# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'George Newkome' 'Luis Echegoyen' 'Frank R. Fronczek' 'Seok-Ho Hwang' 'Olena Lukoyanova' 'Charles N. Moorfield' _publ_contact_author_name 'Prof George Newkome' _publ_contact_author_address ; Polymer Science University of Akron 170 University Cr. Goodyear Polymer Ctr. Akron OH 44325 UNITED STATES OF AMERICA ; _publ_contact_author_email NEWKOME@UAKRON.EDU _publ_requested_journal 'Chemical Communications' _publ_section_title ; Construction of Triangular Alkyne Metallomacrocycles: [M3(1,2-Bis(2,2':6',2''-terpyridin-4-ylethynyl)benzene)3][M= Fe(II), Ru(II)] ; data_SH-002-52 _database_code_depnum_ccdc_archive 'CCDC 252799' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_compound_source 'local laboratory' _chemical_formula_moiety 'C40 H24 N6' _chemical_formula_sum 'C40 H24 N6' _chemical_formula_weight 588.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' _symmetry_cell_setting Triclinic loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.8137(10) _cell_length_b 12.4510(10) _cell_length_c 13.061(2) _cell_angle_alpha 68.247(5) _cell_angle_beta 75.799(5) _cell_angle_gamma 66.262(7) _cell_volume 1485.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 102 _cell_measurement_reflns_used 10180 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 32.6 _exptl_crystal_description fragment _exptl_crystal_colour colorless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.316 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 612 _exptl_absorpt_coefficient_mu 0.080 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 102 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'KappaCCD (with Oxford Cryostream)' _diffrn_measurement_method ' \w scans with \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <2 _diffrn_reflns_number 50790 _diffrn_reflns_av_R_equivalents 0.038 _diffrn_reflns_av_sigmaI/netI 0.061 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.8 _diffrn_reflns_theta_max 32.6 _reflns_number_total 10773 _reflns_number_gt 6775 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Nonius, 2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0626P)^2^+0.2084P] 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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0052(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10773 _refine_ls_number_parameters 443 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.102 _refine_ls_R_factor_gt 0.054 _refine_ls_wR_factor_ref 0.141 _refine_ls_wR_factor_gt 0.122 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.70030(10) 0.39861(9) -0.02000(8) 0.0193(2) Uani 1 1 d . . . N2 N 0.45872(10) 0.27587(9) 0.18188(9) 0.0248(2) Uani 1 1 d . . . N3 N 0.94019(10) 0.55217(10) -0.15795(8) 0.0238(2) Uani 1 1 d . . . N4 N 0.84459(10) 0.00278(9) 0.62412(8) 0.0207(2) Uani 1 1 d . . . N5 N 0.79310(11) 0.07932(10) 0.34018(9) 0.0290(2) Uani 1 1 d . . . C1 C 0.59405(11) 0.69744(10) 0.35888(9) 0.0181(2) Uani 1 1 d . . . C2 C 0.61414(11) 0.63342(10) 0.47147(9) 0.0179(2) Uani 1 1 d . . . C3 C 0.58502(12) 0.70077(11) 0.54535(10) 0.0218(2) Uani 1 1 d . . . H3 H 0.6001 0.6586 0.6209 0.026 Uiso 1 1 calc R . . C4 C 0.53462(13) 0.82795(11) 0.50878(11) 0.0258(3) Uani 1 1 d . . . H4 H 0.5135 0.8728 0.5596 0.031 Uiso 1 1 calc R . . C5 C 0.51466(13) 0.89068(11) 0.39827(11) 0.0271(3) Uani 1 1 d . . . H5 H 0.4799 0.9782 0.3737 0.033 Uiso 1 1 calc R . . C6 C 0.54509(13) 0.82631(11) 0.32376(10) 0.0237(2) Uani 1 1 d . . . H6 H 0.5326 0.8700 0.2479 0.028 Uiso 1 1 calc R . . C7 C 0.62158(12) 0.63195(10) 0.28071(9) 0.0209(2) Uani 1 1 d . . . C8 C 0.64296(12) 0.58021(11) 0.21376(10) 0.0217(2) Uani 1 1 d . . . C9 C 0.66586(12) 0.51678(10) 0.13473(9) 0.0202(2) Uani 1 1 d . . . C10 C 0.60235(12) 0.43181(11) 0.15645(10) 0.0214(2) Uani 1 1 d . . . H10 H 0.5467 0.4128 0.2244 0.026 Uiso 1 1 calc R . . C11 C 0.62185(11) 0.37517(10) 0.07663(9) 0.0196(2) Uani 1 1 d . . . C12 C 0.76311(11) 0.47898(10) -0.03983(9) 0.0182(2) Uani 1 1 d . . . C13 C 0.74919(12) 0.54038(10) 0.03496(9) 0.0194(2) Uani 1 1 d . . . H13 H 0.7952 0.5967 0.0184 0.023 Uiso 1 1 calc R . . C14 C 0.55276(12) 0.28712(10) 0.09283(10) 0.0209(2) Uani 1 1 d . . . C15 C 0.58421(13) 0.22228(11) 0.01745(11) 0.0258(3) Uani 1 1 d . . . H15 H 0.6525 0.2310 -0.0435 0.031 Uiso 1 1 calc R . . C16 C 0.51372(14) 0.14471(12) 0.03321(12) 0.0321(3) Uani 1 1 d . . . H16 H 0.5330 0.0993 -0.0168 0.039 Uiso 1 1 calc R . . C17 C 0.41521(14) 0.13454(12) 0.12257(12) 0.0335(3) Uani 1 1 d . . . H17 H 0.3646 0.0829 0.1347 0.040 Uiso 1 1 calc R . . C18 C 0.39173(13) 0.20135(12) 0.19427(12) 0.0299(3) Uani 1 1 d . . . H18 H 0.3240 0.1937 0.2558 0.036 Uiso 1 1 calc R . . C19 C 0.84863(11) 0.50094(10) -0.14837(9) 0.0190(2) Uani 1 1 d . . . C20 C 0.83139(12) 0.46874(12) -0.23416(10) 0.0239(2) Uani 1 1 d . . . H20 H 0.7657 0.4320 -0.2243 0.029 Uiso 1 1 calc R . . C21 C 0.91260(13) 0.49166(13) -0.33432(11) 0.0293(3) Uani 1 1 d . . . H21 H 0.9023 0.4721 -0.3948 0.035 Uiso 1 1 calc R . . C22 C 1.00851(13) 0.54328(13) -0.34508(11) 0.0290(3) Uani 1 1 d . . . H22 H 1.0664 0.5586 -0.4124 0.035 Uiso 1 1 calc R . . C23 C 1.01807(12) 0.57203(12) -0.25531(11) 0.0265(3) Uani 1 1 d . . . H23 H 1.0838 0.6080 -0.2631 0.032 Uiso 1 1 calc R . . C24 C 0.66200(11) 0.50130(11) 0.50979(9) 0.0200(2) Uani 1 1 d . . . C25 C 0.70261(12) 0.39155(11) 0.53911(10) 0.0221(2) Uani 1 1 d . . . C26 C 0.75221(12) 0.25921(11) 0.56878(10) 0.0210(2) Uani 1 1 d . . . C27 C 0.76810(12) 0.20254(11) 0.48954(10) 0.0220(2) Uani 1 1 d . . . H27 H 0.7487 0.2504 0.4157 0.026 Uiso 1 1 calc R . . C28 C 0.81321(11) 0.07393(11) 0.52154(10) 0.0208(2) Uani 1 1 d . . . C29 C 0.83179(11) 0.05771(10) 0.69940(10) 0.0202(2) Uani 1 1 d . A . C30 C 0.78462(11) 0.18547(10) 0.67562(10) 0.0209(2) Uani 1 1 d . . . H30 H 0.7748 0.2215 0.7311 0.025 Uiso 1 1 calc R . . C31 C 0.82498(12) 0.00835(11) 0.44288(10) 0.0217(2) Uani 1 1 d . . . C32 C 0.86519(13) -0.11974(11) 0.47634(11) 0.0251(3) Uani 1 1 d . . . H32 H 0.8871 -0.1672 0.5497 0.030 Uiso 1 1 calc R . . C33 C 0.87259(14) -0.17652(13) 0.40085(11) 0.0305(3) Uani 1 1 d . . . H33 H 0.8989 -0.2636 0.4217 0.037 Uiso 1 1 calc R . . C34 C 0.84106(14) -0.10454(13) 0.29467(12) 0.0320(3) Uani 1 1 d . . . H34 H 0.8460 -0.1411 0.2408 0.038 Uiso 1 1 calc R . . C35 C 0.80196(14) 0.02236(13) 0.26847(11) 0.0327(3) Uani 1 1 d . . . H35 H 0.7803 0.0715 0.1954 0.039 Uiso 1 1 calc R . . C36 C 0.86997(12) -0.02629(11) 0.81062(10) 0.0242(2) Uani 1 1 d . . . C37 C 0.93077(13) -0.15280(11) 0.83016(11) 0.0272(3) Uani 1 1 d . A . H37 H 0.9498 -0.1866 0.7713 0.033 Uiso 1 1 calc R . . C38 C 0.96347(15) -0.22923(13) 0.93423(12) 0.0361(3) Uani 1 1 d . . . H38A H 0.9835 -0.3161 0.9550 0.043 Uiso 0.50 1 d PR A . H38B H 1.0243 -0.3117 0.9446 0.043 Uiso 0.50 1 d PR . . N6A N 0.8672(3) 0.0335(3) 0.8851(3) 0.0284(7) Uani 0.50 1 d P A 1 C39A C 0.9656(4) -0.1678(4) 1.0119(4) 0.0382(9) Uani 0.50 1 d P A 1 H39A H 1.0025 -0.2151 1.0805 0.046 Uiso 0.50 1 calc PR A 1 C40A C 0.9124(4) -0.0395(3) 0.9821(3) 0.0394(8) Uani 0.50 1 d P A 1 H40A H 0.9082 -0.0018 1.0347 0.047 Uiso 0.50 1 calc PR A 1 N6B N 0.8166(4) 0.0178(3) 0.8936(3) 0.0322(7) Uani 0.50 1 d P A 2 C39B C 0.9084(5) -0.1858(4) 1.0191(4) 0.0443(11) Uani 0.50 1 d P A 2 H39B H 0.9153 -0.2390 1.0933 0.053 Uiso 0.50 1 calc PR A 2 C40B C 0.8398(5) -0.0593(3) 0.9965(3) 0.0493(10) Uani 0.50 1 d P A 2 H40B H 0.8079 -0.0259 1.0567 0.059 Uiso 0.50 1 calc PR A 2 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 N1 0.0203(5) 0.0189(4) 0.0171(5) -0.0054(4) -0.0030(4) -0.0048(4) N2 0.0224(5) 0.0234(5) 0.0224(5) -0.0010(4) -0.0033(4) -0.0067(4) N3 0.0228(5) 0.0278(5) 0.0214(5) -0.0097(4) -0.0002(4) -0.0088(4) N4 0.0191(5) 0.0207(5) 0.0197(5) -0.0044(4) -0.0035(4) -0.0053(4) N5 0.0306(6) 0.0293(6) 0.0224(5) -0.0078(4) -0.0062(4) -0.0038(5) C1 0.0202(5) 0.0177(5) 0.0180(5) -0.0069(4) -0.0002(4) -0.0078(4) C2 0.0173(5) 0.0198(5) 0.0181(5) -0.0067(4) -0.0004(4) -0.0080(4) C3 0.0224(5) 0.0277(6) 0.0178(5) -0.0092(5) -0.0001(4) -0.0104(5) C4 0.0270(6) 0.0259(6) 0.0312(7) -0.0175(5) -0.0014(5) -0.0091(5) C5 0.0322(7) 0.0176(5) 0.0328(7) -0.0094(5) -0.0054(5) -0.0074(5) C6 0.0287(6) 0.0196(5) 0.0216(6) -0.0035(4) -0.0044(5) -0.0088(5) C7 0.0228(6) 0.0198(5) 0.0179(5) -0.0037(4) -0.0019(4) -0.0073(5) C8 0.0238(6) 0.0218(6) 0.0173(5) -0.0055(4) -0.0016(4) -0.0067(5) C9 0.0220(5) 0.0200(5) 0.0165(5) -0.0069(4) -0.0040(4) -0.0031(4) C10 0.0226(6) 0.0230(6) 0.0160(5) -0.0061(4) -0.0009(4) -0.0061(5) C11 0.0196(5) 0.0193(5) 0.0174(5) -0.0043(4) -0.0031(4) -0.0048(4) C12 0.0177(5) 0.0187(5) 0.0163(5) -0.0058(4) -0.0032(4) -0.0031(4) C13 0.0212(5) 0.0193(5) 0.0178(5) -0.0065(4) -0.0033(4) -0.0056(4) C14 0.0208(5) 0.0183(5) 0.0203(6) -0.0022(4) -0.0063(4) -0.0046(4) C15 0.0297(6) 0.0238(6) 0.0245(6) -0.0066(5) -0.0041(5) -0.0102(5) C16 0.0378(7) 0.0261(6) 0.0374(8) -0.0093(6) -0.0088(6) -0.0137(6) C17 0.0317(7) 0.0248(6) 0.0438(8) -0.0023(6) -0.0098(6) -0.0138(6) C18 0.0239(6) 0.0254(6) 0.0315(7) 0.0018(5) -0.0037(5) -0.0090(5) C19 0.0180(5) 0.0179(5) 0.0183(5) -0.0069(4) -0.0018(4) -0.0026(4) C20 0.0246(6) 0.0297(6) 0.0193(6) -0.0103(5) -0.0013(5) -0.0092(5) C21 0.0293(6) 0.0388(7) 0.0212(6) -0.0153(5) 0.0010(5) -0.0099(6) C22 0.0235(6) 0.0374(7) 0.0204(6) -0.0099(5) 0.0042(5) -0.0078(5) C23 0.0207(6) 0.0310(6) 0.0265(6) -0.0093(5) 0.0012(5) -0.0095(5) C24 0.0195(5) 0.0241(6) 0.0169(5) -0.0062(4) -0.0009(4) -0.0091(5) C25 0.0214(5) 0.0243(6) 0.0204(6) -0.0045(5) -0.0016(5) -0.0103(5) C26 0.0190(5) 0.0201(5) 0.0222(6) -0.0030(4) -0.0025(4) -0.0082(4) C27 0.0227(6) 0.0212(5) 0.0194(6) -0.0012(4) -0.0044(5) -0.0082(5) C28 0.0191(5) 0.0223(6) 0.0198(6) -0.0046(4) -0.0037(4) -0.0067(5) C29 0.0175(5) 0.0211(5) 0.0193(6) -0.0040(4) -0.0023(4) -0.0059(4) C30 0.0199(5) 0.0205(5) 0.0208(6) -0.0046(4) -0.0029(4) -0.0066(4) C31 0.0186(5) 0.0243(6) 0.0207(6) -0.0064(5) -0.0029(4) -0.0058(5) C32 0.0266(6) 0.0247(6) 0.0218(6) -0.0060(5) -0.0020(5) -0.0080(5) C33 0.0334(7) 0.0286(7) 0.0300(7) -0.0122(5) 0.0001(6) -0.0103(6) C34 0.0319(7) 0.0387(7) 0.0286(7) -0.0180(6) -0.0009(6) -0.0098(6) C35 0.0342(7) 0.0372(7) 0.0216(6) -0.0102(6) -0.0073(5) -0.0040(6) C36 0.0227(6) 0.0234(6) 0.0198(6) -0.0048(5) -0.0031(5) -0.0025(5) C37 0.0301(6) 0.0233(6) 0.0257(6) -0.0049(5) -0.0076(5) -0.0065(5) C38 0.0378(8) 0.0260(7) 0.0297(7) -0.0043(5) -0.0111(6) 0.0039(6) N6A 0.0345(18) 0.0279(15) 0.0175(12) -0.0092(10) -0.0040(13) -0.0028(13) C39A 0.045(2) 0.035(2) 0.0197(15) -0.0056(13) -0.0113(16) 0.0022(16) C40A 0.050(2) 0.0344(17) 0.0194(14) -0.0094(12) -0.0061(15) 0.0015(16) N6B 0.050(2) 0.0214(13) 0.0230(14) -0.0073(10) -0.0174(16) -0.0022(15) C39B 0.073(3) 0.0237(16) 0.0265(18) -0.0059(13) -0.028(2) 0.004(2) C40B 0.084(3) 0.0296(17) 0.0219(16) -0.0147(13) -0.021(2) 0.0079(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C11 1.3411(14) . ? N1 C12 1.3411(14) . ? N2 C18 1.3357(16) . ? N2 C14 1.3490(15) . ? N3 C19 1.3384(15) . ? N3 C23 1.3404(16) . ? N4 C28 1.3403(15) . ? N4 C29 1.3450(15) . ? N5 C35 1.3354(17) . ? N5 C31 1.3423(16) . ? C1 C6 1.3982(16) . ? C1 C2 1.4119(16) . ? C1 C7 1.4382(15) . ? C2 C3 1.4041(15) . ? C2 C24 1.4338(16) . ? C3 C4 1.3802(17) . ? C3 H3 0.9500 . ? C4 C5 1.3862(18) . ? C4 H4 0.9500 . ? C5 C6 1.3807(17) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.1965(16) . ? C8 C9 1.4394(16) . ? C9 C10 1.3922(16) . ? C9 C13 1.3962(16) . ? C10 C11 1.3951(16) . ? C10 H10 0.9500 . ? C11 C14 1.4883(16) . ? C12 C13 1.3965(15) . ? C12 C19 1.4875(16) . ? C13 H13 0.9500 . ? C14 C15 1.3930(17) . ? C15 C16 1.3873(17) . ? C15 H15 0.9500 . ? C16 C17 1.379(2) . ? C16 H16 0.9500 . ? C17 C18 1.387(2) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.3952(16) . ? C20 C21 1.3875(17) . ? C20 H20 0.9500 . ? C21 C22 1.3809(18) . ? C21 H21 0.9500 . ? C22 C23 1.3834(18) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C25 1.1910(16) . ? C25 C26 1.4388(16) . ? C26 C30 1.3943(17) . ? C26 C27 1.3982(16) . ? C27 C28 1.3971(16) . ? C27 H27 0.9500 . ? C28 C31 1.4875(16) . ? C29 C30 1.3947(16) . ? C29 C36 1.4816(17) . ? C30 H30 0.9500 . ? C31 C32 1.3935(17) . ? C32 C33 1.3823(17) . ? C32 H32 0.9500 . ? C33 C34 1.381(2) . ? C33 H33 0.9500 . ? C34 C35 1.3874(19) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 N6B 1.299(4) . ? C36 C37 1.3889(17) . ? C36 N6A 1.417(4) . ? C37 C38 1.3726(18) . ? C37 H37 0.9500 . ? C38 C39B 1.318(5) . ? C38 C39A 1.489(5) . ? C38 H38A 0.9550 . ? C38 H38B 0.9500 . ? N6A C40A 1.328(5) . ? C39A C40A 1.394(6) . ? C39A H39A 0.9500 . ? C40A H40A 0.9500 . ? N6B C40B 1.344(5) . ? C39B C40B 1.394(5) . ? C39B H39B 0.9500 . ? C40B H40B 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 N1 C12 118.44(10) . . ? C18 N2 C14 117.07(11) . . ? C19 N3 C23 117.16(10) . . ? C28 N4 C29 118.50(10) . . ? C35 N5 C31 117.32(11) . . ? C6 C1 C2 119.23(10) . . ? C6 C1 C7 119.86(11) . . ? C2 C1 C7 120.91(10) . . ? C3 C2 C1 119.17(10) . . ? C3 C2 C24 120.61(10) . . ? C1 C2 C24 120.22(10) . . ? C4 C3 C2 120.36(11) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 120.40(11) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C6 C5 C4 120.20(11) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C5 C6 C1 120.63(11) . . ? C5 C6 H6 119.7 . . ? C1 C6 H6 119.7 . . ? C8 C7 C1 178.35(13) . . ? C7 C8 C9 178.52(13) . . ? C10 C9 C13 118.93(10) . . ? C10 C9 C8 119.88(10) . . ? C13 C9 C8 121.19(10) . . ? C9 C10 C11 118.80(10) . . ? C9 C10 H10 120.6 . . ? C11 C10 H10 120.6 . . ? N1 C11 C10 122.58(10) . . ? N1 C11 C14 115.91(10) . . ? C10 C11 C14 121.49(10) . . ? N1 C12 C13 122.98(10) . . ? N1 C12 C19 115.83(9) . . ? C13 C12 C19 121.19(10) . . ? C9 C13 C12 118.26(10) . . ? C9 C13 H13 120.9 . . ? C12 C13 H13 120.9 . . ? N2 C14 C15 122.90(11) . . ? N2 C14 C11 116.66(10) . . ? C15 C14 C11 120.43(11) . . ? C16 C15 C14 118.61(12) . . ? C16 C15 H15 120.7 . . ? C14 C15 H15 120.7 . . ? C17 C16 C15 119.02(13) . . ? C17 C16 H16 120.5 . . ? C15 C16 H16 120.5 . . ? C16 C17 C18 118.49(12) . . ? C16 C17 H17 120.8 . . ? C18 C17 H17 120.8 . . ? N2 C18 C17 123.87(12) . . ? N2 C18 H18 118.1 . . ? C17 C18 H18 118.1 . . ? N3 C19 C20 123.12(11) . . ? N3 C19 C12 116.66(10) . . ? C20 C19 C12 120.22(10) . . ? C21 C20 C19 118.34(11) . . ? C21 C20 H20 120.8 . . ? C19 C20 H20 120.8 . . ? C22 C21 C20 119.20(12) . . ? C22 C21 H21 120.4 . . ? C20 C21 H21 120.4 . . ? C21 C22 C23 118.25(11) . . ? C21 C22 H22 120.9 . . ? C23 C22 H22 120.9 . . ? N3 C23 C22 123.93(12) . . ? N3 C23 H23 118.0 . . ? C22 C23 H23 118.0 . . ? C25 C24 C2 178.47(12) . . ? C24 C25 C26 177.10(13) . . ? C30 C26 C27 118.90(11) . . ? C30 C26 C25 121.36(11) . . ? C27 C26 C25 119.75(11) . . ? C28 C27 C26 118.45(11) . . ? C28 C27 H27 120.8 . . ? C26 C27 H27 120.8 . . ? N4 C28 C27 122.80(11) . . ? N4 C28 C31 116.15(10) . . ? C27 C28 C31 121.03(11) . . ? N4 C29 C30 122.67(11) . . ? N4 C29 C36 115.73(10) . . ? C30 C29 C36 121.60(11) . . ? C26 C30 C29 118.66(11) . . ? C26 C30 H30 120.7 . . ? C29 C30 H30 120.7 . . ? N5 C31 C32 122.81(11) . . ? N5 C31 C28 116.33(10) . . ? C32 C31 C28 120.85(11) . . ? C33 C32 C31 118.79(12) . . ? C33 C32 H32 120.6 . . ? C31 C32 H32 120.6 . . ? C34 C33 C32 118.93(12) . . ? C34 C33 H33 120.5 . . ? C32 C33 H33 120.5 . . ? C33 C34 C35 118.42(12) . . ? C33 C34 H34 120.8 . . ? C35 C34 H34 120.8 . . ? N5 C35 C34 123.72(13) . . ? N5 C35 H35 118.1 . . ? C34 C35 H35 118.1 . . ? N6B C36 C37 119.86(19) . . ? N6B C36 N6A 26.11(15) . . ? C37 C36 N6A 122.97(18) . . ? N6B C36 C29 117.06(18) . . ? C37 C36 C29 121.15(11) . . ? N6A C36 C29 114.49(18) . . ? C38 C37 C36 120.24(12) . . ? C38 C37 H37 119.9 . . ? C36 C37 H37 119.9 . . ? C39B C38 C37 118.6(2) . . ? C39B C38 C39A 28.6(2) . . ? C37 C38 C39A 115.6(2) . . ? C39B C38 H38A 112.2 . . ? C37 C38 H38A 121.9 . . ? C39A C38 H38A 122.5 . . ? C39B C38 H38B 120.9 . . ? C37 C38 H38B 120.5 . . ? C39A C38 H38B 116.1 . . ? H38A C38 H38B 27.2 . . ? C40A N6A C36 116.1(3) . . ? C40A C39A C38 118.6(3) . . ? C40A C39A H39A 120.7 . . ? C38 C39A H39A 120.7 . . ? N6A C40A C39A 124.5(4) . . ? N6A C40A H40A 117.8 . . ? C39A C40A H40A 117.8 . . ? C36 N6B C40B 118.3(3) . . ? C38 C39B C40B 117.8(3) . . ? C38 C39B H39B 121.1 . . ? C40B C39B H39B 121.1 . . ? N6B C40B C39B 123.1(3) . . ? N6B C40B H40B 118.5 . . ? C39B C40B H40B 118.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -0.28(16) . . . . ? C7 C1 C2 C3 -179.48(10) . . . . ? C6 C1 C2 C24 178.91(10) . . . . ? C7 C1 C2 C24 -0.30(16) . . . . ? C1 C2 C3 C4 1.38(17) . . . . ? C24 C2 C3 C4 -177.80(11) . . . . ? C2 C3 C4 C5 -1.26(18) . . . . ? C3 C4 C5 C6 0.01(19) . . . . ? C4 C5 C6 C1 1.11(19) . . . . ? C2 C1 C6 C5 -0.96(17) . . . . ? C7 C1 C6 C5 178.25(11) . . . . ? C6 C1 C7 C8 -9(4) . . . . ? C2 C1 C7 C8 170(4) . . . . ? C1 C7 C8 C9 -105(6) . . . . ? C7 C8 C9 C10 -11(5) . . . . ? C7 C8 C9 C13 168(5) . . . . ? C13 C9 C10 C11 -1.39(17) . . . . ? C8 C9 C10 C11 177.48(11) . . . . ? C12 N1 C11 C10 0.56(16) . . . . ? C12 N1 C11 C14 178.85(10) . . . . ? C9 C10 C11 N1 0.53(17) . . . . ? C9 C10 C11 C14 -177.66(11) . . . . ? C11 N1 C12 C13 -0.80(16) . . . . ? C11 N1 C12 C19 179.97(10) . . . . ? C10 C9 C13 C12 1.17(16) . . . . ? C8 C9 C13 C12 -177.68(11) . . . . ? N1 C12 C13 C9 -0.07(17) . . . . ? C19 C12 C13 C9 179.12(10) . . . . ? C18 N2 C14 C15 -2.00(17) . . . . ? C18 N2 C14 C11 177.00(10) . . . . ? N1 C11 C14 N2 -170.81(10) . . . . ? C10 C11 C14 N2 7.50(16) . . . . ? N1 C11 C14 C15 8.22(16) . . . . ? C10 C11 C14 C15 -173.48(11) . . . . ? N2 C14 C15 C16 1.44(19) . . . . ? C11 C14 C15 C16 -177.52(11) . . . . ? C14 C15 C16 C17 0.05(19) . . . . ? C15 C16 C17 C18 -0.8(2) . . . . ? C14 N2 C18 C17 1.14(19) . . . . ? C16 C17 C18 N2 0.3(2) . . . . ? C23 N3 C19 C20 -0.28(18) . . . . ? C23 N3 C19 C12 179.81(10) . . . . ? N1 C12 C19 N3 -162.13(10) . . . . ? C13 C12 C19 N3 18.63(16) . . . . ? N1 C12 C19 C20 17.95(16) . . . . ? C13 C12 C19 C20 -161.29(11) . . . . ? N3 C19 C20 C21 -0.39(18) . . . . ? C12 C19 C20 C21 179.53(11) . . . . ? C19 C20 C21 C22 1.05(19) . . . . ? C20 C21 C22 C23 -1.0(2) . . . . ? C19 N3 C23 C22 0.28(19) . . . . ? C21 C22 C23 N3 0.4(2) . . . . ? C3 C2 C24 C25 -166(5) . . . . ? C1 C2 C24 C25 15(5) . . . . ? C2 C24 C25 C26 -11(7) . . . . ? C24 C25 C26 C30 172(2) . . . . ? C24 C25 C26 C27 -8(2) . . . . ? C30 C26 C27 C28 1.36(17) . . . . ? C25 C26 C27 C28 -178.41(10) . . . . ? C29 N4 C28 C27 0.13(16) . . . . ? C29 N4 C28 C31 -178.08(10) . . . . ? C26 C27 C28 N4 -1.48(17) . . . . ? C26 C27 C28 C31 176.65(10) . . . . ? C28 N4 C29 C30 1.35(16) . . . . ? C28 N4 C29 C36 -179.17(10) . . . . ? C27 C26 C30 C29 0.01(16) . . . . ? C25 C26 C30 C29 179.77(10) . . . . ? N4 C29 C30 C26 -1.42(17) . . . . ? C36 C29 C30 C26 179.13(10) . . . . ? C35 N5 C31 C32 -0.43(18) . . . . ? C35 N5 C31 C28 -179.50(11) . . . . ? N4 C28 C31 N5 179.73(10) . . . . ? C27 C28 C31 N5 1.48(16) . . . . ? N4 C28 C31 C32 0.65(16) . . . . ? C27 C28 C31 C32 -177.61(11) . . . . ? N5 C31 C32 C33 -0.05(18) . . . . ? C28 C31 C32 C33 178.97(11) . . . . ? C31 C32 C33 C34 0.55(19) . . . . ? C32 C33 C34 C35 -0.6(2) . . . . ? C31 N5 C35 C34 0.4(2) . . . . ? C33 C34 C35 N5 0.1(2) . . . . ? N4 C29 C36 N6B -156.46(19) . . . . ? C30 C29 C36 N6B 23.0(2) . . . . ? N4 C29 C36 C37 7.69(17) . . . . ? C30 C29 C36 C37 -172.83(11) . . . . ? N4 C29 C36 N6A 174.63(16) . . . . ? C30 C29 C36 N6A -5.9(2) . . . . ? N6B C36 C37 C38 -15.3(2) . . . . ? N6A C36 C37 C38 15.2(2) . . . . ? C29 C36 C37 C38 -179.00(12) . . . . ? C36 C37 C38 C39B 15.9(3) . . . . ? C36 C37 C38 C39A -16.2(3) . . . . ? N6B C36 N6A C40A 83.9(7) . . . . ? C37 C36 N6A C40A -7.5(4) . . . . ? C29 C36 N6A C40A -174.2(3) . . . . ? C39B C38 C39A C40A -92.1(7) . . . . ? C37 C38 C39A C40A 11.2(4) . . . . ? C36 N6A C40A C39A 2.5(5) . . . . ? C38 C39A C40A N6A -4.6(6) . . . . ? C37 C36 N6B C40B 9.8(4) . . . . ? N6A C36 N6B C40B -94.9(7) . . . . ? C29 C36 N6B C40B 174.2(3) . . . . ? C37 C38 C39B C40B -11.3(5) . . . . ? C39A C38 C39B C40B 80.3(7) . . . . ? C36 N6B C40B C39B -5.6(7) . . . . ? C38 C39B C40B N6B 6.4(7) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 32.6 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.36 _refine_diff_density_min -0.26 _refine_diff_density_rms 0.052 # END OF CIF