# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Kevin M. Smith' _publ_contact_author_address ; Department of Chemistry Louisiana State University Choppin Hall Baton Rouge LA 70803 UNITED STATES OF AMERICA ; _publ_contact_author_email KMSMITH@LSU.EDU _publ_section_title ; b-Bilene to a,c-biladiene transformation during synthesis of isoporphyrins and porphyrins ; loop_ _publ_author_name 'K. Smith' 'Frank R. Fronczek' 'Celinah Mwakwari' # Attachment 'Revised5a.CIF' data_Bilene5a _database_code_depnum_ccdc_archive 'CCDC 642291' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_compound_source 'local laboratory' _chemical_formula_moiety 'C37 H51 N4 O4 1+, Cl 1-, 2(C H2 Cl2)' _chemical_formula_sum 'C39 H55 Cl5 N4 O4' _chemical_formula_weight 821.12 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' Cl Cl 0.1484 0.1585 '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' _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_cell_setting Monoclinic 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 18.373(3) _cell_length_b 14.349(3) _cell_length_c 19.252(4) _cell_angle_alpha 90 _cell_angle_beta 116.763(11) _cell_angle_gamma 90 _cell_volume 4531.8(15) _cell_formula_units_Z 4 _cell_measurement_temperature 110 _cell_measurement_reflns_used 10505 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 28.7 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.204 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1736 _exptl_absorpt_coefficient_mu 0.360 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.928 _exptl_absorpt_correction_T_max 0.969 _exptl_absorpt_process_details 'Denzo and Scalepack (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110 _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 'Nonius KappaCCD (with Oxford Cryostream)' _diffrn_measurement_method ' \w scans with \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <2 _diffrn_reflns_number 38008 _diffrn_reflns_av_R_equivalents 0.039 _diffrn_reflns_av_sigmaI/netI 0.0734 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 28.7 _reflns_number_total 11512 _reflns_number_gt 7014 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Nonius, 2000)' _computing_cell_refinement 'Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0717P)^2^] 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 11512 _refine_ls_number_parameters 455 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.093 _refine_ls_R_factor_gt 0.052 _refine_ls_wR_factor_ref 0.143 _refine_ls_wR_factor_gt 0.130 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.004 _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 0.40029(3) 0.57547(3) 0.25425(2) 0.02509(12) Uani 1 1 d . . . O1 O 0.72082(7) 0.50284(9) 0.25149(7) 0.0256(3) Uani 1 1 d . . . O2 O 0.58649(7) 0.47858(9) 0.21747(7) 0.0245(3) Uani 1 1 d . . . O3 O 0.02974(8) 0.59390(10) 0.11646(7) 0.0314(3) Uani 1 1 d . . . O4 O 0.15724(8) 0.63944(10) 0.14067(8) 0.0334(3) Uani 1 1 d . . . N1 N 0.57632(8) 0.65843(10) 0.26651(8) 0.0190(3) Uani 1 1 d . . . H1N H 0.5292 0.6292 0.2472 0.023 Uiso 1 1 calc R . . N2 N 0.48670(9) 0.72079(10) 0.39033(8) 0.0210(3) Uani 1 1 d . . . H2N H 0.4627 0.6746 0.3580 0.025 Uiso 1 1 calc R . . N3 N 0.39920(9) 0.53388(11) 0.41338(8) 0.0226(3) Uani 1 1 d . . . H3N H 0.4078 0.5514 0.3739 0.027 Uiso 1 1 calc R . . N4 N 0.22246(9) 0.49526(11) 0.24651(8) 0.0246(3) Uani 1 1 d . . . H4N H 0.2599 0.5312 0.2438 0.030 Uiso 1 1 calc R . . C1 C 0.64723(11) 0.52746(13) 0.24447(9) 0.0207(4) Uani 1 1 d . . . C2 C 0.64844(10) 0.62131(13) 0.27310(9) 0.0198(4) Uani 1 1 d . . . C3 C 0.70861(11) 0.68871(13) 0.30649(10) 0.0223(4) Uani 1 1 d . . . C4 C 0.67057(11) 0.76806(13) 0.32029(9) 0.0210(4) Uani 1 1 d . . . C5 C 0.58932(11) 0.74726(13) 0.29446(9) 0.0192(4) Uani 1 1 d . . . C6 C 0.52208(11) 0.80480(13) 0.29705(9) 0.0216(4) Uani 1 1 d . . . H6A H 0.4691 0.7844 0.2549 0.026 Uiso 1 1 calc R . . H6B H 0.5301 0.8710 0.2878 0.026 Uiso 1 1 calc R . . C7 C 0.52003(10) 0.79593(12) 0.37413(10) 0.0201(4) Uani 1 1 d . . . C8 C 0.55260(11) 0.85478(13) 0.43935(10) 0.0227(4) Uani 1 1 d . . . C9 C 0.53851(11) 0.81201(13) 0.49682(10) 0.0240(4) Uani 1 1 d . . . C10 C 0.49582(11) 0.72709(13) 0.46592(9) 0.0217(4) Uani 1 1 d . . . C11 C 0.46792(11) 0.66533(13) 0.50377(10) 0.0230(4) Uani 1 1 d . . . H11 H 0.4816 0.6838 0.5556 0.028 Uiso 1 1 calc R . . C12 C 0.42460(11) 0.58280(13) 0.48302(10) 0.0219(4) Uani 1 1 d . . . C13 C 0.39765(11) 0.52945(14) 0.52963(10) 0.0253(4) Uani 1 1 d . . . C14 C 0.35708(11) 0.45117(14) 0.48740(10) 0.0250(4) Uani 1 1 d . . . C15 C 0.35969(11) 0.45604(13) 0.41557(10) 0.0229(4) Uani 1 1 d . . . C16 C 0.32380(11) 0.39167(14) 0.34696(11) 0.0265(4) Uani 1 1 d . . . H16A H 0.3242 0.3271 0.3653 0.032 Uiso 1 1 calc R . . H16B H 0.3575 0.3933 0.3188 0.032 Uiso 1 1 calc R . . C17 C 0.23776(11) 0.41937(13) 0.29255(10) 0.0254(4) Uani 1 1 d . . . C18 C 0.16375(12) 0.38209(15) 0.28140(11) 0.0329(5) Uani 1 1 d . . . C19 C 0.10134(12) 0.43867(15) 0.22603(11) 0.0317(5) Uani 1 1 d . . . C20 C 0.13930(11) 0.50795(14) 0.20432(10) 0.0264(4) Uani 1 1 d . . . C21 C 0.11081(11) 0.58687(14) 0.15113(10) 0.0270(4) Uani 1 1 d . . . C22 C 0.79696(12) 0.68122(15) 0.32653(13) 0.0347(5) Uani 1 1 d . . . H22A H 0.8267 0.6543 0.3786 0.052 Uiso 1 1 calc R . . H22B H 0.8187 0.7434 0.3256 0.052 Uiso 1 1 calc R . . H22C H 0.8035 0.6411 0.2885 0.052 Uiso 1 1 calc R . . C23 C 0.71127(12) 0.85712(14) 0.35881(11) 0.0290(4) Uani 1 1 d . . . H23A H 0.6746 0.9096 0.3339 0.043 Uiso 1 1 calc R . . H23B H 0.7616 0.8651 0.3536 0.043 Uiso 1 1 calc R . . H23C H 0.7243 0.8549 0.4141 0.043 Uiso 1 1 calc R . . C24 C 0.59230(12) 0.94745(14) 0.44516(11) 0.0303(5) Uani 1 1 d . . . H24A H 0.5744 0.9910 0.4736 0.045 Uiso 1 1 calc R . . H24B H 0.5769 0.9717 0.3928 0.045 Uiso 1 1 calc R . . H24C H 0.6516 0.9403 0.4729 0.045 Uiso 1 1 calc R . . C25 C 0.56374(13) 0.84864(14) 0.57742(10) 0.0314(5) Uani 1 1 d . . . H25A H 0.6234 0.8495 0.6061 0.047 Uiso 1 1 calc R . . H25B H 0.5417 0.8083 0.6045 0.047 Uiso 1 1 calc R . . H25C H 0.5426 0.9120 0.5744 0.047 Uiso 1 1 calc R . . C26 C 0.40990(12) 0.55468(15) 0.60965(10) 0.0315(5) Uani 1 1 d . . . H26A H 0.3568 0.5648 0.6089 0.047 Uiso 0.50 1 calc PR . . H26B H 0.4424 0.6118 0.6267 0.047 Uiso 0.50 1 calc PR . . H26C H 0.4385 0.5039 0.6457 0.047 Uiso 0.50 1 calc PR . . H26D H 0.4683 0.5555 0.6453 0.047 Uiso 0.50 1 calc PR . . H26E H 0.3827 0.5086 0.6275 0.047 Uiso 0.50 1 calc PR . . H26F H 0.3867 0.6165 0.6085 0.047 Uiso 0.50 1 calc PR . . C27 C 0.31725(13) 0.37562(15) 0.51172(11) 0.0319(5) Uani 1 1 d . . . H27A H 0.3364 0.3785 0.5681 0.048 Uiso 1 1 calc R . . H27B H 0.3312 0.3149 0.4978 0.048 Uiso 1 1 calc R . . H27C H 0.2580 0.3840 0.4852 0.048 Uiso 1 1 calc R . . C28 C 0.15102(14) 0.29849(17) 0.32126(13) 0.0449(6) Uani 1 1 d . . . H28A H 0.2025 0.2644 0.3481 0.067 Uiso 1 1 calc R . . H28B H 0.1099 0.2577 0.2826 0.067 Uiso 1 1 calc R . . H28C H 0.1323 0.3186 0.3592 0.067 Uiso 1 1 calc R . . C29 C 0.01163(13) 0.42348(19) 0.19936(13) 0.0461(6) Uani 1 1 d . . . H29A H -0.0191 0.4754 0.1660 0.069 Uiso 1 1 calc R . . H29B H 0.0008 0.4201 0.2447 0.069 Uiso 1 1 calc R . . H29C H -0.0052 0.3651 0.1700 0.069 Uiso 1 1 calc R . . C30 C 0.73587(12) 0.40911(14) 0.22831(11) 0.0279(4) Uani 1 1 d . . . C31 C 0.82442(12) 0.41676(16) 0.24374(13) 0.0382(5) Uani 1 1 d . . . H31A H 0.8296 0.4657 0.2107 0.057 Uiso 1 1 calc R . . H31B H 0.8423 0.3571 0.2319 0.057 Uiso 1 1 calc R . . H31C H 0.8584 0.4324 0.2986 0.057 Uiso 1 1 calc R . . C32 C 0.68142(13) 0.39223(16) 0.14291(11) 0.0351(5) Uani 1 1 d . . . H32A H 0.6245 0.3893 0.1337 0.053 Uiso 1 1 calc R . . H32B H 0.6965 0.3332 0.1272 0.053 Uiso 1 1 calc R . . H32C H 0.6879 0.4433 0.1124 0.053 Uiso 1 1 calc R . . C33 C 0.72485(13) 0.33599(15) 0.28026(13) 0.0367(5) Uani 1 1 d . . . H33A H 0.7584 0.3525 0.3350 0.055 Uiso 1 1 calc R . . H33B H 0.7416 0.2749 0.2698 0.055 Uiso 1 1 calc R . . H33C H 0.6674 0.3336 0.2695 0.055 Uiso 1 1 calc R . . C34 C -0.01212(12) 0.67058(15) 0.06135(12) 0.0341(5) Uani 1 1 d . . . C35 C -0.10089(12) 0.65400(17) 0.04196(14) 0.0456(6) Uani 1 1 d . . . H35A H -0.1188 0.5943 0.0147 0.068 Uiso 1 1 calc R . . H35B H -0.1344 0.7044 0.0085 0.068 Uiso 1 1 calc R . . H35C H -0.1067 0.6525 0.0901 0.068 Uiso 1 1 calc R . . C36 C 0.00075(15) 0.65864(19) -0.01046(13) 0.0498(6) Uani 1 1 d . . . H36A H 0.0586 0.6668 0.0035 0.075 Uiso 1 1 calc R . . H36B H -0.0314 0.7053 -0.0494 0.075 Uiso 1 1 calc R . . H36C H -0.0167 0.5961 -0.0319 0.075 Uiso 1 1 calc R . . C37 C 0.01715(14) 0.76374(17) 0.10114(15) 0.0478(6) Uani 1 1 d . . . H37A H 0.0123 0.7648 0.1498 0.072 Uiso 1 1 calc R . . H37B H -0.0162 0.8137 0.0669 0.072 Uiso 1 1 calc R . . H37C H 0.0743 0.7730 0.1125 0.072 Uiso 1 1 calc R . . C38 C 0.26798(13) 0.64918(18) 0.06487(12) 0.0441(6) Uani 1 1 d . . . H38A H 0.2366 0.6986 0.0753 0.053 Uiso 1 1 calc R . . H38B H 0.2908 0.6073 0.1106 0.053 Uiso 1 1 calc R . . Cl2 Cl 0.20226(4) 0.58541(5) -0.01706(4) 0.05137(18) Uani 1 1 d . . . Cl3 Cl 0.34792(4) 0.70014(5) 0.05260(4) 0.05720(19) 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 Cl1 0.0247(2) 0.0322(3) 0.0191(2) -0.00283(19) 0.01052(17) -0.0060(2) O1 0.0228(7) 0.0242(7) 0.0316(7) -0.0025(6) 0.0138(5) 0.0019(6) O2 0.0231(7) 0.0271(7) 0.0261(6) -0.0017(6) 0.0135(5) -0.0020(6) O3 0.0204(7) 0.0380(9) 0.0311(7) -0.0016(6) 0.0074(6) 0.0016(6) O4 0.0256(7) 0.0384(9) 0.0353(7) 0.0049(7) 0.0128(6) -0.0008(6) N1 0.0172(7) 0.0230(8) 0.0181(7) 0.0004(6) 0.0090(6) -0.0014(6) N2 0.0222(8) 0.0235(8) 0.0171(7) -0.0026(6) 0.0087(6) -0.0010(6) N3 0.0248(8) 0.0268(9) 0.0184(7) 0.0042(6) 0.0116(6) 0.0005(7) N4 0.0201(8) 0.0297(9) 0.0260(8) -0.0003(7) 0.0119(6) -0.0055(7) C1 0.0242(10) 0.0243(10) 0.0165(8) 0.0048(7) 0.0116(7) 0.0029(8) C2 0.0199(9) 0.0248(10) 0.0169(8) 0.0049(7) 0.0104(7) 0.0022(8) C3 0.0208(9) 0.0260(10) 0.0221(9) 0.0039(8) 0.0114(7) -0.0010(8) C4 0.0222(9) 0.0223(10) 0.0175(8) 0.0030(7) 0.0081(7) -0.0010(8) C5 0.0247(9) 0.0202(9) 0.0144(8) 0.0029(7) 0.0103(7) 0.0012(7) C6 0.0232(9) 0.0237(10) 0.0176(8) 0.0030(7) 0.0089(7) 0.0033(8) C7 0.0164(9) 0.0226(10) 0.0212(8) 0.0013(7) 0.0083(7) 0.0030(7) C8 0.0218(9) 0.0238(10) 0.0214(9) -0.0018(8) 0.0088(7) 0.0022(8) C9 0.0216(9) 0.0296(11) 0.0199(9) -0.0041(8) 0.0085(7) 0.0031(8) C10 0.0223(9) 0.0272(10) 0.0168(8) -0.0002(7) 0.0099(7) 0.0040(8) C11 0.0224(9) 0.0297(11) 0.0161(8) 0.0001(8) 0.0080(7) 0.0058(8) C12 0.0213(9) 0.0278(10) 0.0168(8) 0.0041(8) 0.0087(7) 0.0062(8) C13 0.0235(10) 0.0338(11) 0.0198(9) 0.0099(8) 0.0107(7) 0.0104(8) C14 0.0232(10) 0.0297(11) 0.0233(9) 0.0077(8) 0.0115(8) 0.0065(8) C15 0.0203(9) 0.0260(10) 0.0242(9) 0.0043(8) 0.0118(7) 0.0042(8) C16 0.0277(10) 0.0245(10) 0.0307(10) 0.0019(8) 0.0161(8) -0.0003(8) C17 0.0262(10) 0.0294(11) 0.0234(9) -0.0017(8) 0.0134(8) -0.0043(8) C18 0.0318(11) 0.0383(12) 0.0327(11) -0.0043(9) 0.0182(9) -0.0105(10) C19 0.0228(10) 0.0434(13) 0.0286(10) -0.0038(9) 0.0114(8) -0.0084(9) C20 0.0193(9) 0.0346(11) 0.0250(9) -0.0046(8) 0.0098(7) -0.0044(8) C21 0.0200(10) 0.0371(12) 0.0248(9) -0.0073(9) 0.0108(8) -0.0038(9) C22 0.0261(11) 0.0311(12) 0.0489(13) -0.0018(10) 0.0186(9) -0.0027(9) C23 0.0258(10) 0.0240(11) 0.0362(11) -0.0004(9) 0.0131(8) -0.0006(8) C24 0.0335(11) 0.0269(11) 0.0294(10) -0.0059(8) 0.0132(9) -0.0045(9) C25 0.0372(12) 0.0324(12) 0.0241(9) -0.0063(9) 0.0134(8) -0.0005(9) C26 0.0359(12) 0.0405(12) 0.0218(9) 0.0067(9) 0.0163(9) 0.0027(10) C27 0.0329(11) 0.0354(12) 0.0303(10) 0.0087(9) 0.0169(9) 0.0024(9) C28 0.0418(13) 0.0508(15) 0.0433(13) 0.0065(11) 0.0201(10) -0.0141(11) C29 0.0269(12) 0.0674(17) 0.0426(13) 0.0012(12) 0.0142(10) -0.0146(11) C30 0.0286(11) 0.0264(11) 0.0319(10) -0.0013(8) 0.0166(9) 0.0051(8) C31 0.0288(11) 0.0399(13) 0.0493(13) -0.0028(10) 0.0205(10) 0.0076(10) C32 0.0354(12) 0.0390(12) 0.0340(11) -0.0054(10) 0.0185(9) 0.0052(10) C33 0.0381(12) 0.0290(12) 0.0455(12) 0.0069(10) 0.0210(10) 0.0061(10) C34 0.0261(11) 0.0356(12) 0.0346(11) -0.0017(9) 0.0083(9) 0.0062(9) C35 0.0250(11) 0.0462(14) 0.0526(14) -0.0097(12) 0.0061(10) 0.0007(10) C36 0.0479(14) 0.0592(17) 0.0357(12) 0.0074(12) 0.0129(11) 0.0179(13) C37 0.0317(12) 0.0397(14) 0.0641(15) -0.0108(12) 0.0148(11) 0.0007(10) C38 0.0347(12) 0.0664(17) 0.0342(11) -0.0017(11) 0.0181(10) -0.0128(12) Cl2 0.0368(3) 0.0617(4) 0.0550(4) -0.0181(3) 0.0201(3) -0.0103(3) Cl3 0.0640(4) 0.0607(4) 0.0635(4) -0.0154(3) 0.0434(3) -0.0306(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C1 1.344(2) . ? O1 C30 1.482(2) . ? O2 C1 1.219(2) . ? O3 C21 1.334(2) . ? O3 C34 1.481(2) . ? O4 C21 1.221(2) . ? N1 C5 1.362(2) . ? N1 C2 1.380(2) . ? N1 H1N 0.8800 . ? N2 C7 1.344(2) . ? N2 C10 1.391(2) . ? N2 H2N 0.8800 . ? N3 C15 1.343(2) . ? N3 C12 1.395(2) . ? N3 H3N 0.8800 . ? N4 C17 1.351(2) . ? N4 C20 1.382(2) . ? N4 H4N 0.8800 . ? C1 C2 1.451(3) . ? C2 C3 1.390(3) . ? C3 C4 1.422(3) . ? C3 C22 1.494(3) . ? C4 C5 1.377(2) . ? C4 C23 1.498(3) . ? C5 C6 1.505(2) . ? C6 C7 1.507(2) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.404(2) . ? C8 C9 1.388(3) . ? C8 C24 1.496(3) . ? C9 C10 1.426(3) . ? C9 C25 1.500(2) . ? C10 C11 1.384(3) . ? C11 C12 1.382(3) . ? C11 H11 0.9500 . ? C12 C13 1.427(3) . ? C13 C14 1.390(3) . ? C13 C26 1.498(2) . ? C14 C15 1.407(2) . ? C14 C27 1.496(3) . ? C15 C16 1.499(3) . ? C16 C17 1.504(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.385(3) . ? C18 C19 1.417(3) . ? C18 C28 1.498(3) . ? C19 C20 1.383(3) . ? C19 C29 1.505(3) . ? C20 C21 1.457(3) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C26 H26D 0.9800 . ? C26 H26E 0.9800 . ? C26 H26F 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C32 1.510(3) . ? C30 C31 1.520(3) . ? C30 C33 1.525(3) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C36 1.514(3) . ? C34 C37 1.514(3) . ? C34 C35 1.519(3) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 Cl3 1.749(2) . ? C38 Cl2 1.751(2) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? 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 O1 C30 121.61(14) . . ? C21 O3 C34 121.16(15) . . ? C5 N1 C2 109.54(14) . . ? C5 N1 H1N 125.2 . . ? C2 N1 H1N 125.2 . . ? C7 N2 C10 109.74(15) . . ? C7 N2 H2N 125.1 . . ? C10 N2 H2N 125.1 . . ? C15 N3 C12 109.88(15) . . ? C15 N3 H3N 125.1 . . ? C12 N3 H3N 125.1 . . ? C17 N4 C20 109.89(15) . . ? C17 N4 H4N 125.1 . . ? C20 N4 H4N 125.1 . . ? O2 C1 O1 125.31(17) . . ? O2 C1 C2 123.40(16) . . ? O1 C1 C2 111.28(15) . . ? N1 C2 C3 107.76(16) . . ? N1 C2 C1 118.25(16) . . ? C3 C2 C1 133.98(17) . . ? C2 C3 C4 106.74(15) . . ? C2 C3 C22 127.96(17) . . ? C4 C3 C22 125.29(16) . . ? C5 C4 C3 107.64(16) . . ? C5 C4 C23 125.60(17) . . ? C3 C4 C23 126.72(16) . . ? N1 C5 C4 108.32(15) . . ? N1 C5 C6 121.72(15) . . ? C4 C5 C6 129.91(17) . . ? C5 C6 C7 111.80(14) . . ? C5 C6 H6A 109.3 . . ? C7 C6 H6A 109.3 . . ? C5 C6 H6B 109.3 . . ? C7 C6 H6B 109.3 . . ? H6A C6 H6B 107.9 . . ? N2 C7 C8 109.28(15) . . ? N2 C7 C6 120.82(15) . . ? C8 C7 C6 129.82(17) . . ? C9 C8 C7 106.83(16) . . ? C9 C8 C24 126.38(17) . . ? C7 C8 C24 126.76(16) . . ? C8 C9 C10 108.08(15) . . ? C8 C9 C25 126.01(18) . . ? C10 C9 C25 125.92(17) . . ? C11 C10 N2 127.63(17) . . ? C11 C10 C9 126.29(16) . . ? N2 C10 C9 106.06(15) . . ? C12 C11 C10 134.29(17) . . ? C12 C11 H11 112.9 . . ? C10 C11 H11 112.9 . . ? C11 C12 N3 127.53(16) . . ? C11 C12 C13 126.57(17) . . ? N3 C12 C13 105.89(16) . . ? C14 C13 C12 108.19(16) . . ? C14 C13 C26 126.13(17) . . ? C12 C13 C26 125.67(18) . . ? C13 C14 C15 106.75(16) . . ? C13 C14 C27 127.69(16) . . ? C15 C14 C27 125.56(18) . . ? N3 C15 C14 109.29(16) . . ? N3 C15 C16 120.94(16) . . ? C14 C15 C16 129.73(17) . . ? C15 C16 C17 110.98(16) . . ? C15 C16 H16A 109.4 . . ? C17 C16 H16A 109.4 . . ? C15 C16 H16B 109.4 . . ? C17 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? N4 C17 C18 108.05(17) . . ? N4 C17 C16 120.85(16) . . ? C18 C17 C16 131.02(18) . . ? C17 C18 C19 107.49(18) . . ? C17 C18 C28 126.8(2) . . ? C19 C18 C28 125.73(19) . . ? C20 C19 C18 106.97(17) . . ? C20 C19 C29 128.68(19) . . ? C18 C19 C29 124.35(19) . . ? N4 C20 C19 107.59(17) . . ? N4 C20 C21 117.89(16) . . ? C19 C20 C21 134.50(18) . . ? O4 C21 O3 125.19(18) . . ? O4 C21 C20 122.64(17) . . ? O3 C21 C20 112.17(16) . . ? C3 C22 H22A 109.5 . . ? C3 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C3 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C4 C23 H23A 109.5 . . ? C4 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C4 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C8 C24 H24A 109.5 . . ? C8 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C8 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C9 C25 H25A 109.5 . . ? C9 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C9 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C13 C26 H26A 109.5 . . ? C13 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C13 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C13 C26 H26D 109.5 . . ? H26A C26 H26D 141.1 . . ? H26B C26 H26D 56.3 . . ? H26C C26 H26D 56.3 . . ? C13 C26 H26E 109.5 . . ? H26A C26 H26E 56.3 . . ? H26B C26 H26E 141.1 . . ? H26C C26 H26E 56.3 . . ? H26D C26 H26E 109.5 . . ? C13 C26 H26F 109.5 . . ? H26A C26 H26F 56.3 . . ? H26B C26 H26F 56.3 . . ? H26C C26 H26F 141.1 . . ? H26D C26 H26F 109.5 . . ? H26E C26 H26F 109.5 . . ? C14 C27 H27A 109.5 . . ? C14 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C14 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C18 C28 H28A 109.5 . . ? C18 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C18 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C19 C29 H29A 109.5 . . ? C19 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C19 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O1 C30 C32 110.57(15) . . ? O1 C30 C31 101.78(15) . . ? C32 C30 C31 110.50(16) . . ? O1 C30 C33 109.21(15) . . ? C32 C30 C33 112.66(18) . . ? C31 C30 C33 111.59(17) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O3 C34 C36 109.02(17) . . ? O3 C34 C37 110.00(16) . . ? C36 C34 C37 113.3(2) . . ? O3 C34 C35 102.33(17) . . ? C36 C34 C35 110.48(18) . . ? C37 C34 C35 111.10(18) . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C34 C37 H37A 109.5 . . ? C34 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C34 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? Cl3 C38 Cl2 112.15(12) . . ? Cl3 C38 H38A 109.2 . . ? Cl2 C38 H38A 109.2 . . ? Cl3 C38 H38B 109.2 . . ? Cl2 C38 H38B 109.2 . . ? H38A C38 H38B 107.9 . . ? 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 C30 O1 C1 O2 -2.0(2) . . . . ? C30 O1 C1 C2 178.26(14) . . . . ? C5 N1 C2 C3 0.24(18) . . . . ? C5 N1 C2 C1 -178.38(14) . . . . ? O2 C1 C2 N1 -2.7(2) . . . . ? O1 C1 C2 N1 177.03(13) . . . . ? O2 C1 C2 C3 179.11(18) . . . . ? O1 C1 C2 C3 -1.1(3) . . . . ? N1 C2 C3 C4 0.25(18) . . . . ? C1 C2 C3 C4 178.57(17) . . . . ? N1 C2 C3 C22 178.98(17) . . . . ? C1 C2 C3 C22 -2.7(3) . . . . ? C2 C3 C4 C5 -0.65(19) . . . . ? C22 C3 C4 C5 -179.41(16) . . . . ? C2 C3 C4 C23 177.06(16) . . . . ? C22 C3 C4 C23 -1.7(3) . . . . ? C2 N1 C5 C4 -0.66(18) . . . . ? C2 N1 C5 C6 -178.17(14) . . . . ? C3 C4 C5 N1 0.80(18) . . . . ? C23 C4 C5 N1 -176.94(16) . . . . ? C3 C4 C5 C6 178.05(16) . . . . ? C23 C4 C5 C6 0.3(3) . . . . ? N1 C5 C6 C7 92.70(19) . . . . ? C4 C5 C6 C7 -84.2(2) . . . . ? C10 N2 C7 C8 0.0(2) . . . . ? C10 N2 C7 C6 177.15(15) . . . . ? C5 C6 C7 N2 -78.7(2) . . . . ? C5 C6 C7 C8 97.7(2) . . . . ? N2 C7 C8 C9 0.6(2) . . . . ? C6 C7 C8 C9 -176.22(17) . . . . ? N2 C7 C8 C24 -177.48(17) . . . . ? C6 C7 C8 C24 5.7(3) . . . . ? C7 C8 C9 C10 -0.9(2) . . . . ? C24 C8 C9 C10 177.13(17) . . . . ? C7 C8 C9 C25 179.08(17) . . . . ? C24 C8 C9 C25 -2.9(3) . . . . ? C7 N2 C10 C11 178.03(18) . . . . ? C7 N2 C10 C9 -0.60(19) . . . . ? C8 C9 C10 C11 -177.71(17) . . . . ? C25 C9 C10 C11 2.3(3) . . . . ? C8 C9 C10 N2 0.9(2) . . . . ? C25 C9 C10 N2 -179.06(17) . . . . ? N2 C10 C11 C12 -0.3(3) . . . . ? C9 C10 C11 C12 178.04(19) . . . . ? C10 C11 C12 N3 3.9(3) . . . . ? C10 C11 C12 C13 -177.07(19) . . . . ? C15 N3 C12 C11 179.08(18) . . . . ? C15 N3 C12 C13 -0.13(19) . . . . ? C11 C12 C13 C14 -179.44(17) . . . . ? N3 C12 C13 C14 -0.2(2) . . . . ? C11 C12 C13 C26 1.5(3) . . . . ? N3 C12 C13 C26 -179.25(16) . . . . ? C12 C13 C14 C15 0.5(2) . . . . ? C26 C13 C14 C15 179.49(17) . . . . ? C12 C13 C14 C27 -179.12(18) . . . . ? C26 C13 C14 C27 -0.1(3) . . . . ? C12 N3 C15 C14 0.4(2) . . . . ? C12 N3 C15 C16 178.32(16) . . . . ? C13 C14 C15 N3 -0.6(2) . . . . ? C27 C14 C15 N3 179.04(17) . . . . ? C13 C14 C15 C16 -178.20(18) . . . . ? C27 C14 C15 C16 1.4(3) . . . . ? N3 C15 C16 C17 -89.1(2) . . . . ? C14 C15 C16 C17 88.3(2) . . . . ? C20 N4 C17 C18 -0.8(2) . . . . ? C20 N4 C17 C16 -177.77(16) . . . . ? C15 C16 C17 N4 73.8(2) . . . . ? C15 C16 C17 C18 -102.4(2) . . . . ? N4 C17 C18 C19 0.0(2) . . . . ? C16 C17 C18 C19 176.53(19) . . . . ? N4 C17 C18 C28 -179.0(2) . . . . ? C16 C17 C18 C28 -2.4(3) . . . . ? C17 C18 C19 C20 0.8(2) . . . . ? C28 C18 C19 C20 179.8(2) . . . . ? C17 C18 C19 C29 -178.18(19) . . . . ? C28 C18 C19 C29 0.7(3) . . . . ? C17 N4 C20 C19 1.3(2) . . . . ? C17 N4 C20 C21 179.95(16) . . . . ? C18 C19 C20 N4 -1.3(2) . . . . ? C29 C19 C20 N4 177.7(2) . . . . ? C18 C19 C20 C21 -179.6(2) . . . . ? C29 C19 C20 C21 -0.6(4) . . . . ? C34 O3 C21 O4 -1.4(3) . . . . ? C34 O3 C21 C20 178.60(15) . . . . ? N4 C20 C21 O4 2.7(3) . . . . ? C19 C20 C21 O4 -179.2(2) . . . . ? N4 C20 C21 O3 -177.30(15) . . . . ? C19 C20 C21 O3 0.9(3) . . . . ? C1 O1 C30 C32 60.3(2) . . . . ? C1 O1 C30 C31 177.74(14) . . . . ? C1 O1 C30 C33 -64.2(2) . . . . ? C21 O3 C34 C36 66.8(2) . . . . ? C21 O3 C34 C37 -58.0(2) . . . . ? C21 O3 C34 C35 -176.19(16) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1N Cl1 0.88 2.55 3.3533(16) 151.9 . N2 H2N Cl1 0.88 2.29 3.1601(16) 167.9 . N3 H3N Cl1 0.88 2.27 3.1301(16) 165.3 . N4 H4N Cl1 0.88 2.58 3.4036(16) 157.2 . _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 28.7 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.43 _refine_diff_density_min -0.46 _refine_diff_density_rms 0.058 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 0.000 395.3 21.9 2 0.234 0.096 0.391 12.0 -0.6 3 1.000 0.500 0.500 395.3 21.7 4 0.234 0.404 0.891 12.0 -0.6 5 0.766 0.596 0.109 12.0 -0.6 6 0.766 0.904 0.609 12.0 -0.6 _platon_squeeze_details ; Disordered solvent regions with volume 849.7 \%A removed using SQUEEZE (Spek, 1990). The total electron count amounts to 44 electrons per cell, approximately equivalent to one DCM molecule. ; # END OF CIF for Bilene5a data_Compound15 _database_code_depnum_ccdc_archive 'CCDC 642292' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_compound_source 'local laboratory' _chemical_formula_moiety 'C62 H72 N8 O4 Zn2' _chemical_formula_sum 'C62 H72 N8 O4 Zn2' _chemical_formula_weight 1124.02 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' _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' _symmetry_cell_setting Triclinic loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.393(3) _cell_length_b 14.837(3) _cell_length_c 16.417(4) _cell_angle_alpha 79.587(8) _cell_angle_beta 75.834(8) _cell_angle_gamma 76.550(9) _cell_volume 2822.0(11) _cell_formula_units_Z 2 _cell_measurement_temperature 90 _cell_measurement_reflns_used 9726 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 25.0 _exptl_crystal_description plate _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.323 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1184 _exptl_absorpt_coefficient_mu 0.905 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.792 _exptl_absorpt_correction_T_max 0.915 _exptl_absorpt_process_details 'Denzo and Scalepack (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90 _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 'KappaCCD (with Oxford Cryostream)' _diffrn_measurement_method ' \w scans with \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <2 _diffrn_reflns_number 33894 _diffrn_reflns_av_R_equivalents 0.037 _diffrn_reflns_av_sigmaI/netI 0.0521 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 25.3 _reflns_number_total 10228 _reflns_number_gt 7797 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Nonius, 2000)' _computing_cell_refinement 'Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0507P)^2^+17.0364P] 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 10228 _refine_ls_number_parameters 705 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.113 _refine_ls_R_factor_gt 0.087 _refine_ls_wR_factor_ref 0.217 _refine_ls_wR_factor_gt 0.205 _refine_ls_goodness_of_fit_ref 1.118 _refine_ls_restrained_S_all 1.118 _refine_ls_shift/su_max 0.005 _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 0.49553(6) 0.55021(5) 0.72891(4) 0.0344(2) Uani 1 1 d . . . Zn2 Zn 0.36707(6) 0.85184(6) 0.72092(5) 0.0407(2) Uani 1 1 d . . . O1 O -0.0165(5) 0.9072(6) 0.7528(4) 0.089(2) Uani 1 1 d . . . O2 O -0.0909(8) 1.0430(11) 0.8142(8) 0.199(7) Uani 1 1 d . . . O3 O 0.8584(6) 0.5205(5) 0.7379(5) 0.088(2) Uani 1 1 d . . . O4 O 0.9314(8) 0.3791(7) 0.7839(9) 0.166(5) Uani 1 1 d . . . N1 N 0.4101(5) 0.4643(4) 0.8131(4) 0.0483(15) Uani 1 1 d . . . N2 N 0.5148(4) 0.6258(4) 0.8104(3) 0.0383(12) Uani 1 1 d . . . N3 N 0.5045(4) 0.8128(4) 0.6346(4) 0.0386(12) Uani 1 1 d . . . N4 N 0.2701(4) 0.9317(4) 0.6439(4) 0.0437(13) Uani 1 1 d . . . N5 N 0.4006(5) 0.9355(4) 0.7893(4) 0.0526(15) Uani 1 1 d . . . N6 N 0.2700(5) 0.7818(4) 0.8148(4) 0.0444(14) Uani 1 1 d . . . N7 N 0.3994(4) 0.6233(4) 0.6498(3) 0.0356(12) Uani 1 1 d . . . N8 N 0.6324(4) 0.5062(4) 0.6435(3) 0.0353(12) Uani 1 1 d . . . C1 C 0.3625(6) 0.3959(6) 0.8023(6) 0.062(2) Uani 1 1 d . . . H1 H 0.3783 0.3700 0.7508 0.075 Uiso 1 1 calc R . . C2 C 0.2872(8) 0.3673(7) 0.8754(8) 0.085(3) Uani 1 1 d . . . C3 C 0.2893(7) 0.4204(8) 0.9355(7) 0.084(3) Uani 1 1 d . . . C4 C 0.3663(6) 0.4825(6) 0.8961(5) 0.057(2) Uani 1 1 d . . . C5 C 0.3905(6) 0.5510(6) 0.9305(5) 0.058(2) Uani 1 1 d . . . H5 H 0.3560 0.5533 0.9887 0.070 Uiso 1 1 calc R . . C6 C 0.4564(6) 0.6174(6) 0.8954(4) 0.0503(19) Uani 1 1 d . . . C7 C 0.4790(8) 0.6854(6) 0.9356(6) 0.065(2) Uani 1 1 d . . . C8 C 0.5516(8) 0.7336(6) 0.8763(6) 0.068(3) Uani 1 1 d . . . C9 C 0.5703(6) 0.6948(5) 0.7996(5) 0.0456(17) Uani 1 1 d . . . C10 C 0.6511(6) 0.7183(5) 0.7174(6) 0.058(2) Uani 1 1 d . . . H10A H 0.6957 0.7604 0.7286 0.069 Uiso 1 1 calc R . . H10B H 0.7052 0.6596 0.7042 0.069 Uiso 1 1 calc R . . C11 C 0.6092(5) 0.7623(4) 0.6381(5) 0.0432(16) Uani 1 1 d . . . C12 C 0.6804(6) 0.7608(5) 0.5565(5) 0.0488(18) Uani 1 1 d . . . C13 C 0.6168(6) 0.8137(5) 0.4997(5) 0.0445(17) Uani 1 1 d . . . C14 C 0.5067(5) 0.8466(4) 0.5487(4) 0.0376(14) Uani 1 1 d . . . C15 C 0.4183(6) 0.9046(4) 0.5159(4) 0.0403(15) Uani 1 1 d . . . H15 H 0.4346 0.9202 0.4560 0.048 Uiso 1 1 calc R . . C16 C 0.3084(6) 0.9441(5) 0.5567(4) 0.0409(15) Uani 1 1 d . . . C17 C 0.2217(6) 1.0046(5) 0.5179(5) 0.0451(16) Uani 1 1 d . . . C18 C 0.1315(6) 1.0292(5) 0.5834(5) 0.0498(18) Uani 1 1 d . . . C19 C 0.1645(6) 0.9837(5) 0.6602(5) 0.0507(18) Uani 1 1 d . . . C20 C 0.1011(7) 0.9977(9) 0.7514(6) 0.086(3) Uani 1 1 d . . . H20 H 0.1455 0.9516 0.7895 0.104 Uiso 1 1 calc R . . C21 C 0.2162(9) 0.2936(9) 0.8875(10) 0.130(6) Uani 1 1 d . . . H21A H 0.2032 0.2653 0.9470 0.196 Uiso 1 1 calc R . . H21B H 0.2564 0.2451 0.8513 0.196 Uiso 1 1 calc R . . H21C H 0.1432 0.3225 0.8721 0.196 Uiso 1 1 calc R . . C22 C 0.2279(9) 0.4196(10) 1.0301(7) 0.127(6) Uani 1 1 d . . . H22A H 0.1646 0.4733 1.0360 0.190 Uiso 1 1 calc R . . H22B H 0.2815 0.4234 1.0638 0.190 Uiso 1 1 calc R . . H22C H 0.1990 0.3616 1.0501 0.190 Uiso 1 1 calc R . . C23 C 0.4318(10) 0.7022(8) 1.0275(6) 0.101(4) Uani 1 1 d . . . H23A H 0.4913 0.6775 1.0601 0.151 Uiso 1 1 calc R . . H23B H 0.3678 0.6705 1.0515 0.151 Uiso 1 1 calc R . . H23C H 0.4061 0.7695 1.0302 0.151 Uiso 1 1 calc R . . C24 C 0.6036(10) 0.8100(7) 0.8886(9) 0.113(5) Uani 1 1 d . . . H24A H 0.6053 0.8575 0.8386 0.170 Uiso 1 1 calc R . . H24B H 0.6812 0.7841 0.8964 0.170 Uiso 1 1 calc R . . H24C H 0.5585 0.8386 0.9387 0.170 Uiso 1 1 calc R . . C25 C 0.8024(6) 0.7127(5) 0.5388(6) 0.059(2) Uani 1 1 d . . . H25A H 0.8323 0.7181 0.4774 0.088 Uiso 1 1 calc R . . H25B H 0.8087 0.6465 0.5622 0.088 Uiso 1 1 calc R . . H25C H 0.8462 0.7419 0.5651 0.088 Uiso 1 1 calc R . . C26 C 0.6538(7) 0.8328(5) 0.4051(5) 0.056(2) Uani 1 1 d . . . H26A H 0.7297 0.7956 0.3869 0.084 Uiso 1 1 calc R . . H26B H 0.6557 0.8994 0.3885 0.084 Uiso 1 1 calc R . . H26C H 0.6001 0.8160 0.3782 0.084 Uiso 1 1 calc R . . C27 C 0.2312(7) 1.0342(5) 0.4245(5) 0.0515(18) Uani 1 1 d . . . H27A H 0.1589 1.0730 0.4142 0.077 Uiso 1 1 calc R . . H27B H 0.2492 0.9787 0.3954 0.077 Uiso 1 1 calc R . . H27C H 0.2916 1.0703 0.4029 0.077 Uiso 1 1 calc R . . C28 C 0.0187(6) 1.0928(6) 0.5781(6) 0.062(2) Uani 1 1 d . . . H28A H -0.0212 1.0664 0.5463 0.092 Uiso 1 1 calc R . . H28B H 0.0309 1.1545 0.5492 0.092 Uiso 1 1 calc R . . H28C H -0.0272 1.0988 0.6354 0.092 Uiso 1 1 calc R . . C29 C 0.1146(8) 1.1034(7) 0.7641(7) 0.091(4) Uani 1 1 d . . . H29A H 0.0817 1.1505 0.7221 0.136 Uiso 1 1 calc R . . H29B H 0.1952 1.1047 0.7564 0.136 Uiso 1 1 calc R . . H29C H 0.0746 1.1171 0.8212 0.136 Uiso 1 1 calc R . . C30 C -0.0126(13) 0.9855(10) 0.7789(9) 0.114(5) Uani 1 1 d . . . C31 C -0.1268(12) 0.8741(14) 0.7807(9) 0.160(7) Uani 1 1 d . . . H31A H -0.1490 0.8671 0.8427 0.240 Uiso 1 1 calc R . . H31B H -0.1180 0.8138 0.7610 0.240 Uiso 1 1 calc R . . H31C H -0.1855 0.9199 0.7567 0.240 Uiso 1 1 calc R . . C32 C 0.4657(7) 1.0007(5) 0.7667(6) 0.061(2) Uani 1 1 d . . . H32 H 0.5137 1.0104 0.7124 0.074 Uiso 1 1 calc R . . C33 C 0.4544(9) 1.0525(6) 0.8327(7) 0.073(3) Uani 1 1 d . . . C34 C 0.3769(9) 1.0172(7) 0.9000(6) 0.074(3) Uani 1 1 d . . . C35 C 0.3441(7) 0.9444(6) 0.8716(5) 0.060(2) Uani 1 1 d . . . C36 C 0.2683(7) 0.8875(6) 0.9174(5) 0.062(2) Uani 1 1 d . . . H36 H 0.2356 0.9003 0.9739 0.075 Uiso 1 1 calc R . . C37 C 0.2332(6) 0.8163(6) 0.8945(5) 0.0542(19) Uani 1 1 d . . . C38 C 0.1514(6) 0.7655(7) 0.9474(5) 0.062(2) Uani 1 1 d . . . C39 C 0.1370(6) 0.7021(6) 0.9002(5) 0.057(2) Uani 1 1 d . . . C40 C 0.2121(5) 0.7162(5) 0.8192(4) 0.0453(17) Uani 1 1 d . . . C41 C 0.2157(5) 0.6603(5) 0.7502(5) 0.0475(17) Uani 1 1 d . . . H41A H 0.2328 0.5936 0.7741 0.057 Uiso 1 1 calc R . . H41B H 0.1375 0.6727 0.7406 0.057 Uiso 1 1 calc R . . C42 C 0.2924(6) 0.6700(5) 0.6650(4) 0.0419(16) Uani 1 1 d . . . C43 C 0.2603(6) 0.7164(5) 0.5872(5) 0.0457(17) Uani 1 1 d . . . C44 C 0.3541(6) 0.6948(5) 0.5231(4) 0.0448(17) Uani 1 1 d . . . C45 C 0.4411(6) 0.6352(4) 0.5631(4) 0.0370(15) Uani 1 1 d . . . C46 C 0.5479(6) 0.5942(5) 0.5235(4) 0.0393(15) Uani 1 1 d . . . H46 H 0.5642 0.6085 0.4635 0.047 Uiso 1 1 calc R . . C47 C 0.6366(6) 0.5347(4) 0.5574(4) 0.0385(15) Uani 1 1 d . . . C48 C 0.7472(6) 0.4962(5) 0.5116(4) 0.0433(16) Uani 1 1 d . . . C49 C 0.8075(6) 0.4448(5) 0.5713(5) 0.0461(17) Uani 1 1 d . . . C50 C 0.7330(5) 0.4529(5) 0.6516(4) 0.0403(15) Uani 1 1 d . . . C51 C 0.7549(6) 0.4079(5) 0.7390(5) 0.0529(19) Uani 1 1 d . . . H51 H 0.6872 0.4364 0.7802 0.063 Uiso 1 1 calc R . . C52 C 0.5173(11) 1.1304(7) 0.8289(8) 0.100(4) Uani 1 1 d . . . H52A H 0.5708 1.1102 0.8668 0.149 Uiso 1 1 calc R . . H52B H 0.4626 1.1863 0.8465 0.149 Uiso 1 1 calc R . . H52C H 0.5590 1.1449 0.7707 0.149 Uiso 1 1 calc R . . C53 C 0.3338(11) 1.0493(8) 0.9871(7) 0.105(4) Uani 1 1 d . . . H53A H 0.3961 1.0347 1.0172 0.158 Uiso 1 1 calc R . . H53B H 0.2728 1.0171 1.0193 0.158 Uiso 1 1 calc R . . H53C H 0.3046 1.1169 0.9807 0.158 Uiso 1 1 calc R . . C54 C 0.0898(8) 0.7787(9) 1.0356(6) 0.092(3) Uani 1 1 d . . . H54A H 0.0127 0.8143 1.0351 0.138 Uiso 1 1 calc R . . H54B H 0.1300 0.8129 1.0602 0.138 Uiso 1 1 calc R . . H54C H 0.0861 0.7176 1.0696 0.138 Uiso 1 1 calc R . . C55 C 0.0622(7) 0.6327(7) 0.9236(6) 0.072(3) Uani 1 1 d . . . H55A H 0.0310 0.6271 0.9848 0.108 Uiso 1 1 calc R . . H55B H 0.1061 0.5719 0.9083 0.108 Uiso 1 1 calc R . . H55C H 0.0000 0.6532 0.8932 0.108 Uiso 1 1 calc R . . C56 C 0.1463(6) 0.7734(6) 0.5799(6) 0.061(2) Uani 1 1 d . . . H56A H 0.1499 0.8071 0.5225 0.092 Uiso 1 1 calc R . . H56B H 0.1226 0.8184 0.6209 0.092 Uiso 1 1 calc R . . H56C H 0.0913 0.7323 0.5915 0.092 Uiso 1 1 calc R . . C57 C 0.3649(7) 0.7248(5) 0.4304(5) 0.055(2) Uani 1 1 d . . . H57A H 0.2926 0.7629 0.4195 0.082 Uiso 1 1 calc R . . H57B H 0.3846 0.6696 0.4008 0.082 Uiso 1 1 calc R . . H57C H 0.4246 0.7617 0.4098 0.082 Uiso 1 1 calc R . . C58 C 0.7869(7) 0.5118(6) 0.4168(5) 0.060(2) Uani 1 1 d . . . H58A H 0.8056 0.5741 0.3996 0.090 Uiso 1 1 calc R . . H58B H 0.7266 0.5072 0.3896 0.090 Uiso 1 1 calc R . . H58C H 0.8545 0.4644 0.3993 0.090 Uiso 1 1 calc R . . C59 C 0.9273(6) 0.3914(6) 0.5541(6) 0.061(2) Uani 1 1 d . . . H59A H 0.9566 0.3941 0.4928 0.092 Uiso 1 1 calc R . . H59B H 0.9295 0.3261 0.5795 0.092 Uiso 1 1 calc R . . H59C H 0.9744 0.4191 0.5788 0.092 Uiso 1 1 calc R . . C60 C 0.7545(9) 0.3009(6) 0.7554(5) 0.075(3) Uani 1 1 d . . . H60A H 0.8175 0.2686 0.7153 0.113 Uiso 1 1 calc R . . H60B H 0.6825 0.2908 0.7476 0.113 Uiso 1 1 calc R . . H60C H 0.7633 0.2763 0.8135 0.113 Uiso 1 1 calc R . . C61 C 0.8525(8) 0.4362(8) 0.7577(6) 0.070(2) Uani 1 1 d . . . C62 C 0.9465(10) 0.5546(9) 0.7577(8) 0.107(4) Uani 1 1 d . . . H62A H 1.0098 0.5025 0.7656 0.160 Uiso 1 1 calc R . . H62B H 0.9171 0.5835 0.8100 0.160 Uiso 1 1 calc R . . H62C H 0.9731 0.6011 0.7112 0.160 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 0.0300(4) 0.0462(4) 0.0308(4) -0.0072(3) -0.0095(3) -0.0103(3) Zn2 0.0318(4) 0.0499(5) 0.0433(5) -0.0079(4) -0.0135(3) -0.0064(3) O1 0.065(4) 0.134(6) 0.070(4) -0.007(4) -0.004(3) -0.042(4) O2 0.087(6) 0.307(16) 0.170(10) -0.132(11) -0.017(6) 0.092(9) O3 0.085(5) 0.087(5) 0.119(6) -0.019(4) -0.051(4) -0.035(4) O4 0.104(7) 0.139(8) 0.270(14) 0.035(9) -0.107(9) -0.031(6) N1 0.029(3) 0.055(4) 0.054(4) -0.001(3) -0.003(3) -0.008(3) N2 0.035(3) 0.050(3) 0.035(3) -0.012(2) -0.013(2) -0.008(2) N3 0.032(3) 0.038(3) 0.049(3) -0.009(2) -0.010(2) -0.010(2) N4 0.031(3) 0.054(3) 0.043(3) -0.003(3) -0.010(2) -0.004(3) N5 0.049(4) 0.057(4) 0.057(4) -0.017(3) -0.021(3) -0.005(3) N6 0.038(3) 0.056(4) 0.041(3) -0.008(3) -0.014(3) -0.005(3) N7 0.033(3) 0.045(3) 0.036(3) -0.007(2) -0.016(2) -0.013(2) N8 0.033(3) 0.044(3) 0.032(3) -0.012(2) -0.008(2) -0.008(2) C1 0.035(4) 0.055(5) 0.098(7) -0.008(4) -0.010(4) -0.017(4) C2 0.044(5) 0.076(7) 0.123(10) 0.011(6) 0.000(5) -0.027(5) C3 0.037(5) 0.092(7) 0.092(8) 0.035(6) 0.007(5) -0.009(5) C4 0.038(4) 0.069(5) 0.050(5) 0.005(4) 0.000(3) -0.003(4) C5 0.049(4) 0.080(6) 0.030(4) 0.005(4) -0.005(3) 0.006(4) C6 0.051(4) 0.070(5) 0.028(4) -0.017(3) -0.016(3) 0.008(4) C7 0.076(6) 0.073(6) 0.054(5) -0.032(4) -0.040(5) 0.016(5) C8 0.078(6) 0.060(5) 0.085(7) -0.034(5) -0.052(5) 0.005(5) C9 0.042(4) 0.049(4) 0.054(4) -0.010(3) -0.028(3) -0.003(3) C10 0.040(4) 0.049(4) 0.096(6) 0.001(4) -0.037(4) -0.015(3) C11 0.031(3) 0.034(4) 0.070(5) -0.014(3) -0.012(3) -0.011(3) C12 0.036(4) 0.036(4) 0.078(5) -0.022(4) -0.004(4) -0.010(3) C13 0.043(4) 0.035(4) 0.058(4) -0.019(3) -0.001(3) -0.015(3) C14 0.040(4) 0.034(3) 0.042(4) -0.010(3) -0.006(3) -0.012(3) C15 0.045(4) 0.038(4) 0.042(4) -0.007(3) -0.009(3) -0.017(3) C16 0.041(4) 0.039(4) 0.046(4) -0.005(3) -0.017(3) -0.008(3) C17 0.048(4) 0.044(4) 0.051(4) 0.000(3) -0.024(3) -0.015(3) C18 0.038(4) 0.049(4) 0.065(5) 0.003(4) -0.022(4) -0.009(3) C19 0.027(3) 0.063(5) 0.057(5) -0.002(4) -0.011(3) -0.002(3) C20 0.040(5) 0.146(10) 0.055(5) 0.005(6) -0.001(4) -0.005(5) C21 0.071(7) 0.101(9) 0.208(16) 0.037(9) -0.019(8) -0.051(7) C22 0.052(6) 0.169(12) 0.098(9) 0.046(8) 0.027(6) 0.005(7) C23 0.117(9) 0.126(9) 0.056(6) -0.052(6) -0.046(6) 0.043(7) C24 0.116(9) 0.081(7) 0.187(13) -0.060(8) -0.110(10) 0.008(6) C25 0.036(4) 0.042(4) 0.100(7) -0.022(4) -0.010(4) -0.009(3) C26 0.060(5) 0.052(4) 0.056(5) -0.021(4) 0.007(4) -0.019(4) C27 0.063(5) 0.042(4) 0.059(5) -0.001(3) -0.032(4) -0.013(3) C28 0.040(4) 0.059(5) 0.086(6) 0.006(4) -0.025(4) -0.010(4) C29 0.068(6) 0.095(7) 0.120(9) -0.079(7) -0.018(6) 0.010(5) C30 0.136(12) 0.110(10) 0.125(11) 0.001(8) -0.065(10) -0.053(9) C31 0.122(11) 0.29(2) 0.108(11) -0.013(12) -0.017(9) -0.129(14) C32 0.060(5) 0.050(5) 0.084(6) -0.013(4) -0.033(5) -0.007(4) C33 0.087(7) 0.061(5) 0.092(7) -0.027(5) -0.040(6) -0.017(5) C34 0.085(7) 0.075(6) 0.077(6) -0.033(5) -0.042(6) -0.002(5) C35 0.061(5) 0.065(5) 0.060(5) -0.017(4) -0.027(4) -0.002(4) C36 0.062(5) 0.082(6) 0.045(5) -0.027(4) -0.019(4) 0.003(5) C37 0.044(4) 0.082(6) 0.040(4) -0.013(4) -0.015(3) -0.007(4) C38 0.041(4) 0.106(7) 0.037(4) -0.007(4) -0.008(3) -0.013(4) C39 0.032(4) 0.087(6) 0.048(4) -0.002(4) -0.007(3) -0.009(4) C40 0.027(3) 0.070(5) 0.036(4) 0.001(3) -0.010(3) -0.008(3) C41 0.026(3) 0.057(4) 0.058(5) -0.005(3) -0.009(3) -0.007(3) C42 0.043(4) 0.050(4) 0.042(4) -0.006(3) -0.019(3) -0.018(3) C43 0.048(4) 0.045(4) 0.056(4) 0.002(3) -0.029(4) -0.019(3) C44 0.057(4) 0.046(4) 0.044(4) -0.002(3) -0.026(4) -0.022(3) C45 0.050(4) 0.040(4) 0.032(3) -0.004(3) -0.018(3) -0.021(3) C46 0.057(4) 0.046(4) 0.025(3) -0.007(3) -0.010(3) -0.026(3) C47 0.047(4) 0.040(4) 0.035(3) -0.016(3) -0.009(3) -0.015(3) C48 0.053(4) 0.042(4) 0.040(4) -0.020(3) 0.004(3) -0.022(3) C49 0.042(4) 0.043(4) 0.057(5) -0.021(3) -0.004(3) -0.011(3) C50 0.037(4) 0.046(4) 0.043(4) -0.013(3) -0.013(3) -0.011(3) C51 0.048(4) 0.059(5) 0.053(5) -0.005(4) -0.023(4) -0.002(4) C52 0.139(10) 0.074(7) 0.117(9) -0.021(6) -0.061(8) -0.041(7) C53 0.141(11) 0.111(9) 0.080(8) -0.045(7) -0.039(7) -0.018(8) C54 0.069(6) 0.150(10) 0.053(6) -0.024(6) 0.007(5) -0.027(7) C55 0.038(4) 0.111(8) 0.063(5) 0.005(5) -0.008(4) -0.021(5) C56 0.047(4) 0.068(5) 0.076(6) 0.012(4) -0.039(4) -0.014(4) C57 0.079(6) 0.053(4) 0.045(4) 0.002(3) -0.033(4) -0.023(4) C58 0.078(6) 0.056(5) 0.046(4) -0.023(4) 0.004(4) -0.021(4) C59 0.046(4) 0.057(5) 0.075(6) -0.028(4) 0.002(4) -0.001(4) C60 0.116(8) 0.068(6) 0.037(4) 0.001(4) -0.024(5) -0.007(5) C61 0.073(6) 0.092(7) 0.053(5) -0.012(5) -0.021(4) -0.021(5) C62 0.119(9) 0.138(11) 0.095(8) -0.046(8) -0.020(7) -0.065(8) _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 N8 1.980(5) . ? Zn1 N2 1.982(5) . ? Zn1 N7 1.982(5) . ? Zn1 N1 1.983(6) . ? Zn2 N3 1.975(5) . ? Zn2 N5 1.986(6) . ? Zn2 N4 1.996(5) . ? Zn2 N6 1.999(6) . ? O1 C30 1.325(14) . ? O1 C31 1.497(13) . ? O2 C30 1.235(17) . ? O3 C61 1.249(11) . ? O3 C62 1.429(11) . ? O4 C61 1.244(12) . ? N1 C1 1.344(10) . ? N1 C4 1.388(10) . ? N2 C9 1.325(9) . ? N2 C6 1.404(9) . ? N3 C11 1.348(8) . ? N3 C14 1.404(8) . ? N4 C19 1.346(8) . ? N4 C16 1.387(9) . ? N5 C32 1.346(10) . ? N5 C35 1.376(10) . ? N6 C40 1.320(9) . ? N6 C37 1.421(9) . ? N7 C42 1.331(8) . ? N7 C45 1.384(8) . ? N8 C50 1.335(8) . ? N8 C47 1.392(8) . ? C1 C2 1.394(13) . ? C1 H1 0.9500 . ? C2 C3 1.377(16) . ? C2 C21 1.515(14) . ? C3 C4 1.439(12) . ? C3 C22 1.551(15) . ? C4 C5 1.369(12) . ? C5 C6 1.382(12) . ? C5 H5 0.9500 . ? C6 C7 1.412(11) . ? C7 C8 1.374(13) . ? C7 C23 1.523(12) . ? C8 C9 1.425(11) . ? C8 C24 1.492(12) . ? C9 C10 1.508(11) . ? C10 C11 1.503(10) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.413(10) . ? C12 C13 1.383(11) . ? C12 C25 1.496(9) . ? C13 C14 1.430(9) . ? C13 C26 1.502(10) . ? C14 C15 1.383(9) . ? C15 C16 1.404(9) . ? C15 H15 0.9500 . ? C16 C17 1.431(9) . ? C17 C18 1.379(10) . ? C17 C27 1.500(10) . ? C18 C19 1.425(10) . ? C18 C28 1.506(10) . ? C19 C20 1.537(12) . ? C20 C30 1.414(16) . ? C20 C29 1.670(15) . ? C20 H20 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.401(12) . ? C32 H32 0.9500 . ? C33 C34 1.387(14) . ? C33 C52 1.522(12) . ? C34 C35 1.424(12) . ? C34 C53 1.519(13) . ? C35 C36 1.397(12) . ? C36 C37 1.374(11) . ? C36 H36 0.9500 . ? C37 C38 1.428(11) . ? C38 C39 1.387(12) . ? C38 C54 1.486(11) . ? C39 C40 1.436(10) . ? C39 C55 1.482(12) . ? C40 C41 1.507(10) . ? C41 C42 1.491(10) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.438(9) . ? C43 C44 1.383(10) . ? C43 C56 1.489(10) . ? C44 C45 1.438(9) . ? C44 C57 1.489(10) . ? C45 C46 1.375(9) . ? C46 C47 1.403(9) . ? C46 H46 0.9500 . ? C47 C48 1.434(9) . ? C48 C49 1.387(10) . ? C48 C58 1.505(10) . ? C49 C50 1.420(9) . ? C49 C59 1.497(10) . ? C50 C51 1.529(10) . ? C51 C61 1.482(11) . ? C51 C60 1.562(11) . ? C51 H51 1.0000 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? 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 N8 Zn1 N2 116.7(2) . . ? N8 Zn1 N7 98.1(2) . . ? N2 Zn1 N7 112.8(2) . . ? N8 Zn1 N1 123.2(2) . . ? N2 Zn1 N1 96.9(2) . . ? N7 Zn1 N1 109.7(2) . . ? N3 Zn2 N5 109.0(2) . . ? N3 Zn2 N4 98.6(2) . . ? N5 Zn2 N4 107.3(2) . . ? N3 Zn2 N6 133.5(2) . . ? N5 Zn2 N6 97.9(3) . . ? N4 Zn2 N6 108.8(2) . . ? C30 O1 C31 116.8(12) . . ? C61 O3 C62 120.2(9) . . ? C1 N1 C4 106.8(7) . . ? C1 N1 Zn1 130.5(6) . . ? C4 N1 Zn1 121.2(5) . . ? C9 N2 C6 106.8(6) . . ? C9 N2 Zn1 131.4(5) . . ? C6 N2 Zn1 121.6(5) . . ? C11 N3 C14 106.2(6) . . ? C11 N3 Zn2 134.0(5) . . ? C14 N3 Zn2 119.6(4) . . ? C19 N4 C16 106.6(6) . . ? C19 N4 Zn2 131.5(5) . . ? C16 N4 Zn2 121.9(4) . . ? C32 N5 C35 106.1(7) . . ? C32 N5 Zn2 130.7(6) . . ? C35 N5 Zn2 122.6(5) . . ? C40 N6 C37 106.1(6) . . ? C40 N6 Zn2 134.7(5) . . ? C37 N6 Zn2 118.1(5) . . ? C42 N7 C45 107.9(5) . . ? C42 N7 Zn1 130.5(4) . . ? C45 N7 Zn1 121.6(4) . . ? C50 N8 C47 107.6(5) . . ? C50 N8 Zn1 131.6(4) . . ? C47 N8 Zn1 120.7(4) . . ? N1 C1 C2 112.1(9) . . ? N1 C1 H1 123.9 . . ? C2 C1 H1 123.9 . . ? C3 C2 C1 106.1(8) . . ? C3 C2 C21 126.3(11) . . ? C1 C2 C21 127.6(12) . . ? C2 C3 C4 107.3(9) . . ? C2 C3 C22 131.2(10) . . ? C4 C3 C22 121.4(12) . . ? C5 C4 N1 124.5(7) . . ? C5 C4 C3 127.8(9) . . ? N1 C4 C3 107.7(9) . . ? C4 C5 C6 131.3(7) . . ? C4 C5 H5 114.4 . . ? C6 C5 H5 114.4 . . ? C5 C6 N2 123.3(7) . . ? C5 C6 C7 128.0(8) . . ? N2 C6 C7 108.6(8) . . ? C8 C7 C6 107.2(7) . . ? C8 C7 C23 126.3(9) . . ? C6 C7 C23 126.5(10) . . ? C7 C8 C9 106.2(7) . . ? C7 C8 C24 127.8(9) . . ? C9 C8 C24 126.0(11) . . ? N2 C9 C8 111.1(7) . . ? N2 C9 C10 121.6(6) . . ? C8 C9 C10 126.9(7) . . ? C11 C10 C9 121.5(6) . . ? C11 C10 H10A 107.0 . . ? C9 C10 H10A 107.0 . . ? C11 C10 H10B 107.0 . . ? C9 C10 H10B 107.0 . . ? H10A C10 H10B 106.7 . . ? N3 C11 C12 111.3(7) . . ? N3 C11 C10 126.0(7) . . ? C12 C11 C10 122.6(6) . . ? C13 C12 C11 107.0(6) . . ? C13 C12 C25 128.4(7) . . ? C11 C12 C25 124.6(7) . . ? C12 C13 C14 106.4(6) . . ? C12 C13 C26 127.6(7) . . ? C14 C13 C26 125.9(7) . . ? C15 C14 N3 126.2(6) . . ? C15 C14 C13 124.7(6) . . ? N3 C14 C13 109.1(6) . . ? C14 C15 C16 130.4(6) . . ? C14 C15 H15 114.8 . . ? C16 C15 H15 114.8 . . ? N4 C16 C15 123.2(6) . . ? N4 C16 C17 109.7(6) . . ? C15 C16 C17 127.0(7) . . ? C18 C17 C16 106.0(6) . . ? C18 C17 C27 128.5(7) . . ? C16 C17 C27 125.5(7) . . ? C17 C18 C19 107.1(6) . . ? C17 C18 C28 128.1(7) . . ? C19 C18 C28 124.8(7) . . ? N4 C19 C18 110.6(7) . . ? N4 C19 C20 121.2(7) . . ? C18 C19 C20 127.8(7) . . ? C30 C20 C19 119.6(10) . . ? C30 C20 C29 111.8(10) . . ? C19 C20 C29 105.4(8) . . ? C30 C20 H20 106.4 . . ? C19 C20 H20 106.4 . . ? C29 C20 H20 106.4 . . ? C2 C21 H21A 109.5 . . ? C2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C3 C22 H22A 109.5 . . ? C3 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C3 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C7 C23 H23A 109.5 . . ? C7 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C7 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C8 C24 H24A 109.5 . . ? C8 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C8 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C12 C25 H25A 109.5 . . ? C12 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C12 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C13 C26 H26A 109.5 . . ? C13 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C13 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C17 C27 H27A 109.5 . . ? C17 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C17 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C18 C28 H28A 109.5 . . ? C18 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C18 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C20 C29 H29A 109.5 . . ? C20 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C20 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O2 C30 O1 129.2(14) . . ? O2 C30 C20 124.2(14) . . ? O1 C30 C20 106.4(14) . . ? O1 C31 H31A 109.5 . . ? O1 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? O1 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N5 C32 C33 111.9(9) . . ? N5 C32 H32 124.0 . . ? C33 C32 H32 124.0 . . ? C34 C33 C32 106.0(8) . . ? C34 C33 C52 128.5(9) . . ? C32 C33 C52 125.5(10) . . ? C33 C34 C35 106.4(8) . . ? C33 C34 C53 127.4(9) . . ? C35 C34 C53 126.1(10) . . ? N5 C35 C36 122.9(7) . . ? N5 C35 C34 109.5(8) . . ? C36 C35 C34 127.6(9) . . ? C37 C36 C35 130.7(8) . . ? C37 C36 H36 114.6 . . ? C35 C36 H36 114.6 . . ? C36 C37 N6 126.3(7) . . ? C36 C37 C38 124.9(8) . . ? N6 C37 C38 108.8(7) . . ? C39 C38 C37 107.1(7) . . ? C39 C38 C54 125.7(8) . . ? C37 C38 C54 127.2(9) . . ? C38 C39 C40 105.6(7) . . ? C38 C39 C55 129.9(7) . . ? C40 C39 C55 124.5(8) . . ? N6 C40 C39 112.5(7) . . ? N6 C40 C41 127.5(6) . . ? C39 C40 C41 120.0(7) . . ? C42 C41 C40 123.1(6) . . ? C42 C41 H41A 106.6 . . ? C40 C41 H41A 106.6 . . ? C42 C41 H41B 106.6 . . ? C40 C41 H41B 106.6 . . ? H41A C41 H41B 106.5 . . ? N7 C42 C43 110.5(6) . . ? N7 C42 C41 122.2(6) . . ? C43 C42 C41 126.6(6) . . ? C44 C43 C42 106.3(6) . . ? C44 C43 C56 128.4(7) . . ? C42 C43 C56 125.3(7) . . ? C43 C44 C45 106.5(6) . . ? C43 C44 C57 127.8(7) . . ? C45 C44 C57 125.7(7) . . ? C46 C45 N7 124.4(6) . . ? C46 C45 C44 126.8(6) . . ? N7 C45 C44 108.7(6) . . ? C45 C46 C47 130.4(6) . . ? C45 C46 H46 114.8 . . ? C47 C46 H46 114.8 . . ? N8 C47 C46 124.6(6) . . ? N8 C47 C48 108.3(6) . . ? C46 C47 C48 127.0(6) . . ? C49 C48 C47 106.8(6) . . ? C49 C48 C58 128.2(7) . . ? C47 C48 C58 125.0(7) . . ? C48 C49 C50 106.4(6) . . ? C48 C49 C59 126.7(7) . . ? C50 C49 C59 126.9(7) . . ? N8 C50 C49 111.0(6) . . ? N8 C50 C51 120.6(6) . . ? C49 C50 C51 128.4(6) . . ? C61 C51 C50 111.9(7) . . ? C61 C51 C60 116.3(7) . . ? C50 C51 C60 112.5(6) . . ? C61 C51 H51 105.0 . . ? C50 C51 H51 105.0 . . ? C60 C51 H51 105.0 . . ? C33 C52 H52A 109.5 . . ? C33 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C33 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C34 C53 H53A 109.5 . . ? C34 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C34 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C38 C54 H54A 109.5 . . ? C38 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C38 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C39 C55 H55A 109.5 . . ? C39 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C39 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C43 C56 H56A 109.5 . . ? C43 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C43 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C44 C57 H57A 109.5 . . ? C44 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C44 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C48 C58 H58A 109.5 . . ? C48 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C48 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C49 C59 H59A 109.5 . . ? C49 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C49 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C51 C60 H60A 109.5 . . ? C51 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C51 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? O4 C61 O3 120.1(10) . . ? O4 C61 C51 123.0(10) . . ? O3 C61 C51 116.6(8) . . ? O3 C62 H62A 109.5 . . ? O3 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? O3 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 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 N8 Zn1 N1 C1 -55.8(7) . . . . ? N2 Zn1 N1 C1 175.8(6) . . . . ? N7 Zn1 N1 C1 58.6(7) . . . . ? N8 Zn1 N1 C4 140.5(5) . . . . ? N2 Zn1 N1 C4 12.1(6) . . . . ? N7 Zn1 N1 C4 -105.2(5) . . . . ? N8 Zn1 N2 C9 43.2(6) . . . . ? N7 Zn1 N2 C9 -69.3(6) . . . . ? N1 Zn1 N2 C9 175.9(6) . . . . ? N8 Zn1 N2 C6 -143.2(5) . . . . ? N7 Zn1 N2 C6 104.4(5) . . . . ? N1 Zn1 N2 C6 -10.5(5) . . . . ? N5 Zn2 N3 C11 63.7(6) . . . . ? N4 Zn2 N3 C11 175.5(6) . . . . ? N6 Zn2 N3 C11 -58.1(7) . . . . ? N5 Zn2 N3 C14 -110.2(5) . . . . ? N4 Zn2 N3 C14 1.6(5) . . . . ? N6 Zn2 N3 C14 128.0(4) . . . . ? N3 Zn2 N4 C19 -177.6(7) . . . . ? N5 Zn2 N4 C19 -64.5(7) . . . . ? N6 Zn2 N4 C19 40.5(7) . . . . ? N3 Zn2 N4 C16 0.4(5) . . . . ? N5 Zn2 N4 C16 113.5(5) . . . . ? N6 Zn2 N4 C16 -141.5(5) . . . . ? N3 Zn2 N5 C32 36.3(7) . . . . ? N4 Zn2 N5 C32 -69.6(7) . . . . ? N6 Zn2 N5 C32 177.8(7) . . . . ? N3 Zn2 N5 C35 -153.1(6) . . . . ? N4 Zn2 N5 C35 101.0(6) . . . . ? N6 Zn2 N5 C35 -11.7(6) . . . . ? N3 Zn2 N6 C40 -57.0(7) . . . . ? N5 Zn2 N6 C40 177.2(6) . . . . ? N4 Zn2 N6 C40 65.8(7) . . . . ? N3 Zn2 N6 C37 137.1(5) . . . . ? N5 Zn2 N6 C37 11.3(5) . . . . ? N4 Zn2 N6 C37 -100.1(5) . . . . ? N8 Zn1 N7 C42 177.4(5) . . . . ? N2 Zn1 N7 C42 -59.1(6) . . . . ? N1 Zn1 N7 C42 47.8(6) . . . . ? N8 Zn1 N7 C45 -4.6(5) . . . . ? N2 Zn1 N7 C45 118.9(5) . . . . ? N1 Zn1 N7 C45 -134.2(5) . . . . ? N2 Zn1 N8 C50 59.0(6) . . . . ? N7 Zn1 N8 C50 179.6(6) . . . . ? N1 Zn1 N8 C50 -60.3(6) . . . . ? N2 Zn1 N8 C47 -117.7(5) . . . . ? N7 Zn1 N8 C47 2.9(5) . . . . ? N1 Zn1 N8 C47 122.9(5) . . . . ? C4 N1 C1 C2 0.2(9) . . . . ? Zn1 N1 C1 C2 -165.3(6) . . . . ? N1 C1 C2 C3 -0.7(11) . . . . ? N1 C1 C2 C21 178.9(9) . . . . ? C1 C2 C3 C4 0.9(11) . . . . ? C21 C2 C3 C4 -178.7(9) . . . . ? C1 C2 C3 C22 -177.6(9) . . . . ? C21 C2 C3 C22 2.8(19) . . . . ? C1 N1 C4 C5 -177.0(7) . . . . ? Zn1 N1 C4 C5 -9.8(10) . . . . ? C1 N1 C4 C3 0.4(8) . . . . ? Zn1 N1 C4 C3 167.5(5) . . . . ? C2 C3 C4 C5 176.4(9) . . . . ? C22 C3 C4 C5 -4.9(14) . . . . ? C2 C3 C4 N1 -0.8(10) . . . . ? C22 C3 C4 N1 177.8(8) . . . . ? N1 C4 C5 C6 2.2(14) . . . . ? C3 C4 C5 C6 -174.7(8) . . . . ? C4 C5 C6 N2 -0.1(13) . . . . ? C4 C5 C6 C7 -178.9(8) . . . . ? C9 N2 C6 C5 -178.7(7) . . . . ? Zn1 N2 C6 C5 6.3(9) . . . . ? C9 N2 C6 C7 0.3(8) . . . . ? Zn1 N2 C6 C7 -174.8(5) . . . . ? C5 C6 C7 C8 178.0(8) . . . . ? N2 C6 C7 C8 -0.9(9) . . . . ? C5 C6 C7 C23 -2.0(13) . . . . ? N2 C6 C7 C23 179.1(7) . . . . ? C6 C7 C8 C9 1.1(9) . . . . ? C23 C7 C8 C9 -178.9(8) . . . . ? C6 C7 C8 C24 -177.6(8) . . . . ? C23 C7 C8 C24 2.4(15) . . . . ? C6 N2 C9 C8 0.5(8) . . . . ? Zn1 N2 C9 C8 174.8(5) . . . . ? C6 N2 C9 C10 174.5(6) . . . . ? Zn1 N2 C9 C10 -11.2(9) . . . . ? C7 C8 C9 N2 -1.0(9) . . . . ? C24 C8 C9 N2 177.7(8) . . . . ? C7 C8 C9 C10 -174.6(7) . . . . ? C24 C8 C9 C10 4.1(13) . . . . ? N2 C9 C10 C11 70.5(9) . . . . ? C8 C9 C10 C11 -116.4(8) . . . . ? C14 N3 C11 C12 -0.8(7) . . . . ? Zn2 N3 C11 C12 -175.2(4) . . . . ? C14 N3 C11 C10 174.8(6) . . . . ? Zn2 N3 C11 C10 0.4(10) . . . . ? C9 C10 C11 N3 23.5(11) . . . . ? C9 C10 C11 C12 -161.4(7) . . . . ? N3 C11 C12 C13 0.5(7) . . . . ? C10 C11 C12 C13 -175.2(6) . . . . ? N3 C11 C12 C25 178.7(6) . . . . ? C10 C11 C12 C25 2.9(10) . . . . ? C11 C12 C13 C14 0.0(7) . . . . ? C25 C12 C13 C14 -178.1(6) . . . . ? C11 C12 C13 C26 -179.4(6) . . . . ? C25 C12 C13 C26 2.6(11) . . . . ? C11 N3 C14 C15 -177.7(6) . . . . ? Zn2 N3 C14 C15 -2.3(8) . . . . ? C11 N3 C14 C13 0.7(7) . . . . ? Zn2 N3 C14 C13 176.1(4) . . . . ? C12 C13 C14 C15 178.0(6) . . . . ? C26 C13 C14 C15 -2.6(10) . . . . ? C12 C13 C14 N3 -0.4(7) . . . . ? C26 C13 C14 N3 178.9(6) . . . . ? N3 C14 C15 C16 0.5(11) . . . . ? C13 C14 C15 C16 -177.7(6) . . . . ? C19 N4 C16 C15 176.4(6) . . . . ? Zn2 N4 C16 C15 -2.0(9) . . . . ? C19 N4 C16 C17 -1.4(8) . . . . ? Zn2 N4 C16 C17 -179.8(4) . . . . ? C14 C15 C16 N4 2.0(11) . . . . ? C14 C15 C16 C17 179.3(7) . . . . ? N4 C16 C17 C18 0.8(8) . . . . ? C15 C16 C17 C18 -176.8(6) . . . . ? N4 C16 C17 C27 -179.7(6) . . . . ? C15 C16 C17 C27 2.6(11) . . . . ? C16 C17 C18 C19 0.0(8) . . . . ? C27 C17 C18 C19 -179.4(7) . . . . ? C16 C17 C18 C28 179.2(7) . . . . ? C27 C17 C18 C28 -0.2(13) . . . . ? C16 N4 C19 C18 1.3(8) . . . . ? Zn2 N4 C19 C18 179.6(5) . . . . ? C16 N4 C19 C20 -171.6(8) . . . . ? Zn2 N4 C19 C20 6.6(12) . . . . ? C17 C18 C19 N4 -0.8(9) . . . . ? C28 C18 C19 N4 179.9(7) . . . . ? C17 C18 C19 C20 171.6(8) . . . . ? C28 C18 C19 C20 -7.7(13) . . . . ? N4 C19 C20 C30 -132.6(11) . . . . ? C18 C19 C20 C30 55.8(15) . . . . ? N4 C19 C20 C29 100.6(9) . . . . ? C18 C19 C20 C29 -71.1(10) . . . . ? C31 O1 C30 O2 -11(2) . . . . ? C31 O1 C30 C20 174.8(10) . . . . ? C19 C20 C30 O2 -129.3(15) . . . . ? C29 C20 C30 O2 -5.5(18) . . . . ? C19 C20 C30 O1 45.7(14) . . . . ? C29 C20 C30 O1 169.5(9) . . . . ? C35 N5 C32 C33 0.5(9) . . . . ? Zn2 N5 C32 C33 172.2(6) . . . . ? N5 C32 C33 C34 -0.4(10) . . . . ? N5 C32 C33 C52 179.0(9) . . . . ? C32 C33 C34 C35 0.1(10) . . . . ? C52 C33 C34 C35 -179.3(9) . . . . ? C32 C33 C34 C53 -179.5(10) . . . . ? C52 C33 C34 C53 1.1(17) . . . . ? C32 N5 C35 C36 -179.6(7) . . . . ? Zn2 N5 C35 C36 7.9(11) . . . . ? C32 N5 C35 C34 -0.5(9) . . . . ? Zn2 N5 C35 C34 -173.0(5) . . . . ? C33 C34 C35 N5 0.2(10) . . . . ? C53 C34 C35 N5 179.8(9) . . . . ? C33 C34 C35 C36 179.3(9) . . . . ? C53 C34 C35 C36 -1.1(15) . . . . ? N5 C35 C36 C37 -0.7(14) . . . . ? C34 C35 C36 C37 -179.7(9) . . . . ? C35 C36 C37 N6 1.1(14) . . . . ? C35 C36 C37 C38 -177.8(8) . . . . ? C40 N6 C37 C36 -177.8(8) . . . . ? Zn2 N6 C37 C36 -8.2(10) . . . . ? C40 N6 C37 C38 1.2(8) . . . . ? Zn2 N6 C37 C38 170.9(5) . . . . ? C36 C37 C38 C39 178.1(8) . . . . ? N6 C37 C38 C39 -1.0(9) . . . . ? C36 C37 C38 C54 -0.3(14) . . . . ? N6 C37 C38 C54 -179.4(8) . . . . ? C37 C38 C39 C40 0.4(9) . . . . ? C54 C38 C39 C40 178.8(8) . . . . ? C37 C38 C39 C55 -179.6(8) . . . . ? C54 C38 C39 C55 -1.2(15) . . . . ? C37 N6 C40 C39 -1.0(8) . . . . ? Zn2 N6 C40 C39 -168.1(5) . . . . ? C37 N6 C40 C41 177.3(7) . . . . ? Zn2 N6 C40 C41 10.2(11) . . . . ? C38 C39 C40 N6 0.4(9) . . . . ? C55 C39 C40 N6 -179.6(7) . . . . ? C38 C39 C40 C41 -178.0(7) . . . . ? C55 C39 C40 C41 1.9(11) . . . . ? N6 C40 C41 C42 2.7(11) . . . . ? C39 C40 C41 C42 -179.1(7) . . . . ? C45 N7 C42 C43 -1.0(7) . . . . ? Zn1 N7 C42 C43 177.2(4) . . . . ? C45 N7 C42 C41 170.1(6) . . . . ? Zn1 N7 C42 C41 -11.7(9) . . . . ? C40 C41 C42 N7 85.1(9) . . . . ? C40 C41 C42 C43 -105.2(8) . . . . ? N7 C42 C43 C44 0.4(7) . . . . ? C41 C42 C43 C44 -170.3(6) . . . . ? N7 C42 C43 C56 178.7(6) . . . . ? C41 C42 C43 C56 8.0(11) . . . . ? C42 C43 C44 C45 0.4(7) . . . . ? C56 C43 C44 C45 -177.9(7) . . . . ? C42 C43 C44 C57 179.4(6) . . . . ? C56 C43 C44 C57 1.2(12) . . . . ? C42 N7 C45 C46 -177.6(6) . . . . ? Zn1 N7 C45 C46 4.0(8) . . . . ? C42 N7 C45 C44 1.2(7) . . . . ? Zn1 N7 C45 C44 -177.1(4) . . . . ? C43 C44 C45 C46 177.8(6) . . . . ? C57 C44 C45 C46 -1.3(11) . . . . ? C43 C44 C45 N7 -1.0(7) . . . . ? C57 C44 C45 N7 179.9(6) . . . . ? N7 C45 C46 C47 -0.5(10) . . . . ? C44 C45 C46 C47 -179.1(6) . . . . ? C50 N8 C47 C46 -177.9(6) . . . . ? Zn1 N8 C47 C46 -0.5(8) . . . . ? C50 N8 C47 C48 -0.4(7) . . . . ? Zn1 N8 C47 C48 177.0(4) . . . . ? C45 C46 C47 N8 -1.6(11) . . . . ? C45 C46 C47 C48 -178.6(6) . . . . ? N8 C47 C48 C49 0.2(7) . . . . ? C46 C47 C48 C49 177.7(6) . . . . ? N8 C47 C48 C58 -178.8(6) . . . . ? C46 C47 C48 C58 -1.4(10) . . . . ? C47 C48 C49 C50 0.1(7) . . . . ? C58 C48 C49 C50 179.1(6) . . . . ? C47 C48 C49 C59 -180.0(7) . . . . ? C58 C48 C49 C59 -0.9(11) . . . . ? C47 N8 C50 C49 0.5(7) . . . . ? Zn1 N8 C50 C49 -176.6(4) . . . . ? C47 N8 C50 C51 -178.2(6) . . . . ? Zn1 N8 C50 C51 4.8(9) . . . . ? C48 C49 C50 N8 -0.3(7) . . . . ? C59 C49 C50 N8 179.7(6) . . . . ? C48 C49 C50 C51 178.2(7) . . . . ? C59 C49 C50 C51 -1.8(12) . . . . ? N8 C50 C51 C61 -122.1(8) . . . . ? C49 C50 C51 C61 59.5(10) . . . . ? N8 C50 C51 C60 104.9(8) . . . . ? C49 C50 C51 C60 -73.6(10) . . . . ? C62 O3 C61 O4 -9.9(16) . . . . ? C62 O3 C61 C51 176.8(8) . . . . ? C50 C51 C61 O4 -130.3(11) . . . . ? C60 C51 C61 O4 0.9(15) . . . . ? C50 C51 C61 O3 42.8(11) . . . . ? C60 C51 C61 O3 174.0(8) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.0 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.36 _refine_diff_density_min -0.80 _refine_diff_density_rms 0.093