data_global #============================================================================== # 1. SUBMISSION DETAILS _publ_contact_autor ; Dr. I. Ivanovic-Burmazovic Institut f\"ur Anorganische Chemie Universit\"at Erlangen-N\"urnberg Egerlandstr. 1 D-91058 Erlangen Bundesrepublik Deutschland ; _publ_contact_author_phone '049 9131 852-7391' _publ_contact_author_fax '049 9131 852-7387' _publ_contact_author_email 'ivana.ivanovic@chemie.uni-erlangen.de' _publ_requested_journal 'Inorg. Chem.' _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider this CIF submission for data deposition. ; #============================================================================== # 2. TITLE AND AUTHOR LIST _publ_section_title ; Seven-Coordinate Complexes with Acyclic and Rigid Pentadentate Chelates as Superoxide Dismutase Mimetics ; loop_ _publ_author_name _publ_author_address 'Liu, G.-F.' ; Institut f\"ur Anorganische Chemie Universit\"at Erlangen-N\"urnberg Egerlandstr. 1 D-91058 Erlangen Bundesrepublik Deutschland ; 'Filipovic, M.' ; Institut f\"ur Anorganische Chemie Universit\"at Erlangen-N\"urnberg Egerlandstr. 1 D-91058 Erlangen Bundesrepublik Deutschland ; 'Heinemann, F. W.' ; Institut f\"ur Anorganische Chemie Universit\"at Erlangen-N\"urnberg Egerlandstr. 1 D-91058 Erlangen Bundesrepublik Deutschland ; 'Ivanovic-Burmazovic, I.' ; Institut f\"ur Anorganische Chemie Universit\"at Erlangen-N\"urnberg Egerlandstr. 1 D-91058 Erlangen Bundesrepublik Deutschland ; #============================================================================== # 3. TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_experimental ; source of material: see actual publication ; _publ_section_references ; ? ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #============================================================================== # 4. RESULTS FOR 2 data_ii0507 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H19 Fe N7 O6, 2(N O3), H2 O' _chemical_formula_sum 'C13 H21 Fe N9 O13' _chemical_formula_weight 567.24 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' 'Fe' 'Fe' 0.3463 0.8444 '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 _symmetry_space_group_name_Hall -P2ybc 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 8.0028(6) _cell_length_b 14.6046(5) _cell_length_c 18.226(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.079(9) _cell_angle_gamma 90.00 _cell_volume 2127.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 309 _cell_measurement_theta_min 6.00 _cell_measurement_theta_max 20.00 _exptl_crystal_description rhomb _exptl_crystal_colour black _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.771 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1168 _exptl_absorpt_coefficient_mu 0.799 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.852 _exptl_absorpt_correction_T_max 0.923 _exptl_absorpt_process_details 'SADABS, Bruker-AXS, 2002' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius KappaCCD' _diffrn_measurement_method ; \f- and \w-rotations with 1.80 \% and 72 sec per frame ; _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54411 _diffrn_reflns_av_R_equivalents 0.0307 _diffrn_reflns_av_sigmaI/netI 0.0181 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 28.70 _reflns_number_total 5491 _reflns_number_gt 4700 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Bruker-Nonius, 2002)' _computing_cell_refinement 'EVALCCD (Duisenberg, 2003)' _computing_data_reduction 'EVALCCD (Duisenberg, 2003)' _computing_structure_solution 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_structure_refinement 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_molecular_graphics 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_publication_material 'SHELXTL 6.12 (Bruker AXS, 2002)' _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^)+(0.0344P)^2^+1.2403P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refxyz _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5491 _refine_ls_number_parameters 388 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0356 _refine_ls_R_factor_gt 0.0262 _refine_ls_wR_factor_ref 0.0671 _refine_ls_wR_factor_gt 0.0629 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.006 _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 Fe1 Fe 0.01948(2) 0.161443(12) 0.143094(10) 0.00687(6) Uani 1 1 d . . . O1 O -0.09736(11) 0.27108(6) 0.07751(5) 0.00998(18) Uani 1 1 d . . . O2 O -0.01218(12) 0.41774(7) -0.06844(5) 0.0133(2) Uani 1 1 d . . . O3 O -0.21688(11) 0.18395(6) 0.19617(5) 0.00990(18) Uani 1 1 d . . . O4 O -0.41598(12) 0.09412(7) 0.34657(5) 0.0149(2) Uani 1 1 d . . . O5 O -0.09600(12) 0.06568(7) 0.06694(5) 0.01151(19) Uani 1 1 d D . . H5A H -0.086(2) 0.0090(10) 0.0746(9) 0.014 Uiso 1 1 d D . . H5B H -0.103(2) 0.0762(12) 0.0221(8) 0.014 Uiso 1 1 d D . . O6 O 0.13758(12) 0.25566(6) 0.22107(5) 0.01094(19) Uani 1 1 d D . . H6A H 0.089(2) 0.2682(12) 0.2582(8) 0.013 Uiso 1 1 d D . . H6B H 0.174(2) 0.3028(10) 0.2035(9) 0.013 Uiso 1 1 d D . . N1 N 0.24781(13) 0.07663(7) 0.15058(6) 0.0082(2) Uani 1 1 d . . . N2 N 0.19102(14) 0.20220(7) 0.05610(6) 0.0086(2) Uani 1 1 d . . . N3 N 0.13375(14) 0.27206(7) 0.01087(6) 0.0088(2) Uani 1 1 d . . . H3N H 0.189(2) 0.2929(11) -0.0247(9) 0.011 Uiso 1 1 d . . . N4 N -0.24285(14) 0.40574(8) -0.00131(6) 0.0115(2) Uani 1 1 d . . . H4A H -0.290(2) 0.3778(12) 0.0345(10) 0.014 Uiso 1 1 d . . . H4B H -0.294(2) 0.4487(12) -0.0241(10) 0.014 Uiso 1 1 d . . . N5 N 0.00710(13) 0.06320(7) 0.23548(6) 0.0083(2) Uani 1 1 d . . . N6 N -0.13414(14) 0.07008(8) 0.27461(6) 0.0091(2) Uani 1 1 d . . . H6N H -0.146(2) 0.0409(12) 0.3122(10) 0.011 Uiso 1 1 d . . . N7 N -0.50677(15) 0.20508(8) 0.26507(6) 0.0116(2) Uani 1 1 d . . . H7D H -0.598(2) 0.2084(12) 0.2840(10) 0.014 Uiso 1 1 d . . . H7E H -0.486(2) 0.2361(12) 0.2284(10) 0.014 Uiso 1 1 d . . . C1 C 0.36962(16) 0.09034(8) 0.10379(7) 0.0089(2) Uani 1 1 d . . . C2 C 0.51608(17) 0.03837(9) 0.10776(7) 0.0117(3) Uani 1 1 d . . . H2 H 0.600(2) 0.0507(12) 0.0753(9) 0.014 Uiso 1 1 d . . . C3 C 0.53401(17) -0.02923(9) 0.16158(7) 0.0123(3) Uani 1 1 d . . . H3 H 0.631(2) -0.0667(12) 0.1657(9) 0.015 Uiso 1 1 d . . . C4 C 0.40856(17) -0.04289(9) 0.21017(7) 0.0109(2) Uani 1 1 d . . . H4 H 0.420(2) -0.0869(12) 0.2474(9) 0.013 Uiso 1 1 d . . . C5 C 0.26617(16) 0.01229(8) 0.20300(7) 0.0085(2) Uani 1 1 d . . . C6 C 0.33573(16) 0.16530(9) 0.04940(7) 0.0096(2) Uani 1 1 d . . . C7 C 0.46352(19) 0.19131(11) -0.00354(8) 0.0168(3) Uani 1 1 d . . . H7A H 0.500(2) 0.1416(13) -0.0278(10) 0.020 Uiso 1 1 d . . . H7B H 0.439(2) 0.2409(13) -0.0304(10) 0.020 Uiso 1 1 d . . . H7C H 0.568(2) 0.2076(13) 0.0250(10) 0.020 Uiso 1 1 d . . . C8 C -0.01841(16) 0.30296(9) 0.02709(7) 0.0084(2) Uani 1 1 d . . . C9 C -0.09237(16) 0.38215(9) -0.01975(7) 0.0092(2) Uani 1 1 d . . . C10 C 0.12519(16) 0.00614(8) 0.25287(7) 0.0079(2) Uani 1 1 d . . . C11 C 0.13467(17) -0.06043(9) 0.31498(7) 0.0112(2) Uani 1 1 d . . . H11A H 0.147(2) -0.1218(12) 0.2968(9) 0.013 Uiso 1 1 d . . . H11B H 0.041(2) -0.0553(12) 0.3432(9) 0.013 Uiso 1 1 d . . . H11C H 0.236(2) -0.0491(11) 0.3454(9) 0.013 Uiso 1 1 d . . . C12 C -0.24072(16) 0.13569(9) 0.25005(7) 0.0085(2) Uani 1 1 d . . . C13 C -0.39868(16) 0.14387(9) 0.29308(7) 0.0095(2) Uani 1 1 d . . . N10 N 0.60923(14) 0.88752(7) 0.38799(6) 0.0105(2) Uani 1 1 d . . . O11 O 0.49759(13) 0.83350(7) 0.36323(5) 0.0152(2) Uani 1 1 d . . . O12 O 0.73903(13) 0.90100(7) 0.35268(6) 0.0169(2) Uani 1 1 d . . . O13 O 0.59219(13) 0.92675(7) 0.44766(5) 0.0166(2) Uani 1 1 d . . . N20 N 0.04480(15) 0.84581(8) 0.11767(6) 0.0117(2) Uani 1 1 d . . . O21 O 0.14820(13) 0.86151(8) 0.07017(5) 0.0179(2) Uani 1 1 d . . . O22 O -0.09141(13) 0.88933(7) 0.11675(6) 0.0190(2) Uani 1 1 d . . . O23 O 0.07629(14) 0.78729(7) 0.16630(6) 0.0201(2) Uani 1 1 d . . . O7 O 0.27440(14) 0.15461(7) 0.38514(6) 0.0155(2) Uani 1 1 d . . . H7F H 0.194(2) 0.1202(13) 0.3904(10) 0.019 Uiso 1 1 d . . . H7G H 0.359(3) 0.1247(13) 0.3853(10) 0.019 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 Fe1 0.00625(9) 0.00773(9) 0.00675(9) 0.00082(6) 0.00151(6) 0.00120(6) O1 0.0101(4) 0.0112(4) 0.0089(4) 0.0020(3) 0.0031(3) 0.0012(3) O2 0.0134(5) 0.0151(5) 0.0118(4) 0.0046(4) 0.0034(4) 0.0017(4) O3 0.0094(4) 0.0114(4) 0.0090(4) 0.0023(3) 0.0019(3) 0.0012(3) O4 0.0143(5) 0.0180(5) 0.0131(5) 0.0062(4) 0.0057(4) 0.0040(4) O5 0.0152(5) 0.0101(4) 0.0091(4) 0.0002(3) 0.0001(4) -0.0008(4) O6 0.0132(5) 0.0101(4) 0.0097(4) -0.0006(3) 0.0031(4) -0.0005(4) N1 0.0080(5) 0.0082(5) 0.0086(5) -0.0008(4) 0.0005(4) 0.0003(4) N2 0.0096(5) 0.0079(5) 0.0081(5) 0.0010(4) 0.0000(4) -0.0002(4) N3 0.0105(5) 0.0089(5) 0.0072(5) 0.0024(4) 0.0024(4) 0.0005(4) N4 0.0115(6) 0.0131(5) 0.0099(5) 0.0040(4) 0.0018(4) 0.0033(4) N5 0.0076(5) 0.0098(5) 0.0078(5) -0.0006(4) 0.0022(4) -0.0005(4) N6 0.0081(5) 0.0116(5) 0.0079(5) 0.0021(4) 0.0036(4) 0.0013(4) N7 0.0084(5) 0.0144(6) 0.0123(6) 0.0031(4) 0.0041(4) 0.0026(4) C1 0.0088(6) 0.0091(6) 0.0090(6) -0.0017(4) 0.0009(4) -0.0009(5) C2 0.0090(6) 0.0139(6) 0.0125(6) -0.0014(5) 0.0029(5) 0.0005(5) C3 0.0085(6) 0.0140(6) 0.0144(6) -0.0019(5) -0.0001(5) 0.0032(5) C4 0.0113(6) 0.0101(6) 0.0109(6) -0.0003(5) -0.0010(5) 0.0011(5) C5 0.0091(6) 0.0082(6) 0.0080(5) -0.0016(4) -0.0002(4) -0.0011(5) C6 0.0097(6) 0.0097(6) 0.0095(6) -0.0010(5) 0.0019(5) -0.0013(5) C7 0.0166(7) 0.0147(7) 0.0202(7) 0.0042(6) 0.0114(6) 0.0018(5) C8 0.0095(6) 0.0076(6) 0.0080(5) -0.0010(4) -0.0005(4) -0.0011(4) C9 0.0116(6) 0.0090(6) 0.0069(5) -0.0007(4) -0.0007(4) -0.0006(5) C10 0.0085(6) 0.0078(5) 0.0074(5) -0.0014(4) 0.0002(4) -0.0008(4) C11 0.0116(6) 0.0114(6) 0.0106(6) 0.0026(5) 0.0020(5) 0.0020(5) C12 0.0078(6) 0.0096(6) 0.0081(6) -0.0017(4) 0.0004(4) -0.0006(4) C13 0.0090(6) 0.0109(6) 0.0088(6) -0.0008(4) 0.0015(5) 0.0000(5) N10 0.0116(5) 0.0078(5) 0.0119(5) 0.0018(4) 0.0005(4) 0.0017(4) O11 0.0151(5) 0.0140(5) 0.0161(5) -0.0017(4) -0.0033(4) -0.0034(4) O12 0.0162(5) 0.0125(5) 0.0231(5) 0.0010(4) 0.0114(4) 0.0006(4) O13 0.0212(5) 0.0156(5) 0.0133(5) -0.0051(4) 0.0056(4) -0.0042(4) N20 0.0143(6) 0.0115(5) 0.0093(5) -0.0021(4) 0.0013(4) -0.0020(4) O21 0.0167(5) 0.0267(6) 0.0109(5) 0.0031(4) 0.0045(4) -0.0017(4) O22 0.0166(5) 0.0138(5) 0.0273(6) 0.0022(4) 0.0059(4) 0.0042(4) O23 0.0216(6) 0.0229(5) 0.0161(5) 0.0096(4) 0.0038(4) 0.0042(4) O7 0.0112(5) 0.0196(5) 0.0164(5) -0.0030(4) 0.0058(4) -0.0008(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 Fe1 O5 2.1444(10) . ? Fe1 O6 2.1592(10) . ? Fe1 O1 2.1788(9) . ? Fe1 O3 2.1951(9) . ? Fe1 N1 2.2057(11) . ? Fe1 N5 2.2184(11) . ? Fe1 N2 2.2330(11) . ? O1 C8 1.2340(16) . ? O2 C9 1.2372(16) . ? O3 C12 1.2320(16) . ? O4 C13 1.2298(16) . ? O5 H5A 0.843(14) . ? O5 H5B 0.831(14) . ? O6 H6A 0.820(14) . ? O6 H6B 0.819(14) . ? N1 C5 1.3425(16) . ? N1 C1 1.3442(17) . ? N2 C6 1.2891(17) . ? N2 N3 1.3749(15) . ? N3 C8 1.3463(17) . ? N3 H3N 0.859(17) . ? N4 C9 1.3135(17) . ? N4 H4A 0.874(18) . ? N4 H4B 0.846(19) . ? N5 C10 1.2868(17) . ? N5 N6 1.3722(15) . ? N6 C12 1.3434(17) . ? N6 H6N 0.818(18) . ? N7 C13 1.3269(17) . ? N7 H7D 0.829(19) . ? N7 H7E 0.832(18) . ? C1 C2 1.3950(18) . ? C1 C6 1.4919(18) . ? C2 C3 1.3937(19) . ? C2 H2 0.938(18) . ? C3 C4 1.3883(19) . ? C3 H3 0.947(18) . ? C4 C5 1.3961(18) . ? C4 H4 0.935(17) . ? C5 C10 1.4890(17) . ? C6 C7 1.4925(18) . ? C7 H7A 0.906(19) . ? C7 H7B 0.889(19) . ? C7 H7C 0.988(19) . ? C8 C9 1.5370(17) . ? C10 C11 1.4911(17) . ? C11 H11A 0.963(18) . ? C11 H11B 0.936(18) . ? C11 H11C 0.971(17) . ? C12 C13 1.5277(18) . ? N10 O13 1.2433(15) . ? N10 O11 1.2574(15) . ? N10 O12 1.2663(15) . ? N20 O23 1.2472(15) . ? N20 O21 1.2504(15) . ? N20 O22 1.2612(16) . ? O7 H7F 0.83(2) . ? O7 H7G 0.80(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 O5 Fe1 O6 178.88(4) . . ? O5 Fe1 O1 88.10(4) . . ? O6 Fe1 O1 93.01(4) . . ? O5 Fe1 O3 91.79(4) . . ? O6 Fe1 O3 88.37(4) . . ? O1 Fe1 O3 77.12(3) . . ? O5 Fe1 N1 90.03(4) . . ? O6 Fe1 N1 89.16(4) . . ? O1 Fe1 N1 140.93(4) . . ? O3 Fe1 N1 141.95(4) . . ? O5 Fe1 N5 91.96(4) . . ? O6 Fe1 N5 87.04(4) . . ? O1 Fe1 N5 148.91(4) . . ? O3 Fe1 N5 71.80(4) . . ? N1 Fe1 N5 70.15(4) . . ? O5 Fe1 N2 88.53(4) . . ? O6 Fe1 N2 91.92(4) . . ? O1 Fe1 N2 71.14(4) . . ? O3 Fe1 N2 148.23(4) . . ? N1 Fe1 N2 69.80(4) . . ? N5 Fe1 N2 139.95(4) . . ? C8 O1 Fe1 117.65(8) . . ? C12 O3 Fe1 116.08(8) . . ? Fe1 O5 H5A 120.0(12) . . ? Fe1 O5 H5B 121.3(12) . . ? H5A O5 H5B 110.2(17) . . ? Fe1 O6 H6A 118.3(12) . . ? Fe1 O6 H6B 115.4(12) . . ? H6A O6 H6B 109.3(17) . . ? C5 N1 C1 120.02(11) . . ? C5 N1 Fe1 119.72(8) . . ? C1 N1 Fe1 120.25(8) . . ? C6 N2 N3 121.72(11) . . ? C6 N2 Fe1 123.06(9) . . ? N3 N2 Fe1 115.20(8) . . ? C8 N3 N2 113.16(10) . . ? C8 N3 H3N 123.6(11) . . ? N2 N3 H3N 123.2(11) . . ? C9 N4 H4A 120.6(11) . . ? C9 N4 H4B 119.7(12) . . ? H4A N4 H4B 119.7(16) . . ? C10 N5 N6 122.27(11) . . ? C10 N5 Fe1 122.93(9) . . ? N6 N5 Fe1 114.75(8) . . ? C12 N6 N5 113.90(11) . . ? C12 N6 H6N 123.3(12) . . ? N5 N6 H6N 122.4(12) . . ? C13 N7 H7D 117.0(12) . . ? C13 N7 H7E 121.4(12) . . ? H7D N7 H7E 121.5(17) . . ? N1 C1 C2 121.46(12) . . ? N1 C1 C6 114.75(11) . . ? C2 C1 C6 123.78(12) . . ? C3 C2 C1 118.45(12) . . ? C3 C2 H2 122.0(11) . . ? C1 C2 H2 119.5(10) . . ? C4 C3 C2 120.01(12) . . ? C4 C3 H3 118.8(10) . . ? C2 C3 H3 121.2(10) . . ? C3 C4 C5 118.16(12) . . ? C3 C4 H4 121.0(10) . . ? C5 C4 H4 120.8(10) . . ? N1 C5 C4 121.89(12) . . ? N1 C5 C10 114.78(11) . . ? C4 C5 C10 123.33(11) . . ? N2 C6 C1 112.09(11) . . ? N2 C6 C7 127.23(12) . . ? C1 C6 C7 120.66(12) . . ? C6 C7 H7A 111.0(12) . . ? C6 C7 H7B 115.1(12) . . ? H7A C7 H7B 116.8(16) . . ? C6 C7 H7C 108.0(11) . . ? H7A C7 H7C 99.7(15) . . ? H7B C7 H7C 104.4(16) . . ? O1 C8 N3 122.85(12) . . ? O1 C8 C9 120.02(11) . . ? N3 C8 C9 117.13(11) . . ? O2 C9 N4 126.25(12) . . ? O2 C9 C8 121.02(12) . . ? N4 C9 C8 112.72(11) . . ? N5 C10 C5 112.40(11) . . ? N5 C10 C11 128.03(12) . . ? C5 C10 C11 119.57(11) . . ? C10 C11 H11A 110.4(10) . . ? C10 C11 H11B 110.8(10) . . ? H11A C11 H11B 111.1(14) . . ? C10 C11 H11C 109.2(10) . . ? H11A C11 H11C 105.1(14) . . ? H11B C11 H11C 110.0(14) . . ? O3 C12 N6 123.43(12) . . ? O3 C12 C13 122.15(11) . . ? N6 C12 C13 114.39(11) . . ? O4 C13 N7 127.18(13) . . ? O4 C13 C12 119.49(12) . . ? N7 C13 C12 113.30(11) . . ? O13 N10 O11 119.60(11) . . ? O13 N10 O12 120.29(11) . . ? O11 N10 O12 120.11(11) . . ? O23 N20 O21 120.11(12) . . ? O23 N20 O22 119.75(11) . . ? O21 N20 O22 120.14(11) . . ? H7F O7 H7G 109.2(18) . . ? 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 N4 H4A O1 0.874(18) 2.301(17) 2.6659(15) 105.1(13) . N7 H7E O3 0.832(18) 2.386(17) 2.7142(15) 104.3(14) . N3 H3N O2 0.859(17) 2.531(16) 2.7925(14) 98.6(12) . N6 H6N O4 0.818(18) 2.408(17) 2.6924(15) 101.4(13) . O5 H5A O22 0.843(14) 1.910(14) 2.7304(14) 164.0(17) 1_545 O5 H5B O21 0.831(14) 1.929(15) 2.7274(14) 160.7(17) 3_565 O6 H6A O23 0.820(14) 1.978(14) 2.7810(14) 166.2(17) 2_545 O6 H6B O12 0.819(14) 1.915(14) 2.7259(14) 170.3(17) 2_645 N3 H3N O7 0.859(17) 1.969(17) 2.8181(15) 169.5(16) 4_565 N4 H4A O13 0.874(18) 2.557(17) 3.0266(16) 114.5(13) 2_545 N4 H4A O11 0.874(18) 2.641(18) 3.4863(16) 163.0(15) 2_545 N4 H4B O13 0.846(19) 2.086(19) 2.9088(15) 163.9(16) 4_475 N4 H4B O4 0.846(19) 2.579(17) 3.0322(16) 114.8(14) 4_565 N6 H6N O12 0.818(18) 2.374(17) 3.0509(15) 140.7(15) 1_445 N6 H6N O2 0.818(18) 2.448(17) 2.9779(15) 123.4(14) 4_566 N7 H7D O7 0.829(19) 2.292(18) 2.9684(16) 139.1(16) 1_455 N7 H7D O6 0.829(19) 2.448(18) 3.0074(15) 125.7(15) 1_455 N7 H7E O11 0.832(18) 2.192(18) 3.0015(15) 164.5(16) 2_545 O7 H7F O2 0.83(2) 1.93(2) 2.7020(15) 155.2(18) 4_566 O7 H7G O4 0.80(2) 2.02(2) 2.7570(15) 152.0(18) 1_655 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.70 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.487 _refine_diff_density_min -0.336 _refine_diff_density_rms 0.061 #===END OF ALL DATA