Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Shyamal Kumar Chattopadhyay' _publ_contact_author_email shch20@hotmail.com _publ_section_title ;Versatility of 2,6-diacetylpyridine (dap) hydrazones in generating double helical structures: synthesis and structural characterization of a binuclear Zn(II) and a trinuclear Mn(II) complex. ; loop_ _publ_author_name S.K.Chattopadhyay A.J.Blake M.Corbella S.Naskar data_znpyne _database_code_depnum_ccdc_archive 'CCDC 622114' _refine_special_details ; One solvent molecule is disordered and partially occupied. It was not possible to model this molecule is terms of atomic sites but the region could be modelled using PLATON SQUEEZE. This program identified regions corresponding to 222 A**3 and 17 electrons per unit cell. The electron density was assigned as 0.25 DMF per asymmetric unit. ; _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H42 N14 O4 Zn2, 2.25(C3 H7 N O)' _chemical_formula_sum 'C52.75 H56.75 N16.25 O6.25 Zn2' _chemical_formula_weight 1149.13 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.368(2) _cell_length_b 14.379(2) _cell_length_c 15.938(2) _cell_angle_alpha 65.408(2) _cell_angle_beta 74.714(2) _cell_angle_gamma 79.138(2) _cell_volume 2676.3(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9682 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.426 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1194 _exptl_absorpt_coefficient_mu 0.963 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min . _exptl_absorpt_correction_T_max . _exptl_absorpt_process_details . _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 24377 _diffrn_reflns_av_R_equivalents 0.057 _diffrn_reflns_av_sigmaI/netI 0.059 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 27.55 _reflns_number_total 11941 _reflns_number_gt 9119 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART version 5.624 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36a (Bruker, 2002)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'enCIFer (Allen et al., 2004); PLATON' _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^)+(0.054P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'sp2 methyl H atoms from delta-F; others placed geometrically' _refine_ls_hydrogen_treatment 'rigid rotor; riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11941 _refine_ls_number_parameters 693 _refine_ls_number_restraints 222 _refine_ls_R_factor_all 0.0496 _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_ref 0.0982 _refine_ls_wR_factor_gt 0.0937 _refine_ls_goodness_of_fit_ref 0.96 _refine_ls_restrained_S_all 0.96 _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 0.295255(17) 0.130742(17) 0.387565(17) 0.02470(7) Uani 1 1 d U . . Zn2 Zn 0.303999(16) 0.136059(16) 0.161355(16) 0.02112(7) Uani 1 1 d U . . N1 N 0.24737(12) 0.00426(12) 0.30599(11) 0.0212(3) Uani 1 1 d U . . C2 C 0.14996(15) -0.00244(15) 0.35822(13) 0.0228(4) Uani 1 1 d U . . C3 C 0.10849(16) -0.09558(16) 0.41348(14) 0.0279(4) Uani 1 1 d U . . H3 H 0.0375 -0.0979 0.4453 0.033 Uiso 1 1 calc R . . C4 C 0.17264(17) -0.18553(16) 0.42143(14) 0.0297(5) Uani 1 1 d U . . H4 H 0.1474 -0.2504 0.4619 0.036 Uiso 1 1 calc R . . C5 C 0.27355(16) -0.17944(15) 0.36982(14) 0.0271(4) Uani 1 1 d U . . H5 H 0.3190 -0.2400 0.3749 0.032 Uiso 1 1 calc R . . C6 C 0.30785(15) -0.08348(15) 0.31021(13) 0.0221(4) Uani 1 1 d U . . C7 C 0.40979(15) -0.07160(14) 0.24400(13) 0.0206(4) Uani 1 1 d U . . C7A C 0.49180(16) -0.15963(15) 0.25459(15) 0.0302(5) Uani 1 1 d U . . H7A H 0.4719 -0.2094 0.2360 0.045 Uiso 1 1 calc R . . H7B H 0.4991 -0.1929 0.3205 0.045 Uiso 1 1 calc R . . H7C H 0.5583 -0.1344 0.2142 0.045 Uiso 1 1 calc R . . O7 O 0.74096(11) 0.50930(11) 0.07585(11) 0.0305(3) Uani 1 1 d U . . N8 N 0.41839(12) 0.01778(12) 0.17611(11) 0.0196(3) Uani 1 1 d U . . O8 O 0.23637(18) 0.2900(2) 0.66047(18) 0.0857(8) Uani 1 1 d U . . N9 N 0.50880(12) 0.03630(12) 0.10860(11) 0.0197(3) Uani 1 1 d U . . O10 O 0.42086(10) 0.19668(10) 0.04544(9) 0.0236(3) Uani 1 1 d U . . C10 C 0.50094(14) 0.13225(14) 0.04363(13) 0.0189(4) Uani 1 1 d U . . C11 C 0.59140(14) 0.16514(14) -0.03572(13) 0.0201(4) Uani 1 1 d U . . C12 C 0.59281(16) 0.27025(15) -0.09185(14) 0.0271(4) Uani 1 1 d U . . H12 H 0.5374 0.3163 -0.0763 0.032 Uiso 1 1 calc R . . C13 C 0.67170(17) 0.30941(16) -0.16889(15) 0.0334(5) Uani 1 1 d U . . H13 H 0.6712 0.3811 -0.2054 0.040 Uiso 1 1 calc R . . C14 C 0.75241(16) 0.24101(17) -0.19193(15) 0.0327(5) Uani 1 1 d U . . H14 H 0.8071 0.2665 -0.2451 0.039 Uiso 1 1 calc R . . C15 C 0.75349(16) 0.13798(16) -0.13889(14) 0.0276(4) Uani 1 1 d U . . H15 H 0.8084 0.0930 -0.1569 0.033 Uiso 1 1 calc R . . N16 N 0.68466(13) -0.00605(12) -0.00514(12) 0.0263(4) Uani 1 1 d U . . H16A H 0.7386 -0.0452 -0.0214 0.032 Uiso 1 1 calc R . . H16B H 0.6366 -0.0332 0.0455 0.032 Uiso 1 1 calc R . . C16 C 0.67546(14) 0.09645(14) -0.05818(13) 0.0211(4) Uani 1 1 d U . . C17 C 0.09155(15) 0.09587(15) 0.35965(13) 0.0229(4) Uani 1 1 d U . . C17A C -0.01997(15) 0.11894(18) 0.35180(16) 0.0309(5) Uani 1 1 d U . . H17A H -0.0515 0.1750 0.3727 0.046 Uiso 1 1 calc R . . H17B H -0.0572 0.0576 0.3915 0.046 Uiso 1 1 calc R . . H17C H -0.0245 0.1393 0.2860 0.046 Uiso 1 1 calc R . . N17 N 0.13465(17) 0.1598(2) 0.71035(16) 0.0521(6) Uani 1 1 d U . . N18 N 0.14473(12) 0.15500(12) 0.37017(11) 0.0221(3) Uani 1 1 d U . . N19 N 0.09493(12) 0.24802(12) 0.37371(11) 0.0229(3) Uani 1 1 d U . . O20 O 0.24831(10) 0.25864(11) 0.41029(10) 0.0268(3) Uani 1 1 d U . . C20 C 0.15602(15) 0.29574(15) 0.39306(13) 0.0232(4) Uani 1 1 d U . . C21 C 0.11761(15) 0.39913(15) 0.39324(13) 0.0247(4) Uani 1 1 d U . . C22 C 0.18583(17) 0.45373(17) 0.40525(15) 0.0306(5) Uani 1 1 d U . . H22 H 0.2533 0.4221 0.4147 0.037 Uiso 1 1 calc R . . C23 C 0.15831(19) 0.55115(17) 0.40377(16) 0.0377(5) Uani 1 1 d U . . H23 H 0.2061 0.5864 0.4119 0.045 Uiso 1 1 calc R . . C24 C 0.05975(19) 0.59767(17) 0.39025(16) 0.0374(5) Uani 1 1 d U . . H24 H 0.0399 0.6651 0.3893 0.045 Uiso 1 1 calc R . . C25 C -0.00889(18) 0.54716(17) 0.37831(15) 0.0346(5) Uani 1 1 d U . . H25 H -0.0757 0.5806 0.3686 0.041 Uiso 1 1 calc R . . N26 N -0.05632(14) 0.39974(14) 0.37003(14) 0.0379(5) Uani 1 1 d U . . H26A H -0.1182 0.4321 0.3626 0.045 Uiso 1 1 calc R . . H26B H -0.0417 0.3371 0.3709 0.045 Uiso 1 1 calc R . . C26 C 0.01668(16) 0.44663(16) 0.38005(14) 0.0275(4) Uani 1 1 d U . . N1' N 0.38483(12) 0.23725(12) 0.22653(11) 0.0226(3) Uani 1 1 d U . . C2' C 0.48714(15) 0.21541(16) 0.22976(14) 0.0250(4) Uani 1 1 d U . . C3' C 0.55741(17) 0.28893(18) 0.17965(16) 0.0350(5) Uani 1 1 d U . . H3' H 0.6296 0.2710 0.1791 0.042 Uiso 1 1 calc R . . C4' C 0.52143(18) 0.38850(18) 0.13057(17) 0.0385(5) Uani 1 1 d U . . H4' H 0.5684 0.4404 0.0979 0.046 Uiso 1 1 calc R . . C5' C 0.41661(17) 0.41252(17) 0.12915(16) 0.0320(5) Uani 1 1 d U . . H5' H 0.3901 0.4812 0.0975 0.038 Uiso 1 1 calc R . . C6' C 0.35085(15) 0.33381(15) 0.17512(14) 0.0239(4) Uani 1 1 d U . . C7' C 0.24309(15) 0.34809(14) 0.16134(13) 0.0216(4) Uani 1 1 d U . . C7B C 0.17603(16) 0.44709(15) 0.14906(15) 0.0273(4) Uani 1 1 d U . . H7D H 0.1655 0.4803 0.0841 0.041 Uiso 1 1 calc R . . HFE H 0.2103 0.4925 0.1624 0.041 Uiso 1 1 calc R . . H7F H 0.1085 0.4331 0.1927 0.041 Uiso 1 1 calc R . . N8' N 0.21587(12) 0.27091(12) 0.15409(11) 0.0199(3) Uani 1 1 d U . . N9' N 0.12031(12) 0.28067(12) 0.13297(11) 0.0202(3) Uani 1 1 d U . . O10' O 0.17901(10) 0.12420(10) 0.11814(10) 0.0237(3) Uani 1 1 d U . . C10' C 0.10962(14) 0.20105(14) 0.11406(13) 0.0195(4) Uani 1 1 d U . . C11' C 0.01246(14) 0.20222(14) 0.08626(13) 0.0214(4) Uani 1 1 d U . . C12' C 0.00073(16) 0.12038(16) 0.06431(15) 0.0296(5) Uani 1 1 d U . . H12' H 0.0553 0.0668 0.0683 0.035 Uiso 1 1 calc R . . C13' C -0.08647(17) 0.11505(18) 0.03738(17) 0.0361(5) Uani 1 1 d U . . H13' H -0.0918 0.0590 0.0224 0.043 Uiso 1 1 calc R . . C14' C -0.16736(17) 0.19303(17) 0.03214(16) 0.0336(5) Uani 1 1 d U . . H14' H -0.2286 0.1895 0.0144 0.040 Uiso 1 1 calc R . . C15' C -0.15893(15) 0.27476(16) 0.05241(15) 0.0281(4) Uani 1 1 d U . . H15' H -0.2147 0.3273 0.0483 0.034 Uiso 1 1 calc R . . C16' C -0.06974(15) 0.28247(15) 0.07907(14) 0.0232(4) Uani 1 1 d U . . N16' N -0.06649(14) 0.36656(13) 0.09645(15) 0.0358(5) Uani 1 1 d U . . H16C H -0.1193 0.4141 0.0909 0.043 Uiso 1 1 calc R . . H16D H -0.0116 0.3735 0.1133 0.043 Uiso 1 1 calc R . . C17' C 0.51589(15) 0.10967(15) 0.29286(14) 0.0246(4) Uani 1 1 d U . . C17B C 0.62334(15) 0.05756(17) 0.27609(16) 0.0311(5) Uani 1 1 d U . . H17D H 0.6507 0.0308 0.3339 0.047 Uiso 1 1 calc R . . H17E H 0.6690 0.1071 0.2252 0.047 Uiso 1 1 calc R . . H17F H 0.6204 0.0007 0.2583 0.047 Uiso 1 1 calc R . . N18' N 0.44191(12) 0.06701(12) 0.36166(11) 0.0229(3) Uani 1 1 d U . . N19' N 0.45937(12) -0.03347(12) 0.42191(12) 0.0234(3) Uani 1 1 d U . . O20' O 0.29188(10) -0.00406(11) 0.50111(10) 0.0283(3) Uani 1 1 d U . . C20' C 0.37564(15) -0.06273(15) 0.49059(14) 0.0234(4) Uani 1 1 d U . . C21' C 0.37904(15) -0.17149(16) 0.55774(14) 0.0258(4) Uani 1 1 d U . . C22' C 0.28723(17) -0.20621(18) 0.62189(16) 0.0335(5) Uani 1 1 d U . . H22' H 0.2274 -0.1586 0.6220 0.040 Uiso 1 1 calc R . . C23' C 0.27938(19) -0.30698(19) 0.68534(17) 0.0414(6) Uani 1 1 d U . . H23' H 0.2156 -0.3283 0.7280 0.050 Uiso 1 1 calc R . . C24' C 0.3672(2) -0.37604(19) 0.68497(18) 0.0472(6) Uani 1 1 d U . . H24' H 0.3632 -0.4459 0.7270 0.057 Uiso 1 1 calc R . . C25' C 0.4597(2) -0.34435(18) 0.62456(18) 0.0452(6) Uani 1 1 d U . . H25' H 0.5193 -0.3926 0.6270 0.054 Uiso 1 1 calc R . . N26' N 0.56287(15) -0.21511(16) 0.50135(15) 0.0521(6) Uani 1 1 d U . . H26C H 0.6172 -0.2609 0.5050 0.063 Uiso 1 1 calc R . . H26D H 0.5691 -0.1515 0.4602 0.063 Uiso 1 1 calc R . . C26' C 0.46880(17) -0.24285(17) 0.55940(16) 0.0353(5) Uani 1 1 d U . . N50 N 0.76380(14) 0.63593(13) 0.11725(13) 0.0302(4) Uani 1 1 d U . . C51 C 0.71538(16) 0.59397(16) 0.08134(15) 0.0284(4) Uani 1 1 d U . . H51 H 0.6557 0.6322 0.0577 0.034 Uiso 1 1 calc R . . C52 C 0.7290(2) 0.73667(17) 0.12001(18) 0.0421(6) Uani 1 1 d U . . H52A H 0.6639 0.7623 0.0971 0.063 Uiso 1 1 calc R . . H52B H 0.7823 0.7840 0.0798 0.063 Uiso 1 1 calc R . . H52C H 0.7172 0.7318 0.1850 0.063 Uiso 1 1 calc R . . C53 C 0.8579(2) 0.58492(19) 0.1522(2) 0.0511(7) Uani 1 1 d U . . H53A H 0.8559 0.5103 0.1765 0.077 Uiso 1 1 calc R . . H53B H 0.8625 0.6046 0.2030 0.077 Uiso 1 1 calc R . . H53C H 0.9189 0.6055 0.1008 0.077 Uiso 1 1 calc R . . C54 C 0.2071(2) 0.2211(3) 0.6506(2) 0.0698(10) Uani 1 1 d U . . H54 H 0.2392 0.2100 0.5944 0.084 Uiso 1 1 calc R . . C55 C 0.0798(3) 0.1734(3) 0.7961(2) 0.0651(8) Uani 1 1 d U . . H55A H 0.1088 0.1220 0.8494 0.098 Uiso 1 1 calc R . . H55B H 0.0058 0.1652 0.8068 0.098 Uiso 1 1 calc R . . H55C H 0.0877 0.2424 0.7904 0.098 Uiso 1 1 calc R . . C56 C 0.1106(2) 0.0739(3) 0.6965(3) 0.0796(11) Uani 1 1 d U . . H56A H 0.1508 0.0737 0.6354 0.119 Uiso 1 1 calc R . . H56B H 0.0361 0.0801 0.6975 0.119 Uiso 1 1 calc R . . H56C H 0.1287 0.0097 0.7470 0.119 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.01847(12) 0.02533(13) 0.02933(14) -0.01062(10) -0.00671(10) 0.00291(9) Zn2 0.01655(11) 0.02053(12) 0.02481(13) -0.00917(10) -0.00462(9) 0.00316(8) N1 0.0207(8) 0.0231(8) 0.0200(8) -0.0087(7) -0.0042(6) -0.0017(6) C2 0.0205(9) 0.0302(10) 0.0207(10) -0.0131(8) -0.0027(8) -0.0034(8) C3 0.0251(10) 0.0353(11) 0.0264(11) -0.0157(9) 0.0001(8) -0.0090(9) C4 0.0377(12) 0.0271(10) 0.0223(10) -0.0072(9) -0.0007(9) -0.0117(9) C5 0.0329(11) 0.0224(10) 0.0226(10) -0.0071(8) -0.0026(9) -0.0032(8) C6 0.0232(10) 0.0238(9) 0.0196(10) -0.0091(8) -0.0041(8) -0.0015(8) C7 0.0226(9) 0.0180(9) 0.0202(9) -0.0069(8) -0.0045(8) -0.0007(7) C7A 0.0274(11) 0.0227(10) 0.0300(11) -0.0053(9) -0.0024(9) 0.0051(8) O7 0.0286(8) 0.0240(7) 0.0372(9) -0.0111(7) -0.0093(7) 0.0032(6) N8 0.0175(8) 0.0216(8) 0.0193(8) -0.0091(7) -0.0023(6) -0.0002(6) O8 0.0582(15) 0.0808(18) 0.0827(18) 0.0094(14) -0.0196(13) -0.0152(13) N9 0.0170(8) 0.0190(7) 0.0200(8) -0.0069(6) -0.0011(6) 0.0005(6) O10 0.0193(7) 0.0210(7) 0.0249(7) -0.0066(6) -0.0037(6) 0.0047(5) C10 0.0185(9) 0.0197(9) 0.0205(9) -0.0101(8) -0.0048(7) -0.0003(7) C11 0.0187(9) 0.0219(9) 0.0207(9) -0.0089(8) -0.0059(7) 0.0000(7) C12 0.0273(10) 0.0234(10) 0.0282(11) -0.0097(9) -0.0044(8) 0.0003(8) C13 0.0358(12) 0.0253(11) 0.0297(12) -0.0031(9) -0.0022(9) -0.0055(9) C14 0.0282(11) 0.0393(12) 0.0257(11) -0.0105(10) 0.0049(9) -0.0116(9) C15 0.0230(10) 0.0335(11) 0.0261(11) -0.0144(9) -0.0005(8) -0.0018(8) N16 0.0233(8) 0.0212(8) 0.0284(9) -0.0098(7) 0.0008(7) 0.0033(7) C16 0.0203(9) 0.0232(9) 0.0219(10) -0.0102(8) -0.0060(8) -0.0012(7) C17 0.0203(9) 0.0294(10) 0.0180(9) -0.0097(8) -0.0016(8) -0.0023(8) C17A 0.0196(10) 0.0441(13) 0.0336(12) -0.0208(11) -0.0043(9) -0.0015(9) N17 0.0420(12) 0.0782(17) 0.0438(13) -0.0329(13) -0.0094(10) 0.0000(11) N18 0.0203(8) 0.0251(8) 0.0200(8) -0.0097(7) -0.0035(6) 0.0012(7) N19 0.0197(8) 0.0251(8) 0.0245(9) -0.0131(7) -0.0041(7) 0.0040(7) O20 0.0213(7) 0.0302(7) 0.0334(8) -0.0166(7) -0.0101(6) 0.0036(6) C20 0.0223(10) 0.0267(10) 0.0186(10) -0.0093(8) -0.0025(8) 0.0010(8) C21 0.0269(10) 0.0257(10) 0.0182(10) -0.0089(8) -0.0009(8) 0.0006(8) C22 0.0290(11) 0.0329(11) 0.0283(11) -0.0140(10) 0.0002(9) -0.0026(9) C23 0.0462(14) 0.0300(11) 0.0358(13) -0.0138(10) 0.0014(11) -0.0123(10) C24 0.0491(14) 0.0213(10) 0.0316(12) -0.0078(9) 0.0033(10) -0.0023(10) C25 0.0360(12) 0.0280(11) 0.0271(11) -0.0058(9) -0.0017(9) 0.0078(9) N26 0.0291(10) 0.0345(10) 0.0506(12) -0.0187(10) -0.0139(9) 0.0093(8) C26 0.0278(10) 0.0281(10) 0.0193(10) -0.0062(9) -0.0009(8) 0.0015(8) N1' 0.0209(8) 0.0241(8) 0.0246(9) -0.0110(7) -0.0041(7) -0.0032(7) C2' 0.0211(10) 0.0306(10) 0.0252(10) -0.0114(9) -0.0066(8) -0.0026(8) C3' 0.0243(11) 0.0414(13) 0.0349(12) -0.0072(10) -0.0086(9) -0.0075(9) C4' 0.0346(12) 0.0372(12) 0.0390(13) -0.0038(11) -0.0084(10) -0.0173(10) C5' 0.0348(12) 0.0265(11) 0.0339(12) -0.0059(9) -0.0116(10) -0.0084(9) C6' 0.0256(10) 0.0249(10) 0.0232(10) -0.0107(8) -0.0056(8) -0.0027(8) C7' 0.0235(9) 0.0203(9) 0.0196(9) -0.0068(8) -0.0038(8) -0.0018(8) C7B 0.0317(11) 0.0211(10) 0.0306(11) -0.0119(9) -0.0086(9) 0.0019(8) N8' 0.0180(8) 0.0205(8) 0.0206(8) -0.0085(7) -0.0035(6) 0.0001(6) N9' 0.0171(7) 0.0214(8) 0.0238(8) -0.0104(7) -0.0071(6) 0.0024(6) O10' 0.0197(7) 0.0228(7) 0.0334(8) -0.0163(6) -0.0101(6) 0.0065(5) C10' 0.0182(9) 0.0207(9) 0.0177(9) -0.0076(8) -0.0030(7) 0.0019(7) C11' 0.0177(9) 0.0244(10) 0.0218(10) -0.0102(8) -0.0034(7) 0.0003(7) C12' 0.0275(11) 0.0292(11) 0.0380(12) -0.0186(10) -0.0115(9) 0.0037(9) C13' 0.0348(12) 0.0384(12) 0.0492(14) -0.0272(12) -0.0176(11) 0.0016(10) C14' 0.0261(11) 0.0417(13) 0.0393(13) -0.0177(11) -0.0140(9) -0.0022(9) C15' 0.0211(10) 0.0298(11) 0.0315(11) -0.0109(9) -0.0084(8) 0.0038(8) C16' 0.0205(9) 0.0233(9) 0.0241(10) -0.0081(8) -0.0057(8) 0.0010(8) N16' 0.0259(9) 0.0282(9) 0.0638(13) -0.0257(10) -0.0230(9) 0.0116(8) C17' 0.0190(9) 0.0302(10) 0.0276(11) -0.0132(9) -0.0073(8) -0.0011(8) C17B 0.0206(10) 0.0389(12) 0.0322(12) -0.0139(10) -0.0050(9) 0.0008(9) N18' 0.0201(8) 0.0263(8) 0.0243(9) -0.0101(7) -0.0082(7) -0.0007(7) N19' 0.0201(8) 0.0242(8) 0.0254(9) -0.0091(7) -0.0085(7) 0.0032(7) O20' 0.0218(7) 0.0305(8) 0.0276(8) -0.0094(6) -0.0055(6) 0.0055(6) C20' 0.0215(10) 0.0296(10) 0.0222(10) -0.0117(9) -0.0095(8) 0.0013(8) C21' 0.0235(10) 0.0296(10) 0.0247(10) -0.0091(9) -0.0101(8) 0.0006(8) C22' 0.0281(11) 0.0361(12) 0.0346(12) -0.0105(10) -0.0093(9) -0.0027(9) C23' 0.0379(13) 0.0416(13) 0.0344(13) -0.0030(11) -0.0042(10) -0.0118(11) C24' 0.0589(17) 0.0319(13) 0.0378(14) 0.0004(11) -0.0118(12) -0.0047(12) C25' 0.0473(15) 0.0312(12) 0.0412(14) -0.0037(11) -0.0098(12) 0.0093(11) N26' 0.0330(11) 0.0385(12) 0.0517(14) 0.0005(10) 0.0020(10) 0.0153(9) C26' 0.0324(12) 0.0340(12) 0.0310(12) -0.0068(10) -0.0079(9) 0.0052(10) N50 0.0346(10) 0.0238(9) 0.0313(10) -0.0109(8) -0.0109(8) 0.0059(7) C51 0.0245(10) 0.0278(11) 0.0265(11) -0.0072(9) -0.0046(8) 0.0036(8) C52 0.0584(16) 0.0297(12) 0.0406(14) -0.0176(11) -0.0197(12) 0.0134(11) C53 0.0514(16) 0.0370(13) 0.080(2) -0.0285(14) -0.0404(15) 0.0132(12) C54 0.0383(16) 0.101(3) 0.0473(18) -0.0126(19) -0.0122(14) 0.0131(17) C55 0.077(2) 0.076(2) 0.0493(17) -0.0338(17) 0.0042(15) -0.0235(17) C56 0.0547(19) 0.132(3) 0.091(3) -0.083(3) -0.0187(18) 0.0029(19) _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 N18 2.0485(16) . ? Zn1 O20 1.9765(14) . ? Zn1 N1' 2.4831(16) . ? Zn1 N18' 2.0161(16) . ? Zn1 O20' 2.0259(14) . ? Zn2 N1 2.3373(16) . ? Zn2 N8 2.0403(15) . ? Zn2 O10 2.0651(14) . ? Zn2 N8' 2.0458(15) . ? Zn2 O10' 2.0266(13) . ? N1 C2 1.344(2) . ? N1 C6 1.350(2) . ? C2 C3 1.385(3) . ? C2 C17 1.487(3) . ? C3 C4 1.388(3) . ? C3 H3 0.9500 . ? C4 C5 1.380(3) . ? C4 H4 0.9500 . ? C5 C6 1.391(3) . ? C5 H5 0.9500 . ? C6 C7 1.476(3) . ? C7 N8 1.292(2) . ? C7 C7A 1.493(3) . ? C7A H7A 0.9800 . ? C7A H7B 0.9800 . ? C7A H7C 0.9800 . ? O7 C51 1.234(2) . ? N8 N9 1.374(2) . ? O8 C54 1.211(4) . ? N9 C10 1.342(2) . ? O10 C10 1.279(2) . ? C10 C11 1.482(3) . ? C11 C12 1.401(3) . ? C11 C16 1.425(3) . ? C12 C13 1.379(3) . ? C12 H12 0.9500 . ? C13 C14 1.399(3) . ? C13 H13 0.9500 . ? C14 C15 1.366(3) . ? C14 H14 0.9500 . ? C15 C16 1.410(3) . ? C15 H15 0.9500 . ? N16 C16 1.361(2) . ? N16 H16A 0.8800 . ? N16 H16B 0.8800 . ? C17 N18 1.291(3) . ? C17 C17A 1.492(3) . ? C17A H17A 0.9800 . ? C17A H17B 0.9800 . ? C17A H17C 0.9800 . ? N17 C54 1.326(4) . ? N17 C55 1.444(3) . ? N17 C56 1.447(4) . ? N18 N19 1.394(2) . ? N19 C20 1.324(3) . ? O20 C20 1.300(2) . ? C20 C21 1.479(3) . ? C21 C22 1.404(3) . ? C21 C26 1.419(3) . ? C22 C23 1.371(3) . ? C22 H22 0.9500 . ? C23 C24 1.388(3) . ? C23 H23 0.9500 . ? C24 C25 1.365(3) . ? C24 H24 0.9500 . ? C25 C26 1.412(3) . ? C25 H25 0.9500 . ? N26 C26 1.361(3) . ? N26 H26A 0.8800 . ? N26 H26B 0.8800 . ? N1' C6' 1.348(2) . ? N1' C2' 1.354(2) . ? C2' C3' 1.383(3) . ? C2' C17' 1.477(3) . ? C3' C4' 1.378(3) . ? C3' H3' 0.9500 . ? C4' C5' 1.382(3) . ? C4' H4' 0.9500 . ? C5' C6' 1.391(3) . ? C5' H5' 0.9500 . ? C6' C7' 1.478(3) . ? C7' N8' 1.288(2) . ? C7' C7B 1.499(3) . ? C7B H7D 0.9800 . ? C7B HFE 0.9800 . ? C7B H7F 0.9800 . ? N8' N9' 1.373(2) . ? N9' C10' 1.339(2) . ? O10' C10' 1.293(2) . ? C10' C11' 1.474(3) . ? C11' C12' 1.405(3) . ? C11' C16' 1.425(3) . ? C12' C13' 1.369(3) . ? C12' H12' 0.9500 . ? C13' C14' 1.395(3) . ? C13' H13' 0.9500 . ? C14' C15' 1.372(3) . ? C14' H14' 0.9500 . ? C15' C16' 1.404(3) . ? C15' H15' 0.9500 . ? C16' N16' 1.359(3) . ? N16' H16C 0.8800 . ? N16' H16D 0.8800 . ? C17' N18' 1.286(3) . ? C17' C17B 1.502(3) . ? C17B H17D 0.9800 . ? C17B H17E 0.9800 . ? C17B H17F 0.9800 . ? N18' N19' 1.379(2) . ? N19' C20' 1.333(3) . ? O20' C20' 1.287(2) . ? C20' C21' 1.483(3) . ? C21' C22' 1.395(3) . ? C21' C26' 1.423(3) . ? C22' C23' 1.384(3) . ? C22' H22' 0.9500 . ? C23' C24' 1.388(3) . ? C23' H23' 0.9500 . ? C24' C25' 1.372(4) . ? C24' H24' 0.9500 . ? C25' C26' 1.401(3) . ? C25' H25' 0.9500 . ? N26' C26' 1.366(3) . ? N26' H26C 0.8800 . ? N26' H26D 0.8800 . ? N50 C51 1.319(3) . ? N50 C52 1.451(3) . ? N50 C53 1.454(3) . ? C51 H51 0.9500 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54 0.9500 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? 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 O20 Zn1 N18' 128.41(6) . . ? O20 Zn1 O20' 117.97(6) . . ? N18' Zn1 O20' 78.48(6) . . ? O20 Zn1 N18 79.19(6) . . ? N18' Zn1 N18 149.32(6) . . ? O20' Zn1 N18 101.47(6) . . ? O20 Zn1 N1' 87.96(6) . . ? N18' Zn1 N1' 71.10(6) . . ? O20' Zn1 N1' 148.56(5) . . ? N18 Zn1 N1' 100.66(6) . . ? O10' Zn2 N8 116.59(6) . . ? O10' Zn2 N8' 78.00(6) . . ? N8 Zn2 N8' 165.34(6) . . ? O10' Zn2 O10 109.54(6) . . ? N8 Zn2 O10 76.73(6) . . ? N8' Zn2 O10 97.70(6) . . ? O10' Zn2 N1 88.51(6) . . ? N8 Zn2 N1 73.31(6) . . ? N8' Zn2 N1 110.15(6) . . ? O10 Zn2 N1 149.62(5) . . ? C2 N1 C6 118.48(17) . . ? C2 N1 Zn2 126.29(12) . . ? C6 N1 Zn2 109.23(12) . . ? N1 C2 C3 122.48(18) . . ? N1 C2 C17 116.01(17) . . ? C3 C2 C17 121.32(17) . . ? C2 C3 C4 118.69(19) . . ? C2 C3 H3 120.7 . . ? C4 C3 H3 120.7 . . ? C5 C4 C3 119.09(19) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? C4 C5 C6 119.15(18) . . ? C4 C5 H5 120.4 . . ? C6 C5 H5 120.4 . . ? N1 C6 C5 121.80(18) . . ? N1 C6 C7 116.05(17) . . ? C5 C6 C7 122.06(17) . . ? N8 C7 C6 114.47(16) . . ? N8 C7 C7A 124.51(18) . . ? C6 C7 C7A 120.95(17) . . ? C7 C7A H7A 109.5 . . ? C7 C7A H7B 109.5 . . ? H7A C7A H7B 109.5 . . ? C7 C7A H7C 109.5 . . ? H7A C7A H7C 109.5 . . ? H7B C7A H7C 109.5 . . ? C7 N8 N9 119.41(15) . . ? C7 N8 Zn2 123.86(13) . . ? N9 N8 Zn2 116.73(11) . . ? C10 N9 N8 110.02(14) . . ? C10 O10 Zn2 112.00(12) . . ? O10 C10 N9 124.52(17) . . ? O10 C10 C11 118.09(16) . . ? N9 C10 C11 117.39(15) . . ? C12 C11 C16 118.72(18) . . ? C12 C11 C10 117.30(16) . . ? C16 C11 C10 123.98(17) . . ? C13 C12 C11 122.40(19) . . ? C13 C12 H12 118.8 . . ? C11 C12 H12 118.8 . . ? C12 C13 C14 118.4(2) . . ? C12 C13 H13 120.8 . . ? C14 C13 H13 120.8 . . ? C15 C14 C13 120.77(19) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C14 C15 C16 121.85(19) . . ? C14 C15 H15 119.1 . . ? C16 C15 H15 119.1 . . ? C16 N16 H16A 120.0 . . ? C16 N16 H16B 120.0 . . ? H16A N16 H16B 120.0 . . ? N16 C16 C15 118.84(17) . . ? N16 C16 C11 123.40(17) . . ? C15 C16 C11 117.75(17) . . ? N18 C17 C2 114.36(17) . . ? N18 C17 C17A 124.97(18) . . ? C2 C17 C17A 120.65(17) . . ? C17 C17A H17A 109.5 . . ? C17 C17A H17B 109.5 . . ? H17A C17A H17B 109.5 . . ? C17 C17A H17C 109.5 . . ? H17A C17A H17C 109.5 . . ? H17B C17A H17C 109.5 . . ? C54 N17 C55 120.3(3) . . ? C54 N17 C56 122.7(3) . . ? C55 N17 C56 116.9(3) . . ? C17 N18 N19 117.85(16) . . ? C17 N18 Zn1 129.20(13) . . ? N19 N18 Zn1 112.92(12) . . ? C20 N19 N18 110.86(15) . . ? C20 O20 Zn1 112.01(12) . . ? O20 C20 N19 124.41(17) . . ? O20 C20 C21 117.75(18) . . ? N19 C20 C21 117.83(17) . . ? C22 C21 C26 118.46(18) . . ? C22 C21 C20 117.93(18) . . ? C26 C21 C20 123.60(19) . . ? C23 C22 C21 122.2(2) . . ? C23 C22 H22 118.9 . . ? C21 C22 H22 118.9 . . ? C22 C23 C24 119.2(2) . . ? C22 C23 H23 120.4 . . ? C24 C23 H23 120.4 . . ? C25 C24 C23 120.4(2) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C24 C25 C26 121.8(2) . . ? C24 C25 H25 119.1 . . ? C26 C25 H25 119.1 . . ? C26 N26 H26A 120.0 . . ? C26 N26 H26B 120.0 . . ? H26A N26 H26B 120.0 . . ? N26 C26 C25 118.81(19) . . ? N26 C26 C21 123.29(19) . . ? C25 C26 C21 117.9(2) . . ? C6' N1' C2' 118.81(17) . . ? C6' N1' Zn1 124.81(12) . . ? C2' N1' Zn1 103.89(12) . . ? N1' C2' C3' 121.55(19) . . ? N1' C2' C17' 114.96(17) . . ? C3' C2' C17' 123.44(18) . . ? C4' C3' C2' 119.2(2) . . ? C4' C3' H3' 120.4 . . ? C2' C3' H3' 120.4 . . ? C3' C4' C5' 119.6(2) . . ? C3' C4' H4' 120.2 . . ? C5' C4' H4' 120.2 . . ? C4' C5' C6' 118.5(2) . . ? C4' C5' H5' 120.8 . . ? C6' C5' H5' 120.8 . . ? N1' C6' C5' 122.01(18) . . ? N1' C6' C7' 115.76(17) . . ? C5' C6' C7' 121.85(18) . . ? N8' C7' C6' 113.71(16) . . ? N8' C7' C7B 123.77(18) . . ? C6' C7' C7B 122.33(17) . . ? C7' C7B H7D 109.5 . . ? C7' C7B HFE 109.5 . . ? H7D C7B HFE 109.5 . . ? C7' C7B H7F 109.5 . . ? H7D C7B H7F 109.5 . . ? HFE C7B H7F 109.5 . . ? C7' N8' N9' 117.84(15) . . ? C7' N8' Zn2 127.10(13) . . ? N9' N8' Zn2 114.91(11) . . ? C10' N9' N8' 110.78(14) . . ? C10' O10' Zn2 111.79(12) . . ? O10' C10' N9' 124.24(17) . . ? O10' C10' C11' 118.35(16) . . ? N9' C10' C11' 117.41(15) . . ? C12' C11' C16' 118.06(17) . . ? C12' C11' C10' 118.23(16) . . ? C16' C11' C10' 123.70(17) . . ? C13' C12' C11' 122.42(19) . . ? C13' C12' H12' 118.8 . . ? C11' C12' H12' 118.8 . . ? C12' C13' C14' 119.1(2) . . ? C12' C13' H13' 120.4 . . ? C14' C13' H13' 120.4 . . ? C15' C14' C13' 120.40(19) . . ? C15' C14' H14' 119.8 . . ? C13' C14' H14' 119.8 . . ? C14' C15' C16' 121.45(18) . . ? C14' C15' H15' 119.3 . . ? C16' C15' H15' 119.3 . . ? N16' C16' C15' 117.98(17) . . ? N16' C16' C11' 123.51(18) . . ? C15' C16' C11' 118.52(18) . . ? C16' N16' H16C 120.0 . . ? C16' N16' H16D 120.0 . . ? H16C N16' H16D 120.0 . . ? N18' C17' C2' 114.66(17) . . ? N18' C17' C17B 123.62(19) . . ? C2' C17' C17B 121.72(18) . . ? C17' C17B H17D 109.5 . . ? C17' C17B H17E 109.5 . . ? H17D C17B H17E 109.5 . . ? C17' C17B H17F 109.5 . . ? H17D C17B H17F 109.5 . . ? H17E C17B H17F 109.5 . . ? C17' N18' N19' 119.14(16) . . ? C17' N18' Zn1 126.00(14) . . ? N19' N18' Zn1 114.76(12) . . ? C20' N19' N18' 110.44(15) . . ? C20' O20' Zn1 110.56(12) . . ? O20' C20' N19' 124.64(18) . . ? O20' C20' C21' 118.17(18) . . ? N19' C20' C21' 117.17(16) . . ? C22' C21' C26' 118.2(2) . . ? C22' C21' C20' 117.49(18) . . ? C26' C21' C20' 124.33(19) . . ? C23' C22' C21' 122.9(2) . . ? C23' C22' H22' 118.5 . . ? C21' C22' H22' 118.5 . . ? C22' C23' C24' 118.2(2) . . ? C22' C23' H23' 120.9 . . ? C24' C23' H23' 120.9 . . ? C25' C24' C23' 120.7(2) . . ? C25' C24' H24' 119.7 . . ? C23' C24' H24' 119.7 . . ? C24' C25' C26' 121.9(2) . . ? C24' C25' H25' 119.1 . . ? C26' C25' H25' 119.1 . . ? C26' N26' H26C 120.0 . . ? C26' N26' H26D 120.0 . . ? H26C N26' H26D 120.0 . . ? N26' C26' C25' 119.5(2) . . ? N26' C26' C21' 122.3(2) . . ? C25' C26' C21' 118.2(2) . . ? C51 N50 C52 122.01(18) . . ? C51 N50 C53 121.25(18) . . ? C52 N50 C53 116.68(19) . . ? O7 C51 N50 125.62(19) . . ? O7 C51 H51 117.2 . . ? N50 C51 H51 117.2 . . ? N50 C52 H52A 109.5 . . ? N50 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? N50 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N50 C53 H53A 109.5 . . ? N50 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? N50 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? O8 C54 N17 126.5(3) . . ? O8 C54 H54 116.8 . . ? N17 C54 H54 116.8 . . ? N17 C55 H55A 109.5 . . ? N17 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? N17 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? N17 C56 H56A 109.5 . . ? N17 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? N17 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 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 O10' Zn2 N1 C2 -47.33(15) . . . . ? N8 Zn2 N1 C2 -165.71(16) . . . . ? N8' Zn2 N1 C2 29.31(16) . . . . ? O10 Zn2 N1 C2 -175.45(13) . . . . ? O10' Zn2 N1 C6 104.66(13) . . . . ? N8 Zn2 N1 C6 -13.72(12) . . . . ? N8' Zn2 N1 C6 -178.70(12) . . . . ? O10 Zn2 N1 C6 -23.47(19) . . . . ? C6 N1 C2 C3 -2.2(3) . . . . ? Zn2 N1 C2 C3 147.51(16) . . . . ? C6 N1 C2 C17 172.96(16) . . . . ? Zn2 N1 C2 C17 -37.3(2) . . . . ? N1 C2 C3 C4 5.5(3) . . . . ? C17 C2 C3 C4 -169.36(18) . . . . ? C2 C3 C4 C5 -3.8(3) . . . . ? C3 C4 C5 C6 -0.9(3) . . . . ? C2 N1 C6 C5 -2.8(3) . . . . ? Zn2 N1 C6 C5 -157.33(16) . . . . ? C2 N1 C6 C7 173.75(16) . . . . ? Zn2 N1 C6 C7 19.26(19) . . . . ? C4 C5 C6 N1 4.4(3) . . . . ? C4 C5 C6 C7 -172.00(18) . . . . ? N1 C6 C7 N8 -15.5(2) . . . . ? C5 C6 C7 N8 161.08(18) . . . . ? N1 C6 C7 C7A 167.58(18) . . . . ? C5 C6 C7 C7A -15.8(3) . . . . ? C6 C7 N8 N9 -177.90(15) . . . . ? C7A C7 N8 N9 -1.1(3) . . . . ? C6 C7 N8 Zn2 1.8(2) . . . . ? C7A C7 N8 Zn2 178.55(15) . . . . ? O10' Zn2 N8 C7 -73.16(16) . . . . ? N8' Zn2 N8 C7 112.4(3) . . . . ? O10 Zn2 N8 C7 -178.60(16) . . . . ? N1 Zn2 N8 C7 6.45(15) . . . . ? O10' Zn2 N8 N9 106.50(12) . . . . ? N8' Zn2 N8 N9 -67.9(3) . . . . ? O10 Zn2 N8 N9 1.07(12) . . . . ? N1 Zn2 N8 N9 -173.89(14) . . . . ? C7 N8 N9 C10 178.51(16) . . . . ? Zn2 N8 N9 C10 -1.17(19) . . . . ? O10' Zn2 O10 C10 -114.59(12) . . . . ? N8 Zn2 O10 C10 -0.74(12) . . . . ? N8' Zn2 O10 C10 165.47(12) . . . . ? N1 Zn2 O10 C10 8.85(19) . . . . ? Zn2 O10 C10 N9 0.4(2) . . . . ? Zn2 O10 C10 C11 -179.94(12) . . . . ? N8 N9 C10 O10 0.5(3) . . . . ? N8 N9 C10 C11 -179.18(15) . . . . ? O10 C10 C11 C12 13.6(3) . . . . ? N9 C10 C11 C12 -166.67(17) . . . . ? O10 C10 C11 C16 -165.85(17) . . . . ? N9 C10 C11 C16 13.9(3) . . . . ? C16 C11 C12 C13 1.1(3) . . . . ? C10 C11 C12 C13 -178.42(19) . . . . ? C11 C12 C13 C14 0.7(3) . . . . ? C12 C13 C14 C15 -0.5(3) . . . . ? C13 C14 C15 C16 -1.4(3) . . . . ? C14 C15 C16 N16 -175.91(19) . . . . ? C14 C15 C16 C11 3.1(3) . . . . ? C12 C11 C16 N16 176.09(18) . . . . ? C10 C11 C16 N16 -4.5(3) . . . . ? C12 C11 C16 C15 -2.9(3) . . . . ? C10 C11 C16 C15 176.56(18) . . . . ? N1 C2 C17 N18 -44.3(2) . . . . ? C3 C2 C17 N18 130.9(2) . . . . ? N1 C2 C17 C17A 137.24(19) . . . . ? C3 C2 C17 C17A -47.6(3) . . . . ? C2 C17 N18 N19 -179.01(15) . . . . ? C17A C17 N18 N19 -0.6(3) . . . . ? C2 C17 N18 Zn1 -1.4(3) . . . . ? C17A C17 N18 Zn1 177.06(14) . . . . ? O20 Zn1 N18 C17 -171.97(18) . . . . ? N18' Zn1 N18 C17 31.4(2) . . . . ? O20' Zn1 N18 C17 -55.32(18) . . . . ? N1' Zn1 N18 C17 102.20(17) . . . . ? O20 Zn1 N18 N19 5.77(12) . . . . ? N18' Zn1 N18 N19 -150.86(13) . . . . ? O20' Zn1 N18 N19 122.42(12) . . . . ? N1' Zn1 N18 N19 -80.06(12) . . . . ? C17 N18 N19 C20 174.40(17) . . . . ? Zn1 N18 N19 C20 -3.61(19) . . . . ? N18' Zn1 O20 C20 158.20(12) . . . . ? O20' Zn1 O20 C20 -104.18(13) . . . . ? N18 Zn1 O20 C20 -6.83(13) . . . . ? N1' Zn1 O20 C20 94.43(13) . . . . ? Zn1 O20 C20 N19 7.7(2) . . . . ? Zn1 O20 C20 C21 -171.04(13) . . . . ? N18 N19 C20 O20 -2.7(3) . . . . ? N18 N19 C20 C21 176.06(16) . . . . ? O20 C20 C21 C22 4.5(3) . . . . ? N19 C20 C21 C22 -174.34(18) . . . . ? O20 C20 C21 C26 -176.86(18) . . . . ? N19 C20 C21 C26 4.3(3) . . . . ? C26 C21 C22 C23 -0.6(3) . . . . ? C20 C21 C22 C23 178.15(19) . . . . ? C21 C22 C23 C24 0.2(3) . . . . ? C22 C23 C24 C25 -0.2(3) . . . . ? C23 C24 C25 C26 0.6(3) . . . . ? C24 C25 C26 N26 178.4(2) . . . . ? C24 C25 C26 C21 -1.0(3) . . . . ? C22 C21 C26 N26 -178.4(2) . . . . ? C20 C21 C26 N26 3.0(3) . . . . ? C22 C21 C26 C25 1.0(3) . . . . ? C20 C21 C26 C25 -177.70(19) . . . . ? O20 Zn1 N1' C6' -32.67(15) . . . . ? N18' Zn1 N1' C6' -164.68(16) . . . . ? O20' Zn1 N1' C6' -179.97(14) . . . . ? N18 Zn1 N1' C6' 45.94(16) . . . . ? O20 Zn1 N1' C2' 108.29(12) . . . . ? N18' Zn1 N1' C2' -23.73(12) . . . . ? O20' Zn1 N1' C2' -39.02(17) . . . . ? N18 Zn1 N1' C2' -173.11(12) . . . . ? C6' N1' C2' C3' -1.8(3) . . . . ? Zn1 N1' C2' C3' -145.64(18) . . . . ? C6' N1' C2' C17' 176.03(17) . . . . ? Zn1 N1' C2' C17' 32.21(18) . . . . ? N1' C2' C3' C4' 4.6(3) . . . . ? C17' C2' C3' C4' -173.0(2) . . . . ? C2' C3' C4' C5' -2.5(4) . . . . ? C3' C4' C5' C6' -2.2(3) . . . . ? C2' N1' C6' C5' -3.1(3) . . . . ? Zn1 N1' C6' C5' 132.60(17) . . . . ? C2' N1' C6' C7' 169.88(17) . . . . ? Zn1 N1' C6' C7' -54.4(2) . . . . ? C4' C5' C6' N1' 5.1(3) . . . . ? C4' C5' C6' C7' -167.5(2) . . . . ? N1' C6' C7' N8' -34.4(2) . . . . ? C5' C6' C7' N8' 138.6(2) . . . . ? N1' C6' C7' C7B 150.33(18) . . . . ? C5' C6' C7' C7B -36.6(3) . . . . ? C6' C7' N8' N9' -174.46(15) . . . . ? C7B C7' N8' N9' 0.7(3) . . . . ? C6' C7' N8' Zn2 0.8(2) . . . . ? C7B C7' N8' Zn2 175.95(14) . . . . ? O10' Zn2 N8' C7' -170.57(17) . . . . ? N8 Zn2 N8' C7' 4.4(4) . . . . ? O10 Zn2 N8' C7' -62.13(17) . . . . ? N1 Zn2 N8' C7' 105.53(17) . . . . ? O10' Zn2 N8' N9' 4.82(12) . . . . ? N8 Zn2 N8' N9' 179.7(2) . . . . ? O10 Zn2 N8' N9' 113.26(12) . . . . ? N1 Zn2 N8' N9' -79.08(13) . . . . ? C7' N8' N9' C10' 170.80(17) . . . . ? Zn2 N8' N9' C10' -5.04(19) . . . . ? N8 Zn2 O10' C10' 177.83(12) . . . . ? N8' Zn2 O10' C10' -3.61(12) . . . . ? O10 Zn2 O10' C10' -97.61(13) . . . . ? N1 Zn2 O10' C10' 107.36(13) . . . . ? Zn2 O10' C10' N9' 2.1(2) . . . . ? Zn2 O10' C10' C11' -178.32(13) . . . . ? N8' N9' C10' O10' 2.0(3) . . . . ? N8' N9' C10' C11' -177.61(15) . . . . ? O10' C10' C11' C12' -0.9(3) . . . . ? N9' C10' C11' C12' 178.74(18) . . . . ? O10' C10' C11' C16' -179.93(18) . . . . ? N9' C10' C11' C16' -0.3(3) . . . . ? C16' C11' C12' C13' -0.6(3) . . . . ? C10' C11' C12' C13' -179.7(2) . . . . ? C11' C12' C13' C14' -0.6(4) . . . . ? C12' C13' C14' C15' 0.9(4) . . . . ? C13' C14' C15' C16' -0.2(3) . . . . ? C14' C15' C16' N16' 178.9(2) . . . . ? C14' C15' C16' C11' -1.0(3) . . . . ? C12' C11' C16' N16' -178.5(2) . . . . ? C10' C11' C16' N16' 0.5(3) . . . . ? C12' C11' C16' C15' 1.3(3) . . . . ? C10' C11' C16' C15' -179.63(18) . . . . ? N1' C2' C17' N18' -26.5(3) . . . . ? C3' C2' C17' N18' 151.3(2) . . . . ? N1' C2' C17' C17B 153.13(18) . . . . ? C3' C2' C17' C17B -29.1(3) . . . . ? C2' C17' N18' N19' 176.85(15) . . . . ? C17B C17' N18' N19' -2.7(3) . . . . ? C2' C17' N18' Zn1 0.8(2) . . . . ? C17B C17' N18' Zn1 -178.83(14) . . . . ? O20 Zn1 N18' C17' -58.68(19) . . . . ? O20' Zn1 N18' C17' -175.38(17) . . . . ? N18 Zn1 N18' C17' 91.5(2) . . . . ? N1' Zn1 N18' C17' 12.69(16) . . . . ? O20 Zn1 N18' N19' 125.09(12) . . . . ? O20' Zn1 N18' N19' 8.39(12) . . . . ? N18 Zn1 N18' N19' -84.73(17) . . . . ? N1' Zn1 N18' N19' -163.54(14) . . . . ? C17' N18' N19' C20' 177.42(17) . . . . ? Zn1 N18' N19' C20' -6.06(19) . . . . ? O20 Zn1 O20' C20' -136.62(12) . . . . ? N18' Zn1 O20' C20' -9.05(13) . . . . ? N18 Zn1 O20' C20' 139.63(13) . . . . ? N1' Zn1 O20' C20' 5.70(19) . . . . ? Zn1 O20' C20' N19' 9.5(2) . . . . ? Zn1 O20' C20' C21' -168.81(13) . . . . ? N18' N19' C20' O20' -2.5(3) . . . . ? N18' N19' C20' C21' 175.79(15) . . . . ? O20' C20' C21' C22' 6.8(3) . . . . ? N19' C20' C21' C22' -171.65(18) . . . . ? O20' C20' C21' C26' -174.77(19) . . . . ? N19' C20' C21' C26' 6.8(3) . . . . ? C26' C21' C22' C23' -1.3(3) . . . . ? C20' C21' C22' C23' 177.2(2) . . . . ? C21' C22' C23' C24' 0.3(4) . . . . ? C22' C23' C24' C25' 1.4(4) . . . . ? C23' C24' C25' C26' -1.9(4) . . . . ? C24' C25' C26' N26' 179.5(2) . . . . ? C24' C25' C26' C21' 0.8(4) . . . . ? C22' C21' C26' N26' -177.9(2) . . . . ? C20' C21' C26' N26' 3.7(3) . . . . ? C22' C21' C26' C25' 0.8(3) . . . . ? C20' C21' C26' C25' -177.7(2) . . . . ? C52 N50 C51 O7 179.3(2) . . . . ? C53 N50 C51 O7 2.2(4) . . . . ? C55 N17 C54 O8 1.8(5) . . . . ? C56 N17 C54 O8 -174.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.38 _refine_diff_density_min -0.41 _refine_diff_density_rms 0.07 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.076 0.649 0.164 12.7 -0.2 2 0.500 0.500 0.500 194.5 16.8 3 0.924 0.351 0.836 12.7 -0.3 _platon_squeeze_details ; ? ; data_mnpyne _database_code_depnum_ccdc_archive 'CCDC 622115' _refine_special_details ; A region of diffuse solvent was modelled using PLATON SQUEEZE. The electron density (322 electrons per unit cell) was accounted for by eight DMSO per unit cell. Details below. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.250 -0.026 0.250 236.6 80.3 2 0.750 -0.016 0.250 236.6 80.3 3 0.250 -0.023 0.750 236.6 80.5 4 0.750 -0.031 0.750 236.6 80.5 _platon_squeeze_details ; ? ; _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C63 H55 Mn3 N21 O8, 2(C2 H6 O S)' _chemical_formula_sum 'C67 H67 Mn3 N21 O10 S2' _chemical_formula_weight 1555.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.393(4) _cell_length_b 9.3846(13) _cell_length_c 28.321(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.473(3) _cell_angle_gamma 90.00 _cell_volume 6656.9(17) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3659 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 26.2 _exptl_crystal_description 'rhombic tablet' _exptl_crystal_colour orange _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.552 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3212 _exptl_absorpt_coefficient_mu 0.701 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min . _exptl_absorpt_correction_T_max . _exptl_absorpt_process_details . _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 17465 _diffrn_reflns_av_R_equivalents 0.054 _diffrn_reflns_av_sigmaI/netI 0.098 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 27.51 _reflns_number_total 7520 _reflns_number_gt 4290 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART version 5.624 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36a (Bruker, 2001)' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'enCIFer (Allen et al., 2004); PLATON' _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^)+(0.041P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'Methyl and water H atoms from delta-F; others placed geometrically' _refine_ls_hydrogen_treatment 'Water H atoms with restraints; methyl H atoms as rigid rotor; riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7520 _refine_ls_number_parameters 439 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0886 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.0964 _refine_ls_wR_factor_gt 0.0893 _refine_ls_goodness_of_fit_ref 0.85 _refine_ls_restrained_S_all 0.85 _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 0.168810(16) 0.30837(4) 0.034695(15) 0.02445(12) Uani 1 1 d . . . O1W O 0.21828(7) 0.4065(2) -0.01346(7) 0.0267(4) Uani 1 1 d D . . H1W1 H 0.2491(6) 0.425(3) 0.0003(9) 0.040 Uiso 1 1 d D . . H1W2 H 0.2215(10) 0.354(3) -0.0367(7) 0.040 Uiso 1 1 d D . . N1 N 0.11571(8) 0.5108(2) 0.02384(8) 0.0258(5) Uani 1 1 d . . . C2 C 0.07459(11) 0.5164(3) -0.01298(10) 0.0283(7) Uani 1 1 d . . . C3 C 0.04433(11) 0.6402(3) -0.02262(11) 0.0349(7) Uani 1 1 d . . . H3 H 0.0149 0.6428 -0.0481 0.042 Uiso 1 1 calc R . . C4 C 0.05805(12) 0.7589(3) 0.00554(11) 0.0385(8) Uani 1 1 d . . . H4 H 0.0378 0.8441 -0.0003 0.046 Uiso 1 1 calc R . . C5 C 0.10106(11) 0.7539(3) 0.04202(11) 0.0341(7) Uani 1 1 d . . . H5 H 0.1110 0.8353 0.0614 0.041 Uiso 1 1 calc R . . C6 C 0.12973(10) 0.6273(3) 0.04994(10) 0.0262(6) Uani 1 1 d . . . C7 C 0.17850(11) 0.6112(3) 0.08650(10) 0.0289(7) Uani 1 1 d . . . C7A C 0.19994(13) 0.7354(3) 0.11685(12) 0.0478(9) Uani 1 1 d . . . H7AA H 0.1758 0.7575 0.1395 0.072 Uiso 1 1 calc R . . H7AB H 0.2027 0.8183 0.0964 0.072 Uiso 1 1 calc R . . H7AC H 0.2353 0.7117 0.1346 0.072 Uiso 1 1 calc R . . N8 N 0.19965(9) 0.4861(2) 0.08805(8) 0.0273(5) Uani 1 1 d . . . N9 N 0.24643(9) 0.4664(2) 0.12019(8) 0.0298(6) Uani 1 1 d . . . O10 O 0.24703(7) 0.24593(19) 0.08258(6) 0.0261(4) Uani 1 1 d . . . C10 C 0.26667(10) 0.3408(3) 0.11316(10) 0.0255(6) Uani 1 1 d . . . C11 C 0.31876(10) 0.3113(3) 0.14501(9) 0.0245(6) Uani 1 1 d . . . C12 C 0.34340(12) 0.4147(3) 0.17587(11) 0.0358(7) Uani 1 1 d . . . H12 H 0.3268 0.5045 0.1781 0.043 Uiso 1 1 calc R . . C13 C 0.39177(12) 0.3864(3) 0.20310(11) 0.0367(7) Uani 1 1 d . . . H13 H 0.4078 0.4592 0.2240 0.044 Uiso 1 1 calc R . . N14 N 0.41789(9) 0.2639(2) 0.20235(8) 0.0264(5) Uani 1 1 d . . . C15 C 0.39340(12) 0.1631(3) 0.17372(10) 0.0336(7) Uani 1 1 d . . . H15 H 0.4102 0.0727 0.1736 0.040 Uiso 1 1 calc R . . C16 C 0.34482(11) 0.1827(3) 0.14408(10) 0.0336(7) Uani 1 1 d . . . H16 H 0.3297 0.1085 0.1234 0.040 Uiso 1 1 calc R . . C17 C 0.06533(11) 0.3851(3) -0.04161(10) 0.0286(7) Uani 1 1 d . . . C17A C 0.02415(12) 0.3822(3) -0.08557(11) 0.0391(8) Uani 1 1 d . . . H17A H 0.0262 0.2913 -0.1022 0.059 Uiso 1 1 calc R . . H17B H 0.0305 0.4608 -0.1067 0.059 Uiso 1 1 calc R . . H17C H -0.0114 0.3924 -0.0767 0.059 Uiso 1 1 calc R . . N18 N 0.09727(9) 0.2822(2) -0.02661(8) 0.0257(5) Uani 1 1 d . . . N19 N 0.09174(9) 0.1553(2) -0.05234(8) 0.0291(6) Uani 1 1 d . . . O20 O 0.17349(7) 0.10219(19) -0.00500(7) 0.0296(5) Uani 1 1 d . . . C20 C 0.13399(11) 0.0727(3) -0.03797(10) 0.0269(7) Uani 1 1 d . . . C21 C 0.13318(11) -0.0662(3) -0.06339(10) 0.0280(7) Uani 1 1 d . . . C22 C 0.09563(12) -0.0966(3) -0.10375(10) 0.0361(8) Uani 1 1 d . . . H22 H 0.0697 -0.0277 -0.1163 0.043 Uiso 1 1 calc R . . C23 C 0.09666(13) -0.2280(3) -0.12520(11) 0.0438(8) Uani 1 1 d . . . H23 H 0.0710 -0.2464 -0.1529 0.053 Uiso 1 1 calc R . . N24 N 0.13134(12) -0.3312(3) -0.10959(10) 0.0497(7) Uani 1 1 d . . . C25 C 0.16727(13) -0.3001(3) -0.07113(12) 0.0433(8) Uani 1 1 d . . . H25 H 0.1925 -0.3716 -0.0592 0.052 Uiso 1 1 calc R . . C26 C 0.17026(12) -0.1713(3) -0.04759(11) 0.0346(7) Uani 1 1 d . . . H26 H 0.1974 -0.1547 -0.0208 0.042 Uiso 1 1 calc R . . Mn2 Mn 0.0000 -0.25125(6) 0.2500 0.02194(14) Uani 1 2 d S . . N1' N 0.0000 -0.4969(3) 0.2500 0.0238(7) Uani 1 2 d S . . C4' C 0.0000 -0.7893(4) 0.2500 0.0328(10) Uani 1 2 d S . . H4' H 0.0000 -0.8906 0.2500 0.039 Uiso 1 2 calc SR . . C5' C 0.02925(11) -0.7172(3) 0.22104(10) 0.0316(7) Uani 1 1 d . . . H5' H 0.0496 -0.7671 0.2011 0.038 Uiso 1 1 calc R . . C6' C 0.02829(10) -0.5678(3) 0.22165(9) 0.0247(6) Uani 1 1 d . . . C7' C 0.05652(11) -0.4770(3) 0.19152(10) 0.0288(7) Uani 1 1 d . . . C7A' C 0.09147(14) -0.5429(3) 0.15960(12) 0.0480(9) Uani 1 1 d . . . H7AD H 0.1079 -0.4675 0.1430 0.072 Uiso 1 1 calc R . . H7AE H 0.0699 -0.6045 0.1360 0.072 Uiso 1 1 calc R . . H7AF H 0.1195 -0.5996 0.1789 0.072 Uiso 1 1 calc R . . N8' N 0.04790(8) -0.3431(2) 0.19512(8) 0.0249(5) Uani 1 1 d . . . N9' N 0.07266(9) -0.2496(2) 0.16764(8) 0.0295(5) Uani 1 1 d . . . O10' O 0.02328(7) -0.07789(18) 0.20100(6) 0.0294(5) Uani 1 1 d . . . C10' C 0.05536(10) -0.1187(3) 0.17412(9) 0.0237(6) Uani 1 1 d . . . C11' C 0.07832(11) -0.0100(3) 0.14428(10) 0.0248(6) Uani 1 1 d . . . C12' C 0.12953(12) 0.0411(3) 0.15828(10) 0.0350(7) Uani 1 1 d . . . H12' H 0.1500 0.0120 0.1879 0.042 Uiso 1 1 calc R . . C13' C 0.15076(12) 0.1351(3) 0.12875(11) 0.0365(7) Uani 1 1 d . . . H13' H 0.1859 0.1695 0.1391 0.044 Uiso 1 1 calc R . . N14' N 0.12483(9) 0.1802(2) 0.08660(8) 0.0262(5) Uani 1 1 d . . . C15' C 0.07533(11) 0.1321(3) 0.07396(10) 0.0320(7) Uani 1 1 d . . . H15' H 0.0557 0.1637 0.0443 0.038 Uiso 1 1 calc R . . C16' C 0.05035(11) 0.0387(3) 0.10109(10) 0.0302(7) Uani 1 1 d . . . H16' H 0.0147 0.0086 0.0903 0.036 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0214(2) 0.0240(2) 0.0286(3) 0.00164(18) 0.00590(17) 0.00217(19) O1W 0.0240(11) 0.0276(12) 0.0295(12) -0.0019(8) 0.0073(9) 0.0014(9) N1 0.0222(12) 0.0262(14) 0.0307(14) 0.0018(10) 0.0093(11) 0.0021(10) C2 0.0269(16) 0.0271(16) 0.0325(17) 0.0046(13) 0.0096(13) 0.0038(13) C3 0.0291(16) 0.0339(18) 0.0406(19) 0.0078(14) 0.0026(14) 0.0094(14) C4 0.0331(18) 0.0357(18) 0.047(2) 0.0045(16) 0.0073(15) 0.0113(15) C5 0.0333(17) 0.0281(16) 0.0425(19) 0.0010(14) 0.0115(14) 0.0060(14) C6 0.0232(15) 0.0255(16) 0.0321(17) 0.0033(13) 0.0105(13) 0.0025(13) C7 0.0261(16) 0.0273(17) 0.0349(18) -0.0037(13) 0.0092(13) 0.0046(13) C7A 0.0397(19) 0.038(2) 0.063(2) -0.0197(17) -0.0019(17) 0.0083(16) N8 0.0221(13) 0.0295(14) 0.0308(14) 0.0012(10) 0.0060(10) 0.0027(10) N9 0.0260(13) 0.0270(14) 0.0349(15) -0.0023(11) 0.0003(11) 0.0050(11) O10 0.0238(10) 0.0270(10) 0.0272(11) -0.0037(9) 0.0037(8) 0.0024(8) C10 0.0264(15) 0.0241(16) 0.0274(16) 0.0013(12) 0.0087(12) -0.0017(12) C11 0.0268(15) 0.0234(15) 0.0244(15) 0.0024(12) 0.0073(12) 0.0020(13) C12 0.0348(18) 0.0258(17) 0.044(2) -0.0048(14) -0.0007(15) 0.0060(13) C13 0.0412(19) 0.0275(17) 0.0384(19) -0.0039(14) -0.0026(15) -0.0037(15) N14 0.0264(13) 0.0228(13) 0.0299(14) 0.0026(10) 0.0043(10) 0.0026(10) C15 0.0359(17) 0.0303(18) 0.0339(18) -0.0010(13) 0.0034(14) 0.0111(14) C16 0.0326(17) 0.0311(17) 0.0345(18) -0.0111(13) -0.0018(14) 0.0011(14) C17 0.0234(15) 0.0315(17) 0.0324(17) 0.0042(13) 0.0086(13) 0.0024(13) C17A 0.0370(18) 0.0376(19) 0.0401(19) 0.0002(15) -0.0010(15) 0.0023(15) N18 0.0251(12) 0.0247(14) 0.0282(13) 0.0029(10) 0.0066(10) -0.0007(10) N19 0.0315(14) 0.0235(14) 0.0322(14) -0.0009(10) 0.0044(11) 0.0011(11) O20 0.0230(11) 0.0291(11) 0.0362(12) -0.0035(9) 0.0033(9) 0.0017(9) C20 0.0272(16) 0.0258(16) 0.0301(17) 0.0024(12) 0.0116(13) -0.0026(13) C21 0.0268(16) 0.0257(16) 0.0339(18) -0.0008(13) 0.0119(13) -0.0044(13) C22 0.0373(19) 0.0347(19) 0.0350(19) -0.0002(14) 0.0019(15) -0.0015(14) C23 0.051(2) 0.038(2) 0.040(2) -0.0051(15) 0.0004(16) -0.0048(16) N24 0.0608(19) 0.0314(16) 0.056(2) -0.0103(14) 0.0067(16) 0.0021(14) C25 0.049(2) 0.0291(18) 0.052(2) 0.0000(16) 0.0096(17) 0.0042(16) C26 0.0371(18) 0.0282(18) 0.0391(19) 0.0007(14) 0.0082(14) -0.0003(14) Mn2 0.0226(3) 0.0187(3) 0.0250(3) 0.000 0.0051(2) 0.000 N1' 0.0292(18) 0.0164(17) 0.0267(19) 0.000 0.0074(15) 0.000 C4' 0.039(3) 0.018(2) 0.042(3) 0.000 0.007(2) 0.000 C5' 0.0372(17) 0.0255(18) 0.0333(17) -0.0048(12) 0.0093(14) 0.0010(13) C6' 0.0248(15) 0.0222(15) 0.0263(16) -0.0001(12) 0.0020(12) 0.0018(12) C7' 0.0336(17) 0.0221(16) 0.0322(17) -0.0043(12) 0.0098(13) 0.0003(13) C7A' 0.067(2) 0.0281(18) 0.058(2) 0.0058(15) 0.0380(19) 0.0097(16) N8' 0.0254(13) 0.0223(13) 0.0270(13) -0.0016(10) 0.0044(10) 0.0000(10) N9' 0.0353(14) 0.0216(12) 0.0338(14) 0.0031(11) 0.0123(11) -0.0006(11) O10' 0.0349(12) 0.0211(11) 0.0354(12) 0.0023(8) 0.0159(9) 0.0032(8) C10' 0.0237(15) 0.0246(16) 0.0218(15) 0.0011(12) 0.0011(12) -0.0005(12) C11' 0.0282(16) 0.0201(15) 0.0287(16) -0.0043(12) 0.0118(12) 0.0043(12) C12' 0.0352(18) 0.0392(19) 0.0303(18) 0.0067(14) 0.0045(14) -0.0019(14) C13' 0.0326(17) 0.0351(18) 0.042(2) 0.0012(15) 0.0061(15) -0.0082(14) N14' 0.0251(13) 0.0254(13) 0.0298(14) 0.0007(11) 0.0094(10) -0.0007(11) C15' 0.0283(17) 0.0330(17) 0.0352(18) 0.0112(13) 0.0067(13) 0.0039(13) C16' 0.0224(15) 0.0311(16) 0.0378(18) 0.0053(13) 0.0064(13) 0.0020(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 O1W 2.2023(19) . ? Mn1 O10 2.2892(18) . ? Mn1 O20 2.2507(18) . ? Mn1 N1 2.321(2) . ? Mn1 N8 2.300(2) . ? Mn1 N18 2.310(2) . ? Mn1 N14' 2.323(2) . ? O1W H1W1 0.83(3) . ? O1W H1W2 0.84(3) . ? N1 C6 1.334(3) . ? N1 C2 1.350(3) . ? C2 C3 1.395(4) . ? C2 C17 1.472(4) . ? C3 C4 1.381(4) . ? C3 H3 0.9500 . ? C4 C5 1.375(4) . ? C4 H4 0.9500 . ? C5 C6 1.393(4) . ? C5 H5 0.9500 . ? C6 C7 1.485(4) . ? C7 N8 1.289(3) . ? C7 C7A 1.497(4) . ? C7A H7AA 0.9800 . ? C7A H7AB 0.9800 . ? C7A H7AC 0.9800 . ? N8 N9 1.385(3) . ? N9 C10 1.314(3) . ? O10 C10 1.284(3) . ? C10 C11 1.499(4) . ? C11 C16 1.379(4) . ? C11 C12 1.384(4) . ? C12 C13 1.364(4) . ? C12 H12 0.9500 . ? C13 N14 1.330(3) . ? C13 H13 0.9500 . ? N14 C15 1.331(3) . ? N14 Mn2 2.294(2) 3 ? C15 C16 1.385(4) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 N18 1.288(3) . ? C17 C17A 1.488(4) . ? C17A H17A 0.9800 . ? C17A H17B 0.9800 . ? C17A H17C 0.9800 . ? N18 N19 1.391(3) . ? N19 C20 1.332(3) . ? O20 C20 1.283(3) . ? C20 C21 1.488(4) . ? C21 C26 1.386(4) . ? C21 C22 1.392(4) . ? C22 C23 1.376(4) . ? C22 H22 0.9500 . ? C23 N24 1.335(4) . ? C23 H23 0.9500 . ? N24 C25 1.333(4) . ? C25 C26 1.376(4) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? Mn2 O10' 2.2786(18) 2 ? Mn2 O10' 2.2786(18) . ? Mn2 N8' 2.293(2) . ? Mn2 N8' 2.293(2) 2 ? Mn2 N14 2.294(2) 4_545 ? Mn2 N14 2.294(2) 3_445 ? Mn2 N1' 2.305(3) . ? N1' C6' 1.339(3) . ? N1' C6' 1.339(3) 2 ? C4' C5' 1.372(3) . ? C4' C5' 1.372(3) 2 ? C4' H4' 0.9500 . ? C5' C6' 1.402(4) . ? C5' H5' 0.9500 . ? C6' C7' 1.473(4) . ? C7' N8' 1.282(3) . ? C7' C7A' 1.500(4) . ? C7A' H7AD 0.9800 . ? C7A' H7AE 0.9800 . ? C7A' H7AF 0.9800 . ? N8' N9' 1.390(3) . ? N9' C10' 1.327(3) . ? O10' C10' 1.263(3) . ? C10' C11' 1.502(4) . ? C11' C12' 1.381(4) . ? C11' C16' 1.387(4) . ? C12' C13' 1.384(4) . ? C12' H12' 0.9500 . ? C13' N14' 1.334(3) . ? C13' H13' 0.9500 . ? N14' C15' 1.328(3) . ? C15' C16' 1.386(4) . ? C15' H15' 0.9500 . ? C16' H16' 0.9500 . ? 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 O1W Mn1 O20 88.17(7) . . ? O1W Mn1 O10 86.92(7) . . ? O20 Mn1 O10 87.93(7) . . ? O1W Mn1 N8 86.35(7) . . ? O20 Mn1 N8 155.70(7) . . ? O10 Mn1 N8 68.15(7) . . ? O1W Mn1 N18 92.13(7) . . ? O20 Mn1 N18 68.46(7) . . ? O10 Mn1 N18 156.39(7) . . ? N8 Mn1 N18 135.37(8) . . ? O1W Mn1 N1 87.34(7) . . ? O20 Mn1 N1 135.64(7) . . ? O10 Mn1 N1 135.77(7) . . ? N8 Mn1 N1 67.73(8) . . ? N18 Mn1 N1 67.64(8) . . ? O1W Mn1 N14' 172.37(7) . . ? O20 Mn1 N14' 86.64(7) . . ? O10 Mn1 N14' 87.32(7) . . ? N8 Mn1 N14' 96.13(8) . . ? N18 Mn1 N14' 91.15(8) . . ? N1 Mn1 N14' 100.27(8) . . ? Mn1 O1W H1W1 113(2) . . ? Mn1 O1W H1W2 112(2) . . ? H1W1 O1W H1W2 106(2) . . ? C6 N1 C2 119.9(2) . . ? C6 N1 Mn1 120.05(17) . . ? C2 N1 Mn1 119.51(17) . . ? N1 C2 C3 121.0(3) . . ? N1 C2 C17 115.2(2) . . ? C3 C2 C17 123.8(3) . . ? C4 C3 C2 118.7(3) . . ? C4 C3 H3 120.6 . . ? C2 C3 H3 120.6 . . ? C5 C4 C3 120.0(3) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 118.7(3) . . ? C4 C5 H5 120.7 . . ? C6 C5 H5 120.7 . . ? N1 C6 C5 121.7(3) . . ? N1 C6 C7 114.8(2) . . ? C5 C6 C7 123.6(3) . . ? N8 C7 C6 114.3(2) . . ? N8 C7 C7A 125.4(3) . . ? C6 C7 C7A 120.3(2) . . ? C7 C7A H7AA 109.5 . . ? C7 C7A H7AB 109.5 . . ? H7AA C7A H7AB 109.5 . . ? C7 C7A H7AC 109.5 . . ? H7AA C7A H7AC 109.5 . . ? H7AB C7A H7AC 109.5 . . ? C7 N8 N9 116.8(2) . . ? C7 N8 Mn1 122.90(18) . . ? N9 N8 Mn1 119.85(16) . . ? C10 N9 N8 109.6(2) . . ? C10 O10 Mn1 115.15(16) . . ? O10 C10 N9 127.3(2) . . ? O10 C10 C11 119.0(2) . . ? N9 C10 C11 113.7(2) . . ? C16 C11 C12 117.2(2) . . ? C16 C11 C10 121.9(2) . . ? C12 C11 C10 120.9(2) . . ? C13 C12 C11 119.5(3) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? N14 C13 C12 124.3(3) . . ? N14 C13 H13 117.8 . . ? C12 C13 H13 117.8 . . ? C13 N14 C15 116.1(2) . . ? C13 N14 Mn2 116.85(18) . 3 ? C15 N14 Mn2 127.05(18) . 3 ? N14 C15 C16 123.7(3) . . ? N14 C15 H15 118.1 . . ? C16 C15 H15 118.1 . . ? C11 C16 C15 119.1(3) . . ? C11 C16 H16 120.4 . . ? C15 C16 H16 120.4 . . ? N18 C17 C2 114.3(2) . . ? N18 C17 C17A 125.4(3) . . ? C2 C17 C17A 120.2(2) . . ? C17 C17A H17A 109.5 . . ? C17 C17A H17B 109.5 . . ? H17A C17A H17B 109.5 . . ? C17 C17A H17C 109.5 . . ? H17A C17A H17C 109.5 . . ? H17B C17A H17C 109.5 . . ? C17 N18 N19 117.8(2) . . ? C17 N18 Mn1 122.88(18) . . ? N19 N18 Mn1 118.93(15) . . ? C20 N19 N18 109.3(2) . . ? C20 O20 Mn1 116.72(16) . . ? O20 C20 N19 126.2(2) . . ? O20 C20 C21 119.2(2) . . ? N19 C20 C21 114.6(2) . . ? C26 C21 C22 117.1(3) . . ? C26 C21 C20 120.9(3) . . ? C22 C21 C20 122.0(3) . . ? C23 C22 C21 119.1(3) . . ? C23 C22 H22 120.5 . . ? C21 C22 H22 120.5 . . ? N24 C23 C22 124.3(3) . . ? N24 C23 H23 117.8 . . ? C22 C23 H23 117.8 . . ? C25 N24 C23 115.9(3) . . ? N24 C25 C26 124.3(3) . . ? N24 C25 H25 117.8 . . ? C26 C25 H25 117.8 . . ? C25 C26 C21 119.2(3) . . ? C25 C26 H26 120.4 . . ? C21 C26 H26 120.4 . . ? O10' Mn2 O10' 88.87(9) 2 . ? O10' Mn2 N8' 154.25(7) 2 . ? O10' Mn2 N8' 68.65(7) . . ? O10' Mn2 N8' 68.65(7) 2 2 ? O10' Mn2 N8' 154.25(7) . 2 ? N8' Mn2 N8' 135.85(11) . 2 ? O10' Mn2 N14 84.22(7) 2 4_545 ? O10' Mn2 N14 90.70(7) . 4_545 ? N8' Mn2 N14 83.68(8) . 4_545 ? N8' Mn2 N14 99.01(8) 2 4_545 ? O10' Mn2 N14 90.70(7) 2 3_445 ? O10' Mn2 N14 84.22(7) . 3_445 ? N8' Mn2 N14 99.01(8) . 3_445 ? N8' Mn2 N14 83.68(8) 2 3_445 ? N14 Mn2 N14 172.90(11) 4_545 3_445 ? O10' Mn2 N1' 135.56(5) 2 . ? O10' Mn2 N1' 135.56(5) . . ? N8' Mn2 N1' 67.93(6) . . ? N8' Mn2 N1' 67.93(6) 2 . ? N14 Mn2 N1' 93.55(6) 4_545 . ? N14 Mn2 N1' 93.55(6) 3_445 . ? C6' N1' C6' 120.5(3) . 2 ? C6' N1' Mn2 119.77(16) . . ? C6' N1' Mn2 119.77(16) 2 . ? C5' C4' C5' 120.8(4) . 2 ? C5' C4' H4' 119.6 . . ? C5' C4' H4' 119.6 2 . ? C4' C5' C6' 118.3(3) . . ? C4' C5' H5' 120.8 . . ? C6' C5' H5' 120.8 . . ? N1' C6' C5' 121.1(3) . . ? N1' C6' C7' 114.9(2) . . ? C5' C6' C7' 124.1(2) . . ? N8' C7' C6' 114.5(2) . . ? N8' C7' C7A' 125.3(3) . . ? C6' C7' C7A' 120.2(2) . . ? C7' C7A' H7AD 109.5 . . ? C7' C7A' H7AE 109.5 . . ? H7AD C7A' H7AE 109.5 . . ? C7' C7A' H7AF 109.5 . . ? H7AD C7A' H7AF 109.5 . . ? H7AE C7A' H7AF 109.5 . . ? C7' N8' N9' 118.4(2) . . ? C7' N8' Mn2 122.59(18) . . ? N9' N8' Mn2 118.78(16) . . ? C10' N9' N8' 108.4(2) . . ? C10' O10' Mn2 114.10(16) . . ? O10' C10' N9' 128.7(2) . . ? O10' C10' C11' 118.8(2) . . ? N9' C10' C11' 112.5(2) . . ? C12' C11' C16' 117.4(3) . . ? C12' C11' C10' 120.6(2) . . ? C16' C11' C10' 122.0(2) . . ? C11' C12' C13' 119.3(3) . . ? C11' C12' H12' 120.3 . . ? C13' C12' H12' 120.3 . . ? N14' C13' C12' 124.0(3) . . ? N14' C13' H13' 118.0 . . ? C12' C13' H13' 118.0 . . ? C15' N14' C13' 116.0(2) . . ? C15' N14' Mn1 122.53(18) . . ? C13' N14' Mn1 120.86(18) . . ? N14' C15' C16' 124.4(3) . . ? N14' C15' H15' 117.8 . . ? C16' C15' H15' 117.8 . . ? C15' C16' C11' 118.9(3) . . ? C15' C16' H16' 120.6 . . ? C11' C16' H16' 120.6 . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.31 _refine_diff_density_min -0.29 _refine_diff_density_rms 0.07 #===END of CIF