# Supplementary Material (ESI) for Perkin Transactions # This journal is © The Royal Society of Chemistry 2002 data_v61-l2 _database_code_CSD 177482 _journal_coden_Cambridge 207 loop_ _publ_author_name _publ_author_address 'Bark, Thomas' ; Department of Chemistry University of Fribourg Perolles 1700 Fribourg Switzerland ; ' Helen Stoeckli-Evans ' ; Institute of Chemistry University of Neuchatel Avenue de Bellevaux 51 2000 Neuchatel Switzerland ; 'von Zelewsky, Alex' ; Department of Chemistry University of Fribourg Perolles 1700 Fribourg Switzerland ; _publ_contact_author_name 'Prof Alexander von Zelewsky' _publ_contact_author_address ; Department of Chemistry University of Fribourg Perolles Fribourg CH-1700 SWITZERLAND ; _publ_contact_author_fax '+41-26-300 97 38' _publ_contact_author_email 'alexander.vonzelewsky@unifr.ch' _publ_requested_journal 'Perkin Transactions 1' _publ_section_title ; New Multitopic Ligands for Self-Assembly Reactions ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H36 N6' _chemical_formula_weight 576.73 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_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 12.9950(8) _cell_length_b 12.0640(10) _cell_length_c 19.5348(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3062.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6893 _cell_measurement_theta_min 1.98 _cell_measurement_theta_max 25.86 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.251 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 0.075 _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 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE Image Plate Diffraction System' _diffrn_measurement_method 'phi oscillation' _diffrn_detector_area_resol_mean 0.81\%A _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 17585 _diffrn_reflns_av_R_equivalents 0.0878 _diffrn_reflns_av_sigmaI/netI 0.1330 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 25.86 _reflns_number_total 5846 _reflns_number_gt 2403 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE (Stoe & Cie GmbH, Darmstadt, 1997)' _computing_cell_refinement 'CELL (Stoe & Cie GmbH, Darmstadt, 1997)' _computing_data_reduction 'INTEGRATE (Stoe & Cie GmbH, Darmstadt, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON/PLUTON (Spek, 1990)' _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^)+(0.0000P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00204(19) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -1(2) _refine_ls_number_reflns 5846 _refine_ls_number_parameters 512 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1207 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.0610 _refine_ls_wR_factor_gt 0.0518 _refine_ls_goodness_of_fit_ref 0.752 _refine_ls_restrained_S_all 0.752 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.001 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 -0.1527(2) -0.18795(19) -0.04679(14) 0.0656(7) Uani 1 1 d . . . N2 N -0.2681(2) -0.3401(2) -0.12178(13) 0.0628(7) Uani 1 1 d . . . N3 N -0.4042(2) -0.06552(18) -0.02840(11) 0.0532(6) Uani 1 1 d . . . N4 N -0.5968(2) 0.13496(19) 0.01862(12) 0.0617(7) Uani 1 1 d . . . N5 N -0.0170(2) -0.42577(18) -0.17153(12) 0.0561(7) Uani 1 1 d . . . N6 N 0.1870(3) -0.5624(2) -0.26313(14) 0.0751(9) Uani 1 1 d . . . C1 C -0.2550(2) -0.1785(2) -0.05169(16) 0.0526(8) Uani 1 1 d . . . C2 C -0.3117(3) -0.2547(3) -0.08777(16) 0.0586(8) Uani 1 1 d . . . H2 H -0.391(2) -0.2502(17) -0.0875(11) 0.049(8) Uiso 1 1 d . . . C3 C -0.1663(3) -0.3472(2) -0.11964(15) 0.0533(8) Uani 1 1 d . . . C4 C -0.1090(3) -0.2721(3) -0.08179(17) 0.0636(9) Uani 1 1 d . . . H4 H -0.026(2) -0.2807(16) -0.0744(11) 0.056(8) Uiso 1 1 d . . . C5 C -0.3020(3) -0.0830(2) -0.01589(14) 0.0525(8) Uani 1 1 d . . . C6 C -0.2425(3) -0.0168(3) 0.02635(17) 0.0653(9) Uani 1 1 d . . . H6 H -0.161(2) -0.0334(18) 0.0283(12) 0.058(8) Uiso 1 1 d . . . C7 C -0.2898(3) 0.0735(3) 0.05808(18) 0.0692(9) Uani 1 1 d . . . H7 H -0.225(3) 0.115(2) 0.0925(17) 0.134(13) Uiso 1 1 d . . . C8 C -0.3929(3) 0.0921(2) 0.04600(16) 0.0623(9) Uani 1 1 d . . . H8 H -0.444(2) 0.156(2) 0.0702(13) 0.079(9) Uiso 1 1 d . . . C9 C -0.4485(3) 0.0225(2) 0.00255(16) 0.0553(8) Uani 1 1 d . . . C10 C -0.5588(2) 0.0415(2) -0.00939(15) 0.0524(8) Uani 1 1 d . . . C11 C -0.6222(2) -0.0307(2) -0.04528(16) 0.0540(8) Uani 1 1 d . . . H11 H -0.5882(17) -0.0951(16) -0.0670(11) 0.041(7) Uiso 1 1 d . . . C12 C -0.7257(2) -0.0108(2) -0.05109(15) 0.0531(8) Uani 1 1 d . . . C13 C -0.8014(3) -0.0832(3) -0.0899(2) 0.0676(10) Uani 1 1 d . . . H13A H -0.795(2) -0.158(2) -0.0744(13) 0.080(10) Uiso 1 1 d . . . H13B H -0.7769(19) -0.0784(18) -0.1328(11) 0.039(9) Uiso 1 1 d . . . C14 C -0.9098(3) -0.0420(2) -0.0814(2) 0.0668(10) Uani 1 1 d . . . H14 H -0.961(2) -0.0824(18) -0.1050(12) 0.060(9) Uiso 1 1 d . . . C15 C -0.9208(2) 0.0838(2) -0.09762(15) 0.0531(8) Uani 1 1 d . . . C16 C -0.8806(2) 0.1012(3) -0.02328(15) 0.0565(9) Uani 1 1 d . . . H16 H -0.9059(18) 0.1638(18) 0.0002(11) 0.047(8) Uiso 1 1 d . . . C17 C -0.7665(2) 0.0853(2) -0.02053(14) 0.0520(8) Uani 1 1 d . . . C18 C -0.6975(3) 0.1547(3) 0.01220(16) 0.0642(9) Uani 1 1 d . . . H18 H -0.727(2) 0.223(2) 0.0377(14) 0.090(10) Uiso 1 1 d . . . C19 C -0.9313(3) -0.0117(3) -0.0068(2) 0.0861(12) Uani 1 1 d . . . H19A H -1.021(2) -0.0098(19) 0.0038(13) 0.079(9) Uiso 1 1 d . . . H19B H -0.899(2) -0.041(2) 0.0290(15) 0.072(11) Uiso 1 1 d . . . C20 C -0.8557(4) 0.1300(3) -0.15641(19) 0.0673(10) Uani 1 1 d . . . H20A H -0.907(3) 0.111(2) -0.1998(18) 0.114(12) Uiso 1 1 d . . . H20B H -0.781(3) 0.107(2) -0.1643(17) 0.108(13) Uiso 1 1 d . . . H20C H -0.865(2) 0.205(2) -0.1635(13) 0.066(10) Uiso 1 1 d . . . C21 C -1.0313(3) 0.1163(3) -0.1066(2) 0.0671(10) Uani 1 1 d . . . H21A H -1.057(2) 0.106(2) -0.1464(15) 0.073(12) Uiso 1 1 d . . . H21B H -1.049(2) 0.200(2) -0.1023(17) 0.108(12) Uiso 1 1 d . . . H21C H -1.078(2) 0.096(2) -0.0683(15) 0.082(11) Uiso 1 1 d . . . C22 C -0.1158(3) -0.4391(2) -0.15801(15) 0.0565(9) Uani 1 1 d . . . C23 C -0.1733(3) -0.5324(3) -0.17623(17) 0.0647(9) Uani 1 1 d . . . H23 H -0.254(2) -0.5359(18) -0.1691(13) 0.064(9) Uiso 1 1 d . . . C24 C -0.1220(3) -0.6157(3) -0.21103(18) 0.0725(11) Uani 1 1 d . . . H24 H -0.163(3) -0.681(2) -0.2259(16) 0.110(13) Uiso 1 1 d . . . C25 C -0.0211(4) -0.6026(3) -0.22648(18) 0.0674(10) Uani 1 1 d . . . H25 H 0.0200(19) -0.6484(18) -0.2524(12) 0.044(8) Uiso 1 1 d . . . C26 C 0.0310(3) -0.5062(2) -0.20673(15) 0.0575(9) Uani 1 1 d . . . C27 C 0.1404(3) -0.4870(2) -0.22277(16) 0.0583(8) Uani 1 1 d . . . C28 C 0.1925(3) -0.3960(2) -0.19732(16) 0.0562(9) Uani 1 1 d . . . H28 H 0.1555(18) -0.3470(17) -0.1707(12) 0.037(7) Uiso 1 1 d . . . C29 C 0.2951(3) -0.3809(2) -0.21324(15) 0.0560(8) Uani 1 1 d . . . C30 C 0.3590(3) -0.2834(3) -0.1884(2) 0.0688(10) Uani 1 1 d . . . H30A H 0.358(2) -0.290(2) -0.1392(14) 0.071(10) Uiso 1 1 d . . . H30B H 0.318(2) -0.207(2) -0.2017(14) 0.092(10) Uiso 1 1 d . . . C31 C 0.4692(3) -0.2921(3) -0.21351(18) 0.0765(11) Uani 1 1 d . . . H31 H 0.521(2) -0.2293(19) -0.1959(14) 0.083(9) Uiso 1 1 d . . . C32 C 0.4729(3) -0.3126(3) -0.29241(19) 0.0836(11) Uani 1 1 d . . . C33 C 0.4537(3) -0.4380(3) -0.2719(2) 0.0843(13) Uani 1 1 d . . . H33 H 0.479(3) -0.499(2) -0.2977(16) 0.101(12) Uiso 1 1 d . . . C34 C 0.3431(3) -0.4561(3) -0.25594(16) 0.0632(9) Uani 1 1 d . . . C35 C 0.2854(4) -0.5446(3) -0.27879(19) 0.0802(11) Uani 1 1 d . . . H35 H 0.3295(19) -0.5996(18) -0.3053(12) 0.057(8) Uiso 1 1 d . . . C36 C 0.5092(3) -0.4113(3) -0.2032(2) 0.0992(13) Uani 1 1 d . . . H36B H 0.4807 -0.4490 -0.1636 0.119 Uiso 1 1 calc R . . H36A H 0.5835 -0.4184 -0.2049 0.119 Uiso 1 1 calc R . . C37 C 0.3947(3) -0.2584(3) -0.33932(17) 0.1031(13) Uani 1 1 d . . . H37C H 0.3983 -0.2918 -0.3839 0.155 Uiso 1 1 calc R . . H37B H 0.4094 -0.1806 -0.3430 0.155 Uiso 1 1 calc R . . H37A H 0.3269 -0.2683 -0.3208 0.155 Uiso 1 1 calc R . . C38 C 0.5833(3) -0.2933(3) -0.3209(2) 0.1331(18) Uani 1 1 d . . . H38C H 0.5885 -0.3245 -0.3660 0.200 Uiso 1 1 calc R . . H38B H 0.6326 -0.3283 -0.2914 0.200 Uiso 1 1 calc R . . H38A H 0.5971 -0.2152 -0.3230 0.200 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.048(2) 0.0615(17) 0.087(2) -0.0077(16) -0.0068(16) -0.0010(15) N2 0.059(2) 0.0585(16) 0.0710(19) 0.0037(14) -0.0053(15) -0.0075(15) N3 0.0531(19) 0.0560(15) 0.0505(16) 0.0051(12) -0.0008(13) 0.0003(14) N4 0.063(2) 0.0640(17) 0.0583(17) -0.0123(13) -0.0069(15) 0.0068(15) N5 0.056(2) 0.0534(15) 0.0585(16) 0.0041(13) -0.0075(15) 0.0099(15) N6 0.071(3) 0.0666(18) 0.088(2) -0.0247(16) -0.0152(18) 0.0172(17) C1 0.039(2) 0.0554(19) 0.064(2) 0.0113(16) -0.0018(16) -0.0080(18) C2 0.041(2) 0.065(2) 0.070(2) 0.0159(18) -0.003(2) -0.0068(19) C3 0.041(2) 0.0523(19) 0.066(2) 0.0154(16) -0.0025(17) -0.0070(16) C4 0.044(2) 0.063(2) 0.084(3) 0.0020(18) -0.005(2) 0.0007(19) C5 0.049(2) 0.0559(18) 0.053(2) 0.0154(16) 0.0041(17) -0.0058(18) C6 0.055(3) 0.075(2) 0.066(2) -0.0009(19) -0.003(2) -0.008(2) C7 0.056(3) 0.086(3) 0.066(2) -0.0011(19) -0.005(2) -0.006(2) C8 0.062(3) 0.063(2) 0.062(2) -0.0044(18) 0.001(2) -0.008(2) C9 0.054(2) 0.0553(19) 0.057(2) 0.0107(16) 0.0022(17) -0.0046(18) C10 0.050(2) 0.0549(19) 0.053(2) 0.0036(16) 0.0005(16) -0.0026(17) C11 0.051(2) 0.0459(17) 0.065(2) -0.0017(17) 0.0065(18) 0.0068(18) C12 0.051(2) 0.0511(17) 0.057(2) 0.0005(16) 0.0019(17) 0.0029(17) C13 0.055(3) 0.051(2) 0.097(3) -0.006(2) -0.002(2) -0.0027(19) C14 0.049(2) 0.058(2) 0.094(3) -0.0046(19) -0.001(2) -0.0082(19) C15 0.051(2) 0.0505(16) 0.058(2) -0.0043(15) 0.0002(16) -0.0007(15) C16 0.062(3) 0.054(2) 0.054(2) -0.0033(17) 0.0050(17) 0.0095(17) C17 0.055(2) 0.0589(19) 0.0423(19) 0.0011(16) -0.0030(16) 0.0075(18) C18 0.063(3) 0.070(2) 0.060(2) -0.0150(18) -0.008(2) 0.011(2) C19 0.065(3) 0.101(3) 0.092(4) 0.041(3) 0.007(2) -0.001(2) C20 0.075(3) 0.070(2) 0.057(2) 0.0003(19) 0.005(2) -0.002(2) C21 0.057(3) 0.075(3) 0.070(3) -0.006(2) -0.009(2) 0.010(2) C22 0.064(3) 0.0455(18) 0.060(2) 0.0126(15) -0.0085(19) 0.0063(18) C23 0.068(3) 0.054(2) 0.073(2) 0.0062(17) -0.003(2) -0.012(2) C24 0.079(3) 0.054(2) 0.085(3) 0.007(2) -0.012(2) -0.013(2) C25 0.086(3) 0.044(2) 0.072(2) -0.0082(18) -0.021(2) 0.006(2) C26 0.062(3) 0.0515(19) 0.059(2) 0.0047(17) -0.0145(18) 0.0072(18) C27 0.068(3) 0.0519(18) 0.055(2) -0.0050(15) -0.0155(18) 0.0111(19) C28 0.065(3) 0.0486(19) 0.055(2) -0.0128(16) 0.0049(18) 0.0101(19) C29 0.063(3) 0.0521(18) 0.053(2) -0.0119(15) -0.0060(18) 0.0098(18) C30 0.072(3) 0.062(2) 0.073(3) -0.019(2) 0.009(2) -0.001(2) C31 0.057(3) 0.086(3) 0.086(3) -0.028(2) -0.010(2) 0.002(2) C32 0.064(3) 0.104(3) 0.083(3) -0.034(2) 0.007(2) 0.008(2) C33 0.069(3) 0.086(3) 0.098(3) -0.046(2) -0.009(2) 0.027(2) C34 0.051(2) 0.073(2) 0.066(2) -0.0224(18) -0.0118(18) 0.0148(19) C35 0.071(3) 0.071(2) 0.098(3) -0.037(2) -0.014(2) 0.022(2) C36 0.070(3) 0.099(3) 0.129(3) -0.023(2) -0.045(3) 0.021(2) C37 0.101(3) 0.141(3) 0.067(3) 0.007(2) 0.014(2) 0.005(3) C38 0.069(3) 0.182(4) 0.148(4) -0.074(3) 0.043(3) -0.014(3) _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 C1 1.337(3) . ? N1 C4 1.349(4) . ? N2 C3 1.327(3) . ? N2 C2 1.350(4) . ? N3 C9 1.351(3) . ? N3 C5 1.366(3) . ? N4 C18 1.336(4) . ? N4 C10 1.346(3) . ? N5 C22 1.321(4) . ? N5 C26 1.343(3) . ? N6 C35 1.332(4) . ? N6 C27 1.348(4) . ? C1 C2 1.373(4) . ? C1 C5 1.480(4) . ? C3 C4 1.387(4) . ? C3 C22 1.490(4) . ? C5 C6 1.384(4) . ? C6 C7 1.395(4) . ? C7 C8 1.379(4) . ? C8 C9 1.396(4) . ? C9 C10 1.471(4) . ? C10 C11 1.389(4) . ? C11 C12 1.371(4) . ? C12 C17 1.407(3) . ? C12 C13 1.518(4) . ? C13 C14 1.503(5) . ? C14 C19 1.528(5) . ? C14 C15 1.557(4) . ? C15 C21 1.500(4) . ? C15 C20 1.531(4) . ? C15 C16 1.557(4) . ? C16 C17 1.497(4) . ? C16 C19 1.547(4) . ? C17 C18 1.384(4) . ? C22 C23 1.397(4) . ? C23 C24 1.385(4) . ? C24 C25 1.355(5) . ? C25 C26 1.400(4) . ? C26 C27 1.474(4) . ? C27 C28 1.382(4) . ? C28 C29 1.381(4) . ? C29 C34 1.382(4) . ? C29 C30 1.519(4) . ? C30 C31 1.518(5) . ? C31 C36 1.542(4) . ? C31 C32 1.562(4) . ? C32 C37 1.517(4) . ? C32 C38 1.557(5) . ? C32 C33 1.584(5) . ? C33 C34 1.486(5) . ? C33 C36 1.558(5) . ? C34 C35 1.379(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 N1 C4 116.5(3) . . ? C3 N2 C2 116.9(3) . . ? C9 N3 C5 117.1(3) . . ? C18 N4 C10 118.0(3) . . ? C22 N5 C26 117.8(3) . . ? C35 N6 C27 117.2(3) . . ? N1 C1 C2 120.9(3) . . ? N1 C1 C5 116.3(3) . . ? C2 C1 C5 122.8(3) . . ? N2 C2 C1 122.5(3) . . ? N2 C3 C4 120.7(3) . . ? N2 C3 C22 118.1(3) . . ? C4 C3 C22 121.2(3) . . ? N1 C4 C3 122.4(3) . . ? N3 C5 C6 124.1(3) . . ? N3 C5 C1 115.9(3) . . ? C6 C5 C1 120.0(3) . . ? C5 C6 C7 118.0(4) . . ? C8 C7 C6 118.6(4) . . ? C7 C8 C9 120.6(3) . . ? N3 C9 C8 121.6(3) . . ? N3 C9 C10 117.9(3) . . ? C8 C9 C10 120.5(3) . . ? N4 C10 C11 120.9(3) . . ? N4 C10 C9 115.1(3) . . ? C11 C10 C9 124.1(3) . . ? C12 C11 C10 120.9(3) . . ? C11 C12 C17 118.6(3) . . ? C11 C12 C13 125.2(3) . . ? C17 C12 C13 116.2(3) . . ? C14 C13 C12 111.2(3) . . ? C13 C14 C19 110.8(3) . . ? C13 C14 C15 112.7(3) . . ? C19 C14 C15 86.9(2) . . ? C21 C15 C20 110.3(3) . . ? C21 C15 C16 113.2(3) . . ? C20 C15 C16 117.7(3) . . ? C21 C15 C14 111.5(3) . . ? C20 C15 C14 117.2(3) . . ? C16 C15 C14 84.9(2) . . ? C17 C16 C19 107.5(3) . . ? C17 C16 C15 110.4(3) . . ? C19 C16 C15 86.2(3) . . ? C18 C17 C12 116.8(3) . . ? C18 C17 C16 125.5(3) . . ? C12 C17 C16 117.6(3) . . ? N4 C18 C17 124.8(3) . . ? C14 C19 C16 86.2(3) . . ? N5 C22 C23 124.6(3) . . ? N5 C22 C3 116.0(3) . . ? C23 C22 C3 119.4(3) . . ? C24 C23 C22 116.9(4) . . ? C25 C24 C23 119.4(4) . . ? C24 C25 C26 120.2(4) . . ? N5 C26 C25 121.1(4) . . ? N5 C26 C27 116.3(3) . . ? C25 C26 C27 122.6(3) . . ? N6 C27 C28 121.7(3) . . ? N6 C27 C26 116.8(3) . . ? C28 C27 C26 121.4(3) . . ? C29 C28 C27 119.8(3) . . ? C34 C29 C28 119.0(3) . . ? C34 C29 C30 117.0(3) . . ? C28 C29 C30 123.9(3) . . ? C31 C30 C29 111.0(3) . . ? C30 C31 C36 109.9(3) . . ? C30 C31 C32 111.0(3) . . ? C36 C31 C32 88.3(3) . . ? C37 C32 C38 109.7(3) . . ? C37 C32 C31 120.5(3) . . ? C38 C32 C31 111.0(3) . . ? C37 C32 C33 117.3(3) . . ? C38 C32 C33 112.3(3) . . ? C31 C32 C33 84.1(3) . . ? C34 C33 C36 107.3(3) . . ? C34 C33 C32 110.3(3) . . ? C36 C33 C32 87.0(3) . . ? C29 C34 C35 117.3(3) . . ? C29 C34 C33 117.8(3) . . ? C35 C34 C33 124.9(3) . . ? N6 C35 C34 124.9(3) . . ? C31 C36 C33 85.6(3) . . ? 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 C4 N1 C1 C2 3.3(5) . . . . ? C4 N1 C1 C5 -177.2(2) . . . . ? C3 N2 C2 C1 -0.7(4) . . . . ? N1 C1 C2 N2 -2.3(5) . . . . ? C5 C1 C2 N2 178.3(3) . . . . ? C2 N2 C3 C4 2.4(4) . . . . ? C2 N2 C3 C22 -178.6(2) . . . . ? C1 N1 C4 C3 -1.7(5) . . . . ? N2 C3 C4 N1 -1.2(5) . . . . ? C22 C3 C4 N1 179.8(3) . . . . ? C9 N3 C5 C6 0.4(4) . . . . ? C9 N3 C5 C1 -178.7(2) . . . . ? N1 C1 C5 N3 171.8(3) . . . . ? C2 C1 C5 N3 -8.7(4) . . . . ? N1 C1 C5 C6 -7.3(4) . . . . ? C2 C1 C5 C6 172.2(3) . . . . ? N3 C5 C6 C7 -0.1(4) . . . . ? C1 C5 C6 C7 178.9(3) . . . . ? C5 C6 C7 C8 0.2(5) . . . . ? C6 C7 C8 C9 -0.5(5) . . . . ? C5 N3 C9 C8 -0.7(4) . . . . ? C5 N3 C9 C10 -179.0(2) . . . . ? C7 C8 C9 N3 0.7(4) . . . . ? C7 C8 C9 C10 179.0(3) . . . . ? C18 N4 C10 C11 1.5(4) . . . . ? C18 N4 C10 C9 -177.2(3) . . . . ? N3 C9 C10 N4 -175.3(2) . . . . ? C8 C9 C10 N4 6.4(4) . . . . ? N3 C9 C10 C11 6.1(4) . . . . ? C8 C9 C10 C11 -172.2(3) . . . . ? N4 C10 C11 C12 -2.3(4) . . . . ? C9 C10 C11 C12 176.2(3) . . . . ? C10 C11 C12 C17 0.8(4) . . . . ? C10 C11 C12 C13 179.1(3) . . . . ? C11 C12 C13 C14 175.7(3) . . . . ? C17 C12 C13 C14 -5.9(5) . . . . ? C12 C13 C14 C19 -44.3(4) . . . . ? C12 C13 C14 C15 51.1(4) . . . . ? C13 C14 C15 C21 165.3(3) . . . . ? C19 C14 C15 C21 -83.4(3) . . . . ? C13 C14 C15 C20 36.9(4) . . . . ? C19 C14 C15 C20 148.2(3) . . . . ? C13 C14 C15 C16 -81.7(3) . . . . ? C19 C14 C15 C16 29.5(3) . . . . ? C21 C15 C16 C17 -170.7(3) . . . . ? C20 C15 C16 C17 -40.0(4) . . . . ? C14 C15 C16 C17 78.1(3) . . . . ? C21 C15 C16 C19 82.0(3) . . . . ? C20 C15 C16 C19 -147.3(3) . . . . ? C14 C15 C16 C19 -29.2(3) . . . . ? C11 C12 C17 C18 1.5(4) . . . . ? C13 C12 C17 C18 -177.0(3) . . . . ? C11 C12 C17 C16 -175.8(3) . . . . ? C13 C12 C17 C16 5.7(4) . . . . ? C19 C16 C17 C18 -133.8(3) . . . . ? C15 C16 C17 C18 133.7(3) . . . . ? C19 C16 C17 C12 43.2(4) . . . . ? C15 C16 C17 C12 -49.3(3) . . . . ? C10 N4 C18 C17 0.9(5) . . . . ? C12 C17 C18 N4 -2.4(5) . . . . ? C16 C17 C18 N4 174.6(3) . . . . ? C13 C14 C19 C16 83.4(3) . . . . ? C15 C14 C19 C16 -29.7(3) . . . . ? C17 C16 C19 C14 -80.5(3) . . . . ? C15 C16 C19 C14 29.7(3) . . . . ? C26 N5 C22 C23 1.7(4) . . . . ? C26 N5 C22 C3 -179.3(2) . . . . ? N2 C3 C22 N5 160.9(3) . . . . ? C4 C3 C22 N5 -20.1(4) . . . . ? N2 C3 C22 C23 -20.1(4) . . . . ? C4 C3 C22 C23 158.9(3) . . . . ? N5 C22 C23 C24 -0.2(5) . . . . ? C3 C22 C23 C24 -179.2(3) . . . . ? C22 C23 C24 C25 -1.0(5) . . . . ? C23 C24 C25 C26 0.7(5) . . . . ? C22 N5 C26 C25 -2.0(4) . . . . ? C22 N5 C26 C27 178.1(2) . . . . ? C24 C25 C26 N5 0.9(5) . . . . ? C24 C25 C26 C27 -179.3(3) . . . . ? C35 N6 C27 C28 -1.3(4) . . . . ? C35 N6 C27 C26 178.9(3) . . . . ? N5 C26 C27 N6 -174.4(2) . . . . ? C25 C26 C27 N6 5.8(4) . . . . ? N5 C26 C27 C28 5.9(4) . . . . ? C25 C26 C27 C28 -173.9(3) . . . . ? N6 C27 C28 C29 0.0(4) . . . . ? C26 C27 C28 C29 179.8(3) . . . . ? C27 C28 C29 C34 1.6(4) . . . . ? C27 C28 C29 C30 179.4(3) . . . . ? C34 C29 C30 C31 -3.3(4) . . . . ? C28 C29 C30 C31 178.8(3) . . . . ? C29 C30 C31 C36 -45.2(4) . . . . ? C29 C30 C31 C32 50.9(4) . . . . ? C30 C31 C32 C37 36.2(5) . . . . ? C36 C31 C32 C37 146.9(3) . . . . ? C30 C31 C32 C38 166.3(3) . . . . ? C36 C31 C32 C38 -83.0(4) . . . . ? C30 C31 C32 C33 -82.1(3) . . . . ? C36 C31 C32 C33 28.6(3) . . . . ? C37 C32 C33 C34 -42.3(4) . . . . ? C38 C32 C33 C34 -170.7(3) . . . . ? C31 C32 C33 C34 79.0(3) . . . . ? C37 C32 C33 C36 -149.7(3) . . . . ? C38 C32 C33 C36 82.0(3) . . . . ? C31 C32 C33 C36 -28.3(3) . . . . ? C28 C29 C34 C35 -1.8(4) . . . . ? C30 C29 C34 C35 -179.8(3) . . . . ? C28 C29 C34 C33 -179.7(3) . . . . ? C30 C29 C34 C33 2.2(4) . . . . ? C36 C33 C34 C29 46.1(4) . . . . ? C32 C33 C34 C29 -47.1(4) . . . . ? C36 C33 C34 C35 -131.7(3) . . . . ? C32 C33 C34 C35 135.1(3) . . . . ? C27 N6 C35 C34 1.1(5) . . . . ? C29 C34 C35 N6 0.4(5) . . . . ? C33 C34 C35 N6 178.3(3) . . . . ? C30 C31 C36 C33 82.7(3) . . . . ? C32 C31 C36 C33 -29.0(3) . . . . ? C34 C33 C36 C31 -81.7(3) . . . . ? C32 C33 C36 C31 28.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.86 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.117 _refine_diff_density_min -0.122 _refine_diff_density_rms 0.029