11) . . . . ? C3' C2' N2 C4' 127.2(10) . . . . ? C3 C2' N2 C4' 152.8(9) . . . . ? C5' C4 N2 N2' 28.4(17) . . . . ? C5 C4 N2 N2' 5.8(16) . . . . ? C4' C4 N2 N2' -2.2(13) . . . . ? C5' C4 N2 C2 -63.1(16) . . . . ? C5 C4 N2 C2 -85.7(14) . . . . ? C4' C4 N2 C2 -93.8(12) . . . . ? N2' C4 N2 C2 -91.5(14) . . . . ? C5' C4 N2 C1 134.9(11) . . . . ? C5 C4 N2 C1 112.4(11) . . . . ? C4' C4 N2 C1 104.3(10) . . . . ? N2' C4 N2 C1 106.5(16) . . . . ? C5' C4 N2 C2' -40.6(16) . . . . ? C5 C4 N2 C2' -63.2(14) . . . . ? C4' C4 N2 C2' -71.2(11) . . . . ? N2' C4 N2 C2' -69.0(12) . . . . ? C5' C4 N2 C1' 88.6(13) . . . . ? C5 C4 N2 C1' 66.0(13) . . . . ? C4' C4 N2 C1' 58.0(10) . . . . ? N2' C4 N2 C1' 60.2(13) . . . . ? C5' C4 N2 C4' 30.6(11) . . . . ? C5 C4 N2 C4' 8.0(10) . . . . ? N2' C4 N2 C4' 2.2(13) . . . . ? C1 C1' N2 N2' -176.7(15) . . . . ? N1' C1' N2 N2' -108.6(13) . . . . ? N1 C1' N2 N2' -120.1(13) . . . . ? C3' C1' N2 N2' -79.3(12) . . . . ? C1 C1' N2 C2 -105.2(11) . . . . ? N1' C1' N2 C2 -37.1(11) . . . . ? N2' C1' N2 C2 71.5(12) . . . . ? N1 C1' N2 C2 -48.6(10) . . . . ? C3' C1' N2 C2 -7.8(8) . . . . ? N1' C1' N2 C1 68.1(9) . . . . ? N2' C1' N2 C1 176.7(15) . . . . ? N1 C1' N2 C1 56.6(8) . . . . ? C3' C1' N2 C1 97.5(8) . . . . ? C1 C1' N2 C2' -120.6(10) . . . . ? N1' C1' N2 C2' -52.4(10) . . . . ? N2' C1' N2 C2' 56.2(12) . . . . ? N1 C1' N2 C2' -64.0(9) . . . . ? C3' C1' N2 C2' -23.1(7) . . . . ? C1 C1' N2 C4 98.6(11) . . . . ? N1' C1' N2 C4 166.7(9) . . . . ? N2' C1' N2 C4 -84.7(14) . . . . ? N1 C1' N2 C4 155.2(9) . . . . ? C3' C1' N2 C4 -163.9(9) . . . . ? C1 C1' N2 C4' 145.2(9) . . . . ? N1' C1' N2 C4' -146.6(9) . . . . ? N2' C1' N2 C4' -38.0(11) . . . . ? N1 C1' N2 C4' -158.2(8) . . . . ? C3' C1' N2 C4' -117.3(6) . . . . ? C5 C4' N2 N2' 166(2) . . . . ? C5' C4' N2 N2' 153.2(17) . . . . ? C4 C4' N2 N2' 177.2(16) . . . . ? C5 C4' N2 C2 106.7(16) . . . . ? C5' C4' N2 C2 94.2(10) . . . . ? N2' C4' N2 C2 -59.1(13) . . . . ? C4 C4' N2 C2 118.1(9) . . . . ? C5 C4' N2 C1 -128.6(15) . . . . ? C5' C4' N2 C1 -141.1(9) . . . . ? N2' C4' N2 C1 65.6(14) . . . . ? C4 C4' N2 C1 -117.2(9) . . . . ? C5 C4' N2 C2' 118.0(16) . . . . ? C5' C4' N2 C2' 105.4(10) . . . . ? N2' C4' N2 C2' -47.8(13) . . . . ? C4 C4' N2 C2' 129.4(9) . . . . ? C5 C4' N2 C4 -11.4(14) . . . . ? C5' C4' N2 C4 -23.9(8) . . . . ? N2' C4' N2 C4 -177.2(16) . . . . ? C5 C4' N2 C1' -151.1(15) . . . . ? C5' C4' N2 C1' -163.7(9) . . . . ? N2' C4' N2 C1' 43.1(13) . . . . ? C4 C4' N2 C1' -139.7(8) . . . . ? N4' C6 N3 C6' -87.7(11) . . . . ? N4 C6 N3 C6' -53.4(8) . . . . ? C6' C6 N3 C8 99.6(8) . . . . ? N4' C6 N3 C8 11.9(9) . . . . ? N4 C6 N3 C8 46.2(6) . . . . ? C6' C6 N3 Zn1 -99.8(8) . . . . ? N4' C6 N3 Zn1 172.5(5) . . . . ? N4 C6 N3 Zn1 -153.2(4) . . . . ? N4 C6' N3 C6 77.8(10) . . . . ? N4' C6' N3 C6 49.1(7) . . . . ? C6 C6' N3 C8 -90.1(8) . . . . ? N4 C6' N3 C8 -12.3(9) . . . . ? N4' C6' N3 C8 -41.0(6) . . . . ? C6 C6' N3 Zn1 108.2(8) . . . . ? N4 C6' N3 Zn1 -174.0(5) . . . . ? N4' C6' N3 Zn1 157.3(4) . . . . ? C7 C8 N3 C6 -19.7(7) . . . . ? C7 C8 N3 C6' 20.3(7) . . . . ? C7 C8 N3 Zn1 -179.5(3) . . . . ? O3 Zn1 N3 C6 122.2(6) 3_757 . . . ? O1 Zn1 N3 C6 -126.2(6) . . . . ? N1 Zn1 N3 C6 -8.5(7) 2_645 . . . ? N1' Zn1 N3 C6 -1.8(7) 2_645 . . . ? O3 Zn1 N3 C6' 74.6(6) 3_757 . . . ? O1 Zn1 N3 C6' -173.9(6) . . . . ? N1 Zn1 N3 C6' -56.1(7) 2_645 . . . ? N1' Zn1 N3 C6' -49.4(7) 2_645 . . . ? O3 Zn1 N3 C8 -82.5(4) 3_757 . . . ? O1 Zn1 N3 C8 29.0(4) . . . . ? N1 Zn1 N3 C8 146.8(5) 2_645 . . . ? N1' Zn1 N3 C8 153.5(5) 2_645 . . . ? C6 C6' N4 N4' 4.5(10) . . . . ? N3 C6' N4 N4' -62.8(10) . . . . ? C6 C6' N4 C7 68.4(9) . . . . ? N3 C6' N4 C7 1.2(10) . . . . ? N4' C6' N4 C7 63.9(7) . . . . ? C6 C6' N4 C9 -110.7(12) . . . . ? N3 C6' N4 C9 -177.9(8) . . . . ? N4' C6' N4 C9 -115.2(13) . . . . ? N3 C6' N4 C6 -67.2(9) . . . . ? N4' C6' N4 C6 -4.5(10) . . . . ? C6 C6' N4 C9' -39.2(11) . . . . ? N3 C6' N4 C9' -106.4(8) . . . . ? N4' C6' N4 C9' -43.6(8) . . . . ? C8 C7 N4 N4' 96.2(7) . . . . ? C8 C7 N4 C6' 10.4(8) . . . . ? N4' C7 N4 C6' -85.8(9) . . . . ? C8 C7 N4 C9 -170.5(8) . . . . ? N4' C7 N4 C9 93.3(11) . . . . ? C8 C7 N4 C6 42.6(6) . . . . ? N4' C7 N4 C6 -53.6(7) . . . . ? C8 C7 N4 C9' 133.5(5) . . . . ? N4' C7 N4 C9' 37.3(6) . . . . ? C10 C9 N4 N4' 27.9(15) . . . . ? C10' C9 N4 N4' 3.0(13) . . . . ? C9' C9 N4 N4' -3.7(10) . . . . ? C10 C9 N4 C6' 136.6(11) . . . . ? C10' C9 N4 C6' 111.8(12) . . . . ? C9' C9 N4 C6' 105.1(11) . . . . ? N4' C9 N4 C6' 108.8(14) . . . . ? C10 C9 N4 C7 -42.3(15) . . . . ? C10' C9 N4 C7 -67.1(12) . . . . ? C9' C9 N4 C7 -73.9(10) . . . . ? N4' C9 N4 C7 -70.2(10) . . . . ? C10 C9 N4 C6 91.5(13) . . . . ? C10' C9 N4 C6 66.7(13) . . . . ? C9' C9 N4 C6 59.9(11) . . . . ? N4' C9 N4 C6 63.7(11) . . . . ? C10 C9 N4 C9' 31.6(10) . . . . ? C10' C9 N4 C9' 6.7(8) . . . . ? N4' C9 N4 C9' 3.7(10) . . . . ? C6' C6 N4 N4' -174.8(12) . . . . ? N3 C6 N4 N4' -113.0(9) . . . . ? N3 C6 N4 C6' 61.8(8) . . . . ? N4' C6 N4 C6' 174.8(12) . . . . ? C6' C6 N4 C7 -117.1(9) . . . . ? N3 C6 N4 C7 -55.3(6) . . . . ? N4' C6 N4 C7 57.7(7) . . . . ? C6' C6 N4 C9 98.6(12) . . . . ? N3 C6 N4 C9 160.4(9) . . . . ? N4' C6 N4 C9 -86.6(12) . . . . ? C6' C6 N4 C9' 146.5(9) . . . . ? N3 C6 N4 C9' -151.6(6) . . . . ? N4' C6 N4 C9' -38.7(8) . . . . ? C10' C9' N4 N4' 166.1(17) . . . . ? C10 C9' N4 N4' 153.9(12) . . . . ? C9 C9' N4 N4' 175.3(12) . . . . ? C10' C9' N4 C6' -127.1(13) . . . . ? C10 C9' N4 C6' -139.3(8) . . . . ? N4' C9' N4 C6' 66.8(11) . . . . ? C9 C9' N4 C6' -117.9(9) . . . . ? C10' C9' N4 C7 119.4(12) . . . . ? C10 C9' N4 C7 107.2(7) . . . . ? N4' C9' N4 C7 -46.6(9) . . . . ? C9 C9' N4 C7 128.6(7) . . . . ? C10' C9' N4 C9 -9.2(11) . . . . ? C10 C9' N4 C9 -21.4(7) . . . . ? N4' C9' N4 C9 -175.3(12) . . . . ? C10' C9' N4 C6 -148.3(12) . . . . ? C10 C9' N4 C6 -160.5(7) . . . . ? N4' C9' N4 C6 45.6(9) . . . . ? C9 C9' N4 C6 -139.1(8) . . . . ? C6' N4 N4' C7 107.1(6) . . . . ? C9 N4 N4' C7 -122.2(7) . . . . ? C6 N4 N4' C7 110.1(5) . . . . ? C9' N4 N4' C7 -126.5(9) . . . . ? C6' N4 N4' C6 -3.0(7) . . . . ? C7 N4 N4' C6 -110.1(5) . . . . ? C9 N4 N4' C6 127.7(7) . . . . ? C9' N4 N4' C6 123.4(9) . . . . ? C6' N4 N4' C9' -126.4(8) . . . . ? C7 N4 N4' C9' 126.5(9) . . . . ? C9 N4 N4' C9' 4.3(11) . . . . ? C6 N4 N4' C9' -123.4(9) . . . . ? C7 N4 N4' C6' -107.1(6) . . . . ? C9 N4 N4' C6' 130.7(9) . . . . ? C6 N4 N4' C6' 3.0(7) . . . . ? C9' N4 N4' C6' 126.4(8) . . . . ? C6' N4 N4' C9 -130.7(9) . . . . ? C7 N4 N4' C9 122.2(7) . . . . ? C6 N4 N4' C9 -127.7(7) . . . . ? C9' N4 N4' C9 -4.3(11) . . . . ? C8 C7 N4' N4 -92.5(7) . . . . ? C8 C7 N4' C6 -10.9(9) . . . . ? N4 C7 N4' C6 81.6(9) . . . . ? C8 C7 N4' C9' 167.6(9) . . . . ? N4 C7 N4' C9' -99.8(11) . . . . ? C8 C7 N4' C6' -41.8(6) . . . . ? N4 C7 N4' C6' 50.8(7) . . . . ? C8 C7 N4' C9 -131.5(5) . . . . ? N4 C7 N4' C9 -38.9(6) . . . . ? C6' C6 N4' N4 4.5(10) . . . . ? N3 C6 N4' N4 75.6(10) . . . . ? C6' C6 N4' C7 -71.9(10) . . . . ? N3 C6 N4' C7 -0.8(11) . . . . ? N4 C6 N4' C7 -76.4(8) . . . . ? C6' C6 N4' C9' 109.5(11) . . . . ? N3 C6 N4' C9' -179.4(8) . . . . ? N4 C6 N4' C9' 105.0(12) . . . . ? N3 C6 N4' C6' 71.1(9) . . . . ? N4 C6 N4' C6' -4.5(10) . . . . ? C6' C6 N4' C9 42.8(10) . . . . ? N3 C6 N4' C9 113.9(8) . . . . ? N4 C6 N4' C9 38.3(7) . . . . ? C10' C9' N4' N4 -18(2) . . . . ? C10 C9' N4' N4 -28.1(13) . . . . ? C9 C9' N4' N4 -3.6(9) . . . . ? C10' C9' N4' C7 69(2) . . . . ? C10 C9' N4' C7 58.7(14) . . . . ? C9 C9' N4' C7 83.2(10) . . . . ? N4 C9' N4' C7 86.8(11) . . . . ? C10' C9' N4' C6 -112.8(19) . . . . ? C10 C9' N4' C6 -123.0(11) . . . . ? C9 C9' N4' C6 -98.5(10) . . . . ? N4 C9' N4' C6 -94.9(13) . . . . ? C10' C9' N4' C6' -73(2) . . . . ? C10 C9' N4' C6' -83.2(12) . . . . ? C9 C9' N4' C6' -58.7(10) . . . . ? N4 C9' N4' C6' -55.1(9) . . . . ? C10' C9' N4' C9 -14.3(16) . . . . ? C10 C9' N4' C9 -24.5(7) . . . . ? N4 C9' N4' C9 3.6(9) . . . . ? C6 C6' N4' N4 -174.4(13) . . . . ? N3 C6' N4' N4 123.0(9) . . . . ? C6 C6' N4' C7 115.0(10) . . . . ? N3 C6' N4' C7 52.4(7) . . . . ? N4 C6' N4' C7 -70.5(8) . . . . ? N3 C6' N4' C6 -62.6(8) . . . . ? N4 C6' N4' C6 174.4(13) . . . . ? C6 C6' N4' C9' -94.3(12) . . . . ? N3 C6' N4' C9' -156.9(8) . . . . ? N4 C6' N4' C9' 80.1(11) . . . . ? C6 C6' N4' C9 -141.3(10) . . . . ? N3 C6' N4' C9 156.1(6) . . . . ? N4 C6' N4' C9 33.2(7) . . . . ? C10 C9 N4' N4 -156.7(13) . . . . ? C10' C9 N4' N4 -177.2(12) . . . . ? C9' C9 N4' N4 175.2(13) . . . . ? C10 C9 N4' C7 -98.1(9) . . . . ? N4 C9 N4' C7 58.6(8) . . . . ? C10' C9 N4' C7 -118.6(8) . . . . ? C9' C9 N4' C7 -126.2(9) . . . . ? C10 C9 N4' C6 144.3(9) . . . . ? N4 C9 N4' C6 -59.0(10) . . . . ? C10' C9 N4' C6 123.8(9) . . . . ? C9' C9 N4' C6 116.2(10) . . . . ? C10 C9 N4' C9' 28.1(9) . . . . ? N4 C9 N4' C9' -175.2(13) . . . . ? C10' C9 N4' C9' 7.7(9) . . . . ? C10 C9 N4' C6' 165.7(8) . . . . ? N4 C9 N4' C6' -37.7(8) . . . . ? C10' C9 N4' C6' 145.2(8) . . . . ? C9' C9 N4' C6' 137.5(8) . . . . ? O2 C11 O1 Zn1 -3.8(4) . . . . ? C12 C11 O1 Zn1 179.9(2) . . . . ? O3 Zn1 O1 C11 -72.0(3) 3_757 . . . ? N1 Zn1 O1 C11 63.3(4) 2_645 . . . ? N1' Zn1 O1 C11 54.2(4) 2_645 . . . ? N3 Zn1 O1 C11 172.8(2) . . . . ? O4 C14 O3 Zn1 -5.7(6) . . . 3_757 ? C13 C14 O3 Zn1 173.9(3) . . . 3_757 ? 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 O1W H2 O1 0.89(3) 2.13(4) 3.004(5) 165(7) 3_757 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.755 _refine_diff_density_min -0.616 _refine_diff_density_rms 0.101 #===End data_compound-9 _database_code_depnum_ccdc_archive 'CCDC 648898' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H19 Co N4 O5' _chemical_formula_weight 382.26 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' Co Co 0.3494 0.9721 '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)/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.348(7) _cell_length_b 17.557(15) _cell_length_c 11.288(9) _cell_angle_alpha 90.00 _cell_angle_beta 103.5190(10) _cell_angle_gamma 90.00 _cell_volume 1609(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2659 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 28.3 _exptl_crystal_description Block _exptl_crystal_colour Violet _exptl_crystal_size_max 0.287 _exptl_crystal_size_mid 0.246 _exptl_crystal_size_min 0.178 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.578 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 792 _exptl_absorpt_coefficient_mu 1.100 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.746 _exptl_absorpt_correction_T_max 0.864 _exptl_absorpt_process_details 'SADABS(Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 9619 _diffrn_reflns_av_R_equivalents 0.0504 _diffrn_reflns_av_sigmaI/netI 0.0571 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 28.34 _reflns_number_total 3751 _reflns_number_gt 2683 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97(Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _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^)+(0.0706P)^2^+1.4577P] 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 3751 _refine_ls_number_parameters 267 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0759 _refine_ls_R_factor_gt 0.0503 _refine_ls_wR_factor_ref 0.1416 _refine_ls_wR_factor_gt 0.1272 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _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 0.7133(13) 0.0792(7) -0.5283(9) 0.061(3) Uani 0.50 1 d P . . C1' C 0.8053(10) 0.0560(5) -0.5022(7) 0.0317(16) Uiso 0.50 1 d P . . C2' C 0.9200(16) 0.1588(8) -0.5272(13) 0.050(4) Uiso 0.50 1 d P . . C2 C 0.8714(15) 0.1736(6) -0.5436(8) 0.033(2) Uani 0.50 1 d P . . C3' C 0.8887(11) 0.1151(6) -0.6293(9) 0.039(2) Uiso 0.50 1 d P . . C3 C 0.8214(13) 0.1329(5) -0.6481(7) 0.0362(18) Uani 0.50 1 d P . . C4 C 0.7947(11) 0.3806(5) 0.0361(7) 0.0402(18) Uiso 0.50 1 d P . . C4' C 0.8986(10) 0.3796(4) 0.0540(6) 0.0301(15) Uani 0.50 1 d P . . C5 C 0.8298(5) 0.3142(2) 0.1957(3) 0.0431(10) Uani 1 1 d . . . H5 H 0.8227 0.3013 0.2742 0.052 Uiso 1 1 calc R . . C6 C 0.8287(6) 0.2635(2) 0.1079(4) 0.0458(10) Uani 1 1 d . . . C7 C 0.7361(13) 0.2786(7) -0.1229(9) 0.076(4) Uani 0.50 1 d P . . C7' C 0.9408(11) 0.2741(6) -0.0902(8) 0.052(2) Uiso 0.50 1 d P . . C8' C 0.8657(11) 0.2293(5) -0.1558(7) 0.044(2) Uani 0.50 1 d P . . C8 C 0.7880(15) 0.2500(8) -0.1793(11) 0.065(3) Uiso 0.50 1 d P . . C9 C 0.8628(15) 0.2097(7) -0.2829(11) 0.063(3) Uiso 0.50 1 d P . . C9' C 0.7875(14) 0.2109(9) -0.2987(10) 0.065(6) Uani 0.50 1 d P . . C10 C 0.9194(15) 0.1399(7) -0.3183(8) 0.044(3) Uani 0.40 1 d P . . C10' C 0.731(2) 0.1884(10) -0.3787(15) 0.057(4) Uiso 0.30 1 d P . . C10" C 0.8445(19) 0.1489(10) -0.3192(14) 0.040(4) Uiso 0.30 1 d P . . C11 C 1.1635(4) 0.5244(2) 0.2979(3) 0.0368(9) Uani 1 1 d . . . C12 C 1.3342(4) 0.5463(3) 0.3702(3) 0.0410(9) Uani 1 1 d . . . H12A H 1.4070 0.5501 0.3148 0.049 Uiso 1 1 calc R . . H12B H 1.3286 0.5963 0.4057 0.049 Uiso 1 1 calc R . . C13 C 1.4078(4) 0.4909(2) 0.4708(3) 0.0295(7) Uani 1 1 d . . . H13 H 1.4043 0.4403 0.4335 0.035 Uiso 1 1 calc R . . C14 C 1.3128(4) 0.4858(2) 0.5693(3) 0.0287(7) Uani 1 1 d . . . N1 N 0.7696(4) 0.06204(18) -0.6247(2) 0.0341(7) Uani 1 1 d . . . N2 N 0.7949(13) 0.1386(6) -0.4679(9) 0.065(3) Uani 0.50 1 d P . . N2' N 0.8642(9) 0.1224(5) -0.4504(7) 0.0301(18) Uiso 0.50 1 d P . . N3 N 0.8424(4) 0.38725(17) 0.1578(2) 0.0350(7) Uani 1 1 d . . . N4' N 0.8928(8) 0.3065(3) 0.0199(5) 0.0334(13) Uani 0.50 1 d P . . N4 N 0.7871(9) 0.3061(4) 0.0038(6) 0.0415(16) Uiso 0.50 1 d P . . O1 O 1.1291(4) 0.5279(2) 0.1856(2) 0.0641(10) Uani 1 1 d . . . O2 O 1.0611(3) 0.50495(16) 0.3576(2) 0.0401(7) Uani 1 1 d . . . O3 O 1.2643(3) 0.42306(17) 0.5972(2) 0.0431(7) Uani 1 1 d . . . O4 O 1.2919(3) 0.54656(16) 0.6266(2) 0.0357(6) Uani 1 1 d . . . Co1 Co 0.84113(5) 0.48580(3) 0.25362(4) 0.02411(15) Uani 1 1 d . . . O1W O 0.9645(5) 0.34499(19) 0.5012(3) 0.0672(10) Uani 1 1 d D . . H1A H 0.888(5) 0.377(3) 0.474(5) 0.101 Uiso 1 1 d D . . H1B H 1.061(4) 0.367(3) 0.533(5) 0.101 Uiso 1 1 d 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 C1 0.063(6) 0.076(7) 0.056(5) -0.040(5) 0.041(5) -0.035(6) C2 0.047(6) 0.027(5) 0.025(4) -0.007(3) 0.009(4) -0.004(5) C3 0.063(6) 0.024(4) 0.022(3) -0.002(3) 0.011(4) -0.005(4) C4' 0.043(4) 0.024(4) 0.026(3) -0.003(3) 0.014(3) -0.003(3) C5 0.069(3) 0.033(2) 0.0317(19) -0.0012(16) 0.0206(18) -0.0020(19) C6 0.063(3) 0.037(2) 0.037(2) -0.0050(17) 0.0106(19) -0.002(2) C7 0.075(7) 0.100(9) 0.048(5) -0.050(6) 0.002(5) 0.029(6) C8' 0.055(5) 0.055(5) 0.020(3) -0.027(3) 0.004(3) 0.013(4) C9' 0.045(6) 0.172(14) 0.071(7) -0.058(9) 0.023(5) -0.027(7) C10 0.046(6) 0.060(8) 0.023(4) -0.023(4) 0.004(4) 0.022(5) C11 0.0319(18) 0.054(3) 0.0240(16) 0.0059(16) 0.0047(13) 0.0081(16) C12 0.0340(19) 0.055(3) 0.0345(19) 0.0147(18) 0.0088(15) -0.0005(18) C13 0.0257(16) 0.042(2) 0.0200(14) -0.0005(14) 0.0039(12) -0.0011(15) C14 0.0212(14) 0.041(2) 0.0217(14) 0.0053(15) 0.0013(11) 0.0032(15) N1 0.0453(17) 0.0342(17) 0.0232(13) -0.0057(12) 0.0085(12) -0.0088(14) N2 0.077(7) 0.071(7) 0.060(5) -0.052(5) 0.042(6) -0.036(6) N3 0.0527(19) 0.0303(17) 0.0229(13) -0.0013(12) 0.0108(13) -0.0003(14) N4' 0.051(4) 0.028(3) 0.023(3) -0.008(2) 0.014(3) -0.008(3) O1 0.0566(19) 0.111(3) 0.0212(13) 0.0088(15) 0.0019(12) -0.0036(18) O2 0.0292(12) 0.063(2) 0.0272(12) -0.0005(12) 0.0049(10) -0.0050(12) O3 0.0429(15) 0.0439(17) 0.0411(14) 0.0162(13) 0.0071(12) -0.0037(13) O4 0.0364(13) 0.0449(16) 0.0273(12) -0.0033(11) 0.0109(10) 0.0000(12) Co1 0.0284(2) 0.0249(2) 0.0184(2) 0.00041(18) 0.00437(16) 0.00026(19) O1W 0.074(2) 0.0347(18) 0.081(3) -0.0118(16) -0.006(2) -0.0001(17) _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 C1' 0.859(12) . ? C1 N1 1.317(8) . ? C1 N2 1.341(12) . ? C1 N2' 1.555(12) . ? C1' N1 1.348(8) . ? C1' N2' 1.345(11) . ? C1' N2 1.509(12) . ? C2' N2' 1.252(16) . ? C2' C3' 1.358(18) . ? C2' N2 1.412(17) . ? C2' C3 1.490(16) . ? C2 N2 1.331(13) . ? C2 C3 1.358(11) . ? C2 N2' 1.396(13) . ? C2 C3' 1.440(14) . ? C3' C3 0.634(10) . ? C3' N1 1.372(10) . ? C3 N1 1.364(8) . ? C4 C4' 0.843(9) . ? C4 N3 1.343(8) . ? C4 N4 1.356(11) . ? C4 N4' 1.572(11) . ? C4' N4' 1.339(9) . ? C4' N3 1.367(7) . ? C4' N4 1.615(10) . ? C5 N3 1.364(5) . ? C5 H5 0.9300 . ? C6 N4 1.368(8) . ? C6 N4' 1.446(7) . ? C7 C8 0.987(14) . ? C7 N4 1.475(11) . ? C7 C8' 1.499(12) . ? C7 C7' 1.664(13) . ? C7 N4' 1.888(11) . ? C7' C8' 1.159(12) . ? C7' C8 1.489(14) . ? C7' N4' 1.504(10) . ? C7' N4 1.930(12) . ? C8' C8 0.736(12) . ? C8' C9 1.470(14) . ? C8' C9' 1.624(12) . ? C8 C9' 1.511(15) . ? C8 C9 1.613(17) . ? C9 C9' 0.612(13) . ? C9 C10" 1.14(2) . ? C9 C10' 1.40(2) . ? C9 C10 1.404(16) . ? C9' C10' 0.998(18) . ? C9' C10" 1.23(2) . ? C10 C10" 0.643(14) . ? C10 N2' 1.487(12) . ? C10 N2 1.765(14) . ? C10' C10" 1.24(2) . ? C10' N2 1.520(18) . ? C10' N2' 1.910(18) . ? C10" N2' 1.597(18) . ? C10" N2 1.643(18) . ? C11 O1 1.234(4) . ? C11 O2 1.253(4) . ? C11 C12 1.517(5) . ? C12 C13 1.513(5) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.512(5) . ? C13 C13 1.559(6) 3_866 ? C13 H13 0.9800 . ? C14 O3 1.240(4) . ? C14 O4 1.280(5) . ? N1 Co1 2.034(3) 2_644 ? N2 N2' 0.633(12) . ? N3 Co1 2.042(3) . ? N4' N4 0.859(8) . ? O2 Co1 1.963(3) . ? O4 Co1 2.021(3) 3_766 ? Co1 O4 2.021(3) 3_766 ? Co1 N1 2.034(3) 2_654 ? O1W H1A 0.86(3) . ? O1W H1B 0.89(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 C1' C1 N1 73.2(8) . . ? C1' C1 N2 83.5(10) . . ? N1 C1 N2 111.1(7) . . ? C1' C1 N2' 59.7(8) . . ? N1 C1 N2' 100.4(6) . . ? C1' C1 C3 87.0(9) . . ? N2 C1 C3 74.0(6) . . ? N2' C1 C3 73.8(5) . . ? C1 C1' N1 69.2(8) . . ? C1 C1' N2' 86.8(10) . . ? N1 C1' N2' 110.4(7) . . ? C1 C1' N2 62.0(9) . . ? N1 C1' N2 100.1(6) . . ? C1 C1' C3' 86.6(9) . . ? N2' C1' C3' 73.3(6) . . ? N2 C1' C3' 74.8(6) . . ? N2' C2' C3' 105.7(13) . . ? C3' C2' N2 104.0(11) . . ? N2' C2' C3 105.2(11) . . ? N2 C2' C3 92.6(10) . . ? N2 C2 C3 102.6(8) . . ? C3 C2 N2' 104.9(8) . . ? N2 C2 C3' 103.9(8) . . ? N2' C2 C3' 94.4(8) . . ? C3 C3' C2' 89.1(15) . . ? C3 C3' N1 75.9(13) . . ? C2' C3' N1 110.4(9) . . ? C3 C3' C2 69.7(13) . . ? N1 C3' C2 105.7(7) . . ? C3 C3' C1' 93.8(14) . . ? C2' C3' C1' 73.6(8) . . ? C2 C3' C1' 77.6(6) . . ? C3' C3 C2 84.3(15) . . ? C3' C3 N1 77.3(13) . . ? C2 C3 N1 111.0(7) . . ? C3' C3 C2' 65.7(14) . . ? N1 C3 C2' 103.5(8) . . ? C3' C3 C1 92.6(14) . . ? C2 C3 C1 76.1(6) . . ? C2' C3 C1 76.6(7) . . ? C4' C4 N3 73.4(8) . . ? C4' C4 N4 91.5(9) . . ? N3 C4 N4 110.0(7) . . ? C4' C4 N4' 58.4(8) . . ? N3 C4 N4' 98.8(6) . . ? C4 C4' N4' 89.2(9) . . ? C4 C4' N3 70.3(8) . . ? N4' C4' N3 110.1(6) . . ? C4 C4' N4 57.1(8) . . ? N3 C4' N4 95.4(5) . . ? C6 C5 N3 112.5(3) . . ? C6 C5 H5 123.8 . . ? N3 C5 H5 123.8 . . ? C5 C6 N4 103.3(5) . . ? C5 C6 N4' 102.9(4) . . ? C8 C7 N4 136.2(12) . . ? N4 C7 C8' 111.6(8) . . ? C8 C7 C7' 62.3(9) . . ? N4 C7 C7' 75.6(6) . . ? C8 C7 N4' 111.2(11) . . ? C8' C7 N4' 88.0(6) . . ? C7' C7 N4' 49.6(4) . . ? C8' C7' N4' 125.1(9) . . ? C8 C7' N4' 108.3(8) . . ? C8' C7' C7 61.1(7) . . ? N4' C7' C7 73.0(5) . . ? C8' C7' N4 102.6(8) . . ? C8 C7' N4 83.1(7) . . ? C7 C7' N4 47.7(4) . . ? C8 C8' C7' 101.3(15) . . ? C8 C8' C9 87.3(14) . . ? C7' C8' C9 131.7(10) . . ? C7' C8' C7 76.3(7) . . ? C9 C8' C7 121.9(9) . . ? C8 C8' C9' 68.0(13) . . ? C7' C8' C9' 143.2(11) . . ? C7 C8' C9' 102.4(8) . . ? C8' C8 C7 120.1(18) . . ? C8' C8 C7' 49.7(11) . . ? C7 C8 C7' 81.7(11) . . ? C8' C8 C9' 85.2(14) . . ? C7 C8 C9' 153.6(14) . . ? C7' C8 C9' 123.7(10) . . ? C8' C8 C9 65.6(12) . . ? C7 C8 C9 173.7(15) . . ? C7' C8 C9 101.5(9) . . ? C9' C9 C10" 83(2) . . ? C10" C9 C10' 57.1(12) . . ? C9' C9 C10 110(2) . . ? C10' C9 C10 78.6(11) . . ? C9' C9 C8' 93.2(18) . . ? C10" C9 C8' 122.7(13) . . ? C10' C9 C8' 130.3(12) . . ? C10 C9 C8' 123.5(10) . . ? C9' C9 C8 69.5(16) . . ? C10" C9 C8 128.9(14) . . ? C10' C9 C8 108.1(11) . . ? C10 C9 C8 143.3(11) . . ? C9 C9' C10' 119(2) . . ? C9 C9' C10" 67(2) . . ? C10' C9' C10" 66.4(13) . . ? C9 C9' C8 88.2(17) . . ? C10' C9' C8 152.9(15) . . ? C10" C9' C8 130.4(15) . . ? C9 C9' C8' 64.7(16) . . ? C10' C9' C8' 166.6(19) . . ? C10" C9' C8' 106.2(13) . . ? C9 C9' C10 50.5(18) . . ? C10' C9' C10 77.0(12) . . ? C8 C9' C10 125.3(11) . . ? C8' C9' C10 98.7(9) . . ? C10" C10 C9 53.1(18) . . ? C10" C10 N2' 87.9(19) . . ? C9 C10 N2' 114.8(9) . . ? N2' C10 C9' 102.9(8) . . ? C10" C10 N2 68.6(18) . . ? C9 C10 N2 97.0(9) . . ? C9' C10 N2 83.2(7) . . ? C9 C10 C10' 50.6(8) . . ? N2' C10 C10' 71.0(7) . . ? N2 C10 C10' 50.9(7) . . ? C9' C10' C10" 65.9(15) . . ? C10" C10' C9 50.8(11) . . ? C9' C10' N2 131.6(16) . . ? C10" C10' N2 72.3(12) . . ? C9 C10' N2 109.4(13) . . ? C9' C10' C10 69.8(13) . . ? C9 C10' C10 50.8(8) . . ? N2 C10' C10 64.2(8) . . ? C9' C10' N2' 115.3(15) . . ? C10" C10' N2' 56.2(10) . . ? C9 C10' N2' 93.5(10) . . ? C10 C10' N2' 47.4(5) . . ? C10 C10" C9 100(2) . . ? C10 C10" C9' 129(3) . . ? C10 C10" C10' 140(3) . . ? C9 C10" C10' 72.1(14) . . ? C9' C10" C10' 47.7(11) . . ? C10 C10" N2' 68.4(18) . . ? C9 C10" N2' 124.8(14) . . ? C9' C10" N2' 124.1(13) . . ? C10' C10" N2' 83.7(12) . . ? C10 C10" N2 90(2) . . ? C9 C10" N2 116.8(14) . . ? C9' C10" N2 105.9(13) . . ? C10' C10" N2 61.9(11) . . ? O1 C11 O2 122.8(4) . . ? O1 C11 C12 120.2(3) . . ? O2 C11 C12 117.0(3) . . ? C13 C12 C11 113.9(3) . . ? C13 C12 H12A 108.8 . . ? C11 C12 H12A 108.8 . . ? C13 C12 H12B 108.8 . . ? C11 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? C12 C13 C14 113.6(3) . . ? C12 C13 C13 111.9(4) . 3_866 ? C14 C13 C13 109.7(3) . 3_866 ? C12 C13 H13 107.1 . . ? C14 C13 H13 107.1 . . ? C13 C13 H13 107.1 3_866 . ? O3 C14 O4 121.4(3) . . ? O3 C14 C13 119.8(3) . . ? O4 C14 C13 118.7(3) . . ? C1 N1 C3 98.2(6) . . ? C1' N1 C3 105.5(5) . . ? C1 N1 C3' 106.1(6) . . ? C1' N1 C3' 96.0(6) . . ? C1 N1 Co1 123.4(4) . 2_644 ? C1' N1 Co1 129.5(4) . 2_644 ? C3 N1 Co1 125.0(4) . 2_644 ? C3' N1 Co1 129.2(4) . 2_644 ? N2' N2 C2 82.4(14) . . ? N2' N2 C1 97.4(16) . . ? C2 N2 C1 107.2(8) . . ? N2' N2 C2' 62.5(13) . . ? C1 N2 C2' 107.4(9) . . ? N2' N2 C1' 63.0(13) . . ? C2 N2 C1' 102.4(7) . . ? C2' N2 C1' 91.5(8) . . ? N2' N2 C10' 119.1(16) . . ? C2 N2 C10' 117.0(11) . . ? C1 N2 C10' 124.7(10) . . ? C2' N2 C10' 125.5(11) . . ? C1' N2 C10' 140.6(10) . . ? N2' N2 C10" 74.7(15) . . ? C2 N2 C10" 124.1(9) . . ? C1 N2 C10" 125.6(10) . . ? C2' N2 C10" 114.8(10) . . ? C1' N2 C10" 110.7(10) . . ? C10' N2 C10" 45.8(9) . . ? N2' N2 C10 54.3(13) . . ? C2 N2 C10 110.2(9) . . ? C1 N2 C10 127.8(11) . . ? C2' N2 C10 96.6(9) . . ? C1' N2 C10 101.7(9) . . ? C10' N2 C10 65.0(8) . . ? N2 N2' C2' 90.9(15) . . ? N2 N2' C1' 92.2(14) . . ? C2' N2' C1' 107.4(10) . . ? N2 N2' C2 70.9(14) . . ? C1' N2' C2 107.8(7) . . ? N2 N2' C10 105.5(15) . . ? C2' N2' C10 120.7(11) . . ? C1' N2' C10 127.7(8) . . ? C2 N2' C10 124.4(9) . . ? N2 N2' C1 58.8(13) . . ? C2' N2' C1 104.0(9) . . ? C2 N2' C1 93.4(7) . . ? C10 N2' C1 133.5(8) . . ? N2 N2' C10" 82.8(14) . . ? C2' N2' C10" 129.0(11) . . ? C1' N2' C10" 123.4(9) . . ? C2 N2' C10" 122.9(9) . . ? C1 N2' C10" 114.9(8) . . ? C2' N2' C10' 109.3(10) . . ? C1' N2' C10' 121.4(8) . . ? C2 N2' C10' 93.5(8) . . ? C10 N2' C10' 61.6(7) . . ? C1 N2' C10' 93.5(7) . . ? C4 N3 C5 102.3(5) . . ? C5 N3 C4' 104.2(4) . . ? C4 N3 Co1 125.3(4) . . ? C5 N3 Co1 128.3(2) . . ? C4' N3 Co1 125.6(4) . . ? N4 N4' C4' 91.9(8) . . ? N4 N4' C6 67.3(7) . . ? C4' N4' C6 107.3(5) . . ? N4 N4' C7' 106.3(8) . . ? C4' N4' C7' 127.0(6) . . ? C6 N4' C7' 125.7(6) . . ? N4 N4' C4 59.5(7) . . ? C6 N4' C4 93.8(5) . . ? C7' N4' C4 131.0(6) . . ? N4 N4' C7 49.0(6) . . ? C4' N4' C7 117.7(6) . . ? C6 N4' C7 99.0(6) . . ? C7' N4' C7 57.4(5) . . ? C4 N4' C7 92.2(6) . . ? N4' N4 C4 87.4(8) . . ? N4' N4 C6 77.2(7) . . ? C4 N4 C6 108.1(6) . . ? N4' N4 C7 104.9(8) . . ? C4 N4 C7 124.2(8) . . ? C6 N4 C7 127.7(8) . . ? N4' N4 C4' 56.0(6) . . ? C6 N4 C4' 97.2(5) . . ? C7 N4 C4' 127.9(8) . . ? N4' N4 C7' 48.4(6) . . ? C4 N4 C7' 115.7(7) . . ? C6 N4 C7' 104.2(5) . . ? C7 N4 C7' 56.6(5) . . ? C4' N4 C7' 91.3(5) . . ? C11 O2 Co1 112.7(2) . . ? C14 O4 Co1 105.4(2) . 3_766 ? O2 Co1 O4 103.38(12) . 3_766 ? O2 Co1 N1 121.36(13) . 2_654 ? O4 Co1 N1 115.77(12) 3_766 2_654 ? O2 Co1 N3 110.00(13) . . ? O4 Co1 N3 100.84(12) 3_766 . ? N1 Co1 N3 103.66(13) 2_654 . ? H1A O1W H1B 113(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 N2 C1 C1' N1 -114.4(7) . . . . ? N2' C1 C1' N1 -113.2(6) . . . . ? C3 C1 C1' N1 -40.2(3) . . . . ? N1 C1 C1' N2' 113.2(6) . . . . ? N2 C1 C1' N2' -1.2(8) . . . . ? C3 C1 C1' N2' 73.0(5) . . . . ? N1 C1 C1' N2 114.4(7) . . . . ? N2' C1 C1' N2 1.2(8) . . . . ? C3 C1 C1' N2 74.2(6) . . . . ? N1 C1 C1' C3' 39.8(4) . . . . ? N2 C1 C1' C3' -74.6(6) . . . . ? N2' C1 C1' C3' -73.4(6) . . . . ? C3 C1 C1' C3' -0.4(5) . . . . ? N2' C2' C3' C3 92.6(16) . . . . ? N2 C2' C3' C3 65.1(17) . . . . ? N2' C2' C3' N1 18.1(12) . . . . ? N2 C2' C3' N1 -9.5(13) . . . . ? C3 C2' C3' N1 -74.5(13) . . . . ? N2' C2' C3' C2 97(3) . . . . ? N2 C2' C3' C2 70(3) . . . . ? C3 C2' C3' C2 5(3) . . . . ? N2' C2' C3' C1' -1.6(7) . . . . ? N2 C2' C3' C1' -29.1(9) . . . . ? C3 C2' C3' C1' -94.2(14) . . . . ? N2 C2 C3' C3 90.3(16) . . . . ? N2' C2 C3' C3 115.7(15) . . . . ? N2 C2 C3' C2' -84(3) . . . . ? C3 C2 C3' C2' -175(3) . . . . ? N2' C2 C3' C2' -59(3) . . . . ? N2 C2 C3' N1 22.4(12) . . . . ? C3 C2 C3' N1 -68.0(12) . . . . ? N2' C2 C3' N1 47.7(9) . . . . ? N2 C2 C3' C1' -8.5(9) . . . . ? C3 C2 C3' C1' -98.8(14) . . . . ? N2' C2 C3' C1' 16.8(6) . . . . ? C1 C1' C3' C3 1.2(16) . . . . ? N1 C1' C3' C3 63.6(13) . . . . ? N2' C1' C3' C3 -86.5(14) . . . . ? N2 C1' C3' C3 -60.7(14) . . . . ? C1 C1' C3' C2' 89.2(10) . . . . ? N1 C1' C3' C2' 151.6(9) . . . . ? N2' C1' C3' C2' 1.5(7) . . . . ? N2 C1' C3' C2' 27.2(8) . . . . ? C1 C1' C3' N1 -62.5(8) . . . . ? N2' C1' C3' N1 -150.1(7) . . . . ? N2 C1' C3' N1 -124.4(8) . . . . ? C1 C1' C3' C2 69.4(10) . . . . ? N1 C1' C3' C2 131.9(8) . . . . ? N2' C1' C3' C2 -18.2(7) . . . . ? N2 C1' C3' C2 7.5(8) . . . . ? C2' C3' C3 C2 1.7(11) . . . . ? N1 C3' C3 C2 113.0(6) . . . . ? C1' C3' C3 C2 75.3(7) . . . . ? C2' C3' C3 N1 -111.3(8) . . . . ? C2 C3' C3 N1 -113.0(6) . . . . ? C1' C3' C3 N1 -37.8(4) . . . . ? N1 C3' C3 C2' 111.3(8) . . . . ? C2 C3' C3 C2' -1.7(11) . . . . ? C1' C3' C3 C2' 73.5(8) . . . . ? C2' C3' C3 C1 -74.0(9) . . . . ? N1 C3' C3 C1 37.3(4) . . . . ? C2 C3' C3 C1 -75.8(6) . . . . ? C1' C3' C3 C1 -0.5(7) . . . . ? N2 C2 C3 C3' -95.9(17) . . . . ? N2' C2 C3 C3' -68.5(16) . . . . ? N2 C2 C3 N1 -21.8(14) . . . . ? N2' C2 C3 N1 5.6(13) . . . . ? C3' C2 C3 N1 74.1(13) . . . . ? N2 C2 C3 C2' -91(3) . . . . ? N2' C2 C3 C2' -64(3) . . . . ? C3' C2 C3 C2' 5(3) . . . . ? N2 C2 C3 C1 -1.8(10) . . . . ? N2' C2 C3 C1 25.6(8) . . . . ? C3' C2 C3 C1 94.1(14) . . . . ? N2' C2' C3 C3' -94.5(17) . . . . ? N2 C2' C3 C3' -118.3(17) . . . . ? N2' C2' C3 C2 91(3) . . . . ? C3' C2' C3 C2 -175(3) . . . . ? N2 C2' C3 C2 67(3) . . . . ? N2' C2' C3 N1 -25.3(12) . . . . ? C3' C2' C3 N1 69.2(14) . . . . ? N2 C2' C3 N1 -49.1(10) . . . . ? N2' C2' C3 C1 4.6(9) . . . . ? C3' C2' C3 C1 99.1(15) . . . . ? N2 C2' C3 C1 -19.2(8) . . . . ? C1' C1 C3 C3' 1.2(16) . . . . ? N1 C1 C3 C3' -66.8(14) . . . . ? N2 C1 C3 C3' 85.3(16) . . . . ? N2' C1 C3 C3' 60.5(14) . . . . ? C1' C1 C3 C2 -82.3(11) . . . . ? N1 C1 C3 C2 -150.3(11) . . . . ? N2 C1 C3 C2 1.8(10) . . . . ? N2' C1 C3 C2 -23.0(8) . . . . ? C1' C1 C3 N1 67.9(9) . . . . ? N2 C1 C3 N1 152.1(11) . . . . ? N2' C1 C3 N1 127.3(9) . . . . ? C1' C1 C3 C2' -63.1(10) . . . . ? N1 C1 C3 C2' -131.0(10) . . . . ? N2 C1 C3 C2' 21.0(9) . . . . ? N2' C1 C3 C2' -3.8(7) . . . . ? N3 C4 C4' N4' 111.7(5) . . . . ? N4 C4 C4' N4' 1.2(6) . . . . ? N4 C4 C4' N3 -110.5(6) . . . . ? N4' C4 C4' N3 -111.7(5) . . . . ? N3 C4 C4' N4 110.5(6) . . . . ? N4' C4 C4' N4 -1.2(6) . . . . ? N3 C5 C6 N4 -19.1(6) . . . . ? N3 C5 C6 N4' 17.3(5) . . . . ? C8 C7 C7' C8' -20.0(12) . . . . ? N4 C7 C7' C8' 147.2(10) . . . . ? N4' C7 C7' C8' 149.0(9) . . . . ? N4 C7 C7' C8 167.1(15) . . . . ? C8' C7 C7' C8 20.0(12) . . . . ? N4' C7 C7' C8 169.0(13) . . . . ? C8 C7 C7' N4' -169.0(13) . . . . ? N4 C7 C7' N4' -1.9(5) . . . . ? C8' C7 C7' N4' -149.0(9) . . . . ? C8 C7 C7' N4 -167.1(15) . . . . ? C8' C7 C7' N4 -147.2(10) . . . . ? N4' C7 C7' N4 1.9(5) . . . . ? N4' C7' C8' C8 61.4(18) . . . . ? C7 C7' C8' C8 24.4(14) . . . . ? N4 C7' C8' C8 48.7(16) . . . . ? C8 C7' C8' C9 96.4(19) . . . . ? N4' C7' C8' C9 157.9(10) . . . . ? C7 C7' C8' C9 120.8(14) . . . . ? N4 C7' C8' C9 145.1(11) . . . . ? C8 C7' C8' C7 -24.4(14) . . . . ? N4' C7' C8' C7 37.0(11) . . . . ? N4 C7' C8' C7 24.3(7) . . . . ? C8 C7' C8' C9' 68.1(19) . . . . ? N4' C7' C8' C9' 129.6(14) . . . . ? C7 C7' C8' C9' 92.5(16) . . . . ? N4 C7' C8' C9' 116.8(14) . . . . ? N4 C7 C8' C8 -169(3) . . . . ? C7' C7 C8' C8 -135(3) . . . . ? N4' C7 C8' C8 -158(2) . . . . ? C8 C7 C8' C7' 135(3) . . . . ? N4 C7 C8' C7' -34.4(10) . . . . ? N4' C7 C8' C7' -23.1(7) . . . . ? C8 C7 C8' C9 4(2) . . . . ? N4 C7 C8' C9 -165.4(10) . . . . ? C7' C7 C8' C9 -131.0(13) . . . . ? N4' C7 C8' C9 -154.1(9) . . . . ? C8 C7 C8' C9' -8(2) . . . . ? N4 C7 C8' C9' -176.7(10) . . . . ? C7' C7 C8' C9' -142.2(11) . . . . ? N4' C7 C8' C9' -165.3(8) . . . . ? C7' C8' C8 C7 -45(2) . . . . ? C9 C8' C8 C7 -176.9(19) . . . . ? C9' C8' C8 C7 172(2) . . . . ? C9 C8' C8 C7' -132.1(12) . . . . ? C7 C8' C8 C7' 45(2) . . . . ? C9' C8' C8 C7' -143.2(10) . . . . ? C7' C8' C8 C9' 143.2(10) . . . . ? C9 C8' C8 C9' 11.1(10) . . . . ? C7 C8' C8 C9' -172(2) . . . . ? C7' C8' C8 C9 132.1(12) . . . . ? C7 C8' C8 C9 176.9(19) . . . . ? C9' C8' C8 C9 -11.1(10) . . . . ? N4 C7 C8 C8' 15(4) . . . . ? C7' C7 C8 C8' 32.9(19) . . . . ? N4' C7 C8 C8' 24(3) . . . . ? N4 C7 C8 C7' -18(2) . . . . ? C8' C7 C8 C7' -32.9(19) . . . . ? N4' C7 C8 C7' -9.0(11) . . . . ? N4 C7 C8 C9' 177(2) . . . . ? C8' C7 C8 C9' 162(5) . . . . ? C7' C7 C8 C9' -165(4) . . . . ? N4' C7 C8 C9' -174(3) . . . . ? N4' C7' C8 C8' -130.9(15) . . . . ? C7 C7' C8 C8' -142(2) . . . . ? N4 C7' C8 C8' -132.4(15) . . . . ? C8' C7' C8 C7 142(2) . . . . ? N4' C7' C8 C7 11.1(13) . . . . ? N4 C7' C8 C7 9.6(11) . . . . ? C8' C7' C8 C9' -45.8(15) . . . . ? N4' C7' C8 C9' -176.7(12) . . . . ? C7 C7' C8 C9' 172(2) . . . . ? N4 C7' C8 C9' -178.2(13) . . . . ? C8' C7' C8 C9 -43.6(13) . . . . ? N4' C7' C8 C9 -174.5(8) . . . . ? C7 C7' C8 C9 174.4(16) . . . . ? N4 C7' C8 C9 -176.0(8) . . . . ? C8 C8' C9 C9' -28(3) . . . . ? C7' C8' C9 C9' -131(2) . . . . ? C7 C8' C9 C9' -30(3) . . . . ? C8 C8' C9 C10" -113(2) . . . . ? C7' C8' C9 C10" 144.7(16) . . . . ? C7 C8' C9 C10" -114.8(16) . . . . ? C9' C8' C9 C10" -84(3) . . . . ? C8 C8' C9 C10' -40(2) . . . . ? C7' C8' C9 C10' -142.9(16) . . . . ? C7 C8' C9 C10' -42(2) . . . . ? C9' C8' C9 C10' -11.9(19) . . . . ? C8 C8' C9 C10 -144.8(17) . . . . ? C7' C8' C9 C10 112.6(16) . . . . ? C7 C8' C9 C10 -146.9(12) . . . . ? C9' C8' C9 C10 -116(3) . . . . ? C7' C8' C9 C8 -102.7(19) . . . . ? C7 C8' C9 C8 -2.1(13) . . . . ? C9' C8' C9 C8 28(3) . . . . ? C8' C8 C9 C9' 150(3) . . . . ? C7' C8 C9 C9' -175(2) . . . . ? C8' C8 C9 C10" 87(2) . . . . ? C7' C8 C9 C10" 122.2(17) . . . . ? C9' C8 C9 C10" -63(3) . . . . ? C8' C8 C9 C10' 148.8(17) . . . . ? C7' C8 C9 C10' -175.9(11) . . . . ? C9' C8 C9 C10' -1(2) . . . . ? C8' C8 C9 C10 54(2) . . . . ? C7' C8 C9 C10 88.9(19) . . . . ? C9' C8 C9 C10 -96(3) . . . . ? C7' C8 C9 C8' 35.3(11) . . . . ? C9' C8 C9 C8' -150(3) . . . . ? C10" C9 C9' C10' -43(3) . . . . ? C10 C9 C9' C10' -38(4) . . . . ? C8' C9 C9' C10' -165(2) . . . . ? C8 C9 C9' C10' -179(3) . . . . ? C10' C9 C9' C10" 43(3) . . . . ? C10 C9 C9' C10" 4.9(14) . . . . ? C8' C9 C9' C10" -122.5(13) . . . . ? C8 C9 C9' C10" -135.9(13) . . . . ? C10" C9 C9' C8 135.9(13) . . . . ? C10' C9 C9' C8 179(3) . . . . ? C10 C9 C9' C8 140.8(12) . . . . ? C8' C9 C9' C8 13.4(12) . . . . ? C10" C9 C9' C8' 122.5(13) . . . . ? C10' C9 C9' C8' 165(2) . . . . ? C10 C9 C9' C8' 127.4(18) . . . . ? C8 C9 C9' C8' -13.4(12) . . . . ? C10" C9 C9' C10 -4.9(14) . . . . ? C10' C9 C9' C10 38(4) . . . . ? C8' C9 C9' C10 -127.4(18) . . . . ? C8 C9 C9' C10 -140.8(12) . . . . ? C8' C8 C9' C9 -28(3) . . . . ? C7 C8 C9' C9 168(4) . . . . ? C7' C8 C9' C9 6(3) . . . . ? C8' C8 C9' C10' 150(4) . . . . ? C7 C8 C9' C10' -14(7) . . . . ? C7' C8 C9' C10' -176(4) . . . . ? C9 C8 C9' C10' 178(6) . . . . ? C8' C8 C9' C10" 30(2) . . . . ? C7 C8 C9' C10" -135(3) . . . . ? C7' C8 C9' C10" 63(2) . . . . ? C9 C8 C9' C10" 57(2) . . . . ? C7 C8 C9' C8' -164(5) . . . . ? C7' C8 C9' C8' 33.3(12) . . . . ? C9 C8 C9' C8' 28(3) . . . . ? C8' C8 C9' C10 9(2) . . . . ? C7 C8 C9' C10 -155(3) . . . . ? C7' C8 C9' C10 42(2) . . . . ? C9 C8 C9' C10 36.7(18) . . . . ? C8 C8' C9' C9 149(3) . . . . ? C7' C8' C9' C9 70(3) . . . . ? C7 C8' C9' C9 154(2) . . . . ? C8 C8' C9' C10' -102(7) . . . . ? C7' C8' C9' C10' 179(6) . . . . ? C9 C8' C9' C10' 109(8) . . . . ? C7 C8' C9' C10' -98(7) . . . . ? C8 C8' C9' C10" -156.9(19) . . . . ? C7' C8' C9' C10" 124.0(18) . . . . ? C9 C8' C9' C10" 54(2) . . . . ? C7 C8' C9' C10" -152.3(12) . . . . ? C7' C8' C9' C8 -79(2) . . . . ? C9 C8' C9' C8 -149(3) . . . . ? C7 C8' C9' C8 4.7(13) . . . . ? C8 C8' C9' C10 -172.5(17) . . . . ? C7' C8' C9' C10 108.5(17) . . . . ? C9 C8' C9' C10 38(2) . . . . ? C7 C8' C9' C10 -167.8(9) . . . . ? C9' C9 C10 C10" -11(3) . . . . ? C10' C9 C10 C10" -34(2) . . . . ? C8' C9 C10 C10" 97(2) . . . . ? C8 C9 C10 C10" 71(3) . . . . ? C9' C9 C10 N2' 56(3) . . . . ? C10" C9 C10 N2' 66(2) . . . . ? C10' C9 C10 N2' 32.5(13) . . . . ? C8' C9 C10 N2' 163.7(10) . . . . ? C8 C9 C10 N2' 137.6(15) . . . . ? C10" C9 C10 C9' 11(3) . . . . ? C10' C9 C10 C9' -23(2) . . . . ? C8' C9 C10 C9' 108(3) . . . . ? C8 C9 C10 C9' 82(3) . . . . ? C9' C9 C10 N2 46(2) . . . . ? C10" C9 C10 N2 56(2) . . . . ? C10' C9 C10 N2 22.5(10) . . . . ? C8' C9 C10 N2 153.7(10) . . . . ? C8 C9 C10 N2 127.5(16) . . . . ? C9' C9 C10 C10' 23(2) . . . . ? C10" C9 C10 C10' 34(2) . . . . ? C8' C9 C10 C10' 131.2(15) . . . . ? C8 C9 C10 C10' 105(2) . . . . ? C9 C9' C10 C10" 164(4) . . . . ? C10' C9' C10 C10" -49(3) . . . . ? C8 C9' C10 C10" 114(3) . . . . ? C8' C9' C10 C10" 118(3) . . . . ? C10' C9' C10 C9 146(3) . . . . ? C10" C9' C10 C9 -164(4) . . . . ? C8 C9' C10 C9 -51(2) . . . . ? C8' C9' C10 C9 -47(2) . . . . ? C9 C9' C10 N2' -130(2) . . . . ? C10' C9' C10 N2' 16.6(15) . . . . ? C10" C9' C10 N2' 66(3) . . . . ? C8 C9' C10 N2' 179.5(11) . . . . ? C8' C9' C10 N2' -176.4(9) . . . . ? C9 C9' C10 N2 -134(3) . . . . ? C10' C9' C10 N2 12.0(13) . . . . ? C10" C9' C10 N2 61(3) . . . . ? C8 C9' C10 N2 174.9(12) . . . . ? C8' C9' C10 N2 179.0(8) . . . . ? C9 C9' C10 C10' -146(3) . . . . ? C10" C9' C10 C10' 49(3) . . . . ? C8 C9' C10 C10' 163(2) . . . . ? C8' C9' C10 C10' 167.1(17) . . . . ? C9 C9' C10' C10" 43(3) . . . . ? C8 C9' C10' C10" -134(4) . . . . ? C8' C9' C10' C10" -59(7) . . . . ? C10 C9' C10' C10" 13.9(10) . . . . ? C10" C9' C10' C9 -43(3) . . . . ? C8 C9' C10' C9 -177(7) . . . . ? C8' C9' C10' C9 -102(8) . . . . ? C10 C9' C10' C9 -29(3) . . . . ? C9 C9' C10' N2 11(5) . . . . ? C10" C9' C10' N2 -33(2) . . . . ? C8 C9' C10' N2 -167(3) . . . . ? C8' C9' C10' N2 -91(7) . . . . ? C10 C9' C10' N2 -19(2) . . . . ? C9 C9' C10' C10 29(3) . . . . ? C10" C9' C10' C10 -13.9(10) . . . . ? C8 C9' C10' C10 -148(4) . . . . ? C8' C9' C10' C10 -73(7) . . . . ? C9 C9' C10' N2' 15(4) . . . . ? C10" C9' C10' N2' -27.8(14) . . . . ? C8 C9' C10' N2' -162(3) . . . . ? C8' C9' C10' N2' -87(7) . . . . ? C10 C9' C10' N2' -13.9(12) . . . . ? C10" C9 C10' C9' 126(4) . . . . ? C10 C9 C10' C9' 144(4) . . . . ? C8' C9 C10' C9' 19(3) . . . . ? C8 C9 C10' C9' 1(3) . . . . ? C9' C9 C10' C10" -126(4) . . . . ? C10 C9 C10' C10" 17.4(11) . . . . ? C8' C9 C10' C10" -107.1(18) . . . . ? C8 C9 C10' C10" -125.2(15) . . . . ? C9' C9 C10' N2 -172(4) . . . . ? C10" C9 C10' N2 -45.3(14) . . . . ? C10 C9 C10' N2 -27.9(12) . . . . ? C8' C9 C10' N2 -152.4(12) . . . . ? C8 C9 C10' N2 -170.5(11) . . . . ? C9' C9 C10' C10 -144(4) . . . . ? C10" C9 C10' C10 -17.4(11) . . . . ? C8' C9 C10' C10 -124.6(17) . . . . ? C8 C9 C10' C10 -142.6(13) . . . . ? C9' C9 C10' N2' -166(4) . . . . ? C10" C9 C10' N2' -39.8(12) . . . . ? C10 C9 C10' N2' -22.4(8) . . . . ? C8' C9 C10' N2' -146.9(13) . . . . ? C8 C9 C10' N2' -165.0(9) . . . . ? C10" C10 C10' C9' 71(4) . . . . ? C9 C10 C10' C9' -14.0(13) . . . . ? N2' C10 C10' C9' -162.9(15) . . . . ? N2 C10 C10' C9' -164.6(17) . . . . ? C9 C10 C10' C10" -84(4) . . . . ? N2' C10 C10' C10" 127(4) . . . . ? C9' C10 C10' C10" -71(4) . . . . ? N2 C10 C10' C10" 125(4) . . . . ? C10" C10 C10' C9 84(4) . . . . ? N2' C10 C10' C9 -148.9(12) . . . . ? C9' C10 C10' C9 14.0(13) . . . . ? N2 C10 C10' C9 -150.7(13) . . . . ? C10" C10 C10' N2 -125(4) . . . . ? C9 C10 C10' N2 150.7(13) . . . . ? N2' C10 C10' N2 1.7(7) . . . . ? C9' C10 C10' N2 164.6(17) . . . . ? C10" C10 C10' N2' -127(4) . . . . ? C9 C10 C10' N2' 148.9(12) . . . . ? C9' C10 C10' N2' 162.9(15) . . . . ? N2 C10 C10' N2' -1.7(7) . . . . ? N2' C10 C10" C9 -123.6(14) . . . . ? C9' C10 C10" C9 -6.5(17) . . . . ? N2 C10 C10" C9 -117.3(17) . . . . ? C10' C10 C10" C9 -74(4) . . . . ? C9 C10 C10" C9' 6.5(17) . . . . ? N2' C10 C10" C9' -117(2) . . . . ? N2 C10 C10" C9' -111(3) . . . . ? C10' C10 C10" C9' -68(4) . . . . ? C9 C10 C10" C10' 74(4) . . . . ? N2' C10 C10" C10' -49(4) . . . . ? C9' C10 C10" C10' 68(4) . . . . ? N2 C10 C10" C10' -43(3) . . . . ? C9 C10 C10" N2' 123.6(14) . . . . ? C9' C10 C10" N2' 117(2) . . . . ? N2 C10 C10" N2' 6.3(10) . . . . ? C10' C10 C10" N2' 49(4) . . . . ? C9 C10 C10" N2 117.3(17) . . . . ? N2' C10 C10" N2 -6.3(10) . . . . ? C9' C10 C10" N2 111(3) . . . . ? C10' C10 C10" N2 43(3) . . . . ? C9' C9 C10" C10 170(3) . . . . ? C10' C9 C10" C10 139(3) . . . . ? C8' C9 C10" C10 -101(2) . . . . ? C8 C9 C10" C10 -133(2) . . . . ? C10' C9 C10" C9' -30(2) . . . . ? C10 C9 C10" C9' -170(3) . . . . ? C8' C9 C10" C9' 90(2) . . . . ? C8 C9 C10" C9' 57(2) . . . . ? C9' C9 C10" C10' 30(2) . . . . ? C10 C9 C10" C10' -139(3) . . . . ? C8' C9 C10" C10' 120.1(15) . . . . ? C8 C9 C10" C10' 87.3(17) . . . . ? C9' C9 C10" N2' 99(2) . . . . ? C10' C9 C10" N2' 68.6(16) . . . . ? C10 C9 C10" N2' -71(2) . . . . ? C8' C9 C10" N2' -171.3(10) . . . . ? C8 C9 C10" N2' 155.9(11) . . . . ? C9' C9 C10" N2 74(2) . . . . ? C10' C9 C10" N2 44.1(13) . . . . ? C10 C9 C10" N2 -95(2) . . . . ? C8' C9 C10" N2 164.1(10) . . . . ? C8 C9 C10" N2 131.4(14) . . . . ? C9 C9' C10" C10 -13(3) . . . . ? C10' C9' C10" C10 126(3) . . . . ? C8 C9' C10" C10 -79(3) . . . . ? C8' C9' C10" C10 -66(3) . . . . ? C10' C9' C10" C9 139(3) . . . . ? C8 C9' C10" C9 -66(2) . . . . ? C8' C9' C10" C9 -52.5(18) . . . . ? C10 C9' C10" C9 13(3) . . . . ? C9 C9' C10" C10' -139(3) . . . . ? C8 C9' C10" C10' 155(2) . . . . ? C8' C9' C10" C10' 168.1(17) . . . . ? C10 C9' C10" C10' -126(3) . . . . ? C9 C9' C10" N2' -102(2) . . . . ? C10' C9' C10" N2' 37.5(17) . . . . ? C8 C9' C10" N2' -167.9(11) . . . . ? C8' C9' C10" N2' -154.4(11) . . . . ? C10 C9' C10" N2' -89(3) . . . . ? C9 C9' C10" N2 -117(2) . . . . ? C10' C9' C10" N2 22.8(14) . . . . ? C8 C9' C10" N2 177.4(11) . . . . ? C8' C9' C10" N2 -169.1(8) . . . . ? C10 C9' C10" N2 -103(3) . . . . ? C9' C10' C10" C10 -104(4) . . . . ? C9 C10' C10" C10 -84(4) . . . . ? N2 C10' C10" C10 51(4) . . . . ? N2' C10' C10" C10 45(4) . . . . ? C9' C10' C10" C9 -19.8(13) . . . . ? N2 C10' C10" C9 135.3(13) . . . . ? C10 C10' C10" C9 84(4) . . . . ? N2' C10' C10" C9 129.8(13) . . . . ? C9 C10' C10" C9' 19.8(13) . . . . ? N2 C10' C10" C9' 155.0(15) . . . . ? C10 C10' C10" C9' 104(4) . . . . ? N2' C10' C10" C9' 149.5(14) . . . . ? C9' C10' C10" N2' -149.5(14) . . . . ? C9 C10' C10" N2' -129.8(13) . . . . ? N2 C10' C10" N2' 5.5(7) . . . . ? C10 C10' C10" N2' -45(4) . . . . ? C9' C10' C10" N2 -155.0(15) . . . . ? C9 C10' C10" N2 -135.3(13) . . . . ? C10 C10' C10" N2 -51(4) . . . . ? N2' C10' C10" N2 -5.5(7) . . . . ? O1 C11 C12 C13 -134.7(4) . . . . ? O2 C11 C12 C13 47.1(5) . . . . ? C11 C12 C13 C14 -63.8(4) . . . . ? C11 C12 C13 C13 171.4(4) . . . 3_866 ? C12 C13 C14 O3 125.7(4) . . . . ? C13 C13 C14 O3 -108.3(4) 3_866 . . . ? C12 C13 C14 O4 -57.9(4) . . . . ? C13 C13 C14 O4 68.2(5) 3_866 . . . ? N2 C1 N1 C1' 75.9(11) . . . . ? N2' C1 N1 C1' 53.8(8) . . . . ? C3 C1 N1 C1' 104.8(10) . . . . ? C1' C1 N1 C3 -104.8(10) . . . . ? N2 C1 N1 C3 -28.9(12) . . . . ? N2' C1 N1 C3 -51.0(9) . . . . ? C1' C1 N1 C3' -78.6(10) . . . . ? N2 C1 N1 C3' -2.7(13) . . . . ? N2' C1 N1 C3' -24.8(9) . . . . ? C3 C1 N1 C3' 26.2(5) . . . . ? C1' C1 N1 Co1 113.1(8) . . . 2_644 ? N2 C1 N1 Co1 -171.0(8) . . . 2_644 ? N2' C1 N1 Co1 166.9(4) . . . 2_644 ? C3 C1 N1 Co1 -142.1(7) . . . 2_644 ? N2' C1' N1 C1 -78.2(10) . . . . ? N2 C1' N1 C1 -54.8(9) . . . . ? C3' C1' N1 C1 -108.8(10) . . . . ? C1 C1' N1 C3 83.2(10) . . . . ? N2' C1' N1 C3 5.1(9) . . . . ? N2 C1' N1 C3 28.5(8) . . . . ? C3' C1' N1 C3 -25.6(5) . . . . ? C1 C1' N1 C3' 108.8(10) . . . . ? N2' C1' N1 C3' 30.6(8) . . . . ? N2 C1' N1 C3' 54.0(7) . . . . ? C1 C1' N1 Co1 -95.7(9) . . . 2_644 ? N2' C1' N1 Co1 -173.9(4) . . . 2_644 ? N2 C1' N1 Co1 -150.5(5) . . . 2_644 ? C3' C1' N1 Co1 155.5(6) . . . 2_644 ? C3' C3 N1 C1 109.8(14) . . . . ? C2 C3 N1 C1 31.1(11) . . . . ? C2' C3 N1 C1 49.0(10) . . . . ? C3' C3 N1 C1' 72.1(14) . . . . ? C2 C3 N1 C1' -6.7(11) . . . . ? C2' C3 N1 C1' 11.3(9) . . . . ? C1 C3 N1 C1' -37.7(5) . . . . ? C2 C3 N1 C3' -78.7(14) . . . . ? C2' C3 N1 C3' -60.8(13) . . . . ? C1 C3 N1 C3' -109.8(14) . . . . ? C3' C3 N1 Co1 -108.9(13) . . . 2_644 ? C2 C3 N1 Co1 172.4(7) . . . 2_644 ? C2' C3 N1 Co1 -169.7(6) . . . 2_644 ? C1 C3 N1 Co1 141.3(7) . . . 2_644 ? C3 C3' N1 C1 -75.8(14) . . . . ? C2' C3' N1 C1 7.8(11) . . . . ? C2 C3' N1 C1 -12.1(10) . . . . ? C1' C3' N1 C1 37.0(6) . . . . ? C3 C3' N1 C1' -112.8(13) . . . . ? C2' C3' N1 C1' -29.1(9) . . . . ? C2 C3' N1 C1' -49.0(8) . . . . ? C2' C3' N1 C3 83.7(14) . . . . ? C2 C3' N1 C3 63.7(12) . . . . ? C1' C3' N1 C3 112.8(13) . . . . ? C3 C3' N1 Co1 91.6(13) . . . 2_644 ? C2' C3' N1 Co1 175.3(6) . . . 2_644 ? C2 C3' N1 Co1 155.4(6) . . . 2_644 ? C1' C3' N1 Co1 -155.6(6) . . . 2_644 ? C3 C2 N2 N2' 98.2(15) . . . . ? C3' C2 N2 N2' 71.5(15) . . . . ? C3 C2 N2 C1 2.8(15) . . . . ? N2' C2 N2 C1 -95.5(16) . . . . ? C3' C2 N2 C1 -23.9(14) . . . . ? C3 C2 N2 C2' 97(3) . . . . ? N2' C2 N2 C2' -2(3) . . . . ? C3' C2 N2 C2' 70(3) . . . . ? C3 C2 N2 C1' 38.1(12) . . . . ? N2' C2 N2 C1' -60.1(12) . . . . ? C3' C2 N2 C1' 11.4(12) . . . . ? C3 C2 N2 C10' -143.0(11) . . . . ? N2' C2 N2 C10' 118.8(18) . . . . ? C3' C2 N2 C10' -169.7(10) . . . . ? C3 C2 N2 C10" 163.9(11) . . . . ? N2' C2 N2 C10" 65.7(16) . . . . ? C3' C2 N2 C10" 137.2(11) . . . . ? C3 C2 N2 C10 145.6(9) . . . . ? N2' C2 N2 C10 47.4(12) . . . . ? C3' C2 N2 C10 118.9(8) . . . . ? C1' C1 N2 N2' 2.6(17) . . . . ? N1 C1 N2 N2' -66.6(18) . . . . ? C3 C1 N2 N2' -86.1(15) . . . . ? C1' C1 N2 C2 86.8(13) . . . . ? N1 C1 N2 C2 17.7(16) . . . . ? N2' C1 N2 C2 84.3(14) . . . . ? C3 C1 N2 C2 -1.9(10) . . . . ? C1' C1 N2 C2' 66.0(13) . . . . ? N1 C1 N2 C2' -3.2(15) . . . . ? N2' C1 N2 C2' 63.4(13) . . . . ? C3 C1 N2 C2' -22.7(10) . . . . ? N1 C1 N2 C1' -69.1(9) . . . . ? N2' C1 N2 C1' -2.6(17) . . . . ? C3 C1 N2 C1' -88.7(8) . . . . ? C1' C1 N2 C10' -130.8(14) . . . . ? N1 C1 N2 C10' 160.1(12) . . . . ? N2' C1 N2 C10' -133(2) . . . . ? C3 C1 N2 C10' 140.5(14) . . . . ? C1' C1 N2 C10" -73.9(14) . . . . ? N1 C1 N2 C10" -143.1(11) . . . . ? N2' C1 N2 C10" -77(2) . . . . ? C3 C1 N2 C10" -162.6(13) . . . . ? C1' C1 N2 C10 -47.3(12) . . . . ? N1 C1 N2 C10 -116.5(10) . . . . ? N2' C1 N2 C10 -49.9(16) . . . . ? C3 C1 N2 C10 -136.0(10) . . . . ? C3' C2' N2 N2' 97.0(16) . . . . ? C3 C2' N2 N2' 119.7(16) . . . . ? N2' C2' N2 C2 178(3) . . . . ? C3' C2' N2 C2 -85(3) . . . . ? C3 C2' N2 C2 -62(2) . . . . ? N2' C2' N2 C1 -89.4(17) . . . . ? C3' C2' N2 C1 7.6(15) . . . . ? C3 C2' N2 C1 30.4(13) . . . . ? N2' C2' N2 C1' -58.3(13) . . . . ? C3' C2' N2 C1' 38.8(11) . . . . ? C3 C2' N2 C1' 61.5(9) . . . . ? N2' C2' N2 C10' 107.5(19) . . . . ? C3' C2' N2 C10' -155.4(12) . . . . ? C3 C2' N2 C10' -132.7(13) . . . . ? N2' C2' N2 C10" 55.4(15) . . . . ? C3' C2' N2 C10" 152.4(10) . . . . ? C3 C2' N2 C10" 175.1(10) . . . . ? N2' C2' N2 C10 43.7(13) . . . . ? C3' C2' N2 C10 140.7(9) . . . . ? C3 C2' N2 C10 163.4(8) . . . . ? C1 C1' N2 N2' -177.1(19) . . . . ? N1 C1' N2 N2' -117.3(15) . . . . ? C3' C1' N2 N2' -82.8(14) . . . . ? C1 C1' N2 C2 -102.5(13) . . . . ? N1 C1' N2 C2 -42.6(10) . . . . ? N2' C1' N2 C2 74.7(13) . . . . ? C3' C1' N2 C2 -8.2(8) . . . . ? N1 C1' N2 C1 59.8(8) . . . . ? N2' C1' N2 C1 177.1(19) . . . . ? C3' C1' N2 C1 94.3(9) . . . . ? C1 C1' N2 C2' -119.3(12) . . . . ? N1 C1' N2 C2' -59.5(9) . . . . ? N2' C1' N2 C2' 57.8(13) . . . . ? C3' C1' N2 C2' -25.0(7) . . . . ? C1 C1' N2 C10' 79.0(18) . . . . ? N1 C1' N2 C10' 138.9(15) . . . . ? N2' C1' N2 C10' -104(2) . . . . ? C3' C1' N2 C10' 173.3(17) . . . . ? C1 C1' N2 C10" 123.4(12) . . . . ? N1 C1' N2 C10" -176.7(8) . . . . ? N2' C1' N2 C10" -59.5(16) . . . . ? C3' C1' N2 C10" -142.3(9) . . . . ? C1 C1' N2 C10 143.6(11) . . . . ? N1 C1' N2 C10 -156.5(6) . . . . ? N2' C1' N2 C10 -39.3(14) . . . . ? C3' C1' N2 C10 -122.1(7) . . . . ? C9' C10' N2 N2' 15(3) . . . . ? C10" C10' N2 N2' -16(2) . . . . ? C9 C10' N2 N2' 19(2) . . . . ? C10 C10' N2 N2' -4.4(19) . . . . ? C9' C10' N2 C2 -81(3) . . . . ? C10" C10' N2 C2 -112.5(14) . . . . ? C9 C10' N2 C2 -77.2(16) . . . . ? C10 C10' N2 C2 -100.9(12) . . . . ? N2' C10' N2 C2 -96.5(19) . . . . ? C9' C10' N2 C1 139(2) . . . . ? C10" C10' N2 C1 108.4(16) . . . . ? C9 C10' N2 C1 143.7(14) . . . . ? C10 C10' N2 C1 120.0(14) . . . . ? N2' C10' N2 C1 124(3) . . . . ? C9' C10' N2 C2' -60(3) . . . . ? C10" C10' N2 C2' -91.4(16) . . . . ? C9 C10' N2 C2' -56.0(19) . . . . ? C10 C10' N2 C2' -79.8(14) . . . . ? N2' C10' N2 C2' -75.3(18) . . . . ? C9' C10' N2 C1' 97(3) . . . . ? C10" C10' N2 C1' 65.9(19) . . . . ? C9 C10' N2 C1' 101.2(18) . . . . ? C10 C10' N2 C1' 77.5(17) . . . . ? N2' C10' N2 C1' 82(3) . . . . ? C9' C10' N2 C10" 31(2) . . . . ? C9 C10' N2 C10" 35.3(11) . . . . ? C10 C10' N2 C10" 11.6(10) . . . . ? N2' C10' N2 C10" 16(2) . . . . ? C9' C10' N2 C10 19(2) . . . . ? C10" C10' N2 C10 -11.6(10) . . . . ? C9 C10' N2 C10 23.7(11) . . . . ? N2' C10' N2 C10 4.4(19) . . . . ? C10 C10" N2 N2' 16(2) . . . . ? C9 C10" N2 N2' 117(2) . . . . ? C9' C10" N2 N2' 146.6(18) . . . . ? C10' C10" N2 N2' 165.5(19) . . . . ? C10 C10" N2 C2 -54(3) . . . . ? C9 C10" N2 C2 48(2) . . . . ? C9' C10" N2 C2 77.2(17) . . . . ? C10' C10" N2 C2 96.1(16) . . . . ? N2' C10" N2 C2 -69.4(15) . . . . ? C10 C10" N2 C1 104(2) . . . . ? C9 C10" N2 C1 -154.9(15) . . . . ? C9' C10" N2 C1 -125.2(15) . . . . ? C10' C10" N2 C1 -106.2(15) . . . . ? N2' C10" N2 C1 88(2) . . . . ? C10 C10" N2 C2' -34(3) . . . . ? C9 C10" N2 C2' 67.7(19) . . . . ? C9' C10" N2 C2' 97.4(15) . . . . ? C10' C10" N2 C2' 116.4(15) . . . . ? N2' C10" N2 C2' -49.2(13) . . . . ? C10 C10" N2 C1' 68(2) . . . . ? C9 C10" N2 C1' 169.6(13) . . . . ? C9' C10" N2 C1' -160.7(11) . . . . ? C10' C10" N2 C1' -141.8(12) . . . . ? N2' C10" N2 C1' 52.7(14) . . . . ? C10 C10" N2 C10' -150(3) . . . . ? C9 C10" N2 C10' -48.6(15) . . . . ? C9' C10" N2 C10' -18.9(12) . . . . ? N2' C10" N2 C10' -165.5(19) . . . . ? C9 C10" N2 C10 101(3) . . . . ? C9' C10" N2 C10 131(3) . . . . ? C10' C10" N2 C10 150(3) . . . . ? N2' C10" N2 C10 -16(2) . . . . ? C10" C10 N2 N2' -161(3) . . . . ? C9 C10 N2 N2' 152.8(19) . . . . ? C9' C10 N2 N2' 166.8(18) . . . . ? C10' C10 N2 N2' 175(2) . . . . ? C10" C10 N2 C2 135(2) . . . . ? C9 C10 N2 C2 88.8(12) . . . . ? N2' C10 N2 C2 -64.0(15) . . . . ? C9' C10 N2 C2 102.9(11) . . . . ? C10' C10 N2 C2 111.3(12) . . . . ? C10" C10 N2 C1 -92(2) . . . . ? C9 C10 N2 C1 -138.1(11) . . . . ? N2' C10 N2 C1 69.1(18) . . . . ? C9' C10 N2 C1 -124.0(11) . . . . ? C10' C10 N2 C1 -115.6(12) . . . . ? C10" C10 N2 C2' 150(2) . . . . ? C9 C10 N2 C2' 103.8(11) . . . . ? N2' C10 N2 C2' -49.0(14) . . . . ? C9' C10 N2 C2' 117.9(10) . . . . ? C10' C10 N2 C2' 126.3(12) . . . . ? C10" C10 N2 C1' -117(2) . . . . ? C9 C10 N2 C1' -163.2(9) . . . . ? N2' C10 N2 C1' 44.0(15) . . . . ? C9' C10 N2 C1' -149.2(8) . . . . ? C10' C10 N2 C1' -140.8(10) . . . . ? C10" C10 N2 C10' 23(2) . . . . ? C9 C10 N2 C10' -22.4(10) . . . . ? N2' C10 N2 C10' -175(2) . . . . ? C9' C10 N2 C10' -8.4(9) . . . . ? C9 C10 N2 C10" -45.7(19) . . . . ? N2' C10 N2 C10" 161(3) . . . . ? C9' C10 N2 C10" -32(2) . . . . ? C10' C10 N2 C10" -23(2) . . . . ? C2 N2 N2' C2' -0.6(11) . . . . ? C1 N2 N2' C2' 105.8(10) . . . . ? C1' N2 N2' C2' 107.4(10) . . . . ? C10' N2 N2' C2' -117.4(15) . . . . ? C10" N2 N2' C2' -129.2(11) . . . . ? C10 N2 N2' C2' -122.3(13) . . . . ? C2 N2 N2' C1' -108.1(7) . . . . ? C1 N2 N2' C1' -1.6(11) . . . . ? C2' N2 N2' C1' -107.4(10) . . . . ? C10' N2 N2' C1' 135.2(13) . . . . ? C10" N2 N2' C1' 123.3(8) . . . . ? C10 N2 N2' C1' 130.2(12) . . . . ? C1 N2 N2' C2 106.5(8) . . . . ? C2' N2 N2' C2 0.6(11) . . . . ? C1' N2 N2' C2 108.1(7) . . . . ? C10' N2 N2' C2 -116.7(15) . . . . ? C10" N2 N2' C2 -128.6(8) . . . . ? C10 N2 N2' C2 -121.7(10) . . . . ? C2 N2 N2' C10 121.7(10) . . . . ? C1 N2 N2' C10 -131.9(9) . . . . ? C2' N2 N2' C10 122.3(13) . . . . ? C1' N2 N2' C10 -130.2(12) . . . . ? C10' N2 N2' C10 5(2) . . . . ? C10" N2 N2' C10 -6.9(11) . . . . ? C2 N2 N2' C1 -106.5(8) . . . . ? C2' N2 N2' C1 -105.8(10) . . . . ? C1' N2 N2' C1 1.6(11) . . . . ? C10' N2 N2' C1 136.8(19) . . . . ? C10" N2 N2' C1 125.0(9) . . . . ? C10 N2 N2' C1 131.9(9) . . . . ? C2 N2 N2' C10" 128.6(8) . . . . ? C1 N2 N2' C10" -125.0(9) . . . . ? C2' N2 N2' C10" 129.2(11) . . . . ? C1' N2 N2' C10" -123.3(8) . . . . ? C10' N2 N2' C10" 11.8(16) . . . . ? C10 N2 N2' C10" 6.9(11) . . . . ? C2 N2 N2' C10' 116.7(15) . . . . ? C1 N2 N2' C10' -136.8(19) . . . . ? C2' N2 N2' C10' 117.4(15) . . . . ? C1' N2 N2' C10' -135.2(13) . . . . ? C10" N2 N2' C10' -11.8(16) . . . . ? C10 N2 N2' C10' -5(2) . . . . ? C3' C2' N2' N2 -90.2(15) . . . . ? C3 C2' N2' N2 -64.0(15) . . . . ? C3' C2' N2' C1' 2.4(11) . . . . ? N2 C2' N2' C1' 92.6(14) . . . . ? C3 C2' N2' C1' 28.6(11) . . . . ? C3' C2' N2' C2 -92(3) . . . . ? N2 C2' N2' C2 -2(3) . . . . ? C3 C2' N2' C2 -66(3) . . . . ? C3' C2' N2' C10 161.2(9) . . . . ? N2 C2' N2' C10 -108.7(17) . . . . ? C3 C2' N2' C10 -172.7(8) . . . . ? C3' C2' N2' C1 -32.2(11) . . . . ? N2 C2' N2' C1 58.0(12) . . . . ? C3 C2' N2' C1 -6.1(11) . . . . ? C3' C2' N2' C10" -171.6(10) . . . . ? N2 C2' N2' C10" -81.5(16) . . . . ? C3 C2' N2' C10" -145.5(11) . . . . ? C3' C2' N2' C10' -131.1(9) . . . . ? N2 C2' N2' C10' -40.9(12) . . . . ? C3 C2' N2' C10' -104.9(10) . . . . ? C1 C1' N2' N2 2.5(17) . . . . ? N1 C1' N2' N2 69.0(16) . . . . ? C3' C1' N2' N2 90.0(15) . . . . ? C1 C1' N2' C2' -89.1(11) . . . . ? N1 C1' N2' C2' -22.7(10) . . . . ? N2 C1' N2' C2' -91.6(16) . . . . ? C3' C1' N2' C2' -1.6(8) . . . . ? C1 C1' N2' C2 -68.1(11) . . . . ? N1 C1' N2' C2 -1.7(10) . . . . ? N2 C1' N2' C2 -70.7(13) . . . . ? C3' C1' N2' C2 19.3(7) . . . . ? C1 C1' N2' C10 114.1(11) . . . . ? N1 C1' N2' C10 -179.4(8) . . . . ? N2 C1' N2' C10 111.6(19) . . . . ? C3' C1' N2' C10 -158.4(9) . . . . ? N1 C1' N2' C1 66.4(8) . . . . ? N2 C1' N2' C1 -2.5(17) . . . . ? C3' C1' N2' C1 87.5(9) . . . . ? C1 C1' N2' C10" 85.4(12) . . . . ? N1 C1' N2' C10" 151.8(9) . . . . ? N2 C1' N2' C10" 82.8(16) . . . . ? C3' C1' N2' C10" 172.8(9) . . . . ? C1 C1' N2' C10' 37.6(12) . . . . ? N1 C1' N2' C10' 104.0(9) . . . . ? N2 C1' N2' C10' 35.1(13) . . . . ? C3' C1' N2' C10' 125.1(8) . . . . ? C3 C2 N2' N2 -88.4(15) . . . . ? C3' C2 N2' N2 -112.6(14) . . . . ? N2 C2 N2' C2' 178(3) . . . . ? C3 C2 N2' C2' 90(3) . . . . ? C3' C2 N2' C2' 66(3) . . . . ? N2 C2 N2' C1' 86.1(13) . . . . ? C3 C2 N2' C1' -2.4(12) . . . . ? C3' C2 N2' C1' -26.5(10) . . . . ? N2 C2 N2' C10 -96.1(16) . . . . ? C3 C2 N2' C10 175.5(9) . . . . ? C3' C2 N2' C10 151.3(8) . . . . ? N2 C2 N2' C1 55.2(12) . . . . ? C3 C2 N2' C1 -33.2(10) . . . . ? C3' C2 N2' C1 -57.3(8) . . . . ? N2 C2 N2' C10" -67.6(14) . . . . ? C3 C2 N2' C10" -156.0(10) . . . . ? C3' C2 N2' C10" 179.9(9) . . . . ? N2 C2 N2' C10' -38.5(12) . . . . ? C3 C2 N2' C10' -126.9(10) . . . . ? C3' C2 N2' C10' -151.1(8) . . . . ? C10" C10 N2' N2 17(3) . . . . ? C9 C10 N2' N2 -30(2) . . . . ? C9' C10 N2' N2 -13.4(19) . . . . ? C10' C10 N2' N2 -3.9(16) . . . . ? C10" C10 N2' C2' 118(2) . . . . ? C9 C10 N2' C2' 70.6(14) . . . . ? C9' C10 N2' C2' 87.2(12) . . . . ? N2 C10 N2' C2' 100.6(19) . . . . ? C10' C10 N2' C2' 96.7(11) . . . . ? C10" C10 N2' C1' -88(2) . . . . ? C9 C10 N2' C1' -135.3(11) . . . . ? C9' C10 N2' C1' -118.8(10) . . . . ? N2 C10 N2' C1' -105.4(19) . . . . ? C10' C10 N2' C1' -109.3(10) . . . . ? C10" C10 N2' C2 94(2) . . . . ? C9 C10 N2' C2 47.3(16) . . . . ? C9' C10 N2' C2 63.8(13) . . . . ? N2 C10 N2' C2 77.3(16) . . . . ? C10' C10 N2' C2 73.3(11) . . . . ? C10" C10 N2' C1 -44(2) . . . . ? C9 C10 N2' C1 -91.4(15) . . . . ? C9' C10 N2' C1 -74.8(13) . . . . ? N2 C10 N2' C1 -61.4(16) . . . . ? C10' C10 N2' C1 -65.3(12) . . . . ? C9 C10 N2' C10" -47.2(18) . . . . ? C9' C10 N2' C10" -30.6(18) . . . . ? N2 C10 N2' C10" -17(3) . . . . ? C10' C10 N2' C10" -21(2) . . . . ? C10" C10 N2' C10' 21(2) . . . . ? C9 C10 N2' C10' -26.1(10) . . . . ? C9' C10 N2' C10' -9.5(8) . . . . ? N2 C10 N2' C10' 3.9(16) . . . . ? C1' C1 N2' N2 -177.0(19) . . . . ? N1 C1 N2' N2 119.5(17) . . . . ? C3 C1 N2' N2 86.9(16) . . . . ? C1' C1 N2' C2' 100.5(12) . . . . ? N1 C1 N2' C2' 37.1(11) . . . . ? N2 C1 N2' C2' -82.4(16) . . . . ? C3 C1 N2' C2' 4.5(8) . . . . ? N1 C1 N2' C1' -63.4(8) . . . . ? N2 C1 N2' C1' 177.0(19) . . . . ? C3 C1 N2' C1' -96.1(9) . . . . ? C1' C1 N2' C2 117.7(11) . . . . ? N1 C1 N2' C2 54.3(9) . . . . ? N2 C1 N2' C2 -65.2(14) . . . . ? C3 C1 N2' C2 21.7(7) . . . . ? C1' C1 N2' C10 -95.4(12) . . . . ? N1 C1 N2' C10 -158.8(9) . . . . ? N2 C1 N2' C10 81.7(18) . . . . ? C3 C1 N2' C10 168.6(10) . . . . ? C1' C1 N2' C10" -113.4(12) . . . . ? N1 C1 N2' C10" -176.8(9) . . . . ? N2 C1 N2' C10" 63.7(16) . . . . ? C3 C1 N2' C10" 150.6(9) . . . . ? C1' C1 N2' C10' -148.5(11) . . . . ? N1 C1 N2' C10' 148.0(9) . . . . ? N2 C1 N2' C10' 28.5(14) . . . . ? C3 C1 N2' C10' 115.4(7) . . . . ? C10 C10" N2' N2 -163(3) . . . . ? C9 C10" N2' N2 -76(2) . . . . ? C9' C10" N2' N2 -40(2) . . . . ? C10' C10" N2' N2 -12.8(17) . . . . ? C10 C10" N2' C2' -78(2) . . . . ? C9 C10" N2' C2' 9(2) . . . . ? C9' C10" N2' C2' 46(2) . . . . ? C10' C10" N2' C2' 72.5(15) . . . . ? N2 C10" N2' C2' 85.3(17) . . . . ? C10 C10" N2' C1' 109(2) . . . . ? C9 C10" N2' C1' -163.7(14) . . . . ? C9' C10" N2' C1' -127.6(14) . . . . ? C10' C10" N2' C1' -100.7(13) . . . . ? N2 C10" N2' C1' -87.9(16) . . . . ? C10 C10" N2' C2 -102(2) . . . . ? C9 C10" N2' C2 -14(2) . . . . ? C9' C10" N2' C2 22(2) . . . . ? C10' C10" N2' C2 48.9(15) . . . . ? N2 C10" N2' C2 61.7(14) . . . . ? C9 C10" N2' C10 87(2) . . . . ? C9' C10" N2' C10 124(3) . . . . ? C10' C10" N2' C10 150(3) . . . . ? N2 C10" N2' C10 163(3) . . . . ? C10 C10" N2' C1 146(2) . . . . ? C9 C10" N2' C1 -126.4(16) . . . . ? C9' C10" N2' C1 -90.3(16) . . . . ? C10' C10" N2' C1 -63.4(13) . . . . ? N2 C10" N2' C1 -50.6(13) . . . . ? C10 C10" N2' C10' -150(3) . . . . ? C9 C10" N2' C10' -63.0(17) . . . . ? C9' C10" N2' C10' -26.9(13) . . . . ? N2 C10" N2' C10' 12.8(17) . . . . ? C9' C10' N2' N2 -168(3) . . . . ? C10" C10' N2' N2 162(2) . . . . ? C9 C10' N2' N2 -162(2) . . . . ? C10 C10' N2' N2 175(2) . . . . ? C9' C10' N2' C2' -97.4(19) . . . . ? C10" C10' N2' C2' -128.2(14) . . . . ? C9 C10' N2' C2' -91.6(12) . . . . ? N2 C10' N2' C2' 70(2) . . . . ? C10 C10' N2' C2' -115.2(11) . . . . ? C9' C10' N2' C1' 136.8(16) . . . . ? C10" C10' N2' C1' 106.0(13) . . . . ? C9 C10' N2' C1' 142.6(10) . . . . ? N2 C10' N2' C1' -55.6(18) . . . . ? C10 C10' N2' C1' 119.0(10) . . . . ? C9' C10' N2' C2 -109.9(18) . . . . ? C10" C10' N2' C2 -140.7(13) . . . . ? C9 C10' N2' C2 -104.0(10) . . . . ? N2 C10' N2' C2 57.8(18) . . . . ? C10 C10' N2' C2 -127.7(10) . . . . ? C9' C10' N2' C10 17.8(16) . . . . ? C10" C10' N2' C10 -13.0(12) . . . . ? C9 C10' N2' C10 23.6(10) . . . . ? N2 C10' N2' C10 -175(2) . . . . ? C9' C10' N2' C1 156.5(17) . . . . ? C10" C10' N2' C1 125.7(12) . . . . ? C9 C10' N2' C1 162.3(10) . . . . ? N2 C10' N2' C1 -35.9(18) . . . . ? C10 C10' N2' C1 138.7(9) . . . . ? C9' C10' N2' C10" 30.8(16) . . . . ? C9 C10' N2' C10" 36.6(11) . . . . ? N2 C10' N2' C10" -162(2) . . . . ? C10 C10' N2' C10" 13.0(12) . . . . ? C4' C4 N3 C5 -97.2(8) . . . . ? N4 C4 N3 C5 -11.8(8) . . . . ? N4' C4 N3 C5 -44.0(6) . . . . ? N4 C4 N3 C4' 85.4(10) . . . . ? N4' C4 N3 C4' 53.2(7) . . . . ? C4' C4 N3 Co1 103.9(8) . . . . ? N4 C4 N3 Co1 -170.7(5) . . . . ? N4' C4 N3 Co1 157.1(3) . . . . ? C6 C5 N3 C4 19.6(6) . . . . ? C6 C5 N3 C4' -17.7(6) . . . . ? C6 C5 N3 Co1 177.6(3) . . . . ? N4' C4' N3 C4 -81.5(9) . . . . ? N4 C4' N3 C4 -52.2(8) . . . . ? C4 C4' N3 C5 91.7(8) . . . . ? N4' C4' N3 C5 10.1(7) . . . . ? N4 C4' N3 C5 39.5(5) . . . . ? C4 C4' N3 Co1 -103.1(8) . . . . ? N4' C4' N3 Co1 175.4(4) . . . . ? N4 C4' N3 Co1 -155.2(3) . . . . ? C4 C4' N4' N4 -1.9(10) . . . . ? N3 C4' N4' N4 66.7(8) . . . . ? C4 C4' N4' C6 -68.8(9) . . . . ? N3 C4' N4' C6 -0.1(8) . . . . ? N4 C4' N4' C6 -66.8(7) . . . . ? C4 C4' N4' C7' 110.2(10) . . . . ? N3 C4' N4' C7' 178.9(7) . . . . ? N4 C4' N4' C7' 112.2(11) . . . . ? N3 C4' N4' C4 68.7(8) . . . . ? N4 C4' N4' C4 1.9(10) . . . . ? C4 C4' N4' C7 41.7(10) . . . . ? N3 C4' N4' C7 110.4(7) . . . . ? N4 C4' N4' C7 43.6(7) . . . . ? C5 C6 N4' N4 -94.9(7) . . . . ? C5 C6 N4' C4' -10.2(7) . . . . ? N4 C6 N4' C4' 84.7(8) . . . . ? C5 C6 N4' C7' 170.8(6) . . . . ? N4 C6 N4' C7' -94.3(9) . . . . ? C5 C6 N4' C4 -40.2(5) . . . . ? N4 C6 N4' C4 54.7(7) . . . . ? C5 C6 N4' C7 -133.0(5) . . . . ? N4 C6 N4' C7 -38.2(7) . . . . ? C8' C7' N4' N4 -30.2(14) . . . . ? C8 C7' N4' N4 -3.6(11) . . . . ? C7 C7' N4' N4 3.2(9) . . . . ? C8' C7' N4' C4' -135.6(11) . . . . ? C8 C7' N4' C4' -108.9(10) . . . . ? C7 C7' N4' C4' -102.1(9) . . . . ? N4 C7' N4' C4' -105.3(12) . . . . ? C8' C7' N4' C6 43.3(13) . . . . ? C8 C7' N4' C6 69.9(10) . . . . ? C7 C7' N4' C6 76.7(8) . . . . ? N4 C7' N4' C6 73.5(9) . . . . ? C8' C7' N4' C4 -93.8(13) . . . . ? C8 C7' N4' C4 -67.1(11) . . . . ? C7 C7' N4' C4 -60.3(9) . . . . ? N4 C7' N4' C4 -63.5(9) . . . . ? C8' C7' N4' C7 -33.4(10) . . . . ? C8 C7' N4' C7 -6.8(8) . . . . ? N4 C7' N4' C7 -3.2(9) . . . . ? C4' C4 N4' N4 177.8(12) . . . . ? N3 C4 N4' N4 113.5(9) . . . . ? N3 C4 N4' C4' -64.3(8) . . . . ? N4 C4 N4' C4' -177.8(12) . . . . ? C4' C4 N4' C6 116.9(8) . . . . ? N3 C4 N4' C6 52.6(6) . . . . ? N4 C4 N4' C6 -60.9(7) . . . . ? C4' C4 N4' C7' -96.8(11) . . . . ? N3 C4 N4' C7' -161.1(7) . . . . ? N4 C4 N4' C7' 85.5(10) . . . . ? C4' C4 N4' C7 -143.9(9) . . . . ? N3 C4 N4' C7 151.8(6) . . . . ? N4 C4 N4' C7 38.4(7) . . . . ? C8 C7 N4' N4 -165.4(18) . . . . ? C8' C7 N4' N4 -155.5(12) . . . . ? C7' C7 N4' N4 -175.9(12) . . . . ? C8 C7 N4' C4' 128.5(13) . . . . ? N4 C7 N4' C4' -66.0(10) . . . . ? C8' C7 N4' C4' 138.5(7) . . . . ? C7' C7 N4' C4' 118.0(8) . . . . ? C8 C7 N4' C6 -116.4(14) . . . . ? N4 C7 N4' C6 49.1(9) . . . . ? C8' C7 N4' C6 -106.4(7) . . . . ? C7' C7 N4' C6 -126.8(7) . . . . ? C8 C7 N4' C7' 10.5(12) . . . . ? N4 C7 N4' C7' 175.9(12) . . . . ? C8' C7 N4' C7' 20.4(6) . . . . ? C8 C7 N4' C4 149.4(14) . . . . ? N4 C7 N4' C4 -45.1(9) . . . . ? C8' C7 N4' C4 159.4(7) . . . . ? C7' C7 N4' C4 139.0(7) . . . . ? C4' N4' N4 C4 1.2(6) . . . . ? C6 N4' N4 C4 109.2(5) . . . . ? C7' N4' N4 C4 -128.3(7) . . . . ? C7 N4' N4 C4 -124.8(9) . . . . ? C4' N4' N4 C6 -108.0(5) . . . . ? C7' N4' N4 C6 122.5(6) . . . . ? C4 N4' N4 C6 -109.2(5) . . . . ? C7 N4' N4 C6 126.1(8) . . . . ? C4' N4' N4 C7 126.0(8) . . . . ? C6 N4' N4 C7 -126.1(8) . . . . ? C7' N4' N4 C7 -3.6(10) . . . . ? C4 N4' N4 C7 124.8(9) . . . . ? C6 N4' N4 C4' 108.0(5) . . . . ? C7' N4' N4 C4' -129.5(8) . . . . ? C4 N4' N4 C4' -1.2(6) . . . . ? C7 N4' N4 C4' -126.0(8) . . . . ? C4' N4' N4 C7' 129.5(8) . . . . ? C6 N4' N4 C7' -122.5(6) . . . . ? C4 N4' N4 C7' 128.3(7) . . . . ? C7 N4' N4 C7' 3.6(10) . . . . ? C4' C4 N4 N4' -1.9(10) . . . . ? N3 C4 N4 N4' -74.8(9) . . . . ? C4' C4 N4 C6 73.8(9) . . . . ? N3 C4 N4 C6 0.9(9) . . . . ? N4' C4 N4 C6 75.7(7) . . . . ? C4' C4 N4 C7 -108.2(11) . . . . ? N3 C4 N4 C7 178.9(8) . . . . ? N4' C4 N4 C7 -106.3(11) . . . . ? N3 C4 N4 C4' -72.9(8) . . . . ? N4' C4 N4 C4' 1.9(10) . . . . ? C4' C4 N4 C7' -42.5(10) . . . . ? N3 C4 N4 C7' -115.4(7) . . . . ? N4' C4 N4 C7' -40.6(6) . . . . ? C5 C6 N4 N4' 93.6(7) . . . . ? C5 C6 N4 C4 10.7(8) . . . . ? N4' C6 N4 C4 -82.9(8) . . . . ? C5 C6 N4 C7 -167.2(8) . . . . ? N4' C6 N4 C7 99.1(11) . . . . ? C5 C6 N4 C4' 41.0(6) . . . . ? N4' C6 N4 C4' -52.6(6) . . . . ? C5 C6 N4 C7' 134.2(5) . . . . ? N4' C6 N4 C7' 40.6(6) . . . . ? C8 C7 N4 N4' 20(2) . . . . ? C8' C7 N4 N4' 26.5(13) . . . . ? C7' C7 N4 N4' 3.2(9) . . . . ? C8 C7 N4 C4 117(2) . . . . ? C8' C7 N4 C4 123.6(10) . . . . ? C7' C7 N4 C4 100.4(9) . . . . ? N4' C7 N4 C4 97.1(12) . . . . ? C8 C7 N4 C6 -65(2) . . . . ? C8' C7 N4 C6 -58.8(13) . . . . ? C7' C7 N4 C6 -82.0(9) . . . . ? N4' C7 N4 C6 -85.3(10) . . . . ? C8 C7 N4 C4' 78(2) . . . . ? C8' C7 N4 C4' 84.7(12) . . . . ? C7' C7 N4 C4' 61.4(9) . . . . ? N4' C7 N4 C4' 58.2(8) . . . . ? C8 C7 N4 C7' 16.6(19) . . . . ? C8' C7 N4 C7' 23.3(7) . . . . ? N4' C7 N4 C7' -3.2(9) . . . . ? C4 C4' N4 N4' 177.7(12) . . . . ? N3 C4' N4 N4' -119.9(8) . . . . ? N4' C4' N4 C4 -177.7(12) . . . . ? N3 C4' N4 C4 62.4(8) . . . . ? C4 C4' N4 C6 -113.1(9) . . . . ? N4' C4' N4 C6 69.2(7) . . . . ? N3 C4' N4 C6 -50.7(6) . . . . ? C4 C4' N4 C7 95.3(11) . . . . ? N4' C4' N4 C7 -82.4(10) . . . . ? N3 C4' N4 C7 157.7(8) . . . . ? C4 C4' N4 C7' 142.5(9) . . . . ? N4' C4' N4 C7' -35.2(6) . . . . ? N3 C4' N4 C7' -155.2(5) . . . . ? C8' C7' N4 N4' 155.0(12) . . . . ? C8 C7' N4 N4' 176.6(11) . . . . ? C7 C7' N4 N4' -175.8(12) . . . . ? C8' C7' N4 C4 -144.6(9) . . . . ? C8 C7' N4 C4 -123.0(8) . . . . ? N4' C7' N4 C4 60.4(9) . . . . ? C7 C7' N4 C4 -115.5(10) . . . . ? C8' C7' N4 C6 97.0(8) . . . . ? C8 C7' N4 C6 118.5(7) . . . . ? N4' C7' N4 C6 -58.1(8) . . . . ? C7 C7' N4 C6 126.1(9) . . . . ? C8' C7' N4 C7 -29.1(9) . . . . ? C8 C7' N4 C7 -7.6(9) . . . . ? N4' C7' N4 C7 175.8(12) . . . . ? C8' C7' N4 C4' -165.2(8) . . . . ? C8 C7' N4 C4' -143.7(7) . . . . ? N4' C7' N4 C4' 39.7(7) . . . . ? C7 C7' N4 C4' -136.1(8) . . . . ? O1 C11 O2 Co1 -2.7(5) . . . . ? C12 C11 O2 Co1 175.5(3) . . . . ? O3 C14 O4 Co1 -4.2(4) . . . 3_766 ? C13 C14 O4 Co1 179.4(2) . . . 3_766 ? C11 O2 Co1 O4 178.5(3) . . . 3_766 ? C11 O2 Co1 N1 -49.5(3) . . . 2_654 ? C11 O2 Co1 N3 71.5(3) . . . . ? C4 N3 Co1 O2 -125.1(5) . . . . ? C5 N3 Co1 O2 81.5(4) . . . . ? C4' N3 Co1 O2 -80.2(5) . . . . ? C4 N3 Co1 O4 126.2(5) . . . 3_766 ? C5 N3 Co1 O4 -27.2(4) . . . 3_766 ? C4' N3 Co1 O4 171.1(5) . . . 3_766 ? C4 N3 Co1 N1 6.1(5) . . . 2_654 ? C5 N3 Co1 N1 -147.3(3) . . . 2_654 ? C4' N3 Co1 N1 51.0(5) . . . 2_654 ? 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 O1W H1B O3 0.89(3) 1.95(3) 2.837(5) 175(5) . _diffrn_measured_fraction_theta_max 0.934 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.646 _refine_diff_density_min -0.388 _refine_diff_density_rms 0.087 #===END