# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name ' Shi-Ping Yan' _publ_contact_author_email yansp@nankai.edu.cn loop_ _publ_author_name 'Shi-Ping Yan' 'Jin-Lei Tian' # Attachment '- complex 1.cif' data_aa _database_code_depnum_ccdc_archive 'CCDC 861138' #TrackingRef '- complex 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H72 Cl4 N10 O10 Zn2' _chemical_formula_sum 'C66 H72 Cl4 N10 O10 Zn2' _chemical_formula_weight 1437.92 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.703(3) _cell_length_b 11.830(2) _cell_length_c 18.743(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.16(3) _cell_angle_gamma 90.00 _cell_volume 3234.6(11) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 9195 _cell_measurement_theta_min 1.8786 _cell_measurement_theta_max 27.9464 _exptl_crystal_description Prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.476 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1492 _exptl_absorpt_coefficient_mu 0.974 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.792 _exptl_absorpt_correction_T_max 0.890 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(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 22309 _diffrn_reflns_av_R_equivalents 0.0441 _diffrn_reflns_av_sigmaI/netI 0.0423 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 25.50 _reflns_number_total 6031 _reflns_number_gt 5138 _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^)+(0.0977P)^2^+7.5024P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6031 _refine_ls_number_parameters 417 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0758 _refine_ls_R_factor_gt 0.0663 _refine_ls_wR_factor_ref 0.1797 _refine_ls_wR_factor_gt 0.1715 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 Zn1 Zn 0.32877(3) 0.64952(4) 0.13705(2) 0.02545(18) Uani 1 1 d . . . C1 C 0.2121(3) 1.1920(4) 0.0154(2) 0.0303(9) Uani 1 1 d . . . H1A H 0.2474 1.2599 0.0281 0.036 Uiso 1 1 calc R . . H1B H 0.2248 1.1690 -0.0321 0.036 Uiso 1 1 calc R . . C2 C 0.3329(3) 1.0527(3) 0.0665(2) 0.0267(9) Uani 1 1 d . . . H2 H 0.3692 1.0798 0.0331 0.032 Uiso 1 1 calc R . . C3 C 0.2019(3) 0.7316(3) 0.2339(2) 0.0218(8) Uani 1 1 d . . . C4 C 0.3129(3) 0.9238(3) 0.1634(2) 0.0233(8) Uani 1 1 d . . . C5 C -0.0097(3) 1.3449(3) 0.0388(2) 0.0318(10) Uani 1 1 d . . . H5 H -0.0271 1.4132 0.0576 0.038 Uiso 1 1 calc R . . C6 C 0.2269(3) 0.9717(3) 0.1669(2) 0.0227(8) Uani 1 1 d . . . H6 H 0.1911 0.9462 0.2011 0.027 Uiso 1 1 calc R . . C7 C 0.1941(3) 1.0574(3) 0.1194(2) 0.0245(8) Uani 1 1 d . . . H7 H 0.1360 1.0870 0.1221 0.029 Uiso 1 1 calc R . . C8 C -0.0481(3) 1.1686(4) -0.0205(2) 0.0322(10) Uani 1 1 d . . . H8 H -0.0911 1.1167 -0.0411 0.039 Uiso 1 1 calc R . . C9 C 0.1121(3) 1.2211(3) 0.0111(2) 0.0269(9) Uani 1 1 d . . . C10 C 0.0445(3) 1.1472(3) -0.0199(2) 0.0314(10) Uani 1 1 d . . . H10 H 0.0624 1.0809 -0.0410 0.038 Uiso 1 1 calc R . . C11 C 0.2457(3) 1.0998(3) 0.0683(2) 0.0245(9) Uani 1 1 d . . . C12 C 0.0820(3) 1.3206(4) 0.0399(2) 0.0305(9) Uani 1 1 d . . . H12 H 0.1252 1.3723 0.0605 0.037 Uiso 1 1 calc R . . C13 C 0.0474(3) 0.6720(4) 0.2404(3) 0.0378(11) Uani 1 1 d . . . H13 H -0.0050 0.6716 0.2635 0.045 Uiso 1 1 calc R . . C14 C 0.4763(3) 0.5208(4) 0.2296(2) 0.0360(11) Uani 1 1 d . . . H14 H 0.4498 0.4598 0.2035 0.043 Uiso 1 1 calc R . . C15 C 0.2875(3) 0.7952(3) 0.2625(2) 0.0246(8) Uani 1 1 d . . . H15A H 0.2703 0.8634 0.2863 0.030 Uiso 1 1 calc R . . H15B H 0.3237 0.7489 0.2982 0.030 Uiso 1 1 calc R . . C16 C 0.3667(3) 0.9670(3) 0.1128(2) 0.0284(9) Uani 1 1 d . . . H16 H 0.4250 0.9380 0.1104 0.034 Uiso 1 1 calc R . . C17 C 0.4418(3) 0.8297(4) 0.2365(3) 0.0315(10) Uani 1 1 d . . . H17A H 0.4483 0.8749 0.2800 0.038 Uiso 1 1 calc R . . H17B H 0.4770 0.8657 0.2024 0.038 Uiso 1 1 calc R . . C18 C -0.0770(3) 1.2688(4) 0.0099(2) 0.0293(9) Uani 1 1 d . . . C19 C 0.1301(3) 0.6111(4) 0.1468(2) 0.0284(9) Uani 1 1 d . . . H19 H 0.1329 0.5682 0.1056 0.034 Uiso 1 1 calc R . . C20 C 0.0497(3) 0.6118(4) 0.1771(3) 0.0341(10) Uani 1 1 d . . . H20 H -0.0017 0.5730 0.1558 0.041 Uiso 1 1 calc R . . C21 C 0.1248(3) 0.7332(4) 0.2691(2) 0.0337(10) Uani 1 1 d . . . H21 H 0.1243 0.7745 0.3113 0.040 Uiso 1 1 calc R . . C22 C 0.4799(3) 0.7129(4) 0.2538(2) 0.0279(9) Uani 1 1 d . . . C23 C -0.4649(3) 1.3303(4) -0.0405(2) 0.0312(10) Uani 1 1 d . . . H23 H -0.4985 1.3653 -0.0797 0.037 Uiso 1 1 calc R . . C24 C 0.5535(3) 0.6979(4) 0.3069(2) 0.0378(11) Uani 1 1 d . . . H24 H 0.5788 0.7594 0.3332 0.045 Uiso 1 1 calc R . . C25 C -0.3300(3) 1.2449(4) 0.0098(2) 0.0343(10) Uani 1 1 d . . . C26 C -0.5046(4) 1.3163(5) 0.0218(3) 0.0473(13) Uani 1 1 d . . . H26 H -0.5640 1.3409 0.0249 0.057 Uiso 1 1 calc R . . C27 C 0.5500(4) 0.5016(5) 0.2808(3) 0.0478(13) Uani 1 1 d . . . H27 H 0.5736 0.4291 0.2889 0.057 Uiso 1 1 calc R . . C28 C 0.5884(4) 0.5923(5) 0.3200(3) 0.0464(13) Uani 1 1 d . . . H28 H 0.6379 0.5813 0.3553 0.056 Uiso 1 1 calc R . . C29 C -0.3662(4) 1.2279(6) 0.0734(3) 0.0598(16) Uani 1 1 d . . . H29 H -0.3319 1.1921 0.1119 0.072 Uiso 1 1 calc R . . C30 C -0.4536(5) 1.2647(6) 0.0789(3) 0.0682(19) Uani 1 1 d . . . H30 H -0.4784 1.2546 0.1217 0.082 Uiso 1 1 calc R . . C31 C -0.2347(3) 1.2040(4) -0.0006(3) 0.0370(11) Uani 1 1 d . . . H31A H -0.2169 1.1428 0.0327 0.044 Uiso 1 1 calc R . . H31B H -0.2351 1.1752 -0.0491 0.044 Uiso 1 1 calc R . . C32 C 0.7914(4) 0.5643(5) 0.1218(4) 0.0590(16) Uani 1 1 d . . . H32A H 0.8049 0.5894 0.0749 0.071 Uiso 1 1 calc R . . H32B H 0.8191 0.6180 0.1571 0.071 Uiso 1 1 calc R . . C33 C 0.6938(4) 0.5662(6) 0.1224(4) 0.073(2) Uani 1 1 d . . . H33A H 0.6653 0.5149 0.0866 0.110 Uiso 1 1 calc R . . H33B H 0.6712 0.6413 0.1119 0.110 Uiso 1 1 calc R . . H33C H 0.6796 0.5436 0.1689 0.110 Uiso 1 1 calc R . . Cl1 Cl 0.30884(7) 0.46364(8) 0.09839(5) 0.0285(3) Uani 1 1 d . . . Cl2 Cl 0.66155(8) 0.92778(10) 0.16423(6) 0.0399(3) Uani 1 1 d . . . N1 N 0.4410(2) 0.6253(3) 0.21574(18) 0.0279(8) Uani 1 1 d . . . N2 N 0.3442(2) 0.8263(3) 0.20601(18) 0.0242(7) Uani 1 1 d . . . N3 N 0.2048(2) 0.6694(3) 0.17392(18) 0.0242(7) Uani 1 1 d . . . N4 N -0.1689(3) 1.2948(3) 0.0114(2) 0.0327(8) Uani 1 1 d . . . H4A H -0.1846 1.3483 -0.0219 0.039 Uiso 1 1 calc R . . H4B H -0.1745 1.3256 0.0546 0.039 Uiso 1 1 calc R . . N5 N -0.3792(2) 1.2951(3) -0.04640(17) 0.0220(7) Uani 1 1 d . . . O1 O 0.5990(3) 0.8570(4) 0.1195(2) 0.0646(12) Uani 1 1 d . . . O2 O 0.6129(3) 1.0177(4) 0.1941(2) 0.0702(13) Uani 1 1 d . . . O3 O 0.7258(3) 0.9722(4) 0.1222(3) 0.0762(15) Uani 1 1 d . . . O4 O 0.7041(5) 0.8634(5) 0.2231(3) 0.105(2) Uani 1 1 d . . . O5 O 0.8329(3) 0.4571(3) 0.13649(18) 0.0475(9) Uani 1 1 d . . . H5A H 0.8283 0.4391 0.1781 0.071 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 Zn1 0.0290(3) 0.0234(3) 0.0259(3) -0.00089(17) 0.0114(2) 0.00013(18) C1 0.032(2) 0.027(2) 0.032(2) 0.0014(17) 0.0041(19) -0.0011(18) C2 0.027(2) 0.025(2) 0.030(2) 0.0022(16) 0.0114(18) -0.0041(17) C3 0.025(2) 0.0167(18) 0.0246(19) 0.0014(15) 0.0057(16) 0.0007(15) C4 0.026(2) 0.0176(19) 0.027(2) 0.0002(15) 0.0065(17) -0.0014(16) C5 0.043(3) 0.022(2) 0.032(2) -0.0036(17) 0.010(2) 0.0004(18) C6 0.025(2) 0.0188(19) 0.0246(19) 0.0011(15) 0.0053(16) -0.0048(16) C7 0.023(2) 0.022(2) 0.029(2) -0.0056(16) 0.0040(17) -0.0009(16) C8 0.036(3) 0.025(2) 0.034(2) -0.0040(18) 0.000(2) -0.0011(18) C9 0.037(2) 0.021(2) 0.0224(19) 0.0052(15) 0.0059(17) 0.0040(17) C10 0.037(3) 0.021(2) 0.036(2) -0.0048(17) 0.004(2) 0.0052(18) C11 0.033(2) 0.0168(19) 0.0234(19) -0.0020(15) 0.0027(17) -0.0044(16) C12 0.037(3) 0.026(2) 0.030(2) -0.0012(17) 0.0076(19) -0.0037(18) C13 0.029(2) 0.035(2) 0.053(3) -0.006(2) 0.022(2) -0.0032(19) C14 0.044(3) 0.028(2) 0.036(2) -0.0003(18) 0.004(2) 0.009(2) C15 0.030(2) 0.023(2) 0.0220(19) 0.0003(15) 0.0075(17) -0.0012(16) C16 0.028(2) 0.024(2) 0.036(2) 0.0011(17) 0.0123(18) 0.0020(17) C17 0.026(2) 0.028(2) 0.040(2) 0.0004(18) 0.0024(19) -0.0030(18) C18 0.032(2) 0.028(2) 0.030(2) 0.0054(17) 0.0110(18) 0.0049(18) C19 0.030(2) 0.025(2) 0.030(2) -0.0024(17) 0.0016(18) 0.0029(17) C20 0.027(2) 0.023(2) 0.051(3) -0.0040(19) 0.001(2) 0.0020(18) C21 0.037(3) 0.031(2) 0.037(2) -0.0094(19) 0.019(2) -0.0059(19) C22 0.028(2) 0.030(2) 0.027(2) -0.0002(17) 0.0066(17) -0.0004(18) C23 0.026(2) 0.037(2) 0.033(2) 0.0033(18) 0.0109(19) 0.0036(18) C24 0.036(3) 0.046(3) 0.030(2) -0.002(2) 0.000(2) 0.005(2) C25 0.033(3) 0.035(2) 0.034(2) 0.0062(19) 0.002(2) -0.0049(19) C26 0.038(3) 0.056(3) 0.054(3) 0.002(3) 0.026(3) 0.007(2) C27 0.056(3) 0.042(3) 0.043(3) 0.002(2) -0.006(3) 0.017(3) C28 0.049(3) 0.052(3) 0.035(3) 0.001(2) -0.008(2) 0.013(3) C29 0.060(4) 0.086(5) 0.034(3) 0.019(3) 0.006(3) 0.007(3) C30 0.076(4) 0.097(5) 0.039(3) 0.017(3) 0.033(3) 0.006(4) C31 0.033(3) 0.035(3) 0.041(3) 0.003(2) -0.007(2) 0.003(2) C32 0.056(4) 0.053(4) 0.070(4) 0.013(3) 0.013(3) 0.012(3) C33 0.039(3) 0.068(4) 0.112(6) 0.009(4) 0.005(4) 0.009(3) Cl1 0.0312(6) 0.0223(5) 0.0338(5) -0.0021(4) 0.0112(4) 0.0001(4) Cl2 0.0369(6) 0.0469(7) 0.0375(6) -0.0086(5) 0.0109(5) -0.0097(5) N1 0.030(2) 0.0306(19) 0.0231(17) 0.0011(14) 0.0035(15) 0.0033(15) N2 0.0244(18) 0.0225(17) 0.0271(17) 0.0006(13) 0.0083(14) -0.0007(14) N3 0.0285(19) 0.0199(16) 0.0250(17) -0.0013(13) 0.0059(15) 0.0011(14) N4 0.036(2) 0.029(2) 0.0337(19) 0.0005(15) 0.0082(17) 0.0022(16) N5 0.0201(17) 0.0212(17) 0.0256(17) 0.0017(13) 0.0067(14) 0.0005(13) O1 0.040(2) 0.078(3) 0.077(3) -0.037(2) 0.011(2) -0.021(2) O2 0.077(3) 0.062(3) 0.078(3) -0.026(2) 0.033(3) 0.001(2) O3 0.065(3) 0.094(3) 0.078(3) -0.030(3) 0.043(2) -0.041(3) O4 0.164(6) 0.078(4) 0.064(3) 0.009(3) -0.022(4) 0.032(4) O5 0.055(2) 0.053(2) 0.0358(18) -0.0011(15) 0.0096(17) 0.0245(18) _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 Zn1 N3 2.042(3) . ? Zn1 N5 2.044(3) 3_575 ? Zn1 N1 2.092(4) . ? Zn1 Cl1 2.3223(11) . ? Zn1 N2 2.454(3) . ? C1 C9 1.503(6) . ? C1 C11 1.514(6) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C16 1.386(6) . ? C2 C11 1.401(6) . ? C2 H2 0.9300 . ? C3 N3 1.348(5) . ? C3 C21 1.382(6) . ? C3 C15 1.506(6) . ? C4 C6 1.394(6) . ? C4 C16 1.406(6) . ? C4 N2 1.445(5) . ? C5 C12 1.377(7) . ? C5 C18 1.396(6) . ? C5 H5 0.9300 . ? C6 C7 1.395(6) . ? C6 H6 0.9300 . ? C7 C11 1.389(6) . ? C7 H7 0.9300 . ? C8 C10 1.383(6) . ? C8 C18 1.404(6) . ? C8 H8 0.9300 . ? C9 C12 1.390(6) . ? C9 C10 1.395(6) . ? C10 H10 0.9300 . ? C12 H12 0.9300 . ? C13 C20 1.388(7) . ? C13 C21 1.398(7) . ? C13 H13 0.9300 . ? C14 N1 1.353(6) . ? C14 C27 1.374(7) . ? C14 H14 0.9300 . ? C15 N2 1.474(5) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16 0.9300 . ? C17 N2 1.477(6) . ? C17 C22 1.510(6) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 N4 1.390(6) . ? C19 N3 1.342(6) . ? C19 C20 1.374(6) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 N1 1.345(6) . ? C22 C24 1.387(6) . ? C23 N5 1.345(5) . ? C23 C26 1.379(6) . ? C23 H23 0.9300 . ? C24 C28 1.362(7) . ? C24 H24 0.9300 . ? C25 N5 1.339(6) . ? C25 C29 1.379(7) . ? C25 C31 1.519(6) . ? C26 C30 1.371(9) . ? C26 H26 0.9300 . ? C27 C28 1.380(8) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C29 C30 1.373(9) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 N4 1.444(6) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 O5 1.418(7) . ? C32 C33 1.437(8) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? Cl2 O3 1.405(4) . ? Cl2 O4 1.420(5) . ? Cl2 O1 1.434(4) . ? Cl2 O2 1.435(4) . ? N4 H4A 0.9000 . ? N4 H4B 0.9000 . ? N5 Zn1 2.044(3) 3_575 ? O5 H5A 0.8200 . ? 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 Zn1 N5 132.51(14) . 3_575 ? N3 Zn1 N1 115.87(14) . . ? N5 Zn1 N1 107.10(14) 3_575 . ? N3 Zn1 Cl1 97.56(10) . . ? N5 Zn1 Cl1 95.09(9) 3_575 . ? N1 Zn1 Cl1 98.51(10) . . ? N3 Zn1 N2 75.60(12) . . ? N5 Zn1 N2 98.36(12) 3_575 . ? N1 Zn1 N2 74.47(13) . . ? Cl1 Zn1 N2 166.18(8) . . ? C9 C1 C11 115.9(3) . . ? C9 C1 H1A 108.3 . . ? C11 C1 H1A 108.3 . . ? C9 C1 H1B 108.3 . . ? C11 C1 H1B 108.3 . . ? H1A C1 H1B 107.4 . . ? C16 C2 C11 122.3(4) . . ? C16 C2 H2 118.8 . . ? C11 C2 H2 118.8 . . ? N3 C3 C21 121.3(4) . . ? N3 C3 C15 117.2(3) . . ? C21 C3 C15 121.4(3) . . ? C6 C4 C16 118.3(4) . . ? C6 C4 N2 121.9(3) . . ? C16 C4 N2 119.7(4) . . ? C12 C5 C18 121.0(4) . . ? C12 C5 H5 119.5 . . ? C18 C5 H5 119.5 . . ? C4 C6 C7 120.6(4) . . ? C4 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C11 C7 C6 121.8(4) . . ? C11 C7 H7 119.1 . . ? C6 C7 H7 119.1 . . ? C10 C8 C18 119.9(4) . . ? C10 C8 H8 120.1 . . ? C18 C8 H8 120.1 . . ? C12 C9 C10 116.6(4) . . ? C12 C9 C1 122.0(4) . . ? C10 C9 C1 121.4(4) . . ? C8 C10 C9 122.6(4) . . ? C8 C10 H10 118.7 . . ? C9 C10 H10 118.7 . . ? C7 C11 C2 116.9(4) . . ? C7 C11 C1 123.4(4) . . ? C2 C11 C1 119.7(4) . . ? C5 C12 C9 122.0(4) . . ? C5 C12 H12 119.0 . . ? C9 C12 H12 119.0 . . ? C20 C13 C21 119.3(4) . . ? C20 C13 H13 120.3 . . ? C21 C13 H13 120.3 . . ? N1 C14 C27 122.4(5) . . ? N1 C14 H14 118.8 . . ? C27 C14 H14 118.8 . . ? N2 C15 C3 113.0(3) . . ? N2 C15 H15A 109.0 . . ? C3 C15 H15A 109.0 . . ? N2 C15 H15B 109.0 . . ? C3 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? C2 C16 C4 120.0(4) . . ? C2 C16 H16 120.0 . . ? C4 C16 H16 120.0 . . ? N2 C17 C22 112.0(3) . . ? N2 C17 H17A 109.2 . . ? C22 C17 H17A 109.2 . . ? N2 C17 H17B 109.2 . . ? C22 C17 H17B 109.2 . . ? H17A C17 H17B 107.9 . . ? N4 C18 C5 119.5(4) . . ? N4 C18 C8 122.6(4) . . ? C5 C18 C8 117.8(4) . . ? N3 C19 C20 123.1(4) . . ? N3 C19 H19 118.4 . . ? C20 C19 H19 118.4 . . ? C19 C20 C13 118.0(4) . . ? C19 C20 H20 121.0 . . ? C13 C20 H20 121.0 . . ? C3 C21 C13 119.1(4) . . ? C3 C21 H21 120.5 . . ? C13 C21 H21 120.5 . . ? N1 C22 C24 121.6(4) . . ? N1 C22 C17 118.0(4) . . ? C24 C22 C17 120.4(4) . . ? N5 C23 C26 122.2(4) . . ? N5 C23 H23 118.9 . . ? C26 C23 H23 118.9 . . ? C28 C24 C22 119.3(5) . . ? C28 C24 H24 120.3 . . ? C22 C24 H24 120.3 . . ? N5 C25 C29 121.0(5) . . ? N5 C25 C31 117.2(4) . . ? C29 C25 C31 121.7(5) . . ? C30 C26 C23 117.8(5) . . ? C30 C26 H26 121.1 . . ? C23 C26 H26 121.1 . . ? C14 C27 C28 118.5(5) . . ? C14 C27 H27 120.7 . . ? C28 C27 H27 120.7 . . ? C24 C28 C27 119.8(5) . . ? C24 C28 H28 120.1 . . ? C27 C28 H28 120.1 . . ? C30 C29 C25 119.0(5) . . ? C30 C29 H29 120.5 . . ? C25 C29 H29 120.5 . . ? C26 C30 C29 120.5(5) . . ? C26 C30 H30 119.7 . . ? C29 C30 H30 119.7 . . ? N4 C31 C25 110.7(4) . . ? N4 C31 H31A 109.5 . . ? C25 C31 H31A 109.5 . . ? N4 C31 H31B 109.5 . . ? C25 C31 H31B 109.5 . . ? H31A C31 H31B 108.1 . . ? O5 C32 C33 114.7(5) . . ? O5 C32 H32A 108.6 . . ? C33 C32 H32A 108.6 . . ? O5 C32 H32B 108.6 . . ? C33 C32 H32B 108.6 . . ? H32A C32 H32B 107.6 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O3 Cl2 O4 112.0(4) . . ? O3 Cl2 O1 108.5(3) . . ? O4 Cl2 O1 109.2(3) . . ? O3 Cl2 O2 110.2(3) . . ? O4 Cl2 O2 106.7(3) . . ? O1 Cl2 O2 110.3(3) . . ? C22 N1 C14 118.3(4) . . ? C22 N1 Zn1 120.9(3) . . ? C14 N1 Zn1 120.7(3) . . ? C4 N2 C15 115.2(3) . . ? C4 N2 C17 114.8(3) . . ? C15 N2 C17 109.8(3) . . ? C4 N2 Zn1 112.8(2) . . ? C15 N2 Zn1 98.2(2) . . ? C17 N2 Zn1 104.4(2) . . ? C19 N3 C3 119.1(4) . . ? C19 N3 Zn1 122.4(3) . . ? C3 N3 Zn1 117.9(3) . . ? C18 N4 C31 117.8(4) . . ? C18 N4 H4A 107.9 . . ? C31 N4 H4A 107.9 . . ? C18 N4 H4B 107.9 . . ? C31 N4 H4B 107.9 . . ? H4A N4 H4B 107.2 . . ? C25 N5 C23 119.5(4) . . ? C25 N5 Zn1 125.4(3) . 3_575 ? C23 N5 Zn1 114.2(3) . 3_575 ? C32 O5 H5A 109.5 . . ? 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 C16 C4 C6 C7 2.3(6) . . . . ? N2 C4 C6 C7 -172.6(4) . . . . ? C4 C6 C7 C11 -1.3(6) . . . . ? C11 C1 C9 C12 106.5(5) . . . . ? C11 C1 C9 C10 -71.1(5) . . . . ? C18 C8 C10 C9 1.0(7) . . . . ? C12 C9 C10 C8 -1.9(6) . . . . ? C1 C9 C10 C8 175.8(4) . . . . ? C6 C7 C11 C2 -0.1(6) . . . . ? C6 C7 C11 C1 179.4(4) . . . . ? C16 C2 C11 C7 0.5(6) . . . . ? C16 C2 C11 C1 -179.0(4) . . . . ? C9 C1 C11 C7 -11.3(6) . . . . ? C9 C1 C11 C2 168.2(4) . . . . ? C18 C5 C12 C9 1.5(7) . . . . ? C10 C9 C12 C5 0.7(6) . . . . ? C1 C9 C12 C5 -177.0(4) . . . . ? N3 C3 C15 N2 28.2(5) . . . . ? C21 C3 C15 N2 -154.3(4) . . . . ? C11 C2 C16 C4 0.5(6) . . . . ? C6 C4 C16 C2 -1.9(6) . . . . ? N2 C4 C16 C2 173.2(4) . . . . ? C12 C5 C18 N4 178.3(4) . . . . ? C12 C5 C18 C8 -2.4(6) . . . . ? C10 C8 C18 N4 -179.5(4) . . . . ? C10 C8 C18 C5 1.2(6) . . . . ? N3 C19 C20 C13 -2.8(7) . . . . ? C21 C13 C20 C19 2.8(7) . . . . ? N3 C3 C21 C13 -2.1(7) . . . . ? C15 C3 C21 C13 -179.5(4) . . . . ? C20 C13 C21 C3 -0.5(7) . . . . ? N2 C17 C22 N1 26.9(5) . . . . ? N2 C17 C22 C24 -153.8(4) . . . . ? N1 C22 C24 C28 1.2(7) . . . . ? C17 C22 C24 C28 -178.1(4) . . . . ? N5 C23 C26 C30 0.2(8) . . . . ? N1 C14 C27 C28 0.9(8) . . . . ? C22 C24 C28 C27 -0.3(8) . . . . ? C14 C27 C28 C24 -0.6(8) . . . . ? N5 C25 C29 C30 -0.8(9) . . . . ? C31 C25 C29 C30 -178.6(6) . . . . ? C23 C26 C30 C29 -0.5(10) . . . . ? C25 C29 C30 C26 0.8(11) . . . . ? N5 C25 C31 N4 84.2(5) . . . . ? C29 C25 C31 N4 -97.9(6) . . . . ? C24 C22 N1 C14 -1.0(6) . . . . ? C17 C22 N1 C14 178.3(4) . . . . ? C24 C22 N1 Zn1 179.0(3) . . . . ? C17 C22 N1 Zn1 -1.7(5) . . . . ? C27 C14 N1 C22 0.0(7) . . . . ? C27 C14 N1 Zn1 179.9(4) . . . . ? N3 Zn1 N1 C22 -78.5(3) . . . . ? N5 Zn1 N1 C22 80.8(3) 3_575 . . . ? Cl1 Zn1 N1 C22 178.8(3) . . . . ? N2 Zn1 N1 C22 -13.4(3) . . . . ? N3 Zn1 N1 C14 101.6(3) . . . . ? N5 Zn1 N1 C14 -99.2(3) 3_575 . . . ? Cl1 Zn1 N1 C14 -1.2(3) . . . . ? N2 Zn1 N1 C14 166.6(3) . . . . ? C6 C4 N2 C15 -11.2(5) . . . . ? C16 C4 N2 C15 174.0(4) . . . . ? C6 C4 N2 C17 -140.2(4) . . . . ? C16 C4 N2 C17 45.0(5) . . . . ? C6 C4 N2 Zn1 100.4(4) . . . . ? C16 C4 N2 Zn1 -74.5(4) . . . . ? C3 C15 N2 C4 79.0(4) . . . . ? C3 C15 N2 C17 -149.6(3) . . . . ? C3 C15 N2 Zn1 -41.0(3) . . . . ? C22 C17 N2 C4 -157.2(3) . . . . ? C22 C17 N2 C15 71.2(4) . . . . ? C22 C17 N2 Zn1 -33.2(4) . . . . ? N3 Zn1 N2 C4 -87.0(3) . . . . ? N5 Zn1 N2 C4 44.8(3) 3_575 . . . ? N1 Zn1 N2 C4 150.3(3) . . . . ? Cl1 Zn1 N2 C4 -148.7(3) . . . . ? N3 Zn1 N2 C15 34.7(2) . . . . ? N5 Zn1 N2 C15 166.6(2) 3_575 . . . ? N1 Zn1 N2 C15 -87.9(2) . . . . ? Cl1 Zn1 N2 C15 -27.0(5) . . . . ? N3 Zn1 N2 C17 147.6(3) . . . . ? N5 Zn1 N2 C17 -80.5(3) 3_575 . . . ? N1 Zn1 N2 C17 25.0(2) . . . . ? Cl1 Zn1 N2 C17 86.0(4) . . . . ? C20 C19 N3 C3 0.3(6) . . . . ? C20 C19 N3 Zn1 170.9(3) . . . . ? C21 C3 N3 C19 2.2(6) . . . . ? C15 C3 N3 C19 179.7(4) . . . . ? C21 C3 N3 Zn1 -168.8(3) . . . . ? C15 C3 N3 Zn1 8.8(4) . . . . ? N5 Zn1 N3 C19 76.3(4) 3_575 . . . ? N1 Zn1 N3 C19 -131.1(3) . . . . ? Cl1 Zn1 N3 C19 -27.8(3) . . . . ? N2 Zn1 N3 C19 164.5(3) . . . . ? N5 Zn1 N3 C3 -113.0(3) 3_575 . . . ? N1 Zn1 N3 C3 39.6(3) . . . . ? Cl1 Zn1 N3 C3 142.9(3) . . . . ? N2 Zn1 N3 C3 -24.8(3) . . . . ? C5 C18 N4 C31 -163.7(4) . . . . ? C8 C18 N4 C31 17.0(6) . . . . ? C25 C31 N4 C18 174.7(4) . . . . ? C29 C25 N5 C23 0.5(7) . . . . ? C31 C25 N5 C23 178.4(4) . . . . ? C29 C25 N5 Zn1 168.8(4) . . . 3_575 ? C31 C25 N5 Zn1 -13.3(6) . . . 3_575 ? C26 C23 N5 C25 -0.2(7) . . . . ? C26 C23 N5 Zn1 -169.7(4) . . . 3_575 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 3.167 _refine_diff_density_min -1.016 _refine_diff_density_rms 0.103 # Attachment '- complex 2.cif' data_shelx _database_code_depnum_ccdc_archive 'CCDC 861139' #TrackingRef '- complex 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H40 Br4 N8 Zn2' _chemical_formula_sum 'C41 H40 Br4 N8 Zn2' _chemical_formula_weight 1095.19 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.5897(18) _cell_length_b 18.367(4) _cell_length_c 27.736(6) _cell_angle_alpha 90.00 _cell_angle_beta 91.810(4) _cell_angle_gamma 90.00 _cell_volume 4373.6(16) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 13993 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 27.2 _exptl_crystal_description needle-shaped _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.663 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2168 _exptl_absorpt_coefficient_mu 4.790 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.439 _exptl_absorpt_correction_T_max 0.59 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(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 32216 _diffrn_reflns_av_R_equivalents 0.0467 _diffrn_reflns_av_sigmaI/netI 0.0443 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 25.01 _reflns_number_total 7699 _reflns_number_gt 7008 _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^)+(0.0372P)^2^+12.5110P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment CONSTR _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7665 _refine_ls_number_parameters 498 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0551 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.1089 _refine_ls_wR_factor_gt 0.1056 _refine_ls_goodness_of_fit_ref 1.130 _refine_ls_restrained_S_all 1.130 _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 Zn1 Zn 0.99796(6) 0.16660(3) 0.34950(2) 0.02231(15) Uani 1 1 d . . . Zn2 Zn 0.39495(7) 0.28631(3) 0.10856(2) 0.02539(15) Uani 1 1 d . . . Br1 Br 0.92968(6) 0.10352(3) 0.27502(2) 0.03222(15) Uani 1 1 d . . . Br2 Br 1.10437(6) 0.08334(3) 0.411237(19) 0.02602(13) Uani 1 1 d . . . Br3 Br 0.50295(7) 0.18453(3) 0.15196(2) 0.04216(17) Uani 1 1 d . . . Br4 Br 0.26566(6) 0.26465(3) 0.030695(19) 0.03520(16) Uani 1 1 d . . . N1 N 0.7756(5) 0.1757(2) 0.37866(15) 0.0212(9) Uani 1 1 d . . . N2 N 1.2014(5) 0.2215(2) 0.32949(15) 0.0223(9) Uani 1 1 d . . . N3 N 0.9924(4) 0.2819(2) 0.39161(15) 0.0218(9) Uani 1 1 d . . . N4 N 0.1897(5) 0.3052(2) 0.14591(15) 0.0268(10) Uani 1 1 d . . . N5 N 0.6040(5) 0.3262(3) 0.08034(16) 0.0300(10) Uani 1 1 d . . . N6 N 0.3767(5) 0.4156(2) 0.11491(15) 0.0245(9) Uani 1 1 d . . . C1 C 0.6510(6) 0.1356(3) 0.36330(19) 0.0248(11) Uani 1 1 d . . . H1 H 0.6578 0.1079 0.3354 0.030 Uiso 1 1 calc R . . C2 C 0.5154(6) 0.1350(3) 0.38803(19) 0.0277(12) Uani 1 1 d . . . H2 H 0.4312 0.1072 0.3769 0.033 Uiso 1 1 calc R . . C3 C 0.5045(6) 0.1758(3) 0.42956(19) 0.0281(12) Uani 1 1 d . . . H3 H 0.4136 0.1756 0.4469 0.034 Uiso 1 1 calc R . . C4 C 0.6308(6) 0.2171(3) 0.44482(19) 0.0257(11) Uani 1 1 d . . . H4 H 0.6254 0.2458 0.4724 0.031 Uiso 1 1 calc R . . C5 C 0.7657(6) 0.2156(3) 0.41886(18) 0.0229(11) Uani 1 1 d . . . C6 C 0.9121(6) 0.2557(3) 0.43414(18) 0.0232(11) Uani 1 1 d . . . H6A H 0.8860 0.2966 0.4545 0.028 Uiso 1 1 calc R . . H6B H 0.9804 0.2235 0.4527 0.028 Uiso 1 1 calc R . . C7 C 1.1601(5) 0.2960(3) 0.40039(18) 0.0234(11) Uani 1 1 d . . . H7A H 1.1967 0.2680 0.4281 0.028 Uiso 1 1 calc R . . H7B H 1.1752 0.3472 0.4078 0.028 Uiso 1 1 calc R . . C8 C 1.2553(5) 0.2764(3) 0.35752(18) 0.0219(11) Uani 1 1 d . . . C9 C 1.3950(6) 0.3115(3) 0.34835(19) 0.0265(12) Uani 1 1 d . . . H9 H 1.4310 0.3489 0.3684 0.032 Uiso 1 1 calc R . . C10 C 1.4790(6) 0.2906(3) 0.3095(2) 0.0298(12) Uani 1 1 d . . . H10 H 1.5717 0.3139 0.3026 0.036 Uiso 1 1 calc R . . C11 C 1.4238(6) 0.2343(3) 0.2807(2) 0.0327(13) Uani 1 1 d . . . H11 H 1.4794 0.2188 0.2543 0.039 Uiso 1 1 calc R . . C12 C 1.2853(6) 0.2014(3) 0.29157(19) 0.0272(12) Uani 1 1 d . . . H12 H 1.2483 0.1638 0.2719 0.033 Uiso 1 1 calc R . . C13 C 0.9136(5) 0.3415(3) 0.36659(17) 0.0198(10) Uani 1 1 d . . . C14 C 0.9611(6) 0.3634(3) 0.32157(19) 0.0313(13) Uani 1 1 d . . . H14 H 1.0418 0.3384 0.3073 0.038 Uiso 1 1 calc R . . C15 C 0.8917(6) 0.4217(3) 0.29714(19) 0.0329(13) Uani 1 1 d . . . H15 H 0.9284 0.4360 0.2674 0.039 Uiso 1 1 calc R . . C16 C 0.7663(6) 0.4589(3) 0.31719(18) 0.0225(11) Uani 1 1 d . . . C17 C 0.7181(6) 0.4365(3) 0.36138(18) 0.0259(11) Uani 1 1 d . . . H17 H 0.6349 0.4603 0.3751 0.031 Uiso 1 1 calc R . . C18 C 0.7902(6) 0.3790(3) 0.38644(19) 0.0266(11) Uani 1 1 d . . . H18 H 0.7554 0.3657 0.4166 0.032 Uiso 1 1 calc R . . C19 C 0.6873(6) 0.5206(3) 0.28961(19) 0.0288(12) Uani 1 1 d . . . H19A H 0.6131 0.5440 0.3102 0.035 Uiso 1 1 calc R . . H19B H 0.7649 0.5565 0.2814 0.035 Uiso 1 1 calc R . . C20 C 0.6034(6) 0.4952(3) 0.24399(18) 0.0228(11) Uani 1 1 d . . . C21 C 0.6758(6) 0.4972(3) 0.20008(19) 0.0269(12) Uani 1 1 d . . . H21 H 0.7758 0.5163 0.1988 0.032 Uiso 1 1 calc R . . C22 C 0.6039(6) 0.4717(3) 0.15811(19) 0.0271(12) Uani 1 1 d . . . H22 H 0.6561 0.4738 0.1293 0.033 Uiso 1 1 calc R . . C23 C 0.4534(6) 0.4428(3) 0.15865(18) 0.0232(11) Uani 1 1 d . . . C24 C 0.3802(6) 0.4413(3) 0.2026(2) 0.0308(12) Uani 1 1 d . . . H24 H 0.2798 0.4225 0.2040 0.037 Uiso 1 1 calc R . . C25 C 0.4536(6) 0.4670(3) 0.2442(2) 0.0302(12) Uani 1 1 d . . . H25 H 0.4014 0.4653 0.2731 0.036 Uiso 1 1 calc R . . C26 C 0.1137(7) 0.2531(3) 0.1698(2) 0.0365(14) Uani 1 1 d . . . H26 H 0.1615 0.2080 0.1742 0.044 Uiso 1 1 calc R . . C27 C -0.0329(7) 0.2637(3) 0.1881(2) 0.0384(14) Uani 1 1 d . . . H27 H -0.0828 0.2265 0.2043 0.046 Uiso 1 1 calc R . . C28 C -0.1029(7) 0.3305(3) 0.1817(2) 0.0368(14) Uani 1 1 d . . . H28 H -0.2018 0.3388 0.1932 0.044 Uiso 1 1 calc R . . C29 C -0.0260(6) 0.3845(3) 0.15836(19) 0.0319(13) Uani 1 1 d . . . H29 H -0.0710 0.4302 0.1544 0.038 Uiso 1 1 calc R . . C30 C 0.1198(6) 0.3701(3) 0.14072(18) 0.0260(11) Uani 1 1 d . . . C31 C 0.2060(6) 0.4280(3) 0.1134(2) 0.0282(12) Uani 1 1 d . . . H31A H 0.1682 0.4285 0.0801 0.034 Uiso 1 1 calc R . . H31B H 0.1843 0.4753 0.1273 0.034 Uiso 1 1 calc R . . C32 C 0.4522(6) 0.4368(3) 0.06966(18) 0.0287(12) Uani 1 1 d . . . H32A H 0.4769 0.4883 0.0709 0.034 Uiso 1 1 calc R . . H32B H 0.3796 0.4290 0.0427 0.034 Uiso 1 1 calc R . . C33 C 0.5984(6) 0.3944(3) 0.06148(19) 0.0287(12) Uani 1 1 d . . . C34 C 0.7215(7) 0.4215(3) 0.0358(2) 0.0378(14) Uani 1 1 d . . . H34 H 0.7169 0.4682 0.0229 0.045 Uiso 1 1 calc R . . C35 C 0.8517(7) 0.3784(4) 0.0294(2) 0.0426(16) Uani 1 1 d . . . H35 H 0.9350 0.3955 0.0121 0.051 Uiso 1 1 calc R . . C36 C 0.8556(7) 0.3090(4) 0.0495(2) 0.0438(16) Uani 1 1 d . . . H36 H 0.9427 0.2795 0.0463 0.053 Uiso 1 1 calc R . . C37 C 0.7307(6) 0.2848(3) 0.0738(2) 0.0339(13) Uani 1 1 d . . . H37 H 0.7329 0.2379 0.0864 0.041 Uiso 1 1 calc R . . C38 C 0.8805(11) 0.0704(5) 0.1318(4) 0.090(3) Uani 1 1 d . . . H38A H 0.9165 0.0973 0.1047 0.134 Uiso 1 1 calc R . . H38B H 0.9669 0.0460 0.1476 0.134 Uiso 1 1 calc R . . H38C H 0.8338 0.1033 0.1541 0.134 Uiso 1 1 calc R . . C39 C 0.7697(10) 0.0187(4) 0.1159(3) 0.062(2) Uani 1 1 d . . . N7 N 0.6779(9) -0.0232(4) 0.1011(3) 0.084(2) Uani 1 1 d . . . C40 C 0.3954(16) 0.0756(5) 0.0327(4) 0.121(5) Uani 1 1 d . . . H40A H 0.4060 0.0355 0.0547 0.181 Uiso 1 1 calc R . . H40B H 0.3412 0.0599 0.0038 0.181 Uiso 1 1 calc R . . H40C H 0.3377 0.1140 0.0474 0.181 Uiso 1 1 calc R . . C41 C 0.5554(17) 0.1034(4) 0.0204(4) 0.094(4) Uani 1 1 d . . . N8 N 0.6843(18) 0.1236(5) 0.0119(3) 0.143(5) 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 Zn1 0.0194(3) 0.0246(3) 0.0228(3) 0.0000(2) -0.0020(2) -0.0002(2) Zn2 0.0257(3) 0.0277(3) 0.0225(3) 0.0012(3) -0.0025(2) 0.0010(2) Br1 0.0285(3) 0.0397(3) 0.0281(3) -0.0073(2) -0.0041(2) -0.0029(2) Br2 0.0221(3) 0.0277(3) 0.0282(3) 0.0045(2) -0.0012(2) 0.0023(2) Br3 0.0500(4) 0.0409(3) 0.0358(3) 0.0101(3) 0.0057(3) 0.0162(3) Br4 0.0262(3) 0.0558(4) 0.0233(3) -0.0057(3) -0.0029(2) -0.0013(3) N1 0.020(2) 0.022(2) 0.022(2) 0.0015(18) -0.0011(17) 0.0037(17) N2 0.024(2) 0.021(2) 0.022(2) 0.0017(18) -0.0024(18) 0.0005(17) N3 0.015(2) 0.027(2) 0.023(2) 0.0046(18) -0.0021(17) -0.0013(17) N4 0.032(2) 0.029(2) 0.019(2) -0.0008(19) -0.0018(19) -0.004(2) N5 0.019(2) 0.046(3) 0.024(2) -0.007(2) -0.0005(18) -0.003(2) N6 0.020(2) 0.030(2) 0.024(2) 0.0026(19) -0.0031(18) 0.0010(18) C1 0.021(3) 0.026(3) 0.027(3) -0.002(2) -0.002(2) -0.002(2) C2 0.022(3) 0.027(3) 0.034(3) 0.005(2) -0.008(2) -0.002(2) C3 0.022(3) 0.033(3) 0.029(3) 0.011(2) 0.001(2) 0.001(2) C4 0.024(3) 0.029(3) 0.023(3) 0.002(2) 0.000(2) 0.007(2) C5 0.020(3) 0.025(3) 0.023(3) 0.008(2) -0.006(2) 0.002(2) C6 0.021(3) 0.030(3) 0.019(3) 0.002(2) -0.001(2) 0.002(2) C7 0.022(3) 0.028(3) 0.020(3) -0.001(2) -0.004(2) -0.001(2) C8 0.018(2) 0.026(3) 0.021(3) 0.005(2) -0.004(2) 0.001(2) C9 0.023(3) 0.028(3) 0.028(3) 0.001(2) -0.002(2) -0.002(2) C10 0.023(3) 0.037(3) 0.030(3) 0.008(3) 0.002(2) -0.006(2) C11 0.030(3) 0.039(3) 0.029(3) 0.004(3) 0.008(2) 0.002(3) C12 0.027(3) 0.032(3) 0.023(3) -0.001(2) 0.001(2) 0.003(2) C13 0.019(2) 0.022(2) 0.018(2) 0.000(2) -0.003(2) -0.002(2) C14 0.024(3) 0.044(3) 0.026(3) 0.002(3) 0.000(2) 0.011(2) C15 0.033(3) 0.044(3) 0.022(3) 0.010(3) 0.001(2) 0.004(3) C16 0.023(3) 0.023(2) 0.021(3) -0.001(2) -0.004(2) -0.001(2) C17 0.026(3) 0.027(3) 0.024(3) -0.004(2) 0.004(2) 0.003(2) C18 0.030(3) 0.027(3) 0.023(3) 0.001(2) 0.004(2) 0.001(2) C19 0.031(3) 0.027(3) 0.028(3) 0.000(2) -0.002(2) 0.000(2) C20 0.024(3) 0.019(2) 0.025(3) 0.002(2) -0.004(2) 0.006(2) C21 0.022(3) 0.026(3) 0.033(3) 0.002(2) -0.005(2) 0.000(2) C22 0.029(3) 0.026(3) 0.026(3) 0.000(2) 0.002(2) 0.000(2) C23 0.025(3) 0.021(2) 0.024(3) -0.002(2) -0.003(2) 0.006(2) C24 0.019(3) 0.042(3) 0.032(3) 0.001(3) 0.001(2) -0.004(2) C25 0.028(3) 0.038(3) 0.025(3) -0.003(2) 0.001(2) 0.001(2) C26 0.041(3) 0.042(3) 0.027(3) 0.002(3) 0.002(3) -0.002(3) C27 0.041(3) 0.045(3) 0.029(3) 0.003(3) 0.002(3) -0.014(3) C28 0.026(3) 0.054(4) 0.031(3) -0.002(3) 0.001(2) -0.003(3) C29 0.024(3) 0.045(3) 0.027(3) -0.001(3) -0.003(2) 0.002(2) C30 0.023(3) 0.035(3) 0.019(3) -0.006(2) -0.005(2) 0.004(2) C31 0.019(3) 0.031(3) 0.034(3) 0.001(2) -0.007(2) 0.004(2) C32 0.034(3) 0.031(3) 0.021(3) 0.004(2) -0.004(2) -0.001(2) C33 0.023(3) 0.038(3) 0.025(3) -0.004(2) 0.000(2) -0.007(2) C34 0.046(4) 0.041(3) 0.026(3) -0.011(3) 0.002(3) -0.016(3) C35 0.023(3) 0.074(5) 0.031(3) -0.023(3) 0.006(2) -0.018(3) C36 0.025(3) 0.069(5) 0.038(4) -0.024(3) -0.004(3) 0.000(3) C37 0.024(3) 0.049(3) 0.028(3) -0.009(3) -0.007(2) 0.005(3) C38 0.083(6) 0.075(6) 0.109(8) -0.008(6) -0.030(6) 0.015(5) C39 0.066(5) 0.046(4) 0.073(6) 0.010(4) 0.015(4) 0.016(4) N7 0.073(5) 0.048(4) 0.133(7) 0.017(4) 0.020(5) -0.003(4) C40 0.218(15) 0.044(5) 0.101(9) -0.007(5) 0.015(9) 0.013(7) C41 0.182(13) 0.027(4) 0.074(7) 0.010(4) 0.038(8) 0.011(6) N8 0.292(16) 0.052(5) 0.089(7) 0.008(5) 0.087(9) -0.014(7) _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 Zn1 N1 2.104(4) . ? Zn1 N2 2.107(4) . ? Zn1 N3 2.420(4) . ? Zn1 Br1 2.4244(9) . ? Zn1 Br2 2.4510(8) . ? Zn2 N4 2.102(4) . ? Zn2 N5 2.112(4) . ? Zn2 N6 2.387(4) . ? Zn2 Br3 2.3946(9) . ? Zn2 Br4 2.4299(9) . ? N1 C5 1.339(6) . ? N1 C1 1.357(6) . ? N2 C12 1.345(6) . ? N2 C8 1.346(6) . ? N3 C13 1.452(6) . ? N3 C6 1.466(6) . ? N3 C7 1.476(6) . ? N4 C30 1.340(7) . ? N4 C26 1.345(7) . ? N5 C37 1.345(7) . ? N5 C33 1.358(7) . ? N6 C23 1.451(6) . ? N6 C32 1.483(7) . ? N6 C31 1.484(6) . ? C1 C2 1.371(7) . ? C2 C3 1.381(8) . ? C3 C4 1.380(7) . ? C4 C5 1.383(7) . ? C5 C6 1.507(7) . ? C7 C8 1.508(7) . ? C8 C9 1.393(7) . ? C9 C10 1.372(7) . ? C10 C11 1.381(8) . ? C11 C12 1.375(7) . ? C13 C14 1.386(7) . ? C13 C18 1.392(7) . ? C14 C15 1.391(7) . ? C15 C16 1.406(7) . ? C16 C17 1.369(7) . ? C16 C19 1.515(7) . ? C17 C18 1.398(7) . ? C19 C20 1.510(7) . ? C20 C21 1.385(7) . ? C20 C25 1.388(7) . ? C21 C22 1.382(7) . ? C22 C23 1.398(7) . ? C23 C24 1.389(7) . ? C24 C25 1.381(7) . ? C26 C27 1.387(8) . ? C27 C28 1.375(8) . ? C28 C29 1.367(8) . ? C29 C30 1.385(7) . ? C30 C31 1.513(7) . ? C32 C33 1.501(7) . ? C33 C34 1.387(8) . ? C34 C35 1.386(9) . ? C35 C36 1.390(9) . ? C36 C37 1.360(8) . ? C38 C39 1.405(12) . ? C39 N7 1.168(10) . ? C40 C41 1.515(16) . ? C41 N8 1.198(16) . ? 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 Zn1 N2 146.46(16) . . ? N1 Zn1 N3 73.32(14) . . ? N2 Zn1 N3 74.77(15) . . ? N1 Zn1 Br1 99.64(11) . . ? N2 Zn1 Br1 100.64(11) . . ? N3 Zn1 Br1 145.24(10) . . ? N1 Zn1 Br2 95.97(11) . . ? N2 Zn1 Br2 100.87(11) . . ? N3 Zn1 Br2 102.80(10) . . ? Br1 Zn1 Br2 111.84(3) . . ? N4 Zn2 N5 149.47(17) . . ? N4 Zn2 N6 75.02(15) . . ? N5 Zn2 N6 74.96(16) . . ? N4 Zn2 Br3 101.47(12) . . ? N5 Zn2 Br3 97.87(13) . . ? N6 Zn2 Br3 139.91(10) . . ? N4 Zn2 Br4 95.63(12) . . ? N5 Zn2 Br4 95.59(12) . . ? N6 Zn2 Br4 101.49(10) . . ? Br3 Zn2 Br4 118.55(3) . . ? C5 N1 C1 119.2(4) . . ? C5 N1 Zn1 116.5(3) . . ? C1 N1 Zn1 123.5(3) . . ? C12 N2 C8 118.3(4) . . ? C12 N2 Zn1 123.0(3) . . ? C8 N2 Zn1 118.6(3) . . ? C13 N3 C6 114.1(4) . . ? C13 N3 C7 112.6(4) . . ? C6 N3 C7 114.0(4) . . ? C13 N3 Zn1 116.4(3) . . ? C6 N3 Zn1 96.8(3) . . ? C7 N3 Zn1 101.5(3) . . ? C30 N4 C26 117.6(5) . . ? C30 N4 Zn2 118.3(3) . . ? C26 N4 Zn2 123.6(4) . . ? C37 N5 C33 119.2(5) . . ? C37 N5 Zn2 123.7(4) . . ? C33 N5 Zn2 116.3(3) . . ? C23 N6 C32 114.7(4) . . ? C23 N6 C31 113.1(4) . . ? C32 N6 C31 113.2(4) . . ? C23 N6 Zn2 112.0(3) . . ? C32 N6 Zn2 99.6(3) . . ? C31 N6 Zn2 102.6(3) . . ? N1 C1 C2 121.5(5) . . ? C1 C2 C3 119.6(5) . . ? C4 C3 C2 118.8(5) . . ? C3 C4 C5 119.5(5) . . ? N1 C5 C4 121.4(5) . . ? N1 C5 C6 115.3(4) . . ? C4 C5 C6 123.3(5) . . ? N3 C6 C5 110.1(4) . . ? N3 C7 C8 112.2(4) . . ? N2 C8 C9 121.6(5) . . ? N2 C8 C7 116.7(4) . . ? C9 C8 C7 121.6(5) . . ? C10 C9 C8 119.4(5) . . ? C9 C10 C11 119.0(5) . . ? C12 C11 C10 119.0(5) . . ? N2 C12 C11 122.7(5) . . ? C14 C13 C18 117.6(5) . . ? C14 C13 N3 120.2(4) . . ? C18 C13 N3 122.2(4) . . ? C13 C14 C15 121.9(5) . . ? C14 C15 C16 120.3(5) . . ? C17 C16 C15 117.7(5) . . ? C17 C16 C19 122.2(5) . . ? C15 C16 C19 120.1(5) . . ? C16 C17 C18 122.0(5) . . ? C13 C18 C17 120.5(5) . . ? C20 C19 C16 112.8(4) . . ? C21 C20 C25 117.1(5) . . ? C21 C20 C19 120.9(5) . . ? C25 C20 C19 122.0(5) . . ? C22 C21 C20 122.0(5) . . ? C21 C22 C23 120.6(5) . . ? C24 C23 C22 117.5(5) . . ? C24 C23 N6 121.3(4) . . ? C22 C23 N6 121.2(5) . . ? C25 C24 C23 121.3(5) . . ? C24 C25 C20 121.5(5) . . ? N4 C26 C27 122.7(6) . . ? C28 C27 C26 118.5(6) . . ? C29 C28 C27 119.6(5) . . ? C28 C29 C30 119.0(5) . . ? N4 C30 C29 122.6(5) . . ? N4 C30 C31 117.1(4) . . ? C29 C30 C31 120.3(5) . . ? N6 C31 C30 112.1(4) . . ? N6 C32 C33 112.5(4) . . ? N5 C33 C34 120.7(5) . . ? N5 C33 C32 116.1(5) . . ? C34 C33 C32 123.2(5) . . ? C35 C34 C33 119.4(6) . . ? C34 C35 C36 118.9(6) . . ? C37 C36 C35 119.2(6) . . ? N5 C37 C36 122.5(6) . . ? N7 C39 C38 177.7(10) . . ? N8 C41 C40 177.5(12) . . ? 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 N2 Zn1 N1 C5 -46.7(5) . . . . ? N3 Zn1 N1 C5 -28.2(3) . . . . ? Br1 Zn1 N1 C5 -173.2(3) . . . . ? Br2 Zn1 N1 C5 73.4(3) . . . . ? N2 Zn1 N1 C1 143.3(4) . . . . ? N3 Zn1 N1 C1 161.7(4) . . . . ? Br1 Zn1 N1 C1 16.7(4) . . . . ? Br2 Zn1 N1 C1 -96.7(4) . . . . ? N1 Zn1 N2 C12 -146.0(4) . . . . ? N3 Zn1 N2 C12 -164.3(4) . . . . ? Br1 Zn1 N2 C12 -19.7(4) . . . . ? Br2 Zn1 N2 C12 95.3(4) . . . . ? N1 Zn1 N2 C8 38.2(5) . . . . ? N3 Zn1 N2 C8 19.8(3) . . . . ? Br1 Zn1 N2 C8 164.5(3) . . . . ? Br2 Zn1 N2 C8 -80.6(3) . . . . ? N1 Zn1 N3 C13 -79.0(3) . . . . ? N2 Zn1 N3 C13 90.6(3) . . . . ? Br1 Zn1 N3 C13 3.8(4) . . . . ? Br2 Zn1 N3 C13 -171.5(3) . . . . ? N1 Zn1 N3 C6 42.2(3) . . . . ? N2 Zn1 N3 C6 -148.3(3) . . . . ? Br1 Zn1 N3 C6 125.0(2) . . . . ? Br2 Zn1 N3 C6 -50.3(3) . . . . ? N1 Zn1 N3 C7 158.4(3) . . . . ? N2 Zn1 N3 C7 -32.1(3) . . . . ? Br1 Zn1 N3 C7 -118.8(3) . . . . ? Br2 Zn1 N3 C7 65.9(3) . . . . ? N5 Zn2 N4 C30 33.4(5) . . . . ? N6 Zn2 N4 C30 22.7(3) . . . . ? Br3 Zn2 N4 C30 161.6(3) . . . . ? Br4 Zn2 N4 C30 -77.7(4) . . . . ? N5 Zn2 N4 C26 -155.3(4) . . . . ? N6 Zn2 N4 C26 -166.0(4) . . . . ? Br3 Zn2 N4 C26 -27.1(4) . . . . ? Br4 Zn2 N4 C26 93.6(4) . . . . ? N4 Zn2 N5 C37 153.2(4) . . . . ? N6 Zn2 N5 C37 163.9(4) . . . . ? Br3 Zn2 N5 C37 24.2(4) . . . . ? Br4 Zn2 N5 C37 -95.7(4) . . . . ? N4 Zn2 N5 C33 -37.0(5) . . . . ? N6 Zn2 N5 C33 -26.3(4) . . . . ? Br3 Zn2 N5 C33 -166.0(3) . . . . ? Br4 Zn2 N5 C33 74.1(4) . . . . ? N4 Zn2 N6 C23 89.6(3) . . . . ? N5 Zn2 N6 C23 -84.8(3) . . . . ? Br3 Zn2 N6 C23 -0.5(4) . . . . ? Br4 Zn2 N6 C23 -177.6(3) . . . . ? N4 Zn2 N6 C32 -148.6(3) . . . . ? N5 Zn2 N6 C32 37.0(3) . . . . ? Br3 Zn2 N6 C32 121.3(3) . . . . ? Br4 Zn2 N6 C32 -55.8(3) . . . . ? N4 Zn2 N6 C31 -32.0(3) . . . . ? N5 Zn2 N6 C31 153.6(3) . . . . ? Br3 Zn2 N6 C31 -122.1(3) . . . . ? Br4 Zn2 N6 C31 60.8(3) . . . . ? C5 N1 C1 C2 -0.1(7) . . . . ? Zn1 N1 C1 C2 169.7(4) . . . . ? N1 C1 C2 C3 -0.1(8) . . . . ? C1 C2 C3 C4 0.7(7) . . . . ? C2 C3 C4 C5 -1.2(7) . . . . ? C1 N1 C5 C4 -0.4(7) . . . . ? Zn1 N1 C5 C4 -170.9(4) . . . . ? C1 N1 C5 C6 177.5(4) . . . . ? Zn1 N1 C5 C6 7.0(5) . . . . ? C3 C4 C5 N1 1.1(7) . . . . ? C3 C4 C5 C6 -176.7(5) . . . . ? C13 N3 C6 C5 71.0(5) . . . . ? C7 N3 C6 C5 -157.7(4) . . . . ? Zn1 N3 C6 C5 -51.9(4) . . . . ? N1 C5 C6 N3 36.7(6) . . . . ? C4 C5 C6 N3 -145.4(5) . . . . ? C13 N3 C7 C8 -84.3(5) . . . . ? C6 N3 C7 C8 143.8(4) . . . . ? Zn1 N3 C7 C8 41.0(4) . . . . ? C12 N2 C8 C9 -0.7(7) . . . . ? Zn1 N2 C8 C9 175.4(4) . . . . ? C12 N2 C8 C7 -178.5(4) . . . . ? Zn1 N2 C8 C7 -2.4(5) . . . . ? N3 C7 C8 N2 -30.4(6) . . . . ? N3 C7 C8 C9 151.8(4) . . . . ? N2 C8 C9 C10 0.9(7) . . . . ? C7 C8 C9 C10 178.6(5) . . . . ? C8 C9 C10 C11 -0.9(8) . . . . ? C9 C10 C11 C12 0.7(8) . . . . ? C8 N2 C12 C11 0.5(7) . . . . ? Zn1 N2 C12 C11 -175.4(4) . . . . ? C10 C11 C12 N2 -0.5(8) . . . . ? C6 N3 C13 C14 -169.0(4) . . . . ? C7 N3 C13 C14 59.1(6) . . . . ? Zn1 N3 C13 C14 -57.5(5) . . . . ? C6 N3 C13 C18 11.6(6) . . . . ? C7 N3 C13 C18 -120.3(5) . . . . ? Zn1 N3 C13 C18 123.0(4) . . . . ? C18 C13 C14 C15 1.5(8) . . . . ? N3 C13 C14 C15 -178.0(5) . . . . ? C13 C14 C15 C16 -2.1(8) . . . . ? C14 C15 C16 C17 1.0(8) . . . . ? C14 C15 C16 C19 -177.7(5) . . . . ? C15 C16 C17 C18 0.4(8) . . . . ? C19 C16 C17 C18 179.2(5) . . . . ? C14 C13 C18 C17 0.0(7) . . . . ? N3 C13 C18 C17 179.4(4) . . . . ? C16 C17 C18 C13 -0.9(8) . . . . ? C17 C16 C19 C20 -112.7(6) . . . . ? C15 C16 C19 C20 66.0(6) . . . . ? C16 C19 C20 C21 -94.2(6) . . . . ? C16 C19 C20 C25 83.7(6) . . . . ? C25 C20 C21 C22 -0.6(7) . . . . ? C19 C20 C21 C22 177.4(5) . . . . ? C20 C21 C22 C23 0.2(8) . . . . ? C21 C22 C23 C24 0.3(7) . . . . ? C21 C22 C23 N6 -179.8(4) . . . . ? C32 N6 C23 C24 165.9(5) . . . . ? C31 N6 C23 C24 33.9(6) . . . . ? Zn2 N6 C23 C24 -81.4(5) . . . . ? C32 N6 C23 C22 -13.9(6) . . . . ? C31 N6 C23 C22 -145.9(5) . . . . ? Zn2 N6 C23 C22 98.7(5) . . . . ? C22 C23 C24 C25 -0.3(8) . . . . ? N6 C23 C24 C25 179.8(5) . . . . ? C23 C24 C25 C20 -0.2(8) . . . . ? C21 C20 C25 C24 0.6(8) . . . . ? C19 C20 C25 C24 -177.4(5) . . . . ? C30 N4 C26 C27 1.2(8) . . . . ? Zn2 N4 C26 C27 -170.1(4) . . . . ? N4 C26 C27 C28 -0.3(9) . . . . ? C26 C27 C28 C29 -0.9(8) . . . . ? C27 C28 C29 C30 1.3(8) . . . . ? C26 N4 C30 C29 -0.8(7) . . . . ? Zn2 N4 C30 C29 171.0(4) . . . . ? C26 N4 C30 C31 -179.5(5) . . . . ? Zn2 N4 C30 C31 -7.7(6) . . . . ? C28 C29 C30 N4 -0.5(8) . . . . ? C28 C29 C30 C31 178.2(5) . . . . ? C23 N6 C31 C30 -82.7(5) . . . . ? C32 N6 C31 C30 144.6(4) . . . . ? Zn2 N6 C31 C30 38.1(5) . . . . ? N4 C30 C31 N6 -24.6(6) . . . . ? C29 C30 C31 N6 156.6(5) . . . . ? C23 N6 C32 C33 75.1(5) . . . . ? C31 N6 C32 C33 -152.9(4) . . . . ? Zn2 N6 C32 C33 -44.7(4) . . . . ? C37 N5 C33 C34 -0.1(7) . . . . ? Zn2 N5 C33 C34 -170.4(4) . . . . ? C37 N5 C33 C32 179.1(4) . . . . ? Zn2 N5 C33 C32 8.8(6) . . . . ? N6 C32 C33 N5 29.1(6) . . . . ? N6 C32 C33 C34 -151.8(5) . . . . ? N5 C33 C34 C35 -0.2(8) . . . . ? C32 C33 C34 C35 -179.3(5) . . . . ? C33 C34 C35 C36 -0.5(8) . . . . ? C34 C35 C36 C37 1.4(8) . . . . ? C33 N5 C37 C36 1.0(8) . . . . ? Zn2 N5 C37 C36 170.6(4) . . . . ? C35 C36 C37 N5 -1.7(8) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.412 _refine_diff_density_min -0.776 _refine_diff_density_rms 0.105 # Attachment '- complex 3.cif' data_dd _database_code_depnum_ccdc_archive 'CCDC 861140' #TrackingRef '- complex 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H40 Cl4 N8 Zn2' _chemical_formula_sum 'C41 H40 Cl4 N8 Zn2' _chemical_formula_weight 917.39 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.5044(17) _cell_length_b 18.377(4) _cell_length_c 27.098(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.98(3) _cell_angle_gamma 90.00 _cell_volume 4234.4(15) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 12884 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 27.9 _exptl_crystal_description needle-shaped _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.439 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1880 _exptl_absorpt_coefficient_mu 1.425 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.774 _exptl_absorpt_correction_T_max 0.855 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(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 34724 _diffrn_reflns_av_R_equivalents 0.0533 _diffrn_reflns_av_sigmaI/netI 0.0463 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 25.01 _reflns_number_total 7453 _reflns_number_gt 6818 _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^)+(0.0403P)^2^+2.0796P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7434 _refine_ls_number_parameters 498 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0468 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.0947 _refine_ls_wR_factor_gt 0.0916 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _refine_ls_shift/su_max 0.002 _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 Zn1 Zn 0.51111(4) 0.165729(17) 0.347425(12) 0.01824(10) Uani 1 1 d . . . Zn2 Zn -0.10592(4) 0.287806(18) 0.107236(12) 0.01987(10) Uani 1 1 d . . . Cl1 Cl 0.61188(8) 0.08724(4) 0.40614(3) 0.02319(17) Uani 1 1 d . . . Cl2 Cl 0.44646(9) 0.10945(4) 0.27483(3) 0.02767(18) Uani 1 1 d . . . Cl3 Cl -0.01847(11) 0.18619(4) 0.14568(3) 0.0368(2) Uani 1 1 d . . . Cl4 Cl -0.22596(9) 0.27666(4) 0.03131(3) 0.02709(18) Uani 1 1 d . . . N1 N 0.2873(3) 0.17540(12) 0.37712(8) 0.0179(5) Uani 1 1 d . . . N2 N 0.5056(3) 0.28154(12) 0.39290(8) 0.0176(5) Uani 1 1 d . . . N3 N 0.7142(3) 0.22234(12) 0.32702(8) 0.0182(5) Uani 1 1 d . . . N4 N 0.1092(3) 0.32774(13) 0.08232(9) 0.0225(6) Uani 1 1 d . . . N5 N -0.1161(3) 0.42016(13) 0.11695(8) 0.0188(5) Uani 1 1 d . . . N6 N -0.3106(3) 0.30876(13) 0.14659(8) 0.0198(5) Uani 1 1 d . . . C1 C 0.1614(3) 0.13742(15) 0.36083(11) 0.0204(6) Uani 1 1 d . . . H1 H 0.1686 0.1117 0.3314 0.024 Uiso 1 1 calc R . . C2 C 0.0229(3) 0.13521(15) 0.38608(11) 0.0225(7) Uani 1 1 d . . . H2 H -0.0623 0.1087 0.3738 0.027 Uiso 1 1 calc R . . C3 C 0.0118(3) 0.17292(15) 0.43005(11) 0.0211(7) Uani 1 1 d . . . H3 H -0.0801 0.1712 0.4481 0.025 Uiso 1 1 calc R . . C4 C 0.1401(3) 0.21333(15) 0.44679(11) 0.0201(6) Uani 1 1 d . . . H4 H 0.1344 0.2401 0.4758 0.024 Uiso 1 1 calc R . . C5 C 0.2763(3) 0.21305(14) 0.41963(10) 0.0177(6) Uani 1 1 d . . . C6 C 0.4245(3) 0.25214(15) 0.43623(10) 0.0182(6) Uani 1 1 d . . . H6A H 0.3980 0.2915 0.4584 0.022 Uiso 1 1 calc R . . H6B H 0.4933 0.2186 0.4539 0.022 Uiso 1 1 calc R . . C7 C 0.6754(3) 0.29404(16) 0.40141(10) 0.0190(6) Uani 1 1 d . . . H7A H 0.7114 0.2645 0.4290 0.023 Uiso 1 1 calc R . . H7B H 0.6925 0.3447 0.4100 0.023 Uiso 1 1 calc R . . C8 C 0.7708(3) 0.27558(14) 0.35660(10) 0.0173(6) Uani 1 1 d . . . C9 C 0.9103(3) 0.31098(15) 0.34709(11) 0.0222(7) Uani 1 1 d . . . H9 H 0.9468 0.3475 0.3681 0.027 Uiso 1 1 calc R . . C10 C 0.9950(4) 0.29159(17) 0.30621(11) 0.0266(7) Uani 1 1 d . . . H10 H 1.0893 0.3148 0.2994 0.032 Uiso 1 1 calc R . . C11 C 0.9382(4) 0.23719(17) 0.27544(11) 0.0275(7) Uani 1 1 d . . . H11 H 0.9930 0.2232 0.2476 0.033 Uiso 1 1 calc R . . C12 C 0.7977(4) 0.20421(16) 0.28728(10) 0.0228(7) Uani 1 1 d . . . H12 H 0.7591 0.1676 0.2667 0.027 Uiso 1 1 calc R . . C13 C 0.4259(3) 0.34271(14) 0.36948(10) 0.0169(6) Uani 1 1 d . . . C14 C 0.4772(4) 0.36882(17) 0.32423(11) 0.0249(7) Uani 1 1 d . . . H14 H 0.5618 0.3466 0.3090 0.030 Uiso 1 1 calc R . . C15 C 0.4036(4) 0.42759(17) 0.30160(10) 0.0252(7) Uani 1 1 d . . . H15 H 0.4410 0.4447 0.2717 0.030 Uiso 1 1 calc R . . C16 C 0.2751(3) 0.46148(15) 0.32266(10) 0.0185(6) Uani 1 1 d . . . C17 C 0.2240(3) 0.43535(15) 0.36728(10) 0.0210(6) Uani 1 1 d . . . H17 H 0.1380 0.4570 0.3821 0.025 Uiso 1 1 calc R . . C18 C 0.2991(3) 0.37685(15) 0.39058(10) 0.0210(6) Uani 1 1 d . . . H18 H 0.2630 0.3606 0.4209 0.025 Uiso 1 1 calc R . . C19 C 0.1907(4) 0.52378(15) 0.29658(10) 0.0236(7) Uani 1 1 d . . . H19A H 0.1145 0.5448 0.3187 0.028 Uiso 1 1 calc R . . H19B H 0.2665 0.5613 0.2886 0.028 Uiso 1 1 calc R . . C20 C 0.1072(3) 0.49910(15) 0.24951(10) 0.0185(6) Uani 1 1 d . . . C21 C 0.1805(3) 0.50279(15) 0.20442(10) 0.0199(6) Uani 1 1 d . . . H21 H 0.2803 0.5232 0.2030 0.024 Uiso 1 1 calc R . . C22 C 0.1099(3) 0.47696(15) 0.16113(10) 0.0195(6) Uani 1 1 d . . . H22 H 0.1637 0.4797 0.1316 0.023 Uiso 1 1 calc R . . C23 C -0.0400(3) 0.44715(15) 0.16161(10) 0.0180(6) Uani 1 1 d . . . C24 C -0.1160(4) 0.44376(17) 0.20703(11) 0.0258(7) Uani 1 1 d . . . H24 H -0.2167 0.4242 0.2085 0.031 Uiso 1 1 calc R . . C25 C -0.0433(4) 0.46919(17) 0.24975(11) 0.0285(7) Uani 1 1 d . . . H25 H -0.0964 0.4662 0.2794 0.034 Uiso 1 1 calc R . . C26 C -0.0362(4) 0.43977(16) 0.07100(10) 0.0219(7) Uani 1 1 d . . . H26A H -0.0096 0.4911 0.0718 0.026 Uiso 1 1 calc R . . H26B H -0.1074 0.4318 0.0432 0.026 Uiso 1 1 calc R . . C27 C 0.1122(4) 0.39563(17) 0.06382(10) 0.0240(7) Uani 1 1 d . . . C28 C 0.2401(4) 0.42265(19) 0.03889(11) 0.0311(8) Uani 1 1 d . . . H28 H 0.2395 0.4697 0.0262 0.037 Uiso 1 1 calc R . . C29 C 0.3698(4) 0.3774(2) 0.03332(12) 0.0381(9) Uani 1 1 d . . . H29 H 0.4569 0.3938 0.0163 0.046 Uiso 1 1 calc R . . C30 C 0.3693(4) 0.3085(2) 0.05284(12) 0.0358(9) Uani 1 1 d . . . H30 H 0.4560 0.2781 0.0499 0.043 Uiso 1 1 calc R . . C31 C 0.2366(4) 0.28561(18) 0.07696(11) 0.0295(8) Uani 1 1 d . . . H31 H 0.2354 0.2389 0.0901 0.035 Uiso 1 1 calc R . . C32 C -0.2878(3) 0.43255(15) 0.11487(11) 0.0207(6) Uani 1 1 d . . . H32A H -0.3234 0.4326 0.0807 0.025 Uiso 1 1 calc R . . H32B H -0.3108 0.4800 0.1287 0.025 Uiso 1 1 calc R . . C33 C -0.3767(3) 0.37515(16) 0.14275(10) 0.0203(6) Uani 1 1 d . . . C34 C -0.5224(3) 0.39021(17) 0.16230(11) 0.0242(7) Uani 1 1 d . . . H34 H -0.5660 0.4364 0.1591 0.029 Uiso 1 1 calc R . . C35 C -0.6020(4) 0.33616(19) 0.18657(11) 0.0315(8) Uani 1 1 d . . . H35 H -0.7005 0.3453 0.1996 0.038 Uiso 1 1 calc R . . C36 C -0.5339(4) 0.26807(19) 0.19131(11) 0.0319(8) Uani 1 1 d . . . H36 H -0.5849 0.2309 0.2079 0.038 Uiso 1 1 calc R . . C37 C -0.3895(4) 0.25664(17) 0.17092(11) 0.0273(7) Uani 1 1 d . . . H37 H -0.3439 0.2108 0.1740 0.033 Uiso 1 1 calc R . . N7 N 0.8197(4) 0.47676(18) 0.39916(14) 0.0563(9) Uani 1 1 d . . . C38 C 0.7444(5) 0.5205(2) 0.38057(14) 0.0453(10) Uani 1 1 d . . . C39 C 0.6486(6) 0.5771(2) 0.3589(2) 0.093(2) Uani 1 1 d . . . H39A H 0.5435 0.5735 0.3710 0.139 Uiso 1 1 calc R . . H39B H 0.6465 0.5718 0.3236 0.139 Uiso 1 1 calc R . . H39C H 0.6919 0.6237 0.3675 0.139 Uiso 1 1 calc R . . N8 N 1.1909(9) 0.1259(3) 0.01441(19) 0.121(3) Uani 1 1 d . . . C40 C 0.8960(9) 0.0855(3) 0.0283(2) 0.104(2) Uani 1 1 d . . . H40A H 0.8937 0.0519 0.0555 0.156 Uiso 1 1 calc R . . H40B H 0.8544 0.0622 -0.0008 0.156 Uiso 1 1 calc R . . H40C H 0.8332 0.1273 0.0359 0.156 Uiso 1 1 calc R . . C41 C 1.0587(12) 0.1082(3) 0.0199(2) 0.101(3) 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 Zn1 0.0167(2) 0.01890(19) 0.01906(19) -0.00112(13) -0.00051(14) 0.00001(14) Zn2 0.0204(2) 0.02128(19) 0.01796(18) 0.00083(13) -0.00016(14) 0.00253(14) Cl1 0.0215(4) 0.0224(4) 0.0257(4) 0.0043(3) 0.0005(3) 0.0035(3) Cl2 0.0249(4) 0.0343(4) 0.0237(4) -0.0096(3) -0.0032(3) 0.0001(3) Cl3 0.0497(6) 0.0301(4) 0.0306(4) 0.0084(3) 0.0049(4) 0.0161(4) Cl4 0.0218(4) 0.0404(4) 0.0191(4) -0.0035(3) -0.0019(3) -0.0008(3) N1 0.0177(14) 0.0171(12) 0.0190(13) 0.0027(9) -0.0019(10) 0.0026(10) N2 0.0140(13) 0.0221(13) 0.0167(12) 0.0019(9) -0.0011(10) 0.0005(10) N3 0.0180(13) 0.0173(12) 0.0193(12) 0.0014(10) -0.0009(10) 0.0015(10) N4 0.0181(14) 0.0311(15) 0.0183(13) -0.0072(10) -0.0007(10) 0.0014(11) N5 0.0164(13) 0.0231(13) 0.0170(12) 0.0017(10) 0.0002(10) -0.0002(10) N6 0.0195(14) 0.0223(13) 0.0175(12) -0.0005(10) -0.0004(10) -0.0020(11) C1 0.0197(17) 0.0172(15) 0.0240(16) -0.0019(12) -0.0070(13) 0.0031(13) C2 0.0182(17) 0.0173(15) 0.0319(17) 0.0029(12) -0.0042(13) -0.0011(13) C3 0.0154(16) 0.0198(15) 0.0281(17) 0.0076(12) 0.0016(12) 0.0012(13) C4 0.0207(17) 0.0192(15) 0.0205(15) 0.0056(11) -0.0016(12) 0.0024(13) C5 0.0169(16) 0.0178(15) 0.0182(15) 0.0065(11) -0.0026(12) 0.0029(12) C6 0.0208(16) 0.0192(15) 0.0145(14) 0.0025(11) -0.0004(12) 0.0002(12) C7 0.0159(16) 0.0217(15) 0.0193(15) 0.0000(11) -0.0023(12) -0.0006(12) C8 0.0161(16) 0.0169(14) 0.0188(15) 0.0050(11) -0.0022(12) 0.0010(12) C9 0.0229(17) 0.0197(15) 0.0239(16) 0.0005(12) -0.0018(13) 0.0005(13) C10 0.0209(17) 0.0300(17) 0.0290(17) 0.0072(13) 0.0029(13) -0.0055(14) C11 0.0276(19) 0.0313(18) 0.0237(17) 0.0019(13) 0.0058(14) 0.0025(15) C12 0.0258(18) 0.0229(16) 0.0198(15) -0.0016(12) -0.0003(13) 0.0014(14) C13 0.0158(16) 0.0174(14) 0.0176(14) 0.0010(11) -0.0025(12) -0.0015(12) C14 0.0182(17) 0.0330(18) 0.0237(16) 0.0031(13) 0.0032(13) 0.0075(14) C15 0.0269(18) 0.0336(18) 0.0153(15) 0.0072(12) 0.0022(13) 0.0026(14) C16 0.0193(16) 0.0184(15) 0.0174(14) 0.0000(11) -0.0062(12) -0.0031(12) C17 0.0194(16) 0.0208(15) 0.0227(16) -0.0043(12) 0.0014(12) 0.0022(13) C18 0.0224(17) 0.0238(16) 0.0167(15) 0.0032(12) 0.0021(12) 0.0004(13) C19 0.0283(18) 0.0191(15) 0.0232(16) -0.0017(12) -0.0025(13) 0.0013(13) C20 0.0224(17) 0.0133(14) 0.0196(15) 0.0018(11) -0.0025(12) 0.0040(12) C21 0.0159(16) 0.0174(15) 0.0261(16) -0.0003(12) -0.0024(12) -0.0014(12) C22 0.0196(17) 0.0198(15) 0.0191(15) 0.0001(11) 0.0023(12) 0.0024(13) C23 0.0191(16) 0.0155(14) 0.0193(15) 0.0005(11) -0.0023(12) 0.0041(12) C24 0.0187(17) 0.0331(18) 0.0256(17) -0.0016(13) 0.0025(13) -0.0079(14) C25 0.0289(19) 0.0376(19) 0.0192(16) 0.0024(13) 0.0032(13) -0.0032(15) C26 0.0253(17) 0.0247(16) 0.0155(15) 0.0008(11) -0.0010(12) -0.0033(13) C27 0.0241(18) 0.0333(18) 0.0145(15) -0.0085(12) -0.0019(12) -0.0055(14) C28 0.033(2) 0.0400(19) 0.0204(16) -0.0110(14) 0.0039(14) -0.0150(16) C29 0.0230(19) 0.065(3) 0.0265(18) -0.0239(17) 0.0060(14) -0.0155(18) C30 0.0171(18) 0.060(2) 0.0302(19) -0.0249(17) -0.0034(14) 0.0054(17) C31 0.0240(18) 0.040(2) 0.0240(17) -0.0112(14) -0.0083(14) 0.0042(15) C32 0.0170(16) 0.0210(15) 0.0239(16) 0.0005(12) -0.0036(12) 0.0028(13) C33 0.0182(16) 0.0259(16) 0.0165(14) -0.0018(12) -0.0049(12) -0.0004(13) C34 0.0188(17) 0.0310(17) 0.0229(16) -0.0051(13) -0.0006(13) 0.0031(14) C35 0.0200(18) 0.049(2) 0.0255(17) -0.0074(15) 0.0034(13) -0.0043(16) C36 0.033(2) 0.039(2) 0.0237(17) 0.0019(14) 0.0039(14) -0.0125(16) C37 0.034(2) 0.0255(17) 0.0229(16) 0.0037(13) 0.0009(14) -0.0022(15) N7 0.057(2) 0.0338(19) 0.078(3) -0.0077(18) 0.0084(19) -0.0020(17) C38 0.058(3) 0.034(2) 0.044(2) -0.0057(17) -0.003(2) -0.013(2) C39 0.102(4) 0.056(3) 0.119(5) 0.028(3) -0.067(4) -0.025(3) N8 0.248(8) 0.051(3) 0.067(3) 0.011(2) 0.081(4) 0.010(4) C40 0.200(8) 0.035(3) 0.077(4) -0.007(3) -0.023(5) 0.009(4) C41 0.215(9) 0.027(3) 0.062(3) 0.010(2) 0.052(5) 0.010(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 Zn1 N1 2.087(2) . ? Zn1 N3 2.099(2) . ? Zn1 Cl2 2.2815(9) . ? Zn1 Cl1 2.3021(9) . ? Zn1 N2 2.460(2) . ? Zn2 N6 2.092(3) . ? Zn2 N4 2.093(3) . ? Zn2 Cl3 2.2580(9) . ? Zn2 Cl4 2.2901(10) . ? Zn2 N5 2.448(2) . ? N1 C1 1.346(4) . ? N1 C5 1.348(4) . ? N2 C13 1.453(3) . ? N2 C6 1.475(3) . ? N2 C7 1.476(4) . ? N3 C12 1.342(4) . ? N3 C8 1.348(3) . ? N4 C31 1.342(4) . ? N4 C27 1.345(4) . ? N5 C23 1.450(3) . ? N5 C26 1.473(4) . ? N5 C32 1.478(4) . ? N6 C33 1.347(4) . ? N6 C37 1.348(4) . ? C1 C2 1.373(4) . ? C1 H1 0.9300 . ? C2 C3 1.383(4) . ? C2 H2 0.9300 . ? C3 C4 1.390(4) . ? C3 H3 0.9300 . ? C4 C5 1.383(4) . ? C4 H4 0.9300 . ? C5 C6 1.512(4) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.510(4) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.381(4) . ? C9 C10 1.378(4) . ? C9 H9 0.9300 . ? C10 C11 1.384(4) . ? C10 H10 0.9300 . ? C11 C12 1.382(4) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C18 1.380(4) . ? C13 C14 1.394(4) . ? C14 C15 1.386(4) . ? C14 H14 0.9300 . ? C15 C16 1.389(4) . ? C15 H15 0.9300 . ? C16 C17 1.378(4) . ? C16 C19 1.519(4) . ? C17 C18 1.396(4) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.519(4) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.382(4) . ? C20 C25 1.393(4) . ? C21 C22 1.392(4) . ? C21 H21 0.9300 . ? C22 C23 1.388(4) . ? C22 H22 0.9300 . ? C23 C24 1.401(4) . ? C24 C25 1.384(4) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 C27 1.515(4) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.383(4) . ? C28 C29 1.392(5) . ? C28 H28 0.9300 . ? C29 C30 1.371(5) . ? C29 H29 0.9300 . ? C30 C31 1.379(5) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 C33 1.508(4) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.384(4) . ? C34 C35 1.376(4) . ? C34 H34 0.9300 . ? C35 C36 1.384(5) . ? C35 H35 0.9300 . ? C36 C37 1.371(4) . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? N7 C38 1.140(5) . ? C38 C39 1.440(6) . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? N8 C41 1.182(10) . ? C40 C41 1.468(9) . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? 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 Zn1 N3 145.05(9) . . ? N1 Zn1 Cl2 99.39(7) . . ? N3 Zn1 Cl2 100.65(7) . . ? N1 Zn1 Cl1 96.78(7) . . ? N3 Zn1 Cl1 101.20(7) . . ? Cl2 Zn1 Cl1 113.15(3) . . ? N1 Zn1 N2 73.02(8) . . ? N3 Zn1 N2 74.09(9) . . ? Cl2 Zn1 N2 144.86(6) . . ? Cl1 Zn1 N2 101.88(6) . . ? N6 Zn2 N4 147.02(9) . . ? N6 Zn2 Cl3 100.80(7) . . ? N4 Zn2 Cl3 98.97(7) . . ? N6 Zn2 Cl4 96.45(7) . . ? N4 Zn2 Cl4 96.90(7) . . ? Cl3 Zn2 Cl4 118.60(3) . . ? N6 Zn2 N5 74.40(8) . . ? N4 Zn2 N5 73.69(9) . . ? Cl3 Zn2 N5 141.63(6) . . ? Cl4 Zn2 N5 99.75(6) . . ? C1 N1 C5 118.7(3) . . ? C1 N1 Zn1 123.7(2) . . ? C5 N1 Zn1 116.74(19) . . ? C13 N2 C6 114.2(2) . . ? C13 N2 C7 113.3(2) . . ? C6 N2 C7 113.8(2) . . ? C13 N2 Zn1 117.58(16) . . ? C6 N2 Zn1 95.45(15) . . ? C7 N2 Zn1 100.72(16) . . ? C12 N3 C8 118.0(3) . . ? C12 N3 Zn1 122.51(19) . . ? C8 N3 Zn1 119.33(19) . . ? C31 N4 C27 118.3(3) . . ? C31 N4 Zn2 123.0(2) . . ? C27 N4 Zn2 117.9(2) . . ? C23 N5 C26 114.6(2) . . ? C23 N5 C32 113.9(2) . . ? C26 N5 C32 113.6(2) . . ? C23 N5 Zn2 114.42(16) . . ? C26 N5 Zn2 97.72(16) . . ? C32 N5 Zn2 100.70(16) . . ? C33 N6 C37 118.1(3) . . ? C33 N6 Zn2 118.50(19) . . ? C37 N6 Zn2 123.0(2) . . ? N1 C1 C2 122.4(3) . . ? N1 C1 H1 118.8 . . ? C2 C1 H1 118.8 . . ? C1 C2 C3 119.1(3) . . ? C1 C2 H2 120.5 . . ? C3 C2 H2 120.5 . . ? C2 C3 C4 119.0(3) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C5 C4 C3 119.0(3) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? N1 C5 C4 121.8(3) . . ? N1 C5 C6 115.4(3) . . ? C4 C5 C6 122.8(3) . . ? N2 C6 C5 109.7(2) . . ? N2 C6 H6A 109.7 . . ? C5 C6 H6A 109.7 . . ? N2 C6 H6B 109.7 . . ? C5 C6 H6B 109.7 . . ? H6A C6 H6B 108.2 . . ? N2 C7 C8 112.1(2) . . ? N2 C7 H7A 109.2 . . ? C8 C7 H7A 109.2 . . ? N2 C7 H7B 109.2 . . ? C8 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? N3 C8 C9 122.0(3) . . ? N3 C8 C7 116.8(2) . . ? C9 C8 C7 121.3(3) . . ? C10 C9 C8 119.4(3) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C9 C10 C11 119.3(3) . . ? C9 C10 H10 120.4 . . ? C11 C10 H10 120.4 . . ? C12 C11 C10 118.1(3) . . ? C12 C11 H11 120.9 . . ? C10 C11 H11 120.9 . . ? N3 C12 C11 123.3(3) . . ? N3 C12 H12 118.4 . . ? C11 C12 H12 118.4 . . ? C18 C13 C14 117.8(3) . . ? C18 C13 N2 122.2(2) . . ? C14 C13 N2 120.0(3) . . ? C15 C14 C13 120.8(3) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C14 C15 C16 121.3(3) . . ? C14 C15 H15 119.3 . . ? C16 C15 H15 119.3 . . ? C17 C16 C15 117.8(3) . . ? C17 C16 C19 121.1(3) . . ? C15 C16 C19 121.0(3) . . ? C16 C17 C18 121.1(3) . . ? C16 C17 H17 119.5 . . ? C18 C17 H17 119.5 . . ? C13 C18 C17 121.2(3) . . ? C13 C18 H18 119.4 . . ? C17 C18 H18 119.4 . . ? C20 C19 C16 112.1(2) . . ? C20 C19 H19A 109.2 . . ? C16 C19 H19A 109.2 . . ? C20 C19 H19B 109.2 . . ? C16 C19 H19B 109.2 . . ? H19A C19 H19B 107.9 . . ? C21 C20 C25 116.8(3) . . ? C21 C20 C19 121.1(3) . . ? C25 C20 C19 122.0(3) . . ? C20 C21 C22 122.3(3) . . ? C20 C21 H21 118.9 . . ? C22 C21 H21 118.9 . . ? C23 C22 C21 120.6(3) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C22 C23 C24 117.6(3) . . ? C22 C23 N5 121.6(3) . . ? C24 C23 N5 120.8(3) . . ? C25 C24 C23 120.9(3) . . ? C25 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? C24 C25 C20 121.8(3) . . ? C24 C25 H25 119.1 . . ? C20 C25 H25 119.1 . . ? N5 C26 C27 112.0(2) . . ? N5 C26 H26A 109.2 . . ? C27 C26 H26A 109.2 . . ? N5 C26 H26B 109.2 . . ? C27 C26 H26B 109.2 . . ? H26A C26 H26B 107.9 . . ? N4 C27 C28 122.4(3) . . ? N4 C27 C26 115.3(3) . . ? C28 C27 C26 122.3(3) . . ? C27 C28 C29 118.0(3) . . ? C27 C28 H28 121.0 . . ? C29 C28 H28 121.0 . . ? C30 C29 C28 120.1(3) . . ? C30 C29 H29 119.9 . . ? C28 C29 H29 119.9 . . ? C29 C30 C31 118.2(3) . . ? C29 C30 H30 120.9 . . ? C31 C30 H30 120.9 . . ? N4 C31 C30 123.0(3) . . ? N4 C31 H31 118.5 . . ? C30 C31 H31 118.5 . . ? N5 C32 C33 112.1(2) . . ? N5 C32 H32A 109.2 . . ? C33 C32 H32A 109.2 . . ? N5 C32 H32B 109.2 . . ? C33 C32 H32B 109.2 . . ? H32A C32 H32B 107.9 . . ? N6 C33 C34 121.8(3) . . ? N6 C33 C32 117.4(3) . . ? C34 C33 C32 120.8(3) . . ? C35 C34 C33 119.3(3) . . ? C35 C34 H34 120.3 . . ? C33 C34 H34 120.3 . . ? C34 C35 C36 119.2(3) . . ? C34 C35 H35 120.4 . . ? C36 C35 H35 120.4 . . ? C37 C36 C35 118.5(3) . . ? C37 C36 H36 120.7 . . ? C35 C36 H36 120.7 . . ? N6 C37 C36 123.0(3) . . ? N6 C37 H37 118.5 . . ? C36 C37 H37 118.5 . . ? N7 C38 C39 177.8(5) . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C41 C40 H40A 109.5 . . ? C41 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C41 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N8 C41 C40 178.2(7) . . ? 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 N3 Zn1 N1 C1 140.8(2) . . . . ? Cl2 Zn1 N1 C1 16.5(2) . . . . ? Cl1 Zn1 N1 C1 -98.4(2) . . . . ? N2 Zn1 N1 C1 161.2(2) . . . . ? N3 Zn1 N1 C5 -50.0(3) . . . . ? Cl2 Zn1 N1 C5 -174.30(18) . . . . ? Cl1 Zn1 N1 C5 70.80(19) . . . . ? N2 Zn1 N1 C5 -29.59(18) . . . . ? N1 Zn1 N2 C13 -77.45(19) . . . . ? N3 Zn1 N2 C13 90.6(2) . . . . ? Cl2 Zn1 N2 C13 4.7(2) . . . . ? Cl1 Zn1 N2 C13 -171.00(18) . . . . ? N1 Zn1 N2 C6 43.50(15) . . . . ? N3 Zn1 N2 C6 -148.48(16) . . . . ? Cl2 Zn1 N2 C6 125.60(14) . . . . ? Cl1 Zn1 N2 C6 -50.06(15) . . . . ? N1 Zn1 N2 C7 158.96(17) . . . . ? N3 Zn1 N2 C7 -33.02(15) . . . . ? Cl2 Zn1 N2 C7 -118.94(15) . . . . ? Cl1 Zn1 N2 C7 65.40(16) . . . . ? N1 Zn1 N3 C12 -143.6(2) . . . . ? Cl2 Zn1 N3 C12 -19.6(2) . . . . ? Cl1 Zn1 N3 C12 96.9(2) . . . . ? N2 Zn1 N3 C12 -163.8(2) . . . . ? N1 Zn1 N3 C8 41.5(3) . . . . ? Cl2 Zn1 N3 C8 165.45(18) . . . . ? Cl1 Zn1 N3 C8 -78.12(19) . . . . ? N2 Zn1 N3 C8 21.19(18) . . . . ? N6 Zn2 N4 C31 147.5(2) . . . . ? Cl3 Zn2 N4 C31 21.2(2) . . . . ? Cl4 Zn2 N4 C31 -99.3(2) . . . . ? N5 Zn2 N4 C31 162.5(2) . . . . ? N6 Zn2 N4 C27 -43.0(3) . . . . ? Cl3 Zn2 N4 C27 -169.30(19) . . . . ? Cl4 Zn2 N4 C27 70.2(2) . . . . ? N5 Zn2 N4 C27 -27.97(19) . . . . ? N6 Zn2 N5 C23 89.09(19) . . . . ? N4 Zn2 N5 C23 -82.47(19) . . . . ? Cl3 Zn2 N5 C23 1.3(2) . . . . ? Cl4 Zn2 N5 C23 -176.87(18) . . . . ? N6 Zn2 N5 C26 -149.40(17) . . . . ? N4 Zn2 N5 C26 39.04(16) . . . . ? Cl3 Zn2 N5 C26 122.85(15) . . . . ? Cl4 Zn2 N5 C26 -55.36(16) . . . . ? N6 Zn2 N5 C32 -33.54(16) . . . . ? N4 Zn2 N5 C32 154.90(17) . . . . ? Cl3 Zn2 N5 C32 -121.29(15) . . . . ? Cl4 Zn2 N5 C32 60.50(16) . . . . ? N4 Zn2 N6 C33 38.0(3) . . . . ? Cl3 Zn2 N6 C33 163.87(18) . . . . ? Cl4 Zn2 N6 C33 -75.33(19) . . . . ? N5 Zn2 N6 C33 23.03(19) . . . . ? N4 Zn2 N6 C37 -150.0(2) . . . . ? Cl3 Zn2 N6 C37 -24.1(2) . . . . ? Cl4 Zn2 N6 C37 96.6(2) . . . . ? N5 Zn2 N6 C37 -165.0(2) . . . . ? C5 N1 C1 C2 -0.5(4) . . . . ? Zn1 N1 C1 C2 168.5(2) . . . . ? N1 C1 C2 C3 -0.4(4) . . . . ? C1 C2 C3 C4 1.5(4) . . . . ? C2 C3 C4 C5 -1.7(4) . . . . ? C1 N1 C5 C4 0.3(4) . . . . ? Zn1 N1 C5 C4 -169.5(2) . . . . ? C1 N1 C5 C6 178.0(2) . . . . ? Zn1 N1 C5 C6 8.2(3) . . . . ? C3 C4 C5 N1 0.8(4) . . . . ? C3 C4 C5 C6 -176.8(2) . . . . ? C13 N2 C6 C5 70.9(3) . . . . ? C7 N2 C6 C5 -156.9(2) . . . . ? Zn1 N2 C6 C5 -52.6(2) . . . . ? N1 C5 C6 N2 37.4(3) . . . . ? C4 C5 C6 N2 -144.9(3) . . . . ? C13 N2 C7 C8 -85.0(3) . . . . ? C6 N2 C7 C8 142.3(2) . . . . ? Zn1 N2 C7 C8 41.5(2) . . . . ? C12 N3 C8 C9 -0.2(4) . . . . ? Zn1 N3 C8 C9 175.0(2) . . . . ? C12 N3 C8 C7 -179.2(2) . . . . ? Zn1 N3 C8 C7 -4.0(3) . . . . ? N2 C7 C8 N3 -30.4(3) . . . . ? N2 C7 C8 C9 150.6(2) . . . . ? N3 C8 C9 C10 0.0(4) . . . . ? C7 C8 C9 C10 178.9(3) . . . . ? C8 C9 C10 C11 0.2(4) . . . . ? C9 C10 C11 C12 -0.2(4) . . . . ? C8 N3 C12 C11 0.2(4) . . . . ? Zn1 N3 C12 C11 -174.8(2) . . . . ? C10 C11 C12 N3 0.0(4) . . . . ? C6 N2 C13 C18 9.4(4) . . . . ? C7 N2 C13 C18 -123.0(3) . . . . ? Zn1 N2 C13 C18 120.1(2) . . . . ? C6 N2 C13 C14 -170.7(3) . . . . ? C7 N2 C13 C14 56.9(3) . . . . ? Zn1 N2 C13 C14 -60.1(3) . . . . ? C18 C13 C14 C15 0.6(4) . . . . ? N2 C13 C14 C15 -179.3(3) . . . . ? C13 C14 C15 C16 -1.2(5) . . . . ? C14 C15 C16 C17 0.8(4) . . . . ? C14 C15 C16 C19 -177.4(3) . . . . ? C15 C16 C17 C18 0.2(4) . . . . ? C19 C16 C17 C18 178.3(2) . . . . ? C14 C13 C18 C17 0.4(4) . . . . ? N2 C13 C18 C17 -179.8(2) . . . . ? C16 C17 C18 C13 -0.7(4) . . . . ? C17 C16 C19 C20 -111.3(3) . . . . ? C15 C16 C19 C20 66.8(4) . . . . ? C16 C19 C20 C21 -92.7(3) . . . . ? C16 C19 C20 C25 84.7(3) . . . . ? C25 C20 C21 C22 -1.1(4) . . . . ? C19 C20 C21 C22 176.5(3) . . . . ? C20 C21 C22 C23 1.0(4) . . . . ? C21 C22 C23 C24 -0.4(4) . . . . ? C21 C22 C23 N5 179.8(2) . . . . ? C26 N5 C23 C22 -11.3(4) . . . . ? C32 N5 C23 C22 -144.4(3) . . . . ? Zn2 N5 C23 C22 100.4(3) . . . . ? C26 N5 C23 C24 168.9(3) . . . . ? C32 N5 C23 C24 35.7(4) . . . . ? Zn2 N5 C23 C24 -79.4(3) . . . . ? C22 C23 C24 C25 -0.1(4) . . . . ? N5 C23 C24 C25 179.7(3) . . . . ? C23 C24 C25 C20 0.1(5) . . . . ? C21 C20 C25 C24 0.5(4) . . . . ? C19 C20 C25 C24 -177.0(3) . . . . ? C23 N5 C26 C27 74.4(3) . . . . ? C32 N5 C26 C27 -152.2(2) . . . . ? Zn2 N5 C26 C27 -47.0(2) . . . . ? C31 N4 C27 C28 1.2(4) . . . . ? Zn2 N4 C27 C28 -168.8(2) . . . . ? C31 N4 C27 C26 179.6(2) . . . . ? Zn2 N4 C27 C26 9.6(3) . . . . ? N5 C26 C27 N4 31.6(3) . . . . ? N5 C26 C27 C28 -150.0(3) . . . . ? N4 C27 C28 C29 -0.4(4) . . . . ? C26 C27 C28 C29 -178.7(3) . . . . ? C27 C28 C29 C30 -0.9(4) . . . . ? C28 C29 C30 C31 1.3(4) . . . . ? C27 N4 C31 C30 -0.8(4) . . . . ? Zn2 N4 C31 C30 168.6(2) . . . . ? C29 C30 C31 N4 -0.4(4) . . . . ? C23 N5 C32 C33 -82.4(3) . . . . ? C26 N5 C32 C33 143.9(2) . . . . ? Zn2 N5 C32 C33 40.5(2) . . . . ? C37 N6 C33 C34 -1.0(4) . . . . ? Zn2 N6 C33 C34 171.4(2) . . . . ? C37 N6 C33 C32 -179.2(2) . . . . ? Zn2 N6 C33 C32 -6.9(3) . . . . ? N5 C32 C33 N6 -27.9(3) . . . . ? N5 C32 C33 C34 153.8(2) . . . . ? N6 C33 C34 C35 0.3(4) . . . . ? C32 C33 C34 C35 178.5(3) . . . . ? C33 C34 C35 C36 0.6(4) . . . . ? C34 C35 C36 C37 -0.9(4) . . . . ? C33 N6 C37 C36 0.7(4) . . . . ? Zn2 N6 C37 C36 -171.3(2) . . . . ? C35 C36 C37 N6 0.2(5) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.506 _refine_diff_density_min -0.475 _refine_diff_density_rms 0.072 data_bb _database_code_depnum_ccdc_archive 'CCDC 861144' #TrackingRef '- L1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H35 Cl2 N5 O2' _chemical_formula_weight 580.54 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' Cl Cl 0.1484 0.1585 '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 14.573(10) _cell_length_b 11.493(8) _cell_length_c 17.074(13) _cell_angle_alpha 90.00 _cell_angle_beta 97.932(14) _cell_angle_gamma 90.00 _cell_volume 2832(4) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 7447 _cell_measurement_theta_min 1.7 _cell_measurement_theta_max 26.0 _exptl_crystal_description Prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.362 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 0.268 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.956 _exptl_absorpt_correction_T_max 0.984 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(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 18780 _diffrn_reflns_av_R_equivalents 0.0909 _diffrn_reflns_av_sigmaI/netI 0.1011 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5008 _reflns_number_gt 3746 _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^)+(0.0590P)^2^+2.0091P] 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 5008 _refine_ls_number_parameters 377 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1206 _refine_ls_R_factor_gt 0.0882 _refine_ls_wR_factor_ref 0.1884 _refine_ls_wR_factor_gt 0.1718 _refine_ls_goodness_of_fit_ref 1.161 _refine_ls_restrained_S_all 1.161 _refine_ls_shift/su_max 0.010 _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 Cl1 Cl 0.08663(8) 0.95117(11) 0.23735(7) 0.0340(3) Uani 1 1 d . . . Cl2 Cl 0.67886(9) 0.91726(11) 0.48564(7) 0.0385(4) Uani 1 1 d . . . O1 O 0.7687(3) 0.4328(3) 0.8301(2) 0.0368(9) Uani 1 1 d . . . O2 O 0.7283(3) 0.1965(4) 0.7809(3) 0.0454(10) Uani 1 1 d . . . N1 N 0.5085(3) -0.2446(3) -0.0148(2) 0.0293(9) Uani 1 1 d . . . H1A H 0.5047 -0.1896 -0.0510 0.035 Uiso 1 1 calc R . . N2 N 0.4989(2) -0.0647(3) -0.1199(2) 0.0242(9) Uani 1 1 d . . . N3 N 0.6706(2) -0.1839(3) -0.0833(2) 0.0254(9) Uani 1 1 d . . . N4 N 0.5336(3) 0.2156(3) 0.3175(2) 0.0288(9) Uani 1 1 d . . . H4 H 0.4955 0.2708 0.2976 0.035 Uiso 1 1 calc R . . N5 N 0.5906(3) 0.1472(3) 0.5189(2) 0.0291(9) Uani 1 1 d . . . H5 H 0.6094 0.0774 0.5071 0.035 Uiso 1 1 calc R . . C1 C 0.4419(3) -0.2570(4) 0.0321(3) 0.0319(12) Uani 1 1 d . . . H1 H 0.3900 -0.2063 0.0246 0.038 Uiso 1 1 calc R . . C2 C 0.4465(3) -0.3409(4) 0.0908(3) 0.0332(12) Uani 1 1 d . . . H2 H 0.3991 -0.3466 0.1236 0.040 Uiso 1 1 calc R . . C3 C 0.5214(3) -0.4166(4) 0.1009(3) 0.0329(12) Uani 1 1 d . . . H3 H 0.5258 -0.4753 0.1405 0.039 Uiso 1 1 calc R . . C4 C 0.5898(3) -0.4051(4) 0.0524(3) 0.0295(11) Uani 1 1 d . . . H4A H 0.6417 -0.4559 0.0584 0.035 Uiso 1 1 calc R . . C5 C 0.5817(3) -0.3188(4) -0.0049(3) 0.0232(10) Uani 1 1 d . . . C6 C 0.6523(3) -0.3040(4) -0.0620(3) 0.0271(11) Uani 1 1 d . . . H6A H 0.7114 -0.3398 -0.0381 0.033 Uiso 1 1 calc R . . H6B H 0.6303 -0.3476 -0.1110 0.033 Uiso 1 1 calc R . . C7 C 0.4265(3) 0.0100(4) -0.1232(3) 0.0236(10) Uani 1 1 d . . . H7 H 0.3828 0.0007 -0.0871 0.028 Uiso 1 1 calc R . . C8 C 0.4149(3) 0.0989(4) -0.1774(3) 0.0287(11) Uani 1 1 d . . . H8 H 0.3638 0.1505 -0.1793 0.034 Uiso 1 1 calc R . . C9 C 0.4797(3) 0.1117(4) -0.2296(3) 0.0335(12) Uani 1 1 d . . . H9 H 0.4731 0.1722 -0.2679 0.040 Uiso 1 1 calc R . . C10 C 0.5541(3) 0.0353(4) -0.2254(3) 0.0284(11) Uani 1 1 d . . . H10 H 0.5991 0.0444 -0.2602 0.034 Uiso 1 1 calc R . . C11 C 0.5626(3) -0.0536(4) -0.1707(3) 0.0244(10) Uani 1 1 d . . . C12 C 0.6402(3) -0.1434(4) -0.1632(3) 0.0271(11) Uani 1 1 d . . . H12A H 0.6192 -0.2113 -0.1965 0.033 Uiso 1 1 calc R . . H12B H 0.6941 -0.1092 -0.1844 0.033 Uiso 1 1 calc R . . C13 C 0.7201(3) -0.1077(4) -0.0284(3) 0.0222(10) Uani 1 1 d . . . C14 C 0.7359(3) 0.0093(4) -0.0477(3) 0.0231(10) Uani 1 1 d . . . H14 H 0.7168 0.0363 -0.1000 0.028 Uiso 1 1 calc R . . C15 C 0.7792(3) 0.0857(4) 0.0091(3) 0.0240(10) Uani 1 1 d . . . H15 H 0.7886 0.1642 -0.0053 0.029 Uiso 1 1 calc R . . C16 C 0.8091(3) 0.0503(4) 0.0863(3) 0.0238(10) Uani 1 1 d . . . C17 C 0.7981(3) -0.0673(4) 0.1037(3) 0.0253(10) Uani 1 1 d . . . H17 H 0.8214 -0.0949 0.1551 0.030 Uiso 1 1 calc R . . C18 C 0.7543(3) -0.1452(4) 0.0485(2) 0.0242(10) Uani 1 1 d . . . H18 H 0.7475 -0.2244 0.0627 0.029 Uiso 1 1 calc R . . C19 C 0.8442(3) 0.1371(4) 0.1510(3) 0.0271(11) Uani 1 1 d . . . H19A H 0.8640 0.2095 0.1268 0.033 Uiso 1 1 calc R . . H19B H 0.8985 0.1041 0.1851 0.033 Uiso 1 1 calc R . . C20 C 0.7680(3) 0.1650(4) 0.2012(3) 0.0253(10) Uani 1 1 d . . . C21 C 0.7557(3) 0.0984(4) 0.2670(3) 0.0283(11) Uani 1 1 d . . . H21 H 0.7999 0.0400 0.2844 0.034 Uiso 1 1 calc R . . C22 C 0.6802(3) 0.1147(4) 0.3082(3) 0.0286(11) Uani 1 1 d . . . H22 H 0.6743 0.0683 0.3533 0.034 Uiso 1 1 calc R . . C23 C 0.6137(3) 0.1985(4) 0.2835(3) 0.0250(10) Uani 1 1 d . . . C24 C 0.6263(3) 0.2690(4) 0.2172(3) 0.0266(11) Uani 1 1 d . . . H24 H 0.5825 0.3281 0.2002 0.032 Uiso 1 1 calc R . . C25 C 0.7019(3) 0.2522(4) 0.1771(3) 0.0296(11) Uani 1 1 d . . . H25 H 0.7093 0.2999 0.1330 0.035 Uiso 1 1 calc R . . C26 C 0.5079(3) 0.1495(4) 0.3833(3) 0.0315(11) Uani 1 1 d . . . H26A H 0.5368 0.0716 0.3835 0.038 Uiso 1 1 calc R . . H26B H 0.4398 0.1385 0.3753 0.038 Uiso 1 1 calc R . . C27 C 0.5361(3) 0.2059(4) 0.4629(3) 0.0260(11) Uani 1 1 d . . . C28 C 0.5062(3) 0.3167(4) 0.4817(3) 0.0334(12) Uani 1 1 d . . . H28 H 0.4674 0.3606 0.4433 0.040 Uiso 1 1 calc R . . C29 C 0.5333(3) 0.3627(4) 0.5566(3) 0.0326(12) Uani 1 1 d . . . H29 H 0.5131 0.4381 0.5693 0.039 Uiso 1 1 calc R . . C30 C 0.5902(3) 0.2980(4) 0.6131(3) 0.0310(11) Uani 1 1 d . . . H30 H 0.6087 0.3287 0.6645 0.037 Uiso 1 1 calc R . . C31 C 0.6189(3) 0.1891(4) 0.5934(3) 0.0315(12) Uani 1 1 d . . . H31 H 0.6577 0.1437 0.6309 0.038 Uiso 1 1 calc R . . H2W H 0.719(4) 0.463(5) 0.812(4) 0.06(2) Uiso 1 1 d . . . H1W H 0.770(4) 0.435(5) 0.884(4) 0.07(2) Uiso 1 1 d . . . H4W H 0.740(5) 0.276(8) 0.798(5) 0.12(3) Uiso 1 1 d . . . H3W H 0.778(5) 0.160(7) 0.782(4) 0.10(3) Uiso 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 Cl1 0.0383(7) 0.0316(7) 0.0319(7) 0.0022(5) 0.0045(5) -0.0015(5) Cl2 0.0524(8) 0.0323(7) 0.0324(7) -0.0002(6) 0.0115(6) 0.0043(6) O1 0.036(2) 0.045(2) 0.031(2) 0.0026(18) 0.0071(18) 0.0044(18) O2 0.041(2) 0.041(3) 0.055(3) 0.003(2) 0.011(2) -0.002(2) N1 0.034(2) 0.029(2) 0.025(2) 0.0059(18) 0.0055(18) -0.0004(18) N2 0.024(2) 0.024(2) 0.025(2) -0.0043(17) 0.0049(17) -0.0029(16) N3 0.027(2) 0.030(2) 0.0199(19) 0.0006(17) 0.0051(17) -0.0001(17) N4 0.032(2) 0.032(2) 0.023(2) 0.0020(18) 0.0054(18) 0.0060(18) N5 0.036(2) 0.027(2) 0.026(2) -0.0002(18) 0.0095(19) 0.0001(18) C1 0.025(3) 0.037(3) 0.035(3) 0.000(2) 0.008(2) 0.003(2) C2 0.032(3) 0.039(3) 0.029(3) 0.005(2) 0.007(2) -0.002(2) C3 0.037(3) 0.028(3) 0.032(3) 0.010(2) 0.000(2) -0.007(2) C4 0.028(3) 0.030(3) 0.030(3) 0.001(2) -0.001(2) 0.000(2) C5 0.022(2) 0.024(3) 0.021(2) -0.0033(19) -0.0028(19) -0.0009(19) C6 0.029(3) 0.024(3) 0.028(2) -0.005(2) 0.005(2) 0.004(2) C7 0.023(2) 0.023(2) 0.025(2) -0.004(2) 0.0033(19) 0.0001(19) C8 0.030(3) 0.024(3) 0.033(3) -0.002(2) 0.005(2) -0.001(2) C9 0.037(3) 0.036(3) 0.027(3) 0.005(2) 0.002(2) -0.003(2) C10 0.030(3) 0.031(3) 0.026(2) 0.002(2) 0.008(2) -0.004(2) C11 0.025(2) 0.030(3) 0.019(2) -0.004(2) 0.0033(19) -0.003(2) C12 0.025(2) 0.035(3) 0.022(2) -0.005(2) 0.003(2) 0.001(2) C13 0.017(2) 0.028(3) 0.022(2) -0.003(2) 0.0050(19) -0.0004(19) C14 0.027(2) 0.024(2) 0.019(2) 0.0045(19) 0.0033(19) 0.002(2) C15 0.024(2) 0.022(3) 0.028(2) 0.002(2) 0.010(2) -0.0008(19) C16 0.021(2) 0.031(3) 0.020(2) -0.002(2) 0.0053(19) 0.0003(19) C17 0.028(2) 0.029(3) 0.020(2) 0.000(2) 0.009(2) 0.004(2) C18 0.026(2) 0.028(3) 0.020(2) -0.001(2) 0.006(2) 0.003(2) C19 0.030(3) 0.029(3) 0.023(2) 0.000(2) 0.004(2) -0.002(2) C20 0.029(3) 0.024(3) 0.022(2) -0.006(2) 0.002(2) -0.006(2) C21 0.033(3) 0.025(3) 0.025(3) -0.003(2) 0.002(2) 0.001(2) C22 0.038(3) 0.029(3) 0.018(2) 0.000(2) 0.003(2) -0.006(2) C23 0.029(2) 0.026(3) 0.020(2) -0.004(2) 0.005(2) -0.005(2) C24 0.032(3) 0.023(3) 0.025(2) 0.000(2) 0.004(2) 0.002(2) C25 0.035(3) 0.029(3) 0.025(3) 0.001(2) 0.006(2) -0.001(2) C26 0.031(3) 0.037(3) 0.027(3) 0.000(2) 0.004(2) -0.002(2) C27 0.023(2) 0.029(3) 0.027(2) 0.000(2) 0.008(2) 0.000(2) C28 0.030(3) 0.042(3) 0.028(3) 0.004(2) 0.005(2) 0.002(2) C29 0.035(3) 0.033(3) 0.032(3) -0.001(2) 0.011(2) 0.000(2) C30 0.031(3) 0.032(3) 0.033(3) -0.010(2) 0.013(2) -0.004(2) C31 0.031(3) 0.040(3) 0.024(2) 0.004(2) 0.006(2) -0.002(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 N1 C1 1.348(5) . ? N1 C5 1.358(6) . ? N2 C7 1.356(5) . ? N2 C11 1.361(5) . ? N3 C13 1.407(6) . ? N3 C12 1.452(6) . ? N3 C6 1.461(6) . ? N4 C23 1.387(5) . ? N4 C26 1.447(6) . ? N5 C27 1.337(6) . ? N5 C31 1.370(6) . ? C1 C2 1.387(7) . ? C2 C3 1.387(7) . ? C3 C4 1.387(6) . ? C4 C5 1.387(6) . ? C5 C6 1.521(6) . ? C7 C8 1.374(6) . ? C8 C9 1.393(6) . ? C9 C10 1.388(6) . ? C10 C11 1.378(6) . ? C11 C12 1.524(6) . ? C13 C18 1.406(6) . ? C13 C14 1.411(6) . ? C14 C15 1.393(6) . ? C15 C16 1.391(6) . ? C16 C17 1.398(6) . ? C16 C19 1.523(6) . ? C17 C18 1.391(6) . ? C19 C20 1.527(6) . ? C20 C21 1.391(6) . ? C20 C25 1.411(6) . ? C21 C22 1.398(6) . ? C22 C23 1.390(6) . ? C23 C24 1.425(6) . ? C24 C25 1.389(6) . ? C26 C27 1.511(6) . ? C27 C28 1.397(6) . ? C28 C29 1.389(7) . ? C29 C30 1.397(7) . ? C30 C31 1.376(6) . ? 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 C5 118.5(4) . . ? C7 N2 C11 120.6(4) . . ? C13 N3 C12 119.2(4) . . ? C13 N3 C6 121.1(4) . . ? C12 N3 C6 119.6(4) . . ? C23 N4 C26 125.0(4) . . ? C27 N5 C31 124.0(4) . . ? N1 C1 C2 122.4(4) . . ? C3 C2 C1 119.0(4) . . ? C4 C3 C2 118.9(4) . . ? C3 C4 C5 119.4(4) . . ? N1 C5 C4 121.7(4) . . ? N1 C5 C6 116.0(4) . . ? C4 C5 C6 122.2(4) . . ? N3 C6 C5 115.4(3) . . ? N2 C7 C8 121.4(4) . . ? C7 C8 C9 118.6(4) . . ? C10 C9 C8 119.6(4) . . ? C11 C10 C9 120.0(4) . . ? N2 C11 C10 119.7(4) . . ? N2 C11 C12 116.5(4) . . ? C10 C11 C12 123.7(4) . . ? N3 C12 C11 115.0(3) . . ? N3 C13 C18 120.9(4) . . ? N3 C13 C14 121.5(4) . . ? C18 C13 C14 117.5(4) . . ? C15 C14 C13 120.7(4) . . ? C16 C15 C14 121.9(4) . . ? C15 C16 C17 117.0(4) . . ? C15 C16 C19 121.7(4) . . ? C17 C16 C19 121.1(4) . . ? C18 C17 C16 122.3(4) . . ? C17 C18 C13 120.4(4) . . ? C16 C19 C20 110.3(4) . . ? C21 C20 C25 117.9(4) . . ? C21 C20 C19 121.5(4) . . ? C25 C20 C19 120.3(4) . . ? C20 C21 C22 122.0(4) . . ? C23 C22 C21 120.3(4) . . ? N4 C23 C22 124.2(4) . . ? N4 C23 C24 117.4(4) . . ? C22 C23 C24 118.3(4) . . ? C25 C24 C23 120.7(4) . . ? C24 C25 C20 120.7(4) . . ? N4 C26 C27 113.9(4) . . ? N5 C27 C28 117.9(4) . . ? N5 C27 C26 119.2(4) . . ? C28 C27 C26 122.9(4) . . ? C29 C28 C27 120.0(5) . . ? C28 C29 C30 120.0(5) . . ? C31 C30 C29 119.1(5) . . ? N5 C31 C30 119.0(5) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.401 _refine_diff_density_min -0.365 _refine_diff_density_rms 0.069