data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dr Yuji Mikata' _publ_contact_author_address ; KYOUSEI Science Center Nara Women's University Kitauoya-Higashi-machi Nara 630-8506 JAPAN ; _publ_contact_author_email mikata@cc.nara-wu.ac.jp _publ_contact_author_fax +81-742-20-3095 _publ_contact_author_phone +81-742-20-3095 _publ_section_references ; ENTER OTHER REFERENCES Rigaku/MSC and Rigaku Corporation. (2004). CrystalStructure 3.6.0. Single Crystal Structure Analysis Software. Rigaku/MSC, 9009 New Trails Drive, The Woodlands, TX, USA 77381-5209. Rigaku, 3-9-12 Akishima, Tokyo 196-8666, Japan. Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W. (1996) CRYSTALS Issue 10, Chemical Crystallography Laboratory, Oxford, UK. ; _publ_section_title ; Tetrakis(2-quinolinylmethyl)ethylenediamine (TQEN) as a new fluorescent sensor for zinc ; loop_ _publ_author_name 'Yuji Mikata' 'Motoko Wakamatsu' 'Shigenobu Yano' data_Q4en _database_code_depnum_ccdc_archive 'CCDC 246544' _audit_creation_date 2004-10-29 _audit_creation_method 'by CrystalStructure 3.6.0' _audit_update_record ? # CHEMICAL DATA _chemical_formula_sum 'C46 H40 Cl12 N6 ' _chemical_formula_moiety 'C46 H40 Cl12 N6 ' _chemical_formula_weight 1102.30 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z #------------------------------------------------------------------------------ _cell_length_a 10.271(6) _cell_length_b 11.240(7) _cell_length_c 13.251(7) _cell_angle_alpha 71.05(2) _cell_angle_beta 64.21(2) _cell_angle_gamma 74.27(3) _cell_volume 1287.6(13) _cell_formula_units_Z 1 _cell_measurement_reflns_used 3625 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 173.1 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.421 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 562.00 _exptl_absorpt_coefficient_mu 0.683 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Higashi, T. (1999). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.788 _exptl_absorpt_correction_T_max 0.872 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo Kalpha' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 9893 _diffrn_reflns_av_R_equivalents 0.024 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9391 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.9370 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 5550 _reflns_number_gt 4492 _reflns_threshold_expression F^2^>2.0sigma(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0660 _refine_ls_wR_factor_ref 0.1720 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 5550 _refine_ls_number_parameters 309 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0020Fo^2^ + 3.0000sigma(Fo^2^) + 0.5000]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 0.52 _refine_diff_density_min -0.55 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Cl(1) Cl -0.38175(12) 0.40705(10) 0.37801(9) 0.0788(3) Uani 1.00 1 d . . . Cl(2) Cl -0.16440(10) 0.29605(13) 0.19145(10) 0.0885(4) Uani 1.00 1 d . . . Cl(3) Cl -0.40598(11) 0.16707(10) 0.35942(8) 0.0714(3) Uani 1.00 1 d . . . Cl(4) Cl -0.22342(11) -0.01732(9) 0.13274(8) 0.0722(3) Uani 1.00 1 d . . . Cl(5) Cl -0.04956(11) -0.26656(11) 0.14449(11) 0.0887(4) Uani 1.00 1 d . . . Cl(6) Cl -0.33538(9) -0.22793(10) 0.32205(7) 0.0663(3) Uani 1.00 1 d . . . N(1) N 0.1202(2) 0.3753(2) 0.4190(2) 0.0304(5) Uani 1.00 1 d . . . N(2) N 0.0126(2) 0.1110(2) 0.6364(2) 0.0311(5) Uani 1.00 1 d . . . N(3) N 0.4261(2) 0.3707(2) 0.1562(2) 0.0275(5) Uani 1.00 1 d . . . C(1) C 0.0496(3) 0.4391(2) 0.5145(2) 0.0326(6) Uani 1.00 1 d . . . C(2) C 0.1636(3) 0.2379(2) 0.4581(2) 0.0346(6) Uani 1.00 1 d . . . C(3) C 0.0320(3) 0.1719(2) 0.5286(2) 0.0308(6) Uani 1.00 1 d . . . C(4) C -0.0667(3) 0.1782(3) 0.4778(2) 0.0424(7) Uani 1.00 1 d . . . C(5) C -0.1881(3) 0.1217(3) 0.5429(3) 0.0465(8) Uani 1.00 1 d . . . C(6) C -0.3434(3) 0.0012(3) 0.7338(3) 0.0490(8) Uani 1.00 1 d . . . C(7) C -0.3634(3) -0.0569(3) 0.8459(3) 0.0532(8) Uani 1.00 1 d . . . C(8) C -0.2586(4) -0.0638(3) 0.8888(3) 0.0520(8) Uani 1.00 1 d . . . C(9) C -0.1336(3) -0.0106(2) 0.8186(2) 0.0415(7) Uani 1.00 1 d . . . C(10) C -0.1099(3) 0.0530(2) 0.7024(2) 0.0306(6) Uani 1.00 1 d . . . C(11) C -0.2155(3) 0.0580(2) 0.6582(2) 0.0361(6) Uani 1.00 1 d . . . C(12) C 0.2459(3) 0.4344(3) 0.3282(2) 0.0352(6) Uani 1.00 1 d . . . C(13) C 0.2866(2) 0.4059(2) 0.2138(2) 0.0291(5) Uani 1.00 1 d . . . C(14) C 0.1755(3) 0.4224(2) 0.1721(2) 0.0358(6) Uani 1.00 1 d . . . C(15) C 0.2137(3) 0.4046(2) 0.0653(2) 0.0346(6) Uani 1.00 1 d . . . C(16) C 0.4109(3) 0.3429(3) -0.1108(2) 0.0393(7) Uani 1.00 1 d . . . C(17) C 0.5548(3) 0.3011(3) -0.1671(2) 0.0432(7) Uani 1.00 1 d . . . C(18) C 0.6572(3) 0.2831(2) -0.1174(2) 0.0409(7) Uani 1.00 1 d . . . C(19) C 0.6143(3) 0.3083(2) -0.0124(2) 0.0332(6) Uani 1.00 1 d . . . C(20) C 0.4658(2) 0.3505(2) 0.0488(2) 0.0277(5) Uani 1.00 1 d . . . C(21) C 0.3617(3) 0.3681(2) -0.0004(2) 0.0304(6) Uani 1.00 1 d . . . C(22) C -0.3498(3) 0.3160(4) 0.2822(3) 0.0571(9) Uani 1.00 1 d . . . C(23) C -0.1782(3) -0.1592(3) 0.2251(3) 0.0493(8) Uani 1.00 1 d . . . H(1) H -0.0068 0.3836 0.5817 0.038 Uiso 1.00 1 c R . . H(2) H 0.1231 0.4592 0.5288 0.038 Uiso 1.00 1 c R . . H(3) H 0.2221 0.2031 0.3928 0.040 Uiso 1.00 1 c R . . H(4) H 0.2187 0.2251 0.5037 0.040 Uiso 1.00 1 c R . . H(5) H -0.0478 0.2218 0.3994 0.055 Uiso 1.00 1 c R . . H(6) H -0.2546 0.1245 0.5097 0.063 Uiso 1.00 1 c R . . H(7) H -0.4145 0.0038 0.7051 0.061 Uiso 1.00 1 c R . . H(8) H -0.4503 -0.0925 0.8959 0.060 Uiso 1.00 1 c R . . H(9) H -0.2737 -0.1060 0.9669 0.060 Uiso 1.00 1 c R . . H(10) H -0.0625 -0.0167 0.8486 0.051 Uiso 1.00 1 c R . . H(11) H 0.2228 0.5239 0.3198 0.042 Uiso 1.00 1 c R . . H(12) H 0.3273 0.4026 0.3507 0.042 Uiso 1.00 1 c R . . H(13) H 0.0758 0.4452 0.2182 0.041 Uiso 1.00 1 c R . . H(14) H 0.1411 0.4176 0.0350 0.043 Uiso 1.00 1 c R . . H(15) H 0.3430 0.3572 -0.1459 0.049 Uiso 1.00 1 c R . . H(16) H 0.5861 0.2823 -0.2399 0.050 Uiso 1.00 1 c R . . H(17) H 0.7572 0.2539 -0.1577 0.044 Uiso 1.00 1 c R . . H(18) H 0.6845 0.2970 0.0198 0.038 Uiso 1.00 1 c R . . H(19) H -0.4057 0.3592 0.2359 0.071 Uiso 1.00 1 c R . . H(20) H -0.1358 -0.1402 0.2680 0.065 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cl(1) 0.1028(8) 0.0770(6) 0.0821(6) 0.0036(5) -0.0621(6) -0.0273(5) Cl(2) 0.0453(5) 0.1330(10) 0.0861(7) -0.0095(5) -0.0245(5) -0.0287(7) Cl(3) 0.0764(6) 0.0820(6) 0.0717(6) -0.0123(5) -0.0423(5) -0.0183(5) Cl(4) 0.0854(7) 0.0698(6) 0.0665(5) -0.0064(5) -0.0413(5) -0.0098(4) Cl(5) 0.0562(5) 0.0984(8) 0.1243(9) 0.0154(5) -0.0329(6) -0.0668(7) Cl(6) 0.0577(5) 0.0879(7) 0.0664(5) -0.0235(4) -0.0298(4) -0.0160(5) N(1) 0.0357(10) 0.0291(10) 0.0213(9) -0.0070(8) -0.0046(8) -0.0068(7) N(2) 0.0365(10) 0.0297(10) 0.0313(9) -0.0073(8) -0.0157(8) -0.0067(8) N(3) 0.0293(10) 0.0275(9) 0.0242(9) -0.0078(7) -0.0077(7) -0.0049(7) C(1) 0.0359(12) 0.0357(12) 0.0227(10) -0.0068(10) -0.0052(9) -0.0098(9) C(2) 0.0354(12) 0.0339(12) 0.0311(11) -0.0035(10) -0.0107(9) -0.0079(10) C(3) 0.0349(12) 0.0294(11) 0.0308(11) -0.0035(9) -0.0144(9) -0.0093(9) C(4) 0.058(2) 0.0371(13) 0.043(1) -0.0076(12) -0.0326(13) -0.0032(11) C(5) 0.053(2) 0.042(1) 0.062(2) -0.0062(12) -0.040(1) -0.0088(13) C(6) 0.041(1) 0.0321(13) 0.081(2) -0.0064(11) -0.028(1) -0.014(1) C(7) 0.044(2) 0.032(1) 0.073(2) -0.0156(12) -0.008(1) -0.012(1) C(8) 0.065(2) 0.038(2) 0.047(2) -0.0243(13) -0.012(1) -0.0024(12) C(9) 0.054(2) 0.0367(13) 0.0371(13) -0.0156(11) -0.0183(12) -0.0049(11) C(10) 0.0347(12) 0.0250(11) 0.0344(12) -0.0060(9) -0.0135(9) -0.0083(9) C(11) 0.0344(12) 0.0272(11) 0.052(1) -0.0028(9) -0.0200(11) -0.0128(10) C(12) 0.0360(12) 0.0420(13) 0.0269(11) -0.0125(10) -0.0050(9) -0.0119(10) C(13) 0.0287(11) 0.0299(11) 0.0241(10) -0.0069(9) -0.0050(8) -0.0057(9) C(14) 0.0274(11) 0.042(1) 0.0325(12) -0.0066(10) -0.0065(9) -0.0078(10) C(15) 0.0327(12) 0.0411(13) 0.0331(11) -0.0085(10) -0.0153(10) -0.0063(10) C(16) 0.053(2) 0.0407(13) 0.0287(11) -0.0180(11) -0.0129(11) -0.0092(10) C(17) 0.056(2) 0.041(1) 0.0290(12) -0.0167(12) -0.0026(11) -0.0156(11) C(18) 0.0387(13) 0.0318(12) 0.0397(13) -0.0056(10) 0.0010(11) -0.0150(11) C(19) 0.0327(12) 0.0283(11) 0.0328(11) -0.0049(9) -0.0071(9) -0.0072(9) C(20) 0.0315(11) 0.0221(10) 0.0269(10) -0.0076(8) -0.0072(9) -0.0054(8) C(21) 0.0352(12) 0.0288(11) 0.0260(10) -0.0110(9) -0.0081(9) -0.0050(9) C(22) 0.046(2) 0.079(2) 0.054(2) -0.003(2) -0.029(1) -0.017(2) C(23) 0.047(2) 0.062(2) 0.054(2) -0.0073(13) -0.0288(13) -0.020(1) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR97 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.6.0' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Cl(1) C(22) 1.752(5) ? . . Cl(2) C(22) 1.754(3) ? . . Cl(3) C(22) 1.754(4) ? . . Cl(4) C(23) 1.756(3) ? . . Cl(5) C(23) 1.757(3) ? . . Cl(6) C(23) 1.755(3) ? . . N(1) C(1) 1.467(3) ? . . N(1) C(2) 1.470(3) ? . . N(1) C(12) 1.466(3) ? . . N(2) C(3) 1.318(3) ? . . N(2) C(10) 1.374(3) ? . . N(3) C(13) 1.315(3) ? . . N(3) C(20) 1.378(3) ? . . C(2) C(3) 1.498(3) ? . . C(3) C(4) 1.419(5) ? . . C(4) C(5) 1.356(4) ? . . C(5) C(11) 1.396(4) ? . . C(6) C(7) 1.361(5) ? . . C(6) C(11) 1.426(4) ? . . C(7) C(8) 1.394(6) ? . . C(8) C(9) 1.374(4) ? . . C(9) C(10) 1.413(3) ? . . C(10) C(11) 1.421(5) ? . . C(12) C(13) 1.506(4) ? . . C(13) C(14) 1.418(4) ? . . C(14) C(15) 1.361(4) ? . . C(15) C(21) 1.407(3) ? . . C(16) C(17) 1.361(4) ? . . C(16) C(21) 1.423(4) ? . . C(17) C(18) 1.407(5) ? . . C(18) C(19) 1.366(4) ? . . C(19) C(20) 1.411(3) ? . . C(20) C(21) 1.420(4) ? . . C(1) H(1) 0.9500 ? . . C(1) H(2) 0.9500 ? . . C(2) H(3) 0.9500 ? . . C(2) H(4) 0.9500 ? . . C(4) H(5) 0.9499 ? . . C(5) H(6) 0.9500 ? . . C(6) H(7) 0.9500 ? . . C(7) H(8) 0.9500 ? . . C(8) H(9) 0.9500 ? . . C(9) H(10) 0.9500 ? . . C(12) H(11) 0.9500 ? . . C(12) H(12) 0.9500 ? . . C(14) H(13) 0.9500 ? . . C(15) H(14) 0.9500 ? . . C(16) H(15) 0.9500 ? . . C(17) H(16) 0.9499 ? . . C(18) H(17) 0.9500 ? . . C(19) H(18) 0.9500 ? . . C(22) H(19) 0.9500 ? . . C(23) H(20) 0.9500 ? . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Cl(1) C(22) Cl(2) 111.0(2) ? . . . Cl(1) C(22) Cl(3) 110.0(2) ? . . . Cl(2) C(22) Cl(3) 110.1(2) ? . . . Cl(4) C(23) Cl(5) 110.3(2) ? . . . Cl(4) C(23) Cl(6) 110.6(2) ? . . . Cl(5) C(23) Cl(6) 110.3(2) ? . . . C(2) N(1) C(1) 112.2(2) ? . . . C(12) N(1) C(1) 111.3(2) ? . . . N(1) C(2) C(3) 110.9(2) ? . . . C(12) N(1) C(2) 110.7(2) ? . . . N(1) C(12) C(13) 112.4(3) ? . . . N(2) C(3) C(2) 118.2(3) ? . . . N(2) C(3) C(4) 122.7(2) ? . . . C(10) N(2) C(3) 118.4(3) ? . . . N(2) C(10) C(9) 119.0(3) ? . . . N(2) C(10) C(11) 122.0(2) ? . . . N(3) C(13) C(12) 117.1(3) ? . . . N(3) C(13) C(14) 123.7(2) ? . . . C(20) N(3) C(13) 117.7(2) ? . . . N(3) C(20) C(19) 118.5(3) ? . . . N(3) C(20) C(21) 122.0(2) ? . . . C(2) C(3) C(4) 119.1(2) ? . . . C(3) C(4) C(5) 118.9(3) ? . . . C(4) C(5) C(11) 120.7(4) ? . . . C(5) C(11) C(10) 117.2(2) ? . . . C(5) C(11) C(6) 124.1(3) ? . . . C(11) C(6) C(7) 120.5(4) ? . . . C(6) C(7) C(8) 120.9(3) ? . . . C(6) C(11) C(10) 118.6(3) ? . . . C(7) C(8) C(9) 120.5(3) ? . . . C(8) C(9) C(10) 120.5(3) ? . . . C(9) C(10) C(11) 119.0(2) ? . . . C(12) C(13) C(14) 119.2(2) ? . . . C(13) C(14) C(15) 119.1(2) ? . . . C(14) C(15) C(21) 119.5(3) ? . . . C(15) C(21) C(20) 117.9(2) ? . . . C(15) C(21) C(16) 123.4(3) ? . . . C(21) C(16) C(17) 120.5(3) ? . . . C(16) C(17) C(18) 120.5(3) ? . . . C(16) C(21) C(20) 118.7(2) ? . . . C(17) C(18) C(19) 120.7(2) ? . . . C(18) C(19) C(20) 120.3(3) ? . . . C(19) C(20) C(21) 119.4(2) ? . . . Cl(1) C(22) H(19) 108.5162 ? . . . Cl(2) C(22) H(19) 108.6091 ? . . . Cl(3) C(22) H(19) 108.6605 ? . . . Cl(4) C(23) H(20) 108.6257 ? . . . Cl(5) C(23) H(20) 108.4423 ? . . . Cl(6) C(23) H(20) 108.5861 ? . . . N(1) C(1) H(1) 109.3579 ? . . . N(1) C(1) H(2) 108.8500 ? . . . N(1) C(2) H(3) 109.2590 ? . . . N(1) C(2) H(4) 108.8725 ? . . . N(1) C(12) H(11) 108.8319 ? . . . N(1) C(12) H(12) 108.5311 ? . . . H(2) C(1) H(1) 109.4619 ? . . . H(3) C(2) C(3) 109.1162 ? . . . H(4) C(2) C(3) 109.1752 ? . . . H(4) C(2) H(3) 109.4552 ? . . . C(3) C(4) H(5) 120.2149 ? . . . H(5) C(4) C(5) 120.8432 ? . . . C(4) C(5) H(6) 119.8012 ? . . . H(6) C(5) C(11) 119.5367 ? . . . H(7) C(6) C(7) 120.1829 ? . . . C(6) C(7) H(8) 119.5938 ? . . . H(7) C(6) C(11) 119.3172 ? . . . H(8) C(7) C(8) 119.5297 ? . . . C(7) C(8) H(9) 119.6834 ? . . . C(8) C(9) H(10) 119.7288 ? . . . H(9) C(8) C(9) 119.8434 ? . . . H(10) C(9) C(10) 119.7430 ? . . . H(11) C(12) C(13) 109.0251 ? . . . H(12) C(12) C(13) 108.5433 ? . . . H(12) C(12) H(11) 109.4540 ? . . . C(13) C(14) H(13) 120.3506 ? . . . H(13) C(14) C(15) 120.5738 ? . . . C(14) C(15) H(14) 120.2919 ? . . . H(14) C(15) C(21) 120.1615 ? . . . H(15) C(16) C(17) 119.9700 ? . . . C(16) C(17) H(16) 119.7899 ? . . . H(15) C(16) C(21) 119.5267 ? . . . H(16) C(17) C(18) 119.7111 ? . . . C(17) C(18) H(17) 119.6697 ? . . . C(18) C(19) H(18) 119.9829 ? . . . H(17) C(18) C(19) 119.6568 ? . . . H(18) C(19) C(20) 119.7429 ? . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 C(1) N(1) C(2) C(3) 68.8(3) ? . . . . C(12) N(1) C(2) C(3) -166.2(2) ? . . . . C(1) N(1) C(12) C(13) -159.2(2) ? . . . . C(2) N(1) C(12) C(13) 75.3(3) ? . . . . C(10) N(2) C(3) C(2) 178.4(2) ? . . . . C(10) N(2) C(3) C(4) -1.1(3) ? . . . . C(3) N(2) C(10) C(9) -178.8(2) ? . . . . C(3) N(2) C(10) C(11) -0.6(3) ? . . . . C(20) N(3) C(13) C(12) -176.8(2) ? . . . . C(20) N(3) C(13) C(14) 0.8(3) ? . . . . C(13) N(3) C(20) C(19) -177.8(2) ? . . . . C(13) N(3) C(20) C(21) 0.9(3) ? . . . . N(1) C(2) C(3) N(2) -119.4(3) ? . . . . N(1) C(2) C(3) C(4) 60.1(3) ? . . . . N(2) C(3) C(4) C(5) 1.5(4) ? . . . . C(2) C(3) C(4) C(5) -178.0(2) ? . . . . C(3) C(4) C(5) C(11) -0.2(4) ? . . . . C(4) C(5) C(11) C(6) 177.1(3) ? . . . . C(4) C(5) C(11) C(10) -1.3(4) ? . . . . C(11) C(6) C(7) C(8) -1.0(4) ? . . . . C(7) C(6) C(11) C(5) -178.6(3) ? . . . . C(7) C(6) C(11) C(10) -0.2(4) ? . . . . C(6) C(7) C(8) C(9) 0.8(5) ? . . . . C(7) C(8) C(9) C(10) 0.6(4) ? . . . . C(8) C(9) C(10) N(2) 176.6(2) ? . . . . C(8) C(9) C(10) C(11) -1.8(4) ? . . . . N(2) C(10) C(11) C(5) 1.7(4) ? . . . . N(2) C(10) C(11) C(6) -176.7(2) ? . . . . C(9) C(10) C(11) C(5) -180.0(2) ? . . . . C(9) C(10) C(11) C(6) 1.5(3) ? . . . . N(1) C(12) C(13) N(3) -134.0(2) ? . . . . N(1) C(12) C(13) C(14) 48.3(3) ? . . . . N(3) C(13) C(14) C(15) -1.9(4) ? . . . . C(12) C(13) C(14) C(15) 175.7(2) ? . . . . C(13) C(14) C(15) C(21) 1.2(4) ? . . . . C(14) C(15) C(21) C(16) 177.6(2) ? . . . . C(14) C(15) C(21) C(20) 0.4(3) ? . . . . C(21) C(16) C(17) C(18) -0.5(4) ? . . . . C(17) C(16) C(21) C(15) -176.3(2) ? . . . . C(17) C(16) C(21) C(20) 0.9(4) ? . . . . C(16) C(17) C(18) C(19) -0.6(4) ? . . . . C(17) C(18) C(19) C(20) 1.3(4) ? . . . . C(18) C(19) C(20) N(3) 177.8(2) ? . . . . C(18) C(19) C(20) C(21) -0.9(3) ? . . . . N(3) C(20) C(21) C(15) -1.4(3) ? . . . . N(3) C(20) C(21) C(16) -178.8(2) ? . . . . C(19) C(20) C(21) C(15) 177.2(2) ? . . . . C(19) C(20) C(21) C(16) -0.2(3) ? . . . . #============================================================================== # End of CIF #============================================================================== #===END data_tqenzn55 _database_code_depnum_ccdc_archive 'CCDC 246545' _audit_creation_date 2004-11-04 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H43.50 Cl2 N8.50 O8 Zn' _chemical_formula_weight 991.67 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' Zn Zn 0.2839 1.4301 '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_cell_setting monoclinic _symmetry_space_group_name_H-M 'C2 /c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 36.5983(14) _cell_length_b 12.5859(2) _cell_length_c 24.8617(9) _cell_angle_alpha 90.00 _cell_angle_beta 127.1400(2) _cell_angle_gamma 90.00 _cell_volume 9129.0(5) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.443 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4104 _exptl_absorpt_coefficient_mu 0.719 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7618 _exptl_absorpt_correction_T_max 0.8131 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 44143 _diffrn_reflns_av_R_equivalents 0.0181 _diffrn_reflns_av_sigmaI/netI 0.0176 _diffrn_reflns_limit_h_min -47 _diffrn_reflns_limit_h_max 47 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10449 _reflns_number_gt 9318 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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/[sigma^2^(Fo^2^)+(0.0740P)^2^+8.3070P] 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 10449 _refine_ls_number_parameters 638 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0465 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.1238 _refine_ls_wR_factor_gt 0.1121 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _refine_ls_shift/su_max 0.007 _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 0.148051(6) 0.791449(15) 0.111334(9) 0.02566(8) Uani 1 1 d . . . Cl1 Cl 0.025974(15) 0.45095(4) 0.14084(2) 0.03905(12) Uani 1 1 d . . . Cl2 Cl 0.13198(4) 0.15146(8) 0.91057(5) 0.0445(2) Uani 0.75 1 d P A 3 Cl3 Cl 0.11351(9) 0.1309(3) 0.89542(14) 0.0363(6) Uani 0.25 1 d P A 3 O1 O 0.03933(7) 0.41536(16) 0.09977(9) 0.0593(4) Uani 1 1 d . . . O2 O -0.01468(6) 0.39777(16) 0.12123(10) 0.0625(5) Uani 1 1 d . . . O3 O 0.01670(9) 0.56186(17) 0.13269(17) 0.0954(9) Uani 1 1 d . . . O4 O 0.06203(7) 0.4296(3) 0.20955(10) 0.0965(9) Uani 1 1 d . . . O5 O 0.11091(9) 0.17876(14) 0.94364(11) 0.0697(6) Uani 1 1 d . A 3 O6 O 0.10143(8) 0.1872(2) 0.84237(10) 0.0751(6) Uani 1 1 d . A 3 O7 O 0.17465(12) 0.2073(3) 0.93852(16) 0.0828(10) Uani 0.75 1 d P A 3 O8 O 0.1423(2) 0.0414(3) 0.9172(3) 0.1131(18) Uani 0.75 1 d P A 3 O9 O 0.0943(3) 0.0343(4) 0.8705(3) 0.0429(14) Uani 0.25 1 d P A 3 O10 O 0.1634(3) 0.1116(14) 0.9460(5) 0.109(5) Uani 0.25 1 d P A 3 N1 N 0.11146(5) 0.85374(11) 0.01071(7) 0.0271(3) Uani 1 1 d . . . N2 N 0.08066(5) 0.73145(12) 0.07215(7) 0.0278(3) Uani 1 1 d . . . N3 N 0.20106(5) 0.85974(11) 0.10901(7) 0.0274(3) Uani 1 1 d . . . N4 N 0.12707(5) 0.96554(11) 0.12352(7) 0.0274(3) Uani 1 1 d . . . N5 N 0.15968(5) 0.72036(11) 0.19808(7) 0.0256(3) Uani 1 1 d . . . N6 N 0.14976(5) 0.61809(12) 0.07557(7) 0.0298(3) Uani 1 1 d . . . N7 N 0.00971(8) 0.0260(2) 0.59484(15) 0.0738(7) Uani 1 1 d . . . N8 N 0.12781(10) 0.6166(3) 0.89229(15) 0.0786(8) Uani 1 1 d . . . N9 N 0.0375(3) 0.8887(8) 0.8166(4) 0.126(3) Uani 0.50 1 d P . . C1 C 0.06618(6) 0.80096(15) -0.03070(9) 0.0331(4) Uani 1 1 d . . . H1 H 0.0692 0.7291 -0.0438 0.040 Uiso 1 1 calc R . . H2 H 0.0447 0.8424 -0.0724 0.040 Uiso 1 1 calc R . . C2 C 0.04759(6) 0.79281(15) 0.00980(9) 0.0330(4) Uani 1 1 d . . . H3 H 0.0435 0.8647 0.0215 0.040 Uiso 1 1 calc R . . H4 H 0.0175 0.7566 -0.0172 0.040 Uiso 1 1 calc R . . C3 C 0.14070(6) 0.82606(15) -0.00934(9) 0.0315(4) Uani 1 1 d . . . H5 H 0.1309 0.8666 -0.0502 0.038 Uiso 1 1 calc R . . H6 H 0.1377 0.7494 -0.0201 0.038 Uiso 1 1 calc R . . C4 C 0.18989(6) 0.85200(14) 0.04747(9) 0.0307(3) Uani 1 1 d . . . C5 C 0.22223(7) 0.86310(18) 0.03450(11) 0.0411(4) Uani 1 1 d . . . H7 H 0.2126 0.8612 -0.0105 0.049 Uiso 1 1 calc R . . C6 C 0.26745(7) 0.87664(18) 0.08705(11) 0.0424(5) Uani 1 1 d . . . H8 H 0.2898 0.8788 0.0792 0.051 Uiso 1 1 calc R . . C7 C 0.32651(7) 0.90409(17) 0.21005(12) 0.0417(5) Uani 1 1 d . . . H9 H 0.3503 0.9043 0.2050 0.050 Uiso 1 1 calc R . . C8 C 0.33693(7) 0.91978(16) 0.27188(12) 0.0424(5) Uani 1 1 d . . . H10 H 0.3680 0.9295 0.3099 0.051 Uiso 1 1 calc R . . C9 C 0.30207(7) 0.92179(16) 0.28010(11) 0.0395(4) Uani 1 1 d . . . H11 H 0.3097 0.9352 0.3234 0.047 Uiso 1 1 calc R . . C10 C 0.25714(6) 0.90455(14) 0.22589(9) 0.0331(4) Uani 1 1 d . . . H12 H 0.2338 0.9067 0.2317 0.040 Uiso 1 1 calc R . . C11 C 0.24588(6) 0.88384(14) 0.16206(9) 0.0291(3) Uani 1 1 d . . . C12 C 0.28057(6) 0.88738(15) 0.15296(10) 0.0350(4) Uani 1 1 d . . . C13 C 0.10745(6) 0.97056(14) 0.01030(9) 0.0296(3) Uani 1 1 d . . . H13 H 0.0786 0.9919 -0.0333 0.036 Uiso 1 1 calc R . . H14 H 0.1331 1.0022 0.0124 0.036 Uiso 1 1 calc R . . C14 C 0.10774(5) 1.01760(14) 0.06609(9) 0.0276(3) Uani 1 1 d . . . C15 C 0.08859(6) 1.12091(15) 0.05412(10) 0.0352(4) Uani 1 1 d . . . H15 H 0.0766 1.1565 0.0128 0.042 Uiso 1 1 calc R . . C16 C 0.08760(6) 1.16837(16) 0.10234(11) 0.0384(4) Uani 1 1 d . . . H16 H 0.0746 1.2371 0.0949 0.046 Uiso 1 1 calc R . . C17 C 0.10327(8) 1.1566(2) 0.21369(12) 0.0478(5) Uani 1 1 d . . . H17 H 0.0898 1.2244 0.2075 0.057 Uiso 1 1 calc R . . C18 C 0.11993(9) 1.1000(2) 0.27099(13) 0.0545(6) Uani 1 1 d . . . H18 H 0.1166 1.1267 0.3035 0.065 Uiso 1 1 calc R . . C19 C 0.14197(9) 1.00269(19) 0.28199(11) 0.0480(5) Uani 1 1 d . . . H19 H 0.1539 0.9645 0.3224 0.058 Uiso 1 1 calc R . . C20 C 0.14667(7) 0.96143(16) 0.23544(10) 0.0374(4) Uani 1 1 d . . . H20 H 0.1634 0.8975 0.2450 0.045 Uiso 1 1 calc R . . C21 C 0.12681(6) 1.01376(14) 0.17345(9) 0.0304(3) Uani 1 1 d . . . C22 C 0.10598(6) 1.11461(16) 0.16336(10) 0.0359(4) Uani 1 1 d . . . C23 C 0.07763(6) 0.75255(15) 0.12730(9) 0.0304(3) Uani 1 1 d . . . H21 H 0.0515 0.7130 0.1195 0.036 Uiso 1 1 calc R . . H22 H 0.0724 0.8293 0.1288 0.036 Uiso 1 1 calc R . . C24 C 0.12155(6) 0.71864(13) 0.19360(9) 0.0280(3) Uani 1 1 d . . . C25 C 0.12158(7) 0.69497(16) 0.24875(10) 0.0352(4) Uani 1 1 d . . . H23 H 0.0935 0.6908 0.2431 0.042 Uiso 1 1 calc R . . C26 C 0.16226(7) 0.67788(17) 0.31068(10) 0.0381(4) Uani 1 1 d . . . H24 H 0.1628 0.6662 0.3489 0.046 Uiso 1 1 calc R . . C27 C 0.24696(7) 0.66042(17) 0.38000(10) 0.0410(4) Uani 1 1 d . . . H25 H 0.2493 0.6507 0.4199 0.049 Uiso 1 1 calc R . . C28 C 0.28547(7) 0.65777(16) 0.38326(10) 0.0420(5) Uani 1 1 d . . . H26 H 0.3146 0.6483 0.4256 0.050 Uiso 1 1 calc R . . C29 C 0.28243(7) 0.66890(16) 0.32445(10) 0.0382(4) Uani 1 1 d . . . H27 H 0.3094 0.6644 0.3270 0.046 Uiso 1 1 calc R . . C30 C 0.24076(6) 0.68623(15) 0.26330(9) 0.0317(4) Uani 1 1 d . . . H28 H 0.2390 0.6925 0.2237 0.038 Uiso 1 1 calc R . . C31 C 0.20075(6) 0.69481(13) 0.25886(9) 0.0271(3) Uani 1 1 d . . . C32 C 0.20343(7) 0.67763(15) 0.31754(9) 0.0325(4) Uani 1 1 d . . . C33 C 0.07639(6) 0.61605(14) 0.05848(10) 0.0335(4) Uani 1 1 d . . . H29 H 0.0456 0.6023 0.0158 0.040 Uiso 1 1 calc R . . H30 H 0.0780 0.5790 0.0950 0.040 Uiso 1 1 calc R . . C34 C 0.11132(6) 0.56755(14) 0.05290(9) 0.0323(4) Uani 1 1 d . . . C35 C 0.10068(8) 0.46423(16) 0.02429(11) 0.0452(5) Uani 1 1 d . . . H31 H 0.0727 0.4309 0.0094 0.054 Uiso 1 1 calc R . . C36 C 0.13076(10) 0.41364(17) 0.01844(12) 0.0514(6) Uani 1 1 d . . . H32 H 0.1240 0.3446 -0.0009 0.062 Uiso 1 1 calc R . . C37 C 0.20456(10) 0.4165(2) 0.03493(14) 0.0568(6) Uani 1 1 d . . . H33 H 0.1984 0.3484 0.0146 0.068 Uiso 1 1 calc R . . C38 C 0.24435(11) 0.4673(2) 0.05776(15) 0.0616(7) Uani 1 1 d . . . H34 H 0.2655 0.4354 0.0525 0.074 Uiso 1 1 calc R . . C39 C 0.25404(9) 0.5671(2) 0.08914(13) 0.0520(6) Uani 1 1 d . . . H35 H 0.2820 0.6020 0.1054 0.062 Uiso 1 1 calc R . . C40 C 0.22346(7) 0.61452(17) 0.09643(11) 0.0399(4) Uani 1 1 d . . . H36 H 0.2309 0.6810 0.1189 0.048 Uiso 1 1 calc R . . C41 C 0.18135(7) 0.56599(15) 0.07115(9) 0.0348(4) Uani 1 1 d . . . C42 C 0.17218(8) 0.46406(16) 0.04118(11) 0.0432(5) Uani 1 1 d . . . C43 C 0.01067(9) 0.0630(3) 0.63647(15) 0.0697(9) Uani 1 1 d . . . C44 C 0.01109(18) 0.1160(6) 0.6885(3) 0.159(3) Uani 1 1 d . . . H37 H -0.0013 0.1879 0.6735 0.238 Uiso 1 1 calc R . . H38 H 0.0426 0.1201 0.7300 0.238 Uiso 1 1 calc R . . H39 H -0.0077 0.0759 0.6974 0.238 Uiso 1 1 calc R . . C45 C 0.10319(10) 0.5460(3) 0.86839(14) 0.0597(7) Uani 1 1 d . . . C46 C 0.07228(12) 0.4570(3) 0.83838(17) 0.0720(8) Uani 1 1 d . . . H40 H 0.0526 0.4639 0.7891 0.108 Uiso 1 1 calc R . . H41 H 0.0533 0.4555 0.8539 0.108 Uiso 1 1 calc R . . H42 H 0.0900 0.3909 0.8516 0.108 Uiso 1 1 calc R . . C47 C 0.0156(3) 0.8244(7) 0.7794(3) 0.0763(18) Uani 0.50 1 d P . . C48 C 0.0000 0.7419(9) 0.7500 0.189(5) Uani 1 2 d S . . 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 0.02166(11) 0.02907(12) 0.02407(11) 0.00216(7) 0.01266(9) -0.00128(7) Cl1 0.0314(2) 0.0412(3) 0.0404(2) -0.00752(19) 0.0195(2) -0.00925(18) Cl2 0.0736(8) 0.0338(4) 0.0383(5) 0.0027(4) 0.0403(6) 0.0040(5) Cl3 0.0347(12) 0.0451(15) 0.0307(11) -0.0048(9) 0.0207(11) -0.0067(10) O1 0.0656(11) 0.0679(12) 0.0595(10) -0.0076(9) 0.0458(9) -0.0073(9) O2 0.0588(10) 0.0632(11) 0.0770(12) -0.0214(9) 0.0471(10) -0.0290(9) O3 0.1068(18) 0.0398(11) 0.173(3) -0.0050(13) 0.102(2) -0.0099(11) O4 0.0509(11) 0.172(3) 0.0425(10) -0.0107(13) 0.0156(9) 0.0166(14) O5 0.1387(19) 0.0378(9) 0.0815(13) -0.0020(9) 0.0922(15) 0.0026(10) O6 0.0867(15) 0.0966(16) 0.0450(10) 0.0111(10) 0.0412(11) -0.0035(12) O7 0.072(2) 0.114(3) 0.0622(18) -0.0003(17) 0.0401(16) -0.0114(18) O8 0.242(6) 0.0456(17) 0.162(4) 0.030(2) 0.179(5) 0.040(2) O9 0.073(4) 0.028(3) 0.041(3) -0.004(2) 0.042(3) 0.004(3) O10 0.037(4) 0.173(14) 0.068(6) -0.006(8) 0.007(4) 0.061(7) N1 0.0273(7) 0.0249(7) 0.0258(7) 0.0002(5) 0.0144(6) -0.0006(5) N2 0.0234(6) 0.0262(7) 0.0298(7) -0.0001(6) 0.0139(6) -0.0013(5) N3 0.0274(7) 0.0262(7) 0.0300(7) 0.0029(5) 0.0181(6) 0.0019(5) N4 0.0261(7) 0.0259(7) 0.0295(7) -0.0018(5) 0.0165(6) -0.0034(5) N5 0.0251(7) 0.0236(7) 0.0287(7) -0.0005(5) 0.0165(6) -0.0004(5) N6 0.0352(7) 0.0260(7) 0.0291(7) 0.0040(6) 0.0199(6) 0.0046(6) N7 0.0443(12) 0.0851(19) 0.0746(17) 0.0049(14) 0.0266(12) -0.0065(12) N8 0.0742(17) 0.100(2) 0.0721(17) -0.0134(16) 0.0494(15) -0.0018(16) N9 0.128(7) 0.153(8) 0.091(5) 0.003(5) 0.063(5) -0.031(6) C1 0.0285(8) 0.0335(9) 0.0253(8) -0.0013(6) 0.0099(7) -0.0044(7) C2 0.0209(8) 0.0344(9) 0.0313(9) 0.0023(7) 0.0093(7) -0.0013(6) C3 0.0367(9) 0.0319(9) 0.0272(8) 0.0017(7) 0.0199(7) 0.0039(7) C4 0.0347(9) 0.0296(8) 0.0315(8) 0.0059(7) 0.0220(7) 0.0049(7) C5 0.0446(10) 0.0498(12) 0.0397(10) 0.0091(9) 0.0312(9) 0.0058(9) C6 0.0400(10) 0.0494(12) 0.0517(12) 0.0107(9) 0.0349(10) 0.0048(9) C7 0.0284(9) 0.0379(10) 0.0574(12) 0.0065(9) 0.0253(9) -0.0003(7) C8 0.0287(9) 0.0333(10) 0.0513(12) -0.0002(8) 0.0168(9) -0.0044(7) C9 0.0357(9) 0.0329(10) 0.0389(10) -0.0053(8) 0.0168(8) -0.0037(7) C10 0.0308(8) 0.0288(9) 0.0365(9) -0.0020(7) 0.0187(8) -0.0013(7) C11 0.0265(8) 0.0241(8) 0.0355(9) 0.0038(6) 0.0181(7) 0.0011(6) C12 0.0322(9) 0.0311(9) 0.0454(10) 0.0066(8) 0.0253(8) 0.0021(7) C13 0.0310(8) 0.0262(8) 0.0293(8) 0.0042(6) 0.0169(7) 0.0028(6) C14 0.0227(7) 0.0261(8) 0.0314(8) -0.0014(6) 0.0148(6) -0.0021(6) C15 0.0311(8) 0.0289(9) 0.0398(9) 0.0021(7) 0.0184(8) 0.0032(7) C16 0.0313(9) 0.0312(9) 0.0495(11) -0.0034(8) 0.0226(9) 0.0029(7) C17 0.0481(12) 0.0469(12) 0.0577(13) -0.0163(10) 0.0368(11) -0.0046(9) C18 0.0659(15) 0.0585(15) 0.0578(14) -0.0210(12) 0.0473(13) -0.0134(12) C19 0.0643(14) 0.0472(12) 0.0417(11) -0.0118(9) 0.0368(11) -0.0187(11) C20 0.0457(10) 0.0335(10) 0.0360(9) -0.0075(7) 0.0262(9) -0.0118(8) C21 0.0284(8) 0.0300(9) 0.0350(9) -0.0069(7) 0.0204(7) -0.0086(7) C22 0.0302(8) 0.0354(10) 0.0455(10) -0.0100(8) 0.0246(8) -0.0059(7) C23 0.0250(8) 0.0322(9) 0.0360(9) 0.0000(7) 0.0194(7) -0.0015(7) C24 0.0291(8) 0.0238(8) 0.0344(9) -0.0015(6) 0.0209(7) -0.0015(6) C25 0.0371(9) 0.0379(10) 0.0420(10) -0.0004(8) 0.0298(9) -0.0015(7) C26 0.0495(11) 0.0382(10) 0.0361(10) 0.0011(8) 0.0308(9) 0.0008(8) C27 0.0492(11) 0.0356(10) 0.0288(9) 0.0026(7) 0.0187(9) 0.0028(8) C28 0.0384(10) 0.0328(10) 0.0330(9) 0.0032(7) 0.0100(8) 0.0061(8) C29 0.0293(9) 0.0329(10) 0.0417(10) 0.0030(8) 0.0158(8) 0.0054(7) C30 0.0305(8) 0.0286(8) 0.0334(9) 0.0017(7) 0.0180(7) 0.0021(7) C31 0.0291(8) 0.0210(7) 0.0284(8) 0.0001(6) 0.0159(7) 0.0000(6) C32 0.0394(9) 0.0270(8) 0.0301(8) -0.0002(7) 0.0204(8) 0.0002(7) C33 0.0316(8) 0.0268(9) 0.0373(9) -0.0028(7) 0.0183(8) -0.0056(7) C34 0.0379(9) 0.0252(8) 0.0287(8) 0.0018(6) 0.0173(7) 0.0016(7) C35 0.0517(12) 0.0282(10) 0.0457(11) -0.0036(8) 0.0241(10) -0.0037(8) C36 0.0746(16) 0.0274(10) 0.0484(12) -0.0035(9) 0.0351(12) 0.0057(10) C37 0.0845(18) 0.0418(12) 0.0595(14) 0.0116(11) 0.0516(14) 0.0264(12) C38 0.0828(19) 0.0574(15) 0.0731(17) 0.0206(13) 0.0620(16) 0.0361(14) C39 0.0573(13) 0.0549(14) 0.0611(14) 0.0209(11) 0.0449(12) 0.0241(11) C40 0.0451(10) 0.0391(10) 0.0445(10) 0.0136(8) 0.0317(9) 0.0145(8) C41 0.0446(10) 0.0309(9) 0.0322(9) 0.0093(7) 0.0249(8) 0.0133(8) C42 0.0630(13) 0.0312(10) 0.0410(10) 0.0076(8) 0.0344(10) 0.0151(9) C43 0.0395(13) 0.101(2) 0.0536(15) -0.0011(15) 0.0202(12) -0.0286(14) C44 0.116(4) 0.284(9) 0.100(3) -0.081(4) 0.078(3) -0.102(5) C45 0.0577(15) 0.0785(19) 0.0502(13) 0.0025(13) 0.0364(13) 0.0163(14) C46 0.091(2) 0.0727(19) 0.0734(19) -0.0048(15) 0.0605(18) 0.0035(16) C47 0.084(4) 0.101(5) 0.057(3) -0.009(4) 0.049(3) -0.020(4) C48 0.366(18) 0.119(7) 0.208(11) 0.000 0.239(13) 0.000 _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 N5 2.1271(14) . ? Zn1 N1 2.1497(14) . ? Zn1 N3 2.1543(14) . ? Zn1 N2 2.1681(14) . ? Zn1 N6 2.3711(15) . ? Zn1 N4 2.4007(15) . ? Cl1 O4 1.418(2) . ? Cl1 O3 1.422(2) . ? Cl1 O2 1.4225(17) . ? Cl1 O1 1.4439(18) . ? Cl2 Cl3 0.598(2) . ? Cl2 O10 1.061(9) . ? Cl2 O8 1.420(3) . ? Cl2 O6 1.427(2) . ? Cl2 O7 1.451(4) . ? Cl2 O5 1.468(2) . ? Cl2 O9 1.846(7) . ? Cl3 O6 1.316(4) . ? Cl3 O9 1.353(7) . ? Cl3 O5 1.395(3) . ? Cl3 O8 1.409(5) . ? Cl3 O10 1.483(7) . ? Cl3 O7 2.045(4) . ? O7 O10 1.323(19) . ? O8 O10 1.105(16) . ? O8 O9 1.406(8) . ? N1 C3 1.469(2) . ? N1 C13 1.477(2) . ? N1 C1 1.479(2) . ? N2 C23 1.465(2) . ? N2 C33 1.478(2) . ? N2 C2 1.483(2) . ? N3 C4 1.328(2) . ? N3 C11 1.382(2) . ? N4 C14 1.322(2) . ? N4 C21 1.387(2) . ? N5 C24 1.331(2) . ? N5 C31 1.380(2) . ? N6 C34 1.321(2) . ? N6 C41 1.390(2) . ? N7 C43 1.116(4) . ? N8 C45 1.143(4) . ? N9 C47 1.121(11) . ? C1 C2 1.521(3) . ? C1 H1 0.9900 . ? C1 H2 0.9900 . ? C2 H3 0.9900 . ? C2 H4 0.9900 . ? C3 C4 1.507(3) . ? C3 H5 0.9900 . ? C3 H6 0.9900 . ? C4 C5 1.409(3) . ? C5 C6 1.365(3) . ? C5 H7 0.9500 . ? C6 C12 1.408(3) . ? C6 H8 0.9500 . ? C7 C8 1.356(3) . ? C7 C12 1.416(3) . ? C7 H9 0.9500 . ? C8 C9 1.409(3) . ? C8 H10 0.9500 . ? C9 C10 1.375(3) . ? C9 H11 0.9500 . ? C10 C11 1.402(3) . ? C10 H12 0.9500 . ? C11 C12 1.418(2) . ? C13 C14 1.502(2) . ? C13 H13 0.9900 . ? C13 H14 0.9900 . ? C14 C15 1.421(2) . ? C15 C16 1.359(3) . ? C15 H15 0.9500 . ? C16 C22 1.407(3) . ? C16 H16 0.9500 . ? C17 C18 1.364(4) . ? C17 C22 1.416(3) . ? C17 H17 0.9500 . ? C18 C19 1.400(4) . ? C18 H18 0.9500 . ? C19 C20 1.371(3) . ? C19 H19 0.9500 . ? C20 C21 1.409(3) . ? C20 H20 0.9500 . ? C21 C22 1.423(3) . ? C23 C24 1.511(2) . ? C23 H21 0.9900 . ? C23 H22 0.9900 . ? C24 C25 1.402(3) . ? C25 C26 1.366(3) . ? C25 H23 0.9500 . ? C26 C32 1.410(3) . ? C26 H24 0.9500 . ? C27 C28 1.362(3) . ? C27 C32 1.417(3) . ? C27 H25 0.9500 . ? C28 C29 1.405(3) . ? C28 H26 0.9500 . ? C29 C30 1.373(3) . ? C29 H27 0.9500 . ? C30 C31 1.404(3) . ? C30 H28 0.9500 . ? C31 C32 1.419(2) . ? C33 C34 1.497(3) . ? C33 H29 0.9900 . ? C33 H30 0.9900 . ? C34 C35 1.419(3) . ? C35 C36 1.354(3) . ? C35 H31 0.9500 . ? C36 C42 1.409(4) . ? C36 H32 0.9500 . ? C37 C38 1.362(4) . ? C37 C42 1.418(3) . ? C37 H33 0.9500 . ? C38 C39 1.406(4) . ? C38 H34 0.9500 . ? C39 C40 1.374(3) . ? C39 H35 0.9500 . ? C40 C41 1.405(3) . ? C40 H36 0.9500 . ? C41 C42 1.418(3) . ? C43 C44 1.449(6) . ? C44 H37 0.9800 . ? C44 H38 0.9800 . ? C44 H39 0.9800 . ? C45 C46 1.440(5) . ? C46 H40 0.9800 . ? C46 H41 0.9800 . ? C46 H42 0.9800 . ? C47 C47 1.195(14) 2_556 ? C47 C48 1.198(11) . ? C48 C47 1.198(11) 2_556 ? 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 N5 Zn1 N1 159.40(6) . . ? N5 Zn1 N3 124.25(5) . . ? N1 Zn1 N3 76.21(5) . . ? N5 Zn1 N2 77.65(6) . . ? N1 Zn1 N2 82.17(6) . . ? N3 Zn1 N2 157.73(6) . . ? N5 Zn1 N6 87.63(5) . . ? N1 Zn1 N6 92.18(5) . . ? N3 Zn1 N6 97.41(5) . . ? N2 Zn1 N6 77.96(5) . . ? N5 Zn1 N4 98.01(5) . . ? N1 Zn1 N4 78.00(5) . . ? N3 Zn1 N4 90.06(5) . . ? N2 Zn1 N4 90.63(5) . . ? N6 Zn1 N4 165.94(5) . . ? O4 Cl1 O3 109.06(19) . . ? O4 Cl1 O2 110.10(16) . . ? O3 Cl1 O2 107.62(14) . . ? O4 Cl1 O1 109.08(13) . . ? O3 Cl1 O1 110.94(15) . . ? O2 Cl1 O1 110.02(11) . . ? Cl3 Cl2 O10 124.3(11) . . ? Cl3 Cl2 O8 76.8(5) . . ? O10 Cl2 O8 50.4(9) . . ? Cl3 Cl2 O6 67.1(4) . . ? O10 Cl2 O6 144.6(6) . . ? O8 Cl2 O6 114.1(3) . . ? Cl3 Cl2 O7 172.2(4) . . ? O10 Cl2 O7 61.3(10) . . ? O8 Cl2 O7 106.5(3) . . ? O6 Cl2 O7 105.13(18) . . ? Cl3 Cl2 O5 71.2(4) . . ? O10 Cl2 O5 108.4(7) . . ? O8 Cl2 O5 110.84(16) . . ? O6 Cl2 O5 106.98(16) . . ? O7 Cl2 O5 113.31(18) . . ? Cl3 Cl2 O9 28.9(4) . . ? O10 Cl2 O9 98.7(10) . . ? O8 Cl2 O9 48.9(3) . . ? O6 Cl2 O9 79.4(2) . . ? O7 Cl2 O9 151.9(3) . . ? O5 Cl2 O9 90.9(2) . . ? Cl2 Cl3 O6 88.1(4) . . ? Cl2 Cl3 O9 138.8(6) . . ? O6 Cl3 O9 104.8(3) . . ? Cl2 Cl3 O5 84.9(4) . . ? O6 Cl3 O5 118.3(3) . . ? O9 Cl3 O5 119.7(3) . . ? Cl2 Cl3 O8 78.8(5) . . ? O6 Cl3 O8 122.5(3) . . ? O9 Cl3 O8 61.2(4) . . ? O5 Cl3 O8 115.9(3) . . ? Cl2 Cl3 O10 36.2(8) . . ? O6 Cl3 O10 115.8(7) . . ? O9 Cl3 O10 105.9(7) . . ? O5 Cl3 O10 91.6(5) . . ? O8 Cl3 O10 44.9(6) . . ? Cl2 Cl3 O7 5.5(3) . . ? O6 Cl3 O7 82.6(2) . . ? O9 Cl3 O7 139.8(4) . . ? O5 Cl3 O7 88.2(2) . . ? O8 Cl3 O7 81.2(3) . . ? O10 Cl3 O7 40.2(7) . . ? Cl3 O5 Cl2 23.95(9) . . ? Cl3 O6 Cl2 24.77(10) . . ? O10 O7 Cl2 44.7(3) . . ? O10 O7 Cl3 46.4(3) . . ? Cl2 O7 Cl3 2.28(12) . . ? O10 O8 O9 128.3(6) . . ? O10 O8 Cl3 71.1(5) . . ? O9 O8 Cl3 57.4(3) . . ? O10 O8 Cl2 47.7(5) . . ? O9 O8 Cl2 81.6(3) . . ? Cl3 O8 Cl2 24.42(10) . . ? Cl3 O9 O8 61.4(4) . . ? Cl3 O9 Cl2 12.32(18) . . ? O8 O9 Cl2 49.5(2) . . ? Cl2 O10 O8 81.9(8) . . ? Cl2 O10 O7 74.1(10) . . ? O8 O10 O7 142.3(11) . . ? Cl2 O10 Cl3 19.5(3) . . ? O8 O10 Cl3 64.1(6) . . ? O7 O10 Cl3 93.4(8) . . ? C3 N1 C13 108.87(14) . . ? C3 N1 C1 113.37(14) . . ? C13 N1 C1 112.17(14) . . ? C3 N1 Zn1 103.81(10) . . ? C13 N1 Zn1 111.13(10) . . ? C1 N1 Zn1 107.17(11) . . ? C23 N2 C33 109.63(14) . . ? C23 N2 C2 114.13(14) . . ? C33 N2 C2 111.41(14) . . ? C23 N2 Zn1 102.98(10) . . ? C33 N2 Zn1 112.29(11) . . ? C2 N2 Zn1 106.11(11) . . ? C4 N3 C11 118.56(15) . . ? C4 N3 Zn1 110.25(12) . . ? C11 N3 Zn1 129.14(12) . . ? C14 N4 C21 117.47(15) . . ? C14 N4 Zn1 108.63(11) . . ? C21 N4 Zn1 133.46(12) . . ? C24 N5 C31 118.80(15) . . ? C24 N5 Zn1 111.34(12) . . ? C31 N5 Zn1 128.85(12) . . ? C34 N6 C41 117.50(16) . . ? C34 N6 Zn1 109.93(12) . . ? C41 N6 Zn1 132.47(13) . . ? N1 C1 C2 109.29(14) . . ? N1 C1 H1 109.8 . . ? C2 C1 H1 109.8 . . ? N1 C1 H2 109.8 . . ? C2 C1 H2 109.8 . . ? H1 C1 H2 108.3 . . ? N2 C2 C1 108.55(15) . . ? N2 C2 H3 110.0 . . ? C1 C2 H3 110.0 . . ? N2 C2 H4 110.0 . . ? C1 C2 H4 110.0 . . ? H3 C2 H4 108.4 . . ? N1 C3 C4 109.47(14) . . ? N1 C3 H5 109.8 . . ? C4 C3 H5 109.8 . . ? N1 C3 H6 109.8 . . ? C4 C3 H6 109.8 . . ? H5 C3 H6 108.2 . . ? N3 C4 C5 122.68(17) . . ? N3 C4 C3 117.27(15) . . ? C5 C4 C3 120.01(16) . . ? C6 C5 C4 119.58(18) . . ? C6 C5 H7 120.2 . . ? C4 C5 H7 120.2 . . ? C5 C6 C12 119.37(18) . . ? C5 C6 H8 120.3 . . ? C12 C6 H8 120.3 . . ? C8 C7 C12 120.58(19) . . ? C8 C7 H9 119.7 . . ? C12 C7 H9 119.7 . . ? C7 C8 C9 120.50(18) . . ? C7 C8 H10 119.7 . . ? C9 C8 H10 119.7 . . ? C10 C9 C8 120.4(2) . . ? C10 C9 H11 119.8 . . ? C8 C9 H11 119.8 . . ? C9 C10 C11 119.92(18) . . ? C9 C10 H12 120.0 . . ? C11 C10 H12 120.0 . . ? N3 C11 C10 119.29(16) . . ? N3 C11 C12 121.04(17) . . ? C10 C11 C12 119.67(17) . . ? C6 C12 C7 123.02(18) . . ? C6 C12 C11 118.24(17) . . ? C7 C12 C11 118.71(18) . . ? N1 C13 C14 116.15(14) . . ? N1 C13 H13 108.2 . . ? C14 C13 H13 108.2 . . ? N1 C13 H14 108.2 . . ? C14 C13 H14 108.2 . . ? H13 C13 H14 107.4 . . ? N4 C14 C15 123.67(17) . . ? N4 C14 C13 120.17(15) . . ? C15 C14 C13 116.08(16) . . ? C16 C15 C14 119.33(18) . . ? C16 C15 H15 120.3 . . ? C14 C15 H15 120.3 . . ? C15 C16 C22 119.32(18) . . ? C15 C16 H16 120.3 . . ? C22 C16 H16 120.3 . . ? C18 C17 C22 120.2(2) . . ? C18 C17 H17 119.9 . . ? C22 C17 H17 119.9 . . ? C17 C18 C19 120.2(2) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? C20 C19 C18 121.2(2) . . ? C20 C19 H19 119.4 . . ? C18 C19 H19 119.4 . . ? C19 C20 C21 120.1(2) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? N4 C21 C20 119.79(17) . . ? N4 C21 C22 121.68(17) . . ? C20 C21 C22 118.52(17) . . ? C16 C22 C17 122.0(2) . . ? C16 C22 C21 118.39(17) . . ? C17 C22 C21 119.6(2) . . ? N2 C23 C24 109.75(14) . . ? N2 C23 H21 109.7 . . ? C24 C23 H21 109.7 . . ? N2 C23 H22 109.7 . . ? C24 C23 H22 109.7 . . ? H21 C23 H22 108.2 . . ? N5 C24 C25 122.65(17) . . ? N5 C24 C23 117.23(15) . . ? C25 C24 C23 119.93(16) . . ? C26 C25 C24 119.51(17) . . ? C26 C25 H23 120.2 . . ? C24 C25 H23 120.2 . . ? C25 C26 C32 119.64(17) . . ? C25 C26 H24 120.2 . . ? C32 C26 H24 120.2 . . ? C28 C27 C32 120.48(19) . . ? C28 C27 H25 119.8 . . ? C32 C27 H25 119.8 . . ? C27 C28 C29 120.44(18) . . ? C27 C28 H26 119.8 . . ? C29 C28 H26 119.8 . . ? C30 C29 C28 120.34(19) . . ? C30 C29 H27 119.8 . . ? C28 C29 H27 119.8 . . ? C29 C30 C31 120.50(18) . . ? C29 C30 H28 119.7 . . ? C31 C30 H28 119.7 . . ? N5 C31 C30 119.91(16) . . ? N5 C31 C32 120.99(16) . . ? C30 C31 C32 119.09(16) . . ? C26 C32 C27 123.03(18) . . ? C26 C32 C31 118.03(17) . . ? C27 C32 C31 118.93(18) . . ? N2 C33 C34 116.37(15) . . ? N2 C33 H29 108.2 . . ? C34 C33 H29 108.2 . . ? N2 C33 H30 108.2 . . ? C34 C33 H30 108.2 . . ? H29 C33 H30 107.3 . . ? N6 C34 C35 123.68(19) . . ? N6 C34 C33 120.89(16) . . ? C35 C34 C33 115.39(18) . . ? C36 C35 C34 119.3(2) . . ? C36 C35 H31 120.3 . . ? C34 C35 H31 120.3 . . ? C35 C36 C42 119.5(2) . . ? C35 C36 H32 120.2 . . ? C42 C36 H32 120.2 . . ? C38 C37 C42 120.7(2) . . ? C38 C37 H33 119.7 . . ? C42 C37 H33 119.7 . . ? C37 C38 C39 119.9(2) . . ? C37 C38 H34 120.0 . . ? C39 C38 H34 120.0 . . ? C40 C39 C38 120.6(3) . . ? C40 C39 H35 119.7 . . ? C38 C39 H35 119.7 . . ? C39 C40 C41 120.9(2) . . ? C39 C40 H36 119.6 . . ? C41 C40 H36 119.6 . . ? N6 C41 C40 119.98(18) . . ? N6 C41 C42 121.58(19) . . ? C40 C41 C42 118.44(19) . . ? C36 C42 C37 122.3(2) . . ? C36 C42 C41 118.3(2) . . ? C37 C42 C41 119.4(2) . . ? N7 C43 C44 177.0(5) . . ? C43 C44 H37 109.5 . . ? C43 C44 H38 109.5 . . ? H37 C44 H38 109.5 . . ? C43 C44 H39 109.5 . . ? H37 C44 H39 109.5 . . ? H38 C44 H39 109.5 . . ? N8 C45 C46 179.9(6) . . ? C45 C46 H40 109.5 . . ? C45 C46 H41 109.5 . . ? H40 C46 H41 109.5 . . ? C45 C46 H42 109.5 . . ? H40 C46 H42 109.5 . . ? H41 C46 H42 109.5 . . ? N9 C47 C47 133.5(6) . 2_556 ? N9 C47 C48 165.7(10) . . ? C47 C47 C48 60.1(4) 2_556 . ? C47 C48 C47 59.8(9) . 2_556 ? 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 O10 Cl2 Cl3 O6 -141.5(8) . . . . ? O8 Cl2 Cl3 O6 -123.7(2) . . . . ? O7 Cl2 Cl3 O6 -8(3) . . . . ? O5 Cl2 Cl3 O6 118.6(2) . . . . ? O9 Cl2 Cl3 O6 -110.6(7) . . . . ? O10 Cl2 Cl3 O9 -30.9(12) . . . . ? O8 Cl2 Cl3 O9 -13.1(7) . . . . ? O6 Cl2 Cl3 O9 110.6(7) . . . . ? O7 Cl2 Cl3 O9 103(3) . . . . ? O5 Cl2 Cl3 O9 -130.8(8) . . . . ? O10 Cl2 Cl3 O5 99.9(8) . . . . ? O8 Cl2 Cl3 O5 117.8(2) . . . . ? O6 Cl2 Cl3 O5 -118.6(2) . . . . ? O7 Cl2 Cl3 O5 -126(3) . . . . ? O9 Cl2 Cl3 O5 130.8(8) . . . . ? O10 Cl2 Cl3 O8 -17.9(8) . . . . ? O6 Cl2 Cl3 O8 123.7(2) . . . . ? O7 Cl2 Cl3 O8 116(3) . . . . ? O5 Cl2 Cl3 O8 -117.8(2) . . . . ? O9 Cl2 Cl3 O8 13.1(7) . . . . ? O8 Cl2 Cl3 O10 17.9(8) . . . . ? O6 Cl2 Cl3 O10 141.5(8) . . . . ? O7 Cl2 Cl3 O10 134(3) . . . . ? O5 Cl2 Cl3 O10 -99.9(8) . . . . ? O9 Cl2 Cl3 O10 30.9(12) . . . . ? O10 Cl2 Cl3 O7 -134(3) . . . . ? O8 Cl2 Cl3 O7 -116(3) . . . . ? O6 Cl2 Cl3 O7 8(3) . . . . ? O5 Cl2 Cl3 O7 126(3) . . . . ? O9 Cl2 Cl3 O7 -103(3) . . . . ? O6 Cl3 O5 Cl2 -85.1(4) . . . . ? O9 Cl3 O5 Cl2 145.0(7) . . . . ? O8 Cl3 O5 Cl2 74.8(5) . . . . ? O10 Cl3 O5 Cl2 35.6(8) . . . . ? O7 Cl3 O5 Cl2 -4.5(3) . . . . ? O10 Cl2 O5 Cl3 -120.9(11) . . . . ? O8 Cl2 O5 Cl3 -67.2(5) . . . . ? O6 Cl2 O5 Cl3 57.8(4) . . . . ? O7 Cl2 O5 Cl3 173.1(5) . . . . ? O9 Cl2 O5 Cl3 -21.4(4) . . . . ? O9 Cl3 O6 Cl2 -140.4(6) . . . . ? O5 Cl3 O6 Cl2 83.1(4) . . . . ? O8 Cl3 O6 Cl2 -75.4(5) . . . . ? O10 Cl3 O6 Cl2 -24.1(7) . . . . ? O7 Cl3 O6 Cl2 -0.7(3) . . . . ? O10 Cl2 O6 Cl3 117.5(18) . . . . ? O8 Cl2 O6 Cl3 62.6(5) . . . . ? O7 Cl2 O6 Cl3 178.9(5) . . . . ? O5 Cl2 O6 Cl3 -60.3(4) . . . . ? O9 Cl2 O6 Cl3 27.4(4) . . . . ? Cl3 Cl2 O7 O10 -137(3) . . . . ? O8 Cl2 O7 O10 -23.1(7) . . . . ? O6 Cl2 O7 O10 -144.5(7) . . . . ? O5 Cl2 O7 O10 99.0(7) . . . . ? O9 Cl2 O7 O10 -48.7(9) . . . . ? O10 Cl2 O7 Cl3 137(3) . . . . ? O8 Cl2 O7 Cl3 114(3) . . . . ? O6 Cl2 O7 Cl3 -7(3) . . . . ? O5 Cl2 O7 Cl3 -124(3) . . . . ? O9 Cl2 O7 Cl3 88(3) . . . . ? Cl2 Cl3 O7 O10 41(3) . . . . ? O6 Cl3 O7 O10 -146.5(7) . . . . ? O9 Cl3 O7 O10 -42.1(8) . . . . ? O5 Cl3 O7 O10 94.7(7) . . . . ? O8 Cl3 O7 O10 -21.9(7) . . . . ? O6 Cl3 O7 Cl2 172(3) . . . . ? O9 Cl3 O7 Cl2 -83(3) . . . . ? O5 Cl3 O7 Cl2 53(3) . . . . ? O8 Cl3 O7 Cl2 -63(3) . . . . ? O10 Cl3 O7 Cl2 -41(3) . . . . ? Cl2 Cl3 O8 O10 14.9(8) . . . . ? O6 Cl3 O8 O10 95.3(9) . . . . ? O9 Cl3 O8 O10 -174.9(9) . . . . ? O5 Cl3 O8 O10 -63.7(8) . . . . ? O7 Cl3 O8 O10 19.9(8) . . . . ? Cl2 Cl3 O8 O9 -170.2(5) . . . . ? O6 Cl3 O8 O9 -89.8(4) . . . . ? O5 Cl3 O8 O9 111.2(4) . . . . ? O10 Cl3 O8 O9 174.9(9) . . . . ? O7 Cl3 O8 O9 -165.2(3) . . . . ? O6 Cl3 O8 Cl2 80.4(4) . . . . ? O9 Cl3 O8 Cl2 170.2(5) . . . . ? O5 Cl3 O8 Cl2 -78.6(4) . . . . ? O10 Cl3 O8 Cl2 -14.9(8) . . . . ? O7 Cl3 O8 Cl2 5.0(3) . . . . ? Cl3 Cl2 O8 O10 -160.8(10) . . . . ? O6 Cl2 O8 O10 142.0(10) . . . . ? O7 Cl2 O8 O10 26.5(10) . . . . ? O5 Cl2 O8 O10 -97.1(10) . . . . ? O9 Cl2 O8 O10 -169.1(10) . . . . ? Cl3 Cl2 O8 O9 8.3(4) . . . . ? O10 Cl2 O8 O9 169.1(10) . . . . ? O6 Cl2 O8 O9 -48.8(3) . . . . ? O7 Cl2 O8 O9 -164.4(3) . . . . ? O5 Cl2 O8 O9 72.0(3) . . . . ? O10 Cl2 O8 Cl3 160.8(10) . . . . ? O6 Cl2 O8 Cl3 -57.2(4) . . . . ? O7 Cl2 O8 Cl3 -172.7(4) . . . . ? O5 Cl2 O8 Cl3 63.7(4) . . . . ? O9 Cl2 O8 Cl3 -8.3(4) . . . . ? Cl2 Cl3 O9 O8 14.6(7) . . . . ? O6 Cl3 O9 O8 119.2(3) . . . . ? O5 Cl3 O9 O8 -105.1(4) . . . . ? O10 Cl3 O9 O8 -3.8(6) . . . . ? O7 Cl3 O9 O8 23.0(5) . . . . ? O6 Cl3 O9 Cl2 104.6(8) . . . . ? O5 Cl3 O9 Cl2 -119.8(9) . . . . ? O8 Cl3 O9 Cl2 -14.6(7) . . . . ? O10 Cl3 O9 Cl2 -18.4(8) . . . . ? O7 Cl3 O9 Cl2 8.4(4) . . . . ? O10 O8 O9 Cl3 6.2(11) . . . . ? Cl2 O8 O9 Cl3 -4.1(2) . . . . ? O10 O8 O9 Cl2 10.3(10) . . . . ? Cl3 O8 O9 Cl2 4.1(2) . . . . ? O10 Cl2 O9 Cl3 154.6(10) . . . . ? O8 Cl2 O9 Cl3 163.0(9) . . . . ? O6 Cl2 O9 Cl3 -61.3(7) . . . . ? O7 Cl2 O9 Cl3 -163.6(8) . . . . ? O5 Cl2 O9 Cl3 45.8(7) . . . . ? Cl3 Cl2 O9 O8 -163.0(9) . . . . ? O10 Cl2 O9 O8 -8.5(7) . . . . ? O6 Cl2 O9 O8 135.6(3) . . . . ? O7 Cl2 O9 O8 33.3(6) . . . . ? O5 Cl2 O9 O8 -117.3(3) . . . . ? Cl3 Cl2 O10 O8 22.8(11) . . . . ? O6 Cl2 O10 O8 -75.7(19) . . . . ? O7 Cl2 O10 O8 -150.8(9) . . . . ? O5 Cl2 O10 O8 102.2(6) . . . . ? O9 Cl2 O10 O8 8.3(8) . . . . ? Cl3 Cl2 O10 O7 173.6(5) . . . . ? O8 Cl2 O10 O7 150.8(9) . . . . ? O6 Cl2 O10 O7 75.1(15) . . . . ? O5 Cl2 O10 O7 -107.0(5) . . . . ? O9 Cl2 O10 O7 159.0(4) . . . . ? O8 Cl2 O10 Cl3 -22.8(11) . . . . ? O6 Cl2 O10 Cl3 -98.5(16) . . . . ? O7 Cl2 O10 Cl3 -173.6(5) . . . . ? O5 Cl2 O10 Cl3 79.4(7) . . . . ? O9 Cl2 O10 Cl3 -14.5(6) . . . . ? O9 O8 O10 Cl2 -13.8(13) . . . . ? Cl3 O8 O10 Cl2 -8.3(4) . . . . ? O9 O8 O10 O7 -64.0(18) . . . . ? Cl3 O8 O10 O7 -58.5(12) . . . . ? Cl2 O8 O10 O7 -50.3(11) . . . . ? O9 O8 O10 Cl3 -5.5(10) . . . . ? Cl2 O8 O10 Cl3 8.3(4) . . . . ? Cl3 O7 O10 Cl2 -2.14(16) . . . . ? Cl2 O7 O10 O8 52.3(11) . . . . ? Cl3 O7 O10 O8 50.2(11) . . . . ? Cl2 O7 O10 Cl3 2.14(16) . . . . ? O6 Cl3 O10 Cl2 43.7(8) . . . . ? O9 Cl3 O10 Cl2 159.4(8) . . . . ? O5 Cl3 O10 Cl2 -79.0(7) . . . . ? O8 Cl3 O10 Cl2 154.7(12) . . . . ? O7 Cl3 O10 Cl2 6.2(5) . . . . ? Cl2 Cl3 O10 O8 -154.7(12) . . . . ? O6 Cl3 O10 O8 -111.0(8) . . . . ? O9 Cl3 O10 O8 4.7(8) . . . . ? O5 Cl3 O10 O8 126.3(6) . . . . ? O7 Cl3 O10 O8 -148.5(10) . . . . ? Cl2 Cl3 O10 O7 -6.2(5) . . . . ? O6 Cl3 O10 O7 37.5(8) . . . . ? O9 Cl3 O10 O7 153.2(5) . . . . ? O5 Cl3 O10 O7 -85.2(6) . . . . ? O8 Cl3 O10 O7 148.5(10) . . . . ? N5 Zn1 N1 C3 -144.99(15) . . . . ? N3 Zn1 N1 C3 41.19(11) . . . . ? N2 Zn1 N1 C3 -133.43(11) . . . . ? N6 Zn1 N1 C3 -55.91(11) . . . . ? N4 Zn1 N1 C3 134.25(11) . . . . ? N5 Zn1 N1 C13 98.13(18) . . . . ? N3 Zn1 N1 C13 -75.68(11) . . . . ? N2 Zn1 N1 C13 109.69(12) . . . . ? N6 Zn1 N1 C13 -172.78(11) . . . . ? N4 Zn1 N1 C13 17.37(11) . . . . ? N5 Zn1 N1 C1 -24.8(2) . . . . ? N3 Zn1 N1 C1 161.43(12) . . . . ? N2 Zn1 N1 C1 -13.19(11) . . . . ? N6 Zn1 N1 C1 64.33(12) . . . . ? N4 Zn1 N1 C1 -105.52(12) . . . . ? N5 Zn1 N2 C23 38.71(10) . . . . ? N1 Zn1 N2 C23 -137.15(11) . . . . ? N3 Zn1 N2 C23 -151.04(14) . . . . ? N6 Zn1 N2 C23 128.92(11) . . . . ? N4 Zn1 N2 C23 -59.35(11) . . . . ? N5 Zn1 N2 C33 -79.13(12) . . . . ? N1 Zn1 N2 C33 105.01(12) . . . . ? N3 Zn1 N2 C33 91.12(18) . . . . ? N6 Zn1 N2 C33 11.07(12) . . . . ? N4 Zn1 N2 C33 -177.20(12) . . . . ? N5 Zn1 N2 C2 158.93(12) . . . . ? N1 Zn1 N2 C2 -16.93(11) . . . . ? N3 Zn1 N2 C2 -30.8(2) . . . . ? N6 Zn1 N2 C2 -110.87(12) . . . . ? N4 Zn1 N2 C2 60.86(12) . . . . ? N5 Zn1 N3 C4 150.78(11) . . . . ? N1 Zn1 N3 C4 -31.85(12) . . . . ? N2 Zn1 N3 C4 -17.7(2) . . . . ? N6 Zn1 N3 C4 58.59(12) . . . . ? N4 Zn1 N3 C4 -109.47(12) . . . . ? N5 Zn1 N3 C11 -12.39(17) . . . . ? N1 Zn1 N3 C11 164.98(15) . . . . ? N2 Zn1 N3 C11 179.16(14) . . . . ? N6 Zn1 N3 C11 -104.58(15) . . . . ? N4 Zn1 N3 C11 87.36(15) . . . . ? N5 Zn1 N4 C14 -165.31(11) . . . . ? N1 Zn1 N4 C14 -5.84(11) . . . . ? N3 Zn1 N4 C14 70.04(11) . . . . ? N2 Zn1 N4 C14 -87.70(11) . . . . ? N6 Zn1 N4 C14 -52.3(3) . . . . ? N5 Zn1 N4 C21 6.56(15) . . . . ? N1 Zn1 N4 C21 166.03(16) . . . . ? N3 Zn1 N4 C21 -118.08(15) . . . . ? N2 Zn1 N4 C21 84.18(15) . . . . ? N6 Zn1 N4 C21 119.6(2) . . . . ? N1 Zn1 N5 C24 -14.5(2) . . . . ? N3 Zn1 N5 C24 158.19(11) . . . . ? N2 Zn1 N5 C24 -26.27(11) . . . . ? N6 Zn1 N5 C24 -104.45(12) . . . . ? N4 Zn1 N5 C24 62.61(12) . . . . ? N1 Zn1 N5 C31 177.27(14) . . . . ? N3 Zn1 N5 C31 -10.00(16) . . . . ? N2 Zn1 N5 C31 165.55(15) . . . . ? N6 Zn1 N5 C31 87.36(14) . . . . ? N4 Zn1 N5 C31 -105.57(14) . . . . ? N5 Zn1 N6 C34 74.80(12) . . . . ? N1 Zn1 N6 C34 -84.58(12) . . . . ? N3 Zn1 N6 C34 -160.96(12) . . . . ? N2 Zn1 N6 C34 -3.07(12) . . . . ? N4 Zn1 N6 C34 -39.4(3) . . . . ? N5 Zn1 N6 C41 -109.23(16) . . . . ? N1 Zn1 N6 C41 91.38(16) . . . . ? N3 Zn1 N6 C41 15.01(16) . . . . ? N2 Zn1 N6 C41 172.90(16) . . . . ? N4 Zn1 N6 C41 136.6(2) . . . . ? C3 N1 C1 C2 155.09(15) . . . . ? C13 N1 C1 C2 -81.09(17) . . . . ? Zn1 N1 C1 C2 41.15(16) . . . . ? C23 N2 C2 C1 156.58(14) . . . . ? C33 N2 C2 C1 -78.60(17) . . . . ? Zn1 N2 C2 C1 43.90(15) . . . . ? N1 C1 C2 N2 -58.83(18) . . . . ? C13 N1 C3 C4 73.10(17) . . . . ? C1 N1 C3 C4 -161.29(14) . . . . ? Zn1 N1 C3 C4 -45.35(15) . . . . ? C11 N3 C4 C5 2.6(3) . . . . ? Zn1 N3 C4 C5 -162.54(16) . . . . ? C11 N3 C4 C3 -179.75(15) . . . . ? Zn1 N3 C4 C3 15.06(19) . . . . ? N1 C3 C4 N3 21.3(2) . . . . ? N1 C3 C4 C5 -160.99(17) . . . . ? N3 C4 C5 C6 3.7(3) . . . . ? C3 C4 C5 C6 -173.86(19) . . . . ? C4 C5 C6 C12 -4.8(3) . . . . ? C12 C7 C8 C9 -1.3(3) . . . . ? C7 C8 C9 C10 2.1(3) . . . . ? C8 C9 C10 C11 0.6(3) . . . . ? C4 N3 C11 C10 172.60(16) . . . . ? Zn1 N3 C11 C10 -25.4(2) . . . . ? C4 N3 C11 C12 -7.7(2) . . . . ? Zn1 N3 C11 C12 154.25(13) . . . . ? C9 C10 C11 N3 175.75(17) . . . . ? C9 C10 C11 C12 -3.9(3) . . . . ? C5 C6 C12 C7 -178.5(2) . . . . ? C5 C6 C12 C11 -0.1(3) . . . . ? C8 C7 C12 C6 176.3(2) . . . . ? C8 C7 C12 C11 -2.1(3) . . . . ? N3 C11 C12 C6 6.5(3) . . . . ? C10 C11 C12 C6 -173.82(18) . . . . ? N3 C11 C12 C7 -175.03(17) . . . . ? C10 C11 C12 C7 4.6(3) . . . . ? C3 N1 C13 C14 -141.36(15) . . . . ? C1 N1 C13 C14 92.34(18) . . . . ? Zn1 N1 C13 C14 -27.62(18) . . . . ? C21 N4 C14 C15 2.6(2) . . . . ? Zn1 N4 C14 C15 175.94(14) . . . . ? C21 N4 C14 C13 179.12(15) . . . . ? Zn1 N4 C14 C13 -7.52(18) . . . . ? N1 C13 C14 N4 24.1(2) . . . . ? N1 C13 C14 C15 -159.08(15) . . . . ? N4 C14 C15 C16 -3.5(3) . . . . ? C13 C14 C15 C16 179.86(17) . . . . ? C14 C15 C16 C22 0.6(3) . . . . ? C22 C17 C18 C19 3.4(4) . . . . ? C17 C18 C19 C20 -1.0(4) . . . . ? C18 C19 C20 C21 -3.8(3) . . . . ? C14 N4 C21 C20 179.57(16) . . . . ? Zn1 N4 C21 C20 8.3(2) . . . . ? C14 N4 C21 C22 1.0(2) . . . . ? Zn1 N4 C21 C22 -170.34(12) . . . . ? C19 C20 C21 N4 -172.51(18) . . . . ? C19 C20 C21 C22 6.1(3) . . . . ? C15 C16 C22 C17 -175.73(19) . . . . ? C15 C16 C22 C21 2.7(3) . . . . ? C18 C17 C22 C16 177.4(2) . . . . ? C18 C17 C22 C21 -1.0(3) . . . . ? N4 C21 C22 C16 -3.6(3) . . . . ? C20 C21 C22 C16 177.80(17) . . . . ? N4 C21 C22 C17 174.85(17) . . . . ? C20 C21 C22 C17 -3.8(3) . . . . ? C33 N2 C23 C24 73.96(17) . . . . ? C2 N2 C23 C24 -160.28(14) . . . . ? Zn1 N2 C23 C24 -45.75(15) . . . . ? C31 N5 C24 C25 2.0(2) . . . . ? Zn1 N5 C24 C25 -167.56(14) . . . . ? C31 N5 C24 C23 176.93(15) . . . . ? Zn1 N5 C24 C23 7.41(18) . . . . ? N2 C23 C24 N5 27.7(2) . . . . ? N2 C23 C24 C25 -157.22(16) . . . . ? N5 C24 C25 C26 3.3(3) . . . . ? C23 C24 C25 C26 -171.53(18) . . . . ? C24 C25 C26 C32 -4.0(3) . . . . ? C32 C27 C28 C29 -1.9(3) . . . . ? C27 C28 C29 C30 2.2(3) . . . . ? C28 C29 C30 C31 1.1(3) . . . . ? C24 N5 C31 C30 174.00(16) . . . . ? Zn1 N5 C31 C30 -18.6(2) . . . . ? C24 N5 C31 C32 -6.5(2) . . . . ? Zn1 N5 C31 C32 160.98(13) . . . . ? C29 C30 C31 N5 174.99(17) . . . . ? C29 C30 C31 C32 -4.6(3) . . . . ? C25 C26 C32 C27 -179.95(19) . . . . ? C25 C26 C32 C31 -0.4(3) . . . . ? C28 C27 C32 C26 178.0(2) . . . . ? C28 C27 C32 C31 -1.6(3) . . . . ? N5 C31 C32 C26 5.7(3) . . . . ? C30 C31 C32 C26 -174.79(17) . . . . ? N5 C31 C32 C27 -174.73(17) . . . . ? C30 C31 C32 C27 4.8(3) . . . . ? C23 N2 C33 C34 -131.85(16) . . . . ? C2 N2 C33 C34 100.85(18) . . . . ? Zn1 N2 C33 C34 -18.02(19) . . . . ? C41 N6 C34 C35 -0.3(3) . . . . ? Zn1 N6 C34 C35 176.32(16) . . . . ? C41 N6 C34 C33 177.35(16) . . . . ? Zn1 N6 C34 C33 -6.0(2) . . . . ? N2 C33 C34 N6 16.5(3) . . . . ? N2 C33 C34 C35 -165.60(17) . . . . ? N6 C34 C35 C36 -1.0(3) . . . . ? C33 C34 C35 C36 -178.8(2) . . . . ? C34 C35 C36 C42 0.4(3) . . . . ? C42 C37 C38 C39 1.3(4) . . . . ? C37 C38 C39 C40 -0.7(4) . . . . ? C38 C39 C40 C41 -1.8(3) . . . . ? C34 N6 C41 C40 -177.98(17) . . . . ? Zn1 N6 C41 C40 6.3(3) . . . . ? C34 N6 C41 C42 2.3(3) . . . . ? Zn1 N6 C41 C42 -173.40(13) . . . . ? C39 C40 C41 N6 -176.27(18) . . . . ? C39 C40 C41 C42 3.4(3) . . . . ? C35 C36 C42 C37 -178.4(2) . . . . ? C35 C36 C42 C41 1.5(3) . . . . ? C38 C37 C42 C36 -179.7(2) . . . . ? C38 C37 C42 C41 0.4(3) . . . . ? N6 C41 C42 C36 -2.9(3) . . . . ? C40 C41 C42 C36 177.36(19) . . . . ? N6 C41 C42 C37 176.94(18) . . . . ? C40 C41 C42 C37 -2.8(3) . . . . ? N9 C47 C48 C47 -164(4) . . . 2_556 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.734 _refine_diff_density_min -0.505 _refine_diff_density_rms 0.121 #============================================================================== # End of CIF #============================================================================== #===END #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== data_tpen723 _database_code_depnum_ccdc_archive 'CCDC 246546' _audit_creation_date 2004-11-04 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26.67 H30.67 Cl2 N6 O8.67 Zn' _chemical_formula_weight 710.27 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' 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 'C2 /c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 41.337(3) _cell_length_b 9.4307(4) _cell_length_c 24.1542(17) _cell_angle_alpha 90.00 _cell_angle_beta 108.421(3) _cell_angle_gamma 90.00 _cell_volume 8933.7(10) _cell_formula_units_Z 12 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.584 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4393 _exptl_absorpt_coefficient_mu 1.067 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7403 _exptl_absorpt_correction_T_max 0.7403 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type 'Mo Kalpha' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean 14.62 _diffrn_reflns_number 43100 _diffrn_reflns_av_R_equivalents 0.0235 _diffrn_reflns_av_sigmaI/netI 0.0196 _diffrn_reflns_limit_h_min -53 _diffrn_reflns_limit_h_max 53 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10214 _reflns_number_gt 9086 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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/[sigma^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10214 _refine_ls_number_parameters 778 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0627 _refine_ls_R_factor_gt 0.0557 _refine_ls_wR_factor_ref 0.1884 _refine_ls_wR_factor_gt 0.1804 _refine_ls_goodness_of_fit_ref 1.461 _refine_ls_restrained_S_all 1.461 _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 0.167771(8) 0.24245(3) 0.592335(15) 0.03337(13) Uani 1 1 d . . . Zn2 Zn 0.0000 0.20836(5) 0.2500 0.03195(14) Uani 1 2 d S . . Cl1 Cl 0.17802(2) -0.24673(8) 0.70660(4) 0.0443(2) Uani 1 1 d . . . Cl2 Cl 0.15329(3) -0.24532(12) 0.37912(5) 0.0668(3) Uani 1 1 d . . . Cl3 Cl -0.008768(18) 0.69278(8) 0.39136(3) 0.03917(19) Uani 1 1 d . . . O1 O 0.16990(9) -0.1146(3) 0.72828(16) 0.0771(9) Uani 1 1 d . . . O2 O 0.20629(10) -0.2249(3) 0.68705(19) 0.0790(10) Uani 1 1 d . . . O3 O 0.15012(10) -0.2966(4) 0.66135(17) 0.0983(13) Uani 1 1 d . . . O4 O 0.18658(7) -0.3503(3) 0.75306(12) 0.0649(7) Uani 1 1 d . . . O5 O 0.14405(15) -0.3601(7) 0.4105(2) 0.141(2) Uani 1 1 d . . . O6 O 0.17394(12) -0.1511(5) 0.42195(18) 0.1150(14) Uani 1 1 d . . . O7 O 0.12443(11) -0.1802(5) 0.3423(3) 0.138(2) Uani 1 1 d . . . O8 O 0.17266(12) -0.3024(6) 0.34737(19) 0.1126(15) Uani 1 1 d . . . O9 O -0.02609(7) 0.8236(3) 0.38495(14) 0.0671(8) Uani 1 1 d . . . O10 O 0.02118(16) 0.7155(7) 0.4426(2) 0.0792(17) Uani 0.60 1 d P . . O11 O -0.0272(2) 0.5804(6) 0.4064(4) 0.094(2) Uani 0.60 1 d P . . O12 O 0.0024(2) 0.6477(8) 0.3456(3) 0.066(2) Uani 0.60 1 d P . . O13 O -0.0007(3) 0.6230(12) 0.4424(3) 0.081(3) Uani 0.40 1 d P . . O14 O -0.0369(3) 0.6164(12) 0.3499(6) 0.115(4) Uani 0.40 1 d P . . O15 O 0.0157(4) 0.7012(14) 0.3632(8) 0.114(7) Uani 0.40 1 d P . . N1 N 0.13259(6) 0.2829(3) 0.64136(11) 0.0370(5) Uani 1 1 d . . . N2 N 0.20510(7) 0.2398(2) 0.67982(12) 0.0360(5) Uani 1 1 d . . . N3 N 0.12623(6) 0.3184(3) 0.52433(11) 0.0397(6) Uani 1 1 d . . . N4 N 0.14044(6) 0.0386(3) 0.58144(11) 0.0377(5) Uani 1 1 d . . . N5 N 0.20930(6) 0.1449(3) 0.57427(11) 0.0370(5) Uani 1 1 d . . . N6 N 0.19320(6) 0.4523(3) 0.59466(12) 0.0401(6) Uani 1 1 d . . . N7 N 0.03689(7) 0.0327(3) 0.27388(11) 0.0399(5) Uani 1 1 d . . . N8 N 0.04587(6) 0.3170(3) 0.26168(10) 0.0363(5) Uani 1 1 d . . . N9 N 0.00840(6) 0.1922(3) 0.34362(10) 0.0365(5) Uani 1 1 d . . . C1 C 0.15415(9) 0.3252(4) 0.70055(14) 0.0425(7) Uani 1 1 d . . . H1 H 0.1424(10) 0.329(4) 0.7265(17) 0.051 Uiso 1 1 d . . . H2 H 0.1631(9) 0.412(4) 0.6934(16) 0.051 Uiso 1 1 d . . . C2 C 0.18545(9) 0.2297(4) 0.72080(15) 0.0435(7) Uani 1 1 d . . . H3 H 0.1999(11) 0.252(4) 0.762(2) 0.052 Uiso 1 1 d . . . H4 H 0.1786(10) 0.131(5) 0.7200(16) 0.052 Uiso 1 1 d . . . C3 C 0.11077(8) 0.4002(4) 0.60842(15) 0.0463(7) Uani 1 1 d . . . H5 H 0.1232(9) 0.497(4) 0.6182(15) 0.048(9) Uiso 1 1 d . . . H6 H 0.0887(9) 0.412(4) 0.6122(16) 0.049(10) Uiso 1 1 d . . . C4 C 0.10314(7) 0.3857(3) 0.54342(14) 0.0390(6) Uani 1 1 d . . . C5 C 0.07464(8) 0.4486(3) 0.50401(16) 0.0464(7) Uani 1 1 d . . . H7 H 0.0585(10) 0.501(4) 0.5184(16) 0.057(11) Uiso 1 1 d . . . C6 C 0.07022(8) 0.4432(4) 0.44526(16) 0.0516(8) Uani 1 1 d . . . H8 H 0.0514(13) 0.501(6) 0.423(2) 0.089(15) Uiso 1 1 d . . . C7 C 0.09388(9) 0.3723(4) 0.42599(16) 0.0501(8) Uani 1 1 d . . . H9 H 0.0906(8) 0.363(4) 0.3871(16) 0.038(8) Uiso 1 1 d . . . C8 C 0.12137(8) 0.3093(4) 0.46699(15) 0.0459(7) Uani 1 1 d . . . H10 H 0.1401(16) 0.254(5) 0.451(3) 0.087(17) Uiso 1 1 d . . . C9 C 0.11235(9) 0.1551(4) 0.64330(16) 0.0446(7) Uani 1 1 d . . . H11 H 0.0892(10) 0.179(4) 0.6355(17) 0.053 Uiso 1 1 d . . . H12 H 0.1198(9) 0.118(4) 0.6815(18) 0.053 Uiso 1 1 d . . . C10 C 0.11329(7) 0.0418(3) 0.59988(12) 0.0357(6) Uani 1 1 d . . . C11 C 0.08737(8) -0.0574(3) 0.58220(14) 0.0416(7) Uani 1 1 d . . . H13 H 0.0663(9) -0.039(4) 0.5931(15) 0.050 Uiso 1 1 d . . . C12 C 0.08977(8) -0.1619(4) 0.54416(16) 0.0479(8) Uani 1 1 d . . . H14 H 0.0746(12) -0.228(4) 0.525(2) 0.058 Uiso 1 1 d . . . C13 C 0.11752(9) -0.1674(4) 0.52509(16) 0.0471(8) Uani 1 1 d . . . H15 H 0.1178(12) -0.216(5) 0.502(2) 0.057 Uiso 1 1 d . . . C14 C 0.14240(8) -0.0646(3) 0.54438(14) 0.0429(7) Uani 1 1 d . . . H16 H 0.1610(9) -0.058(4) 0.5282(15) 0.050(10) Uiso 1 1 d . . . C15 C 0.22538(8) 0.1112(3) 0.67901(14) 0.0397(6) Uani 1 1 d . . . H17 H 0.2124(8) 0.028(4) 0.6809(14) 0.037(8) Uiso 1 1 d . . . H18 H 0.2459(10) 0.102(4) 0.7046(17) 0.053(10) Uiso 1 1 d . . . C16 C 0.23345(7) 0.0995(3) 0.62306(13) 0.0367(6) Uani 1 1 d . . . C17 C 0.26344(8) 0.0394(4) 0.62004(15) 0.0461(7) Uani 1 1 d . . . H19 H 0.2812(10) 0.013(4) 0.6548(18) 0.060(11) Uiso 1 1 d . . . C18 C 0.26880(8) 0.0253(4) 0.56705(16) 0.0512(8) Uani 1 1 d . . . H20 H 0.2891(10) -0.027(4) 0.5612(17) 0.057(10) Uiso 1 1 d . . . C19 C 0.24368(9) 0.0712(4) 0.51705(16) 0.0493(8) Uani 1 1 d . . . H21 H 0.2461(7) 0.056(3) 0.4837(14) 0.027(7) Uiso 1 1 d . . . C20 C 0.21475(8) 0.1309(4) 0.52287(15) 0.0454(7) Uani 1 1 d . . . H22 H 0.2022(9) 0.165(4) 0.4929(17) 0.046(10) Uiso 1 1 d . . . C21 C 0.22690(9) 0.3678(4) 0.69053(16) 0.0506(8) Uani 1 1 d . . . H23 H 0.2504(11) 0.338(5) 0.6990(18) 0.061 Uiso 1 1 d . . . H24 H 0.2220(10) 0.439(5) 0.7127(18) 0.061 Uiso 1 1 d . . . C22 C 0.22276(7) 0.4606(3) 0.63842(15) 0.0416(7) Uani 1 1 d . . . C23 C 0.24778(9) 0.5570(4) 0.63810(19) 0.0524(8) Uani 1 1 d . . . H25 H 0.2686(11) 0.555(4) 0.6692(18) 0.062 Uiso 1 1 d . . . C24 C 0.24182(11) 0.6535(4) 0.5937(2) 0.0612(10) Uani 1 1 d . . . H26 H 0.2580(13) 0.727(5) 0.588(2) 0.073 Uiso 1 1 d . . . C25 C 0.21078(11) 0.6505(4) 0.5499(2) 0.0558(9) Uani 1 1 d . . . H27 H 0.2076(12) 0.684(5) 0.521(2) 0.067 Uiso 1 1 d . . . C26 C 0.18762(8) 0.5469(4) 0.55140(16) 0.0460(7) Uani 1 1 d . . . H28 H 0.1650(8) 0.540(3) 0.5217(14) 0.033(8) Uiso 1 1 d . . . C27 C 0.01719(10) -0.0945(4) 0.24573(17) 0.0519(8) Uani 1 1 d . . . H29 H 0.0140(8) -0.089(3) 0.2062(15) 0.036(8) Uiso 1 1 d . . . H30 H 0.0281(11) -0.176(5) 0.2621(18) 0.058(11) Uiso 1 1 d . . . C28 C 0.06337(9) 0.0756(4) 0.24880(15) 0.0474(8) Uani 1 1 d . . . H31 H 0.0859(8) 0.019(4) 0.2666(14) 0.036(8) Uiso 1 1 d . . . H32 H 0.0563(10) 0.064(4) 0.2075(18) 0.056(11) Uiso 1 1 d . . . C29 C 0.07138(8) 0.2308(4) 0.25930(14) 0.0414(7) Uani 1 1 d . . . C30 C 0.10371(9) 0.2860(5) 0.2658(2) 0.0620(11) Uani 1 1 d . . . H33 H 0.1228(13) 0.213(5) 0.270(2) 0.074 Uiso 1 1 d . . . C31 C 0.10965(10) 0.4278(5) 0.2750(2) 0.0715(12) Uani 1 1 d . . . H34 H 0.1346(12) 0.478(5) 0.279(2) 0.085 Uiso 1 1 d . . . C32 C 0.08339(9) 0.5155(5) 0.27712(19) 0.0596(10) Uani 1 1 d . . . H35 H 0.0877(11) 0.618(5) 0.2839(19) 0.071 Uiso 1 1 d . . . C33 C 0.05215(8) 0.4559(4) 0.27029(14) 0.0427(7) Uani 1 1 d . . . H36 H 0.0334(8) 0.518(4) 0.2715(14) 0.038(8) Uiso 1 1 d . . . C34 C 0.05098(10) 0.0188(4) 0.33793(15) 0.0495(8) Uani 1 1 d . . . H37 H 0.0531(10) -0.072(5) 0.3478(17) 0.056(11) Uiso 1 1 d . . . H38 H 0.0732(10) 0.057(4) 0.3534(16) 0.048(10) Uiso 1 1 d . . . C35 C 0.03137(8) 0.0958(3) 0.37138(12) 0.0389(6) Uani 1 1 d . . . C36 C 0.03802(10) 0.0683(4) 0.43069(14) 0.0509(8) Uani 1 1 d . . . H39 H 0.0548(10) -0.003(5) 0.4468(18) 0.061 Uiso 1 1 d . . . C37 C 0.02130(10) 0.1442(4) 0.46155(14) 0.0536(9) Uani 1 1 d . . . H40 H 0.0247(10) 0.126(5) 0.4985(19) 0.065 Uiso 1 1 d . . . C38 C -0.00156(10) 0.2479(4) 0.43354(15) 0.0478(8) Uani 1 1 d . . . H41 H -0.0157(9) 0.303(4) 0.4507(16) 0.041(9) Uiso 1 1 d . . . C39 C -0.00744(9) 0.2686(4) 0.37401(15) 0.0420(7) Uani 1 1 d . . . H42 H -0.0229(9) 0.325(4) 0.3569(15) 0.038(9) Uiso 1 1 d . . . O16 O 0.15047(15) 0.1263(5) 0.3889(2) 0.1287(17) Uani 1 1 d . . . H46 H 0.1528 0.0408 0.3992 0.193 Uiso 1 1 calc R . . C40 C 0.17754(15) 0.1675(8) 0.3717(3) 0.0983(18) Uani 1 1 d . . . H43 H 0.1775 0.2709 0.3680 0.147 Uiso 1 1 calc R . . H44 H 0.1757 0.1241 0.3339 0.147 Uiso 1 1 calc R . . H45 H 0.1988 0.1368 0.4007 0.147 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 0.02694(19) 0.0332(2) 0.0357(2) 0.00024(12) 0.00387(14) 0.00054(11) Zn2 0.0328(2) 0.0317(3) 0.0299(2) 0.000 0.00792(18) 0.000 Cl1 0.0400(4) 0.0323(4) 0.0557(5) 0.0008(3) 0.0079(3) -0.0023(3) Cl2 0.0519(5) 0.0900(8) 0.0616(6) -0.0106(5) 0.0221(5) -0.0080(5) Cl3 0.0412(4) 0.0395(4) 0.0390(4) 0.0007(3) 0.0157(3) 0.0031(3) O1 0.100(2) 0.0345(14) 0.119(3) 0.0022(15) 0.066(2) 0.0067(14) O2 0.083(2) 0.0617(18) 0.113(3) -0.0108(17) 0.061(2) -0.0075(15) O3 0.087(2) 0.074(2) 0.091(2) 0.0192(19) -0.0346(19) -0.0241(19) O4 0.0692(17) 0.0505(15) 0.0632(16) 0.0127(13) 0.0040(13) 0.0051(13) O5 0.168(5) 0.165(5) 0.109(3) -0.001(3) 0.070(3) -0.077(4) O6 0.128(3) 0.122(4) 0.083(3) -0.023(2) 0.017(2) -0.038(3) O7 0.074(3) 0.093(3) 0.218(6) 0.018(3) 0.003(3) 0.023(2) O8 0.108(3) 0.161(4) 0.079(2) -0.002(3) 0.043(2) 0.045(3) O9 0.0674(17) 0.0584(17) 0.084(2) 0.0131(15) 0.0366(15) 0.0240(14) O10 0.073(4) 0.083(4) 0.055(3) -0.020(3) -0.018(3) 0.021(3) O11 0.104(5) 0.054(3) 0.152(7) 0.024(4) 0.081(5) 0.001(3) O12 0.095(5) 0.070(5) 0.041(2) 0.002(3) 0.034(3) 0.027(3) O13 0.117(7) 0.096(7) 0.036(4) 0.025(4) 0.035(4) 0.049(6) O14 0.095(7) 0.097(8) 0.146(10) -0.059(8) 0.030(7) -0.012(6) O15 0.117(11) 0.086(9) 0.196(18) 0.086(10) 0.129(12) 0.070(8) N1 0.0343(12) 0.0347(12) 0.0385(13) -0.0049(10) 0.0068(10) 0.0020(10) N2 0.0360(13) 0.0266(12) 0.0391(13) -0.0017(9) 0.0027(11) -0.0009(9) N3 0.0284(11) 0.0416(14) 0.0436(14) 0.0009(11) 0.0034(10) 0.0018(10) N4 0.0324(11) 0.0339(13) 0.0448(13) -0.0050(10) 0.0092(10) 0.0011(9) N5 0.0283(11) 0.0379(13) 0.0407(13) 0.0029(10) 0.0051(9) 0.0024(9) N6 0.0332(12) 0.0328(13) 0.0523(14) 0.0044(11) 0.0105(10) 0.0014(10) N7 0.0492(14) 0.0341(13) 0.0354(12) -0.0003(10) 0.0120(10) 0.0076(11) N8 0.0294(11) 0.0420(14) 0.0352(12) 0.0015(10) 0.0070(9) 0.0013(10) N9 0.0395(12) 0.0377(13) 0.0307(12) -0.0002(10) 0.0085(10) 0.0001(10) C1 0.0443(16) 0.0397(17) 0.0403(16) -0.0112(13) 0.0087(13) 0.0028(13) C2 0.0509(19) 0.0424(18) 0.0328(16) -0.0037(13) 0.0068(14) 0.0034(14) C3 0.0389(16) 0.0459(19) 0.0494(18) -0.0076(14) 0.0072(13) 0.0112(14) C4 0.0285(13) 0.0317(14) 0.0512(16) -0.0042(12) 0.0046(11) -0.0023(11) C5 0.0357(15) 0.0359(16) 0.0587(19) 0.0024(14) 0.0024(13) 0.0030(12) C6 0.0378(16) 0.0465(19) 0.059(2) 0.0128(16) -0.0009(14) 0.0044(14) C7 0.0407(16) 0.057(2) 0.0471(19) 0.0089(16) 0.0057(13) -0.0011(15) C8 0.0358(15) 0.052(2) 0.0462(18) 0.0086(15) 0.0079(13) 0.0010(13) C9 0.0402(16) 0.0455(18) 0.0522(19) -0.0052(15) 0.0203(14) -0.0052(13) C10 0.0333(13) 0.0339(15) 0.0367(14) 0.0022(11) 0.0063(11) -0.0002(11) C11 0.0371(15) 0.0386(16) 0.0460(16) 0.0032(13) 0.0085(12) -0.0032(12) C12 0.0423(16) 0.0367(17) 0.0558(19) -0.0014(15) 0.0027(14) -0.0056(13) C13 0.0512(18) 0.0348(17) 0.0488(18) -0.0092(14) 0.0065(14) 0.0017(14) C14 0.0389(15) 0.0382(16) 0.0495(17) -0.0076(13) 0.0109(13) 0.0024(12) C15 0.0352(14) 0.0351(16) 0.0422(16) 0.0047(13) 0.0026(12) 0.0049(12) C16 0.0309(13) 0.0294(14) 0.0455(15) 0.0013(12) 0.0061(11) -0.0017(10) C17 0.0357(15) 0.0437(18) 0.0524(18) 0.0012(14) 0.0048(13) 0.0051(13) C18 0.0393(16) 0.053(2) 0.061(2) -0.0026(16) 0.0163(14) 0.0081(14) C19 0.0502(18) 0.051(2) 0.0493(19) 0.0029(16) 0.0195(15) 0.0108(15) C20 0.0413(16) 0.0518(19) 0.0405(16) 0.0041(15) 0.0092(13) 0.0084(14) C21 0.0426(17) 0.0359(17) 0.057(2) -0.0044(15) -0.0077(15) -0.0086(13) C22 0.0316(13) 0.0308(14) 0.0603(19) -0.0090(13) 0.0116(12) -0.0010(11) C23 0.0434(17) 0.0436(19) 0.074(2) -0.0168(17) 0.0237(17) -0.0090(14) C24 0.070(2) 0.0415(19) 0.090(3) -0.0122(19) 0.050(2) -0.0156(18) C25 0.071(2) 0.0381(18) 0.072(3) 0.0063(17) 0.043(2) 0.0025(17) C26 0.0435(16) 0.0382(17) 0.0592(19) 0.0072(14) 0.0206(15) 0.0072(13) C27 0.076(2) 0.0308(16) 0.0479(19) -0.0016(14) 0.0185(17) 0.0056(16) C28 0.0501(18) 0.0509(19) 0.0448(18) 0.0019(14) 0.0202(14) 0.0194(15) C29 0.0340(15) 0.0544(19) 0.0360(15) 0.0053(13) 0.0115(12) 0.0058(12) C30 0.0364(18) 0.080(3) 0.076(3) 0.021(2) 0.0267(18) 0.0117(18) C31 0.0391(18) 0.082(3) 0.092(3) 0.027(2) 0.0186(19) -0.0077(19) C32 0.0462(18) 0.055(2) 0.069(2) 0.0175(19) 0.0064(16) -0.0110(16) C33 0.0389(15) 0.0420(17) 0.0420(16) 0.0074(13) 0.0052(12) -0.0021(13) C34 0.059(2) 0.044(2) 0.0413(17) 0.0084(14) 0.0110(15) 0.0169(16) C35 0.0461(15) 0.0349(15) 0.0334(14) 0.0016(11) 0.0092(12) -0.0007(12) C36 0.064(2) 0.0472(19) 0.0349(16) 0.0059(14) 0.0069(14) 0.0007(16) C37 0.076(2) 0.052(2) 0.0301(15) 0.0003(14) 0.0142(15) -0.0150(18) C38 0.055(2) 0.057(2) 0.0339(16) -0.0078(14) 0.0177(15) -0.0125(15) C39 0.0417(17) 0.0469(18) 0.0361(16) -0.0066(13) 0.0105(13) -0.0019(14) O16 0.179(5) 0.095(3) 0.135(4) 0.009(3) 0.083(4) 0.026(3) C40 0.092(4) 0.131(5) 0.078(3) 0.034(3) 0.036(3) 0.005(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 N3 2.092(2) . ? Zn1 N5 2.111(2) . ? Zn1 N1 2.180(3) . ? Zn1 N2 2.188(3) . ? Zn1 N4 2.203(3) . ? Zn1 N6 2.233(3) . ? Zn2 N8 2.094(2) . ? Zn2 N8 2.094(2) 2 ? Zn2 N9 2.182(2) 2 ? Zn2 N9 2.182(2) . ? Zn2 N7 2.201(2) 2 ? Zn2 N7 2.201(2) . ? Cl1 O3 1.396(3) . ? Cl1 O2 1.407(3) . ? Cl1 O1 1.432(3) . ? Cl1 O4 1.445(3) . ? Cl2 O8 1.381(4) . ? Cl2 O7 1.386(4) . ? Cl2 O6 1.425(4) . ? Cl2 O5 1.440(5) . ? Cl3 O13 1.344(6) . ? Cl3 O15 1.388(11) . ? Cl3 O12 1.392(7) . ? Cl3 O9 1.410(3) . ? Cl3 O11 1.417(5) . ? Cl3 O14 1.461(10) . ? Cl3 O10 1.463(5) . ? O10 O13 1.254(13) . ? O11 O13 1.233(13) . ? O11 O14 1.339(14) . ? O12 O15 0.768(18) . ? O12 O14 1.685(14) . ? N1 C9 1.477(4) . ? N1 C1 1.480(4) . ? N1 C3 1.489(4) . ? N2 C2 1.468(5) . ? N2 C15 1.478(4) . ? N2 C21 1.479(4) . ? N3 C8 1.338(4) . ? N3 C4 1.343(4) . ? N4 C10 1.332(4) . ? N4 C14 1.342(4) . ? N5 C20 1.336(4) . ? N5 C16 1.351(4) . ? N6 C26 1.337(4) . ? N6 C22 1.342(4) . ? N7 C28 1.465(4) . ? N7 C34 1.477(4) . ? N7 C27 1.488(4) . ? N8 C33 1.339(4) . ? N8 C29 1.347(4) . ? N9 C35 1.333(4) . ? N9 C39 1.338(4) . ? C1 C2 1.524(5) . ? C1 H1 0.91(4) . ? C1 H2 0.93(4) . ? C2 H3 1.01(5) . ? C2 H4 0.97(4) . ? C3 C4 1.507(5) . ? C3 H5 1.04(4) . ? C3 H6 0.95(4) . ? C4 C5 1.392(4) . ? C5 C6 1.373(5) . ? C5 H7 0.98(4) . ? C6 C7 1.381(5) . ? C6 H8 0.96(5) . ? C7 C8 1.384(5) . ? C7 H9 0.91(3) . ? C8 H10 1.10(6) . ? C9 C10 1.506(4) . ? C9 H11 0.94(4) . ? C9 H12 0.94(4) . ? C10 C11 1.385(4) . ? C11 C12 1.372(5) . ? C11 H13 1.00(4) . ? C12 C13 1.365(5) . ? C12 H14 0.90(5) . ? C13 C14 1.382(5) . ? C13 H15 0.72(5) . ? C14 H16 0.97(4) . ? C15 C16 1.495(4) . ? C15 H17 0.96(4) . ? C15 H18 0.88(4) . ? C16 C17 1.386(4) . ? C17 C18 1.373(5) . ? C17 H19 0.96(4) . ? C18 C19 1.390(5) . ? C18 H20 1.02(4) . ? C19 C20 1.369(5) . ? C19 H21 0.85(3) . ? C20 H22 0.81(4) . ? C21 C22 1.498(5) . ? C21 H23 0.97(4) . ? C21 H24 0.92(4) . ? C22 C23 1.379(4) . ? C23 C24 1.369(6) . ? C23 H25 0.95(4) . ? C24 C25 1.381(6) . ? C24 H26 1.00(5) . ? C25 C26 1.377(5) . ? C25 H27 0.74(5) . ? C26 H28 0.98(3) . ? C27 C27 1.499(8) 2 ? C27 H29 0.92(3) . ? C27 H30 0.92(5) . ? C28 C29 1.504(5) . ? C28 H31 1.04(3) . ? C28 H32 0.95(4) . ? C29 C30 1.396(5) . ? C30 C31 1.365(7) . ? C30 H33 1.03(5) . ? C31 C32 1.378(6) . ? C31 H34 1.11(5) . ? C32 C33 1.370(5) . ? C32 H35 0.99(5) . ? C33 H36 0.98(3) . ? C34 C35 1.501(5) . ? C34 H37 0.88(4) . ? C34 H38 0.95(4) . ? C35 C36 1.395(4) . ? C36 C37 1.368(5) . ? C36 H39 0.96(4) . ? C37 C38 1.379(6) . ? C37 H40 0.87(4) . ? C38 C39 1.394(5) . ? C38 H41 0.97(4) . ? C39 H42 0.84(4) . ? O16 C40 1.368(7) . ? O16 H46 0.8400 . ? C40 H43 0.9800 . ? C40 H44 0.9800 . ? C40 H45 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 N3 Zn1 N5 120.41(10) . . ? N3 Zn1 N1 81.00(10) . . ? N5 Zn1 N1 156.10(10) . . ? N3 Zn1 N2 156.30(10) . . ? N5 Zn1 N2 79.82(10) . . ? N1 Zn1 N2 82.26(10) . . ? N3 Zn1 N4 86.69(10) . . ? N5 Zn1 N4 90.87(9) . . ? N1 Zn1 N4 79.19(9) . . ? N2 Zn1 N4 106.49(9) . . ? N3 Zn1 N6 88.82(10) . . ? N5 Zn1 N6 89.09(9) . . ? N1 Zn1 N6 102.76(10) . . ? N2 Zn1 N6 78.65(9) . . ? N4 Zn1 N6 174.77(9) . . ? N8 Zn2 N8 121.44(14) . 2 ? N8 Zn2 N9 90.82(9) . 2 ? N8 Zn2 N9 93.08(9) 2 2 ? N8 Zn2 N9 93.08(9) . . ? N8 Zn2 N9 90.82(9) 2 . ? N9 Zn2 N9 172.01(14) 2 . ? N8 Zn2 N7 157.83(10) . 2 ? N8 Zn2 N7 79.05(10) 2 2 ? N9 Zn2 N7 78.81(9) 2 2 ? N9 Zn2 N7 95.12(9) . 2 ? N8 Zn2 N7 79.05(10) . . ? N8 Zn2 N7 157.83(10) 2 . ? N9 Zn2 N7 95.12(9) 2 . ? N9 Zn2 N7 78.81(9) . . ? N7 Zn2 N7 82.39(14) 2 . ? O3 Cl1 O2 110.8(3) . . ? O3 Cl1 O1 110.4(2) . . ? O2 Cl1 O1 108.12(18) . . ? O3 Cl1 O4 108.6(2) . . ? O2 Cl1 O4 109.5(2) . . ? O1 Cl1 O4 109.4(2) . . ? O8 Cl2 O7 110.4(4) . . ? O8 Cl2 O6 109.1(3) . . ? O7 Cl2 O6 112.7(3) . . ? O8 Cl2 O5 107.3(4) . . ? O7 Cl2 O5 110.7(4) . . ? O6 Cl2 O5 106.5(3) . . ? O13 Cl3 O15 117.9(8) . . ? O13 Cl3 O12 121.9(5) . . ? O15 Cl3 O12 32.1(8) . . ? O13 Cl3 O9 120.0(4) . . ? O15 Cl3 O9 108.7(5) . . ? O12 Cl3 O9 117.7(4) . . ? O13 Cl3 O11 52.9(6) . . ? O15 Cl3 O11 134.6(7) . . ? O12 Cl3 O11 108.3(5) . . ? O9 Cl3 O11 112.8(3) . . ? O13 Cl3 O14 107.6(8) . . ? O15 Cl3 O14 103.7(10) . . ? O12 Cl3 O14 72.3(6) . . ? O9 Cl3 O14 95.2(5) . . ? O11 Cl3 O14 55.4(6) . . ? O13 Cl3 O10 52.9(6) . . ? O15 Cl3 O10 81.5(9) . . ? O12 Cl3 O10 108.1(4) . . ? O9 Cl3 O10 103.3(3) . . ? O11 Cl3 O10 105.8(5) . . ? O14 Cl3 O10 158.2(6) . . ? O13 O10 Cl3 58.7(4) . . ? O13 O11 O14 123.3(8) . . ? O13 O11 Cl3 60.5(5) . . ? O14 O11 Cl3 64.0(5) . . ? O15 O12 Cl3 73.7(12) . . ? O15 O12 O14 128.0(15) . . ? Cl3 O12 O14 55.7(5) . . ? O11 O13 O10 135.0(7) . . ? O11 O13 Cl3 66.6(5) . . ? O10 O13 Cl3 68.4(5) . . ? O11 O14 Cl3 60.6(6) . . ? O11 O14 O12 97.1(7) . . ? Cl3 O14 O12 51.9(4) . . ? O12 O15 Cl3 74.2(12) . . ? C9 N1 C1 111.3(3) . . ? C9 N1 C3 111.7(3) . . ? C1 N1 C3 113.2(2) . . ? C9 N1 Zn1 110.88(19) . . ? C1 N1 Zn1 105.68(19) . . ? C3 N1 Zn1 103.6(2) . . ? C2 N2 C15 113.1(2) . . ? C2 N2 C21 111.8(3) . . ? C15 N2 C21 110.8(3) . . ? C2 N2 Zn1 106.28(19) . . ? C15 N2 Zn1 103.10(18) . . ? C21 N2 Zn1 111.35(19) . . ? C8 N3 C4 119.7(3) . . ? C8 N3 Zn1 127.4(2) . . ? C4 N3 Zn1 112.8(2) . . ? C10 N4 C14 118.3(3) . . ? C10 N4 Zn1 113.25(19) . . ? C14 N4 Zn1 125.1(2) . . ? C20 N5 C16 118.9(3) . . ? C20 N5 Zn1 128.5(2) . . ? C16 N5 Zn1 112.5(2) . . ? C26 N6 C22 117.8(3) . . ? C26 N6 Zn1 127.4(2) . . ? C22 N6 Zn1 112.1(2) . . ? C28 N7 C34 111.0(3) . . ? C28 N7 C27 113.9(3) . . ? C34 N7 C27 112.6(3) . . ? C28 N7 Zn2 103.31(19) . . ? C34 N7 Zn2 110.66(19) . . ? C27 N7 Zn2 104.7(2) . . ? C33 N8 C29 118.8(3) . . ? C33 N8 Zn2 128.5(2) . . ? C29 N8 Zn2 112.8(2) . . ? C35 N9 C39 119.1(3) . . ? C35 N9 Zn2 115.1(2) . . ? C39 N9 Zn2 125.9(2) . . ? N1 C1 C2 110.0(3) . . ? N1 C1 H1 113(2) . . ? C2 C1 H1 113(3) . . ? N1 C1 H2 102(2) . . ? C2 C1 H2 103(2) . . ? H1 C1 H2 115(3) . . ? N2 C2 C1 109.8(3) . . ? N2 C2 H3 112(2) . . ? C1 C2 H3 112(2) . . ? N2 C2 H4 106(2) . . ? C1 C2 H4 110(2) . . ? H3 C2 H4 107(3) . . ? N1 C3 C4 112.4(3) . . ? N1 C3 H5 111(2) . . ? C4 C3 H5 104(2) . . ? N1 C3 H6 118(2) . . ? C4 C3 H6 103(2) . . ? H5 C3 H6 107(3) . . ? N3 C4 C5 120.4(3) . . ? N3 C4 C3 117.6(3) . . ? C5 C4 C3 121.8(3) . . ? C6 C5 C4 119.9(3) . . ? C6 C5 H7 120(2) . . ? C4 C5 H7 120(2) . . ? C5 C6 C7 119.3(3) . . ? C5 C6 H8 111(3) . . ? C7 C6 H8 129(3) . . ? C6 C7 C8 118.4(3) . . ? C6 C7 H9 120(2) . . ? C8 C7 H9 121(2) . . ? N3 C8 C7 122.3(3) . . ? N3 C8 H10 120(3) . . ? C7 C8 H10 118(3) . . ? N1 C9 C10 114.7(3) . . ? N1 C9 H11 111(2) . . ? C10 C9 H11 106(2) . . ? N1 C9 H12 109(2) . . ? C10 C9 H12 110(2) . . ? H11 C9 H12 106(3) . . ? N4 C10 C11 122.2(3) . . ? N4 C10 C9 117.3(3) . . ? C11 C10 C9 120.4(3) . . ? C12 C11 C10 118.6(3) . . ? C12 C11 H13 124(2) . . ? C10 C11 H13 117(2) . . ? C13 C12 C11 120.0(3) . . ? C13 C12 H14 109(3) . . ? C11 C12 H14 131(3) . . ? C12 C13 C14 118.3(3) . . ? C12 C13 H15 120(4) . . ? C14 C13 H15 121(4) . . ? N4 C14 C13 122.5(3) . . ? N4 C14 H16 116(2) . . ? C13 C14 H16 121(2) . . ? N2 C15 C16 111.2(3) . . ? N2 C15 H17 110.0(19) . . ? C16 C15 H17 106(2) . . ? N2 C15 H18 120(3) . . ? C16 C15 H18 101(2) . . ? H17 C15 H18 109(3) . . ? N5 C16 C17 120.7(3) . . ? N5 C16 C15 116.8(3) . . ? C17 C16 C15 122.5(3) . . ? C18 C17 C16 120.0(3) . . ? C18 C17 H19 119(2) . . ? C16 C17 H19 121(2) . . ? C17 C18 C19 118.9(3) . . ? C17 C18 H20 124(2) . . ? C19 C18 H20 117(2) . . ? C20 C19 C18 118.4(3) . . ? C20 C19 H21 122(2) . . ? C18 C19 H21 119(2) . . ? N5 C20 C19 123.1(3) . . ? N5 C20 H22 123(3) . . ? C19 C20 H22 114(3) . . ? N2 C21 C22 115.4(3) . . ? N2 C21 H23 108(3) . . ? C22 C21 H23 101(3) . . ? N2 C21 H24 118(3) . . ? C22 C21 H24 94(3) . . ? H23 C21 H24 118(4) . . ? N6 C22 C23 122.1(3) . . ? N6 C22 C21 117.5(3) . . ? C23 C22 C21 120.2(3) . . ? C24 C23 C22 119.6(4) . . ? C24 C23 H25 122(3) . . ? C22 C23 H25 118(3) . . ? C23 C24 C25 118.7(3) . . ? C23 C24 H26 127(3) . . ? C25 C24 H26 115(3) . . ? C26 C25 C24 118.7(4) . . ? C26 C25 H27 114(4) . . ? C24 C25 H27 124(4) . . ? N6 C26 C25 123.0(3) . . ? N6 C26 H28 114.5(19) . . ? C25 C26 H28 122.4(19) . . ? N7 C27 C27 110.1(2) . 2 ? N7 C27 H29 108(2) . . ? C27 C27 H29 108(2) 2 . ? N7 C27 H30 111(3) . . ? C27 C27 H30 107(3) 2 . ? H29 C27 H30 113(3) . . ? N7 C28 C29 110.6(3) . . ? N7 C28 H31 112.0(17) . . ? C29 C28 H31 108.0(18) . . ? N7 C28 H32 112(2) . . ? C29 C28 H32 106(2) . . ? H31 C28 H32 108(3) . . ? N8 C29 C30 120.3(3) . . ? N8 C29 C28 117.4(3) . . ? C30 C29 C28 122.3(3) . . ? C31 C30 C29 120.1(4) . . ? C31 C30 H33 123(3) . . ? C29 C30 H33 116(3) . . ? C30 C31 C32 119.3(4) . . ? C30 C31 H34 123(3) . . ? C32 C31 H34 117(3) . . ? C33 C32 C31 118.2(4) . . ? C33 C32 H35 122(3) . . ? C31 C32 H35 119(3) . . ? N8 C33 C32 123.3(3) . . ? N8 C33 H36 118(2) . . ? C32 C33 H36 119(2) . . ? N7 C34 C35 114.8(3) . . ? N7 C34 H37 110(3) . . ? C35 C34 H37 110(3) . . ? N7 C34 H38 113(2) . . ? C35 C34 H38 103(2) . . ? H37 C34 H38 105(3) . . ? N9 C35 C36 121.4(3) . . ? N9 C35 C34 118.7(3) . . ? C36 C35 C34 119.9(3) . . ? C37 C36 C35 119.5(3) . . ? C37 C36 H39 125(2) . . ? C35 C36 H39 115(2) . . ? C36 C37 C38 119.3(3) . . ? C36 C37 H40 121(3) . . ? C38 C37 H40 120(3) . . ? C37 C38 C39 118.3(3) . . ? C37 C38 H41 126(2) . . ? C39 C38 H41 116(2) . . ? N9 C39 C38 122.3(3) . . ? N9 C39 H42 120(2) . . ? C38 C39 H42 117(2) . . ? C40 O16 H46 109.5 . . ? O16 C40 H43 109.5 . . ? O16 C40 H44 109.5 . . ? H43 C40 H44 109.5 . . ? O16 C40 H45 109.5 . . ? H43 C40 H45 109.5 . . ? H44 C40 H45 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 O15 Cl3 O10 O13 -134.9(7) . . . . ? O12 Cl3 O10 O13 -116.8(6) . . . . ? O9 Cl3 O10 O13 117.8(5) . . . . ? O11 Cl3 O10 O13 -0.9(6) . . . . ? O14 Cl3 O10 O13 -29.2(16) . . . . ? O15 Cl3 O11 O13 94.5(13) . . . . ? O12 Cl3 O11 O13 116.6(6) . . . . ? O9 Cl3 O11 O13 -111.3(5) . . . . ? O14 Cl3 O11 O13 168.6(8) . . . . ? O10 Cl3 O11 O13 0.9(6) . . . . ? O13 Cl3 O11 O14 -168.6(8) . . . . ? O15 Cl3 O11 O14 -74.0(13) . . . . ? O12 Cl3 O11 O14 -51.9(7) . . . . ? O9 Cl3 O11 O14 80.2(6) . . . . ? O10 Cl3 O11 O14 -167.7(6) . . . . ? O13 Cl3 O12 O15 -92.5(16) . . . . ? O9 Cl3 O12 O15 80.9(15) . . . . ? O11 Cl3 O12 O15 -149.7(14) . . . . ? O14 Cl3 O12 O15 167.5(16) . . . . ? O10 Cl3 O12 O15 -35.4(16) . . . . ? O13 Cl3 O12 O14 100.1(9) . . . . ? O15 Cl3 O12 O14 -167.5(16) . . . . ? O9 Cl3 O12 O14 -86.5(6) . . . . ? O11 Cl3 O12 O14 42.9(6) . . . . ? O10 Cl3 O12 O14 157.1(7) . . . . ? O14 O11 O13 O10 10.9(16) . . . . ? Cl3 O11 O13 O10 -1.4(9) . . . . ? O14 O11 O13 Cl3 12.3(8) . . . . ? Cl3 O10 O13 O11 1.4(9) . . . . ? O15 Cl3 O13 O11 -126.5(10) . . . . ? O12 Cl3 O13 O11 -89.6(7) . . . . ? O9 Cl3 O13 O11 97.1(5) . . . . ? O14 Cl3 O13 O11 -9.9(7) . . . . ? O10 Cl3 O13 O11 -178.9(7) . . . . ? O15 Cl3 O13 O10 52.4(10) . . . . ? O12 Cl3 O13 O10 89.3(7) . . . . ? O9 Cl3 O13 O10 -84.0(5) . . . . ? O11 Cl3 O13 O10 178.9(7) . . . . ? O14 Cl3 O13 O10 169.0(5) . . . . ? O13 O11 O14 Cl3 -11.9(8) . . . . ? O13 O11 O14 O12 26.5(11) . . . . ? Cl3 O11 O14 O12 38.5(4) . . . . ? O13 Cl3 O14 O11 9.6(6) . . . . ? O15 Cl3 O14 O11 135.2(6) . . . . ? O12 Cl3 O14 O11 128.4(6) . . . . ? O9 Cl3 O14 O11 -114.2(4) . . . . ? O10 Cl3 O14 O11 33.6(16) . . . . ? O13 Cl3 O14 O12 -118.8(5) . . . . ? O15 Cl3 O14 O12 6.8(8) . . . . ? O9 Cl3 O14 O12 117.5(4) . . . . ? O11 Cl3 O14 O12 -128.4(6) . . . . ? O10 Cl3 O14 O12 -94.7(15) . . . . ? O15 O12 O14 O11 -59(2) . . . . ? Cl3 O12 O14 O11 -43.5(5) . . . . ? O15 O12 O14 Cl3 -15(2) . . . . ? O14 O12 O15 Cl3 13.2(17) . . . . ? O13 Cl3 O15 O12 106.4(16) . . . . ? O9 Cl3 O15 O12 -112.7(13) . . . . ? O11 Cl3 O15 O12 42(2) . . . . ? O14 Cl3 O15 O12 -12.3(16) . . . . ? O10 Cl3 O15 O12 146.1(15) . . . . ? N3 Zn1 N1 C9 91.7(2) . . . . ? N5 Zn1 N1 C9 -63.5(3) . . . . ? N2 Zn1 N1 C9 -105.1(2) . . . . ? N4 Zn1 N1 C9 3.4(2) . . . . ? N6 Zn1 N1 C9 178.4(2) . . . . ? N3 Zn1 N1 C1 -147.6(2) . . . . ? N5 Zn1 N1 C1 57.3(3) . . . . ? N2 Zn1 N1 C1 15.6(2) . . . . ? N4 Zn1 N1 C1 124.1(2) . . . . ? N6 Zn1 N1 C1 -60.8(2) . . . . ? N3 Zn1 N1 C3 -28.27(19) . . . . ? N5 Zn1 N1 C3 176.5(2) . . . . ? N2 Zn1 N1 C3 134.89(19) . . . . ? N4 Zn1 N1 C3 -116.6(2) . . . . ? N6 Zn1 N1 C3 58.4(2) . . . . ? N3 Zn1 N2 C2 59.3(3) . . . . ? N5 Zn1 N2 C2 -150.2(2) . . . . ? N1 Zn1 N2 C2 13.94(19) . . . . ? N4 Zn1 N2 C2 -62.3(2) . . . . ? N6 Zn1 N2 C2 118.7(2) . . . . ? N3 Zn1 N2 C15 178.5(2) . . . . ? N5 Zn1 N2 C15 -30.97(19) . . . . ? N1 Zn1 N2 C15 133.2(2) . . . . ? N4 Zn1 N2 C15 56.9(2) . . . . ? N6 Zn1 N2 C15 -122.1(2) . . . . ? N3 Zn1 N2 C21 -62.6(4) . . . . ? N5 Zn1 N2 C21 87.9(2) . . . . ? N1 Zn1 N2 C21 -108.0(2) . . . . ? N4 Zn1 N2 C21 175.7(2) . . . . ? N6 Zn1 N2 C21 -3.3(2) . . . . ? N5 Zn1 N3 C8 2.6(3) . . . . ? N1 Zn1 N3 C8 -166.1(3) . . . . ? N2 Zn1 N3 C8 148.4(3) . . . . ? N4 Zn1 N3 C8 -86.5(3) . . . . ? N6 Zn1 N3 C8 90.8(3) . . . . ? N5 Zn1 N3 C4 -175.79(19) . . . . ? N1 Zn1 N3 C4 15.6(2) . . . . ? N2 Zn1 N3 C4 -30.0(4) . . . . ? N4 Zn1 N3 C4 95.1(2) . . . . ? N6 Zn1 N3 C4 -87.5(2) . . . . ? N3 Zn1 N4 C10 -71.5(2) . . . . ? N5 Zn1 N4 C10 168.1(2) . . . . ? N1 Zn1 N4 C10 10.0(2) . . . . ? N2 Zn1 N4 C10 88.5(2) . . . . ? N6 Zn1 N4 C10 -102.4(10) . . . . ? N3 Zn1 N4 C14 87.6(2) . . . . ? N5 Zn1 N4 C14 -32.8(2) . . . . ? N1 Zn1 N4 C14 169.0(3) . . . . ? N2 Zn1 N4 C14 -112.5(2) . . . . ? N6 Zn1 N4 C14 56.7(11) . . . . ? N3 Zn1 N5 C20 5.1(3) . . . . ? N1 Zn1 N5 C20 156.3(3) . . . . ? N2 Zn1 N5 C20 -161.7(3) . . . . ? N4 Zn1 N5 C20 91.7(3) . . . . ? N6 Zn1 N5 C20 -83.0(3) . . . . ? N3 Zn1 N5 C16 -178.61(19) . . . . ? N1 Zn1 N5 C16 -27.3(4) . . . . ? N2 Zn1 N5 C16 14.7(2) . . . . ? N4 Zn1 N5 C16 -91.9(2) . . . . ? N6 Zn1 N5 C16 93.3(2) . . . . ? N3 Zn1 N6 C26 -24.0(3) . . . . ? N5 Zn1 N6 C26 96.5(3) . . . . ? N1 Zn1 N6 C26 -104.5(3) . . . . ? N2 Zn1 N6 C26 176.3(3) . . . . ? N4 Zn1 N6 C26 6.9(11) . . . . ? N3 Zn1 N6 C22 175.4(2) . . . . ? N5 Zn1 N6 C22 -64.2(2) . . . . ? N1 Zn1 N6 C22 94.9(2) . . . . ? N2 Zn1 N6 C22 15.6(2) . . . . ? N4 Zn1 N6 C22 -153.8(9) . . . . ? N8 Zn2 N7 C28 -33.3(2) . . . . ? N8 Zn2 N7 C28 167.8(2) 2 . . . ? N9 Zn2 N7 C28 56.5(2) 2 . . . ? N9 Zn2 N7 C28 -128.7(2) . . . . ? N7 Zn2 N7 C28 134.5(2) 2 . . . ? N8 Zn2 N7 C34 85.6(2) . . . . ? N8 Zn2 N7 C34 -73.3(4) 2 . . . ? N9 Zn2 N7 C34 175.4(2) 2 . . . ? N9 Zn2 N7 C34 -9.8(2) . . . . ? N7 Zn2 N7 C34 -106.6(3) 2 . . . ? N8 Zn2 N7 C27 -152.9(2) . . . . ? N8 Zn2 N7 C27 48.3(3) 2 . . . ? N9 Zn2 N7 C27 -63.0(2) 2 . . . ? N9 Zn2 N7 C27 111.7(2) . . . . ? N7 Zn2 N7 C27 14.94(16) 2 . . . ? N8 Zn2 N8 C33 9.2(2) 2 . . . ? N9 Zn2 N8 C33 103.3(3) 2 . . . ? N9 Zn2 N8 C33 -83.7(3) . . . . ? N7 Zn2 N8 C33 164.7(2) 2 . . . ? N7 Zn2 N8 C33 -161.7(3) . . . . ? N8 Zn2 N8 C29 -170.2(2) 2 . . . ? N9 Zn2 N8 C29 -76.1(2) 2 . . . ? N9 Zn2 N8 C29 96.9(2) . . . . ? N7 Zn2 N8 C29 -14.7(4) 2 . . . ? N7 Zn2 N8 C29 19.0(2) . . . . ? N8 Zn2 N9 C35 -75.4(2) . . . . ? N8 Zn2 N9 C35 163.1(2) 2 . . . ? N9 Zn2 N9 C35 43.8(2) 2 . . . ? N7 Zn2 N9 C35 84.0(2) 2 . . . ? N7 Zn2 N9 C35 2.8(2) . . . . ? N8 Zn2 N9 C39 105.1(3) . . . . ? N8 Zn2 N9 C39 -16.5(3) 2 . . . ? N9 Zn2 N9 C39 -135.8(3) 2 . . . ? N7 Zn2 N9 C39 -95.5(3) 2 . . . ? N7 Zn2 N9 C39 -176.7(3) . . . . ? C9 N1 C1 C2 77.8(3) . . . . ? C3 N1 C1 C2 -155.4(3) . . . . ? Zn1 N1 C1 C2 -42.6(3) . . . . ? C15 N2 C2 C1 -153.6(3) . . . . ? C21 N2 C2 C1 80.5(3) . . . . ? Zn1 N2 C2 C1 -41.1(3) . . . . ? N1 C1 C2 N2 58.9(4) . . . . ? C9 N1 C3 C4 -82.2(3) . . . . ? C1 N1 C3 C4 151.2(3) . . . . ? Zn1 N1 C3 C4 37.2(3) . . . . ? C8 N3 C4 C5 -1.4(4) . . . . ? Zn1 N3 C4 C5 177.1(2) . . . . ? C8 N3 C4 C3 -176.7(3) . . . . ? Zn1 N3 C4 C3 1.8(3) . . . . ? N1 C3 C4 N3 -28.4(4) . . . . ? N1 C3 C4 C5 156.4(3) . . . . ? N3 C4 C5 C6 -0.7(5) . . . . ? C3 C4 C5 C6 174.3(3) . . . . ? C4 C5 C6 C7 1.4(5) . . . . ? C5 C6 C7 C8 -0.1(5) . . . . ? C4 N3 C8 C7 2.8(5) . . . . ? Zn1 N3 C8 C7 -175.4(3) . . . . ? C6 C7 C8 N3 -2.1(5) . . . . ? C1 N1 C9 C10 -132.5(3) . . . . ? C3 N1 C9 C10 99.9(3) . . . . ? Zn1 N1 C9 C10 -15.1(3) . . . . ? C14 N4 C10 C11 0.2(4) . . . . ? Zn1 N4 C10 C11 160.8(2) . . . . ? C14 N4 C10 C9 177.6(3) . . . . ? Zn1 N4 C10 C9 -21.8(3) . . . . ? N1 C9 C10 N4 25.4(4) . . . . ? N1 C9 C10 C11 -157.1(3) . . . . ? N4 C10 C11 C12 -0.4(5) . . . . ? C9 C10 C11 C12 -177.7(3) . . . . ? C10 C11 C12 C13 0.8(5) . . . . ? C11 C12 C13 C14 -1.0(5) . . . . ? C10 N4 C14 C13 -0.4(5) . . . . ? Zn1 N4 C14 C13 -158.5(3) . . . . ? C12 C13 C14 N4 0.8(5) . . . . ? C2 N2 C15 C16 157.4(3) . . . . ? C21 N2 C15 C16 -76.2(3) . . . . ? Zn1 N2 C15 C16 43.0(3) . . . . ? C20 N5 C16 C17 0.1(4) . . . . ? Zn1 N5 C16 C17 -176.6(2) . . . . ? C20 N5 C16 C15 -177.1(3) . . . . ? Zn1 N5 C16 C15 6.2(3) . . . . ? N2 C15 C16 N5 -35.4(4) . . . . ? N2 C15 C16 C17 147.4(3) . . . . ? N5 C16 C17 C18 -0.2(5) . . . . ? C15 C16 C17 C18 176.9(3) . . . . ? C16 C17 C18 C19 -0.5(5) . . . . ? C17 C18 C19 C20 1.1(6) . . . . ? C16 N5 C20 C19 0.6(5) . . . . ? Zn1 N5 C20 C19 176.7(3) . . . . ? C18 C19 C20 N5 -1.2(6) . . . . ? C2 N2 C21 C22 -127.0(3) . . . . ? C15 N2 C21 C22 105.9(3) . . . . ? Zn1 N2 C21 C22 -8.3(4) . . . . ? C26 N6 C22 C23 -3.8(5) . . . . ? Zn1 N6 C22 C23 158.9(3) . . . . ? C26 N6 C22 C21 171.9(3) . . . . ? Zn1 N6 C22 C21 -25.4(4) . . . . ? N2 C21 C22 N6 23.4(5) . . . . ? N2 C21 C22 C23 -160.9(3) . . . . ? N6 C22 C23 C24 4.0(5) . . . . ? C21 C22 C23 C24 -171.6(3) . . . . ? C22 C23 C24 C25 -0.6(5) . . . . ? C23 C24 C25 C26 -2.6(5) . . . . ? C22 N6 C26 C25 0.3(5) . . . . ? Zn1 N6 C26 C25 -159.4(3) . . . . ? C24 C25 C26 N6 2.9(5) . . . . ? C28 N7 C27 C27 -155.6(3) . . . 2 ? C34 N7 C27 C27 76.8(4) . . . 2 ? Zn2 N7 C27 C27 -43.5(4) . . . 2 ? C34 N7 C28 C29 -76.1(3) . . . . ? C27 N7 C28 C29 155.4(3) . . . . ? Zn2 N7 C28 C29 42.5(3) . . . . ? C33 N8 C29 C30 0.1(5) . . . . ? Zn2 N8 C29 C30 179.5(3) . . . . ? C33 N8 C29 C28 -179.2(3) . . . . ? Zn2 N8 C29 C28 0.2(3) . . . . ? N7 C28 C29 N8 -31.2(4) . . . . ? N7 C28 C29 C30 149.5(3) . . . . ? N8 C29 C30 C31 0.4(6) . . . . ? C28 C29 C30 C31 179.7(4) . . . . ? C29 C30 C31 C32 -0.8(7) . . . . ? C30 C31 C32 C33 0.5(7) . . . . ? C29 N8 C33 C32 -0.3(5) . . . . ? Zn2 N8 C33 C32 -179.7(3) . . . . ? C31 C32 C33 N8 0.0(6) . . . . ? C28 N7 C34 C35 129.6(3) . . . . ? C27 N7 C34 C35 -101.3(4) . . . . ? Zn2 N7 C34 C35 15.4(4) . . . . ? C39 N9 C35 C36 3.1(5) . . . . ? Zn2 N9 C35 C36 -176.4(3) . . . . ? C39 N9 C35 C34 -175.3(3) . . . . ? Zn2 N9 C35 C34 5.2(4) . . . . ? N7 C34 C35 N9 -14.3(5) . . . . ? N7 C34 C35 C36 167.3(3) . . . . ? N9 C35 C36 C37 -1.7(5) . . . . ? C34 C35 C36 C37 176.6(3) . . . . ? C35 C36 C37 C38 -0.8(5) . . . . ? C36 C37 C38 C39 1.7(5) . . . . ? C35 N9 C39 C38 -2.1(5) . . . . ? Zn2 N9 C39 C38 177.4(2) . . . . ? C37 C38 C39 N9 -0.4(5) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.181 _refine_diff_density_min -1.037 _refine_diff_density_rms 0.084