# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_year ? _journal_page_first ? _publ_contact_author_name 'Robert Buchanan' _publ_contact_author_address ; Chemistry University of Louisville 2320 South Brook Street Room 138 Louisville KY 40292 UNITED STATES OF AMERICA ; _publ_contact_author_email BOB.BUCHANAN@LOUISVILLE.EDU _publ_section_title ; A supramolecular assembly of side-by-side polyimidazole tripod coils stabilized by ð-ð stacking and unique boric acid templated hydrogen bonding interactions ; loop_ _publ_author_name 'Robert Buchanan' 'Lionel E. Cheruzel' 'Mark S. Mashuta' data_rmb164s _database_code_depnum_ccdc_archive 'CCDC 239617' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; bis((1-methylimidazol-2-yl)methyl)(1-methyl-4-nitro -imidazol- 2-yl)methyl)amine boric acid ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H43 B N16 O7' _chemical_formula_weight 750.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 15.7997(18) _cell_length_b 8.2540(9) _cell_length_c 27.530(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.861(2) _cell_angle_gamma 90.00 _cell_volume 3585.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5397 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 27.53 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.301 _exptl_crystal_size_mid 0.173 _exptl_crystal_size_min 0.081 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.390 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1584 _exptl_absorpt_coefficient_mu 0.103 _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 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29945 _diffrn_reflns_av_R_equivalents 0.0273 _diffrn_reflns_av_sigmaI/netI 0.0395 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 28.30 _reflns_number_total 8345 _reflns_number_gt 6562 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0514P)^2^+0.9500P] 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 0.0000(2) _refine_ls_extinction_expression Fc^*^==kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8345 _refine_ls_number_parameters 540 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0585 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.1130 _refine_ls_wR_factor_gt 0.1066 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.097 _refine_ls_shift/su_max 7.485 _refine_ls_shift/su_mean 0.015 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 O1 O 0.17604(7) -0.30799(13) 0.23391(4) 0.0289(3) Uani 1 1 d . . . O2 O 0.07978(8) -0.43957(13) 0.27127(4) 0.0361(3) Uani 1 1 d . . . O3 O 0.68497(7) 1.27706(12) 0.23026(4) 0.0266(2) Uani 1 1 d . . . O4 O 0.57961(8) 1.41284(13) 0.25695(4) 0.0340(3) Uani 1 1 d . . . N1 N 0.13710(7) 0.03963(14) 0.33618(4) 0.0186(2) Uani 1 1 d . . . N2 N 0.06272(7) -0.18901(13) 0.33513(4) 0.0183(2) Uani 1 1 d . . . N3 N -0.15057(7) 0.31199(14) 0.32395(4) 0.0186(2) Uani 1 1 d . . . N4 N -0.22720(7) 0.25890(14) 0.38709(4) 0.0182(2) Uani 1 1 d . . . N5 N 0.02556(7) 0.48763(14) 0.43607(4) 0.0208(3) Uani 1 1 d . . . N6 N 0.10003(7) 0.31659(14) 0.48305(4) 0.0229(3) Uani 1 1 d . . . N7 N 0.12410(8) -0.31962(14) 0.26587(4) 0.0234(3) Uani 1 1 d . . . N8 N -0.02434(7) 0.13364(13) 0.39666(4) 0.0151(2) Uani 1 1 d . . . N9 N 0.64475(7) 0.97985(13) 0.34542(4) 0.0174(2) Uani 1 1 d . . . N10 N 0.56226(7) 1.19532(13) 0.33123(4) 0.0191(2) Uani 1 1 d . . . N11 N 0.56323(7) 0.58906(14) 0.45885(4) 0.0208(3) Uani 1 1 d . . . N12 N 0.59198(7) 0.80351(14) 0.50532(4) 0.0221(3) Uani 1 1 d . . . N13 N 0.37341(8) 0.66885(15) 0.32972(4) 0.0227(3) Uani 1 1 d . . . N14 N 0.28233(7) 0.74035(14) 0.38415(4) 0.0202(3) Uani 1 1 d . . . N15 N 0.62786(8) 1.29723(14) 0.25907(4) 0.0214(3) Uani 1 1 d . . . N16 N 0.48137(7) 0.88900(13) 0.40019(4) 0.0173(2) Uani 1 1 d . . . C1 C 0.07630(8) -0.05043(16) 0.35777(5) 0.0167(3) Uani 1 1 d . . . C2 C 0.11707(9) -0.18600(16) 0.29850(5) 0.0182(3) Uani 1 1 d . . . C3 C 0.16427(9) -0.04763(17) 0.29819(5) 0.0198(3) Uani 1 1 d . . . H3 H 0.2065 -0.0189 0.2764 0.027(4) Uiso 1 1 calc R . . C4 C 0.16935(10) 0.19781(17) 0.35253(6) 0.0257(3) Uani 1 1 d . . . H4A H 0.2116 0.2361 0.3303 0.073(7) Uiso 1 1 calc R . . H4B H 0.1956 0.1878 0.3854 0.074(7) Uiso 1 1 calc R . . H4C H 0.1224 0.2754 0.3528 0.054(6) Uiso 1 1 calc R . . C5 C 0.03732(8) 0.00176(16) 0.40347(5) 0.0171(3) Uani 1 1 d . . . H5A H 0.0088 -0.0926 0.4177 0.017(4) Uiso 1 1 calc R . . H5B H 0.0829 0.0372 0.4271 0.018(4) Uiso 1 1 calc R . . C6 C -0.16299(8) 0.20994(16) 0.36166(5) 0.0166(3) Uani 1 1 d . . . C7 C -0.25650(9) 0.39827(17) 0.36464(5) 0.0204(3) Uani 1 1 d . . . H7 H -0.3026 0.4614 0.3749 0.024(4) Uiso 1 1 calc R . . C8 C -0.21007(9) 0.43265(16) 0.32583(5) 0.0207(3) Uani 1 1 d . . . H8 H -0.2173 0.5221 0.3043 0.029(4) Uiso 1 1 calc R . . C9 C -0.08444(10) 0.29891(19) 0.28908(5) 0.0262(3) Uani 1 1 d . . . H9A H -0.0357 0.2411 0.3041 0.069(7) Uiso 1 1 calc R . . H9B H -0.0669 0.4076 0.2794 0.064(7) Uiso 1 1 calc R . . H9C H -0.1063 0.2393 0.2603 0.073(7) Uiso 1 1 calc R . . C10 C -0.10545(8) 0.07162(16) 0.37475(5) 0.0167(3) Uani 1 1 d . . . H10A H -0.1326 -0.0004 0.3981 0.016(4) Uiso 1 1 calc R . . H10B H -0.0946 0.0077 0.3453 0.018(4) Uiso 1 1 calc R . . C11 C 0.03019(9) 0.33572(17) 0.45527(5) 0.0188(3) Uani 1 1 d . . . C12 C 0.14101(9) 0.46408(17) 0.48173(5) 0.0232(3) Uani 1 1 d . . . H12 H 0.1934 0.4881 0.4986 0.027(4) Uiso 1 1 calc R . . C13 C 0.09642(9) 0.56906(18) 0.45320(5) 0.0237(3) Uani 1 1 d . . . H13 H 0.1111 0.6780 0.4463 0.039(5) Uiso 1 1 calc R . . C14 C -0.04300(10) 0.55511(18) 0.40488(6) 0.0272(3) Uani 1 1 d . . . H14A H -0.0859 0.4714 0.3978 0.043(5) Uiso 1 1 calc R . . H14B H -0.0203 0.5929 0.3744 0.059(6) Uiso 1 1 calc R . . H14C H -0.0689 0.6463 0.4215 0.060(6) Uiso 1 1 calc R . . C15 C -0.03604(8) 0.20969(16) 0.44465(5) 0.0166(3) Uani 1 1 d . . . H15A H -0.0325 0.1256 0.4703 0.014(3) Uiso 1 1 calc R . . H15B H -0.0929 0.2600 0.4448 0.018(4) Uiso 1 1 calc R . . C16 C 0.57870(8) 1.07203(16) 0.36055(5) 0.0177(3) Uani 1 1 d . . . C17 C 0.67275(9) 1.04937(16) 0.30465(5) 0.0182(3) Uani 1 1 d . . . H17 H 0.7182 1.0150 0.2858 0.029(4) Uiso 1 1 calc R . . C18 C 0.62085(9) 1.17999(16) 0.29682(5) 0.0182(3) Uani 1 1 d . . . C19 C 0.68237(9) 0.83979(17) 0.37076(5) 0.0228(3) Uani 1 1 d . . . H19A H 0.7258 0.7919 0.3510 0.043(5) Uiso 1 1 calc R . . H19B H 0.6382 0.7592 0.3761 0.036(5) Uiso 1 1 calc R . . H19C H 0.7083 0.8743 0.4022 0.034(5) Uiso 1 1 calc R . . C20 C 0.53505(9) 1.03427(16) 0.40605(5) 0.0195(3) Uani 1 1 d . . . H20A H 0.5780 1.0166 0.4330 0.022(4) Uiso 1 1 calc R . . H20B H 0.4996 1.1277 0.4148 0.022(4) Uiso 1 1 calc R . . C21 C 0.53903(9) 0.74111(16) 0.47149(5) 0.0181(3) Uani 1 1 d . . . C22 C 0.65213(9) 0.68536(18) 0.51462(6) 0.0261(3) Uani 1 1 d . . . H22 H 0.6990 0.6954 0.5374 0.031(4) Uiso 1 1 calc R . . C23 C 0.63534(9) 0.55258(18) 0.48670(6) 0.0251(3) Uani 1 1 d . . . H23 H 0.6669 0.4547 0.4865 0.031(5) Uiso 1 1 calc R . . C24 C 0.52152(10) 0.48510(18) 0.42232(6) 0.0292(3) Uani 1 1 d . . . H24A H 0.4650 0.4561 0.4326 0.047(5) Uiso 1 1 calc R . . H24B H 0.5551 0.3865 0.4186 0.072(7) Uiso 1 1 calc R . . H24C H 0.5164 0.5427 0.3912 0.065(7) Uiso 1 1 calc R . . C25 C 0.46322(8) 0.82372(16) 0.44890(5) 0.0181(3) Uani 1 1 d . . . H25A H 0.4156 0.7459 0.4456 0.020(4) Uiso 1 1 calc R . . H25B H 0.4461 0.9134 0.4702 0.019(4) Uiso 1 1 calc R . . C26 C 0.35057(9) 0.78425(17) 0.36180(5) 0.0190(3) Uani 1 1 d . . . C27 C 0.26019(9) 0.59057(18) 0.36548(5) 0.0230(3) Uani 1 1 d . . . H27 H 0.2130 0.5284 0.3746 0.029(4) Uiso 1 1 calc R . . C28 C 0.31591(9) 0.54502(18) 0.33205(5) 0.0252(3) Uani 1 1 d . . . H28 H 0.3152 0.4471 0.3139 0.035(5) Uiso 1 1 calc R . . C29 C 0.44405(10) 0.6781(2) 0.29777(6) 0.0328(4) Uani 1 1 d . . . H29A H 0.4269 0.7402 0.2686 0.060(7) Uiso 1 1 calc R . . H29B H 0.4606 0.5685 0.2884 0.053(6) Uiso 1 1 calc R . . H29C H 0.4922 0.7318 0.3149 0.038(5) Uiso 1 1 calc R . . C30 C 0.40159(9) 0.93227(16) 0.37305(5) 0.0202(3) Uani 1 1 d . . . H30A H 0.4145 0.9878 0.3424 0.023(4) Uiso 1 1 calc R . . H30B H 0.3686 1.0077 0.3927 0.022(4) Uiso 1 1 calc R . . B B 0.22948(10) 0.94740(19) 0.49760(6) 0.0187(3) Uani 1 1 d . . . O5 O 0.22410(6) 0.96681(12) 0.44837(3) 0.0214(2) Uani 1 1 d . . . H5O H 0.2441 0.8847 0.4350 0.046(6) Uiso 1 1 calc R . . O6 O 0.19158(6) 1.05853(12) 0.52660(4) 0.0232(2) Uani 1 1 d . . . H6O H 0.1662 1.1283 0.5091 0.053(6) Uiso 1 1 calc R . . O7 O 0.26916(7) 0.81673(12) 0.51832(4) 0.0247(2) Uani 1 1 d . . . H7O H 0.2564 0.8090 0.5475 0.053(6) 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 O1 0.0353(6) 0.0272(6) 0.0254(6) -0.0022(4) 0.0144(5) 0.0035(5) O2 0.0449(7) 0.0231(6) 0.0417(7) -0.0104(5) 0.0157(6) -0.0121(5) O3 0.0357(6) 0.0229(5) 0.0223(5) 0.0004(4) 0.0135(5) -0.0025(4) O4 0.0413(7) 0.0239(6) 0.0374(6) 0.0086(5) 0.0090(5) 0.0104(5) N1 0.0202(6) 0.0149(6) 0.0210(6) 0.0009(4) 0.0037(5) -0.0004(5) N2 0.0182(6) 0.0167(6) 0.0203(6) 0.0007(4) 0.0038(5) 0.0016(4) N3 0.0197(6) 0.0187(6) 0.0176(6) 0.0016(4) 0.0025(5) 0.0007(4) N4 0.0175(6) 0.0185(6) 0.0187(6) 0.0008(5) 0.0023(4) 0.0000(5) N5 0.0213(6) 0.0180(6) 0.0233(6) -0.0018(5) 0.0031(5) -0.0024(5) N6 0.0202(6) 0.0206(6) 0.0278(7) -0.0051(5) 0.0002(5) 0.0027(5) N7 0.0273(7) 0.0203(6) 0.0231(6) -0.0026(5) 0.0060(5) 0.0009(5) N8 0.0151(5) 0.0140(5) 0.0164(5) -0.0012(4) 0.0023(4) 0.0007(4) N9 0.0190(6) 0.0143(5) 0.0191(6) -0.0015(4) 0.0039(4) -0.0026(4) N10 0.0207(6) 0.0153(6) 0.0217(6) -0.0021(4) 0.0053(5) -0.0029(5) N11 0.0226(6) 0.0140(6) 0.0266(6) -0.0013(5) 0.0088(5) -0.0010(5) N12 0.0207(6) 0.0194(6) 0.0266(6) -0.0027(5) 0.0037(5) 0.0007(5) N13 0.0238(6) 0.0239(6) 0.0210(6) -0.0048(5) 0.0074(5) -0.0036(5) N14 0.0191(6) 0.0219(6) 0.0200(6) -0.0017(5) 0.0040(5) -0.0023(5) N15 0.0265(6) 0.0182(6) 0.0200(6) -0.0011(5) 0.0049(5) -0.0019(5) N16 0.0190(6) 0.0150(6) 0.0182(6) -0.0002(4) 0.0050(4) -0.0042(4) C1 0.0154(6) 0.0149(6) 0.0199(7) 0.0027(5) 0.0019(5) 0.0016(5) C2 0.0201(7) 0.0157(7) 0.0189(7) -0.0006(5) 0.0031(5) 0.0017(5) C3 0.0206(7) 0.0199(7) 0.0193(7) 0.0020(5) 0.0057(5) 0.0008(5) C4 0.0294(8) 0.0168(7) 0.0316(8) -0.0019(6) 0.0076(6) -0.0067(6) C5 0.0185(6) 0.0145(6) 0.0184(6) 0.0020(5) 0.0028(5) 0.0018(5) C6 0.0169(6) 0.0167(6) 0.0163(6) -0.0001(5) 0.0008(5) -0.0026(5) C7 0.0183(7) 0.0187(7) 0.0243(7) 0.0003(5) 0.0008(5) 0.0031(5) C8 0.0234(7) 0.0167(7) 0.0218(7) 0.0025(5) 0.0000(6) 0.0022(5) C9 0.0284(8) 0.0283(8) 0.0230(7) 0.0053(6) 0.0109(6) 0.0038(6) C10 0.0174(6) 0.0145(6) 0.0182(6) -0.0010(5) 0.0019(5) -0.0011(5) C11 0.0190(7) 0.0201(7) 0.0175(7) -0.0041(5) 0.0048(5) 0.0010(5) C12 0.0161(7) 0.0219(7) 0.0317(8) -0.0083(6) 0.0020(6) -0.0004(6) C13 0.0211(7) 0.0209(7) 0.0296(8) -0.0049(6) 0.0064(6) -0.0041(6) C14 0.0314(8) 0.0211(8) 0.0285(8) 0.0056(6) -0.0047(6) -0.0040(6) C15 0.0182(6) 0.0153(6) 0.0165(6) -0.0002(5) 0.0028(5) 0.0009(5) C16 0.0192(7) 0.0138(6) 0.0204(7) -0.0040(5) 0.0045(5) -0.0043(5) C17 0.0198(7) 0.0171(7) 0.0180(6) -0.0035(5) 0.0047(5) -0.0032(5) C18 0.0216(7) 0.0153(7) 0.0180(7) -0.0012(5) 0.0037(5) -0.0030(5) C19 0.0247(7) 0.0194(7) 0.0246(7) 0.0032(6) 0.0038(6) 0.0016(6) C20 0.0237(7) 0.0152(6) 0.0203(7) -0.0031(5) 0.0074(6) -0.0045(5) C21 0.0209(7) 0.0142(6) 0.0199(7) 0.0000(5) 0.0080(5) -0.0012(5) C22 0.0212(7) 0.0256(8) 0.0314(8) 0.0008(6) 0.0028(6) 0.0037(6) C23 0.0218(7) 0.0197(7) 0.0347(8) 0.0031(6) 0.0101(6) 0.0038(6) C24 0.0344(9) 0.0181(7) 0.0358(9) -0.0084(6) 0.0091(7) -0.0048(6) C25 0.0195(7) 0.0153(6) 0.0200(7) -0.0007(5) 0.0065(5) -0.0019(5) C26 0.0198(7) 0.0198(7) 0.0176(6) -0.0004(5) 0.0024(5) 0.0005(5) C27 0.0220(7) 0.0241(7) 0.0230(7) -0.0026(6) 0.0033(6) -0.0067(6) C28 0.0281(8) 0.0229(7) 0.0247(7) -0.0060(6) 0.0030(6) -0.0058(6) C29 0.0301(8) 0.0398(10) 0.0299(9) -0.0106(7) 0.0150(7) -0.0092(7) C30 0.0214(7) 0.0173(7) 0.0223(7) 0.0010(5) 0.0048(6) -0.0012(5) B 0.0162(7) 0.0200(8) 0.0202(8) 0.0004(6) 0.0027(6) -0.0042(6) O5 0.0227(5) 0.0222(5) 0.0196(5) -0.0003(4) 0.0033(4) 0.0047(4) O6 0.0279(6) 0.0205(5) 0.0216(5) 0.0019(4) 0.0040(4) 0.0043(4) O7 0.0300(6) 0.0219(5) 0.0227(5) 0.0023(4) 0.0073(4) 0.0057(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 N7 1.2365(15) . ? O2 N7 1.2261(16) . ? O3 N15 1.2420(15) . ? O4 N15 1.2209(16) . ? N1 C3 1.3570(17) . ? N1 C1 1.3731(17) . ? N1 C4 1.4642(18) . ? N2 C1 1.3150(17) . ? N2 C2 1.3570(17) . ? N3 C6 1.3587(17) . ? N3 C8 1.3723(17) . ? N3 C9 1.4577(18) . ? N4 C6 1.3241(17) . ? N4 C7 1.3751(18) . ? N5 C11 1.3613(18) . ? N5 C13 1.3691(18) . ? N5 C14 1.4589(19) . ? N6 C11 1.3202(18) . ? N6 C12 1.3801(19) . ? N7 C2 1.4301(18) . ? N8 C5 1.4666(16) . ? N8 C10 1.4802(17) . ? N8 C15 1.4826(16) . ? N9 C17 1.3542(17) . ? N9 C16 1.3730(17) . ? N9 C19 1.4613(18) . ? N10 C16 1.3167(18) . ? N10 C18 1.3630(17) . ? N11 C21 1.3623(17) . ? N11 C23 1.3745(19) . ? N11 C24 1.4546(19) . ? N12 C21 1.3246(18) . ? N12 C22 1.3768(18) . ? N13 C26 1.3599(17) . ? N13 C28 1.3710(19) . ? N13 C29 1.4571(18) . ? N14 C26 1.3186(18) . ? N14 C27 1.3774(18) . ? N15 C18 1.4283(17) . ? N16 C20 1.4729(17) . ? N16 C30 1.4767(18) . ? N16 C25 1.4864(17) . ? C1 C5 1.4918(18) . ? C2 C3 1.3643(19) . ? C3 H3 0.9500 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C10 1.4924(18) . ? C7 C8 1.356(2) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C15 1.4940(18) . ? C12 C13 1.345(2) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C20 1.4926(18) . ? C17 C18 1.3652(19) . ? C17 H17 0.9500 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C25 1.4873(19) . ? C22 C23 1.357(2) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C30 1.4879(19) . ? C27 C28 1.358(2) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? B O7 1.3587(19) . ? B O5 1.3632(18) . ? B O6 1.3730(18) . ? O5 H5O 0.8400 . ? O6 H6O 0.8400 . ? O7 H7O 0.8400 . ? 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 C3 N1 C1 107.53(11) . . ? C3 N1 C4 126.27(12) . . ? C1 N1 C4 126.15(12) . . ? C1 N2 C2 104.00(11) . . ? C6 N3 C8 107.21(11) . . ? C6 N3 C9 126.36(12) . . ? C8 N3 C9 126.40(12) . . ? C6 N4 C7 105.51(11) . . ? C11 N5 C13 106.94(12) . . ? C11 N5 C14 127.17(12) . . ? C13 N5 C14 125.85(12) . . ? C11 N6 C12 105.01(12) . . ? O2 N7 O1 123.52(12) . . ? O2 N7 C2 118.94(12) . . ? O1 N7 C2 117.53(12) . . ? C5 N8 C10 110.58(10) . . ? C5 N8 C15 108.18(10) . . ? C10 N8 C15 111.45(10) . . ? C17 N9 C16 107.55(11) . . ? C17 N9 C19 126.08(11) . . ? C16 N9 C19 126.21(11) . . ? C16 N10 C18 103.55(11) . . ? C21 N11 C23 107.14(12) . . ? C21 N11 C24 126.64(13) . . ? C23 N11 C24 126.21(12) . . ? C21 N12 C22 105.14(12) . . ? C26 N13 C28 107.09(11) . . ? C26 N13 C29 126.26(12) . . ? C28 N13 C29 126.62(12) . . ? C26 N14 C27 105.71(12) . . ? O4 N15 O3 123.09(12) . . ? O4 N15 C18 119.56(12) . . ? O3 N15 C18 117.33(12) . . ? C20 N16 C30 109.32(11) . . ? C20 N16 C25 109.40(10) . . ? C30 N16 C25 110.24(10) . . ? N2 C1 N1 111.53(12) . . ? N2 C1 C5 125.90(12) . . ? N1 C1 C5 122.40(12) . . ? N2 C2 C3 112.72(12) . . ? N2 C2 N7 121.64(12) . . ? C3 C2 N7 125.59(12) . . ? N1 C3 C2 104.21(12) . . ? N1 C3 H3 127.9 . . ? C2 C3 H3 127.9 . . ? N1 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N8 C5 C1 113.96(11) . . ? N8 C5 H5A 108.8 . . ? C1 C5 H5A 108.8 . . ? N8 C5 H5B 108.8 . . ? C1 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? N4 C6 N3 111.00(12) . . ? N4 C6 C10 125.41(12) . . ? N3 C6 C10 123.32(12) . . ? C8 C7 N4 110.23(12) . . ? C8 C7 H7 124.9 . . ? N4 C7 H7 124.9 . . ? C7 C8 N3 106.04(12) . . ? C7 C8 H8 127.0 . . ? N3 C8 H8 127.0 . . ? N3 C9 H9A 109.5 . . ? N3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N8 C10 C6 109.78(10) . . ? N8 C10 H10A 109.7 . . ? C6 C10 H10A 109.7 . . ? N8 C10 H10B 109.7 . . ? C6 C10 H10B 109.7 . . ? H10A C10 H10B 108.2 . . ? N6 C11 N5 111.23(12) . . ? N6 C11 C15 125.95(13) . . ? N5 C11 C15 122.81(12) . . ? C13 C12 N6 110.54(13) . . ? C13 C12 H12 124.7 . . ? N6 C12 H12 124.7 . . ? C12 C13 N5 106.28(13) . . ? C12 C13 H13 126.9 . . ? N5 C13 H13 126.9 . . ? N5 C14 H14A 109.5 . . ? N5 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N5 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N8 C15 C11 110.61(10) . . ? N8 C15 H15A 109.5 . . ? C11 C15 H15A 109.5 . . ? N8 C15 H15B 109.5 . . ? C11 C15 H15B 109.5 . . ? H15A C15 H15B 108.1 . . ? N10 C16 N9 111.83(12) . . ? N10 C16 C20 126.20(12) . . ? N9 C16 C20 121.94(12) . . ? N9 C17 C18 104.30(11) . . ? N9 C17 H17 127.9 . . ? C18 C17 H17 127.9 . . ? N10 C18 C17 112.77(12) . . ? N10 C18 N15 121.52(12) . . ? C17 C18 N15 125.60(12) . . ? N9 C19 H19A 109.5 . . ? N9 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N9 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N16 C20 C16 111.45(11) . . ? N16 C20 H20A 109.3 . . ? C16 C20 H20A 109.3 . . ? N16 C20 H20B 109.3 . . ? C16 C20 H20B 109.3 . . ? H20A C20 H20B 108.0 . . ? N12 C21 N11 111.24(12) . . ? N12 C21 C25 125.66(12) . . ? N11 C21 C25 123.09(12) . . ? C23 C22 N12 110.68(13) . . ? C23 C22 H22 124.7 . . ? N12 C22 H22 124.7 . . ? C22 C23 N11 105.79(13) . . ? C22 C23 H23 127.1 . . ? N11 C23 H23 127.1 . . ? N11 C24 H24A 109.5 . . ? N11 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N11 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N16 C25 C21 110.84(11) . . ? N16 C25 H25A 109.5 . . ? C21 C25 H25A 109.5 . . ? N16 C25 H25B 109.5 . . ? C21 C25 H25B 109.5 . . ? H25A C25 H25B 108.1 . . ? N14 C26 N13 111.12(12) . . ? N14 C26 C30 125.15(12) . . ? N13 C26 C30 123.49(12) . . ? C28 C27 N14 109.90(12) . . ? C28 C27 H27 125.1 . . ? N14 C27 H27 125.1 . . ? C27 C28 N13 106.19(13) . . ? C27 C28 H28 126.9 . . ? N13 C28 H28 126.9 . . ? N13 C29 H29A 109.5 . . ? N13 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N13 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N16 C30 C26 110.28(11) . . ? N16 C30 H30A 109.6 . . ? C26 C30 H30A 109.6 . . ? N16 C30 H30B 109.6 . . ? C26 C30 H30B 109.6 . . ? H30A C30 H30B 108.1 . . ? O7 B O5 121.01(13) . . ? O7 B O6 119.46(13) . . ? O5 B O6 119.49(13) . . ? B O5 H5O 109.5 . . ? B O6 H6O 109.5 . . ? B O7 H7O 109.5 . . ? _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.938 _refine_diff_density_max 0.556 _refine_diff_density_min -0.203 _refine_diff_density_rms 0.056