Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Liang Nian Ji' 'Hong Deng' 'Hong Xu' 'Hao Zhang' _publ_contact_author_name 'Prof Liang Nian Ji' _publ_contact_author_address ; School of Chemistry & Chemical Eng. Zhongshan University Sate Key Lab of Optoelectronic Mate Guangzhou Guangdong 510275 CHINA ; _publ_contact_author_email 'CESJLN@ZSU.EDU.CN' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Ruthenium(Άς) complexes containing asymmetric ligand : synthesis, characterization, crystal structure and DNA-binding ; data_complex1 _database_code_CSD 192534 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H29 Cl2 N9 O8 Ru' _chemical_formula_weight 923.68 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 0.0000 '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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 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 P2(1)/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 14.5050(17) _cell_length_b 11.5560(13) _cell_length_c 23.864(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.850(2) _cell_angle_gamma 90.00 _cell_volume 3952.5(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.552 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1872 _exptl_absorpt_coefficient_mu 0.597 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7545 _exptl_absorpt_correction_T_max 0.9211 _exptl_absorpt_process_details 'SADABS' _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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23100 _diffrn_reflns_av_R_equivalents 0.0295 _diffrn_reflns_av_sigmaI/netI 0.0403 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 27.22 _reflns_number_total 8682 _reflns_number_gt 5448 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0438P)^2^+4.5218P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8682 _refine_ls_number_parameters 532 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0817 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.1225 _refine_ls_wR_factor_gt 0.1040 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.292151(18) 0.74969(2) 0.069452(11) 0.03743(9) Uani 1 1 d . . . C1 C 0.4757(2) 0.6732(3) 0.03301(16) 0.0476(9) Uani 1 1 d . . . H1A H 0.4677 0.7325 0.0064 0.057 Uiso 1 1 calc R . . C2 C 0.5560(3) 0.6074(4) 0.03876(18) 0.0550(10) Uani 1 1 d . . . H2A H 0.6011 0.6252 0.0163 0.066 Uiso 1 1 calc R . . C3 C 0.5049(2) 0.4980(3) 0.10648(17) 0.0480(9) Uani 1 1 d . . . H3A H 0.5127 0.4366 0.1320 0.058 Uiso 1 1 calc R . . C4 C 0.4245(2) 0.5636(3) 0.10245(15) 0.0387(8) Uani 1 1 d . . . C5 C 0.3489(2) 0.5437(3) 0.13526(14) 0.0363(7) Uani 1 1 d . . . C6 C 0.2761(2) 0.4409(3) 0.19677(14) 0.0380(8) Uani 1 1 d . . . C7 C 0.1965(2) 0.5112(3) 0.18032(14) 0.0376(8) Uani 1 1 d . . . C8 C 0.2806(2) 0.3467(3) 0.23920(15) 0.0431(8) Uani 1 1 d . . . C9 C 0.3205(3) 0.2420(4) 0.2283(2) 0.0629(11) Uani 1 1 d . . . H9A H 0.3455 0.2318 0.1950 0.076 Uiso 1 1 calc R . . C10 C 0.3233(3) 0.1520(4) 0.2672(2) 0.0789(15) Uani 1 1 d . . . H10A H 0.3502 0.0818 0.2597 0.095 Uiso 1 1 calc R . . C11 C 0.2869(3) 0.1658(5) 0.3163(2) 0.0725(14) Uani 1 1 d . . . H11A H 0.2876 0.1045 0.3417 0.087 Uiso 1 1 calc R . . C12 C 0.2491(3) 0.2704(4) 0.32807(19) 0.0657(13) Uani 1 1 d . . . H12A H 0.2259 0.2803 0.3620 0.079 Uiso 1 1 calc R . . C13 C 0.2452(3) 0.3616(4) 0.28979(16) 0.0518(10) Uani 1 1 d . . . H13A H 0.2191 0.4320 0.2979 0.062 Uiso 1 1 calc R . . C14 C 0.1037(2) 0.4932(3) 0.19763(15) 0.0430(8) Uani 1 1 d . . . C15 C 0.0536(3) 0.5873(4) 0.21210(19) 0.0587(11) Uani 1 1 d . . . H15A H 0.0802 0.6607 0.2137 0.070 Uiso 1 1 calc R . . C16 C -0.0362(3) 0.5728(5) 0.2243(2) 0.0753(14) Uani 1 1 d . . . H16A H -0.0693 0.6362 0.2347 0.090 Uiso 1 1 calc R . . C17 C -0.0758(3) 0.4650(5) 0.2212(2) 0.0787(15) Uani 1 1 d . . . H17A H -0.1362 0.4556 0.2292 0.094 Uiso 1 1 calc R . . C18 C -0.0275(3) 0.3709(5) 0.2064(2) 0.0710(14) Uani 1 1 d . . . H18A H -0.0552 0.2982 0.2042 0.085 Uiso 1 1 calc R . . C19 C 0.0627(3) 0.3837(4) 0.19469(18) 0.0551(10) Uani 1 1 d . . . H19A H 0.0957 0.3196 0.1849 0.066 Uiso 1 1 calc R . . C20 C 0.2213(3) 0.5813(4) -0.02623(18) 0.0620(11) Uani 1 1 d . . . H20A H 0.2839 0.5635 -0.0259 0.074 Uiso 1 1 calc R . . C21 C 0.1553(4) 0.5226(5) -0.0629(2) 0.0801(15) Uani 1 1 d . . . H21A H 0.1729 0.4661 -0.0869 0.096 Uiso 1 1 calc R . . C22 C 0.0642(4) 0.5481(5) -0.0635(2) 0.0924(19) Uani 1 1 d . . . H22A H 0.0186 0.5083 -0.0877 0.111 Uiso 1 1 calc R . . C23 C 0.0390(3) 0.6326(5) -0.0286(2) 0.0844(16) Uani 1 1 d . . . H23A H -0.0236 0.6510 -0.0290 0.101 Uiso 1 1 calc R . . C24 C 0.1085(3) 0.6908(4) 0.00782(18) 0.0589(11) Uani 1 1 d . . . C25 C 0.0907(3) 0.7846(4) 0.0462(2) 0.0634(12) Uani 1 1 d . . . C26 C 0.0032(4) 0.8296(6) 0.0496(3) 0.107(2) Uani 1 1 d . . . H26A H -0.0494 0.7995 0.0272 0.128 Uiso 1 1 calc R . . C27 C -0.0052(4) 0.9189(7) 0.0864(4) 0.125(3) Uani 1 1 d . . . H27A H -0.0639 0.9481 0.0896 0.150 Uiso 1 1 calc R . . C28 C 0.0726(4) 0.9652(6) 0.1183(3) 0.104(2) Uani 1 1 d . . . H28A H 0.0676 1.0270 0.1426 0.125 Uiso 1 1 calc R . . C29 C 0.1587(3) 0.9181(4) 0.1136(2) 0.0692(13) Uani 1 1 d . . . H29A H 0.2118 0.9486 0.1354 0.083 Uiso 1 1 calc R . . C30 C 0.4077(3) 0.8315(4) 0.18029(16) 0.0525(10) Uani 1 1 d . . . H30A H 0.3860 0.7650 0.1960 0.063 Uiso 1 1 calc R . . C31 C 0.4693(3) 0.9022(4) 0.21434(18) 0.0606(11) Uani 1 1 d . . . H31A H 0.4899 0.8828 0.2520 0.073 Uiso 1 1 calc R . . C32 C 0.4997(3) 1.0011(4) 0.1917(2) 0.0673(13) Uani 1 1 d . . . H32A H 0.5407 1.0505 0.2141 0.081 Uiso 1 1 calc R . . C33 C 0.4692(3) 1.0273(4) 0.13568(19) 0.0596(11) Uani 1 1 d . . . H33A H 0.4894 1.0946 0.1200 0.072 Uiso 1 1 calc R . . C34 C 0.4088(2) 0.9534(3) 0.10290(16) 0.0431(9) Uani 1 1 d . . . C35 C 0.3754(2) 0.9697(3) 0.04198(16) 0.0426(8) Uani 1 1 d . . . C36 C 0.3981(3) 1.0639(4) 0.01096(19) 0.0580(11) Uani 1 1 d . . . H36A H 0.4351 1.1231 0.0287 0.070 Uiso 1 1 calc R . . C37 C 0.3659(3) 1.0695(4) -0.0460(2) 0.0650(12) Uani 1 1 d . . . H37A H 0.3802 1.1330 -0.0670 0.078 Uiso 1 1 calc R . . C38 C 0.3127(3) 0.9814(4) -0.07191(19) 0.0652(12) Uani 1 1 d . . . H38A H 0.2913 0.9837 -0.1107 0.078 Uiso 1 1 calc R . . C39 C 0.2914(3) 0.8892(4) -0.03958(16) 0.0566(10) Uani 1 1 d . . . H39A H 0.2551 0.8294 -0.0572 0.068 Uiso 1 1 calc R . . N1 N 0.40944(19) 0.6535(2) 0.06485(12) 0.0393(7) Uani 1 1 d . . . N3 N 0.27765(18) 0.6192(2) 0.12414(12) 0.0367(6) Uani 1 1 d . . . N4 N 0.19882(19) 0.6011(2) 0.14572(12) 0.0389(7) Uani 1 1 d . . . N5 N 0.35222(19) 0.4575(2) 0.17253(12) 0.0407(7) Uani 1 1 d . . . N6 N 0.1993(2) 0.6633(3) 0.00916(13) 0.0451(7) Uani 1 1 d . . . N7 N 0.1676(2) 0.8299(3) 0.07850(14) 0.0480(8) Uani 1 1 d . . . N8 N 0.37781(19) 0.8549(2) 0.12553(12) 0.0410(7) Uani 1 1 d . . . N9 N 0.3211(2) 0.8826(2) 0.01630(12) 0.0418(7) Uani 1 1 d . . . N2 N 0.5718(2) 0.5194(3) 0.07513(15) 0.0564(9) Uani 1 1 d . . . Cl1 Cl 0.24161(7) 0.27490(10) 0.05308(5) 0.0639(3) Uani 1 1 d . . . Cl2 Cl -0.30453(8) 0.25383(10) 0.18636(6) 0.0721(3) Uani 1 1 d . . . O1 O 0.1901(3) 0.3688(4) 0.07102(18) 0.1161(16) Uani 1 1 d . . . O2 O 0.2209(4) 0.1753(5) 0.0774(3) 0.180(3) Uani 1 1 d . . . O3 O 0.3383(2) 0.2969(4) 0.06736(17) 0.1025(13) Uani 1 1 d . . . O4 O 0.2205(3) 0.2618(4) -0.00661(18) 0.1306(18) Uani 1 1 d . . . O5 O -0.2955(4) 0.3602(4) 0.2137(3) 0.166(3) Uani 1 1 d . . . O6 O -0.2288(3) 0.2333(5) 0.1588(2) 0.140(2) Uani 1 1 d . . . O7 O -0.3116(4) 0.1633(4) 0.2244(2) 0.1339(17) Uani 1 1 d . . . O8 O -0.3884(3) 0.2491(4) 0.1457(3) 0.158(2) Uani 1 1 d . . . 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 Ru 0.03905(15) 0.03740(15) 0.03561(15) 0.00368(13) 0.00499(11) -0.00412(13) C1 0.048(2) 0.049(2) 0.049(2) -0.0006(17) 0.0172(18) -0.0088(18) C2 0.048(2) 0.060(3) 0.061(3) -0.004(2) 0.021(2) -0.007(2) C3 0.044(2) 0.052(2) 0.047(2) 0.0019(18) 0.0081(17) 0.0009(18) C4 0.0366(18) 0.0409(19) 0.038(2) 0.0001(15) 0.0043(15) -0.0049(15) C5 0.0363(17) 0.0360(18) 0.0352(18) 0.0030(14) 0.0016(14) -0.0026(15) C6 0.0401(18) 0.0368(19) 0.0353(19) 0.0027(14) -0.0004(15) -0.0070(15) C7 0.0395(18) 0.0363(18) 0.0363(18) 0.0004(15) 0.0033(15) -0.0042(15) C8 0.0425(19) 0.045(2) 0.040(2) 0.0103(16) 0.0025(16) -0.0036(16) C9 0.066(3) 0.054(3) 0.073(3) 0.020(2) 0.021(2) 0.011(2) C10 0.082(3) 0.056(3) 0.104(4) 0.030(3) 0.032(3) 0.018(2) C11 0.062(3) 0.073(3) 0.080(4) 0.038(3) 0.002(3) -0.002(2) C12 0.063(3) 0.083(4) 0.050(2) 0.016(2) 0.007(2) -0.009(2) C13 0.056(2) 0.056(2) 0.042(2) 0.0063(18) 0.0020(18) -0.0059(19) C14 0.0379(18) 0.050(2) 0.040(2) 0.0050(16) 0.0039(15) -0.0068(17) C15 0.049(2) 0.059(3) 0.070(3) -0.006(2) 0.017(2) -0.007(2) C16 0.055(3) 0.092(4) 0.084(4) -0.005(3) 0.027(2) 0.004(3) C17 0.048(3) 0.111(4) 0.080(4) 0.016(3) 0.019(2) -0.016(3) C18 0.055(3) 0.079(3) 0.078(3) 0.023(3) 0.006(2) -0.026(2) C19 0.049(2) 0.053(2) 0.062(3) 0.014(2) 0.0026(19) -0.0112(19) C20 0.071(3) 0.063(3) 0.049(3) -0.005(2) -0.001(2) -0.006(2) C21 0.098(4) 0.081(4) 0.054(3) -0.008(2) -0.011(3) -0.022(3) C22 0.099(4) 0.103(4) 0.063(3) 0.005(3) -0.028(3) -0.040(4) C23 0.057(3) 0.111(5) 0.077(4) 0.016(3) -0.017(3) -0.018(3) C24 0.049(2) 0.070(3) 0.054(3) 0.013(2) -0.0030(19) -0.010(2) C25 0.038(2) 0.077(3) 0.075(3) 0.017(2) 0.006(2) 0.003(2) C26 0.052(3) 0.137(6) 0.129(6) -0.004(5) 0.010(3) 0.018(3) C27 0.068(4) 0.147(7) 0.164(7) -0.011(6) 0.033(4) 0.039(4) C28 0.094(4) 0.101(5) 0.125(6) -0.017(4) 0.042(4) 0.025(4) C29 0.067(3) 0.066(3) 0.080(3) -0.002(3) 0.027(3) 0.013(2) C30 0.060(2) 0.055(2) 0.040(2) -0.0008(18) 0.0001(18) -0.007(2) C31 0.060(3) 0.072(3) 0.048(2) -0.008(2) 0.001(2) -0.007(2) C32 0.061(3) 0.078(3) 0.062(3) -0.021(2) 0.006(2) -0.022(2) C33 0.063(3) 0.058(3) 0.059(3) -0.005(2) 0.015(2) -0.020(2) C34 0.043(2) 0.039(2) 0.049(2) -0.0014(17) 0.0129(17) -0.0045(16) C35 0.0442(19) 0.0355(19) 0.050(2) 0.0037(16) 0.0143(17) -0.0017(16) C36 0.071(3) 0.045(2) 0.060(3) 0.005(2) 0.018(2) -0.006(2) C37 0.084(3) 0.048(2) 0.068(3) 0.018(2) 0.026(3) 0.000(2) C38 0.086(3) 0.062(3) 0.046(2) 0.018(2) 0.008(2) 0.002(2) C39 0.077(3) 0.054(2) 0.038(2) 0.0111(18) 0.006(2) -0.008(2) N1 0.0394(15) 0.0423(17) 0.0372(16) -0.0014(13) 0.0085(13) -0.0043(13) N3 0.0387(15) 0.0361(15) 0.0357(16) 0.0047(12) 0.0071(12) -0.0050(12) N4 0.0367(15) 0.0408(16) 0.0397(17) 0.0067(13) 0.0076(13) -0.0063(13) N5 0.0406(16) 0.0413(17) 0.0389(16) 0.0031(13) 0.0021(13) -0.0027(13) N6 0.0446(17) 0.0485(18) 0.0403(17) 0.0041(14) 0.0007(14) -0.0085(14) N7 0.0453(17) 0.0477(19) 0.053(2) 0.0123(15) 0.0155(15) 0.0058(15) N8 0.0435(16) 0.0433(17) 0.0362(16) -0.0016(13) 0.0058(13) -0.0079(13) N9 0.0520(17) 0.0374(16) 0.0371(16) 0.0113(13) 0.0108(14) -0.0024(14) N2 0.0449(18) 0.062(2) 0.065(2) -0.0011(18) 0.0161(17) 0.0007(16) Cl1 0.0497(6) 0.0709(8) 0.0697(7) -0.0081(6) 0.0050(5) -0.0058(5) Cl2 0.0667(7) 0.0546(6) 0.0990(9) -0.0080(7) 0.0256(7) -0.0120(6) O1 0.083(2) 0.146(4) 0.113(3) -0.055(3) -0.005(2) 0.042(3) O2 0.201(6) 0.119(4) 0.241(7) 0.060(4) 0.097(5) -0.035(4) O3 0.0542(19) 0.147(3) 0.108(3) -0.052(3) 0.0167(19) -0.017(2) O4 0.119(3) 0.172(5) 0.088(3) -0.059(3) -0.025(3) 0.034(3) O5 0.165(5) 0.096(3) 0.266(7) -0.090(4) 0.121(5) -0.066(3) O6 0.084(3) 0.213(6) 0.132(4) -0.086(4) 0.041(3) -0.047(3) O7 0.176(5) 0.093(3) 0.125(4) 0.027(3) -0.003(3) -0.030(3) O8 0.082(3) 0.098(3) 0.275(7) 0.035(4) -0.033(4) -0.006(2) _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 Ru N3 2.026(3) . ? Ru N1 2.050(3) . ? Ru N6 2.070(3) . ? Ru N7 2.071(3) . ? Ru N8 2.074(3) . ? Ru N9 2.076(3) . ? C1 N1 1.333(4) . ? C1 C2 1.379(5) . ? C1 H1A 0.9300 . ? C2 N2 1.334(5) . ? C2 H2A 0.9300 . ? C3 N2 1.337(5) . ? C3 C4 1.381(5) . ? C3 H3A 0.9300 . ? C4 N1 1.368(4) . ? C4 C5 1.460(5) . ? C5 N5 1.332(4) . ? C5 N3 1.347(4) . ? C6 N5 1.337(4) . ? C6 C7 1.417(5) . ? C6 C8 1.482(5) . ? C7 N4 1.331(4) . ? C7 C14 1.482(5) . ? C8 C9 1.383(5) . ? C8 C13 1.393(5) . ? C9 C10 1.389(6) . ? C9 H9A 0.9300 . ? C10 C11 1.368(7) . ? C10 H10A 0.9300 . ? C11 C12 1.374(7) . ? C11 H11A 0.9300 . ? C12 C13 1.390(6) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 C15 1.381(5) . ? C14 C19 1.395(5) . ? C15 C16 1.388(6) . ? C15 H15A 0.9300 . ? C16 C17 1.369(7) . ? C16 H16A 0.9300 . ? C17 C18 1.369(7) . ? C17 H17A 0.9300 . ? C18 C19 1.387(6) . ? C18 H18A 0.9300 . ? C19 H19A 0.9300 . ? C20 N6 1.340(5) . ? C20 C21 1.373(6) . ? C20 H20A 0.9300 . ? C21 C22 1.352(8) . ? C21 H21A 0.9300 . ? C22 C23 1.369(8) . ? C22 H22A 0.9300 . ? C23 C24 1.398(6) . ? C23 H23A 0.9300 . ? C24 N6 1.349(5) . ? C24 C25 1.468(7) . ? C25 N7 1.360(5) . ? C25 C26 1.386(6) . ? C26 C27 1.371(9) . ? C26 H26A 0.9300 . ? C27 C28 1.370(9) . ? C27 H27A 0.9300 . ? C28 C29 1.382(7) . ? C28 H28A 0.9300 . ? C29 N7 1.339(5) . ? C29 H29A 0.9300 . ? C30 N8 1.340(5) . ? C30 C31 1.379(5) . ? C30 H30A 0.9300 . ? C31 C32 1.366(6) . ? C31 H31A 0.9300 . ? C32 C33 1.376(6) . ? C32 H32A 0.9300 . ? C33 C34 1.378(5) . ? C33 H33A 0.9300 . ? C34 N8 1.365(4) . ? C34 C35 1.472(5) . ? C35 N9 1.364(4) . ? C35 C36 1.385(5) . ? C36 C37 1.369(6) . ? C36 H36A 0.9300 . ? C37 C38 1.366(6) . ? C37 H37A 0.9300 . ? C38 C39 1.378(5) . ? C38 H38A 0.9300 . ? C39 N9 1.339(5) . ? C39 H39A 0.9300 . ? N3 N4 1.341(4) . ? Cl1 O2 1.343(5) . ? Cl1 O3 1.415(3) . ? Cl1 O4 1.418(4) . ? Cl1 O1 1.420(4) . ? Cl2 O6 1.386(4) . ? Cl2 O5 1.388(4) . ? Cl2 O7 1.399(4) . ? Cl2 O8 1.436(5) . ? 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 N3 Ru N1 78.47(11) . . ? N3 Ru N6 88.16(11) . . ? N1 Ru N6 99.10(12) . . ? N3 Ru N7 95.01(11) . . ? N1 Ru N7 173.21(11) . . ? N6 Ru N7 78.66(13) . . ? N3 Ru N8 97.58(11) . . ? N1 Ru N8 86.15(11) . . ? N6 Ru N8 172.93(12) . . ? N7 Ru N8 96.66(12) . . ? N3 Ru N9 174.34(11) . . ? N1 Ru N9 96.97(11) . . ? N6 Ru N9 95.92(12) . . ? N7 Ru N9 89.66(12) . . ? N8 Ru N9 78.65(12) . . ? N1 C1 C2 121.4(4) . . ? N1 C1 H1A 119.3 . . ? C2 C1 H1A 119.3 . . ? N2 C2 C1 122.9(4) . . ? N2 C2 H2A 118.6 . . ? C1 C2 H2A 118.6 . . ? N2 C3 C4 122.5(4) . . ? N2 C3 H3A 118.7 . . ? C4 C3 H3A 118.7 . . ? N1 C4 C3 120.7(3) . . ? N1 C4 C5 114.4(3) . . ? C3 C4 C5 124.9(3) . . ? N5 C5 N3 124.3(3) . . ? N5 C5 C4 121.5(3) . . ? N3 C5 C4 114.2(3) . . ? N5 C6 C7 119.4(3) . . ? N5 C6 C8 116.7(3) . . ? C7 C6 C8 124.0(3) . . ? N4 C7 C6 121.5(3) . . ? N4 C7 C14 113.2(3) . . ? C6 C7 C14 125.3(3) . . ? C9 C8 C13 119.4(4) . . ? C9 C8 C6 119.4(3) . . ? C13 C8 C6 121.2(3) . . ? C8 C9 C10 120.0(4) . . ? C8 C9 H9A 120.0 . . ? C10 C9 H9A 120.0 . . ? C11 C10 C9 120.7(5) . . ? C11 C10 H10A 119.7 . . ? C9 C10 H10A 119.7 . . ? C10 C11 C12 119.7(4) . . ? C10 C11 H11A 120.1 . . ? C12 C11 H11A 120.1 . . ? C11 C12 C13 120.7(4) . . ? C11 C12 H12A 119.7 . . ? C13 C12 H12A 119.7 . . ? C12 C13 C8 119.5(4) . . ? C12 C13 H13A 120.2 . . ? C8 C13 H13A 120.2 . . ? C15 C14 C19 119.4(3) . . ? C15 C14 C7 119.6(3) . . ? C19 C14 C7 120.8(3) . . ? C14 C15 C16 120.3(4) . . ? C14 C15 H15A 119.9 . . ? C16 C15 H15A 119.9 . . ? C17 C16 C15 119.9(5) . . ? C17 C16 H16A 120.1 . . ? C15 C16 H16A 120.1 . . ? C18 C17 C16 120.6(4) . . ? C18 C17 H17A 119.7 . . ? C16 C17 H17A 119.7 . . ? C17 C18 C19 120.3(4) . . ? C17 C18 H18A 119.9 . . ? C19 C18 H18A 119.9 . . ? C18 C19 C14 119.6(4) . . ? C18 C19 H19A 120.2 . . ? C14 C19 H19A 120.2 . . ? N6 C20 C21 122.7(5) . . ? N6 C20 H20A 118.7 . . ? C21 C20 H20A 118.7 . . ? C22 C21 C20 118.9(5) . . ? C22 C21 H21A 120.5 . . ? C20 C21 H21A 120.5 . . ? C21 C22 C23 120.1(5) . . ? C21 C22 H22A 120.0 . . ? C23 C22 H22A 120.0 . . ? C22 C23 C24 119.1(5) . . ? C22 C23 H23A 120.5 . . ? C24 C23 H23A 120.5 . . ? N6 C24 C23 120.6(5) . . ? N6 C24 C25 115.1(4) . . ? C23 C24 C25 124.3(4) . . ? N7 C25 C26 120.0(5) . . ? N7 C25 C24 115.5(3) . . ? C26 C25 C24 124.5(5) . . ? C27 C26 C25 119.6(6) . . ? C27 C26 H26A 120.2 . . ? C25 C26 H26A 120.2 . . ? C28 C27 C26 120.1(6) . . ? C28 C27 H27A 119.9 . . ? C26 C27 H27A 119.9 . . ? C27 C28 C29 118.6(6) . . ? C27 C28 H28A 120.7 . . ? C29 C28 H28A 120.7 . . ? N7 C29 C28 121.8(5) . . ? N7 C29 H29A 119.1 . . ? C28 C29 H29A 119.1 . . ? N8 C30 C31 122.6(4) . . ? N8 C30 H30A 118.7 . . ? C31 C30 H30A 118.7 . . ? C32 C31 C30 118.8(4) . . ? C32 C31 H31A 120.6 . . ? C30 C31 H31A 120.6 . . ? C31 C32 C33 119.5(4) . . ? C31 C32 H32A 120.2 . . ? C33 C32 H32A 120.2 . . ? C32 C33 C34 119.8(4) . . ? C32 C33 H33A 120.1 . . ? C34 C33 H33A 120.1 . . ? N8 C34 C33 120.8(4) . . ? N8 C34 C35 114.8(3) . . ? C33 C34 C35 124.4(3) . . ? N9 C35 C36 120.6(4) . . ? N9 C35 C34 115.4(3) . . ? C36 C35 C34 124.0(4) . . ? C37 C36 C35 119.6(4) . . ? C37 C36 H36A 120.2 . . ? C35 C36 H36A 120.2 . . ? C38 C37 C36 119.9(4) . . ? C38 C37 H37A 120.1 . . ? C36 C37 H37A 120.1 . . ? C37 C38 C39 118.8(4) . . ? C37 C38 H38A 120.6 . . ? C39 C38 H38A 120.6 . . ? N9 C39 C38 122.4(4) . . ? N9 C39 H39A 118.8 . . ? C38 C39 H39A 118.8 . . ? C1 N1 C4 116.6(3) . . ? C1 N1 Ru 128.0(3) . . ? C4 N1 Ru 115.3(2) . . ? N4 N3 C5 119.8(3) . . ? N4 N3 Ru 122.9(2) . . ? C5 N3 Ru 117.1(2) . . ? C7 N4 N3 117.7(3) . . ? C5 N5 C6 116.7(3) . . ? C20 N6 C24 118.6(4) . . ? C20 N6 Ru 125.8(3) . . ? C24 N6 Ru 115.5(3) . . ? C29 N7 C25 119.9(4) . . ? C29 N7 Ru 125.2(3) . . ? C25 N7 Ru 114.9(3) . . ? C30 N8 C34 118.5(3) . . ? C30 N8 Ru 125.7(3) . . ? C34 N8 Ru 115.7(2) . . ? C39 N9 C35 118.7(3) . . ? C39 N9 Ru 125.9(3) . . ? C35 N9 Ru 115.4(2) . . ? C2 N2 C3 116.0(3) . . ? O2 Cl1 O3 109.3(3) . . ? O2 Cl1 O4 108.3(4) . . ? O3 Cl1 O4 108.3(3) . . ? O2 Cl1 O1 111.1(3) . . ? O3 Cl1 O1 109.8(2) . . ? O4 Cl1 O1 110.0(3) . . ? O6 Cl2 O5 110.5(3) . . ? O6 Cl2 O7 108.8(4) . . ? O5 Cl2 O7 111.6(4) . . ? O6 Cl2 O8 108.9(4) . . ? O5 Cl2 O8 111.1(3) . . ? O7 Cl2 O8 105.7(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 N1 C1 C2 N2 1.4(6) . . . . ? N2 C3 C4 N1 1.1(6) . . . . ? N2 C3 C4 C5 179.5(3) . . . . ? N1 C4 C5 N5 178.2(3) . . . . ? C3 C4 C5 N5 -0.3(5) . . . . ? N1 C4 C5 N3 -1.6(4) . . . . ? C3 C4 C5 N3 179.8(3) . . . . ? N5 C6 C7 N4 -7.1(5) . . . . ? C8 C6 C7 N4 174.1(3) . . . . ? N5 C6 C7 C14 171.5(3) . . . . ? C8 C6 C7 C14 -7.3(5) . . . . ? N5 C6 C8 C9 -42.6(5) . . . . ? C7 C6 C8 C9 136.3(4) . . . . ? N5 C6 C8 C13 137.5(4) . . . . ? C7 C6 C8 C13 -43.6(5) . . . . ? C13 C8 C9 C10 1.3(6) . . . . ? C6 C8 C9 C10 -178.6(4) . . . . ? C8 C9 C10 C11 0.0(8) . . . . ? C9 C10 C11 C12 -1.6(8) . . . . ? C10 C11 C12 C13 1.8(7) . . . . ? C11 C12 C13 C8 -0.5(6) . . . . ? C9 C8 C13 C12 -1.1(6) . . . . ? C6 C8 C13 C12 178.8(3) . . . . ? N4 C7 C14 C15 -42.5(5) . . . . ? C6 C7 C14 C15 138.8(4) . . . . ? N4 C7 C14 C19 131.8(4) . . . . ? C6 C7 C14 C19 -46.9(5) . . . . ? C19 C14 C15 C16 0.9(6) . . . . ? C7 C14 C15 C16 175.2(4) . . . . ? C14 C15 C16 C17 -1.0(7) . . . . ? C15 C16 C17 C18 0.4(8) . . . . ? C16 C17 C18 C19 0.4(8) . . . . ? C17 C18 C19 C14 -0.5(7) . . . . ? C15 C14 C19 C18 -0.1(6) . . . . ? C7 C14 C19 C18 -174.4(4) . . . . ? N6 C20 C21 C22 0.0(8) . . . . ? C20 C21 C22 C23 1.0(8) . . . . ? C21 C22 C23 C24 -0.6(8) . . . . ? C22 C23 C24 N6 -0.8(7) . . . . ? C22 C23 C24 C25 178.5(5) . . . . ? N6 C24 C25 N7 -1.0(6) . . . . ? C23 C24 C25 N7 179.7(4) . . . . ? N6 C24 C25 C26 177.0(5) . . . . ? C23 C24 C25 C26 -2.4(8) . . . . ? N7 C25 C26 C27 -0.9(9) . . . . ? C24 C25 C26 C27 -178.8(6) . . . . ? C25 C26 C27 C28 1.7(11) . . . . ? C26 C27 C28 C29 -1.6(11) . . . . ? C27 C28 C29 N7 0.6(9) . . . . ? N8 C30 C31 C32 1.4(7) . . . . ? C30 C31 C32 C33 -0.8(7) . . . . ? C31 C32 C33 C34 -0.2(7) . . . . ? C32 C33 C34 N8 0.7(6) . . . . ? C32 C33 C34 C35 -176.8(4) . . . . ? N8 C34 C35 N9 -2.1(5) . . . . ? C33 C34 C35 N9 175.5(4) . . . . ? N8 C34 C35 C36 179.7(3) . . . . ? C33 C34 C35 C36 -2.6(6) . . . . ? N9 C35 C36 C37 -0.1(6) . . . . ? C34 C35 C36 C37 178.0(4) . . . . ? C35 C36 C37 C38 -0.9(7) . . . . ? C36 C37 C38 C39 1.1(7) . . . . ? C37 C38 C39 N9 -0.1(7) . . . . ? C2 C1 N1 C4 -1.3(5) . . . . ? C2 C1 N1 Ru 173.1(3) . . . . ? C3 C4 N1 C1 0.1(5) . . . . ? C5 C4 N1 C1 -178.5(3) . . . . ? C3 C4 N1 Ru -175.0(3) . . . . ? C5 C4 N1 Ru 6.4(4) . . . . ? N3 Ru N1 C1 179.0(3) . . . . ? N6 Ru N1 C1 92.8(3) . . . . ? N7 Ru N1 C1 163.0(9) . . . . ? N8 Ru N1 C1 -82.4(3) . . . . ? N9 Ru N1 C1 -4.3(3) . . . . ? N3 Ru N1 C4 -6.6(2) . . . . ? N6 Ru N1 C4 -92.8(2) . . . . ? N7 Ru N1 C4 -22.7(11) . . . . ? N8 Ru N1 C4 92.0(2) . . . . ? N9 Ru N1 C4 170.0(2) . . . . ? N5 C5 N3 N4 -8.7(5) . . . . ? C4 C5 N3 N4 171.1(3) . . . . ? N5 C5 N3 Ru 176.1(3) . . . . ? C4 C5 N3 Ru -4.1(4) . . . . ? N1 Ru N3 N4 -169.2(3) . . . . ? N6 Ru N3 N4 -69.6(3) . . . . ? N7 Ru N3 N4 8.9(3) . . . . ? N8 Ru N3 N4 106.3(3) . . . . ? N9 Ru N3 N4 154.2(11) . . . . ? N1 Ru N3 C5 5.8(2) . . . . ? N6 Ru N3 C5 105.5(2) . . . . ? N7 Ru N3 C5 -176.1(2) . . . . ? N8 Ru N3 C5 -78.7(2) . . . . ? N9 Ru N3 C5 -30.8(13) . . . . ? C6 C7 N4 N3 3.8(5) . . . . ? C14 C7 N4 N3 -174.9(3) . . . . ? C5 N3 N4 C7 3.7(4) . . . . ? Ru N3 N4 C7 178.6(2) . . . . ? N3 C5 N5 C6 5.3(5) . . . . ? C4 C5 N5 C6 -174.5(3) . . . . ? C7 C6 N5 C5 2.5(5) . . . . ? C8 C6 N5 C5 -178.6(3) . . . . ? C21 C20 N6 C24 -1.4(6) . . . . ? C21 C20 N6 Ru 175.9(3) . . . . ? C23 C24 N6 C20 1.8(6) . . . . ? C25 C24 N6 C20 -177.6(4) . . . . ? C23 C24 N6 Ru -175.8(3) . . . . ? C25 C24 N6 Ru 4.8(5) . . . . ? N3 Ru N6 C20 -87.0(3) . . . . ? N1 Ru N6 C20 -8.9(3) . . . . ? N7 Ru N6 C20 177.6(3) . . . . ? N8 Ru N6 C20 128.6(9) . . . . ? N9 Ru N6 C20 89.1(3) . . . . ? N3 Ru N6 C24 90.4(3) . . . . ? N1 Ru N6 C24 168.4(3) . . . . ? N7 Ru N6 C24 -5.1(3) . . . . ? N8 Ru N6 C24 -54.0(10) . . . . ? N9 Ru N6 C24 -93.5(3) . . . . ? C28 C29 N7 C25 0.2(7) . . . . ? C28 C29 N7 Ru -178.3(4) . . . . ? C26 C25 N7 C29 0.0(7) . . . . ? C24 C25 N7 C29 178.0(4) . . . . ? C26 C25 N7 Ru 178.6(4) . . . . ? C24 C25 N7 Ru -3.3(5) . . . . ? N3 Ru N7 C29 95.9(3) . . . . ? N1 Ru N7 C29 111.7(10) . . . . ? N6 Ru N7 C29 -177.0(3) . . . . ? N8 Ru N7 C29 -2.3(3) . . . . ? N9 Ru N7 C29 -80.9(3) . . . . ? N3 Ru N7 C25 -82.6(3) . . . . ? N1 Ru N7 C25 -66.8(11) . . . . ? N6 Ru N7 C25 4.5(3) . . . . ? N8 Ru N7 C25 179.1(3) . . . . ? N9 Ru N7 C25 100.6(3) . . . . ? C31 C30 N8 C34 -0.9(6) . . . . ? C31 C30 N8 Ru 175.9(3) . . . . ? C33 C34 N8 C30 -0.2(5) . . . . ? C35 C34 N8 C30 177.6(3) . . . . ? C33 C34 N8 Ru -177.3(3) . . . . ? C35 C34 N8 Ru 0.5(4) . . . . ? N3 Ru N8 C30 -0.5(3) . . . . ? N1 Ru N8 C30 -78.3(3) . . . . ? N6 Ru N8 C30 143.6(9) . . . . ? N7 Ru N8 C30 95.5(3) . . . . ? N9 Ru N8 C30 -176.2(3) . . . . ? N3 Ru N8 C34 176.4(2) . . . . ? N1 Ru N8 C34 98.6(3) . . . . ? N6 Ru N8 C34 -39.5(11) . . . . ? N7 Ru N8 C34 -87.6(3) . . . . ? N9 Ru N8 C34 0.7(2) . . . . ? C38 C39 N9 C35 -0.9(6) . . . . ? C38 C39 N9 Ru 179.2(3) . . . . ? C36 C35 N9 C39 1.0(5) . . . . ? C34 C35 N9 C39 -177.2(3) . . . . ? C36 C35 N9 Ru -179.0(3) . . . . ? C34 C35 N9 Ru 2.7(4) . . . . ? N3 Ru N9 C39 129.5(11) . . . . ? N1 Ru N9 C39 93.5(3) . . . . ? N6 Ru N9 C39 -6.5(3) . . . . ? N7 Ru N9 C39 -85.1(3) . . . . ? N8 Ru N9 C39 178.1(3) . . . . ? N3 Ru N9 C35 -50.5(13) . . . . ? N1 Ru N9 C35 -86.5(3) . . . . ? N6 Ru N9 C35 173.5(3) . . . . ? N7 Ru N9 C35 95.0(3) . . . . ? N8 Ru N9 C35 -1.9(2) . . . . ? C1 C2 N2 C3 -0.2(6) . . . . ? C4 C3 N2 C2 -1.0(6) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.22 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.671 _refine_diff_density_min -0.710 _refine_diff_density_rms 0.075 data_dta _database_code_CSD 192535 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H9 N5' _chemical_formula_weight 283.29 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 0.0000 '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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 11.133(10) _cell_length_b 26.01(2) _cell_length_c 13.574(12) _cell_angle_alpha 90.00 _cell_angle_beta 106.140(16) _cell_angle_gamma 90.00 _cell_volume 3775(6) _cell_formula_units_Z 12 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.495 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1752 _exptl_absorpt_coefficient_mu 0.095 _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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11008 _diffrn_reflns_av_R_equivalents 0.0384 _diffrn_reflns_av_sigmaI/netI 0.0522 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 27.10 _reflns_number_total 4092 _reflns_number_gt 2375 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.1000P)^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 none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0(10) _refine_ls_number_reflns 4092 _refine_ls_number_parameters 595 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1071 _refine_ls_R_factor_gt 0.0467 _refine_ls_wR_factor_ref 0.1672 _refine_ls_wR_factor_gt 0.1227 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C2 C -0.1659(8) 0.1004(3) 0.6432(6) 0.062(2) Uani 1 1 d . . . H2A H -0.1913 0.0697 0.6665 0.075 Uiso 1 1 calc R . . N2 N -0.0653(5) 0.17996(19) 0.6868(4) 0.0512(14) Uani 1 1 d . . . N3 N 0.0011(4) 0.27329(17) 0.6307(3) 0.0413(11) Uani 1 1 d . . . N4 N -0.0816(4) 0.24797(17) 0.4547(3) 0.0469(12) Uani 1 1 d . . . N5 N -0.0493(4) 0.29344(18) 0.4197(4) 0.0483(12) Uani 1 1 d . . . C19 C 0.3323(6) 0.7277(2) 0.1431(5) 0.0518(17) Uani 1 1 d . . . H19A H 0.3042 0.7578 0.1664 0.062 Uiso 1 1 calc R . . N7 N 0.4451(5) 0.65001(18) 0.1878(4) 0.0445(12) Uani 1 1 d . . . N8 N 0.5189(4) 0.55822(16) 0.1318(3) 0.0388(10) Uani 1 1 d . . . N9 N 0.4344(4) 0.58235(17) -0.0452(3) 0.0457(12) Uani 1 1 d . . . N10 N 0.4653(4) 0.53672(18) -0.0796(3) 0.0476(12) Uani 1 1 d . . . C36 C 0.4575(8) -0.0630(3) 0.0410(6) 0.068(2) Uani 1 1 d . . . H36A H 0.4904 -0.0922 0.0188 0.082 Uiso 1 1 calc R . . N12 N 0.3433(5) 0.0141(2) -0.0052(5) 0.0508(14) Uani 1 1 d . . . N13 N 0.2682(5) 0.10563(17) 0.0502(4) 0.0399(11) Uani 1 1 d . . . N14 N 0.3550(4) 0.08148(18) 0.2259(4) 0.0443(13) Uani 1 1 d . . . N15 N 0.3240(5) 0.12726(17) 0.2615(4) 0.0424(12) Uani 1 1 d . . . C1 C -0.1026(7) 0.1348(2) 0.7133(5) 0.0613(17) Uani 1 1 d . . . H1A H -0.0845 0.1265 0.7826 0.074 Uiso 1 1 calc R . . N1 N -0.1935(6) 0.1083(2) 0.5426(4) 0.0685(16) Uani 1 1 d . . . C3 C -0.1549(7) 0.1529(3) 0.5156(6) 0.0572(18) Uani 1 1 d . . . H3A H -0.1702 0.1600 0.4460 0.069 Uiso 1 1 calc R . . C4 C -0.0928(5) 0.18967(19) 0.5857(4) 0.0407(13) Uani 1 1 d . . . C5 C -0.0549(6) 0.2404(2) 0.5547(5) 0.0409(14) Uani 1 1 d . . . C6 C 0.0322(5) 0.31679(19) 0.5964(4) 0.0398(12) Uani 1 1 d . . . C7 C 0.0979(5) 0.3611(2) 0.6532(5) 0.0379(13) Uani 1 1 d . . . C8 C 0.1456(7) 0.3736(2) 0.7541(5) 0.0497(16) Uani 1 1 d . . . H8A H 0.1353 0.3517 0.8053 0.060 Uiso 1 1 calc R . . C9 C 0.2104(6) 0.4202(2) 0.7793(6) 0.0526(18) Uani 1 1 d . . . H9A H 0.2420 0.4288 0.8481 0.063 Uiso 1 1 calc R . . C10 C 0.2291(6) 0.4534(2) 0.7071(5) 0.0536(17) Uani 1 1 d . . . H10A H 0.2745 0.4834 0.7275 0.064 Uiso 1 1 calc R . . C11 C 0.1791(6) 0.4423(2) 0.5998(5) 0.0436(16) Uani 1 1 d . . . C12 C 0.1883(6) 0.4714(2) 0.5152(6) 0.057(2) Uani 1 1 d . . . H12A H 0.2300 0.5028 0.5253 0.069 Uiso 1 1 calc R . . C13 C 0.1355(7) 0.4535(3) 0.4170(6) 0.0552(18) Uani 1 1 d . . . H13A H 0.1441 0.4732 0.3622 0.066 Uiso 1 1 calc R . . C14 C 0.0698(6) 0.4073(2) 0.3957(6) 0.0490(17) Uani 1 1 d . . . H14A H 0.0337 0.3967 0.3285 0.059 Uiso 1 1 calc R . . C15 C 0.1140(6) 0.3960(2) 0.5781(5) 0.0394(14) Uani 1 1 d . . . C16 C 0.0600(6) 0.3779(2) 0.4769(5) 0.0404(14) Uani 1 1 d . . . C17 C 0.0068(5) 0.32729(18) 0.4889(4) 0.0396(12) Uani 1 1 d . . . C18 C 0.4004(6) 0.6937(2) 0.2127(5) 0.0531(15) Uani 1 1 d . . . H18A H 0.4166 0.7018 0.2819 0.064 Uiso 1 1 calc R . . N6 N 0.3044(5) 0.71906(18) 0.0418(4) 0.0541(13) Uani 1 1 d . . . C20 C 0.3506(5) 0.6755(2) 0.0150(5) 0.0441(15) Uani 1 1 d . . . H20A H 0.3372 0.6684 -0.0544 0.053 Uiso 1 1 calc R . . C21 C 0.4177(5) 0.64044(19) 0.0863(4) 0.0376(12) Uani 1 1 d . . . C22 C 0.4604(5) 0.5907(2) 0.0556(4) 0.0371(13) Uani 1 1 d . . . C23 C 0.5497(5) 0.51418(19) 0.0981(4) 0.0365(11) Uani 1 1 d . . . C24 C 0.6148(5) 0.4700(2) 0.1545(4) 0.0372(13) Uani 1 1 d . . . C25 C 0.6673(6) 0.4588(2) 0.2574(5) 0.0434(15) Uani 1 1 d . . . H25A H 0.6622 0.4819 0.3084 0.052 Uiso 1 1 calc R . . C26 C 0.7279(6) 0.4118(2) 0.2816(5) 0.0476(17) Uani 1 1 d . . . H26A H 0.7649 0.4042 0.3503 0.057 Uiso 1 1 calc R . . C27 C 0.7362(6) 0.3761(2) 0.2098(5) 0.0492(16) Uani 1 1 d . . . H27A H 0.7769 0.3450 0.2303 0.059 Uiso 1 1 calc R . . C28 C 0.6824(6) 0.3865(2) 0.1034(5) 0.0409(14) Uani 1 1 d . . . C29 C 0.6816(6) 0.3546(2) 0.0184(6) 0.0497(17) Uani 1 1 d . . . H29A H 0.7186 0.3223 0.0288 0.060 Uiso 1 1 calc R . . C30 C 0.6254(7) 0.3718(2) -0.0796(6) 0.0536(17) Uani 1 1 d . . . H30A H 0.6260 0.3503 -0.1342 0.064 Uiso 1 1 calc R . . C31 C 0.5676(6) 0.4199(2) -0.1016(5) 0.0437(16) Uani 1 1 d . . . H31A H 0.5303 0.4300 -0.1689 0.052 Uiso 1 1 calc R . . C32 C 0.6238(5) 0.4338(2) 0.0811(5) 0.0386(13) Uani 1 1 d . . . C33 C 0.5675(6) 0.4516(2) -0.0210(5) 0.0387(14) Uani 1 1 d . . . C34 C 0.5206(5) 0.50288(19) -0.0090(4) 0.0375(12) Uani 1 1 d . . . C35 C 0.3877(6) -0.0298(2) -0.0307(5) 0.0551(17) Uani 1 1 d . . . H35A H 0.3708 -0.0384 -0.0998 0.066 Uiso 1 1 calc R . . N11 N 0.4797(6) -0.0550(2) 0.1395(5) 0.0632(16) Uani 1 1 d . . . C37 C 0.4348(6) -0.0115(2) 0.1648(6) 0.0525(18) Uani 1 1 d . . . H37A H 0.4480 -0.0042 0.2341 0.063 Uiso 1 1 calc R . . C38 C 0.3699(5) 0.0233(2) 0.0945(5) 0.0376(13) Uani 1 1 d . . . C39 C 0.3277(6) 0.0733(2) 0.1258(5) 0.0385(14) Uani 1 1 d . . . C40 C 0.2359(5) 0.14947(18) 0.0841(5) 0.0346(12) Uani 1 1 d . . . C41 C 0.1682(5) 0.1933(2) 0.0274(5) 0.0379(14) Uani 1 1 d . . . C42 C 0.1185(6) 0.2047(2) -0.0733(5) 0.0461(16) Uani 1 1 d . . . H42A H 0.1266 0.1822 -0.1243 0.055 Uiso 1 1 calc R . . C43 C 0.0544(6) 0.2517(2) -0.0986(6) 0.0490(17) Uani 1 1 d . . . H43A H 0.0182 0.2596 -0.1673 0.059 Uiso 1 1 calc R . . C44 C 0.0437(6) 0.2863(2) -0.0248(6) 0.0509(17) Uani 1 1 d . . . H44A H 0.0004 0.3169 -0.0445 0.061 Uiso 1 1 calc R . . C45 C 0.0976(6) 0.2759(2) 0.0806(5) 0.0457(16) Uani 1 1 d . . . C46 C 0.0928(6) 0.3063(2) 0.1654(5) 0.0481(17) Uani 1 1 d . . . H46A H 0.0521 0.3379 0.1548 0.058 Uiso 1 1 calc R . . C47 C 0.1476(6) 0.2897(2) 0.2632(5) 0.0482(16) Uani 1 1 d . . . H47A H 0.1422 0.3102 0.3178 0.058 Uiso 1 1 calc R . . C48 C 0.2119(6) 0.2426(2) 0.2843(5) 0.0452(16) Uani 1 1 d . . . H48A H 0.2507 0.2326 0.3515 0.054 Uiso 1 1 calc R . . C49 C 0.1594(6) 0.2289(2) 0.1038(5) 0.0379(14) Uani 1 1 d . . . C50 C 0.2160(6) 0.2117(2) 0.2033(5) 0.0412(15) Uani 1 1 d . . . C51 C 0.2643(5) 0.1604(2) 0.1910(4) 0.0366(13) Uani 1 1 d . . . 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 C2 0.086(5) 0.044(4) 0.058(5) -0.003(3) 0.021(4) -0.012(3) N2 0.069(4) 0.046(3) 0.038(3) 0.003(2) 0.014(3) -0.004(3) N3 0.048(3) 0.044(3) 0.030(2) -0.001(2) 0.008(2) 0.003(2) N4 0.060(3) 0.045(3) 0.034(3) 0.001(2) 0.010(2) -0.003(2) N5 0.062(3) 0.049(3) 0.036(3) 0.001(2) 0.017(2) -0.001(2) C19 0.060(4) 0.044(4) 0.053(5) 0.002(3) 0.018(3) 0.005(3) N7 0.061(3) 0.041(3) 0.029(3) 0.001(2) 0.010(2) 0.002(2) N8 0.044(3) 0.040(2) 0.030(2) 0.0017(19) 0.008(2) 0.0011(19) N9 0.060(3) 0.044(3) 0.033(3) -0.0022(19) 0.013(2) -0.001(2) N10 0.059(3) 0.049(3) 0.034(3) -0.002(2) 0.012(2) 0.003(2) C36 0.100(6) 0.051(4) 0.060(6) 0.000(4) 0.032(5) 0.017(4) N12 0.066(4) 0.046(3) 0.043(4) 0.001(2) 0.018(3) 0.009(3) N13 0.046(3) 0.039(3) 0.035(3) 0.002(2) 0.012(2) 0.002(2) N14 0.055(3) 0.044(3) 0.034(3) 0.001(2) 0.013(3) 0.002(2) N15 0.052(3) 0.042(3) 0.032(3) 0.000(2) 0.009(2) 0.005(2) C1 0.092(5) 0.049(3) 0.043(4) 0.004(3) 0.020(4) -0.003(3) N1 0.093(5) 0.060(3) 0.051(4) -0.003(3) 0.017(3) -0.023(3) C3 0.072(5) 0.055(4) 0.042(4) -0.001(3) 0.012(3) -0.012(3) C4 0.046(3) 0.041(3) 0.035(3) -0.004(2) 0.012(2) 0.002(3) C5 0.044(3) 0.047(3) 0.033(3) -0.003(3) 0.014(3) 0.001(3) C6 0.039(3) 0.043(3) 0.036(3) 0.001(2) 0.009(2) 0.003(2) C7 0.037(3) 0.047(3) 0.031(3) -0.001(3) 0.011(2) 0.000(3) C8 0.059(4) 0.049(4) 0.042(4) -0.001(3) 0.014(3) 0.001(3) C9 0.067(4) 0.047(4) 0.038(4) -0.006(3) 0.006(3) 0.000(3) C10 0.057(4) 0.048(4) 0.047(4) -0.004(3) -0.001(3) -0.004(3) C11 0.043(4) 0.042(3) 0.047(4) 0.002(3) 0.015(3) 0.000(3) C12 0.068(5) 0.041(3) 0.069(6) 0.013(3) 0.030(4) 0.008(3) C13 0.065(5) 0.054(4) 0.050(5) 0.009(3) 0.022(3) 0.002(3) C14 0.054(4) 0.050(4) 0.045(4) 0.004(3) 0.017(3) 0.007(3) C15 0.044(4) 0.041(3) 0.034(4) 0.001(3) 0.013(3) 0.006(3) C16 0.045(4) 0.042(3) 0.038(4) 0.001(3) 0.018(3) 0.006(3) C17 0.044(3) 0.040(3) 0.035(3) -0.001(2) 0.013(2) 0.005(2) C18 0.077(5) 0.043(3) 0.041(4) -0.001(3) 0.018(3) 0.007(3) N6 0.065(3) 0.046(3) 0.050(3) 0.005(2) 0.012(3) 0.009(2) C20 0.051(4) 0.045(3) 0.033(3) 0.006(3) 0.006(3) 0.005(3) C21 0.039(3) 0.040(3) 0.034(3) 0.004(2) 0.010(2) -0.001(2) C22 0.036(3) 0.045(3) 0.029(3) 0.004(3) 0.006(2) 0.000(2) C23 0.042(3) 0.039(3) 0.029(3) -0.002(2) 0.011(2) -0.002(2) C24 0.046(3) 0.039(3) 0.027(3) 0.000(2) 0.010(3) -0.004(2) C25 0.051(4) 0.047(3) 0.031(4) -0.002(3) 0.009(3) 0.001(3) C26 0.059(4) 0.043(3) 0.037(4) 0.005(3) 0.007(3) 0.006(3) C27 0.063(4) 0.046(4) 0.034(4) 0.003(3) 0.008(3) 0.003(3) C28 0.055(4) 0.031(3) 0.035(3) 0.000(2) 0.010(3) -0.001(2) C29 0.069(4) 0.035(3) 0.048(4) -0.008(3) 0.021(3) 0.003(3) C30 0.071(5) 0.046(4) 0.048(4) -0.009(3) 0.024(4) -0.002(3) C31 0.058(4) 0.047(4) 0.027(4) -0.003(3) 0.014(3) -0.003(3) C32 0.042(3) 0.043(3) 0.031(3) -0.002(3) 0.011(3) 0.000(3) C33 0.045(3) 0.039(3) 0.033(3) -0.003(2) 0.012(3) -0.001(2) C34 0.046(3) 0.039(3) 0.028(3) 0.001(2) 0.011(2) -0.001(2) C35 0.076(5) 0.052(4) 0.038(4) -0.003(3) 0.016(4) 0.005(4) N11 0.087(5) 0.049(3) 0.053(4) 0.009(3) 0.018(3) 0.017(3) C37 0.068(5) 0.045(4) 0.043(4) 0.000(3) 0.014(4) 0.009(3) C38 0.037(3) 0.040(3) 0.035(4) 0.001(3) 0.011(3) -0.004(2) C39 0.041(3) 0.041(3) 0.032(4) 0.004(3) 0.008(3) -0.004(3) C40 0.041(3) 0.033(3) 0.031(3) -0.002(2) 0.012(2) -0.004(2) C41 0.046(4) 0.037(3) 0.032(3) -0.004(2) 0.013(3) -0.003(3) C42 0.062(4) 0.041(3) 0.037(4) 0.001(3) 0.016(3) 0.004(3) C43 0.064(4) 0.048(4) 0.033(4) 0.005(3) 0.009(3) 0.002(3) C44 0.067(5) 0.033(3) 0.054(5) 0.005(3) 0.020(4) 0.000(3) C45 0.054(4) 0.041(3) 0.044(4) -0.002(3) 0.016(3) -0.005(3) C46 0.056(4) 0.042(3) 0.043(4) -0.002(3) 0.009(3) 0.005(3) C47 0.059(4) 0.044(3) 0.043(4) -0.013(3) 0.017(3) -0.002(3) C48 0.054(4) 0.048(3) 0.031(4) -0.005(3) 0.009(3) -0.005(3) C49 0.043(3) 0.033(3) 0.038(4) 0.002(3) 0.011(3) -0.002(3) C50 0.048(4) 0.040(3) 0.036(4) -0.003(3) 0.014(3) -0.005(3) C51 0.036(3) 0.044(3) 0.027(3) 0.000(3) 0.005(2) -0.003(2) _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 C2 N1 1.330(9) . ? C2 C1 1.353(10) . ? N2 C1 1.329(7) . ? N2 C4 1.344(7) . ? N3 C6 1.306(7) . ? N3 C5 1.353(8) . ? N4 C5 1.321(8) . ? N4 N5 1.360(6) . ? N5 C17 1.312(7) . ? C19 N6 1.342(8) . ? C19 C18 1.360(8) . ? N7 C18 1.322(7) . ? N7 C21 1.349(7) . ? N8 C23 1.314(6) . ? N8 C22 1.353(7) . ? N9 C22 1.336(7) . ? N9 N10 1.354(6) . ? N10 C34 1.320(7) . ? C36 N11 1.307(9) . ? C36 C35 1.369(10) . ? N12 C38 1.325(8) . ? N12 C35 1.327(7) . ? N13 C40 1.316(7) . ? N13 C39 1.349(7) . ? N14 C39 1.325(8) . ? N14 N15 1.364(7) . ? N15 C51 1.322(7) . ? N1 C3 1.324(8) . ? C3 C4 1.390(9) . ? C4 C5 1.480(8) . ? C6 C17 1.433(8) . ? C6 C7 1.464(8) . ? C7 C8 1.363(9) . ? C7 C15 1.413(9) . ? C8 C9 1.402(9) . ? C9 C10 1.364(10) . ? C10 C11 1.436(10) . ? C11 C15 1.394(7) . ? C11 C12 1.404(9) . ? C12 C13 1.380(10) . ? C13 C14 1.395(9) . ? C14 C16 1.370(9) . ? C15 C16 1.418(9) . ? C16 C17 1.471(8) . ? N6 C20 1.335(7) . ? C20 C21 1.388(8) . ? C21 C22 1.478(7) . ? C23 C34 1.429(8) . ? C23 C24 1.456(8) . ? C24 C25 1.387(8) . ? C24 C32 1.395(8) . ? C25 C26 1.391(8) . ? C26 C27 1.367(9) . ? C27 C28 1.426(10) . ? C28 C32 1.386(8) . ? C28 C29 1.419(9) . ? C29 C30 1.379(10) . ? C30 C31 1.400(9) . ? C31 C33 1.369(8) . ? C32 C33 1.431(8) . ? C33 C34 1.458(8) . ? N11 C37 1.320(8) . ? C37 C38 1.367(9) . ? C38 C39 1.486(8) . ? C40 C51 1.425(8) . ? C40 C41 1.461(8) . ? C41 C42 1.358(9) . ? C41 C49 1.415(8) . ? C42 C43 1.408(9) . ? C43 C44 1.375(9) . ? C44 C45 1.415(10) . ? C45 C49 1.396(9) . ? C45 C46 1.411(9) . ? C46 C47 1.368(9) . ? C47 C48 1.408(9) . ? C48 C50 1.374(9) . ? C49 C50 1.395(9) . ? C50 C51 1.463(8) . ? 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 N1 C2 C1 123.1(7) . . ? C1 N2 C4 116.3(6) . . ? C6 N3 C5 112.8(5) . . ? C5 N4 N5 118.9(5) . . ? C17 N5 N4 116.9(5) . . ? N6 C19 C18 121.8(6) . . ? C18 N7 C21 115.2(5) . . ? C23 N8 C22 113.3(5) . . ? C22 N9 N10 119.5(5) . . ? C34 N10 N9 116.5(5) . . ? N11 C36 C35 122.4(7) . . ? C38 N12 C35 115.3(6) . . ? C40 N13 C39 113.4(5) . . ? C39 N14 N15 119.6(5) . . ? C51 N15 N14 116.1(5) . . ? N2 C1 C2 122.3(7) . . ? C3 N1 C2 114.8(6) . . ? N1 C3 C4 123.4(7) . . ? N2 C4 C3 119.9(5) . . ? N2 C4 C5 117.1(5) . . ? C3 C4 C5 123.0(6) . . ? N4 C5 N3 127.8(5) . . ? N4 C5 C4 115.1(5) . . ? N3 C5 C4 117.0(5) . . ? N3 C6 C17 122.1(5) . . ? N3 C6 C7 129.5(5) . . ? C17 C6 C7 108.3(4) . . ? C8 C7 C15 118.6(6) . . ? C8 C7 C6 135.7(6) . . ? C15 C7 C6 105.7(5) . . ? C7 C8 C9 118.8(6) . . ? C10 C9 C8 122.8(7) . . ? C9 C10 C11 120.5(6) . . ? C15 C11 C12 116.5(6) . . ? C15 C11 C10 114.8(5) . . ? C12 C11 C10 128.7(6) . . ? C13 C12 C11 119.9(6) . . ? C12 C13 C14 123.3(7) . . ? C16 C14 C13 117.9(7) . . ? C11 C15 C7 124.4(5) . . ? C11 C15 C16 123.2(5) . . ? C7 C15 C16 112.4(5) . . ? C14 C16 C15 119.1(6) . . ? C14 C16 C17 135.5(6) . . ? C15 C16 C17 105.4(5) . . ? N5 C17 C6 121.4(5) . . ? N5 C17 C16 130.3(5) . . ? C6 C17 C16 108.2(5) . . ? N7 C18 C19 124.0(6) . . ? C20 N6 C19 115.2(5) . . ? N6 C20 C21 122.7(6) . . ? N7 C21 C20 121.1(5) . . ? N7 C21 C22 116.8(5) . . ? C20 C21 C22 122.1(5) . . ? N9 C22 N8 127.0(5) . . ? N9 C22 C21 115.9(5) . . ? N8 C22 C21 117.1(5) . . ? N8 C23 C34 121.7(5) . . ? N8 C23 C24 130.1(5) . . ? C34 C23 C24 108.2(5) . . ? C25 C24 C32 118.9(5) . . ? C25 C24 C23 134.8(5) . . ? C32 C24 C23 106.3(5) . . ? C24 C25 C26 117.6(6) . . ? C27 C26 C25 123.6(7) . . ? C26 C27 C28 120.1(6) . . ? C32 C28 C29 116.4(5) . . ? C32 C28 C27 115.4(5) . . ? C29 C28 C27 128.2(6) . . ? C30 C29 C28 119.6(6) . . ? C29 C30 C31 123.7(6) . . ? C33 C31 C30 118.0(6) . . ? C28 C32 C24 124.5(5) . . ? C28 C32 C33 123.5(5) . . ? C24 C32 C33 112.0(5) . . ? C31 C33 C32 118.8(5) . . ? C31 C33 C34 136.0(6) . . ? C32 C33 C34 105.2(5) . . ? N10 C34 C23 121.9(5) . . ? N10 C34 C33 129.6(5) . . ? C23 C34 C33 108.4(5) . . ? N12 C35 C36 122.3(7) . . ? C36 N11 C37 115.2(6) . . ? N11 C37 C38 123.4(7) . . ? N12 C38 C37 121.2(6) . . ? N12 C38 C39 116.8(5) . . ? C37 C38 C39 121.9(6) . . ? N14 C39 N13 127.3(5) . . ? N14 C39 C38 115.6(5) . . ? N13 C39 C38 117.1(5) . . ? N13 C40 C51 121.6(5) . . ? N13 C40 C41 129.9(6) . . ? C51 C40 C41 108.4(5) . . ? C42 C41 C49 120.2(6) . . ? C42 C41 C40 135.1(6) . . ? C49 C41 C40 104.8(5) . . ? C41 C42 C43 118.2(6) . . ? C44 C43 C42 122.1(7) . . ? C43 C44 C45 120.9(6) . . ? C49 C45 C46 115.8(7) . . ? C49 C45 C44 116.1(6) . . ? C46 C45 C44 128.1(6) . . ? C47 C46 C45 120.4(6) . . ? C46 C47 C48 122.5(6) . . ? C50 C48 C47 118.3(6) . . ? C50 C49 C45 124.2(6) . . ? C50 C49 C41 113.2(6) . . ? C45 C49 C41 122.6(7) . . ? C48 C50 C49 118.7(6) . . ? C48 C50 C51 136.0(6) . . ? C49 C50 C51 105.3(5) . . ? N15 C51 C40 122.0(5) . . ? N15 C51 C50 129.7(6) . . ? C40 C51 C50 108.3(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 C5 N4 N5 C17 -0.3(7) . . . . ? C22 N9 N10 C34 -0.1(7) . . . . ? C39 N14 N15 C51 1.8(8) . . . . ? C4 N2 C1 C2 -0.6(10) . . . . ? N1 C2 C1 N2 1.5(12) . . . . ? C1 C2 N1 C3 -0.4(11) . . . . ? C2 N1 C3 C4 -1.5(11) . . . . ? C1 N2 C4 C3 -1.1(10) . . . . ? C1 N2 C4 C5 178.4(5) . . . . ? N1 C3 C4 N2 2.3(11) . . . . ? N1 C3 C4 C5 -177.2(6) . . . . ? N5 N4 C5 N3 1.0(9) . . . . ? N5 N4 C5 C4 -179.6(5) . . . . ? C6 N3 C5 N4 -1.2(8) . . . . ? C6 N3 C5 C4 179.5(5) . . . . ? N2 C4 C5 N4 178.8(6) . . . . ? C3 C4 C5 N4 -1.7(8) . . . . ? N2 C4 C5 N3 -1.8(7) . . . . ? C3 C4 C5 N3 177.8(6) . . . . ? C5 N3 C6 C17 0.6(7) . . . . ? C5 N3 C6 C7 -177.5(5) . . . . ? N3 C6 C7 C8 -1.4(11) . . . . ? C17 C6 C7 C8 -179.7(7) . . . . ? N3 C6 C7 C15 176.2(6) . . . . ? C17 C6 C7 C15 -2.2(6) . . . . ? C15 C7 C8 C9 -1.0(9) . . . . ? C6 C7 C8 C9 176.3(6) . . . . ? C7 C8 C9 C10 -0.7(11) . . . . ? C8 C9 C10 C11 1.6(11) . . . . ? C9 C10 C11 C15 -0.8(9) . . . . ? C9 C10 C11 C12 179.9(6) . . . . ? C15 C11 C12 C13 -0.7(8) . . . . ? C10 C11 C12 C13 178.7(7) . . . . ? C11 C12 C13 C14 1.1(11) . . . . ? C12 C13 C14 C16 -1.5(10) . . . . ? C12 C11 C15 C7 178.4(6) . . . . ? C10 C11 C15 C7 -1.0(7) . . . . ? C12 C11 C15 C16 0.7(7) . . . . ? C10 C11 C15 C16 -178.8(7) . . . . ? C8 C7 C15 C11 1.9(8) . . . . ? C6 C7 C15 C11 -176.2(5) . . . . ? C8 C7 C15 C16 179.9(6) . . . . ? C6 C7 C15 C16 1.8(6) . . . . ? C13 C14 C16 C15 1.3(9) . . . . ? C13 C14 C16 C17 -176.3(6) . . . . ? C11 C15 C16 C14 -1.0(8) . . . . ? C7 C15 C16 C14 -179.0(5) . . . . ? C11 C15 C16 C17 177.3(4) . . . . ? C7 C15 C16 C17 -0.8(6) . . . . ? N4 N5 C17 C6 -0.2(7) . . . . ? N4 N5 C17 C16 175.7(5) . . . . ? N3 C6 C17 N5 0.0(8) . . . . ? C7 C6 C17 N5 178.5(5) . . . . ? N3 C6 C17 C16 -176.7(5) . . . . ? C7 C6 C17 C16 1.8(6) . . . . ? C14 C16 C17 N5 0.9(11) . . . . ? C15 C16 C17 N5 -177.0(5) . . . . ? C14 C16 C17 C6 177.2(7) . . . . ? C15 C16 C17 C6 -0.7(6) . . . . ? C21 N7 C18 C19 -0.5(9) . . . . ? N6 C19 C18 N7 0.2(10) . . . . ? C18 C19 N6 C20 -1.4(9) . . . . ? C19 N6 C20 C21 2.9(9) . . . . ? C18 N7 C21 C20 1.9(8) . . . . ? C18 N7 C21 C22 -176.9(5) . . . . ? N6 C20 C21 N7 -3.3(9) . . . . ? N6 C20 C21 C22 175.5(5) . . . . ? N10 N9 C22 N8 1.6(8) . . . . ? N10 N9 C22 C21 -177.0(4) . . . . ? C23 N8 C22 N9 -1.0(8) . . . . ? C23 N8 C22 C21 177.7(5) . . . . ? N7 C21 C22 N9 -178.8(5) . . . . ? C20 C21 C22 N9 2.4(8) . . . . ? N7 C21 C22 N8 2.4(7) . . . . ? C20 C21 C22 N8 -176.4(5) . . . . ? C22 N8 C23 C34 -1.0(7) . . . . ? C22 N8 C23 C24 178.9(5) . . . . ? N8 C23 C24 C25 -1.4(11) . . . . ? C34 C23 C24 C25 178.5(6) . . . . ? N8 C23 C24 C32 -179.6(5) . . . . ? C34 C23 C24 C32 0.3(6) . . . . ? C32 C24 C25 C26 0.8(9) . . . . ? C23 C24 C25 C26 -177.2(6) . . . . ? C24 C25 C26 C27 -1.3(10) . . . . ? C25 C26 C27 C28 0.9(10) . . . . ? C26 C27 C28 C32 -0.1(9) . . . . ? C26 C27 C28 C29 179.9(6) . . . . ? C32 C28 C29 C30 0.7(9) . . . . ? C27 C28 C29 C30 -179.3(7) . . . . ? C28 C29 C30 C31 0.0(11) . . . . ? C29 C30 C31 C33 0.4(10) . . . . ? C29 C28 C32 C24 179.7(6) . . . . ? C27 C28 C32 C24 -0.3(8) . . . . ? C29 C28 C32 C33 -1.7(8) . . . . ? C27 C28 C32 C33 178.3(6) . . . . ? C25 C24 C32 C28 -0.1(9) . . . . ? C23 C24 C32 C28 178.5(5) . . . . ? C25 C24 C32 C33 -178.8(5) . . . . ? C23 C24 C32 C33 -0.2(7) . . . . ? C30 C31 C33 C32 -1.3(9) . . . . ? C30 C31 C33 C34 179.7(7) . . . . ? C28 C32 C33 C31 2.1(8) . . . . ? C24 C32 C33 C31 -179.2(6) . . . . ? C28 C32 C33 C34 -178.6(5) . . . . ? C24 C32 C33 C34 0.1(7) . . . . ? N9 N10 C34 C23 -1.8(8) . . . . ? N9 N10 C34 C33 -178.3(5) . . . . ? N8 C23 C34 N10 2.4(8) . . . . ? C24 C23 C34 N10 -177.4(5) . . . . ? N8 C23 C34 C33 179.7(5) . . . . ? C24 C23 C34 C33 -0.2(6) . . . . ? C31 C33 C34 N10 -3.9(11) . . . . ? C32 C33 C34 N10 177.0(6) . . . . ? C31 C33 C34 C23 179.2(7) . . . . ? C32 C33 C34 C23 0.1(6) . . . . ? C38 N12 C35 C36 -0.8(10) . . . . ? N11 C36 C35 N12 3.6(13) . . . . ? C35 C36 N11 C37 -2.9(12) . . . . ? C36 N11 C37 C38 -0.3(11) . . . . ? C35 N12 C38 C37 -2.4(9) . . . . ? C35 N12 C38 C39 176.8(5) . . . . ? N11 C37 C38 N12 3.0(10) . . . . ? N11 C37 C38 C39 -176.0(6) . . . . ? N15 N14 C39 N13 -1.4(9) . . . . ? N15 N14 C39 C38 177.5(5) . . . . ? C40 N13 C39 N14 0.1(8) . . . . ? C40 N13 C39 C38 -178.8(5) . . . . ? N12 C38 C39 N14 179.7(6) . . . . ? C37 C38 C39 N14 -1.2(8) . . . . ? N12 C38 C39 N13 -1.4(7) . . . . ? C37 C38 C39 N13 177.7(6) . . . . ? C39 N13 C40 C51 0.7(7) . . . . ? C39 N13 C40 C41 -178.2(6) . . . . ? N13 C40 C41 C42 -1.1(12) . . . . ? C51 C40 C41 C42 179.9(7) . . . . ? N13 C40 C41 C49 179.2(6) . . . . ? C51 C40 C41 C49 0.2(6) . . . . ? C49 C41 C42 C43 -2.6(9) . . . . ? C40 C41 C42 C43 177.8(6) . . . . ? C41 C42 C43 C44 1.6(10) . . . . ? C42 C43 C44 C45 0.1(10) . . . . ? C43 C44 C45 C49 -0.9(10) . . . . ? C43 C44 C45 C46 -178.3(6) . . . . ? C49 C45 C46 C47 0.7(9) . . . . ? C44 C45 C46 C47 178.1(7) . . . . ? C45 C46 C47 C48 0.8(10) . . . . ? C46 C47 C48 C50 -2.1(10) . . . . ? C46 C45 C49 C50 -1.0(10) . . . . ? C44 C45 C49 C50 -178.7(5) . . . . ? C46 C45 C49 C41 177.6(5) . . . . ? C44 C45 C49 C41 -0.1(9) . . . . ? C42 C41 C49 C50 -179.4(6) . . . . ? C40 C41 C49 C50 0.4(7) . . . . ? C42 C41 C49 C45 1.9(9) . . . . ? C40 C41 C49 C45 -178.4(6) . . . . ? C47 C48 C50 C49 1.7(9) . . . . ? C47 C48 C50 C51 -175.8(7) . . . . ? C45 C49 C50 C48 -0.2(10) . . . . ? C41 C49 C50 C48 -179.0(6) . . . . ? C45 C49 C50 C51 178.0(5) . . . . ? C41 C49 C50 C51 -0.8(7) . . . . ? N14 N15 C51 C40 -1.1(8) . . . . ? N14 N15 C51 C50 178.4(5) . . . . ? N13 C40 C51 N15 -0.1(9) . . . . ? C41 C40 C51 N15 179.0(5) . . . . ? N13 C40 C51 C50 -179.8(5) . . . . ? C41 C40 C51 C50 -0.7(6) . . . . ? C48 C50 C51 N15 -1.0(12) . . . . ? C49 C50 C51 N15 -178.8(5) . . . . ? C48 C50 C51 C40 178.6(7) . . . . ? C49 C50 C51 C40 0.9(6) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.174 _refine_diff_density_min -0.263 _refine_diff_density_rms 0.048 #========================================end