# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name _publ_author_address 'Karolina Suwala' ; Department of Chemistry Warsaw University of Technology Noakowskiego 3, PL-00-664 Warszawa Poland e-mail: lewin@ch.pw.edu.pl ; 'Michal Leszczynski' ; Department of Chemistry Warsaw University of Technology Noakowskiego 3, PL-00-664 Warszawa Poland e-mail: lewin@ch.pw.edu.pl ; 'Arkadiusz Kornowicz' ; Department of Chemistry Warsaw University of Technology Noakowskiego 3, PL-00-664 Warszawa Poland e-mail: lewin@ch.pw.edu.pl ; J.Lewinski ; Department of Chemistry Warsaw University of Technology Noakowskiego 3, PL-00-664 Warszawa Poland ; 'Iwona Justyniak' ; Institute of Physical Chemistry, Polish Academy of Sciences Kasprzaka 44/52, PL-01-224 Warszawa Poland ; ; Z.Kaszkur ; ; Institute of Physical Chemistry, Polish Academy of Sciences Kasprzaka 44/52, PL-01-224 Warszawa Poland ; 'Andrew E. H. Wheatley' ; Institute of Organic Chemistry, University of Cambridge Lensfield Road, Cambridge, CB2 1EW (UK) ; 'Maciej Cabaj' ; Institute of Organic Chemistry, University of Cambridge Lensfield Road, Cambridge, CB2 1EW (UK) ; _publ_contact_author_name 'Dr Janusz Lewinski' _publ_contact_author_address ; Department of Chemistry Warsaw University of Technology Noakowskiego 3, PL-00-664 Warszawa Poland ; _publ_contact_author_phone '048 22 2347315' _publ_contact_author_fax '048 22 2347279' _publ_contact_author_email lewin@ch.pw.edu.pl _publ_section_title ; Synthesis, Structure and Unique Reactivity of the Ethylzinc Derivative of a Bicyclic Guanidine ; # Attachment '- CCDC-805379.txt' # 3. data comp 1_3 data_shelxl_1_3 _database_code_depnum_ccdc_archive 'CCDC 805379' #TrackingRef '- CCDC-805379.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H51 N9 Zn3' _chemical_formula_weight 697.94 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' O O 0.0106 0.0060 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/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 38.0471(5) _cell_length_b 10.2929(8) _cell_length_c 18.4412(2) _cell_angle_alpha 90.00 _cell_angle_beta 107.167(4) _cell_angle_gamma 90.00 _cell_volume 6900.1(6) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5665 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 25.028 _exptl_crystal_description rectangular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.344 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2928 _exptl_absorpt_coefficient_mu 2.098 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'Scalepak (Otwinowski, Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device '\k-geometry diffractometr' _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method 'area detector \w scans' _diffrn_measurement_details ; 333 frames, \w rotation 0.8\% per frame (142s per frame) 56 frames, \w rotation 0.8\% per frame (142s per frame) 116 frames, \w rotation 0.8\% per frame (142s per frame) ; _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7810 _diffrn_reflns_av_R_equivalents 0.0306 _diffrn_reflns_av_sigmaI/netI 0.0369 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 21.97 _reflns_number_total 4189 _reflns_number_gt 3522 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'Denzo & Scalepak (Otwinowski, Minor, 1997)' _computing_data_reduction 'Denzo & Scalepak (Otwinowski, Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; DIAMOND v2.1 (Brandenburg, 1999) Ortep-3 for Windows, L.J.Farrugia (1997) J.Appl.Cryst. 30, 565, ORTEP III (Burnett, Johnson, 1996) ; _computing_publication_material ; SHELXL-97 (Sheldrick, 1997), ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0252P)^2^+120.5671P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4189 _refine_ls_number_parameters 370 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.0635 _refine_ls_R_factor_gt 0.0527 _refine_ls_wR_factor_ref 0.1287 _refine_ls_wR_factor_gt 0.1241 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.114 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1037(2) 0.4807(8) -0.0300(5) 0.050(2) Uani 1 1 d . E . H1A H 0.0794 0.4387 -0.0382 0.059 Uiso 1 1 calc R . . H1B H 0.1069 0.4960 -0.0807 0.059 Uiso 1 1 calc R . . C2 C 0.1310(4) 0.3902(11) 0.0084(7) 0.123(6) Uani 1 1 d . . . H2A H 0.1285 0.3106 -0.0218 0.184 Uiso 1 1 calc R . . H2B H 0.1278 0.3698 0.0580 0.184 Uiso 1 1 calc R . . H2C H 0.1554 0.4278 0.0155 0.184 Uiso 1 1 calc R . . C3 C 0.0938(2) 0.9061(8) 0.2431(4) 0.043(2) Uani 1 1 d . . . H3A H 0.1081 0.9866 0.2598 0.052 Uiso 1 1 calc R . . H3B H 0.0674 0.9291 0.2310 0.052 Uiso 1 1 calc R . . C4 C 0.1031(3) 0.8099(9) 0.3105(5) 0.058(3) Uani 1 1 d . . . H4A H 0.0973 0.8499 0.3538 0.086 Uiso 1 1 calc R . . H4B H 0.1294 0.7885 0.3248 0.086 Uiso 1 1 calc R . . H4C H 0.0886 0.7304 0.2957 0.086 Uiso 1 1 calc R . . C5 C 0.2307(3) 0.6351(11) 0.1734(5) 0.069(3) Uani 1 1 d . E . H5A H 0.2423 0.6537 0.2280 0.083 Uiso 1 1 calc R . . H5B H 0.2347 0.5418 0.1654 0.083 Uiso 1 1 calc R . . C6 C 0.2502(3) 0.7124(14) 0.1290(7) 0.095(4) Uani 1 1 d . . . H6A H 0.2764 0.6896 0.1451 0.142 Uiso 1 1 calc R . . H6B H 0.2474 0.8052 0.1377 0.142 Uiso 1 1 calc R . . H6C H 0.2397 0.6931 0.0748 0.142 Uiso 1 1 calc R . . C7 C 0.0425(2) 0.7448(9) -0.1148(4) 0.041(2) Uani 1 1 d . . . H7A H 0.0166 0.7343 -0.1155 0.050 Uiso 1 1 calc R . . H7B H 0.0515 0.6597 -0.1273 0.050 Uiso 1 1 calc R . . C8 C 0.0448(2) 0.8439(9) -0.1737(4) 0.040(2) Uani 1 1 d . . . H8A H 0.0306 0.8144 -0.2251 0.048 Uiso 1 1 calc R . . H8B H 0.0707 0.8570 -0.1728 0.048 Uiso 1 1 calc R . . C9 C 0.0288(2) 0.9694(8) -0.1536(4) 0.041(2) Uani 1 1 d . . . H9A H 0.0356 1.0423 -0.1820 0.049 Uiso 1 1 calc R . . H9B H 0.0017 0.9630 -0.1691 0.049 Uiso 1 1 calc R . . C10 C 0.0310(2) 1.1240(8) -0.0545(4) 0.039(2) Uani 1 1 d . . . H10A H 0.0042 1.1348 -0.0790 0.046 Uiso 1 1 calc R . . H10B H 0.0440 1.1917 -0.0748 0.046 Uiso 1 1 calc R . . C11 C 0.0394(2) 1.1410(8) 0.0304(4) 0.0361(19) Uani 1 1 d . . . H11A H 0.0388 1.2343 0.0431 0.043 Uiso 1 1 calc R . . H11B H 0.0208 1.0949 0.0488 0.043 Uiso 1 1 calc R . . C12 C 0.0771(2) 1.0856(7) 0.0672(4) 0.0331(19) Uani 1 1 d . . . H12A H 0.0953 1.1304 0.0472 0.040 Uiso 1 1 calc R . . H12B H 0.0840 1.1003 0.1227 0.040 Uiso 1 1 calc R . . C13 C 0.06182(19) 0.9076(7) -0.0195(4) 0.0290(18) Uani 1 1 d . . . C15 C 0.1596(2) 0.7642(9) -0.0372(4) 0.049(2) Uani 1 1 d . . . H15A H 0.1435 0.7000 -0.0713 0.059 Uiso 1 1 calc R . . H15B H 0.1854 0.7381 -0.0298 0.059 Uiso 1 1 calc R . . C16 C 0.1530(3) 0.8976(10) -0.0737(5) 0.064(3) Uani 1 1 d . . . H16A H 0.1591 0.8969 -0.1224 0.077 Uiso 1 1 calc R . . H16B H 0.1269 0.9226 -0.0840 0.077 Uiso 1 1 calc R . . C17 C 0.1772(3) 0.9924(10) -0.0199(7) 0.070(3) Uani 1 1 d . . . H17A H 0.2032 0.9763 -0.0176 0.084 Uiso 1 1 calc R . . H17B H 0.1708 1.0817 -0.0392 0.084 Uiso 1 1 calc R . . C18 C 0.1887(3) 1.0877(9) 0.1108(7) 0.075(4) Uani 1 1 d . . . H18A H 0.1819 1.1725 0.0852 0.090 Uiso 1 1 calc R . . H18B H 0.2159 1.0815 0.1271 0.090 Uiso 1 1 calc R . . C19 C 0.1755(3) 1.0835(9) 0.1795(7) 0.075(4) Uani 1 1 d . . . H19A H 0.1902 1.1435 0.2188 0.090 Uiso 1 1 calc R . . H19B H 0.1494 1.1104 0.1661 0.090 Uiso 1 1 calc R . . C20 C 0.1796(2) 0.9492(8) 0.2086(5) 0.058(3) Uani 1 1 d . . . H20A H 0.2060 0.9255 0.2244 0.070 Uiso 1 1 calc R . . H20B H 0.1708 0.9445 0.2539 0.070 Uiso 1 1 calc R . . C21 C 0.1612(2) 0.8723(8) 0.0798(5) 0.044(2) Uani 1 1 d . E . C22 C 0.0487(2) 0.6478(8) 0.1059(5) 0.045(2) Uani 1 1 d D . . H22A H 0.0422 0.6920 0.1479 0.054 Uiso 1 1 calc R A 1 H22B H 0.0369 0.6959 0.0585 0.054 Uiso 1 1 calc R A 1 C24 C 0.0500(3) 0.4581(12) 0.1802(7) 0.121(6) Uani 1 1 d D . . H24A H 0.0411 0.5081 0.2173 0.145 Uiso 1 1 calc R B 1 H24B H 0.0417 0.3669 0.1801 0.145 Uiso 1 1 calc R B 1 C25 C 0.1089(3) 0.3678(9) 0.2556(5) 0.077(4) Uani 1 1 d D . . H25A H 0.1072 0.2811 0.2316 0.093 Uiso 1 1 calc R C 1 H25B H 0.0975 0.3628 0.2973 0.093 Uiso 1 1 calc R C 1 C27 C 0.1637(3) 0.4415(9) 0.2296(7) 0.081(4) Uani 1 1 d D . . H27A H 0.1622 0.3646 0.1966 0.098 Uiso 1 1 calc R D 1 H27B H 0.1900 0.4656 0.2503 0.098 Uiso 1 1 calc R D 1 C28 C 0.1078(3) 0.5546(7) 0.1683(5) 0.044(2) Uani 1 1 d . . . N1 N 0.06445(16) 0.7848(6) -0.0397(3) 0.0303(15) Uani 1 1 d . E . N2 N 0.04240(16) 0.9959(6) -0.0726(3) 0.0312(15) Uani 1 1 d . . . N3 N 0.07750(16) 0.9449(6) 0.0516(3) 0.0311(15) Uani 1 1 d . . . N4 N 0.15192(17) 0.7645(6) 0.0359(4) 0.0373(16) Uani 1 1 d . E . N5 N 0.1734(2) 0.9821(7) 0.0558(5) 0.055(2) Uani 1 1 d . . . N6 N 0.15910(18) 0.8549(6) 0.1520(4) 0.0448(18) Uani 1 1 d . E . N7 N 0.08862(17) 0.6497(6) 0.1208(3) 0.0305(15) Uani 1 1 d . E . N8 N 0.0893(2) 0.4646(7) 0.1989(4) 0.056(2) Uani 1 1 d . E . N9 N 0.1437(2) 0.5497(6) 0.1836(4) 0.0455(19) Uani 1 1 d . E . Zn1 Zn 0.10148(2) 0.65564(9) 0.01742(5) 0.0321(3) Uani 1 1 d . . . Zn2 Zn 0.10318(3) 0.84559(9) 0.14772(5) 0.0365(3) Uani 1 1 d . E . Zn3 Zn 0.17703(3) 0.66420(9) 0.15041(5) 0.0438(3) Uani 1 1 d . . . C23 C 0.0352(3) 0.5188(12) 0.0991(7) 0.049(3) Uani 0.75 1 d PU E 1 H23A H 0.0443 0.4695 0.0622 0.058 Uiso 0.75 1 calc PR E 1 H23B H 0.0080 0.5182 0.0818 0.058 Uiso 0.75 1 calc PR E 1 C23A C 0.0308(7) 0.5944(19) 0.1651(15) 0.047(5) Uani 0.25 1 d PDU E 2 H23C H 0.0038 0.5866 0.1440 0.057 Uiso 0.25 1 calc PR E 2 H23D H 0.0368 0.6485 0.2116 0.057 Uiso 0.25 1 calc PR E 2 C26 C 0.1504(3) 0.4092(13) 0.2880(7) 0.048(3) Uani 0.75 1 d PDU E 1 H26A H 0.1526 0.4844 0.3225 0.057 Uiso 0.75 1 calc PR E 1 H26B H 0.1649 0.3365 0.3173 0.057 Uiso 0.75 1 calc PR E 1 C26A C 0.1396(7) 0.3189(17) 0.226(2) 0.070(9) Uani 0.25 1 d PDU E 2 H26C H 0.1298 0.2870 0.1728 0.083 Uiso 0.25 1 calc PR E 2 H26D H 0.1536 0.2483 0.2579 0.083 Uiso 0.25 1 calc PR E 2 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 C1 0.047(5) 0.040(5) 0.063(6) -0.020(5) 0.019(5) -0.004(4) C2 0.214(16) 0.055(8) 0.069(8) -0.028(6) -0.004(9) 0.069(9) C3 0.054(5) 0.041(5) 0.030(4) -0.006(4) 0.006(4) 0.000(4) C4 0.064(6) 0.055(6) 0.041(5) 0.009(5) -0.004(5) 0.004(5) C5 0.076(7) 0.068(7) 0.047(6) -0.007(5) -0.009(5) 0.037(6) C6 0.066(8) 0.126(12) 0.084(9) 0.033(8) 0.012(7) 0.025(8) C7 0.031(5) 0.056(6) 0.032(5) -0.013(4) 0.002(4) -0.003(4) C8 0.028(4) 0.067(6) 0.023(4) -0.004(4) 0.005(3) 0.004(4) C9 0.043(5) 0.053(6) 0.026(4) -0.001(4) 0.009(4) 0.009(4) C10 0.040(5) 0.039(5) 0.036(5) 0.004(4) 0.009(4) 0.012(4) C11 0.042(5) 0.029(5) 0.039(5) 0.000(4) 0.015(4) 0.007(4) C12 0.044(5) 0.025(4) 0.028(4) 0.001(4) 0.007(4) 0.007(4) C13 0.027(4) 0.034(5) 0.026(4) 0.007(4) 0.007(3) 0.003(4) C15 0.046(5) 0.066(7) 0.032(5) 0.003(5) 0.007(4) -0.019(5) C16 0.052(6) 0.081(8) 0.053(6) 0.032(6) 0.006(5) 0.001(6) C17 0.045(6) 0.047(6) 0.110(9) 0.037(6) 0.009(6) -0.009(5) C18 0.046(6) 0.017(5) 0.132(11) -0.012(6) -0.021(7) -0.003(4) C19 0.063(7) 0.035(6) 0.101(9) -0.027(6) -0.018(7) 0.013(5) C20 0.048(6) 0.036(6) 0.068(6) -0.028(5) -0.016(5) 0.011(4) C21 0.016(4) 0.028(5) 0.067(7) -0.004(5) -0.020(4) 0.002(4) C22 0.070(6) 0.038(5) 0.040(5) 0.009(4) 0.039(5) 0.013(5) C24 0.099(10) 0.084(9) 0.130(11) 0.077(9) -0.045(8) -0.051(8) C25 0.145(11) 0.037(6) 0.057(6) 0.031(5) 0.040(7) 0.015(6) C27 0.088(8) 0.029(6) 0.091(8) 0.020(6) -0.028(7) 0.002(5) C28 0.077(7) 0.016(5) 0.036(5) -0.004(4) 0.011(5) -0.005(5) N1 0.031(4) 0.030(4) 0.026(3) -0.006(3) 0.001(3) 0.004(3) N2 0.035(4) 0.040(4) 0.018(3) 0.001(3) 0.008(3) 0.007(3) N3 0.035(4) 0.026(4) 0.030(4) -0.006(3) 0.007(3) 0.004(3) N4 0.036(4) 0.030(4) 0.039(4) -0.004(3) 0.001(3) -0.005(3) N5 0.048(5) 0.031(4) 0.069(6) 0.014(4) -0.008(4) -0.008(4) N6 0.045(4) 0.026(4) 0.042(4) -0.014(3) -0.018(3) 0.010(3) N7 0.051(4) 0.019(3) 0.021(3) -0.001(3) 0.011(3) 0.003(3) N8 0.082(6) 0.029(4) 0.044(4) 0.002(4) -0.001(4) -0.009(4) N9 0.062(5) 0.021(4) 0.040(4) 0.003(3) -0.005(4) 0.009(4) Zn1 0.0338(5) 0.0264(5) 0.0318(5) -0.0076(4) 0.0032(4) 0.0017(4) Zn2 0.0548(6) 0.0228(5) 0.0251(5) -0.0036(4) 0.0015(4) 0.0064(4) Zn3 0.0495(6) 0.0299(6) 0.0398(6) -0.0050(5) -0.0055(5) 0.0131(5) C23 0.030(6) 0.061(8) 0.058(7) -0.011(6) 0.017(5) -0.006(6) C23A 0.030(10) 0.072(12) 0.052(11) -0.006(10) 0.031(9) -0.024(10) C26 0.031(7) 0.056(8) 0.056(8) 0.005(6) 0.012(6) 0.004(6) C26A 0.068(17) 0.047(17) 0.070(17) 0.004(15) -0.015(16) 0.004(15) _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 C1 C2 1.418(14) . ? C1 Zn1 2.014(8) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.547(11) . ? C3 Zn2 1.994(8) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.490(15) . ? C5 Zn3 1.981(10) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 N1 1.450(9) . ? C7 C8 1.512(11) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.519(11) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 N2 1.455(9) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 N2 1.458(10) . ? C10 C11 1.513(10) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.506(10) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 N3 1.478(9) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 N3 1.327(9) . ? C13 N1 1.330(10) . ? C13 N2 1.380(9) . ? C15 N4 1.461(10) . ? C15 C16 1.517(13) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.498(14) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 N5 1.449(13) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 N5 1.484(12) . ? C18 C19 1.495(15) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.474(13) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 N6 1.469(10) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 N5 1.346(11) . ? C21 N4 1.357(10) . ? C21 N6 1.370(11) . ? C21 Zn3 2.487(8) . ? C22 C23 1.415(14) . ? C22 N7 1.463(10) . ? C22 C23A 1.547(10) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C24 N8 1.433(14) . ? C24 C23A 1.568(10) . ? C24 C23 1.566(15) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 N8 1.476(11) . ? C25 C26A 1.518(10) . ? C25 C26 1.575(9) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C27 C26 1.359(15) . ? C27 N9 1.469(11) . ? C27 C26A 1.550(10) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 N9 1.310(11) . ? C28 N7 1.372(10) . ? C28 N8 1.382(11) . ? N1 Zn1 1.996(6) . ? N3 Zn2 2.029(6) . ? N4 Zn1 2.161(6) . ? N4 Zn3 2.290(6) . ? N6 Zn3 2.081(6) . ? N6 Zn2 2.108(7) . ? N7 Zn1 2.105(6) . ? N7 Zn2 2.111(6) . ? N9 Zn3 1.958(8) . ? Zn1 Zn2 3.0836(12) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C23A H23C 0.9900 . ? C23A H23D 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C26A H26C 0.9900 . ? C26A H26D 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 Zn1 119.3(7) . . ? C2 C1 H1A 107.5 . . ? Zn1 C1 H1A 107.5 . . ? C2 C1 H1B 107.5 . . ? Zn1 C1 H1B 107.5 . . ? H1A C1 H1B 107.0 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 Zn2 116.8(6) . . ? C4 C3 H3A 108.1 . . ? Zn2 C3 H3A 108.1 . . ? C4 C3 H3B 108.1 . . ? Zn2 C3 H3B 108.1 . . ? H3A C3 H3B 107.3 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 Zn3 116.8(7) . . ? C6 C5 H5A 108.1 . . ? Zn3 C5 H5A 108.1 . . ? C6 C5 H5B 108.1 . . ? Zn3 C5 H5B 108.1 . . ? H5A C5 H5B 107.3 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N1 C7 C8 110.9(7) . . ? N1 C7 H7A 109.5 . . ? C8 C7 H7A 109.5 . . ? N1 C7 H7B 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 108.1 . . ? C7 C8 C9 106.7(6) . . ? C7 C8 H8A 110.4 . . ? C9 C8 H8A 110.4 . . ? C7 C8 H8B 110.4 . . ? C9 C8 H8B 110.4 . . ? H8A C8 H8B 108.6 . . ? N2 C9 C8 111.3(6) . . ? N2 C9 H9A 109.4 . . ? C8 C9 H9A 109.4 . . ? N2 C9 H9B 109.4 . . ? C8 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? N2 C10 C11 110.8(6) . . ? N2 C10 H10A 109.5 . . ? C11 C10 H10A 109.5 . . ? N2 C10 H10B 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 108.1 . . ? C12 C11 C10 107.7(6) . . ? C12 C11 H11A 110.2 . . ? C10 C11 H11A 110.2 . . ? C12 C11 H11B 110.2 . . ? C10 C11 H11B 110.2 . . ? H11A C11 H11B 108.5 . . ? N3 C12 C11 110.3(6) . . ? N3 C12 H12A 109.6 . . ? C11 C12 H12A 109.6 . . ? N3 C12 H12B 109.6 . . ? C11 C12 H12B 109.6 . . ? H12A C12 H12B 108.1 . . ? N3 C13 N1 120.1(7) . . ? N3 C13 N2 120.1(7) . . ? N1 C13 N2 119.7(6) . . ? N4 C15 C16 110.9(8) . . ? N4 C15 H15A 109.5 . . ? C16 C15 H15A 109.5 . . ? N4 C15 H15B 109.5 . . ? C16 C15 H15B 109.5 . . ? H15A C15 H15B 108.0 . . ? C17 C16 C15 107.9(7) . . ? C17 C16 H16A 110.1 . . ? C15 C16 H16A 110.1 . . ? C17 C16 H16B 110.1 . . ? C15 C16 H16B 110.1 . . ? H16A C16 H16B 108.4 . . ? N5 C17 C16 111.9(7) . . ? N5 C17 H17A 109.2 . . ? C16 C17 H17A 109.2 . . ? N5 C17 H17B 109.2 . . ? C16 C17 H17B 109.2 . . ? H17A C17 H17B 107.9 . . ? N5 C18 C19 113.3(9) . . ? N5 C18 H18A 108.9 . . ? C19 C18 H18A 108.9 . . ? N5 C18 H18B 108.9 . . ? C19 C18 H18B 108.9 . . ? H18A C18 H18B 107.7 . . ? C20 C19 C18 108.0(9) . . ? C20 C19 H19A 110.1 . . ? C18 C19 H19A 110.1 . . ? C20 C19 H19B 110.1 . . ? C18 C19 H19B 110.1 . . ? H19A C19 H19B 108.4 . . ? N6 C20 C19 112.7(8) . . ? N6 C20 H20A 109.1 . . ? C19 C20 H20A 109.1 . . ? N6 C20 H20B 109.1 . . ? C19 C20 H20B 109.1 . . ? H20A C20 H20B 107.8 . . ? N5 C21 N4 123.1(9) . . ? N5 C21 N6 123.7(8) . . ? N4 C21 N6 113.1(7) . . ? N5 C21 Zn3 147.3(5) . . ? N4 C21 Zn3 65.7(4) . . ? N6 C21 Zn3 56.8(4) . . ? C23 C22 N7 111.0(7) . . ? C23 C22 C23A 60.4(11) . . ? N7 C22 C23A 121.4(12) . . ? C23 C22 H22A 109.4 . . ? N7 C22 H22A 109.4 . . ? C23A C22 H22A 49.3 . . ? C23 C22 H22B 109.4 . . ? N7 C22 H22B 109.4 . . ? C23A C22 H22B 128.6 . . ? H22A C22 H22B 108.0 . . ? N8 C24 C23A 113.5(13) . . ? N8 C24 C23 105.5(10) . . ? C23A C24 C23 57.0(11) . . ? N8 C24 H24A 110.7 . . ? C23A C24 H24A 54.7 . . ? C23 C24 H24A 110.7 . . ? N8 C24 H24B 110.6 . . ? C23A C24 H24B 135.9 . . ? C23 C24 H24B 110.6 . . ? H24A C24 H24B 108.8 . . ? N8 C25 C26A 104.4(15) . . ? N8 C25 C26 109.1(8) . . ? C26A C25 C26 55.5(12) . . ? N8 C25 H25A 109.9 . . ? C26A C25 H25A 59.6 . . ? C26 C25 H25A 109.9 . . ? N8 C25 H25B 109.9 . . ? C26A C25 H25B 145.7 . . ? C26 C25 H25B 109.9 . . ? H25A C25 H25B 108.3 . . ? C26 C27 N9 113.1(11) . . ? C26 C27 C26A 59.0(13) . . ? N9 C27 C26A 113.0(15) . . ? C26 C27 H27A 109.0 . . ? N9 C27 H27A 109.0 . . ? C26A C27 H27A 52.7 . . ? C26 C27 H27B 109.0 . . ? N9 C27 H27B 109.0 . . ? C26A C27 H27B 137.6 . . ? H27A C27 H27B 107.8 . . ? N9 C28 N7 119.3(7) . . ? N9 C28 N8 120.8(8) . . ? N7 C28 N8 119.9(8) . . ? C13 N1 C7 117.9(6) . . ? C13 N1 Zn1 125.8(5) . . ? C7 N1 Zn1 115.6(5) . . ? C13 N2 C9 124.0(6) . . ? C13 N2 C10 124.5(6) . . ? C9 N2 C10 111.4(6) . . ? C13 N3 C12 116.6(6) . . ? C13 N3 Zn2 132.7(5) . . ? C12 N3 Zn2 110.7(4) . . ? C21 N4 C15 117.6(7) . . ? C21 N4 Zn1 125.5(5) . . ? C15 N4 Zn1 105.2(5) . . ? C21 N4 Zn3 81.7(5) . . ? C15 N4 Zn3 135.0(5) . . ? Zn1 N4 Zn3 91.2(2) . . ? C21 N5 C17 121.4(8) . . ? C21 N5 C18 119.6(9) . . ? C17 N5 C18 118.3(8) . . ? C21 N6 C20 115.6(8) . . ? C21 N6 Zn3 89.8(5) . . ? C20 N6 Zn3 121.7(5) . . ? C21 N6 Zn2 108.5(5) . . ? C20 N6 Zn2 112.0(6) . . ? Zn3 N6 Zn2 106.8(3) . . ? C28 N7 C22 116.0(7) . . ? C28 N7 Zn1 112.1(5) . . ? C22 N7 Zn1 109.7(4) . . ? C28 N7 Zn2 118.6(5) . . ? C22 N7 Zn2 104.1(5) . . ? Zn1 N7 Zn2 94.0(2) . . ? C28 N8 C24 123.7(8) . . ? C28 N8 C25 121.9(8) . . ? C24 N8 C25 114.3(8) . . ? C28 N9 C27 118.9(8) . . ? C28 N9 Zn3 129.7(6) . . ? C27 N9 Zn3 111.3(7) . . ? N1 Zn1 C1 118.7(3) . . ? N1 Zn1 N7 100.4(2) . . ? C1 Zn1 N7 114.7(3) . . ? N1 Zn1 N4 101.2(2) . . ? C1 Zn1 N4 112.5(3) . . ? N7 Zn1 N4 107.8(2) . . ? N1 Zn1 Zn2 80.68(17) . . ? C1 Zn1 Zn2 155.7(3) . . ? N7 Zn1 Zn2 43.07(16) . . ? N4 Zn1 Zn2 74.62(17) . . ? C3 Zn2 N3 116.6(3) . . ? C3 Zn2 N6 113.2(3) . . ? N3 Zn2 N6 103.3(3) . . ? C3 Zn2 N7 113.7(3) . . ? N3 Zn2 N7 104.5(2) . . ? N6 Zn2 N7 104.1(2) . . ? C3 Zn2 Zn1 156.5(3) . . ? N3 Zn2 Zn1 75.21(16) . . ? N6 Zn2 Zn1 81.19(17) . . ? N7 Zn2 Zn1 42.91(15) . . ? N9 Zn3 C5 124.3(4) . . ? N9 Zn3 N6 108.5(3) . . ? C5 Zn3 N6 117.5(4) . . ? N9 Zn3 N4 115.3(3) . . ? C5 Zn3 N4 112.9(3) . . ? N6 Zn3 N4 62.5(2) . . ? N9 Zn3 C21 127.1(3) . . ? C5 Zn3 C21 108.5(4) . . ? N6 Zn3 C21 33.4(3) . . ? N4 Zn3 C21 32.7(2) . . ? C22 C23 C24 105.7(9) . . ? C22 C23 H23A 110.6 . . ? C24 C23 H23A 110.6 . . ? C22 C23 H23B 110.6 . . ? C24 C23 H23B 110.6 . . ? H23A C23 H23B 108.7 . . ? C22 C23A C24 99.5(9) . . ? C22 C23A H23C 111.9 . . ? C24 C23A H23C 111.9 . . ? C22 C23A H23D 111.9 . . ? C24 C23A H23D 111.9 . . ? H23C C23A H23D 109.6 . . ? C27 C26 C25 109.4(9) . . ? C27 C26 H26A 109.8 . . ? C25 C26 H26A 109.8 . . ? C27 C26 H26B 109.8 . . ? C25 C26 H26B 109.8 . . ? H26A C26 H26B 108.2 . . ? C25 C26A C27 102.8(11) . . ? C25 C26A H26C 111.2 . . ? C27 C26A H26C 111.2 . . ? C25 C26A H26D 111.2 . . ? C27 C26A H26D 111.2 . . ? H26C C26A H26D 109.1 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 21.97 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.891 _refine_diff_density_min -0.745 _refine_diff_density_rms 0.096 # Attachment '- CCDC-805380.txt' #======================================================= # 3. data comp 1_4 data_shelxl_1_4 _database_code_depnum_ccdc_archive 'CCDC 805380' #TrackingRef '- CCDC-805380.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H68 N12 O Zn5' _chemical_formula_weight 1011.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P n a 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 19.9841(4) _cell_length_b 10.5322(10) _cell_length_c 20.1641(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4244.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5328 _cell_measurement_theta_min 0.407 _cell_measurement_theta_max 27.485 _exptl_crystal_description hexagonal _exptl_crystal_colour colorless _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.38 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.584 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2104 _exptl_absorpt_coefficient_mu 2.830 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'Scalepak (Otwinowski, Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device '\k-geometry diffractometr' _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method 'area detector \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6162 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0510 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 24.10 _reflns_number_total 6162 _reflns_number_gt 5375 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'Denzo & Scalepak (Otwinowski, Minor, 1997)' _computing_data_reduction 'Denzo & Scalepak (Otwinowski, Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; DIAMOND v2.1 (Brandenburg, 1999) Ortep-3 for Windows, L.J.Farrugia (1997) J.Appl.Cryst. 30, 565, ORTEP III (Burnett, Johnson, 1996) ; _computing_publication_material ; SHELXL-97 (Sheldrick, 1997), ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0739P)^2^+41.0429P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.46(4) _refine_ls_number_reflns 6162 _refine_ls_number_parameters 540 _refine_ls_number_restraints 71 _refine_ls_R_factor_all 0.0805 _refine_ls_R_factor_gt 0.0643 _refine_ls_wR_factor_ref 0.1824 _refine_ls_wR_factor_gt 0.1488 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.103 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.001 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 C1 C 0.3552(7) 0.5364(13) 0.2064(7) 0.048(4) Uani 1 1 d . . . H1A H 0.3497 0.5457 0.2550 0.057 Uiso 1 1 calc R . . H1B H 0.3885 0.6003 0.1920 0.057 Uiso 1 1 calc R . . C2 C 0.2889(8) 0.5683(15) 0.1739(10) 0.068(5) Uani 1 1 d . . . H2A H 0.2931 0.5600 0.1256 0.102 Uiso 1 1 calc R . . H2B H 0.2763 0.6557 0.1850 0.102 Uiso 1 1 calc R . . H2C H 0.2543 0.5099 0.1899 0.102 Uiso 1 1 calc R . . C3 C 0.5763(13) 0.0638(18) 0.2719(13) 0.111(10) Uani 1 1 d . . . H3A H 0.6100 0.1246 0.2887 0.134 Uiso 1 1 calc R A 1 H3B H 0.5506 0.0311 0.3103 0.134 Uiso 1 1 calc R A 1 C5 C 0.5374(10) 0.3855(14) -0.0150(10) 0.076(6) Uani 1 1 d . . . H5A H 0.5027 0.4436 -0.0324 0.091 Uiso 1 1 calc R . . H5B H 0.5798 0.4340 -0.0129 0.091 Uiso 1 1 calc R . . C6 C 0.5466(13) 0.2797(17) -0.0648(9) 0.099(9) Uani 1 1 d . . . H6A H 0.5592 0.3158 -0.1078 0.149 Uiso 1 1 calc R . . H6B H 0.5047 0.2323 -0.0693 0.149 Uiso 1 1 calc R . . H6C H 0.5820 0.2223 -0.0495 0.149 Uiso 1 1 calc R . . C7 C 0.3472(6) 0.5188(13) -0.0149(7) 0.040(3) Uani 1 1 d . . . H7A H 0.3509 0.5152 -0.0639 0.047 Uiso 1 1 calc R . . H7B H 0.3004 0.5417 -0.0040 0.047 Uiso 1 1 calc R . . C8 C 0.3924(8) 0.6222(13) 0.0101(12) 0.070(6) Uani 1 1 d . . . H8A H 0.3878 0.6295 0.0583 0.106 Uiso 1 1 calc R . . H8B H 0.3801 0.7029 -0.0108 0.106 Uiso 1 1 calc R . . H8C H 0.4389 0.6016 -0.0010 0.106 Uiso 1 1 calc R . . C9 C 0.2951(13) 0.2500(18) 0.2791(12) 0.105(9) Uani 1 1 d . . . H9A H 0.3157 0.2762 0.3216 0.126 Uiso 1 1 calc R . . H9B H 0.2716 0.3246 0.2604 0.126 Uiso 1 1 calc R . . C10 C 0.2477(10) 0.1510(17) 0.2913(12) 0.088(7) Uani 1 1 d . . . H10A H 0.2229 0.1334 0.2498 0.105 Uiso 1 1 calc R . . H10B H 0.2151 0.1807 0.3248 0.105 Uiso 1 1 calc R . . C11 C 0.2792(8) 0.0299(15) 0.3153(8) 0.053(4) Uani 1 1 d . . . H11A H 0.2889 0.0368 0.3633 0.064 Uiso 1 1 calc R . . H11B H 0.2477 -0.0416 0.3087 0.064 Uiso 1 1 calc R . . C12 C 0.3669(9) -0.1225(15) 0.2891(8) 0.059(4) Uani 1 1 d . . . H12A H 0.3367 -0.1839 0.2670 0.071 Uiso 1 1 calc R . . H12B H 0.3668 -0.1420 0.3371 0.071 Uiso 1 1 calc R . . C13 C 0.4350(8) -0.1402(15) 0.2633(7) 0.052(4) Uani 1 1 d . . . H13A H 0.4459 -0.2317 0.2602 0.062 Uiso 1 1 calc R . . H13B H 0.4681 -0.0988 0.2928 0.062 Uiso 1 1 calc R . . C14 C 0.4358(7) -0.0795(11) 0.1951(6) 0.039(3) Uani 1 1 d . E . H14A H 0.4803 -0.0928 0.1748 0.047 Uiso 1 1 calc R . . H14B H 0.4022 -0.1223 0.1667 0.047 Uiso 1 1 calc R . . C15 C 0.3687(6) 0.0912(12) 0.2368(5) 0.032(3) Uani 1 1 d . E . C16 C 0.6301(7) 0.1926(19) 0.1289(11) 0.086(7) Uani 1 1 d . E . H16A H 0.6471 0.1251 0.1586 0.104 Uiso 1 1 calc R . . H16B H 0.6334 0.2745 0.1527 0.104 Uiso 1 1 calc R . . C17 C 0.6728(8) 0.198(2) 0.0673(13) 0.100(9) Uani 1 1 d . . . H17A H 0.7197 0.2182 0.0790 0.120 Uiso 1 1 calc R . . H17B H 0.6559 0.2640 0.0366 0.120 Uiso 1 1 calc R . . C18 C 0.6687(7) 0.0680(16) 0.0350(10) 0.066(5) Uani 1 1 d . E . H18A H 0.6855 0.0739 -0.0111 0.079 Uiso 1 1 calc R . . H18B H 0.6979 0.0082 0.0594 0.079 Uiso 1 1 calc R . . C19 C 0.5943(8) -0.0863(13) -0.0119(9) 0.051(4) Uani 1 1 d . E . H19A H 0.6300 -0.1496 -0.0036 0.061 Uiso 1 1 calc R . . H19B H 0.5990 -0.0552 -0.0580 0.061 Uiso 1 1 calc R . . C20 C 0.5254(7) -0.1481(12) -0.0026(7) 0.045(3) Uani 1 1 d . . . H20A H 0.5160 -0.2070 -0.0398 0.053 Uiso 1 1 calc R . . H20B H 0.5243 -0.1970 0.0393 0.053 Uiso 1 1 calc R . . C21 C 0.4747(6) -0.0455(13) -0.0009(6) 0.040(3) Uani 1 1 d . E . H21A H 0.4763 0.0024 -0.0431 0.048 Uiso 1 1 calc R . . H21B H 0.4296 -0.0836 0.0031 0.048 Uiso 1 1 calc R . . C22 C 0.5485(6) 0.0732(14) 0.0662(6) 0.038(3) Uani 1 1 d . E . C23 C 0.4796(9) 0.3300(19) 0.3079(8) 0.088(7) Uani 1 1 d D . . H23A H 0.4677 0.2424 0.3213 0.106 Uiso 1 1 calc R B 1 H23B H 0.4431 0.3878 0.3218 0.106 Uiso 1 1 calc R B 1 C28 C 0.5781(7) 0.5630(12) 0.1340(10) 0.075(6) Uani 1 1 d D . . H28A H 0.5716 0.5779 0.0859 0.091 Uiso 1 1 calc R C 1 H28B H 0.6254 0.5377 0.1400 0.091 Uiso 1 1 calc R C 1 C29 C 0.5293(8) 0.4376(13) 0.2153(12) 0.064(6) Uani 1 1 d . . . C30 C 0.3365(9) 0.1939(15) -0.1001(7) 0.056(4) Uani 1 1 d . . . H30A H 0.3619 0.1228 -0.1200 0.067 Uiso 1 1 calc R . . H30B H 0.3564 0.2745 -0.1158 0.067 Uiso 1 1 calc R . . C31 C 0.2629(9) 0.1866(15) -0.1221(7) 0.056(4) Uani 1 1 d . . . H31A H 0.2364 0.2551 -0.1010 0.067 Uiso 1 1 calc R . . H31B H 0.2593 0.1953 -0.1708 0.067 Uiso 1 1 calc R . . C32 C 0.2376(7) 0.0578(12) -0.1001(7) 0.042(3) Uani 1 1 d . . . H32A H 0.1880 0.0581 -0.1008 0.050 Uiso 1 1 calc R . . H32B H 0.2531 -0.0074 -0.1319 0.050 Uiso 1 1 calc R . . C33 C 0.2317(7) -0.0934(12) -0.0084(7) 0.044(3) Uani 1 1 d . . . H33A H 0.2400 -0.1616 -0.0412 0.053 Uiso 1 1 calc R . . H33B H 0.1827 -0.0824 -0.0043 0.053 Uiso 1 1 calc R . . C34 C 0.2596(7) -0.1345(11) 0.0582(7) 0.040(3) Uani 1 1 d . . . H34A H 0.3020 -0.1817 0.0520 0.048 Uiso 1 1 calc R . . H34B H 0.2273 -0.1906 0.0811 0.048 Uiso 1 1 calc R . . C35 C 0.2719(6) -0.0156(12) 0.0990(7) 0.041(3) Uani 1 1 d . E . H35A H 0.2292 0.0303 0.1054 0.049 Uiso 1 1 calc R . . H35B H 0.2892 -0.0398 0.1433 0.049 Uiso 1 1 calc R . . C36 C 0.3071(6) 0.0921(11) 0.0011(6) 0.032(3) Uani 1 1 d . E . N1 N 0.3482(6) 0.2100(11) 0.2328(5) 0.044(3) Uani 1 1 d . . . N2 N 0.3404(6) 0.0058(11) 0.2794(6) 0.044(3) Uani 1 1 d . . . N3 N 0.4214(5) 0.0562(10) 0.1966(5) 0.038(2) Uani 1 1 d . . . N4 N 0.5590(5) 0.1669(11) 0.1130(6) 0.050(3) Uani 1 1 d . . . N5 N 0.6009(5) 0.0187(11) 0.0342(7) 0.050(3) Uani 1 1 d . . . N6 N 0.4857(5) 0.0419(10) 0.0543(5) 0.031(2) Uani 1 1 d . . . N7 N 0.4897(7) 0.3370(12) 0.2363(6) 0.053(4) Uani 1 1 d . D . N8 N 0.5513(8) 0.5228(14) 0.2626(7) 0.090(6) Uani 1 1 d D D . N9 N 0.5383(6) 0.4561(12) 0.1511(8) 0.056(4) Uani 1 1 d . D . N10 N 0.3413(5) 0.1871(10) -0.0276(5) 0.034(2) Uani 1 1 d . . . N11 N 0.2606(5) 0.0234(9) -0.0329(5) 0.031(2) Uani 1 1 d . . . N12 N 0.3198(5) 0.0671(9) 0.0664(4) 0.030(2) Uani 1 1 d . . . O14 O 0.4152(4) 0.3028(7) 0.0970(4) 0.0290(16) Uani 1 1 d . . . Zn1 Zn 0.39284(7) 0.36388(14) 0.18838(7) 0.0344(4) Uani 1 1 d . D . Zn2 Zn 0.51501(9) 0.15182(17) 0.21054(8) 0.0468(5) Uani 1 1 d . D . Zn3 Zn 0.51139(8) 0.33802(15) 0.07945(9) 0.0440(4) Uani 1 1 d . D . Zn4 Zn 0.36578(7) 0.34798(13) 0.02104(7) 0.0333(3) Uani 1 1 d . D . Zn5 Zn 0.40723(7) 0.11810(12) 0.10116(7) 0.0278(3) Uani 1 1 d . D . C24 C 0.5467(11) 0.371(3) 0.3400(11) 0.043(6) Uani 0.51(3) 1 d PDU D 1 H24A H 0.5410 0.3614 0.3885 0.052 Uiso 0.51(3) 1 calc PR D 1 H24B H 0.5804 0.3069 0.3264 0.052 Uiso 0.51(3) 1 calc PR D 1 C24A C 0.4553(13) 0.444(2) 0.3486(14) 0.062(8) Uani 0.49(3) 1 d PDU D 2 H24C H 0.4503 0.4263 0.3965 0.075 Uiso 0.49(3) 1 calc PR D 2 H24D H 0.4148 0.4854 0.3304 0.075 Uiso 0.49(3) 1 calc PR D 2 C25 C 0.5779(14) 0.500(3) 0.3285(9) 0.057(6) Uani 0.59(3) 1 d PDU D 1 H25A H 0.5622 0.5636 0.3610 0.069 Uiso 0.59(3) 1 calc PR D 1 H25B H 0.6274 0.4964 0.3287 0.069 Uiso 0.59(3) 1 calc PR D 1 C25A C 0.5213(17) 0.512(4) 0.3302(11) 0.067(7) Uani 0.41(3) 1 d PDU D 2 H25C H 0.5164 0.6000 0.3465 0.081 Uiso 0.41(3) 1 calc PR D 2 H25D H 0.5562 0.4720 0.3582 0.081 Uiso 0.41(3) 1 calc PR D 2 C4 C 0.6136(13) -0.053(2) 0.2352(12) 0.057(8) Uani 0.62(3) 1 d P E 1 H4A H 0.6434 -0.0956 0.2667 0.085 Uiso 0.62(3) 1 calc PR E 1 H4B H 0.6400 -0.0201 0.1979 0.085 Uiso 0.62(3) 1 calc PR E 1 H4C H 0.5803 -0.1131 0.2187 0.085 Uiso 0.62(3) 1 calc PR E 1 C4A C 0.6217(14) 0.128(3) 0.3193(15) 0.027(8) Uani 0.38(3) 1 d P E 2 H4A1 H 0.6455 0.0647 0.3457 0.041 Uiso 0.38(3) 1 calc PR E 2 H4A2 H 0.5954 0.1831 0.3488 0.041 Uiso 0.38(3) 1 calc PR E 2 H4A3 H 0.6541 0.1801 0.2948 0.041 Uiso 0.38(3) 1 calc PR E 2 C27 C 0.5694(13) 0.6908(15) 0.1683(9) 0.049(6) Uani 0.59(3) 1 d PDU D 1 H27A H 0.5230 0.7234 0.1661 0.059 Uiso 0.59(3) 1 calc PR D 1 H27B H 0.6013 0.7560 0.1525 0.059 Uiso 0.59(3) 1 calc PR D 1 C27A C 0.6244(14) 0.583(3) 0.1954(12) 0.046(6) Uani 0.41(3) 1 d PDU D 2 H27C H 0.6530 0.6556 0.1829 0.055 Uiso 0.41(3) 1 calc PR D 2 H27D H 0.6543 0.5077 0.1948 0.055 Uiso 0.41(3) 1 calc PR D 2 C26 C 0.5879(13) 0.636(2) 0.2371(10) 0.063(6) Uani 0.66(3) 1 d PDU D 1 H26A H 0.6361 0.6145 0.2361 0.076 Uiso 0.66(3) 1 calc PR D 1 H26B H 0.5823 0.7051 0.2700 0.076 Uiso 0.66(3) 1 calc PR D 1 C26A C 0.6092(17) 0.605(4) 0.273(2) 0.053(7) Uani 0.34(3) 1 d PDU D 2 H26C H 0.6435 0.5698 0.3028 0.064 Uiso 0.34(3) 1 calc PR D 2 H26D H 0.5979 0.6938 0.2842 0.064 Uiso 0.34(3) 1 calc PR D 2 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 C1 0.064(10) 0.035(8) 0.044(8) 0.000(6) 0.010(7) 0.023(7) C2 0.053(10) 0.047(9) 0.104(15) 0.001(9) 0.017(9) 0.017(8) C3 0.15(2) 0.047(11) 0.14(2) -0.005(12) -0.104(18) 0.014(12) C5 0.088(13) 0.030(8) 0.108(15) -0.012(8) 0.074(12) 0.004(8) C6 0.18(2) 0.052(11) 0.065(12) -0.024(9) 0.079(14) -0.013(12) C7 0.029(7) 0.052(9) 0.037(7) 0.003(6) 0.001(6) -0.002(6) C8 0.056(10) 0.027(7) 0.129(19) 0.015(9) 0.017(11) -0.007(7) C9 0.16(2) 0.055(12) 0.099(16) 0.019(11) 0.087(16) 0.031(13) C10 0.079(13) 0.061(12) 0.123(18) 0.036(11) 0.052(13) 0.022(10) C11 0.054(9) 0.060(10) 0.045(9) 0.017(7) 0.009(7) 0.001(8) C12 0.083(12) 0.058(10) 0.037(8) 0.018(7) -0.002(8) 0.016(9) C13 0.066(10) 0.061(10) 0.028(7) 0.013(7) -0.001(7) 0.009(8) C14 0.061(8) 0.032(6) 0.023(6) 0.005(5) 0.000(6) 0.019(6) C15 0.039(7) 0.047(8) 0.010(5) 0.001(5) -0.002(5) 0.014(6) C16 0.034(8) 0.097(14) 0.129(18) -0.082(13) -0.027(10) 0.012(9) C17 0.037(9) 0.086(13) 0.18(2) -0.078(15) 0.020(12) -0.023(9) C18 0.035(8) 0.072(11) 0.091(13) -0.039(10) 0.003(8) 0.016(7) C19 0.058(9) 0.025(7) 0.070(10) -0.008(7) 0.015(8) -0.003(7) C20 0.066(9) 0.036(7) 0.031(7) -0.004(6) 0.002(6) 0.009(7) C21 0.042(8) 0.046(8) 0.032(7) -0.017(6) 0.015(6) -0.011(6) C22 0.030(7) 0.060(9) 0.023(7) -0.018(6) 0.002(5) 0.006(6) C23 0.129(18) 0.103(15) 0.032(9) -0.029(9) -0.039(10) 0.055(14) C28 0.037(8) 0.031(8) 0.158(19) -0.037(9) -0.039(10) 0.003(7) C29 0.046(9) 0.021(7) 0.125(18) -0.028(9) -0.050(11) 0.008(7) C30 0.081(12) 0.054(9) 0.032(8) 0.002(7) 0.013(8) -0.019(8) C31 0.087(12) 0.056(9) 0.024(7) -0.001(6) -0.007(7) 0.008(9) C32 0.046(8) 0.038(7) 0.041(8) -0.007(6) -0.022(6) -0.001(6) C33 0.047(8) 0.033(7) 0.053(9) -0.014(6) 0.001(7) -0.006(6) C34 0.043(7) 0.029(7) 0.047(8) 0.005(6) 0.008(6) 0.007(6) C35 0.040(7) 0.050(8) 0.033(7) 0.017(7) 0.004(6) -0.007(6) C36 0.026(6) 0.023(6) 0.048(8) -0.001(5) -0.009(6) 0.002(5) N1 0.064(8) 0.047(7) 0.020(5) 0.004(5) 0.012(5) 0.017(6) N2 0.049(7) 0.044(7) 0.039(7) 0.013(5) -0.005(5) 0.006(6) N3 0.043(6) 0.048(6) 0.022(5) 0.003(5) -0.003(5) 0.009(5) N4 0.023(6) 0.070(8) 0.057(8) -0.031(7) -0.011(5) 0.009(5) N5 0.032(6) 0.049(7) 0.069(9) -0.025(6) 0.009(6) -0.001(5) N6 0.033(6) 0.038(6) 0.023(5) 0.004(4) 0.006(4) -0.002(5) N7 0.063(8) 0.059(8) 0.037(6) -0.029(6) -0.027(6) 0.031(7) N8 0.116(14) 0.071(10) 0.084(12) -0.041(9) -0.054(11) 0.016(10) N9 0.030(6) 0.059(9) 0.078(10) -0.036(7) -0.011(6) 0.000(6) N10 0.047(6) 0.041(6) 0.014(5) 0.005(4) -0.005(4) -0.014(5) N11 0.032(6) 0.030(6) 0.032(5) 0.003(4) -0.009(4) -0.008(4) N12 0.038(6) 0.038(5) 0.013(5) 0.011(4) 0.003(4) -0.015(5) O14 0.036(4) 0.028(4) 0.023(4) 0.003(3) 0.001(3) -0.008(4) Zn1 0.0413(8) 0.0374(8) 0.0245(7) -0.0027(7) -0.0003(7) 0.0087(7) Zn2 0.0479(10) 0.0515(10) 0.0409(9) -0.0163(8) -0.0192(7) 0.0176(8) Zn3 0.0362(8) 0.0413(9) 0.0545(10) -0.0211(8) 0.0134(8) -0.0083(7) Zn4 0.0406(8) 0.0354(8) 0.0240(7) 0.0043(6) -0.0005(6) -0.0053(6) Zn5 0.0318(7) 0.0314(7) 0.0202(6) -0.0004(6) -0.0005(6) -0.0010(6) C24 0.047(12) 0.069(14) 0.013(10) -0.011(10) -0.012(9) -0.006(11) C24A 0.076(17) 0.086(19) 0.025(13) -0.019(13) -0.011(13) 0.019(15) C25 0.063(12) 0.074(12) 0.036(10) -0.010(9) 0.002(10) 0.003(10) C25A 0.075(14) 0.080(14) 0.047(12) -0.006(12) -0.027(12) 0.003(13) C4 0.069(17) 0.051(16) 0.050(15) 0.042(12) 0.002(12) 0.016(13) C4A 0.021(15) 0.035(19) 0.026(17) 0.004(13) -0.002(12) -0.008(13) C27 0.053(11) 0.056(12) 0.038(11) -0.010(9) 0.010(9) -0.003(10) C27A 0.049(12) 0.056(13) 0.033(12) -0.017(11) 0.000(10) 0.001(11) C26 0.066(12) 0.077(12) 0.046(11) -0.031(10) -0.009(10) -0.005(10) C26A 0.056(13) 0.071(14) 0.033(13) -0.009(12) -0.002(12) 0.001(12) _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 C1 C2 1.52(2) . ? C1 Zn1 2.001(12) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4A 1.48(3) . ? C3 C4 1.62(3) . ? C3 Zn2 1.972(17) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C5 C6 1.51(2) . ? C5 Zn3 2.036(18) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.50(2) . ? C7 Zn4 1.975(14) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.43(3) . ? C9 N1 1.47(2) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.50(2) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 N2 1.445(18) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 N2 1.464(19) . ? C12 C13 1.47(2) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.517(17) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 N3 1.458(15) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 N1 1.319(17) . ? C15 N2 1.365(16) . ? C15 N3 1.380(15) . ? C16 N4 1.480(17) . ? C16 C17 1.51(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.52(2) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 N5 1.451(18) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 N5 1.450(18) . ? C19 C20 1.54(2) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.482(19) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 N6 1.462(15) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 N6 1.318(16) . ? C22 N5 1.358(16) . ? C22 N4 1.382(16) . ? C23 N7 1.46(2) . ? C23 C24A 1.533(10) . ? C23 C24 1.549(10) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C28 N9 1.42(2) . ? C28 C27 1.524(10) . ? C28 C27A 1.560(10) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 N9 1.32(3) . ? C29 N8 1.38(2) . ? C29 N7 1.39(2) . ? C30 N10 1.466(17) . ? C30 C31 1.54(2) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.51(2) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 N11 1.477(16) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 N11 1.445(16) . ? C33 C34 1.52(2) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.518(19) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 N12 1.451(15) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 N10 1.342(16) . ? C36 N11 1.362(15) . ? C36 N12 1.367(15) . ? N1 Zn1 2.055(12) . ? N3 Zn5 2.052(10) . ? N3 Zn2 2.143(11) . ? N4 Zn3 2.148(12) . ? N4 Zn2 2.161(13) . ? N6 Zn5 1.999(10) . ? N7 Zn2 2.080(11) . ? N7 Zn1 2.182(11) . ? N8 C25 1.450(10) . ? N8 C26A 1.460(10) . ? N8 C26 1.491(10) . ? N8 C25A 1.493(10) . ? N9 Zn3 1.981(12) . ? N10 Zn4 2.018(10) . ? N12 Zn5 1.958(10) . ? O14 Zn4 1.884(8) . ? O14 Zn5 1.953(7) . ? O14 Zn3 1.989(8) . ? O14 Zn1 2.002(9) . ? Zn1 Zn5 3.1425(18) . ? Zn2 Zn5 3.103(2) . ? Zn3 Zn4 3.141(2) . ? Zn3 Zn5 3.145(2) . ? Zn4 Zn5 3.026(2) . ? C24 C25 1.52(4) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C24A C25A 1.545(10) . ? C24A H24C 0.9900 . ? C24A H24D 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C25A H25C 0.9900 . ? C25A H25D 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C4A H4A1 0.9800 . ? C4A H4A2 0.9800 . ? C4A H4A3 0.9800 . ? C27 C26 1.547(10) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C27A C26A 1.60(5) . ? C27A H27C 0.9900 . ? C27A H27D 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C26A H26C 0.9900 . ? C26A H26D 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 Zn1 116.8(11) . . ? C2 C1 H1A 108.1 . . ? Zn1 C1 H1A 108.1 . . ? C2 C1 H1B 108.1 . . ? Zn1 C1 H1B 108.1 . . ? H1A C1 H1B 107.3 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4A C3 C4 111(2) . . ? C4A C3 Zn2 124.6(17) . . ? C4 C3 Zn2 110.9(15) . . ? C4A C3 H3A 20.9 . . ? C4 C3 H3A 109.5 . . ? Zn2 C3 H3A 109.5 . . ? C4A C3 H3B 88.4 . . ? C4 C3 H3B 109.5 . . ? Zn2 C3 H3B 109.5 . . ? H3A C3 H3B 108.0 . . ? C6 C5 Zn3 118.1(12) . . ? C6 C5 H5A 107.8 . . ? Zn3 C5 H5A 107.8 . . ? C6 C5 H5B 107.8 . . ? Zn3 C5 H5B 107.8 . . ? H5A C5 H5B 107.1 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 Zn4 115.1(10) . . ? C8 C7 H7A 108.5 . . ? Zn4 C7 H7A 108.5 . . ? C8 C7 H7B 108.5 . . ? Zn4 C7 H7B 108.5 . . ? H7A C7 H7B 107.5 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 N1 112.2(16) . . ? C10 C9 H9A 109.2 . . ? N1 C9 H9A 109.2 . . ? C10 C9 H9B 109.2 . . ? N1 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? C9 C10 C11 113.4(19) . . ? C9 C10 H10A 108.9 . . ? C11 C10 H10A 108.9 . . ? C9 C10 H10B 108.9 . . ? C11 C10 H10B 108.9 . . ? H10A C10 H10B 107.7 . . ? N2 C11 C10 110.0(12) . . ? N2 C11 H11A 109.7 . . ? C10 C11 H11A 109.7 . . ? N2 C11 H11B 109.7 . . ? C10 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? N2 C12 C13 113.9(13) . . ? N2 C12 H12A 108.8 . . ? C13 C12 H12A 108.8 . . ? N2 C12 H12B 108.8 . . ? C13 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? C12 C13 C14 106.1(12) . . ? C12 C13 H13A 110.5 . . ? C14 C13 H13A 110.5 . . ? C12 C13 H13B 110.5 . . ? C14 C13 H13B 110.5 . . ? H13A C13 H13B 108.7 . . ? N3 C14 C13 113.1(11) . . ? N3 C14 H14A 109.0 . . ? C13 C14 H14A 109.0 . . ? N3 C14 H14B 109.0 . . ? C13 C14 H14B 109.0 . . ? H14A C14 H14B 107.8 . . ? N1 C15 N2 122.4(11) . . ? N1 C15 N3 117.0(11) . . ? N2 C15 N3 120.6(11) . . ? N4 C16 C17 111.8(15) . . ? N4 C16 H16A 109.3 . . ? C17 C16 H16A 109.3 . . ? N4 C16 H16B 109.3 . . ? C17 C16 H16B 109.3 . . ? H16A C16 H16B 107.9 . . ? C16 C17 C18 106.8(16) . . ? C16 C17 H17A 110.4 . . ? C18 C17 H17A 110.4 . . ? C16 C17 H17B 110.4 . . ? C18 C17 H17B 110.4 . . ? H17A C17 H17B 108.6 . . ? N5 C18 C17 112.2(11) . . ? N5 C18 H18A 109.2 . . ? C17 C18 H18A 109.2 . . ? N5 C18 H18B 109.2 . . ? C17 C18 H18B 109.2 . . ? H18A C18 H18B 107.9 . . ? N5 C19 C20 109.0(11) . . ? N5 C19 H19A 109.9 . . ? C20 C19 H19A 109.9 . . ? N5 C19 H19B 109.9 . . ? C20 C19 H19B 109.9 . . ? H19A C19 H19B 108.3 . . ? C21 C20 C19 107.9(11) . . ? C21 C20 H20A 110.1 . . ? C19 C20 H20A 110.1 . . ? C21 C20 H20B 110.1 . . ? C19 C20 H20B 110.1 . . ? H20A C20 H20B 108.4 . . ? N6 C21 C20 112.0(11) . . ? N6 C21 H21A 109.2 . . ? C20 C21 H21A 109.2 . . ? N6 C21 H21B 109.2 . . ? C20 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? N6 C22 N5 122.9(11) . . ? N6 C22 N4 116.6(10) . . ? N5 C22 N4 120.6(11) . . ? N7 C23 C24A 122.2(18) . . ? N7 C23 C24 106.2(17) . . ? C24A C23 C24 80.5(17) . . ? N7 C23 H23A 110.5 . . ? C24A C23 H23A 120.6 . . ? C24 C23 H23A 110.5 . . ? N7 C23 H23B 110.5 . . ? C24A C23 H23B 30.0 . . ? C24 C23 H23B 110.5 . . ? H23A C23 H23B 108.7 . . ? N9 C28 C27 121.7(17) . . ? N9 C28 C27A 104.1(19) . . ? C27 C28 C27A 65.8(17) . . ? N9 C28 H28A 106.9 . . ? C27 C28 H28A 106.9 . . ? C27A C28 H28A 146.5 . . ? N9 C28 H28B 106.9 . . ? C27 C28 H28B 106.9 . . ? C27A C28 H28B 51.1 . . ? H28A C28 H28B 106.7 . . ? N9 C29 N8 122.6(17) . . ? N9 C29 N7 119.2(13) . . ? N8 C29 N7 118(2) . . ? N10 C30 C31 110.3(12) . . ? N10 C30 H30A 109.6 . . ? C31 C30 H30A 109.6 . . ? N10 C30 H30B 109.6 . . ? C31 C30 H30B 109.6 . . ? H30A C30 H30B 108.1 . . ? C32 C31 C30 106.2(12) . . ? C32 C31 H31A 110.5 . . ? C30 C31 H31A 110.5 . . ? C32 C31 H31B 110.5 . . ? C30 C31 H31B 110.5 . . ? H31A C31 H31B 108.7 . . ? N11 C32 C31 112.6(10) . . ? N11 C32 H32A 109.1 . . ? C31 C32 H32A 109.1 . . ? N11 C32 H32B 109.1 . . ? C31 C32 H32B 109.1 . . ? H32A C32 H32B 107.8 . . ? N11 C33 C34 113.5(11) . . ? N11 C33 H33A 108.9 . . ? C34 C33 H33A 108.9 . . ? N11 C33 H33B 108.9 . . ? C34 C33 H33B 108.9 . . ? H33A C33 H33B 107.7 . . ? C33 C34 C35 107.7(10) . . ? C33 C34 H34A 110.2 . . ? C35 C34 H34A 110.2 . . ? C33 C34 H34B 110.2 . . ? C35 C34 H34B 110.2 . . ? H34A C34 H34B 108.5 . . ? N12 C35 C34 110.8(11) . . ? N12 C35 H35A 109.5 . . ? C34 C35 H35A 109.5 . . ? N12 C35 H35B 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 108.1 . . ? N10 C36 N11 121.7(11) . . ? N10 C36 N12 117.7(10) . . ? N11 C36 N12 120.6(11) . . ? C15 N1 C9 117.1(12) . . ? C15 N1 Zn1 129.8(9) . . ? C9 N1 Zn1 111.3(10) . . ? C15 N2 C11 123.3(11) . . ? C15 N2 C12 122.8(12) . . ? C11 N2 C12 113.7(12) . . ? C15 N3 C14 115.1(10) . . ? C15 N3 Zn5 111.2(7) . . ? C14 N3 Zn5 108.6(7) . . ? C15 N3 Zn2 117.7(8) . . ? C14 N3 Zn2 106.9(8) . . ? Zn5 N3 Zn2 95.4(4) . . ? C22 N4 C16 115.1(11) . . ? C22 N4 Zn3 108.5(9) . . ? C16 N4 Zn3 109.9(11) . . ? C22 N4 Zn2 120.5(9) . . ? C16 N4 Zn2 101.9(11) . . ? Zn3 N4 Zn2 99.7(4) . . ? C22 N5 C19 123.8(11) . . ? C22 N5 C18 124.3(11) . . ? C19 N5 C18 111.4(11) . . ? C22 N6 C21 116.0(10) . . ? C22 N6 Zn5 124.1(8) . . ? C21 N6 Zn5 119.6(8) . . ? C29 N7 C23 114.7(14) . . ? C29 N7 Zn2 120.0(11) . . ? C23 N7 Zn2 103.5(10) . . ? C29 N7 Zn1 105.8(9) . . ? C23 N7 Zn1 108.8(10) . . ? Zn2 N7 Zn1 103.1(5) . . ? C29 N8 C25 129.8(17) . . ? C29 N8 C26A 137(2) . . ? C25 N8 C26A 71(2) . . ? C29 N8 C26 115.9(17) . . ? C25 N8 C26 105.6(16) . . ? C26A N8 C26 35(2) . . ? C29 N8 C25A 117(2) . . ? C25 N8 C25A 45.5(17) . . ? C26A N8 C25A 104(2) . . ? C26 N8 C25A 125.0(19) . . ? C29 N9 C28 115.6(13) . . ? C29 N9 Zn3 125.8(11) . . ? C28 N9 Zn3 118.1(12) . . ? C36 N10 C30 115.6(10) . . ? C36 N10 Zn4 122.7(8) . . ? C30 N10 Zn4 117.3(8) . . ? C36 N11 C33 123.6(10) . . ? C36 N11 C32 122.9(10) . . ? C33 N11 C32 113.4(10) . . ? C36 N12 C35 115.5(10) . . ? C36 N12 Zn5 117.3(8) . . ? C35 N12 Zn5 126.2(8) . . ? Zn4 O14 Zn5 104.1(4) . . ? Zn4 O14 Zn3 108.4(4) . . ? Zn5 O14 Zn3 105.8(4) . . ? Zn4 O14 Zn1 123.3(4) . . ? Zn5 O14 Zn1 105.2(4) . . ? Zn3 O14 Zn1 108.7(4) . . ? C1 Zn1 O14 122.9(5) . . ? C1 Zn1 N1 118.3(5) . . ? O14 Zn1 N1 104.2(4) . . ? C1 Zn1 N7 111.8(5) . . ? O14 Zn1 N7 99.6(4) . . ? N1 Zn1 N7 95.1(5) . . ? C1 Zn1 Zn5 152.2(4) . . ? O14 Zn1 Zn5 36.9(2) . . ? N1 Zn1 Zn5 68.6(3) . . ? N7 Zn1 Zn5 93.4(3) . . ? C3 Zn2 N7 115.8(7) . . ? C3 Zn2 N3 113.8(8) . . ? N7 Zn2 N3 105.1(5) . . ? C3 Zn2 N4 110.7(10) . . ? N7 Zn2 N4 104.9(5) . . ? N3 Zn2 N4 105.7(4) . . ? C3 Zn2 Zn5 145.4(6) . . ? N7 Zn2 Zn5 96.7(3) . . ? N3 Zn2 Zn5 41.2(3) . . ? N4 Zn2 Zn5 69.1(3) . . ? N9 Zn3 O14 104.5(4) . . ? N9 Zn3 C5 117.3(7) . . ? O14 Zn3 C5 117.3(7) . . ? N9 Zn3 N4 100.2(5) . . ? O14 Zn3 N4 102.4(4) . . ? C5 Zn3 N4 112.8(6) . . ? N9 Zn3 Zn4 120.3(3) . . ? O14 Zn3 Zn4 34.7(2) . . ? C5 Zn3 Zn4 83.0(6) . . ? N4 Zn3 Zn4 123.8(3) . . ? N9 Zn3 Zn5 122.7(5) . . ? O14 Zn3 Zn5 36.7(2) . . ? C5 Zn3 Zn5 118.7(5) . . ? N4 Zn3 Zn5 68.4(3) . . ? Zn4 Zn3 Zn5 57.56(5) . . ? O14 Zn4 C7 128.9(5) . . ? O14 Zn4 N10 108.1(4) . . ? C7 Zn4 N10 122.7(5) . . ? O14 Zn4 Zn5 38.8(2) . . ? C7 Zn4 Zn5 167.5(4) . . ? N10 Zn4 Zn5 69.8(3) . . ? O14 Zn4 Zn3 36.9(2) . . ? C7 Zn4 Zn3 110.0(4) . . ? N10 Zn4 Zn3 112.3(3) . . ? Zn5 Zn4 Zn3 61.28(5) . . ? O14 Zn5 N12 109.3(4) . . ? O14 Zn5 N6 108.4(4) . . ? N12 Zn5 N6 114.9(4) . . ? O14 Zn5 N3 110.2(4) . . ? N12 Zn5 N3 111.8(4) . . ? N6 Zn5 N3 102.0(4) . . ? O14 Zn5 Zn4 37.1(2) . . ? N12 Zn5 Zn4 77.5(3) . . ? N6 Zn5 Zn4 106.5(3) . . ? N3 Zn5 Zn4 142.5(3) . . ? O14 Zn5 Zn2 81.9(2) . . ? N12 Zn5 Zn2 154.9(3) . . ? N6 Zn5 Zn2 80.6(3) . . ? N3 Zn5 Zn2 43.4(3) . . ? Zn4 Zn5 Zn2 118.55(6) . . ? O14 Zn5 Zn1 37.9(3) . . ? N12 Zn5 Zn1 110.2(3) . . ? N6 Zn5 Zn1 131.8(3) . . ? N3 Zn5 Zn1 75.5(3) . . ? Zn4 Zn5 Zn1 67.34(4) . . ? Zn2 Zn5 Zn1 64.63(5) . . ? O14 Zn5 Zn3 37.5(2) . . ? N12 Zn5 Zn3 138.0(3) . . ? N6 Zn5 Zn3 73.2(3) . . ? N3 Zn5 Zn3 105.9(3) . . ? Zn4 Zn5 Zn3 61.15(5) . . ? Zn2 Zn5 Zn3 63.59(5) . . ? Zn1 Zn5 Zn3 62.08(5) . . ? C25 C24 C23 123(2) . . ? C25 C24 H24A 106.6 . . ? C23 C24 H24A 106.7 . . ? C25 C24 H24B 106.7 . . ? C23 C24 H24B 106.7 . . ? H24A C24 H24B 106.6 . . ? C23 C24A C25A 88(2) . . ? C23 C24A H24C 114.0 . . ? C25A C24A H24C 114.0 . . ? C23 C24A H24D 114.0 . . ? C25A C24A H24D 114.0 . . ? H24C C24A H24D 111.2 . . ? N8 C25 C24 98.0(18) . . ? N8 C25 H25A 112.2 . . ? C24 C25 H25A 112.2 . . ? N8 C25 H25B 112.2 . . ? C24 C25 H25B 112.2 . . ? H25A C25 H25B 109.8 . . ? N8 C25A C24A 127(2) . . ? N8 C25A H25C 105.7 . . ? C24A C25A H25C 105.7 . . ? N8 C25A H25D 105.6 . . ? C24A C25A H25D 105.7 . . ? H25C C25A H25D 106.1 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C4A H4A1 109.5 . . ? C3 C4A H4A2 109.5 . . ? H4A1 C4A H4A2 109.5 . . ? C3 C4A H4A3 109.5 . . ? H4A1 C4A H4A3 109.5 . . ? H4A2 C4A H4A3 109.5 . . ? C28 C27 C26 92.9(15) . . ? C28 C27 H27A 113.1 . . ? C26 C27 H27A 113.1 . . ? C28 C27 H27B 113.1 . . ? C26 C27 H27B 113.1 . . ? H27A C27 H27B 110.5 . . ? C28 C27A C26A 133(3) . . ? C28 C27A H27C 104.0 . . ? C26A C27A H27C 104.0 . . ? C28 C27A H27D 104.0 . . ? C26A C27A H27D 104.1 . . ? H27C C27A H27D 105.5 . . ? N8 C26 C27 119.4(17) . . ? N8 C26 H26A 107.5 . . ? C27 C26 H26A 107.5 . . ? N8 C26 H26B 107.5 . . ? C27 C26 H26B 107.5 . . ? H26A C26 H26B 107.0 . . ? N8 C26A C27A 86(2) . . ? N8 C26A H26C 114.3 . . ? C27A C26A H26C 114.3 . . ? N8 C26A H26D 114.3 . . ? C27A C26A H26D 114.3 . . ? H26C C26A H26D 111.5 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 24.10 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.889 _refine_diff_density_min -0.772 _refine_diff_density_rms 0.149 # Attachment '- CCDC-843486.txt' # 3. data comp 2 data_shelxl_2 _database_code_depnum_ccdc_archive 'CCDC 843486' #TrackingRef '- CCDC-843486.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H74 Cl2 N12 O4 Zn4' _chemical_formula_weight 1119.57 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' O O 0.0106 0.0060 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3691(2) _cell_length_b 10.1339(4) _cell_length_c 13.1572(5) _cell_angle_alpha 94.3290(10) _cell_angle_beta 105.682(2) _cell_angle_gamma 95.588(2) _cell_volume 1190.21(7) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4751 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description rectangular _exptl_crystal_colour yellow _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.34 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.562 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 584 _exptl_absorpt_coefficient_mu 2.157 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device '\k-geometry diffractometr' _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method 'area detector \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9435 _diffrn_reflns_av_R_equivalents 0.0240 _diffrn_reflns_av_sigmaI/netI 0.0331 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 27.52 _reflns_number_total 5337 _reflns_number_gt 4688 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'Denzo & Scalepak (Otwinowski, Minor, 1997)' _computing_data_reduction 'Denzo & Scalepak (Otwinowski, Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; DIAMOND v2.1 (Brandenburg, 1999) Ortep-3 for Windows, L.J.Farrugia (1997) J.Appl.Cryst. 30, 565, ORTEP III (Burnett, Johnson, 1996) ; _computing_publication_material ; SHELXL-97 (Sheldrick, 1997), ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0143P)^2^+3.3783P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5337 _refine_ls_number_parameters 281 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0453 _refine_ls_R_factor_gt 0.0376 _refine_ls_wR_factor_ref 0.0837 _refine_ls_wR_factor_gt 0.0794 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.000 _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 C1 C -0.2489(3) 0.3946(3) 0.5308(2) 0.0213(6) Uani 1 1 d . . . H1A H -0.2631 0.2984 0.5393 0.026 Uiso 1 1 calc R . . H1B H -0.2996 0.4066 0.4562 0.026 Uiso 1 1 calc R . . C2 C -0.3188(3) 0.4713(3) 0.6039(2) 0.0254(6) Uani 1 1 d . . . H2A H -0.2710 0.4572 0.6776 0.038 Uiso 1 1 calc R . . H2B H -0.4258 0.4398 0.5860 0.038 Uiso 1 1 calc R . . H2C H -0.3050 0.5665 0.5955 0.038 Uiso 1 1 calc R . . C3 C 0.3654(3) 0.4762(3) 0.7711(2) 0.0255(6) Uani 1 1 d . . . H3A H 0.3310 0.5478 0.8107 0.031 Uiso 1 1 calc R . . H3B H 0.4472 0.5166 0.7447 0.031 Uiso 1 1 calc R . . C4 C 0.4216(3) 0.3719(3) 0.8438(2) 0.0286(7) Uani 1 1 d . . . H4A H 0.3387 0.3269 0.8666 0.034 Uiso 1 1 calc R . . H4B H 0.4998 0.4142 0.9078 0.034 Uiso 1 1 calc R . . C5 C 0.4853(3) 0.2718(3) 0.7819(2) 0.0247(6) Uani 1 1 d . . . H5A H 0.5910 0.3039 0.7887 0.030 Uiso 1 1 calc R . . H5B H 0.4823 0.1855 0.8124 0.030 Uiso 1 1 calc R . . C6 C 0.4555(3) 0.1497(3) 0.6094(2) 0.0229(6) Uani 1 1 d . . . H6A H 0.4342 0.0616 0.6334 0.027 Uiso 1 1 calc R . . H6B H 0.5650 0.1696 0.6232 0.027 Uiso 1 1 calc R . . C7 C 0.3812(4) 0.1452(3) 0.4915(2) 0.0276(7) Uani 1 1 d . . . H7A H 0.4007 0.0638 0.4536 0.033 Uiso 1 1 calc R . . H7B H 0.4216 0.2239 0.4632 0.033 Uiso 1 1 calc R . . C8 C 0.2144(3) 0.1449(3) 0.4750(2) 0.0253(6) Uani 1 1 d . . . H8A H 0.1636 0.1414 0.3982 0.030 Uiso 1 1 calc R . . H8B H 0.1744 0.0646 0.5016 0.030 Uiso 1 1 calc R . . C9 C 0.2745(3) 0.3081(3) 0.6270(2) 0.0175(5) Uani 1 1 d . . . C10 C 0.0403(3) 0.5759(3) 0.9011(2) 0.0252(6) Uani 1 1 d . . . H10A H 0.0305 0.4799 0.9111 0.030 Uiso 1 1 calc R . . H10B H -0.0494 0.6127 0.9116 0.030 Uiso 1 1 calc R . . C11 C 0.1777(4) 0.6468(4) 0.9822(2) 0.0341(8) Uani 1 1 d . . . H11A H 0.1711 0.6344 1.0548 0.041 Uiso 1 1 calc R . . H11B H 0.2680 0.6102 0.9728 0.041 Uiso 1 1 calc R . . C12 C 0.1867(4) 0.7913(4) 0.9667(2) 0.0358(8) Uani 1 1 d . . . H12A H 0.1107 0.8319 0.9940 0.043 Uiso 1 1 calc R . . H12B H 0.2863 0.8364 1.0079 0.043 Uiso 1 1 calc R . . C13 C 0.1957(4) 0.9512(3) 0.8377(3) 0.0323(7) Uani 1 1 d . . . H13A H 0.3037 0.9799 0.8697 0.039 Uiso 1 1 calc R . . H13B H 0.1403 1.0073 0.8746 0.039 Uiso 1 1 calc R . . C14 C 0.1549(4) 0.9734(3) 0.7219(3) 0.0333(7) Uani 1 1 d . . . H14A H 0.2131 1.0558 0.7117 0.040 Uiso 1 1 calc R . . H14B H 0.0473 0.9832 0.6963 0.040 Uiso 1 1 calc R . . C15 C 0.1900(4) 0.8538(3) 0.6607(3) 0.0278(6) Uani 1 1 d . . . H15A H 0.1665 0.8670 0.5845 0.033 Uiso 1 1 calc R . . H15B H 0.2980 0.8455 0.6864 0.033 Uiso 1 1 calc R . . C16 C 0.1035(3) 0.7109(3) 0.7738(2) 0.0203(6) Uani 1 1 d . . . C17 C 0.4337(4) 0.1735(3) 1.0838(3) 0.0313(7) Uani 1 1 d . . . H17A H 0.4377 0.1535 1.0099 0.038 Uiso 1 1 calc R . . H17B H 0.5270 0.2298 1.1244 0.038 Uiso 1 1 calc R . . C18 C 0.2995(4) 0.2448(4) 1.0855(3) 0.0382(8) Uani 1 1 d . . . H18A H 0.3298 0.3407 1.1102 0.046 Uiso 1 1 calc R . . H18B H 0.2266 0.2353 1.0144 0.046 Uiso 1 1 calc R . . C19 C 0.2355(8) 0.1745(8) 1.1631(6) 0.127(4) Uani 1 1 d . . . H19A H 0.2381 0.2382 1.2247 0.152 Uiso 1 1 calc R . . H19B H 0.1304 0.1370 1.1286 0.152 Uiso 1 1 calc R . . C20 C 0.3220(5) 0.0715(4) 1.1970(3) 0.0489(10) Uani 1 1 d . . . H20A H 0.2557 -0.0121 1.1932 0.059 Uiso 1 1 calc R . . H20B H 0.3826 0.0951 1.2717 0.059 Uiso 1 1 calc R . . O1 O -0.0914(2) 0.43921(19) 0.55330(14) 0.0167(4) Uani 1 1 d . . . O2 O 0.4170(3) 0.0527(2) 1.1313(2) 0.0365(5) Uani 1 1 d . . . N1 N 0.2416(2) 0.4133(2) 0.68136(18) 0.0182(5) Uani 1 1 d . . . N2 N 0.4013(3) 0.2517(2) 0.66922(18) 0.0198(5) Uani 1 1 d . . . N3 N 0.1833(3) 0.2643(2) 0.53088(18) 0.0188(5) Uani 1 1 d . . . N4 N 0.0489(3) 0.5915(2) 0.79286(18) 0.0206(5) Uani 1 1 d . . . N5 N 0.1624(3) 0.8122(3) 0.8546(2) 0.0275(6) Uani 1 1 d . . . N6 N 0.1032(3) 0.7313(2) 0.67402(19) 0.0208(5) Uani 1 1 d . . . Zn1 Zn 0.04094(3) 0.42361(3) 0.70187(2) 0.01798(9) Uani 1 1 d . . . Zn2 Zn 0.02843(3) 0.36594(3) 0.45649(2) 0.01605(8) Uani 1 1 d . . . Cl1 Cl -0.06427(9) 0.24502(8) 0.75992(6) 0.03014(17) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0163(13) 0.0266(15) 0.0209(14) 0.0038(11) 0.0057(10) 0.0006(11) C2 0.0207(14) 0.0311(16) 0.0287(16) 0.0079(13) 0.0118(12) 0.0065(12) C3 0.0213(14) 0.0283(16) 0.0232(15) -0.0052(12) 0.0022(11) 0.0026(12) C4 0.0238(15) 0.0410(19) 0.0189(14) -0.0006(13) 0.0013(11) 0.0092(13) C5 0.0212(14) 0.0340(17) 0.0180(14) 0.0066(12) 0.0015(11) 0.0082(12) C6 0.0243(14) 0.0248(15) 0.0215(14) 0.0048(11) 0.0060(11) 0.0116(11) C7 0.0333(17) 0.0332(17) 0.0203(14) 0.0029(12) 0.0091(12) 0.0186(13) C8 0.0312(16) 0.0241(15) 0.0181(14) -0.0022(11) 0.0008(11) 0.0129(12) C9 0.0191(13) 0.0181(13) 0.0175(13) 0.0054(10) 0.0072(10) 0.0035(10) C10 0.0301(16) 0.0348(17) 0.0128(13) 0.0034(12) 0.0080(11) 0.0077(13) C11 0.0294(17) 0.057(2) 0.0135(14) 0.0013(14) 0.0030(12) 0.0058(15) C12 0.0318(17) 0.053(2) 0.0182(15) -0.0106(14) 0.0060(13) -0.0047(15) C13 0.0308(17) 0.0278(17) 0.0338(18) -0.0120(14) 0.0080(14) -0.0031(13) C14 0.0368(18) 0.0213(16) 0.0408(19) -0.0037(14) 0.0134(15) -0.0034(13) C15 0.0314(16) 0.0215(15) 0.0285(16) -0.0014(12) 0.0085(13) -0.0043(12) C16 0.0158(13) 0.0267(15) 0.0164(13) -0.0030(11) 0.0013(10) 0.0063(11) C17 0.0279(16) 0.0296(17) 0.0348(18) 0.0010(14) 0.0078(13) 0.0003(13) C18 0.041(2) 0.037(2) 0.041(2) 0.0114(16) 0.0163(16) 0.0100(16) C19 0.143(6) 0.173(7) 0.159(6) 0.141(6) 0.131(6) 0.134(6) C20 0.073(3) 0.045(2) 0.040(2) 0.0111(18) 0.030(2) 0.018(2) O1 0.0145(9) 0.0204(10) 0.0161(9) 0.0044(7) 0.0047(7) 0.0033(7) O2 0.0359(13) 0.0273(12) 0.0483(15) 0.0046(11) 0.0147(11) 0.0058(10) N1 0.0159(11) 0.0221(12) 0.0148(11) -0.0004(9) 0.0012(9) 0.0049(9) N2 0.0198(11) 0.0245(12) 0.0163(11) 0.0038(9) 0.0049(9) 0.0082(9) N3 0.0211(12) 0.0213(12) 0.0145(11) 0.0004(9) 0.0042(9) 0.0078(9) N4 0.0244(12) 0.0252(13) 0.0133(11) 0.0030(9) 0.0057(9) 0.0068(10) N5 0.0259(13) 0.0338(15) 0.0197(12) -0.0058(11) 0.0051(10) -0.0004(11) N6 0.0228(12) 0.0205(12) 0.0175(11) 0.0008(9) 0.0044(9) 0.0005(9) Zn1 0.02004(17) 0.02169(17) 0.01406(16) 0.00457(12) 0.00581(12) 0.00646(12) Zn2 0.01772(16) 0.01709(16) 0.01347(15) 0.00210(11) 0.00373(12) 0.00425(11) Cl1 0.0383(4) 0.0258(4) 0.0328(4) 0.0114(3) 0.0174(3) 0.0072(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 O1 1.443(3) . ? C1 C2 1.512(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 N1 1.465(3) . ? C3 C4 1.517(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.519(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 N2 1.467(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 N2 1.463(4) . ? C6 C7 1.514(4) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.518(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 N3 1.463(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 N3 1.336(3) . ? C9 N1 1.346(3) . ? C9 N2 1.367(3) . ? C10 N4 1.467(3) . ? C10 C11 1.508(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.491(5) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 N5 1.464(4) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 N5 1.459(4) . ? C13 C14 1.507(5) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.516(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 N6 1.465(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 N4 1.336(4) . ? C16 N6 1.344(4) . ? C16 N5 1.377(4) . ? C17 O2 1.429(4) . ? C17 C18 1.514(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.505(6) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.409(6) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 O2 1.414(4) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? O1 Zn2 2.0289(19) 2_566 ? O1 Zn1 2.0389(18) . ? O1 Zn2 2.0557(18) . ? N1 Zn1 1.981(2) . ? N3 Zn2 1.949(2) . ? N4 Zn1 1.988(2) . ? N6 Zn2 1.950(2) 2_566 ? Zn1 Cl1 2.2580(8) . ? Zn1 Zn2 3.0856(4) 2_566 ? Zn2 N6 1.950(2) 2_566 ? Zn2 O1 2.0289(19) 2_566 ? Zn2 Zn2 3.0200(6) 2_566 ? Zn2 Zn1 3.0856(4) 2_566 ? 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 O1 C1 C2 111.4(2) . . ? O1 C1 H1A 109.4 . . ? C2 C1 H1A 109.4 . . ? O1 C1 H1B 109.4 . . ? C2 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C3 C4 109.3(3) . . ? N1 C3 H3A 109.8 . . ? C4 C3 H3A 109.8 . . ? N1 C3 H3B 109.8 . . ? C4 C3 H3B 109.8 . . ? H3A C3 H3B 108.3 . . ? C3 C4 C5 107.4(2) . . ? C3 C4 H4A 110.2 . . ? C5 C4 H4A 110.2 . . ? C3 C4 H4B 110.2 . . ? C5 C4 H4B 110.2 . . ? H4A C4 H4B 108.5 . . ? N2 C5 C4 111.6(2) . . ? N2 C5 H5A 109.3 . . ? C4 C5 H5A 109.3 . . ? N2 C5 H5B 109.3 . . ? C4 C5 H5B 109.3 . . ? H5A C5 H5B 108.0 . . ? N2 C6 C7 110.9(2) . . ? N2 C6 H6A 109.5 . . ? C7 C6 H6A 109.5 . . ? N2 C6 H6B 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? C6 C7 C8 108.3(2) . . ? C6 C7 H7A 110.0 . . ? C8 C7 H7A 110.0 . . ? C6 C7 H7B 110.0 . . ? C8 C7 H7B 110.0 . . ? H7A C7 H7B 108.4 . . ? N3 C8 C7 110.8(3) . . ? N3 C8 H8A 109.5 . . ? C7 C8 H8A 109.5 . . ? N3 C8 H8B 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? N3 C9 N1 118.3(2) . . ? N3 C9 N2 121.8(2) . . ? N1 C9 N2 119.9(2) . . ? N4 C10 C11 110.9(3) . . ? N4 C10 H10A 109.5 . . ? C11 C10 H10A 109.5 . . ? N4 C10 H10B 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 108.0 . . ? C12 C11 C10 108.0(3) . . ? C12 C11 H11A 110.1 . . ? C10 C11 H11A 110.1 . . ? C12 C11 H11B 110.1 . . ? C10 C11 H11B 110.1 . . ? H11A C11 H11B 108.4 . . ? N5 C12 C11 111.8(3) . . ? N5 C12 H12A 109.3 . . ? C11 C12 H12A 109.3 . . ? N5 C12 H12B 109.3 . . ? C11 C12 H12B 109.3 . . ? H12A C12 H12B 107.9 . . ? N5 C13 C14 112.8(3) . . ? N5 C13 H13A 109.0 . . ? C14 C13 H13A 109.0 . . ? N5 C13 H13B 109.0 . . ? C14 C13 H13B 109.0 . . ? H13A C13 H13B 107.8 . . ? C13 C14 C15 107.9(3) . . ? C13 C14 H14A 110.1 . . ? C15 C14 H14A 110.1 . . ? C13 C14 H14B 110.1 . . ? C15 C14 H14B 110.1 . . ? H14A C14 H14B 108.4 . . ? N6 C15 C14 110.8(3) . . ? N6 C15 H15A 109.5 . . ? C14 C15 H15A 109.5 . . ? N6 C15 H15B 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 108.1 . . ? N4 C16 N6 119.1(2) . . ? N4 C16 N5 121.3(3) . . ? N6 C16 N5 119.6(3) . . ? O2 C17 C18 106.9(3) . . ? O2 C17 H17A 110.3 . . ? C18 C17 H17A 110.3 . . ? O2 C17 H17B 110.3 . . ? C18 C17 H17B 110.3 . . ? H17A C17 H17B 108.6 . . ? C19 C18 C17 103.0(3) . . ? C19 C18 H18A 111.2 . . ? C17 C18 H18A 111.2 . . ? C19 C18 H18B 111.2 . . ? C17 C18 H18B 111.2 . . ? H18A C18 H18B 109.1 . . ? C20 C19 C18 108.2(4) . . ? C20 C19 H19A 110.1 . . ? C18 C19 H19A 110.1 . . ? C20 C19 H19B 110.1 . . ? C18 C19 H19B 110.1 . . ? H19A C19 H19B 108.4 . . ? C19 C20 O2 109.3(3) . . ? C19 C20 H20A 109.8 . . ? O2 C20 H20A 109.8 . . ? C19 C20 H20B 109.8 . . ? O2 C20 H20B 109.8 . . ? H20A C20 H20B 108.3 . . ? C1 O1 Zn2 118.09(16) . 2_566 ? C1 O1 Zn1 117.59(16) . . ? Zn2 O1 Zn1 98.67(8) 2_566 . ? C1 O1 Zn2 119.90(16) . . ? Zn2 O1 Zn2 95.35(8) 2_566 . ? Zn1 O1 Zn2 103.05(8) . . ? C20 O2 C17 107.3(3) . . ? C9 N1 C3 114.2(2) . . ? C9 N1 Zn1 122.71(19) . . ? C3 N1 Zn1 114.36(18) . . ? C9 N2 C6 123.0(2) . . ? C9 N2 C5 124.0(2) . . ? C6 N2 C5 112.4(2) . . ? C9 N3 C8 118.0(2) . . ? C9 N3 Zn2 122.23(19) . . ? C8 N3 Zn2 119.25(18) . . ? C16 N4 C10 117.6(2) . . ? C16 N4 Zn1 123.52(19) . . ? C10 N4 Zn1 115.88(19) . . ? C16 N5 C13 123.9(3) . . ? C16 N5 C12 122.4(3) . . ? C13 N5 C12 113.5(3) . . ? C16 N6 C15 116.6(2) . . ? C16 N6 Zn2 126.8(2) . 2_566 ? C15 N6 Zn2 115.56(19) . 2_566 ? N1 Zn1 N4 108.19(10) . . ? N1 Zn1 O1 103.89(8) . . ? N4 Zn1 O1 108.45(9) . . ? N1 Zn1 Cl1 117.12(7) . . ? N4 Zn1 Cl1 112.16(7) . . ? O1 Zn1 Cl1 106.42(6) . . ? N1 Zn1 Zn2 92.26(7) . 2_566 ? N4 Zn1 Zn2 75.80(7) . 2_566 ? O1 Zn1 Zn2 40.54(5) . 2_566 ? Cl1 Zn1 Zn2 142.79(3) . 2_566 ? N3 Zn2 N6 113.26(10) . 2_566 ? N3 Zn2 O1 116.84(9) . 2_566 ? N6 Zn2 O1 115.15(9) 2_566 2_566 ? N3 Zn2 O1 112.32(8) . . ? N6 Zn2 O1 111.33(9) 2_566 . ? O1 Zn2 O1 84.65(8) 2_566 . ? N3 Zn2 Zn2 124.18(7) . 2_566 ? N6 Zn2 Zn2 122.21(7) 2_566 2_566 ? O1 Zn2 Zn2 42.67(5) 2_566 2_566 ? O1 Zn2 Zn2 41.98(5) . 2_566 ? N3 Zn2 Zn1 144.17(7) . 2_566 ? N6 Zn2 Zn1 74.62(7) 2_566 2_566 ? O1 Zn2 Zn1 40.79(5) 2_566 2_566 ? O1 Zn2 Zn1 95.04(5) . 2_566 ? Zn2 Zn2 Zn1 63.330(12) 2_566 2_566 ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.983 _refine_diff_density_min -0.908 _refine_diff_density_rms 0.089