# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1759 data_global _audit_creation_date ? _audit_creation_method 'CIFmaker on Quansan personal computer' _audit_update_record ? _publ_contact_author ; Prof. Corrado Rizzoli Universit\'a di Parma Dipartimento di Chimica Generale ed Inorganica, Chimica Analitica, Chimica Fisica Viale delle Scienze 17A I-43100 Parma Italy ; _publ_contact_author_phone '[039]521 905 449' _publ_contact_author_fax '[039]521 905 556' _publ_contact_author_email 'rizzoli@at@ipruniv.cce.unipr.it' _publ_section_title ; The Redox Chemistry of Dibenzotetramethyltetraaza[14]annulene-Mn(II): Functionalization of Manganese in a Macrocyclic Environment ; _jounal_name_full 'J. Chem. Soc., Dalton Transactions' ######## Please note: paper submitted ########### loop_ _publ_author_name _publ_author_address 'Federico Franceschi' ; Institut de Chemie Minerale et Analytique Universite de Lausanne BCH CH-1015 Lausanne Switzerland ; 'Joelle Hesschenbrouck' ; Institut de Chemie Minerale et Analytique Universite de Lausanne BCH CH-1015 Lausanne Switzerland ; 'Euro Solari' ; Institut de Chemie Minerale et Analytique Universite de Lausanne BCH CH-1015 Lausanne Switzerland ; 'Carlo Floriani(*)' ; Institut de Chemie Minerale et Analytique Universite de Lausanne BCH CH-1015 Lausanne Switzerland ; 'Nazzareno Re' ; Facolt\'a di Farmacia Universit\'a degli Studi "G. D'Annunzio" I-66013 Chieti Italy ; 'Corrado Rizzoli' ; Dipartimento di Chimica Generale ed Inorganica, Chimica Analitica, Chimica Fisica Viale delle Scienze 17A Universit\'a di Parma I-43100 Parma Italy ; 'Angiola Chiesi-Villa' ; Dipartimento di Chimica Generale ed Inorganica, Chimica Analitica, Chimica Fisica Universit\'a di Parma Viale delle Scienze 17A I-43100 Parma Italy ; _publ_section_references ; ; _publ_section_explt_prep ; North, A.C.T; Phillips, D.C; Mathews, F.S. (1968) Acta Cryst., A, Cryst. Phys., Diffr., Theor. Gen. Crystallogr., A24, 351-359 Otwinowski, Z., Minor, W. Processing of X-ray Diffraction Data Collected in Oscillation Mode, Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p. 307-326 (1997) Carter, C.W., Sweet, Jr. and R.M., Eds., Academic Press Sheldrick, G.M. (1976). SHELX76, Programs for the solution of crystal structures. Univ. of Cambridge, England Sheldrick, G.M. (1986). SHELX86, Programs for the solution of crystal structures. Univ. of Gottingen, Germany Sheldrick, G.M. (1993). SHELXL93, Program for the crystal structure refinement. Univ. of Gottingen, Germany TEXSAN - TEXRAY Structure Analysis Package, Molecular Structure Corporation (1985). ; _publ_section_explt_refinement ; ; ######################################################################## ###### #### Complex 3 Crystallographic Data data_COMPLEX_3 _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C29.5H29.5ClMnN5.5' _chemical_formula_weight 551.48 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Mn' 'Mn' -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 12.828(3) _cell_length_b 13.487(3) _cell_length_c 9.040(2) _cell_angle_alpha 92.49(2) _cell_angle_beta 105.25(2) _cell_angle_gamma 61.77(2) _cell_volume 1323.4(6) _cell_formula_units_Z 2.00 _cell_measurement_temperature 25 _cell_measurement_reflns_used 298 _cell_measurement_theta_min 32.4 _cell_measurement_theta_max 41.3 _exptl_crystal_description flattened_prism _exptl_crystal_colour red _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.3839 _exptl_crystal_density_method not_measured _exptl_crystal_F_000 574.0 _exptl_absorpt_coefficient_mu 5.2445 _exptl_absorpt_correction_type 'North et al. 1968' _exptl_absorpt_correction_T_min 0.684 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focussealedtube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku AFC6S' _diffrn_measurement_method 'omega/2theta' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2.7 _diffrn_reflns_number 5213 _diffrn_reflns_av_R_equivalents 0.0407 _diffrn_reflns_av_sigmaI/netI 0.1016 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.74 _diffrn_reflns_theta_max 70.25 _reflns_number_total 4973 _reflns_number_observed 2583 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'TEXSAN Software' _computing_cell_refinement 'TEXSAN Software' _computing_data_reduction 'TEXSAN Software' _computing_structure_solution 'SHELXS-76 (Sheldrick, 1976)' _computing_structure_refinement 'SHELXS-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 714 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses of fit S are based on F^2^, conventional R- factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R factor obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1255P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment not_refined _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4259 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1547 _refine_ls_R_factor_obs 0.0635 _refine_ls_wR_factor_all 0.2521 _refine_ls_wR_factor_obs 0.1744 _refine_ls_goodness_of_fit_all 1.022 _refine_ls_goodness_of_fit_obs 1.158 _refine_ls_restrained_S_all 1.189 _refine_ls_restrained_S_obs 1.158 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_aniso_ratio _atom_site_occupancy # # R=Rmax./Rmin.=ratio of the maximum and minimum # principal axes of atomic displacement ellipsoids # # Table of coordinates # -------------------- # # atom x/a y/b z/c Ueq tmf calc att R SOF MN1 0.33962(9) -0.10732(8) 0.0579(1) 0.0367(4) aniso . . 1.52 1.0000 CL1 0.3222(2) -0.2275(1) 0.2213(2) 0.0558(8) aniso . . 2.04 1.0000 N1 0.1721(4) 0.0194(4) -0.0058(5) 0.0427(19) aniso . . 1.46 1.0000 N2 0.3188(4) -0.1662(4) -0.1439(5) 0.0433(23) aniso . . 1.70 1.0000 N3 0.5141(4) -0.1938(4) 0.0633(5) 0.0388(23) aniso . . 1.44 1.0000 N4 0.3665(4) -0.0023(4) 0.2004(5) 0.0387(22) aniso . . 1.77 1.0000 N5 0.1756(9) -0.4070(7) -0.5126(9) 0.0987(57) aniso . . 1.95 1.0000 C1 -0.0113(7) 0.1716(7) -0.1885(8) 0.0646(35) aniso . . 2.17 1.0000 C2 0.1014(6) 0.0586(5) -0.1498(7) 0.0467(28) aniso . . 1.54 1.0000 C3 0.1345(6) -0.0033(6) -0.2727(7) 0.0510(31) aniso . . 2.15 1.0000 C4 0.2321(6) -0.1093(5) -0.2740(7) 0.0456(27) aniso . . 2.05 1.0000 C5 0.2430(7) -0.1544(7) -0.4273(7) 0.0611(36) aniso . . 2.34 1.0000 C6 0.4219(6) -0.2763(5) -0.1286(7) 0.0434(30) aniso . . 1.73 1.0000 C7 0.4187(7) -0.3674(6) -0.2033(7) 0.0535(35) aniso . . 2.21 1.0000 C8 0.5230(7) -0.4722(6) -0.1713(8) 0.0595(40) aniso . . 2.41 1.0000 C9 0.6300(7) -0.4884(6) -0.0629(9) 0.0615(37) aniso . . 2.43 1.0000 C10 0.6320(6) -0.3973(5) 0.0165(7) 0.0501(29) aniso . . 1.53 1.0000 C11 0.5304(6) -0.2916(5) -0.0158(7) 0.0441(30) aniso . . 2.21 1.0000 C12 0.7238(6) -0.2230(6) 0.0881(8) 0.0559(31) aniso . . 1.30 1.0000 C13 0.5991(5) -0.1611(5) 0.1180(6) 0.0403(25) aniso . . 1.58 1.0000 C14 0.5736(6) -0.0643(5) 0.2006(7) 0.0466(30) aniso . . 2.06 1.0000 C15 0.4680(6) 0.0093(5) 0.2398(6) 0.0401(29) aniso . . 2.23 1.0000 C16 0.4675(7) 0.1106(6) 0.3205(7) 0.0540(34) aniso . . 2.75 1.0000 C17 0.2553(6) 0.0665(4) 0.2381(6) 0.0412(25) aniso . . 1.91 1.0000 C18 0.2410(7) 0.1135(5) 0.3790(7) 0.0524(31) aniso . . 2.03 1.0000 C19 0.1277(8) 0.1702(6) 0.4055(8) 0.0619(42) aniso . . 3.11 1.0000 C20 0.0263(8) 0.1787(6) 0.2967(10) 0.0702(40) aniso . . 3.00 1.0000 C21 0.0349(6) 0.1309(5) 0.1589(8) 0.0564(32) aniso . . 1.72 1.0000 C22 0.1481(6) 0.0767(5) 0.1282(7) 0.0426(27) aniso . . 1.85 1.0000 C23 0.2837(12) -0.4576(11) -0.5480(10) 0.0928(75) aniso . . 2.91 1.0000 C24 0.3595(10) -0.5718(12) -0.5153(12) 0.1001(61) aniso . . 2.41 1.0000 C25 0.3261(15) -0.6356(9) -0.4517(12) 0.1234(81) aniso . . 4.38 1.0000 C26 0.2151(15) -0.5870(12) -0.4260(12) 0.1034(81) aniso . . 2.76 1.0000 C27 0.1464(10) -0.4759(12) -0.4548(12) 0.1012(75) aniso . . 2.13 1.0000 C28 0.0430(13) 0.5679(10) -0.0275(18) 0.1024(71) aniso . . 2.15 1.0000 C29 0.0911(11) 0.5028(16) 0.1023(14) 0.128(10) aniso . . 4.64 1.0000 C30 0.0487(13) 0.4319(13) 0.1285(16) 0.1251(75) aniso . . 3.41 1.0000 H11 -0.02610(0) 0.20800(0) -0.09600(0) 0.0800(0) iso calc C1 1.00 1.0000 H12 -0.08240(0) 0.16490(0) -0.24340(0) 0.0800(0) iso calc C1 1.00 1.0000 H13 -0.00090(0) 0.22060(0) -0.25280(0) 0.0800(0) iso calc C1 1.00 1.0000 H3 0.08360(0) 0.03050(0) -0.37110(0) 0.0800(0) iso calc C3 1.00 1.0000 H51 0.31510(0) -0.22810(0) -0.41270(0) 0.0800(0) iso calc C5 1.00 1.0000 H52 0.25170(0) -0.10470(0) -0.49160(0) 0.0800(0) iso calc C5 1.00 1.0000 H53 0.17160(0) -0.16130(0) -0.47960(0) 0.0800(0) iso calc C5 1.00 1.0000 H7 0.34470(0) -0.35830(0) -0.27420(0) 0.0800(0) iso calc C7 1.00 1.0000 H8 0.52160(0) -0.53320(0) -0.22530(0) 0.0800(0) iso calc C8 1.00 1.0000 H9 0.70090(0) -0.55990(0) -0.04290(0) 0.0800(0) iso calc C9 1.00 1.0000 H10 0.70440(0) -0.40840(0) 0.09260(0) 0.0800(0) iso calc C10 1.00 1.0000 H121 0.73040(0) -0.28740(0) 0.03010(0) 0.0800(0) iso calc C12 1.00 1.0000 H122 0.78840(0) -0.25030(0) 0.18250(0) 0.0800(0) iso calc C12 1.00 1.0000 H123 0.73580(0) -0.17390(0) 0.02720(0) 0.0800(0) iso calc C12 1.00 1.0000 H14 0.63940(0) -0.04790(0) 0.23360(0) 0.0800(0) iso calc C14 1.00 1.0000 H161 0.38960(0) 0.15670(0) 0.34300(0) 0.0800(0) iso calc C16 1.00 1.0000 H162 0.48070(0) 0.15710(0) 0.25690(0) 0.0800(0) iso calc C16 1.00 1.0000 H163 0.53200(0) 0.08640(0) 0.41680(0) 0.0800(0) iso calc C16 1.00 1.0000 H18 0.31100(0) 0.10650(0) 0.45470(0) 0.0800(0) iso calc C18 1.00 1.0000 H19 0.12100(0) 0.20130(0) 0.49980(0) 0.0800(0) iso calc C19 1.00 1.0000 H20 -0.05320(0) 0.21850(0) 0.31480(0) 0.0800(0) iso calc C20 1.00 1.0000 H21 -0.03530(0) 0.13490(0) 0.08550(0) 0.0800(0) iso calc C21 1.00 1.0000 H23 0.31030(0) -0.41480(0) -0.59750(0) 0.0800(0) iso calc C23 1.00 1.0000 H24 0.43980(0) -0.60650(0) -0.53490(0) 0.0800(0) iso calc C24 1.00 1.0000 H25 0.38250(0) -0.71410(0) -0.42250(0) 0.0800(0) iso calc C25 1.00 1.0000 H26 0.18320(0) -0.63030(0) -0.39230(0) 0.0800(0) iso calc C26 1.00 1.0000 H27 0.07030(0) -0.43960(0) -0.42790(0) 0.0800(0) iso calc C27 1.00 1.0000 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 #label U11 U22 U33 U23 U13 U12 MN1 0.0430(5) 0.0356(5) 0.0325(4) -0.0079(3) 0.0112(4) -0.0195(4) CL1 0.0674(11) 0.0441(8) 0.0611(10) -0.0026(7) 0.0320(8) -0.0232(8) N1 0.0394(27) 0.0447(26) 0.0440(26) -0.0097(22) 0.0100(21) -0.0214(23) N2 0.0471(29) 0.0455(26) 0.0381(25) -0.0119(21) 0.0094(21) -0.0246(24) N3 0.0405(26) 0.0446(26) 0.0381(24) -0.0101(21) 0.0143(20) -0.0243(22) N4 0.0524(29) 0.0375(24) 0.0356(23) -0.0069(19) 0.0155(21) -0.0274(23) N5 0.1265(77) 0.0990(62) 0.0694(47) -0.0122(43) 0.0297(48) -0.0519(60) C1 0.0560(43) 0.0670(46) 0.0489(38) 0.0052(34) 0.0004(32) -0.0183(37) C2 0.0461(34) 0.0482(33) 0.0540(36) -0.0055(28) 0.0149(28) -0.0285(29) C3 0.0630(42) 0.0589(38) 0.0366(30) 0.0019(28) 0.0027(28) -0.0385(35) C4 0.0590(38) 0.0468(33) 0.0393(31) -0.0085(26) 0.0096(27) -0.0342(31) C5 0.0767(50) 0.0759(48) 0.0388(33) -0.0135(33) 0.0124(32) -0.0453(42) C6 0.0559(38) 0.0390(30) 0.0403(30) -0.0097(25) 0.0162(27) -0.0257(29) C7 0.0741(47) 0.0573(38) 0.0444(34) -0.0177(30) 0.0221(32) -0.0414(37) C8 0.0801(52) 0.0515(38) 0.0613(42) -0.0237(33) 0.0307(38) -0.0384(38) C9 0.0752(50) 0.0422(34) 0.0749(47) -0.0159(33) 0.0399(41) -0.0253(35) C10 0.0529(38) 0.0415(32) 0.0566(37) -0.0075(28) 0.0220(30) -0.0198(29) C11 0.0623(40) 0.0414(30) 0.0424(31) -0.0134(25) 0.0279(29) -0.0294(30) C12 0.0522(40) 0.0524(38) 0.0617(41) 0.0001(32) 0.0126(32) -0.0250(33) C13 0.0475(33) 0.0407(29) 0.0353(28) 0.0005(23) 0.0128(24) -0.0219(27) C14 0.0544(38) 0.0532(35) 0.0381(30) -0.0054(27) 0.0044(26) -0.0346(32) C15 0.0575(37) 0.0428(30) 0.0273(25) -0.0022(23) 0.0099(25) -0.0303(29) C16 0.0729(46) 0.0550(37) 0.0413(33) -0.0110(29) 0.0057(31) -0.0419(36) C17 0.0523(35) 0.0315(27) 0.0390(30) -0.0067(23) 0.0178(26) -0.0169(26) C18 0.0703(45) 0.0404(32) 0.0454(34) -0.0093(27) 0.0201(31) -0.0240(32) C19 0.0949(59) 0.0513(39) 0.0549(39) -0.0206(32) 0.0436(41) -0.0366(41) C20 0.0837(56) 0.0551(41) 0.0886(57) -0.0221(40) 0.0574(48) -0.0304(41) C21 0.0590(42) 0.0484(36) 0.0715(44) -0.0110(33) 0.0316(35) -0.0268(33) C22 0.0523(36) 0.0322(27) 0.0455(32) -0.0064(25) 0.0215(28) -0.0182(26) C23 0.1355(94) 0.1346(94) 0.0607(51) -0.0254(57) 0.0361(56) -0.1024(87) C24 0.0922(75) 0.1132(88) 0.0717(62) -0.0272(62) 0.0226(53) -0.0322(69) C25 0.173(13) 0.060(6) 0.066(6) -0.010(5) 0.004(7) -0.014(8) C26 0.169(13) 0.107(9) 0.078(6) -0.019(6) 0.039(7) -0.099(10) C27 0.107(9) 0.137(10) 0.075(6) -0.029(7) 0.036(6) -0.067(8) C28 0.119(10) 0.086(7) 0.130(10) -0.022(7) 0.046(8) -0.065(7) C29 0.111(9) 0.231(17) 0.070(7) -0.051(9) 0.023(7) -0.106(12) C30 0.079(8) 0.136(11) 0.114(10) 0.034(8) 0.042(7) -0.004(7) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag MN1 CL1 2.363(3) yes MN1 N1 1.957(4) yes MN1 N2 1.962(5) yes MN1 N3 1.962(5) yes MN1 N4 1.963(5) yes N1 C2 1.335(7) yes N1 C22 1.431(8) yes N2 C4 1.339(6) yes N2 C6 1.427(7) yes N3 C11 1.425(8) yes N3 C13 1.33(1) yes N4 C15 1.34(1) yes N4 C17 1.410(8) yes N5 C23 1.35(1) yes N5 C27 1.32(2) yes C1 C2 1.494(8) yes C2 C3 1.394(9) yes C3 C4 1.387(8) yes C4 C5 1.503(9) yes C6 C7 1.39(1) yes C6 C11 1.421(9) yes C7 C8 1.384(9) yes C8 C9 1.39(1) yes C9 C10 1.40(1) yes C10 C11 1.376(7) yes C12 C13 1.51(0) yes C13 C14 1.417(9) yes C14 C15 1.377(9) yes C15 C16 1.52(1) yes C17 C18 1.414(8) yes C17 C22 1.418(9) yes C18 C19 1.37(1) yes C19 C20 1.37(1) yes C20 C21 1.38(1) yes C21 C22 1.38(1) yes C23 C24 1.37(1) yes C24 C25 1.33(2) yes C25 C26 1.34(2) yes C26 C27 1.32(1) yes C28 C29 1.31(2) yes C29 C30 1.36(3) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag N3 MN1 N4 93.1(2) yes N2 MN1 N4 154.1(2) yes N2 MN1 N3 82.1(2) yes N1 MN1 N4 82.6(2) yes N1 MN1 N3 155.8(2) yes N1 MN1 N2 91.5(2) yes CL1 MN1 N4 101.7(2) yes CL1 MN1 N3 101.4(2) yes CL1 MN1 N2 104.2(2) yes CL1 MN1 N1 102.8(2) yes MN1 N1 C22 107.0(4) yes MN1 N1 C2 126.9(4) yes C2 N1 C22 125.1(5) yes MN1 N2 C6 106.5(4) yes MN1 N2 C4 126.4(4) yes C4 N2 C6 126.7(5) yes MN1 N3 C13 125.9(4) yes MN1 N3 C11 107.6(5) yes C11 N3 C13 126.2(6) yes MN1 N4 C17 107.6(4) yes MN1 N4 C15 125.4(4) yes C15 N4 C17 126.6(5) yes C23 N5 C27 115(1) yes N1 C2 C1 122.6(6) yes C1 C2 C3 116.9(6) yes N1 C2 C3 120.4(6) yes C2 C3 C4 130.4(6) yes N2 C4 C3 121.1(6) yes C3 C4 C5 117.9(6) yes N2 C4 C5 120.8(6) yes N2 C6 C11 114.6(5) yes N2 C6 C7 125.0(6) yes C7 C6 C11 120.1(6) yes C6 C7 C8 119.7(7) yes C7 C8 C9 121.0(7) yes C8 C9 C10 119.4(7) yes C9 C10 C11 120.8(7) yes C6 C11 C10 119.0(6) yes N3 C11 C10 127.4(6) yes N3 C11 C6 113.2(5) yes N3 C13 C12 121.1(6) yes C12 C13 C14 117.7(7) yes N3 C13 C14 121.2(6) yes C13 C14 C15 130.1(7) yes N4 C15 C14 122.3(6) yes C14 C15 C16 117.1(7) yes N4 C15 C16 120.5(7) yes N4 C17 C22 114.9(5) yes N4 C17 C18 127.3(6) yes C18 C17 C22 117.2(6) yes C17 C18 C19 121.3(6) yes C18 C19 C20 119.9(7) yes C19 C20 C21 121.6(9) yes C20 C21 C22 119.2(7) yes C17 C22 C21 120.8(6) yes N1 C22 C21 125.5(6) yes N1 C22 C17 113.6(6) yes N5 C23 C24 121(1) yes C23 C24 C25 121(1) yes C24 C25 C26 119(1) yes C25 C26 C27 118(2) yes N5 C27 C26 126(1) yes C28 C29 C30 121(1) yes _refine_diff_density_max 0.412 _refine_diff_density_min -0.528 _refine_diff_density_rms 0.085 #===END ######################################################################## ###### #### Complex 4B Crystallographic Data data_COMPLEX_4B _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C54H62BMnN4O4' _chemical_formula_weight 896.86 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Mn' 'Mn' -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 '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 12.260(2) _cell_length_b 16.785(2) _cell_length_c 11.637(1) _cell_angle_alpha 99.11(2) _cell_angle_beta 91.60(2) _cell_angle_gamma 81.55(2) _cell_volume 2338.8(5) _cell_formula_units_Z 2.00 _cell_measurement_temperature 25 _cell_measurement_reflns_used 143 _cell_measurement_theta_min 18.3 _cell_measurement_theta_max 27.4 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.2735 _exptl_crystal_density_method not_measured _exptl_crystal_F_000 952.0 _exptl_absorpt_coefficient_mu 2.6782 _exptl_absorpt_correction_type 'North et al. 1968' _exptl_absorpt_correction_T_min 0.855 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 143 _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focussealedtube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku AFC6S' _diffrn_measurement_method 'omega/2theta' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 3.2 _diffrn_reflns_number 8081 _diffrn_reflns_av_R_equivalents 0.1435 _diffrn_reflns_av_sigmaI/netI 0.0895 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_theta_max 70.11 _reflns_number_total 7633 _reflns_number_observed 4553 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'TEXSAN Software' _computing_cell_refinement 'TEXSAN Software' _computing_data_reduction 'TEXSAN Software' _computing_structure_solution 'SHELXS-76 (Sheldrick, 1976)' _computing_structure_refinement 'SHELXS-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 904 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses of fit S are based on F^2^, conventional R- factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R factor obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1552P)^2^+0.1594P] 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 not_refined _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6729 _refine_ls_number_parameters 577 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1391 _refine_ls_R_factor_obs 0.0738 _refine_ls_wR_factor_all 0.3055 _refine_ls_wR_factor_obs 0.2019 _refine_ls_goodness_of_fit_all 1.085 _refine_ls_goodness_of_fit_obs 1.175 _refine_ls_restrained_S_all 1.355 _refine_ls_restrained_S_obs 1.175 _refine_ls_shift/esd_max 0.061 _refine_ls_shift/esd_mean 0.014 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_aniso_ratio _atom_site_occupancy # # R=Rmax./Rmin.=ratio of the maximum and minimum # principal axes of atomic displacement ellipsoids # # Table of coordinates # -------------------- # # atom x/a y/b z/c Ueq tmf calc att R SOF MN1 0.24209(7) 0.24421(5) -0.21877(7) 0.0275(3) aniso . . 2.59 1.0000 O1 0.1257(4) 0.3405(2) -0.3031(4) 0.0537(17) aniso . . 3.93 1.0000 O2 0.1484(6) 0.3301(5) -0.6025(6) 0.1092(30) aniso . . 2.32 1.0000 O3 0.3618(3) 0.1428(2) -0.1239(3) 0.0308(12) aniso . . 2.03 1.0000 O4 0.5943(3) 0.0817(2) -0.1875(4) 0.0473(15) aniso . . 2.05 1.0000 N1 0.3683(4) 0.2423(2) -0.3145(4) 0.0280(14) aniso . . 2.45 1.0000 N2 0.1870(4) 0.1538(2) -0.3139(4) 0.0276(14) aniso . . 1.71 1.0000 N3 0.1288(4) 0.2336(2) -0.1127(4) 0.0273(13) aniso . . 3.02 1.0000 N4 0.3033(4) 0.3299(2) -0.1173(4) 0.0274(13) aniso . . 3.23 1.0000 B1 0.2645(5) -0.2653(3) -0.2710(5) 0.0235(17) aniso . . 3.13 1.0000 C1 0.5342(5) 0.1661(4) -0.4190(5) 0.0376(17) aniso . . 2.10 1.0000 C2 0.4176(5) 0.1737(3) -0.3787(4) 0.0303(17) aniso . . 1.87 1.0000 C3 0.3622(5) 0.1058(3) -0.4046(4) 0.0328(18) aniso . . 6.27 1.0000 C4 0.2542(5) 0.0947(3) -0.3819(4) 0.0279(16) aniso . . 3.59 1.0000 C5 0.2175(5) 0.0144(3) -0.4259(5) 0.0372(19) aniso . . 2.40 1.0000 C6 0.0749(4) 0.1520(3) -0.2876(4) 0.0258(16) aniso . . 2.67 1.0000 C7 -0.0041(5) 0.1233(3) -0.3620(4) 0.0300(16) aniso . . 2.67 1.0000 C8 -0.1139(5) 0.1334(3) -0.3243(5) 0.0321(17) aniso . . 2.58 1.0000 C9 -0.1431(4) 0.1712(3) -0.2151(5) 0.0291(15) aniso . . 1.86 1.0000 C10 -0.0652(4) 0.2029(3) -0.1391(4) 0.0300(16) aniso . . 1.69 1.0000 C11 0.0440(4) 0.1950(3) -0.1743(4) 0.0263(16) aniso . . 3.03 1.0000 C12 0.0782(5) 0.2160(3) 0.0854(5) 0.0374(19) aniso . . 2.36 1.0000 C13 0.1414(4) 0.2527(3) 0.0040(4) 0.0283(16) aniso . . 3.02 1.0000 C14 0.2178(4) 0.3021(3) 0.0529(4) 0.0294(15) aniso . . 1.99 1.0000 C15 0.2918(4) 0.3419(3) -0.0018(4) 0.0279(16) aniso . . 1.54 1.0000 C16 0.3579(5) 0.3969(3) 0.0760(5) 0.0344(19) aniso . . 1.70 1.0000 C17 0.3713(4) 0.3679(3) -0.1842(4) 0.0262(15) aniso . . 2.31 1.0000 C18 0.3932(4) 0.4479(3) -0.1594(5) 0.0305(15) aniso . . 3.65 1.0000 C19 0.4549(5) 0.4783(3) -0.2366(5) 0.0391(20) aniso . . 2.85 1.0000 C20 0.4943(5) 0.4300(4) -0.3382(5) 0.0407(21) aniso . . 2.62 1.0000 C21 0.4693(5) 0.3514(3) -0.3671(5) 0.0371(18) aniso . . 1.88 1.0000 C22 0.4090(4) 0.3193(3) -0.2911(4) 0.0277(17) aniso . . 1.57 1.0000 C23 0.0630(9) 0.4118(5) -0.2121(12) 0.1196(50) aniso . . 8.05 1.0000 C24 0.1419(10) 0.3686(7) -0.4004(12) 0.1127(57) aniso . . 2.75 1.0000 C25 0.1389(9) 0.3037(5) -0.4949(9) 0.0906(39) aniso . . 3.52 1.0000 C26 0.0554(9) 0.3786(8) -0.6397(9) 0.1149(56) aniso . . 2.96 1.0000 C27 0.3137(5) 0.0798(3) -0.0864(5) 0.0423(21) aniso . . 2.86 1.0000 C28 0.4568(5) 0.1626(3) -0.0588(5) 0.0395(19) aniso . . 1.61 1.0000 C29 0.5557(5) 0.0973(4) -0.0720(5) 0.0431(20) aniso . . 1.74 1.0000 C30 0.6901(5) 0.0217(4) -0.1974(6) 0.0461(22) aniso . . 2.35 1.0000 C31 0.2643(4) -0.3135(3) -0.1556(4) 0.0263(15) aniso . . 3.25 1.0000 C32 0.3418(5) -0.3066(3) -0.0659(4) 0.0338(16) aniso . . 1.81 1.0000 C33 0.3319(5) -0.3395(4) 0.0366(5) 0.0409(18) aniso . . 2.18 1.0000 C34 0.2472(6) -0.3825(3) 0.0496(5) 0.0417(20) aniso . . 5.89 1.0000 C35 0.1696(5) -0.3911(3) -0.0381(5) 0.0416(19) aniso . . 3.25 1.0000 C36 0.1792(5) -0.3577(3) -0.1401(5) 0.0334(16) aniso . . 2.84 1.0000 C37 0.1656(4) -0.1856(3) -0.2438(4) 0.0289(16) aniso . . 2.60 1.0000 C38 0.0766(4) -0.1662(3) -0.3171(4) 0.0316(18) aniso . . 2.02 1.0000 C39 0.0006(5) -0.0955(3) -0.2901(5) 0.0366(19) aniso . . 3.02 1.0000 C40 0.0120(5) -0.0414(3) -0.1898(5) 0.0386(19) aniso . . 4.76 1.0000 C41 0.0965(5) -0.0599(3) -0.1137(5) 0.0341(18) aniso . . 3.51 1.0000 C42 0.1704(5) -0.1318(3) -0.1392(5) 0.0322(18) aniso . . 1.57 1.0000 C43 0.2471(4) -0.3247(3) -0.3935(4) 0.0263(15) aniso . . 1.67 1.0000 C44 0.2516(5) -0.4093(3) -0.4057(4) 0.0316(19) aniso . . 1.84 1.0000 C45 0.2410(5) -0.4579(3) -0.5131(5) 0.0389(19) aniso . . 2.62 1.0000 C46 0.2228(5) -0.4227(3) -0.6145(5) 0.0421(19) aniso . . 3.98 1.0000 C47 0.2200(6) -0.3394(4) -0.6070(4) 0.0428(20) aniso . . 3.53 1.0000 C48 0.2331(5) -0.2926(3) -0.4993(4) 0.0323(16) aniso . . 2.12 1.0000 C49 0.3833(4) -0.2335(3) -0.2807(4) 0.0267(16) aniso . . 3.52 1.0000 C50 0.4024(5) -0.1516(3) -0.2660(5) 0.0303(17) aniso . . 3.34 1.0000 C51 0.5044(5) -0.1276(3) -0.2741(5) 0.0378(18) aniso . . 1.81 1.0000 C52 0.5961(5) -0.1848(4) -0.3014(5) 0.0417(20) aniso . . 2.00 1.0000 C53 0.5835(5) -0.2685(4) -0.3187(5) 0.0398(20) aniso . . 1.70 1.0000 C54 0.4800(5) -0.2901(3) -0.3090(4) 0.0348(18) aniso . . 1.81 1.0000 H11 0.57830(0) 0.20280(0) -0.37860(0) 0.0500(0) iso calc C1 1.00 1.0000 H12 0.54430(0) 0.17130(0) -0.51220(0) 0.0500(0) iso calc C1 1.00 1.0000 H13 0.58010(0) 0.11900(0) -0.40190(0) 0.0500(0) iso calc C1 1.00 1.0000 H3 0.38830(0) 0.06670(0) -0.44680(0) 0.0500(0) iso calc C3 1.00 1.0000 H51 0.14960(0) 0.00210(0) -0.40070(0) 0.0500(0) iso calc C5 1.00 1.0000 H52 0.27080(0) -0.01740(0) -0.40610(0) 0.0500(0) iso calc C5 1.00 1.0000 H53 0.19410(0) 0.00950(0) -0.49990(0) 0.0500(0) iso calc C5 1.00 1.0000 H7 0.01480(0) 0.08570(0) -0.43810(0) 0.0500(0) iso calc C7 1.00 1.0000 H8 -0.16100(0) 0.11650(0) -0.38620(0) 0.0500(0) iso calc C8 1.00 1.0000 H9 -0.21390(0) 0.17790(0) -0.19990(0) 0.0500(0) iso calc C9 1.00 1.0000 H10 -0.08310(0) 0.22460(0) -0.06300(0) 0.0500(0) iso calc C10 1.00 1.0000 H121 0.04160(0) 0.17380(0) 0.04850(0) 0.0500(0) iso calc C12 1.00 1.0000 H122 0.02330(0) 0.24310(0) 0.11870(0) 0.0500(0) iso calc C12 1.00 1.0000 H123 0.13370(0) 0.19450(0) 0.15200(0) 0.0500(0) iso calc C12 1.00 1.0000 H14 0.22200(0) 0.30600(0) 0.13870(0) 0.0500(0) iso calc C14 1.00 1.0000 H161 0.42080(0) 0.40570(0) 0.04210(0) 0.0500(0) iso calc C16 1.00 1.0000 H162 0.38560(0) 0.37820(0) 0.14350(0) 0.0500(0) iso calc C16 1.00 1.0000 H163 0.31880(0) 0.44710(0) 0.10890(0) 0.0500(0) iso calc C16 1.00 1.0000 H18 0.36400(0) 0.49310(0) -0.08290(0) 0.0500(0) iso calc C18 1.00 1.0000 H19 0.47450(0) 0.53690(0) -0.21200(0) 0.0500(0) iso calc C19 1.00 1.0000 H20 0.53210(0) 0.45350(0) -0.39080(0) 0.0500(0) iso calc C20 1.00 1.0000 H21 0.49680(0) 0.31060(0) -0.44200(0) 0.0500(0) iso calc C21 1.00 1.0000 H231 0.05060(0) 0.39160(0) -0.13670(0) 0.0500(0) iso calc C23 1.00 1.0000 H232 -0.00950(0) 0.43370(0) -0.24030(0) 0.0500(0) iso calc C23 1.00 1.0000 H233 0.10680(0) 0.45730(0) -0.19130(0) 0.0500(0) iso calc C23 1.00 1.0000 H241 0.21210(0) 0.39150(0) -0.39870(0) 0.0500(0) iso calc C24 1.00 1.0000 H242 0.08060(0) 0.41550(0) -0.41140(0) 0.0500(0) iso calc C24 1.00 1.0000 H251 0.05280(0) 0.29720(0) -0.46270(0) 0.0500(0) iso calc C25 1.00 1.0000 H252 0.20730(0) 0.25430(0) -0.48400(0) 0.0500(0) iso calc C25 1.00 1.0000 H261 0.06680(0) 0.39530(0) -0.71730(0) 0.0500(0) iso calc C26 1.00 1.0000 H262 0.03350(0) 0.43070(0) -0.58510(0) 0.0500(0) iso calc C26 1.00 1.0000 H263 -0.01190(0) 0.35060(0) -0.64960(0) 0.0500(0) iso calc C26 1.00 1.0000 H271 0.23180(0) 0.07780(0) -0.12860(0) 0.0500(0) iso calc C27 1.00 1.0000 H272 0.29430(0) 0.08980(0) -0.00590(0) 0.0500(0) iso calc C27 1.00 1.0000 H273 0.35870(0) 0.02860(0) -0.09700(0) 0.0500(0) iso calc C27 1.00 1.0000 H281 0.43790(0) 0.18660(0) 0.02850(0) 0.0500(0) iso calc C28 1.00 1.0000 H282 0.47910(0) 0.19900(0) -0.08740(0) 0.0500(0) iso calc C28 1.00 1.0000 H291 0.61770(0) 0.11120(0) -0.02380(0) 0.0500(0) iso calc C29 1.00 1.0000 H292 0.54150(0) 0.03780(0) -0.05530(0) 0.0500(0) iso calc C29 1.00 1.0000 H301 0.71730(0) 0.01040(0) -0.27700(0) 0.0500(0) iso calc C30 1.00 1.0000 H302 0.67710(0) -0.02970(0) -0.17810(0) 0.0500(0) iso calc C30 1.00 1.0000 H303 0.75010(0) 0.04180(0) -0.14740(0) 0.0500(0) iso calc C30 1.00 1.0000 H32 0.40800(0) -0.27640(0) -0.06450(0) 0.0500(0) iso calc C32 1.00 1.0000 H33 0.38190(0) -0.33070(0) 0.08260(0) 0.0500(0) iso calc C33 1.00 1.0000 H34 0.24480(0) -0.40780(0) 0.11370(0) 0.0500(0) iso calc C34 1.00 1.0000 H35 0.11140(0) -0.41890(0) -0.03190(0) 0.0500(0) iso calc C35 1.00 1.0000 H36 0.12320(0) -0.36500(0) -0.20740(0) 0.0500(0) iso calc C36 1.00 1.0000 H38 0.06250(0) -0.20340(0) -0.39310(0) 0.0500(0) iso calc C38 1.00 1.0000 H39 -0.06660(0) -0.08660(0) -0.33820(0) 0.0500(0) iso calc C39 1.00 1.0000 H40 -0.03430(0) -0.00380(0) -0.17910(0) 0.0500(0) iso calc C40 1.00 1.0000 H41 0.10040(0) -0.02310(0) -0.02870(0) 0.0500(0) iso calc C41 1.00 1.0000 H42 0.22720(0) -0.13930(0) -0.08930(0) 0.0500(0) iso calc C42 1.00 1.0000 H44 0.26660(0) -0.43990(0) -0.33320(0) 0.0500(0) iso calc C44 1.00 1.0000 H45 0.24750(0) -0.51730(0) -0.51210(0) 0.0500(0) iso calc C45 1.00 1.0000 H46 0.22490(0) -0.45540(0) -0.68990(0) 0.0500(0) iso calc C46 1.00 1.0000 H47 0.19860(0) -0.31420(0) -0.67890(0) 0.0500(0) iso calc C47 1.00 1.0000 H48 0.22490(0) -0.23850(0) -0.50420(0) 0.0500(0) iso calc C48 1.00 1.0000 H50 0.35040(0) -0.10780(0) -0.24800(0) 0.0500(0) iso calc C50 1.00 1.0000 H51 0.51210(0) -0.08090(0) -0.26040(0) 0.0500(0) iso calc C5 1.00 1.0000 H52 0.67390(0) -0.17100(0) -0.30670(0) 0.0500(0) iso calc C5 1.00 1.0000 H53 0.65300(0) -0.31260(0) -0.34210(0) 0.0500(0) iso calc C5 1.00 1.0000 H54 0.46960(0) -0.34770(0) -0.31800(0) 0.0500(0) iso calc C54 1.00 1.0000 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 #label U11 U22 U33 U23 U13 U12 MN1 0.0359(5) 0.0197(4) 0.0257(4) -0.0029(3) 0.0089(3) -0.0057(3) O1 0.0573(29) 0.0268(20) 0.0796(33) 0.0209(21) -0.0090(25) -0.0030(20) O2 0.1252(60) 0.1114(57) 0.0849(47) 0.0294(42) -0.0062(43) 0.0168(46) O3 0.0344(21) 0.0245(17) 0.0360(20) 0.0113(15) -0.0043(16) -0.0064(15) O4 0.0442(25) 0.0432(23) 0.0538(26) 0.0158(20) 0.0067(20) 0.0063(20) N1 0.0380(26) 0.0167(19) 0.0281(22) 0.0014(16) 0.0047(19) -0.0008(18) N2 0.0324(25) 0.0227(20) 0.0268(21) 0.0008(17) 0.0055(19) -0.0026(19) N3 0.0312(25) 0.0173(19) 0.0305(22) -0.0053(16) 0.0081(19) -0.0026(18) N4 0.0322(24) 0.0127(17) 0.0360(23) 0.0022(16) 0.0056(19) 0.0008(17) B1 0.0314(32) 0.0127(22) 0.0256(27) 0.0055(20) -0.0029(24) 0.0013(23) C1 0.0349(32) 0.0418(31) 0.0327(29) -0.0001(24) 0.0105(25) 0.0003(26) C2 0.0401(32) 0.0270(25) 0.0238(25) 0.0050(20) 0.0044(23) -0.0021(23) C3 0.0483(35) 0.0191(22) 0.0259(25) -0.0086(19) 0.0145(24) 0.0011(23) C4 0.0428(33) 0.0156(22) 0.0227(24) -0.0036(18) 0.0056(23) -0.0020(22) C5 0.0440(35) 0.0228(25) 0.0414(31) -0.0043(22) -0.0003(27) -0.0038(24) C6 0.0320(29) 0.0157(20) 0.0313(25) 0.0094(19) 0.0010(22) -0.0018(21) C7 0.0386(31) 0.0155(21) 0.0342(27) 0.0035(20) -0.0003(24) 0.0004(22) C8 0.0412(33) 0.0175(22) 0.0377(28) 0.0051(20) -0.0037(25) -0.0042(23) C9 0.0312(30) 0.0200(22) 0.0350(27) 0.0028(20) 0.0034(24) -0.0013(22) C10 0.0335(31) 0.0236(23) 0.0340(28) 0.0048(21) 0.0040(23) -0.0060(23) C11 0.0340(30) 0.0159(21) 0.0310(26) 0.0074(19) 0.0068(23) -0.0046(21) C12 0.0429(35) 0.0365(29) 0.0332(28) 0.0027(23) 0.0144(26) -0.0075(27) C13 0.0255(27) 0.0259(24) 0.0289(26) -0.0020(20) 0.0086(22) 0.0065(21) C14 0.0330(30) 0.0242(24) 0.0275(25) -0.0013(20) 0.0019(23) 0.0022(23) C15 0.0340(30) 0.0241(23) 0.0250(25) 0.0015(19) 0.0023(22) -0.0042(22) C16 0.0368(32) 0.0324(27) 0.0335(28) 0.0010(22) -0.0058(25) -0.0095(25) C17 0.0333(29) 0.0159(21) 0.0300(25) 0.0062(19) -0.0018(22) -0.0026(21) C18 0.0336(30) 0.0128(20) 0.0445(30) 0.0044(20) -0.0030(25) -0.0022(21) C19 0.0441(35) 0.0256(26) 0.0516(35) 0.0098(25) -0.0053(29) -0.0145(26) C20 0.0413(35) 0.0419(31) 0.0463(34) 0.0206(27) -0.0016(28) -0.0162(28) C21 0.0415(34) 0.0284(26) 0.0427(32) 0.0078(23) 0.0077(27) -0.0057(25) C22 0.0320(29) 0.0219(23) 0.0298(26) 0.0066(20) 0.0003(23) -0.0032(22) C23 0.116(8) 0.038(4) 0.198(13) 0.023(6) -0.073(9) 0.004(5) C24 0.1290(98) 0.0965(80) 0.1295(99) 0.0571(77) -0.0307(79) -0.0354(72) C25 0.1267(84) 0.0536(47) 0.0912(68) 0.0284(48) 0.0291(61) 0.0121(52) C26 0.085(7) 0.165(12) 0.079(7) 0.010(7) -0.013(6) 0.019(7) C27 0.0556(39) 0.0239(25) 0.0487(34) 0.0121(25) 0.0058(30) -0.0023(27) C28 0.0459(36) 0.0337(29) 0.0386(30) 0.0050(24) -0.0081(27) -0.0066(27) C29 0.0419(36) 0.0381(31) 0.0453(34) 0.0027(26) -0.0049(29) 0.0024(27) C30 0.0400(35) 0.0301(29) 0.0671(42) 0.0073(28) 0.0048(31) -0.0005(27) C31 0.0334(29) 0.0135(20) 0.0293(26) 0.0006(18) 0.0056(23) 0.0036(21) C32 0.0413(33) 0.0316(26) 0.0260(26) 0.0029(21) -0.0008(24) 0.0016(25) C33 0.0529(38) 0.0355(29) 0.0299(28) 0.0043(23) -0.0022(27) 0.0070(28) C34 0.0715(44) 0.0191(24) 0.0287(28) 0.0027(21) 0.0125(29) 0.0137(27) C35 0.0604(41) 0.0237(25) 0.0409(32) -0.0003(23) 0.0208(30) -0.0090(27) C36 0.0438(34) 0.0223(24) 0.0313(27) -0.0002(20) 0.0118(25) 0.0019(24) C37 0.0318(30) 0.0229(23) 0.0329(26) 0.0021(20) 0.0134(23) -0.0065(22) C38 0.0360(31) 0.0370(28) 0.0223(25) 0.0063(21) 0.0058(23) -0.0035(25) C39 0.0388(33) 0.0347(28) 0.0337(28) 0.0127(23) 0.0012(25) 0.0116(26) C40 0.0453(35) 0.0227(24) 0.0452(32) 0.0109(23) 0.0175(28) 0.0136(25) C41 0.0412(33) 0.0191(23) 0.0392(29) 0.0002(21) 0.0156(26) 0.0029(23) C42 0.0329(30) 0.0301(26) 0.0336(28) 0.0022(22) 0.0070(24) -0.0065(23) C43 0.0264(27) 0.0227(23) 0.0276(25) -0.0007(19) 0.0037(21) -0.0008(21) C44 0.0408(32) 0.0284(25) 0.0267(25) 0.0086(21) 0.0000(23) -0.0037(24) C45 0.0589(40) 0.0272(26) 0.0307(28) -0.0011(22) 0.0033(27) -0.0120(27) C46 0.0647(43) 0.0276(26) 0.0285(27) -0.0072(22) 0.0080(28) 0.0001(28) C47 0.0662(43) 0.0388(30) 0.0213(26) 0.0074(22) 0.0026(27) 0.0029(30) C48 0.0425(33) 0.0229(24) 0.0304(27) 0.0059(21) 0.0038(25) 0.0013(24) C49 0.0324(29) 0.0165(22) 0.0285(25) 0.0026(19) 0.0103(22) 0.0063(21) C50 0.0399(32) 0.0148(21) 0.0376(28) 0.0036(19) 0.0033(24) -0.0086(22) C51 0.0436(35) 0.0273(26) 0.0419(31) 0.0004(23) 0.0024(27) -0.0077(26) C52 0.0398(35) 0.0555(37) 0.0345(30) 0.0134(27) 0.0000(26) -0.0152(30) C53 0.0378(34) 0.0489(34) 0.0328(30) 0.0104(25) 0.0030(26) -0.0016(28) C54 0.0384(33) 0.0399(30) 0.0287(27) 0.0104(23) 0.0048(24) -0.0079(26) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag MN1 O1 2.315(4) yes MN1 N1 1.925(5) yes MN1 N2 1.927(4) yes MN1 N3 1.929(5) yes MN1 N4 1.938(4) yes O1 C23 1.59(1) yes O1 C24 1.32(1) yes O2 C25 1.41(1) yes O2 C26 1.40(1) yes O3 C27 1.414(7) yes O3 C28 1.423(7) yes O4 C29 1.410(7) yes O4 C30 1.425(7) yes N1 C2 1.341(6) yes N1 C22 1.437(7) yes N2 C4 1.355(6) yes N2 C6 1.422(7) yes N3 C11 1.423(7) yes N3 C13 1.355(6) yes N4 C15 1.336(7) yes N4 C17 1.434(7) yes B1 C31 1.674(8) yes B1 C37 1.664(7) yes B1 C43 1.633(7) yes B1 C49 1.636(8) yes C1 C2 1.498(9) yes C2 C3 1.399(8) yes C3 C4 1.402(9) yes C4 C5 1.493(8) yes C6 C7 1.370(7) yes C6 C11 1.431(6) yes C7 C8 1.406(9) yes C8 C9 1.360(8) yes C9 C10 1.390(7) yes C10 C11 1.393(7) yes C12 C13 1.498(8) yes C13 C14 1.392(7) yes C14 C15 1.421(8) yes C15 C16 1.498(7) yes C17 C18 1.392(7) yes C17 C22 1.424(6) yes C18 C19 1.391(9) yes C19 C20 1.379(8) yes C20 C21 1.386(9) yes C21 C22 1.387(8) yes C24 C25 1.42(1) yes C28 C29 1.504(8) yes C31 C32 1.394(7) yes C31 C36 1.397(8) yes C32 C33 1.407(8) yes C33 C34 1.37(1) yes C34 C35 1.381(9) yes C35 C36 1.405(9) yes C37 C38 1.398(7) yes C37 C42 1.401(7) yes C38 C39 1.396(7) yes C39 C40 1.378(7) yes C40 C41 1.377(8) yes C41 C42 1.395(7) yes C43 C44 1.398(7) yes C43 C48 1.417(7) yes C44 C45 1.394(7) yes C45 C46 1.400(8) yes C46 C47 1.382(9) yes C47 C48 1.388(7) yes C49 C50 1.411(7) yes C49 C54 1.417(7) yes C50 C51 1.379(9) yes C51 C52 1.376(8) yes C52 C53 1.42(1) yes C53 C54 1.382(9) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag N3 MN1 N4 95.9(2) yes N2 MN1 N4 176.1(2) yes N2 MN1 N3 83.6(2) yes N1 MN1 N4 84.5(2) yes N1 MN1 N3 171.5(2) yes N1 MN1 N2 95.4(2) yes O1 MN1 N4 90.5(2) yes O1 MN1 N3 91.8(2) yes O1 MN1 N2 93.3(2) yes O1 MN1 N1 96.6(2) yes MN1 O1 C24 127.4(6) yes MN1 O1 C23 114.0(5) yes C23 O1 C24 109.5(7) yes C25 O2 C26 116.0(8) yes C27 O3 C28 113.9(4) yes C29 O4 C30 110.0(5) yes MN1 N1 C22 110.1(3) yes MN1 N1 C2 122.4(4) yes C2 N1 C22 126.7(5) yes MN1 N2 C6 110.9(3) yes MN1 N2 C4 122.1(4) yes C4 N2 C6 126.3(4) yes MN1 N3 C13 121.3(4) yes MN1 N3 C11 110.2(3) yes C11 N3 C13 128.0(4) yes MN1 N4 C17 109.3(3) yes MN1 N4 C15 122.6(3) yes C15 N4 C17 127.6(4) yes C43 B1 C49 106.3(4) yes C37 B1 C49 109.7(4) yes C37 B1 C43 113.5(4) yes C31 B1 C49 110.1(4) yes C31 B1 C43 112.4(4) yes C31 B1 C37 104.7(4) yes N1 C2 C1 121.4(5) yes C1 C2 C3 118.4(5) yes N1 C2 C3 120.1(5) yes C2 C3 C4 131.7(5) yes N2 C4 C3 120.4(4) yes C3 C4 C5 118.9(5) yes N2 C4 C5 120.5(5) yes N2 C6 C11 112.6(4) yes N2 C6 C7 127.1(4) yes C7 C6 C11 119.7(5) yes C6 C7 C8 119.5(5) yes C7 C8 C9 121.1(6) yes C8 C9 C10 120.5(5) yes C9 C10 C11 119.8(4) yes C6 C11 C10 119.2(4) yes N3 C11 C10 125.9(4) yes N3 C11 C6 114.5(4) yes N3 C13 C12 120.4(4) yes C12 C13 C14 117.4(4) yes N3 C13 C14 122.1(4) yes C13 C14 C15 129.9(4) yes N4 C15 C14 121.6(4) yes C14 C15 C16 117.0(4) yes N4 C15 C16 121.4(4) yes N4 C17 C22 114.3(4) yes N4 C17 C18 126.3(4) yes C18 C17 C22 119.1(5) yes C17 C18 C19 119.9(5) yes C18 C19 C20 120.6(5) yes C19 C20 C21 120.4(5) yes C20 C21 C22 120.1(5) yes C17 C22 C21 119.7(5) yes N1 C22 C21 125.9(5) yes N1 C22 C17 114.0(4) yes O1 C24 C25 108.0(9) yes O2 C25 C24 111.5(9) yes O3 C28 C29 115.5(5) yes O4 C29 C28 110.8(5) yes B1 C31 C36 120.6(4) yes B1 C31 C32 122.8(5) yes C32 C31 C36 116.4(4) yes C31 C32 C33 121.6(5) yes C32 C33 C34 120.7(6) yes C33 C34 C35 119.1(5) yes C34 C35 C36 120.1(6) yes C31 C36 C35 122.1(5) yes B1 C37 C42 118.4(5) yes B1 C37 C38 125.8(4) yes C38 C37 C42 115.8(5) yes C37 C38 C39 121.9(5) yes C38 C39 C40 120.6(5) yes C39 C40 C41 119.1(5) yes C40 C41 C42 120.2(5) yes C37 C42 C41 122.3(5) yes B1 C43 C48 120.6(4) yes B1 C43 C44 124.8(4) yes C44 C43 C48 114.6(4) yes C43 C44 C45 122.7(5) yes C44 C45 C46 120.5(5) yes C45 C46 C47 118.9(5) yes C46 C47 C48 119.4(5) yes C43 C48 C47 123.9(5) yes B1 C49 C54 120.4(4) yes B1 C49 C50 126.5(5) yes C50 C49 C54 113.1(5) yes C49 C50 C51 124.5(5) yes C50 C51 C52 120.4(5) yes C51 C52 C53 118.6(6) yes C52 C53 C54 119.3(6) yes C49 C54 C53 124.2(5) yes _refine_diff_density_max 0.896 _refine_diff_density_min -1.092 _refine_diff_density_rms 0.093 #===END ######################################################################## ###### #### Complex 6 Crystallographic Data data_COMPLEX_6 _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C26H30MnN5O2' _chemical_formula_weight 499.49 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Mn' 'Mn' -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P21/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 10.892(2) _cell_length_b 13.884(2) _cell_length_c 16.057(2) _cell_angle_alpha 90.00(0) _cell_angle_beta 103.89(1) _cell_angle_gamma 90.00(0) _cell_volume 2357.2(6) _cell_formula_units_Z 4.00 _cell_measurement_temperature 25 _cell_measurement_reflns_used 143 _cell_measurement_theta_min 22.3 _cell_measurement_theta_max 39.2 _exptl_crystal_description flattened_prism _exptl_crystal_colour red _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.4075 _exptl_crystal_density_method not_measured _exptl_crystal_F_000 1048.0 _exptl_absorpt_coefficient_mu 4.8335 _exptl_absorpt_correction_type 'North et al. 1968' _exptl_absorpt_correction_T_min 0.567 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 143 _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focussealedtube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku AFC6S' _diffrn_measurement_method 'omega/2theta' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1.8 _diffrn_reflns_number 4183 _diffrn_reflns_av_R_equivalents 0.1094 _diffrn_reflns_av_sigmaI/netI 0.1373 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 4.18 _diffrn_reflns_theta_max 70.05 _reflns_number_total 3961 _reflns_number_observed 1926 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'TEXSAN Software' _computing_cell_refinement 'TEXSAN Software' _computing_data_reduction 'TEXSAN Software' _computing_structure_solution 'SHELXS-76 (Sheldrick, 1976)' _computing_structure_refinement 'SHELXS-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 671 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses of fit S are based on F^2^, conventional R- factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R factor obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1481P)^2^+6.7452P] 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 not_refined _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0017(4) _refine_ls_number_reflns 3290 _refine_ls_number_parameters 306 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.2015 _refine_ls_R_factor_obs 0.0853 _refine_ls_wR_factor_all 0.3750 _refine_ls_wR_factor_obs 0.2255 _refine_ls_goodness_of_fit_all 1.063 _refine_ls_goodness_of_fit_obs 1.215 _refine_ls_restrained_S_all 1.403 _refine_ls_restrained_S_obs 1.214 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_aniso_ratio _atom_site_occupancy # # R=Rmax./Rmin.=ratio of the maximum and minimum # principal axes of atomic displacement ellipsoids # # Table of coordinates # -------------------- # # atom x/a y/b z/c Ueq tmf calc att R SOF MN1 0.1406(1) 0.1346(1) 0.40039(9) 0.0254(4) aniso . . 1.61 1.0000 O1 0.3198(7) 0.1406(6) 0.2998(4) 0.0554(30) aniso . . 3.78 1.0000 O2 0.5914(10) 0.4754(7) 0.4064(5) 0.0796(37) aniso . . 3.67 1.0000 N1 -0.0027(6) 0.2157(5) 0.3434(4) 0.0247(24) aniso . . 1.52 1.0000 N2 0.1963(6) 0.2289(5) 0.4902(4) 0.0267(24) aniso . . 2.55 1.0000 N3 0.2312(7) 0.0490(5) 0.4892(4) 0.0259(26) aniso . . 1.35 1.0000 N4 0.0248(7) 0.0335(5) 0.3432(4) 0.0264(24) aniso . . 1.78 1.0000 N5 0.2396(7) 0.1407(5) 0.3403(4) 0.0294(23) aniso . . 1.74 1.0000 C1 -0.1641(9) 0.3469(7) 0.3304(7) 0.0392(35) aniso . . 2.15 1.0000 C2 -0.0410(9) 0.2971(6) 0.3733(6) 0.0308(32) aniso . . 2.31 1.0000 C3 0.0254(10) 0.3382(6) 0.4509(6) 0.0323(30) aniso . . 3.42 1.0000 C4 0.1361(9) 0.3079(6) 0.5070(6) 0.0301(31) aniso . . 5.90 1.0000 C5 0.1764(9) 0.3662(7) 0.5895(6) 0.0369(33) aniso . . 2.07 1.0000 C6 0.3153(9) 0.1989(6) 0.5415(5) 0.0294(31) aniso . . 1.85 1.0000 C7 0.4150(9) 0.2592(7) 0.5835(6) 0.0385(36) aniso . . 2.83 1.0000 C8 0.5319(10) 0.2207(8) 0.6227(7) 0.0467(40) aniso . . 1.61 1.0000 C9 0.5536(9) 0.1202(8) 0.6193(6) 0.0402(36) aniso . . 2.97 1.0000 C10 0.4569(9) 0.0603(7) 0.5791(5) 0.0318(31) aniso . . 1.81 1.0000 C11 0.3364(9) 0.0975(7) 0.5396(5) 0.0310(30) aniso . . 3.37 1.0000 C12 0.2672(10) -0.0997(7) 0.5798(6) 0.0377(33) aniso . . 3.21 1.0000 C13 0.2009(9) -0.0432(6) 0.5045(5) 0.0268(29) aniso . . 4.59 1.0000 C14 0.0978(8) -0.0880(6) 0.4502(6) 0.0270(30) aniso . . 3.22 1.0000 C15 -0.0979(9) -0.1184(6) 0.3362(6) 0.0335(31) aniso . . 2.06 1.0000 C16 0.0155(8) -0.0551(6) 0.3767(6) 0.0284(28) aniso . . 1.92 1.0000 C17 -0.0478(8) 0.0686(6) 0.2672(6) 0.0297(30) aniso . . 2.04 1.0000 C18 -0.0976(8) 0.0183(7) 0.1904(5) 0.0302(32) aniso . . 2.13 1.0000 C19 -0.1564(9) 0.0629(7) 0.1173(5) 0.0330(32) aniso . . 1.91 1.0000 C20 -0.1728(8) 0.1626(7) 0.1152(6) 0.0326(29) aniso . . 2.07 1.0000 C21 -0.1280(9) 0.2153(7) 0.1892(6) 0.0349(35) aniso . . 2.16 1.0000 C22 -0.0656(8) 0.1708(6) 0.2649(6) 0.0267(28) aniso . . 2.00 1.0000 C23 0.5457(15) 0.3934(10) 0.4420(9) 0.0800(58) aniso . . 2.87 1.0000 C24A 0.4125(21) 0.3867(15) 0.3912(14) 0.1066(96) iso . . 4.64 0.5000 C24B 0.4497(38) 0.3460(27) 0.3874(25) 0.099(11) iso . . 0.00 0.5000 C25A 0.4154(25) 0.4435(21) 0.3039(16) 0.0562(61) iso . . 0.00 0.5000 C25B 0.4345(25) 0.3841(20) 0.3076(17) 0.0597(64) iso . . 0.00 0.5000 C26 0.5234(22) 0.4814(11) 0.3209(9) 0.205(22) aniso . . 0.00 1.0000 H11 -0.20330(0) 0.31410(0) 0.27840(0) 0.0800(0) iso calc C1 1.00 1.0000 H12 -0.14690(0) 0.41250(0) 0.31790(0) 0.0800(0) iso calc C1 1.00 1.0000 H13 -0.22010(0) 0.34630(0) 0.36860(0) 0.0800(0) iso calc C1 1.00 1.0000 H3 -0.01180(0) 0.39350(0) 0.46660(0) 0.0800(0) iso calc C3 1.00 1.0000 H51 0.25260(0) 0.34010(0) 0.62450(0) 0.0800(0) iso calc C5 1.00 1.0000 H52 0.11010(0) 0.36180(0) 0.62050(0) 0.0800(0) iso calc C5 1.00 1.0000 H53 0.18800(0) 0.43200(0) 0.57640(0) 0.0800(0) iso calc C5 1.00 1.0000 H7 0.40180(0) 0.32510(0) 0.58500(0) 0.0800(0) iso calc C7 1.00 1.0000 H8 0.59620(0) 0.26110(0) 0.65170(0) 0.0800(0) iso calc C8 1.00 1.0000 H9 0.63320(0) 0.09520(0) 0.64400(0) 0.0800(0) iso calc C9 1.00 1.0000 H10 0.47130(0) -0.00560(0) 0.57830(0) 0.0800(0) iso calc C10 1.00 1.0000 H121 0.33730(0) -0.06310(0) 0.61280(0) 0.0800(0) iso calc C12 1.00 1.0000 H122 0.29860(0) -0.15870(0) 0.56120(0) 0.0800(0) iso calc C12 1.00 1.0000 H123 0.20980(0) -0.11430(0) 0.61490(0) 0.0800(0) iso calc C12 1.00 1.0000 H14 0.08110(0) -0.15020(0) 0.46600(0) 0.0800(0) iso calc C14 1.00 1.0000 H151 -0.14720(0) -0.08730(0) 0.28590(0) 0.0800(0) iso calc C15 1.00 1.0000 H152 -0.14870(0) -0.12880(0) 0.37640(0) 0.0800(0) iso calc C15 1.00 1.0000 H153 -0.06800(0) -0.17940(0) 0.32030(0) 0.0800(0) iso calc C15 1.00 1.0000 H18 -0.08800(0) -0.04820(0) 0.18990(0) 0.0800(0) iso calc C18 1.00 1.0000 H19 -0.18680(0) 0.02700(0) 0.06790(0) 0.0800(0) iso calc C19 1.00 1.0000 H20 -0.21300(0) 0.19340(0) 0.06410(0) 0.0800(0) iso calc C20 1.00 1.0000 H21 -0.14140(0) 0.28180(0) 0.18780(0) 0.0800(0) iso calc C21 1.00 1.0000 H231 0.54510(0) 0.40490(0) 0.50120(0) 0.0800(0) iso calc C23 1.00 1.0000 H232 0.60310(0) 0.33820(0) 0.44090(0) 0.0800(0) iso calc C23 1.00 1.0000 H241 0.35640(0) 0.42340(0) 0.42210(0) 0.0800(0) iso calc C24A 1.00 0.5000 H242 0.38200(0) 0.32210(0) 0.38470(0) 0.0800(0) iso calc C24A 1.00 0.5000 H243 0.44750(0) 0.27670(0) 0.38880(0) 0.0800(0) iso calc C24A 1.00 0.5000 H244 0.35980(0) 0.36200(0) 0.40450(0) 0.0800(0) iso calc C24A 1.00 0.5000 H251 0.40590(0) 0.39060(0) 0.25700(0) 0.0800(0) iso calc C25A 1.00 0.5000 H252 0.34170(0) 0.48370(0) 0.28470(0) 0.0800(0) iso calc C25A 1.00 0.5000 H253 0.34700(0) 0.39640(0) 0.27400(0) 0.0800(0) iso calc C25A 1.00 0.5000 H254 0.46870(0) 0.33620(0) 0.27160(0) 0.0800(0) iso calc C25B 1.00 0.5000 H261 0.49070(0) 0.54560(0) 0.30820(0) 0.0800(0) iso calc C25A 1.00 1.0000 H262 0.57920(0) 0.46690(0) 0.28300(0) 0.0800(0) iso calc C26 1.00 1.0000 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 #label U11 U22 U33 U23 U13 U12 MN1 0.0282(8) 0.0259(7) 0.0247(7) 0.0007(6) 0.0114(5) -0.0011(7) O1 0.0529(46) 0.0741(54) 0.0508(43) -0.0072(41) 0.0351(38) -0.0095(43) O2 0.0993(74) 0.0890(69) 0.0553(55) -0.0059(49) 0.0277(51) -0.0498(60) N1 0.0237(39) 0.0264(37) 0.0241(37) -0.0043(29) 0.0055(31) 0.0014(32) N2 0.0211(38) 0.0323(40) 0.0269(39) 0.0018(31) 0.0064(31) -0.0092(33) N3 0.0265(41) 0.0237(36) 0.0289(39) -0.0019(30) 0.0096(33) -0.0011(32) N4 0.0294(41) 0.0210(35) 0.0290(40) 0.0027(29) 0.0071(33) 0.0055(32) N5 0.0339(42) 0.0321(39) 0.0222(34) -0.0049(32) 0.0064(32) -0.0001(36) C1 0.0335(55) 0.0309(52) 0.0533(61) 0.0037(44) 0.0105(47) 0.0069(44) C2 0.0321(51) 0.0283(44) 0.0361(51) 0.0066(38) 0.0163(41) 0.0093(41) C3 0.0547(63) 0.0166(42) 0.0303(47) -0.0013(35) 0.0196(46) -0.0002(42) C4 0.0331(52) 0.0305(48) 0.0353(50) -0.0003(39) 0.0250(43) -0.0107(42) C5 0.0454(58) 0.0335(48) 0.0329(48) -0.0087(42) 0.0117(44) -0.0080(47) C6 0.0356(54) 0.0307(48) 0.0251(46) -0.0014(37) 0.0133(41) -0.0011(42) C7 0.0335(54) 0.0505(60) 0.0361(53) -0.0012(45) 0.0172(44) -0.0117(49) C8 0.0466(67) 0.0563(68) 0.0396(59) -0.0028(50) 0.0148(51) -0.0031(56) C9 0.0283(52) 0.0662(71) 0.0286(46) 0.0033(49) 0.0114(41) 0.0037(51) C10 0.0294(51) 0.0417(52) 0.0238(45) 0.0014(40) 0.0055(39) -0.0029(44) C11 0.0301(52) 0.0446(54) 0.0227(43) 0.0061(38) 0.0146(39) 0.0080(44) C12 0.0530(66) 0.0300(47) 0.0285(49) 0.0109(39) 0.0067(47) 0.0093(47) C13 0.0441(55) 0.0241(43) 0.0139(40) 0.0058(32) 0.0104(38) -0.0001(41) C14 0.0272(49) 0.0200(41) 0.0397(51) 0.0054(37) 0.0193(42) -0.0007(38) C15 0.0319(53) 0.0315(51) 0.0396(52) -0.0043(40) 0.0134(43) -0.0091(42) C16 0.0266(48) 0.0298(46) 0.0315(49) -0.0075(38) 0.0121(39) -0.0026(40) C17 0.0313(52) 0.0217(43) 0.0389(53) -0.0039(38) 0.0142(44) -0.0033(38) C18 0.0229(48) 0.0405(51) 0.0270(46) -0.0035(40) 0.0057(38) -0.0071(42) C19 0.0346(55) 0.0407(53) 0.0251(49) 0.0019(40) 0.0098(41) -0.0044(45) C20 0.0232(48) 0.0421(55) 0.0295(49) 0.0029(39) 0.0007(37) 0.0013(41) C21 0.0380(55) 0.0379(52) 0.0340(52) 0.0011(41) 0.0187(44) 0.0059(45) C22 0.0182(44) 0.0282(44) 0.0345(49) -0.0007(38) 0.0080(37) -0.0004(37) C23 0.079(10) 0.081(10) 0.072(9) 0.024(8) 0.004(8) -0.028(8) C26 0.205(22) 0.066(10) 0.054(9) 0.003(7) 0.040(11) -0.025(12) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag MN1 N1 1.964(6) yes MN1 N2 1.934(7) yes MN1 N3 1.935(7) yes MN1 N4 1.962(7) yes MN1 N5 1.612(8) yes O1 N5 1.21(1) yes O2 C23 1.42(1) yes O2 C26 1.40(1) yes N1 C2 1.33(1) yes N1 C22 1.43(1) yes N2 C4 1.34(1) yes N2 C6 1.42(1) yes N3 C11 1.41(1) yes N3 C13 1.36(1) yes N4 C16 1.36(1) yes N4 C17 1.37(1) yes C1 C2 1.52(1) yes C2 C3 1.40(1) yes C3 C4 1.39(1) yes C4 C5 1.52(1) yes C6 C7 1.41(1) yes C6 C11 1.43(1) yes C7 C8 1.38(1) yes C8 C9 1.42(1) yes C9 C10 1.38(1) yes C10 C11 1.41(1) yes C12 C13 1.48(1) yes C13 C14 1.39(1) yes C14 C16 1.38(1) yes C15 C16 1.53(1) yes C17 C18 1.41(1) yes C17 C22 1.43(1) yes C18 C19 1.35(1) yes C19 C20 1.40(1) yes C20 C21 1.38(1) yes C21 C22 1.39(1) yes C23 C24A 1.49(2) yes C23 C24B 1.36(3) yes C24A C24B 0.71(4) yes C24A C25A 1.62(3) yes C24A C25B 1.42(3) yes C24B C25A 1.88(4) yes C24B C25B 1.36(4) yes C25A C25B 0.85(4) yes C25A C26 1.26(3) yes C25B C26 1.65(3) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag N4 MN1 N5 101.8(3) yes N3 MN1 N5 100.2(3) yes N3 MN1 N4 93.6(3) yes N2 MN1 N5 106.0(3) yes N2 MN1 N4 152.2(3) yes N2 MN1 N3 81.6(3) yes N1 MN1 N5 105.2(3) yes N1 MN1 N4 80.9(3) yes N1 MN1 N3 154.6(3) yes N1 MN1 N2 91.8(3) yes C23 O2 C26 107(1) yes MN1 N1 C22 108.7(5) yes MN1 N1 C2 126.9(6) yes C2 N1 C22 124.3(7) yes MN1 N2 C6 108.2(5) yes MN1 N2 C4 128.6(6) yes C4 N2 C6 123.1(7) yes MN1 N3 C13 127.5(6) yes MN1 N3 C11 109.3(6) yes C11 N3 C13 123.2(7) yes MN1 N4 C17 109.3(5) yes MN1 N4 C16 124.3(6) yes C16 N4 C17 126.3(8) yes MN1 N5 O1 174.9(6) yes N1 C2 C1 122.8(8) yes C1 C2 C3 115.4(8) yes N1 C2 C3 121.7(8) yes C2 C3 C4 129.5(8) yes N2 C4 C3 120.7(8) yes C3 C4 C5 115.3(8) yes N2 C4 C5 123.9(8) yes N2 C6 C11 113.9(8) yes N2 C6 C7 126.5(8) yes C7 C6 C11 119.1(8) yes C6 C7 C8 120.5(9) yes C7 C8 C9 120(1) yes C8 C9 C10 120(1) yes C9 C10 C11 121.0(9) yes C6 C11 C10 119.2(9) yes N3 C11 C10 128.7(8) yes N3 C11 C6 111.8(8) yes N3 C13 C12 123.8(8) yes C12 C13 C14 116.0(8) yes N3 C13 C14 120.1(8) yes C13 C14 C16 130.5(8) yes C14 C16 C15 117.8(8) yes N4 C16 C15 118.9(8) yes N4 C16 C14 123.1(8) yes N4 C17 C22 114.8(8) yes N4 C17 C18 128.4(8) yes C18 C17 C22 116.6(8) yes C17 C18 C19 122.6(9) yes C18 C19 C20 120.6(8) yes C19 C20 C21 119.2(9) yes C20 C21 C22 121.0(9) yes C17 C22 C21 119.9(8) yes N1 C22 C21 127.6(8) yes N1 C22 C17 112.2(8) yes O2 C23 C24B 115(2) yes O2 C23 C24A 103(1) yes C24A C23 C24B 28(2) yes C23 C24A C25B 99(2) yes C23 C24A C25A 103(2) yes C23 C24A C24B 66(4) yes C25A C24A C25B 32(2) yes C24B C24A C25B 71(4) yes C24B C24A C25A 101(4) yes C23 C24B C24A 86(4) yes C24A C24B C25B 80(4) yes C24A C24B C25A 58(3) yes C23 C24B C25B 109(3) yes C23 C24B C25A 96(2) yes C25A C24B C25B 24(2) yes C24A C25A C24B 22(1) yes C24B C25A C26 98(2) yes C24B C25A C25B 41(2) yes C24A C25A C26 103(2) yes C24A C25A C25B 61(2) yes C25B C25A C26 101(3) yes C24B C25B C25A 115(3) yes C24A C25B C25A 87(3) yes C24A C25B C24B 29(2) yes C25A C25B C26 49(2) yes C24B C25B C26 105(2) yes C24A C25B C26 95(2) yes C25A C26 C25B 30(2) yes O2 C26 C25B 104(1) yes O2 C26 C25A 116(2) yes _refine_diff_density_max 0.779 _refine_diff_density_min -0.682 _refine_diff_density_rms 0.128 #===END ######################################################################## ###### #### Complex 8 Crystallographic Data data_COMPLEX_8 _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C60H82Mn2N8Na2O5' _chemical_formula_weight 1151.21 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Mn' 'Mn' 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.0362 0.0249 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P21/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 10.593(3) _cell_length_b 19.228(5) _cell_length_c 15.663(5) _cell_angle_alpha 90.00(0) _cell_angle_beta 107.71(3) _cell_angle_gamma 90.00(0) _cell_volume 3039.(2) _cell_formula_units_Z 2.00 _cell_measurement_temperature 25 _cell_measurement_reflns_used 143 _cell_measurement_theta_min 20.2 _cell_measurement_theta_max 27.2 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.2580 _exptl_crystal_density_method not_measured _exptl_crystal_F_000 1220.0 _exptl_absorpt_coefficient_mu 0.4624 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min 0.933 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 143 _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focussealedtube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku AFC6S' _diffrn_measurement_method 'omega/2theta' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.8 _diffrn_reflns_number 7343 _diffrn_reflns_av_R_equivalents 0.0847 _diffrn_reflns_av_sigmaI/netI 0.2441 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 27.51 _reflns_number_total 6977 _reflns_number_observed 2119 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'TEXSAN Software' _computing_cell_refinement 'TEXSAN Software' _computing_data_reduction 'TEXSAN Software' _computing_structure_solution 'SHELXS-76 (Sheldrick, 1976)' _computing_structure_refinement 'SHELXS-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1819 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses of fit S are based on F^2^, conventional R- factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R factor obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1069P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment not_refined _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5158 _refine_ls_number_parameters 342 _refine_ls_number_restraints 39 _refine_ls_R_factor_all 0.2783 _refine_ls_R_factor_obs 0.0641 _refine_ls_wR_factor_all 0.2877 _refine_ls_wR_factor_obs 0.1598 _refine_ls_goodness_of_fit_all 0.955 _refine_ls_goodness_of_fit_obs 1.199 _refine_ls_restrained_S_all 1.157 _refine_ls_restrained_S_obs 1.201 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_aniso_ratio _atom_site_occupancy # # R=Rmax./Rmin.=ratio of the maximum and minimum # principal axes of atomic displacement ellipsoids # # Table of coordinates # -------------------- # # atom x/a y/b z/c Ueq tmf calc att R SOF MN1 0.10638(9) 0.06892(5) 0.43591(6) 0.0341(3) aniso . . 1.33 1.0000 NA1 -0.0913(3) 0.1180(2) 0.2636(2) 0.0608(12) aniso . . 2.52 1.0000 O1 0.0034(6) 0.1044(3) 0.1476(3) 0.0734(23) aniso . . 1.89 1.0000 O2 -0.1802(10) 0.2260(6) 0.2110(7) 0.0353(19) iso . . 1.48 0.5000 O3 -0.3377(9) 0.1170(5) 0.1990(7) 0.0383(20) iso . . 1.42 0.5000 O4 -0.2643(10) 0.1822(5) 0.2005(7) 0.0411(22) iso . . 1.65 0.5000 N1 -0.0677(5) 0.0147(2) 0.3663(3) 0.0361(18) aniso . . 1.55 1.0000 N2 -0.0186(5) 0.1544(3) 0.4274(3) 0.0399(23) aniso . . 2.23 1.0000 N3 0.2131(5) 0.1509(3) 0.3979(3) 0.0399(24) aniso . . 2.23 1.0000 N4 0.1667(4) 0.0096(3) 0.3420(3) 0.0365(23) aniso . . 1.87 1.0000 C1 -0.2334(6) -0.0449(3) 0.4249(4) 0.0401(22) aniso . . 2.13 1.0000 C2 -0.1637(6) 0.0132(3) 0.4098(4) 0.0527(29) aniso . . 1.74 1.0000 C3 -0.1807(6) 0.0774(4) 0.4559(4) 0.0386(23) aniso . . 2.11 1.0000 C4 -0.1197(6) 0.1413(3) 0.4641(4) 0.0499(29) aniso . . 1.25 1.0000 C5 -0.1564(6) 0.1923(4) 0.5259(5) 0.0581(32) aniso . . 2.74 1.0000 C6 0.0335(6) 0.2191(3) 0.4180(4) 0.0566(32) aniso . . 2.08 1.0000 C7 -0.0286(7) 0.2828(4) 0.4157(4) 0.0471(28) aniso . . 2.24 1.0000 C8 0.0273(8) 0.3444(4) 0.3980(5) 0.0358(22) aniso . . 1.60 1.0000 C9 0.1469(8) 0.3431(4) 0.3812(5) 0.0574(28) aniso . . 1.71 1.0000 C10 0.2102(7) 0.2806(4) 0.3799(4) 0.0412(26) aniso . . 2.33 1.0000 C11 0.1596(6) 0.2184(3) 0.4011(4) 0.0410(23) aniso . . 1.65 1.0000 C12 0.4529(7) 0.1869(4) 0.4363(5) 0.0413(24) aniso . . 1.98 1.0000 C13 0.3386(6) 0.1352(4) 0.4050(4) 0.0453(24) aniso . . 1.81 1.0000 C14 0.3763(6) 0.0676(4) 0.3911(4) 0.0401(23) aniso . . 1.53 1.0000 C15 0.3000(6) 0.0071(4) 0.3584(4) 0.0473(28) aniso . . 1.78 1.0000 C16 0.3740(6) -0.0579(4) 0.3488(4) 0.0551(29) aniso . . 2.30 1.0000 C17 0.0755(6) -0.0401(3) 0.2945(4) 0.0509(25) aniso . . 2.34 1.0000 C18 0.0946(6) -0.0829(4) 0.2287(4) 0.0455(28) aniso . . 1.37 1.0000 C19 -0.0073(7) -0.1271(4) 0.1781(5) 0.0355(22) aniso . . 1.68 1.0000 C20 -0.1272(7) -0.1260(4) 0.1938(5) 0.1340(63) aniso . . 4.48 1.0000 C21 -0.1504(6) -0.0815(3) 0.2562(4) 0.0955(51) aniso . . 2.12 1.0000 C22 -0.0512(6) -0.0374(3) 0.3096(4) 0.0964(44) aniso . . 2.44 1.0000 C23 0.1785(10) 0.1626(7) 0.1069(8) 0.0761(41) aniso . . 2.34 1.0000 C24 0.1440(10) 0.1158(6) 0.1648(6) 0.0873(41) aniso . . 2.02 1.0000 C25 -0.0525(11) 0.0663(6) 0.0685(6) 0.1209(81) aniso . . 0.00 1.0000 C26 -0.1833(10) 0.0428(4) 0.0639(5) 0.1064(73) aniso . . 0.00 1.0000 C27 -0.1066(9) 0.2697(5) 0.1704(6) 0.0948(68) aniso . . 0.00 1.0000 C28A -0.3157(13) 0.2284(9) 0.1504(10) 0.0667(44) iso . . 0.00 0.5000 C29A -0.3846(26) 0.1874(8) 0.2078(18) 0.145(12) iso . . 0.00 0.5000 C30A -0.4312(17) 0.0638(9) 0.2108(13) 0.0924(62) iso . . 0.00 0.5000 C28B -0.2528(12) 0.2465(7) 0.1518(10) 0.0599(41) iso . . 0.00 0.5000 C29B -0.4055(12) 0.1693(8) 0.1800(12) 0.0672(52) iso . . 0.00 0.5000 C30B -0.4113(13) 0.1010(7) 0.2294(9) 0.0430(0) iso . . 0.00 0.5000 H11 -0.23560(0) -0.08250(0) 0.38280(0) 0.0800(0) iso calc C1 1.00 1.0000 H12 -0.32530(0) -0.03370(0) 0.42230(0) 0.0800(0) iso calc C1 1.00 1.0000 H3 -0.24630(0) 0.07370(0) 0.48510(0) 0.0800(0) iso calc C3 1.00 1.0000 H51 -0.10960(0) 0.23540(0) 0.52720(0) 0.0800(0) iso calc C5 1.00 1.0000 H52 -0.13520(0) 0.17380(0) 0.58530(0) 0.0800(0) iso calc C5 1.00 1.0000 H53 -0.25080(0) 0.20170(0) 0.50410(0) 0.0800(0) iso calc C5 1.00 1.0000 H7 -0.11240(0) 0.28400(0) 0.42690(0) 0.0800(0) iso calc C7 1.00 1.0000 H8 -0.01570(0) 0.38750(0) 0.39980(0) 0.0800(0) iso calc C8 1.00 1.0000 H9 0.18740(0) 0.38520(0) 0.36990(0) 0.0800(0) iso calc C9 1.00 1.0000 H10 0.29090(0) 0.27950(0) 0.36530(0) 0.0800(0) iso calc C10 1.00 1.0000 H121 0.42140(0) 0.23290(0) 0.44460(0) 0.0800(0) iso calc C12 1.00 1.0000 H122 0.50050(0) 0.19100(0) 0.39170(0) 0.0800(0) iso calc C12 1.00 1.0000 H123 0.51690(0) 0.17270(0) 0.49200(0) 0.0800(0) iso calc C12 1.00 1.0000 H14 0.46820(0) 0.06030(0) 0.40530(0) 0.0800(0) iso calc C14 1.00 1.0000 H161 0.31390(0) -0.09580(0) 0.32700(0) 0.0800(0) iso calc C16 1.00 1.0000 H162 0.43560(0) -0.07090(0) 0.40620(0) 0.0800(0) iso calc C16 1.00 1.0000 H163 0.42380(0) -0.04950(0) 0.30750(0) 0.0800(0) iso calc C16 1.00 1.0000 H18 0.17650(0) -0.08200(0) 0.21530(0) 0.0800(0) iso calc C18 1.00 1.0000 H19 0.00840(0) -0.15690(0) 0.13470(0) 0.0800(0) iso calc C19 1.00 1.0000 H20 -0.19540(0) -0.15540(0) 0.16140(0) 0.0800(0) iso calc C20 1.00 1.0000 H21 -0.23540(0) -0.08030(0) 0.26390(0) 0.0800(0) iso calc C21 1.00 1.0000 H231 0.27180(0) 0.17070(0) 0.11910(0) 0.0800(0) iso calc C23 1.00 1.0000 H232 0.13930(0) 0.20990(0) 0.11180(0) 0.0800(0) iso calc C23 1.00 1.0000 H233 0.14140(0) 0.15030(0) 0.04390(0) 0.0800(0) iso calc C23 1.00 1.0000 H241 0.18730(0) 0.07080(0) 0.15880(0) 0.0800(0) iso calc C24 1.00 1.0000 H242 0.18520(0) 0.13040(0) 0.22660(0) 0.0800(0) iso calc C24 1.00 1.0000 H251 0.00140(0) 0.02520(0) 0.06400(0) 0.0800(0) iso calc C25 1.00 1.0000 H252 -0.05910(0) 0.09400(0) 0.01390(0) 0.0800(0) iso calc C25 1.00 1.0000 H261 -0.22480(0) 0.01600(0) 0.00930(0) 0.0800(0) iso calc C26 1.00 1.0000 H262 -0.24030(0) 0.08190(0) 0.06430(0) 0.0800(0) iso calc C26 1.00 1.0000 H263 -0.18000(0) 0.01320(0) 0.11430(0) 0.0800(0) iso calc C26 1.00 1.0000 H271 -0.01740(0) 0.27530(0) 0.20640(0) 0.0800(0) iso calc C27 1.00 1.0000 H272 -0.14780(0) 0.31590(0) 0.15760(0) 0.0800(0) iso calc C27 1.00 1.0000 H273 -0.10710(0) 0.25060(0) 0.11200(0) 0.0800(0) iso calc C27 1.00 1.0000 H281 -0.30620(0) 0.20610(0) 0.08520(0) 0.0800(0) iso calc C28A 1.00 0.5000 H282 -0.34220(0) 0.27600(0) 0.12670(0) 0.0800(0) iso calc C28A 1.00 0.5000 H283 -0.29670(0) 0.28460(0) 0.17610(0) 0.0800(0) iso calc C28A 1.00 0.5000 H284 -0.29570(0) 0.24310(0) 0.09050(0) 0.0800(0) iso calc C28A 1.00 0.5000 H291 -0.37140(0) 0.20660(0) 0.25040(0) 0.0800(0) iso calc C29A 1.00 0.5000 H292 -0.48050(0) 0.18940(0) 0.15960(0) 0.0800(0) iso calc C29A 1.00 0.5000 H293 -0.45550(0) 0.16100(0) 0.11540(0) 0.0800(0) iso calc C29A 1.00 0.5000 H294 -0.45700(0) 0.19390(0) 0.20720(0) 0.0800(0) iso calc C29A 1.00 0.5000 H301 -0.41110(0) 0.02260(0) 0.23250(0) 0.0800(0) iso calc C30A 1.00 0.5000 H302 -0.52540(0) 0.07380(0) 0.18340(0) 0.0800(0) iso calc C30A 1.00 0.5000 H303 -0.44490(0) 0.08620(0) 0.28420(0) 0.0800(0) iso calc C30A 1.00 0.5000 H304 -0.49970(0) 0.07270(0) 0.20850(0) 0.0800(0) iso calc C30A 1.00 0.5000 H305 -0.36590(0) 0.08970(0) 0.28240(0) 0.0800(0) iso calc O3 1.00 0.5000 H306 -0.36440(0) 0.05700(0) 0.19110(0) 0.0800(0) iso calc O3 1.00 0.5000 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 #label U11 U22 U33 U23 U13 U12 MN1 0.0297(4) 0.0343(5) 0.0386(5) -0.0001(5) 0.0110(4) -0.0009(5) NA1 0.0900(21) 0.0509(18) 0.0414(15) 0.0076(13) 0.0198(15) 0.0109(16) O1 0.0844(41) 0.0841(43) 0.0520(32) 0.0018(29) 0.0210(30) 0.0120(33) N1 0.0412(29) 0.0295(29) 0.0374(28) 0.0012(23) 0.0152(23) 0.0026(23) N2 0.0333(28) 0.0411(34) 0.0401(29) 0.0047(25) 0.0104(23) -0.0013(24) N3 0.0386(31) 0.0484(36) 0.0389(29) -0.0074(26) 0.0154(25) -0.0019(26) N4 0.0288(26) 0.0419(32) 0.0356(27) -0.0026(25) 0.0065(22) -0.0022(23) C1 0.0296(32) 0.0373(38) 0.0519(39) 0.0027(29) 0.0108(29) -0.0073(27) C1' 0.0296(32) 0.0373(38) 0.0519(39) 0.0027(29) 0.0108(29) -0.0073(27) C2 0.0297(31) 0.0429(39) 0.0336(33) 0.0041(30) 0.0044(27) 0.0070(29) C3 0.0336(32) 0.0433(42) 0.0460(35) 0.0096(33) 0.0161(28) 0.0107(32) C4 0.0348(34) 0.0332(38) 0.0447(36) -0.0007(30) 0.0145(30) 0.0039(28) C5 0.0433(39) 0.0548(47) 0.0641(46) -0.0053(39) 0.0227(35) 0.0000(36) C6 0.0532(39) 0.0285(35) 0.0323(32) 0.0040(28) 0.0107(29) 0.0023(31) C7 0.0514(41) 0.0471(45) 0.0500(42) 0.0047(35) 0.0137(34) 0.0016(35) C8 0.0781(55) 0.0343(41) 0.0643(48) 0.0137(36) 0.0250(43) 0.0056(38) C9 0.0706(51) 0.0431(46) 0.0605(47) 0.0044(36) 0.0265(41) -0.0099(39) C10 0.0585(43) 0.0382(41) 0.0501(41) 0.0050(33) 0.0245(35) -0.0092(35) C11 0.0441(36) 0.0335(36) 0.0319(32) -0.0018(28) 0.0146(28) -0.0061(30) C12 0.0535(43) 0.0558(49) 0.0609(46) 0.0009(38) 0.0143(37) -0.0128(38) C13 0.0430(39) 0.0534(47) 0.0312(33) 0.0004(32) 0.0171(30) -0.0087(34) C14 0.0370(32) 0.0491(40) 0.0392(33) -0.0045(36) 0.0151(27) -0.0067(36) C15 0.0470(38) 0.0503(43) 0.0288(32) -0.0017(30) 0.0149(29) 0.0025(34) C16 0.0344(33) 0.0480(48) 0.0537(39) -0.0029(34) 0.0136(30) 0.0058(31) C17 0.0433(37) 0.0401(38) 0.0336(33) 0.0013(30) 0.0067(29) 0.0040(31) C18 0.0391(35) 0.0546(50) 0.0446(37) -0.0102(34) 0.0072(30) 0.0014(32) C19 0.0548(45) 0.0525(47) 0.0547(43) -0.0194(37) 0.0118(36) 0.0020(38) C20 0.0452(40) 0.0468(44) 0.0553(43) -0.0148(36) 0.0073(34) -0.0116(35) C21 0.0443(37) 0.0417(45) 0.0494(38) -0.0018(32) 0.0127(32) -0.0058(32) C22 0.0340(33) 0.0283(33) 0.0413(35) -0.0015(28) 0.0070(28) -0.0025(28) C24 0.0852(69) 0.1248(93) 0.0760(65) 0.0259(60) 0.0238(55) 0.0143(65) C25 0.1209(81) 0.1090(84) 0.0622(57) -0.0162(60) 0.0321(58) 0.0078(74) C26 0.1064(73) 0.0631(58) 0.0505(48) -0.0028(40) 0.0115(48) -0.0059(52) C27 0.0948(68) 0.0881(74) 0.0854(63) 0.0223(53) 0.0368(55) 0.0271(55) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag MN1 NA1 3.020(3) yes MN1 N1 2.110(5) yes MN1 N2 2.089(6) yes MN1 N3 2.128(6) yes MN1 N4 2.108(5) yes MN1 C1' 2.234(6) yes NA1 O1 2.342(7) yes NA1 O2 2.33(1) yes NA1 O3 2.50(0) yes NA1 O4 2.18(1) yes NA1 N1 2.520(6) yes NA1 N2 2.542(6) yes O1 C24 1.45(1) yes O1 C25 1.41(1) yes O2 O4 1.20(1) yes O2 C27 1.42(1) yes O2 C28A 1.46(1) yes O2 C28B 1.08(1) yes O3 O4 1.47(1) yes O3 C29A 1.46(2) yes O3 C30A 1.47(2) yes O3 C29B 1.22(1) yes O3 C30B 1.07(1) yes O4 C28A 1.20(1) yes O4 C29A 1.32(3) yes O4 C28B 1.48(1) yes O4 C29B 1.45(1) yes N1 C2 1.386(9) yes N1 C22 1.385(8) yes N2 C4 1.384(9) yes N2 C6 1.387(8) yes N3 C11 1.423(8) yes N3 C13 1.334(9) yes N4 C15 1.357(8) yes N4 C17 1.401(7) yes C1 C2 1.398(9) yes C2 C3 1.47(1) yes C3 C4 1.38(1) yes C4 C5 1.51(1) yes C6 C7 1.39(1) yes C6 C11 1.44(1) yes C7 C8 1.39(1) yes C8 C9 1.37(1) yes C9 C10 1.38(1) yes C10 C11 1.39(1) yes C12 C13 1.53(1) yes C13 C14 1.40(1) yes C14 C15 1.42(1) yes C15 C16 1.51(1) yes C17 C18 1.38(1) yes C17 C22 1.43(1) yes C18 C19 1.41(0) yes C19 C20 1.37(1) yes C20 C21 1.38(1) yes C21 C22 1.410(8) yes C23 C24 1.40(1) yes C25 C26 1.44(1) yes C27 C28B 1.55(1) yes C28A C29A 1.54(3) yes C28A C28B 0.75(2) yes C28A C29B 1.64(2) yes C29A C29B 0.55(2) yes C29A C30B 1.74(2) yes C30A C30B 0.78(2) yes C29B C30B 1.53(2) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag N4 MN1 C1' 110.4(2) yes N3 MN1 C1' 102.3(2) yes N3 MN1 N4 84.6(2) yes N2 MN1 C1' 114.0(2) yes N2 MN1 N4 134.6(2) yes N2 MN1 N3 77.3(2) yes N1 MN1 C1' 125.1(2) yes N1 MN1 N4 77.0(2) yes N1 MN1 N3 132.6(2) yes N1 MN1 N2 85.3(2) yes NA1 MN1 C1' 169.9(2) yes NA1 MN1 N4 79.7(1) yes NA1 MN1 N3 78.6(2) yes NA1 MN1 N2 56.2(2) yes NA1 MN1 N1 55.5(2) yes MN1 NA1 N2 43.1(1) yes MN1 NA1 N1 43.6(1) yes MN1 NA1 O4 147.2(3) yes MN1 NA1 O3 135.6(3) yes MN1 NA1 O2 133.8(3) yes MN1 NA1 O1 108.3(2) yes N1 NA1 N2 68.4(2) yes O4 NA1 N2 104.8(3) yes O4 NA1 N1 129.9(3) yes O3 NA1 N2 111.7(3) yes O3 NA1 N1 98.1(3) yes O3 NA1 O4 35.9(4) yes O2 NA1 N2 94.4(3) yes O2 NA1 N1 151.8(3) yes O2 NA1 O4 30.7(4) yes O2 NA1 O3 66.6(4) yes O1 NA1 N2 138.1(2) yes O1 NA1 N1 115.1(2) yes O1 NA1 O4 102.2(3) yes O1 NA1 O3 109.1(3) yes O1 NA1 O2 92.7(3) yes NA1 O1 C25 125.2(6) yes NA1 O1 C24 119.9(4) yes C24 O1 C25 112.1(7) yes NA1 O2 C28B 137(1) yes NA1 O2 C28A 118.1(9) yes NA1 O2 C27 117.9(8) yes NA1 O2 O4 68.0(7) yes C28A O2 C28B 30(1) yes C27 O2 C28B 75(1) yes C27 O2 C28A 105(1) yes O4 O2 C28B 80(1) yes O4 O2 C28A 52.5(9) yes O4 O2 C27 147(1) yes NA1 O3 C30B 129(1) yes NA1 O3 C29B 123.9(9) yes NA1 O3 C30A 127.9(9) yes NA1 O3 C29A 107.3(9) yes NA1 O3 O4 60.3(6) yes C29B O3 C30B 84(1) yes C30A O3 C30B 31(1) yes C30A O3 C29B 104(1) yes C29A O3 C30B 85(1) yes C29A O3 C29B 21(1) yes C29A O3 C30A 112(1) yes O4 O3 C30B 133(1) yes O4 O3 C29B 64.6(9) yes O4 O3 C30A 164(1) yes O4 O3 C29A 53.3(8) yes O2 O4 O3 165(1) yes NA1 O4 O3 83.8(6) yes NA1 O4 O2 81.3(8) yes O3 O4 C29B 49.3(8) yes O3 O4 C28B 146(1) yes O3 O4 C29A 63(1) yes O3 O4 C28A 119(1) yes O2 O4 C29B 145(1) yes O2 O4 C28B 46.3(8) yes O2 O4 C29A 129(1) yes O2 O4 C28A 75(1) yes NA1 O4 C29B 132.1(9) yes NA1 O4 C28B 121.2(8) yes NA1 O4 C29A 135(1) yes NA1 O4 C28A 150(1) yes C28B O4 C29B 106(1) yes C29A O4 C29B 22(1) yes C29A O4 C28B 102(1) yes C28A O4 C29B 76(1) yes C28A O4 C28B 30.2(9) yes C28A O4 C29A 75(1) yes MN1 N1 NA1 80.9(2) yes NA1 N1 C22 99.7(3) yes NA1 N1 C2 112.7(3) yes MN1 N1 C22 115.3(4) yes MN1 N1 C2 114.4(4) yes C2 N1 C22 123.7(5) yes MN1 N2 NA1 80.8(2) yes NA1 N2 C6 98.5(3) yes NA1 N2 C4 109.5(4) yes MN1 N2 C6 116.6(4) yes MN1 N2 C4 112.7(4) yes C4 N2 C6 126.2(5) yes MN1 N3 C13 114.2(5) yes MN1 N3 C11 114.5(4) yes C11 N3 C13 126.9(6) yes MN1 N4 C17 115.7(4) yes MN1 N4 C15 113.9(4) yes C15 N4 C17 125.9(5) yes N1 C2 C1 127.2(5) yes C1 C2 C3 116.0(6) yes N1 C2 C3 116.3(6) yes C2 C3 C4 132.2(6) yes N2 C4 C3 121.6(6) yes C3 C4 C5 115.8(6) yes N2 C4 C5 122.1(6) yes N2 C6 C11 115.7(5) yes N2 C6 C7 126.5(6) yes C7 C6 C11 117.6(6) yes C6 C7 C8 122.1(7) yes C7 C8 C9 119.9(7) yes C8 C9 C10 120.1(8) yes C9 C10 C11 121.4(7) yes C6 C11 C10 118.8(6) yes N3 C11 C10 126.1(6) yes N3 C11 C6 114.6(5) yes N3 C13 C12 123.5(6) yes C12 C13 C14 114.8(6) yes N3 C13 C14 121.5(6) yes C13 C14 C15 131.3(6) yes N4 C15 C14 119.0(6) yes C14 C15 C16 117.3(6) yes N4 C15 C16 123.6(6) yes N4 C17 C22 114.6(5) yes N4 C17 C18 124.7(6) yes C18 C17 C22 120.1(6) yes C17 C18 C19 121.1(6) yes C18 C19 C20 118.9(7) yes C19 C20 C21 121.0(7) yes C20 C21 C22 122.2(6) yes C17 C22 C21 116.5(6) yes N1 C22 C21 126.8(6) yes N1 C22 C17 116.1(5) yes O1 C24 C23 115.6(9) yes O1 C25 C26 110.4(8) yes O2 C27 C28B 42.4(7) yes O2 C28A O4 52.5(9) yes O4 C28A C29B 59(1) yes O4 C28A C28B 96(2) yes O4 C28A C29A 56(1) yes O2 C28A C29B 110(1) yes O2 C28A C28B 46(1) yes O2 C28A C29A 99(1) yes C28B C28A C29B 155(2) yes C29A C28A C29B 19.6(9) yes C29A C28A C28B 143(2) yes O4 C29A C28A 49(1) yes O3 C29A C28A 101(1) yes O3 C29A O4 63.7(9) yes C28A C29A C30B 138(2) yes C28A C29A C29B 91(3) yes O4 C29A C30B 99(2) yes O4 C29A C29B 93(4) yes O3 C29A C30B 38.1(9) yes O3 C29A C29B 53(2) yes C29B C29A C30B 60(3) yes O3 C30A C30B 45(2) yes C27 C28B C28A 166(2) yes O4 C28B C28A 54(2) yes O4 C28B C27 112(1) yes O2 C28B C28A 105(2) yes O2 C28B C27 62(1) yes O2 C28B O4 53.3(9) yes C28A C29B C29A 70(3) yes O4 C29B C29A 65(3) yes O4 C29B C28A 45.3(8) yes O3 C29B C29A 105(3) yes O3 C29B C28A 107(1) yes O3 C29B O4 66(1) yes C29A C29B C30B 102(3) yes C28A C29B C30B 148(1) yes O4 C29B C30B 103(1) yes O3 C29B C30B 44.1(8) yes C30A C30B C29B 130(2) yes C29A C30B C29B 18(1) yes C29A C30B C30A 148(2) yes O3 C30B C29B 52(1) yes O3 C30B C30A 104(2) yes O3 C30B C29A 57(1) yes _refine_diff_density_max 0.431 _refine_diff_density_min -0.732 _refine_diff_density_rms 0.083 #===END ######################################################################## ###### #### Complex 9 Crystallographic Data data_COMPLEX_9 _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C68H92Mn2N8Na4O6' _chemical_formula_weight 1319.36 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Mn' 'Mn' 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.0362 0.0249 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _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 14.640(3) _cell_length_b 15.823(3) _cell_length_c 16.375(3) _cell_angle_alpha 97.72(3) _cell_angle_beta 102.28(3) _cell_angle_gamma 101.94(3) _cell_volume 3563.(1) _cell_formula_units_Z 2.00 _cell_measurement_temperature 25 _cell_measurement_reflns_used 223 _cell_measurement_theta_min 30.5 _cell_measurement_theta_max 40.1 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.2299 _exptl_crystal_density_method not_measured _exptl_crystal_F_000 1396.0 _exptl_absorpt_coefficient_mu 0.4139 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min 0.965 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 223 _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focussealedtube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'MAR345 Imaging Plate' _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21769 _diffrn_reflns_av_R_equivalents 0.0535 _diffrn_reflns_av_sigmaI/netI 0.0916 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 27.45 _reflns_number_total 11988 _reflns_number_observed 7849 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'DENZO/HKL Software' _computing_cell_refinement 'DENZO/HKL Software' _computing_data_reduction 'DENZO/HKL Software' _computing_structure_solution 'SHELXS-76 (Sheldrick, 1976)' _computing_structure_refinement 'SHELXS-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 914 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses of fit S are based on F^2^, conventional R- factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R factor obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+( 0.1647)^2^+ 2.03P] 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 not_refined _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7849 _refine_ls_number_parameters 788 _refine_ls_number_restraints 101 _refine_ls_R_factor_all 0.1895 _refine_ls_R_factor_obs 0.0770 _refine_ls_wR_factor_all 0.3672 _refine_ls_wR_factor_obs 0.2191 _refine_ls_goodness_of_fit_all 1.469 _refine_ls_goodness_of_fit_obs 1.092 _refine_ls_restrained_S_all 1.466 _refine_ls_restrained_S_obs 1.093 _refine_ls_shift/esd_max -0.006 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_aniso_ratio _atom_site_occupancy # # R=Rmax./Rmin.=ratio of the maximum and minimum # principal axes of atomic displacement ellipsoids # # Table of coordinates # -------------------- # # atom x/a y/b z/c Ueq tmf calc att R SOF MN1A 0.05542(6) -0.04767(5) 0.02989(5) 0.0311(3) aniso . . 1.26 1.0000 NA1A 0.2806(2) 0.0084(2) 0.0582(2) 0.0427(9) aniso . . 1.63 1.0000 NA2A -0.0263(2) -0.2444(1) -0.0492(2) 0.0402(8) aniso . . 1.64 1.0000 O1A 0.4255(3) -0.0245(3) 0.0995(3) 0.0515(18) aniso . . 2.18 1.0000 O2A -0.0267(4) -0.3771(3) -0.1283(3) 0.0550(18) aniso . . 2.18 1.0000 O3A -0.0831(3) -0.2959(3) 0.0573(3) 0.0473(18) aniso . . 1.72 1.0000 N1A 0.0656(3) 0.0293(3) -0.0769(3) 0.0326(16) aniso . . 1.35 1.0000 N2A 0.1384(3) -0.1318(3) -0.0185(3) 0.0346(16) aniso . . 1.36 1.0000 N3A 0.1640(3) -0.0529(3) 0.1386(3) 0.0357(17) aniso . . 1.60 1.0000 N4A 0.0744(3) 0.1015(3) 0.0760(3) 0.0328(17) aniso . . 1.35 1.0000 C1A 0.0389(4) 0.0072(4) -0.2342(4) 0.0396(20) aniso . . 1.32 1.0000 C2A 0.0454(4) -0.0371(4) -0.1562(3) 0.0344(20) aniso . . 1.61 1.0000 C3A 0.1220(4) -0.0891(4) -0.1554(4) 0.0349(20) aniso . . 1.67 1.0000 C4A 0.1636(4) -0.1302(4) -0.0961(4) 0.0329(19) aniso . . 1.36 1.0000 C5A 0.2445(4) -0.1720(4) -0.1123(4) 0.0447(24) aniso . . 1.69 1.0000 C6A 0.1714(4) -0.1788(4) 0.0433(4) 0.0346(20) aniso . . 1.78 1.0000 C7A 0.1818(4) -0.2638(4) 0.0288(4) 0.0393(21) aniso . . 1.68 1.0000 C8A 0.2078(4) -0.3085(4) 0.0951(4) 0.0426(22) aniso . . 1.63 1.0000 C9A 0.2207(4) -0.2682(4) 0.1770(4) 0.0439(23) aniso . . 1.87 1.0000 C10A 0.2081(4) -0.1834(4) 0.1945(4) 0.0423(21) aniso . . 1.61 1.0000 C11A 0.1833(4) -0.1356(4) 0.1298(4) 0.0349(19) aniso . . 1.57 1.0000 C12A 0.2774(5) 0.0101(4) 0.2834(4) 0.0483(24) aniso . . 1.85 1.0000 C13A 0.1904(4) 0.0090(4) 0.2133(3) 0.0368(20) aniso . . 1.38 1.0000 C14A 0.1473(4) 0.0763(4) 0.2224(4) 0.0375(19) aniso . . 1.31 1.0000 C15A 0.0654(4) 0.1024(4) 0.1650(3) 0.0346(19) aniso . . 1.43 1.0000 C16A 0.0658(4) 0.1950(4) 0.2090(4) 0.0382(22) aniso . . 1.44 1.0000 C17A 0.1607(4) 0.1257(4) 0.0525(3) 0.0323(19) aniso . . 1.38 1.0000 C18A 0.2482(4) 0.1790(4) 0.1010(4) 0.0366(18) aniso . . 1.37 1.0000 C19A 0.3297(4) 0.1951(4) 0.0670(4) 0.0437(24) aniso . . 1.51 1.0000 C20A 0.3243(4) 0.1584(4) -0.0146(4) 0.0417(22) aniso . . 1.89 1.0000 C21A 0.2376(4) 0.1037(4) -0.0667(4) 0.0397(21) aniso . . 1.42 1.0000 C22A 0.1537(4) 0.0855(4) -0.0366(4) 0.0330(20) aniso . . 1.45 1.0000 C23A 0.5179(5) 0.0374(5) 0.1268(5) 0.0610(27) aniso . . 1.97 1.0000 C24A 0.5729(7) 0.0105(6) 0.2036(6) 0.0890(40) aniso . . 3.85 1.0000 C25A 0.5160(6) -0.0764(5) 0.2095(5) 0.0691(31) aniso . . 2.09 1.0000 C26A 0.4409(5) -0.1053(4) 0.1252(5) 0.0585(27) aniso . . 2.35 1.0000 C27A -0.0122(7) -0.4009(5) -0.2117(5) 0.0815(39) aniso . . 3.33 1.0000 C28A -0.0106(14) -0.4984(8) -0.2105(9) 0.0713(33) iso . . 3.19 0.5000 C29A 0.0345(9) -0.5053(8) -0.1185(7) 0.0547(26) iso . . 1.76 0.5000 C28C 0.0222(13) -0.4839(9) -0.2251(11) 0.0707(35) iso . . 2.73 0.5000 C29C -0.0353(17) -0.5198(12) -0.1641(11) 0.0679(31) iso . . 2.56 0.5000 C30A -0.0248(6) -0.4491(4) -0.0841(6) 0.0530(23) aniso . . 1.37 1.0000 C31A -0.0439(5) -0.2470(4) 0.1427(4) 0.0323(3) aniso . . 1.15 1.0000 C32A -0.1270(6) -0.2615(6) 0.1863(5) 0.0446(9) aniso . . 1.71 1.0000 C33A -0.1952(6) -0.3432(6) 0.1342(5) 0.0513(9) aniso . . 1.97 1.0000 C34A -0.1837(5) -0.3395(5) 0.0474(4) 0.0545(17) aniso . . 2.48 1.0000 MN1B 0.49434(6) 0.47427(5) 0.57010(5) 0.0790(23) aniso . . 3.15 1.0000 NA1B 0.4754(2) 0.5992(2) 0.7254(1) 0.0615(20) aniso . . 1.98 1.0000 NA2B 0.3715(2) 0.2865(2) 0.5477(2) 0.0344(17) aniso . . 1.28 1.0000 O1B 0.4546(3) 0.6210(3) 0.8573(3) 0.0364(17) aniso . . 1.47 1.0000 O2B 0.2522(4) 0.1653(4) 0.5484(4) 0.0391(18) aniso . . 1.53 1.0000 O3B 0.4831(4) 0.2056(3) 0.5658(3) 0.0326(16) aniso . . 1.32 1.0000 N1B 0.5931(3) 0.6034(3) 0.5526(3) 0.0412(21) aniso . . 1.37 1.0000 N2B 0.5711(3) 0.4912(3) 0.6991(3) 0.0363(21) aniso . . 1.63 1.0000 N3B 0.3844(4) 0.4407(3) 0.6380(3) 0.0380(19) aniso . . 1.60 1.0000 N4B 0.4081(3) 0.5580(3) 0.5017(3) 0.0371(19) aniso . . 1.61 1.0000 C1B 0.7702(4) 0.6629(4) 0.5759(4) 0.0459(23) aniso . . 1.76 1.0000 C2B 0.6898(4) 0.5891(4) 0.5870(4) 0.0366(19) aniso . . 1.45 1.0000 C3B 0.7129(4) 0.5876(4) 0.6827(4) 0.0443(24) aniso . . 1.69 1.0000 C4B 0.6645(4) 0.5450(4) 0.7316(4) 0.0534(29) aniso . . 2.11 1.0000 C5B 0.7069(5) 0.5659(4) 0.8262(4) 0.0546(27) aniso . . 2.23 1.0000 C6B 0.5249(4) 0.4290(4) 0.7381(4) 0.0452(22) aniso . . 1.57 1.0000 C7B 0.5677(5) 0.3859(4) 0.7996(4) 0.0375(21) aniso . . 1.37 1.0000 C8B 0.5124(5) 0.3213(5) 0.8315(4) 0.0509(26) aniso . . 1.79 1.0000 C9B 0.4126(5) 0.2982(4) 0.8029(4) 0.0369(21) aniso . . 1.69 1.0000 C10B 0.3691(4) 0.3362(4) 0.7391(4) 0.0382(20) aniso . . 1.81 1.0000 C11B 0.4209(4) 0.4026(4) 0.7067(4) 0.0354(19) aniso . . 1.53 1.0000 C12B 0.2367(5) 0.4589(5) 0.6851(4) 0.0403(20) aniso . . 1.51 1.0000 C13B 0.2951(4) 0.4610(4) 0.6200(4) 0.0358(21) aniso . . 1.52 1.0000 C14B 0.2619(4) 0.4882(4) 0.5471(4) 0.0403(20) aniso . . 1.36 1.0000 C15B 0.3067(4) 0.5041(4) 0.4725(4) 0.0462(23) aniso . . 1.82 1.0000 C16B 0.2438(4) 0.5519(4) 0.4178(4) 0.0470(22) aniso . . 1.96 1.0000 C17B 0.5473(4) 0.6578(4) 0.5953(3) 0.0402(22) aniso . . 1.65 1.0000 C18B 0.5896(4) 0.7284(4) 0.6635(4) 0.0360(20) aniso . . 1.53 1.0000 C19B 0.5329(5) 0.7746(4) 0.7021(4) 0.0622(32) aniso . . 2.29 1.0000 C20B 0.4346(5) 0.7519(4) 0.6723(4) 0.0701(34) aniso . . 1.86 1.0000 C21B 0.3888(4) 0.6802(4) 0.6047(4) 0.0723(34) aniso . . 2.45 1.0000 C22B 0.4421(4) 0.6330(4) 0.5650(4) 0.0621(29) aniso . . 2.53 1.0000 C23B 0.4724(6) 0.5691(5) 0.9205(5) 0.1625(76) aniso . . 3.00 1.0000 C24B 0.3836(6) 0.5525(6) 0.9533(5) 0.0682(35) aniso . . 1.33 1.0000 C25B 0.3323(6) 0.6218(6) 0.9278(5) 0.0869(46) aniso . . 2.54 1.0000 C26B 0.3979(6) 0.6758(5) 0.8847(5) 0.0928(41) aniso . . 3.91 1.0000 C27B 0.1601(19) 0.1270(18) 0.5014(17) 0.0775(36) iso . . 3.07 0.5000 C28B 0.1291(26) 0.0666(25) 0.5644(23) 0.165(11) iso . . 0.00 0.5000 C27D 0.1821(14) 0.1074(12) 0.4757(12) 0.0678(46) iso . . 0.00 0.5000 C28D 0.1634(17) 0.0220(16) 0.4940(16) 0.1078(66) iso . . 0.00 0.5000 C29B 0.2104(14) 0.0298(10) 0.5872(12) 0.196(14) aniso . . 0.00 1.0000 C30B 0.2855(15) 0.1066(13) 0.6037(12) 0.0786(49) iso . . 0.00 0.5000 C30D 0.2442(14) 0.1199(13) 0.6248(12) 0.0762(47) iso . . 0.00 0.5000 C31B 0.5805(6) 0.2409(5) 0.6193(5) 0.0727(52) aniso . . 0.00 1.0000 C32B 0.6412(7) 0.1959(7) 0.5803(6) 0.0844(61) aniso . . 0.00 1.0000 C33B 0.5810(8) 0.1165(6) 0.5265(7) 0.0973(68) aniso . . 0.00 1.0000 C34B 0.4867(7) 0.1379(5) 0.4992(6) 0.0924(63) aniso . . 0.00 1.0000 H11A -0.00930(0) 0.04130(0) -0.23560(0) 0.0800(0) iso calc C1A 1.00 1.0000 H12A 0.02170(0) -0.03570(0) -0.28470(0) 0.0800(0) iso calc C1A 1.00 1.0000 H13A 0.10000(0) 0.04710(0) -0.23020(0) 0.0800(0) iso calc C1A 1.00 1.0000 H3A 0.14590(0) -0.09170(0) -0.20410(0) 0.0800(0) iso calc C3A 1.00 1.0000 H51A 0.26740(0) -0.19890(0) -0.06440(0) 0.0800(0) iso calc C5A 1.00 1.0000 H52A 0.29830(0) -0.12750(0) -0.11760(0) 0.0800(0) iso calc C5A 1.00 1.0000 H53A 0.22270(0) -0.21570(0) -0.16280(0) 0.0800(0) iso calc C5A 1.00 1.0000 H7A 0.17070(0) -0.29290(0) -0.02700(0) 0.0800(0) iso calc C7A 1.00 1.0000 H8A 0.21560(0) -0.36570(0) 0.08350(0) 0.0800(0) iso calc C8A 1.00 1.0000 H9A 0.23860(0) -0.29650(0) 0.22180(0) 0.0800(0) iso calc C9A 1.00 1.0000 H10A 0.21340(0) -0.15810(0) 0.25060(0) 0.0800(0) iso calc C10A 1.00 1.0000 H121 0.30180(0) -0.04040(0) 0.27010(0) 0.0800(0) iso calc C12A 1.00 1.0000 H122 0.25940(0) 0.00950(0) 0.33670(0) 0.0800(0) iso calc C12A 1.00 1.0000 H123 0.32740(0) 0.06270(0) 0.28940(0) 0.0800(0) iso calc C12A 1.00 1.0000 H14A 0.17380(0) 0.11490(0) 0.27460(0) 0.0800(0) iso calc C14A 1.00 1.0000 H161 0.01670(0) 0.21670(0) 0.17720(0) 0.0800(0) iso calc C16A 1.00 1.0000 H162 0.12830(0) 0.23480(0) 0.21440(0) 0.0800(0) iso calc C16A 1.00 1.0000 H163 0.05720(0) 0.19330(0) 0.26580(0) 0.0800(0) iso calc C16A 1.00 1.0000 H18A 0.25260(0) 0.20520(0) 0.15780(0) 0.0800(0) iso calc C18A 1.00 1.0000 H19A 0.38880(0) 0.23190(0) 0.10210(0) 0.0800(0) iso calc C19A 1.00 1.0000 H20A 0.37880(0) 0.16850(0) -0.03720(0) 0.0800(0) iso calc C20A 1.00 1.0000 H21A 0.23430(0) 0.07850(0) -0.12280(0) 0.0800(0) iso calc C21A 1.00 1.0000 H231 0.51050(0) 0.09730(0) 0.14120(0) 0.0800(0) iso calc C23A 1.00 1.0000 H232 0.55150(0) 0.03680(0) 0.08110(0) 0.0800(0) iso calc C23A 1.00 1.0000 H241 0.63850(0) 0.00640(0) 0.19620(0) 0.0800(0) iso calc C24A 1.00 1.0000 H242 0.58520(0) 0.05470(0) 0.25480(0) 0.0800(0) iso calc C24A 1.00 1.0000 H251 0.48520(0) -0.07000(0) 0.25710(0) 0.0800(0) iso calc C25A 1.00 1.0000 H252 0.55650(0) -0.11770(0) 0.22020(0) 0.0800(0) iso calc C25A 1.00 1.0000 H261 0.46630(0) -0.13910(0) 0.08260(0) 0.0800(0) iso calc C26A 1.00 1.0000 H262 0.38220(0) -0.14400(0) 0.12960(0) 0.0800(0) iso calc C26A 1.00 1.0000 H271 0.04820(0) -0.36630(0) -0.22000(0) 0.0800(0) iso calc C27A 1.00 1.0000 H272 -0.06510(0) -0.39490(0) -0.25820(0) 0.0800(0) iso calc C27A 1.00 1.0000 H281 -0.07550(0) -0.53520(0) -0.23200(0) 0.0800(0) iso calc C28A 1.00 0.5000 H282 0.02790(0) -0.51710(0) -0.24900(0) 0.0800(0) iso calc C28A 1.00 0.5000 H283 0.08930(0) -0.47870(0) -0.20890(0) 0.0800(0) iso calc C28A 1.00 0.5000 H284 -0.00400(0) -0.51880(0) -0.28640(0) 0.0800(0) iso calc C28A 1.00 0.5000 H291 0.01790(0) -0.56630(0) -0.11000(0) 0.0800(0) iso calc C29A 1.00 0.5000 H292 0.10190(0) -0.48070(0) -0.10090(0) 0.0800(0) iso calc C29A 1.00 0.5000 H293 -0.01780(0) -0.56970(0) -0.14920(0) 0.0800(0) iso calc C28A 1.00 0.5000 H294 -0.10510(0) -0.53720(0) -0.19610(0) 0.0800(0) iso calc C28A 1.00 0.5000 H301 -0.09160(0) -0.48420(0) -0.09250(0) 0.0800(0) iso calc C30A 1.00 1.0000 H302 0.00140(0) -0.42830(0) -0.02420(0) 0.0800(0) iso calc C30A 1.00 1.0000 H311 -0.01910(0) -0.18420(0) 0.14320(0) 0.0800(0) iso calc C31A 1.00 1.0000 H312 0.00990(0) -0.26780(0) 0.17290(0) 0.0800(0) iso calc C31A 1.00 1.0000 H321 -0.10460(0) -0.26500(0) 0.24690(0) 0.0800(0) iso calc C32A 1.00 1.0000 H322 -0.15820(0) -0.21100(0) 0.18660(0) 0.0800(0) iso calc C32A 1.00 1.0000 H331 -0.17650(0) -0.39610(0) 0.15430(0) 0.0800(0) iso calc C33A 1.00 1.0000 H332 -0.26150(0) -0.34810(0) 0.13900(0) 0.0800(0) iso calc C33A 1.00 1.0000 H341 -0.20030(0) -0.39860(0) 0.01130(0) 0.0800(0) iso calc C34A 1.00 1.0000 H342 -0.22670(0) -0.30660(0) 0.01860(0) 0.0800(0) iso calc C34A 1.00 1.0000 H11B 0.76160(0) 0.66750(0) 0.51700(0) 0.0800(0) iso calc C1B 1.00 1.0000 H12B 0.83260(0) 0.64950(0) 0.59530(0) 0.0800(0) iso calc C1B 1.00 1.0000 H13B 0.77100(0) 0.71780(0) 0.60880(0) 0.0800(0) iso calc C1B 1.00 1.0000 H3B 0.77340(0) 0.62490(0) 0.71260(0) 0.0800(0) iso calc C3B 1.00 1.0000 H51B 0.66680(0) 0.53160(0) 0.85460(0) 0.0800(0) iso calc C5B 1.00 1.0000 H52B 0.71500(0) 0.62760(0) 0.84750(0) 0.0800(0) iso calc C5B 1.00 1.0000 H53B 0.77030(0) 0.55330(0) 0.83870(0) 0.0800(0) iso calc C5B 1.00 1.0000 H7B 0.63500(0) 0.40000(0) 0.81970(0) 0.0800(0) iso calc C7B 1.00 1.0000 H8B 0.54410(0) 0.29460(0) 0.87350(0) 0.0800(0) iso calc C8B 1.00 1.0000 H9B 0.37550(0) 0.25720(0) 0.82680(0) 0.0800(0) iso calc C9B 1.00 1.0000 H10B 0.30160(0) 0.31660(0) 0.71570(0) 0.0800(0) iso calc C10B 1.00 1.0000 H124 0.26850(0) 0.43830(0) 0.73370(0) 0.0800(0) iso calc C12B 1.00 1.0000 H125 0.17390(0) 0.42050(0) 0.66120(0) 0.0800(0) iso calc C12B 1.00 1.0000 H126 0.23000(0) 0.51730(0) 0.70390(0) 0.0800(0) iso calc C12B 1.00 1.0000 H14B 0.20110(0) 0.50010(0) 0.54170(0) 0.0800(0) iso calc C14B 1.00 1.0000 H164 0.27020(0) 0.56390(0) 0.36920(0) 0.0800(0) iso calc C16B 1.00 1.0000 H165 0.24410(0) 0.60760(0) 0.45010(0) 0.0800(0) iso calc C16B 1.00 1.0000 H166 0.17950(0) 0.51700(0) 0.39700(0) 0.0800(0) iso calc C16B 1.00 1.0000 H18B 0.65730(0) 0.74450(0) 0.68460(0) 0.0800(0) iso calc C18B 1.00 1.0000 H19B 0.56240(0) 0.82160(0) 0.74830(0) 0.0800(0) iso calc C19B 1.00 1.0000 H20B 0.39630(0) 0.78390(0) 0.69710(0) 0.0800(0) iso calc C20B 1.00 1.0000 H21B 0.32080(0) 0.66430(0) 0.58580(0) 0.0800(0) iso calc C21B 1.00 1.0000 H233 0.52920(0) 0.60090(0) 0.96670(0) 0.0800(0) iso calc C23B 1.00 1.0000 H234 0.48590(0) 0.51490(0) 0.89660(0) 0.0800(0) iso calc C23B 1.00 1.0000 H243 0.34220(0) 0.49320(0) 0.92860(0) 0.0800(0) iso calc C24B 1.00 1.0000 H244 0.39870(0) 0.55660(0) 1.01560(0) 0.0800(0) iso calc C24B 1.00 1.0000 H253 0.32060(0) 0.65690(0) 0.97800(0) 0.0800(0) iso calc C25B 1.00 1.0000 H254 0.26760(0) 0.59510(0) 0.88920(0) 0.0800(0) iso calc C25B 1.00 1.0000 H263 0.36210(0) 0.69700(0) 0.83700(0) 0.0800(0) iso calc C26B 1.00 1.0000 H264 0.43930(0) 0.73010(0) 0.92500(0) 0.0800(0) iso calc C26B 1.00 1.0000 H273 0.16960(0) 0.09460(0) 0.43680(0) 0.0800(0) iso calc C27B 1.00 0.5000 H274 0.12020(0) 0.16210(0) 0.47990(0) 0.0800(0) iso calc C27B 1.00 0.5000 H275 0.13130(0) 0.12420(0) 0.44730(0) 0.0800(0) iso calc C27B 1.00 0.5000 H276 0.22360(0) 0.10280(0) 0.42320(0) 0.0800(0) iso calc C27D 1.00 0.5000 H285 0.07890(0) 0.07330(0) 0.57320(0) 0.0800(0) iso calc C28B 1.00 0.5000 H286 0.07760(0) -0.00160(0) 0.49830(0) 0.0800(0) iso calc C28B 1.00 0.5000 H287 0.19130(0) -0.02450(0) 0.45760(0) 0.0800(0) iso calc C28D 1.00 0.5000 H288 0.09310(0) -0.00680(0) 0.47200(0) 0.0800(0) iso calc C28D 1.00 0.5000 H295 0.19580(0) 0.02340(0) 0.64720(0) 0.0800(0) iso calc C29B 1.00 1.0000 H296 0.21740(0) -0.02240(0) 0.56480(0) 0.0800(0) iso calc C28D 1.00 1.0000 H303 0.34490(0) 0.08350(0) 0.58420(0) 0.0800(0) iso calc C30B 1.00 0.5000 H304 0.31910(0) 0.13310(0) 0.66360(0) 0.0800(0) iso calc C30B 1.00 0.5000 H305 0.31420(0) 0.12860(0) 0.66200(0) 0.0800(0) iso calc C30B 1.00 0.5000 H306 0.21160(0) 0.14560(0) 0.66140(0) 0.0800(0) iso calc C30D 1.00 0.5000 H313 0.58390(0) 0.23130(0) 0.67760(0) 0.0800(0) iso calc C31B 1.00 1.0000 H314 0.60030(0) 0.30490(0) 0.62240(0) 0.0800(0) iso calc C31B 1.00 1.0000 H323 0.67460(0) 0.23280(0) 0.54720(0) 0.0800(0) iso calc C32B 1.00 1.0000 H324 0.68930(0) 0.18110(0) 0.62280(0) 0.0800(0) iso calc C32B 1.00 1.0000 H333 0.57620(0) 0.06790(0) 0.55460(0) 0.0800(0) iso calc C33B 1.00 1.0000 H334 0.60600(0) 0.10240(0) 0.47570(0) 0.0800(0) iso calc C33B 1.00 1.0000 H343 0.47870(0) 0.15680(0) 0.44410(0) 0.0800(0) iso calc C34B 1.00 1.0000 H344 0.43400(0) 0.08460(0) 0.49180(0) 0.0800(0) iso calc C34B 1.00 1.0000 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 #label U11 U22 U33 U23 U13 U12 MN1A 0.0319(4) 0.0302(4) 0.0329(4) 0.0082(3) 0.0079(3) 0.0100(3) NA1A 0.0358(12) 0.0422(13) 0.0530(14) 0.0159(11) 0.0110(11) 0.0116(10) NA2A 0.0479(13) 0.0323(11) 0.0439(13) 0.0100(10) 0.0167(10) 0.0104(10) O1A 0.0352(22) 0.0462(25) 0.0734(31) 0.0173(23) 0.0100(22) 0.0102(19) O2A 0.0652(30) 0.0392(23) 0.0568(28) 0.0040(21) 0.0044(23) 0.0189(22) O3A 0.0500(25) 0.0509(25) 0.0472(25) 0.0135(21) 0.0229(21) 0.0121(21) N1A 0.0375(25) 0.0308(23) 0.0285(22) 0.0056(19) 0.0068(20) 0.0076(20) N2A 0.0363(25) 0.0361(25) 0.0350(24) 0.0105(21) 0.0103(20) 0.0130(21) N3A 0.0386(26) 0.0355(26) 0.0359(25) 0.0099(21) 0.0074(21) 0.0155(21) N4A 0.0368(25) 0.0315(24) 0.0336(24) 0.0077(20) 0.0119(20) 0.0117(20) C1A 0.0432(32) 0.0412(32) 0.0360(30) 0.0108(26) 0.0115(26) 0.0099(27) C2A 0.0440(32) 0.0324(29) 0.0281(27) 0.0067(23) 0.0098(24) 0.0107(25) C3A 0.0423(31) 0.0331(29) 0.0348(29) 0.0072(24) 0.0165(25) 0.0133(25) C4A 0.0315(27) 0.0337(28) 0.0349(29) 0.0053(24) 0.0121(23) 0.0077(24) C5A 0.0444(33) 0.0476(35) 0.0503(36) 0.0130(30) 0.0191(29) 0.0193(29) C6A 0.0332(28) 0.0355(30) 0.0397(31) 0.0165(26) 0.0108(25) 0.0104(24) C7A 0.0386(31) 0.0327(30) 0.0484(34) 0.0100(26) 0.0094(27) 0.0121(25) C8A 0.0387(32) 0.0362(31) 0.0539(37) 0.0122(29) 0.0099(28) 0.0104(26) C9A 0.0457(34) 0.0469(35) 0.0463(35) 0.0183(30) 0.0116(29) 0.0207(29) C10A 0.0434(33) 0.0441(33) 0.0422(33) 0.0165(28) 0.0087(27) 0.0135(28) C11A 0.0298(28) 0.0350(29) 0.0411(31) 0.0135(25) 0.0074(24) 0.0079(24) C12A 0.0475(36) 0.0559(39) 0.0424(34) 0.0098(31) 0.0037(29) 0.0214(32) C13A 0.0398(31) 0.0399(32) 0.0302(28) 0.0076(25) 0.0069(25) 0.0098(27) C14A 0.0424(32) 0.0368(31) 0.0330(29) 0.0062(25) 0.0081(25) 0.0102(26) C15A 0.0411(31) 0.0342(29) 0.0294(27) 0.0056(24) 0.0089(24) 0.0114(25) C16A 0.0450(33) 0.0344(30) 0.0343(29) 0.0037(25) 0.0090(26) 0.0104(27) C17A 0.0317(28) 0.0287(27) 0.0345(29) 0.0072(24) 0.0053(24) 0.0052(23) C18A 0.0332(29) 0.0332(29) 0.0413(31) 0.0075(26) 0.0064(25) 0.0063(25) C19A 0.0381(32) 0.0424(33) 0.0491(36) 0.0124(30) 0.0101(28) 0.0050(27) C20A 0.0318(30) 0.0408(33) 0.0553(38) 0.0148(30) 0.0137(28) 0.0082(26) C21A 0.0401(32) 0.0404(32) 0.0421(33) 0.0139(27) 0.0135(27) 0.0103(27) C22A 0.0322(28) 0.0312(28) 0.0373(29) 0.0114(24) 0.0091(24) 0.0079(24) C23A 0.0441(37) 0.0553(43) 0.0804(52) 0.0168(39) 0.0113(37) 0.0063(33) C24A 0.0774(57) 0.0568(49) 0.0990(66) 0.0117(48) -0.0290(53) -0.0039(44) C25A 0.0702(49) 0.0688(50) 0.0690(49) 0.0250(42) 0.0032(41) 0.0252(42) C26A 0.0447(36) 0.0448(37) 0.0850(52) 0.0221(37) 0.0074(36) 0.0110(31) C27A 0.1079(68) 0.0859(59) 0.0542(45) -0.0045(41) 0.0038(44) 0.0591(55) C30A 0.0771(52) 0.0388(37) 0.1064(63) 0.0210(41) 0.0285(48) 0.0219(36) C31A 0.0673(45) 0.0419(35) 0.0527(39) 0.0109(32) 0.0147(35) 0.0073(33) C32A 0.0832(56) 0.0754(52) 0.0510(42) 0.0046(39) 0.0323(41) 0.0019(45) C33A 0.0653(48) 0.0804(54) 0.0579(44) 0.0086(41) 0.0318(39) 0.0032(42) C34A 0.0521(38) 0.0558(40) 0.0509(38) 0.0143(33) 0.0139(32) 0.0084(33) MN1B 0.0339(5) 0.0329(5) 0.0309(4) 0.0075(4) 0.0084(3) 0.0087(4) NA1B 0.0554(15) 0.0456(14) 0.0393(12) 0.0089(11) 0.0174(11) 0.0204(12) NA2B 0.0530(14) 0.0383(13) 0.0586(16) 0.0148(12) 0.0055(12) 0.0073(11) O1B 0.0640(29) 0.0645(29) 0.0529(27) 0.0181(23) 0.0305(23) 0.0337(24) O2B 0.0820(37) 0.0605(32) 0.0748(35) 0.0288(29) -0.0051(30) -0.0109(29) O3B 0.0624(30) 0.0477(27) 0.0673(31) 0.0084(24) -0.0010(26) 0.0168(24) N1B 0.0328(24) 0.0364(25) 0.0363(25) 0.0098(21) 0.0093(20) 0.0109(20) N2B 0.0391(26) 0.0391(26) 0.0343(25) 0.0122(22) 0.0092(21) 0.0133(22) N3B 0.0404(26) 0.0448(28) 0.0353(25) 0.0136(22) 0.0092(21) 0.0132(23) N4B 0.0296(23) 0.0338(24) 0.0325(23) 0.0058(20) 0.0039(19) 0.0077(20) C1B 0.0375(31) 0.0391(32) 0.0432(33) 0.0073(27) 0.0063(26) 0.0050(26) C2B 0.0340(29) 0.0388(31) 0.0324(29) 0.0092(25) 0.0024(24) 0.0052(26) C3B 0.0303(28) 0.0392(32) 0.0403(31) 0.0060(27) 0.0024(25) 0.0066(25) C4B 0.0338(29) 0.0402(31) 0.0355(30) 0.0054(26) 0.0024(25) 0.0123(26) C5B 0.0461(34) 0.0494(36) 0.0353(31) 0.0062(28) 0.0019(27) 0.0061(30) C6B 0.0435(32) 0.0334(29) 0.0362(30) 0.0069(25) 0.0150(26) 0.0113(26) C7B 0.0525(37) 0.0383(32) 0.0433(34) 0.0110(28) 0.0078(29) 0.0156(29) C8B 0.0666(45) 0.0532(40) 0.0488(37) 0.0234(33) 0.0152(34) 0.0231(35) C9B 0.0702(47) 0.0456(37) 0.0561(41) 0.0230(33) 0.0241(36) 0.0141(34) C10B 0.0471(35) 0.0428(34) 0.0501(36) 0.0148(30) 0.0190(30) 0.0097(29) C11B 0.0399(31) 0.0385(31) 0.0376(30) 0.0122(26) 0.0111(26) 0.0126(26) C12B 0.0457(36) 0.0696(45) 0.0427(34) 0.0174(33) 0.0137(29) 0.0187(33) C13B 0.0306(28) 0.0457(33) 0.0366(30) 0.0074(27) 0.0122(24) 0.0100(26) C14B 0.0304(28) 0.0443(33) 0.0447(32) 0.0113(27) 0.0144(25) 0.0126(26) C15B 0.0313(28) 0.0367(30) 0.0398(30) 0.0121(26) 0.0071(25) 0.0105(25) C16B 0.0371(31) 0.0437(33) 0.0394(31) 0.0083(27) 0.0039(26) 0.0136(27) C17B 0.0428(32) 0.0342(30) 0.0329(29) 0.0082(25) 0.0088(25) 0.0144(26) C18B 0.0434(33) 0.0349(31) 0.0393(31) 0.0041(26) 0.0074(27) 0.0073(27) C19B 0.0543(39) 0.0370(33) 0.0433(33) 0.0000(28) 0.0067(30) 0.0128(30) C20B 0.0572(39) 0.0428(35) 0.0455(34) 0.0069(29) 0.0115(30) 0.0239(32) C21B 0.0491(34) 0.0373(31) 0.0374(31) 0.0062(26) 0.0113(27) 0.0176(28) C22B 0.0400(31) 0.0352(30) 0.0365(30) 0.0107(25) 0.0093(25) 0.0149(26) C23B 0.0770(50) 0.0753(51) 0.0533(41) 0.0227(38) 0.0250(37) 0.0441(43) C24B 0.0822(55) 0.0726(52) 0.0637(48) 0.0275(42) 0.0284(42) 0.0170(44) C25B 0.0655(48) 0.1024(65) 0.0681(50) 0.0284(48) 0.0326(41) 0.0378(47) C26B 0.0792(52) 0.0599(44) 0.0687(47) 0.0210(38) 0.0392(41) 0.0369(40) C29B 0.196(14) 0.113(10) 0.188(13) 0.079(10) 0.054(11) 0.018(10) C31B 0.0727(52) 0.0615(47) 0.0691(50) 0.0134(41) 0.0119(42) 0.0186(41) C32B 0.0844(61) 0.1082(76) 0.0672(53) 0.0079(52) -0.0009(47) 0.0476(59) C33B 0.0973(68) 0.0540(49) 0.1164(76) -0.0126(51) 0.0056(60) 0.0348(50) C34B 0.0924(63) 0.0438(41) 0.0794(55) -0.0034(40) -0.0060(49) 0.0172(43) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag MN1A NA1A 3.146(3) yes MN1A NA2A 3.085(2) yes MN1A N1A 2.274(5) yes MN1A N2A 2.161(5) yes MN1A N3A 2.143(5) yes MN1A N4A 2.319(5) yes NA1A O1A 2.274(6) yes NA1A N2A 2.657(5) yes NA1A N3A 2.490(6) yes NA1A C17A 2.803(8) yes NA1A C21A 2.743(8) yes NA1A C22A 2.751(7) yes NA2A O2A 2.313(5) yes NA2A O3A 2.262(6) yes NA2A N2A 2.590(5) yes O1A C23A 1.437(8) yes O1A C26A 1.444(9) yes O2A C27A 1.44(1) yes O2A C30A 1.43(1) yes O3A C31A 1.438(7) yes O3A C34A 1.456(8) yes N1A C2A 1.490(7) yes N1A C22A 1.377(6) yes N2A C4A 1.398(9) yes N2A C6A 1.398(8) yes N3A C11A 1.390(8) yes N3A C13A 1.388(7) yes N4A C15A 1.489(7) yes N4A C17A 1.392(8) yes C1A C2A 1.532(9) yes C2A C3A 1.52(0) yes C3A C4A 1.35(0) yes C4A C5A 1.52(0) yes C6A C7A 1.379(9) yes C6A C11A 1.446(9) yes C7A C8A 1.40(1) yes C8A C9A 1.361(9) yes C9A C10A 1.392(9) yes C10A C11A 1.41(1) yes C12A C13A 1.518(8) yes C13A C14A 1.35(1) yes C14A C15A 1.524(9) yes C15A C16A 1.542(9) yes C17A C18A 1.387(7) yes C17A C22A 1.485(8) yes C18A C19A 1.412(9) yes C19A C20A 1.362(9) yes C20A C21A 1.405(7) yes C21A C22A 1.408(9) yes C23A C24A 1.51(1) yes C24A C25A 1.48(1) yes C25A C26A 1.52(1) yes C27A C28A 1.55(1) yes C27A C28C 1.51(1) yes C28A C29A 1.54(1) yes C28A C28C 0.60(2) yes C28A C29C 0.98(2) yes C29A C28C 1.80(2) yes C29A C29C 1.09(2) yes C29A C30A 1.50(1) yes C28C C29C 1.53(3) yes C29C C30A 1.56(2) yes C31A C32A 1.53(1) yes C32A C33A 1.48(1) yes C33A C34A 1.47(1) yes MN1B NA1B 3.103(3) yes MN1B NA2B 3.068(3) yes MN1B N1B 2.336(5) yes MN1B N2B 2.124(5) yes MN1B N3B 2.162(6) yes MN1B N4B 2.257(5) yes NA1B O1B 2.236(5) yes NA1B N2B 2.474(6) yes NA1B N3B 2.637(5) yes NA1B C17B 2.754(6) yes NA1B C18B 2.805(7) yes NA1B C20B 2.809(8) yes NA1B C21B 2.728(7) yes NA1B C22B 2.714(7) yes NA2B O2B 2.315(7) yes NA2B O3B 2.271(7) yes NA2B N3B 2.626(6) yes O1B C23B 1.42(1) yes O1B C26B 1.41(1) yes O2B C27B 1.37(2) yes O2B C27D 1.45(1) yes O2B C30B 1.46(2) yes O2B C30D 1.54(2) yes O3B C31B 1.456(9) yes O3B C34B 1.44(1) yes N1B C2B 1.483(8) yes N1B C17B 1.399(8) yes N2B C4B 1.402(6) yes N2B C6B 1.382(8) yes N3B C11B 1.405(8) yes N3B C13B 1.391(9) yes N4B C15B 1.491(7) yes N4B C22B 1.391(7) yes C1B C2B 1.537(8) yes C2B C3B 1.536(9) yes C3B C4B 1.34(1) yes C4B C5B 1.504(9) yes C6B C7B 1.40(1) yes C6B C11B 1.450(8) yes C7B C8B 1.40(1) yes C8B C9B 1.39(1) yes C9B C10B 1.38(1) yes C10B C11B 1.397(9) yes C12B C13B 1.50(1) yes C13B C14B 1.351(9) yes C14B C15B 1.53(1) yes C15B C16B 1.530(9) yes C17B C18B 1.401(7) yes C17B C22B 1.464(8) yes C18B C19B 1.40(1) yes C19B C20B 1.37(1) yes C20B C21B 1.412(8) yes C21B C22B 1.38(1) yes C23B C24B 1.50(1) yes C24B C25B 1.51(1) yes C25B C26B 1.50(1) yes C27B C28B 1.57(5) yes C27B C27D 0.66(3) yes C27B C28D 1.66(3) yes C28B C27D 1.91(4) yes C28B C28D 1.50(4) yes C28B C29B 1.43(4) yes C28B C30D 1.73(3) yes C27D C28D 1.41(3) yes C28D C29B 1.51(3) yes C29B C30B 1.41(2) yes C29B C30D 1.41(2) yes C30B C30D 0.81(3) yes C31B C32B 1.44(1) yes C32B C33B 1.43(1) yes C33B C34B 1.48(1) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag N3A MN1A N4A 91.1(2) yes N2A MN1A N4A 137.3(3) yes N2A MN1A N3A 74.9(2) yes N1A MN1A N4A 68.2(2) yes N1A MN1A N3A 130.3(3) yes N1A MN1A N2A 90.3(2) yes NA2A MN1A N4A 164.7(2) yes NA2A MN1A N3A 101.6(2) yes NA2A MN1A N2A 55.9(2) yes NA2A MN1A N1A 108.5(2) yes NA1A MN1A N4A 82.9(2) yes NA1A MN1A N3A 52.1(2) yes NA1A MN1A N2A 56.5(2) yes NA1A MN1A N1A 80.0(2) yes NA1A MN1A NA2A 111.7(2) yes MN1A NA1A C22A 55.8(2) yes MN1A NA1A C21A 83.7(2) yes MN1A NA1A C17A 55.5(2) yes MN1A NA1A N3A 42.8(2) yes MN1A NA1A N2A 42.7(2) yes MN1A NA1A O1A 148.2(2) yes C21A NA1A C22A 29.7(2) yes C17A NA1A C22A 31.0(2) yes C17A NA1A C21A 52.9(2) yes N3A NA1A C22A 93.8(2) yes N3A NA1A C21A 123.5(3) yes N3A NA1A C17A 77.7(2) yes N2A NA1A C22A 79.4(2) yes N2A NA1A C21A 94.2(2) yes N2A NA1A C17A 94.4(2) yes N2A NA1A N3A 61.0(2) yes O1A NA1A C22A 153.8(3) yes O1A NA1A C21A 124.1(3) yes O1A NA1A C17A 152.2(3) yes O1A NA1A N3A 112.3(2) yes O1A NA1A N2A 113.2(3) yes MN1A NA2A N2A 43.7(2) yes MN1A NA2A O3A 101.1(2) yes MN1A NA2A O2A 154.9(3) yes O3A NA2A N2A 121.2(2) yes O2A NA2A N2A 112.0(3) yes O2A NA2A O3A 98.6(2) yes NA1A O1A C26A 126.2(5) yes NA1A O1A C23A 126.1(5) yes C23A O1A C26A 105.9(6) yes NA2A O2A C30A 116.6(5) yes NA2A O2A C27A 132.7(5) yes C27A O2A C30A 109.8(6) yes NA2A O3A C34A 123.1(4) yes NA2A O3A C31A 118.8(4) yes C31A O3A C34A 109.1(5) yes MN1A N1A C22A 96.0(4) yes MN1A N1A C2A 106.3(4) yes C2A N1A C22A 125.5(6) yes NA1A N2A NA2A 158.7(3) yes MN1A N2A NA2A 80.4(2) yes MN1A N2A NA1A 80.8(2) yes NA2A N2A C6A 86.5(4) yes NA2A N2A C4A 107.1(4) yes NA1A N2A C6A 90.4(4) yes NA1A N2A C4A 91.8(4) yes MN1A N2A C6A 109.7(4) yes MN1A N2A C4A 123.8(4) yes C4A N2A C6A 126.1(6) yes MN1A N3A NA1A 85.2(2) yes NA1A N3A C13A 102.5(4) yes NA1A N3A C11A 94.5(4) yes MN1A N3A C13A 122.9(4) yes MN1A N3A C11A 109.4(4) yes C11A N3A C13A 125.8(5) yes MN1A N4A C17A 94.1(4) yes MN1A N4A C15A 100.6(4) yes C15A N4A C17A 125.1(5) yes N1A C2A C1A 110.7(5) yes C1A C2A C3A 107.9(5) yes N1A C2A C3A 112.8(5) yes C2A C3A C4A 131.6(6) yes N2A C4A C3A 122.2(6) yes C3A C4A C5A 118.8(6) yes N2A C4A C5A 118.9(6) yes N2A C6A C11A 114.4(6) yes N2A C6A C7A 126.3(6) yes C7A C6A C11A 118.8(6) yes C6A C7A C8A 122.4(6) yes C7A C8A C9A 119.4(6) yes C8A C9A C10A 120.1(6) yes C9A C10A C11A 122.3(6) yes C6A C11A C10A 116.8(6) yes N3A C11A C10A 127.8(6) yes N3A C11A C6A 115.3(6) yes N3A C13A C12A 120.7(6) yes C12A C13A C14A 117.3(5) yes N3A C13A C14A 121.5(5) yes C13A C14A C15A 133.3(6) yes N4A C15A C14A 114.1(5) yes C14A C15A C16A 105.2(5) yes N4A C15A C16A 111.5(5) yes NA1A C17A N4A 118.1(4) yes N4A C17A C22A 112.4(6) yes N4A C17A C18A 128.8(5) yes NA1A C17A C22A 72.6(4) yes NA1A C17A C18A 78.0(4) yes C18A C17A C22A 118.8(6) yes C17A C18A C19A 121.1(6) yes C18A C19A C20A 120.7(6) yes C19A C20A C21A 120.8(6) yes NA1A C21A C20A 78.2(4) yes C20A C21A C22A 121.3(6) yes NA1A C21A C22A 75.4(4) yes C17A C22A C21A 117.4(6) yes N1A C22A C21A 128.6(6) yes N1A C22A C17A 113.9(6) yes NA1A C22A C21A 74.8(4) yes NA1A C22A C17A 76.4(4) yes NA1A C22A N1A 114.3(4) yes O1A C23A C24A 106.4(7) yes C23A C24A C25A 106.6(8) yes C24A C25A C26A 104.2(7) yes O1A C26A C25A 104.8(6) yes O2A C27A C28C 114.6(8) yes O2A C27A C28A 99.1(7) yes C28A C27A C28C 22.5(9) yes C27A C28A C29C 112(2) yes C27A C28A C28C 75(2) yes C27A C28A C29A 107.7(9) yes C28C C28A C29C 151(3) yes C29A C28A C29C 45(1) yes C29A C28A C28C 106(3) yes C28A C29A C30A 91.6(9) yes C28A C29A C29C 39(1) yes C28A C29A C28C 18.6(9) yes C29C C29A C30A 72(1) yes C28C C29A C30A 101.7(9) yes C28C C29A C29C 58(1) yes C28A C28C C29A 55(2) yes C27A C28C C29A 98(1) yes C27A C28C C28A 83(2) yes C29A C28C C29C 37.1(9) yes C28A C28C C29C 18(2) yes C27A C28C C29C 89(1) yes C29A C29C C28C 85(2) yes C28A C29C C28C 11(1) yes C28A C29C C29A 96(2) yes C28C C29C C30A 112(1) yes C29A C29C C30A 66(1) yes C28A C29C C30A 116(2) yes C29A C30A C29C 41.6(9) yes O2A C30A C29C 95.9(8) yes O2A C30A C29A 109.3(7) yes O3A C31A C32A 105.5(6) yes C31A C32A C33A 104.2(7) yes C32A C33A C34A 103.6(7) yes O3A C34A C33A 105.8(6) yes N3B MN1B N4B 89.7(2) yes N2B MN1B N4B 131.4(2) yes N2B MN1B N3B 75.1(2) yes N1B MN1B N4B 68.1(2) yes N1B MN1B N3B 136.4(2) yes N1B MN1B N2B 91.6(2) yes NA2B MN1B N4B 110.7(2) yes NA2B MN1B N3B 57.2(2) yes NA2B MN1B N2B 99.3(2) yes NA2B MN1B N1B 165.1(2) yes NA1B MN1B N4B 80.3(2) yes NA1B MN1B N3B 56.8(2) yes NA1B MN1B N2B 52.5(2) yes NA1B MN1B N1B 82.0(2) yes NA1B MN1B NA2B 112.7(1) yes MN1B NA1B C22B 56.6(2) yes MN1B NA1B C21B 83.9(2) yes MN1B NA1B C20B 108.7(2) yes MN1B NA1B C18B 83.7(2) yes MN1B NA1B C17B 56.6(1) yes MN1B NA1B N3B 43.3(1) yes MN1B NA1B N2B 43.0(1) yes MN1B NA1B O1B 149.9(2) yes C21B NA1B C22B 29.5(2) yes C20B NA1B C22B 52.2(2) yes C20B NA1B C21B 29.5(2) yes C18B NA1B C22B 53.0(2) yes C18B NA1B C21B 60.7(2) yes C18B NA1B C20B 50.7(2) yes C17B NA1B C22B 31.1(2) yes C17B NA1B C21B 53.1(2) yes C17B NA1B C20B 60.8(2) yes C17B NA1B C18B 29.2(2) yes N3B NA1B C22B 79.6(2) yes N3B NA1B C21B 92.9(2) yes N3B NA1B C20B 121.9(2) yes N3B NA1B C18B 124.6(2) yes N3B NA1B C17B 95.5(2) yes N2B NA1B C22B 95.4(2) yes N2B NA1B C21B 124.7(2) yes N2B NA1B C20B 140.5(2) yes N2B NA1B C18B 93.1(2) yes N2B NA1B C17B 79.8(2) yes N2B NA1B N3B 61.4(2) yes O1B NA1B C22B 149.9(3) yes O1B NA1B C21B 120.5(2) yes O1B NA1B C20B 100.2(2) yes O1B NA1B C18B 122.4(2) yes O1B NA1B C17B 151.5(2) yes O1B NA1B N3B 113.0(2) yes O1B NA1B N2B 114.7(2) yes MN1B NA2B N3B 43.8(1) yes MN1B NA2B O3B 103.1(2) yes MN1B NA2B O2B 164.0(3) yes O3B NA2B N3B 126.2(3) yes O2B NA2B N3B 120.8(3) yes O2B NA2B O3B 90.3(3) yes NA1B O1B C26B 124.2(5) yes NA1B O1B C23B 127.7(5) yes C23B O1B C26B 106.4(6) yes NA2B O2B C30D 125.8(8) yes NA2B O2B C30B 113.8(9) yes NA2B O2B C27D 127.7(9) yes NA2B O2B C27B 136(1) yes C30B O2B C30D 31(1) yes C27D O2B C30D 106(1) yes C27D O2B C30B 105(1) yes C27B O2B C30D 96(1) yes C27B O2B C30B 110(2) yes C27B O2B C27D 27(1) yes NA2B O3B C34B 122.2(5) yes NA2B O3B C31B 122.9(5) yes C31B O3B C34B 107.8(7) yes MN1B N1B C17B 93.5(4) yes MN1B N1B C2B 100.7(4) yes C2B N1B C17B 125.6(5) yes MN1B N2B NA1B 84.5(2) yes NA1B N2B C6B 95.8(4) yes NA1B N2B C4B 100.1(4) yes MN1B N2B C6B 109.9(4) yes MN1B N2B C4B 122.8(4) yes C4B N2B C6B 125.9(5) yes NA1B N3B NA2B 154.9(3) yes MN1B N3B NA2B 79.0(2) yes MN1B N3B NA1B 79.9(2) yes NA2B N3B C13B 109.3(4) yes NA2B N3B C11B 83.5(4) yes NA1B N3B C13B 93.9(4) yes NA1B N3B C11B 90.7(4) yes MN1B N3B C13B 124.6(4) yes MN1B N3B C11B 109.2(5) yes C11B N3B C13B 126.0(6) yes MN1B N4B C22B 96.3(4) yes MN1B N4B C15B 106.2(4) yes C15B N4B C22B 126.1(6) yes N1B C2B C1B 111.4(6) yes C1B C2B C3B 105.1(5) yes N1B C2B C3B 114.0(6) yes C2B C3B C4B 132.9(6) yes N2B C4B C3B 122.2(6) yes C3B C4B C5B 118.0(6) yes N2B C4B C5B 119.3(6) yes N2B C6B C11B 114.9(6) yes N2B C6B C7B 127.3(7) yes C7B C6B C11B 117.7(6) yes C6B C7B C8B 121.5(7) yes C7B C8B C9B 120.5(7) yes C8B C9B C10B 119.1(7) yes C9B C10B C11B 122.4(7) yes C6B C11B C10B 118.6(6) yes N3B C11B C10B 126.6(6) yes N3B C11B C6B 114.3(6) yes N3B C13B C12B 119.8(6) yes C12B C13B C14B 118.7(6) yes N3B C13B C14B 121.5(6) yes C13B C14B C15B 131.4(6) yes N4B C15B C14B 112.0(5) yes C14B C15B C16B 106.5(6) yes N4B C15B C16B 110.2(6) yes NA1B C17B N1B 117.1(4) yes N1B C17B C22B 113.6(5) yes N1B C17B C18B 127.9(6) yes NA1B C17B C22B 72.9(3) yes NA1B C17B C18B 77.4(4) yes C18B C17B C22B 118.4(6) yes NA1B C18B C17B 73.4(4) yes C17B C18B C19B 121.1(6) yes NA1B C18B C19B 76.6(4) yes C18B C19B C20B 120.1(6) yes NA1B C20B C19B 76.8(4) yes C19B C20B C21B 120.7(7) yes NA1B C20B C21B 72.1(4) yes NA1B C21B C20B 78.4(4) yes C20B C21B C22B 120.9(7) yes NA1B C21B C22B 74.7(4) yes C17B C22B C21B 118.8(6) yes N4B C22B C21B 127.9(6) yes N4B C22B C17B 113.2(6) yes NA1B C22B C21B 75.9(4) yes NA1B C22B C17B 76.0(3) yes NA1B C22B N4B 114.0(4) yes O1B C23B C24B 105.8(7) yes C23B C24B C25B 105.3(8) yes C24B C25B C26B 104.0(8) yes O1B C26B C25B 106.0(7) yes O2B C27B C28D 99(2) yes O2B C27B C27D 84(3) yes O2B C27B C28B 97(2) yes C27D C27B C28D 56(3) yes C28B C27B C28D 55(2) yes C28B C27B C27D 111(4) yes C27B C28B C30D 82(2) yes C27B C28B C29B 102(3) yes C27B C28B C28D 65(2) yes C27B C28B C27D 19(1) yes C29B C28B C30D 52(2) yes C28D C28B C30D 94(2) yes C28D C28B C29B 62(2) yes C27D C28B C30D 81(2) yes C27D C28B C29B 88(2) yes C27D C28B C28D 47(2) yes C27B C27D C28B 50(3) yes O2B C27D C28B 81(1) yes O2B C27D C27B 69(3) yes C28B C27D C28D 51(2) yes C27B C27D C28D 100(3) yes O2B C27D C28D 108(2) yes C28B C28D C27D 82(2) yes C27B C28D C27D 23(1) yes C27B C28D C28B 59(2) yes C27D C28D C29B 107(2) yes C28B C28D C29B 57(2) yes C27B C28D C29B 95(2) yes C28B C29B C28D 61(2) yes C28D C29B C30D 109(2) yes C28D C29B C30B 103(2) yes C28B C29B C30D 75(2) yes C28B C29B C30B 100(2) yes C30B C29B C30D 33(1) yes O2B C30B C29B 107(2) yes C29B C30B C30D 74(2) yes O2B C30B C30D 79(2) yes C29B C30D C30B 73(2) yes C28B C30D C30B 112(3) yes C28B C30D C29B 53(2) yes O2B C30D C30B 70(2) yes O2B C30D C29B 103(1) yes O2B C30D C28B 85(2) yes O3B C31B C32B 105.9(7) yes C31B C32B C33B 107.8(9) yes C32B C33B C34B 103.9(9) yes O3B C34B C33B 106.0(8) yes _refine_diff_density_max 1.21 _refine_diff_density_min -0.57 _refine_diff_density_rms 0.00 #===END ### END OF FILE ###