# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'R. E. Mulvey' _publ_contact_author_email R.E.MULVEY@STRATH.AC.UK _publ_section_title ; Potassium-mediated zincation of ferrocene and ruthenocene: potassium, the architect behind supramolecular structural variations ; loop_ _publ_author_name 'R. E. Mulvey' 'William Clegg' 'Ben Conway' 'Pablo Garcia-Alvarez' 'Alan R. Kennedy' ; J.Klett ; 'Luca Russo' # Attachment 'benpaper.cif' data_rem502 _database_code_depnum_ccdc_archive 'CCDC 731814' #---------------------------------------------------------------------- #----------------COMPOUND 1 ------------------------------------------ #---------------------------------------------------------------------- _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H47 K N4 Zn' _chemical_formula_sum 'C20 H47 K N4 Zn' _chemical_formula_weight 448.09 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' K K 0.2009 0.2494 '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 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 24.7840(7) _cell_length_b 8.4806(2) _cell_length_c 48.933(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.929(3) _cell_angle_gamma 90.00 _cell_volume 10260.7(6) _cell_formula_units_Z 16 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7571 _cell_measurement_theta_min 2.88 _cell_measurement_theta_max 28.56 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.160 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3904 _exptl_absorpt_coefficient_mu 1.130 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.560 _exptl_absorpt_correction_T_max 0.840 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET) (compiled Apr 21 2008,18:23:10) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube with Enhance optics' _diffrn_radiation_monochromator 'mirror optics' _diffrn_measurement_device_type 'Oxford Diffraction Gemini A Ultra diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3968 _diffrn_reflns_number 48234 _diffrn_reflns_av_R_equivalents 0.0786 _diffrn_reflns_av_sigmaI/netI 0.1877 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -57 _diffrn_reflns_limit_l_max 58 _diffrn_reflns_theta_min 2.89 _diffrn_reflns_theta_max 25.00 _reflns_number_total 17948 _reflns_number_gt 7814 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.31 (release 08-01-2009 CrysAlis171 .NET) (compiled Jan 8 2009,16:24:04) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.31 (release 08-01-2009 CrysAlis171 .NET) (compiled Jan 8 2009,16:24:04) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.31 (release 08-01-2009 CrysAlis171 .NET) (compiled Jan 8 2009,16:24:04) ; _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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. Analysis of the data indicates probable twinning, and several possible twin laws were identified. The best results were obtained with the twin law (0 0 -0.5, 0 -1 0, -2 0 0), representing two orientations of the structure in which the a and c axes (in approximately 1:2 length ratio) are exchanged; the minor component contributes 9.1(3)% to the diffraction pattern. It is clear, however, that this is not a complete description of the twinning, which is actually more complex. Two CH2CH2 segments were found to be disordered, both in approximately 2:1 ratio. The disorder was resolved for these atoms, but not for methyl or other carbon atoms attached to the adjacent N atoms. To aid the disorder refinement, soft restraints (similarity of N-C and C-C distances, similarity and 'rigid bond' restraints on anisotropic U values) were applied to these atoms. ; _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^)+(0.0867P)^2^+17.0884P] 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 17948 _refine_ls_number_parameters 976 _refine_ls_number_restraints 126 _refine_ls_R_factor_all 0.1879 _refine_ls_R_factor_gt 0.0959 _refine_ls_wR_factor_ref 0.2332 _refine_ls_wR_factor_gt 0.2119 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.006 _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 0.68755(5) 0.28931(14) 0.02420(2) 0.0289(3) Uani 1 1 d . . . Zn2 Zn 0.45146(4) 0.44945(13) 0.15623(2) 0.0317(3) Uani 1 1 d . . . Zn3 Zn 0.18559(5) 0.30111(15) 0.27195(2) 0.0316(3) Uani 1 1 d . . . Zn4 Zn 0.04523(4) 0.92613(13) 0.09140(2) 0.0343(3) Uani 1 1 d . . . K1 K 0.79756(8) 0.5235(2) 0.02287(4) 0.0286(5) Uani 1 1 d . A . K2 K 0.45551(10) 0.2225(2) 0.09941(4) 0.0307(5) Uani 1 1 d . B . K3 K 0.29954(8) 0.5279(2) 0.27104(4) 0.0306(5) Uani 1 1 d . . . K4 K 0.04328(9) 0.7081(3) 0.14971(4) 0.0361(6) Uani 1 1 d . . . N1 N 0.7193(3) 0.4196(8) 0.05606(14) 0.0235(17) Uani 1 1 d . A . N2 N 0.9051(3) 0.3993(11) 0.0283(3) 0.061(3) Uani 1 1 d DU . . N3 N 0.8827(4) 0.7423(9) 0.0277(3) 0.053(3) Uani 1 1 d DU . . N4 N 0.7872(4) 0.7913(10) -0.01139(18) 0.038(2) Uani 1 1 d . . . N5 N 0.3885(3) 0.3282(8) 0.13824(14) 0.0212(17) Uani 1 1 d . B . N6 N 0.5239(3) -0.0509(9) 0.10573(15) 0.037(2) Uani 1 1 d DU . . N7 N 0.4545(4) 0.0128(9) 0.05459(18) 0.046(2) Uani 1 1 d DU . . N8 N 0.4419(3) 0.3572(9) 0.04449(15) 0.0303(19) Uani 1 1 d . . . N9 N 0.2202(3) 0.4237(8) 0.30406(14) 0.0254(18) Uani 1 1 d . . . N10 N 0.4062(3) 0.3903(10) 0.28120(19) 0.041(2) Uani 1 1 d . . . N11 N 0.3901(4) 0.7354(8) 0.27204(18) 0.030(2) Uani 1 1 d . . . N12 N 0.2901(3) 0.8076(10) 0.23798(16) 0.036(2) Uani 1 1 d . . . N13 N 0.1083(3) 0.8051(9) 0.10945(16) 0.0296(19) Uani 1 1 d . . . N14 N 0.0615(4) 0.8535(10) 0.20278(16) 0.040(2) Uani 1 1 d . . . N15 N 0.0435(4) 0.5104(10) 0.19643(17) 0.043(2) Uani 1 1 d . . . N16 N -0.0241(3) 0.4317(9) 0.14579(17) 0.038(2) Uani 1 1 d . . . C1 C 0.6255(4) 0.1420(13) 0.0291(2) 0.048(3) Uani 1 1 d . . . H1A H 0.6201 0.1309 0.0486 0.072 Uiso 1 1 calc R . . H1B H 0.6335 0.0386 0.0214 0.072 Uiso 1 1 calc R . . H1C H 0.5926 0.1847 0.0196 0.072 Uiso 1 1 calc R . . C2 C 0.7226(4) 0.3184(11) -0.01181(18) 0.031(2) Uani 1 1 d . . . H2A H 0.7612 0.2925 -0.0092 0.046 Uiso 1 1 calc R . . H2B H 0.7185 0.4282 -0.0178 0.046 Uiso 1 1 calc R . . H2C H 0.7052 0.2485 -0.0257 0.046 Uiso 1 1 calc R . . C3 C 0.7449(4) 0.3208(11) 0.07804(19) 0.030(2) Uani 1 1 d . . . C4 C 0.7947(4) 0.3997(13) 0.0935(2) 0.040(3) Uani 1 1 d . A . H4A H 0.8177 0.4473 0.0802 0.059 Uiso 1 1 calc R . . H4B H 0.8154 0.3199 0.1043 0.059 Uiso 1 1 calc R . . H4C H 0.7824 0.4815 0.1058 0.059 Uiso 1 1 calc R . . C5 C 0.7664(4) 0.1735(11) 0.0648(2) 0.041(3) Uani 1 1 d . A . H5A H 0.7362 0.1144 0.0558 0.062 Uiso 1 1 calc R . . H5B H 0.7850 0.1074 0.0790 0.062 Uiso 1 1 calc R . . H5C H 0.7918 0.2037 0.0513 0.062 Uiso 1 1 calc R . . C6 C 0.7047(4) 0.2703(11) 0.0994(2) 0.034(3) Uani 1 1 d . A . H6A H 0.6788 0.1927 0.0910 0.041 Uiso 1 1 calc R . . H6B H 0.7250 0.2182 0.1151 0.041 Uiso 1 1 calc R . . C7 C 0.6741(4) 0.4069(13) 0.1098(2) 0.044(3) Uani 1 1 d . . . H7A H 0.6993 0.4796 0.1201 0.052 Uiso 1 1 calc R A . H7B H 0.6473 0.3689 0.1224 0.052 Uiso 1 1 calc R . . C8 C 0.6455(4) 0.4926(12) 0.0861(2) 0.037(3) Uani 1 1 d . A . H8A H 0.6265 0.5854 0.0932 0.044 Uiso 1 1 calc R . . H8B H 0.6179 0.4220 0.0771 0.044 Uiso 1 1 calc R . . C9 C 0.6838(4) 0.5471(11) 0.06516(18) 0.030(2) Uani 1 1 d . . . C10 C 0.6495(4) 0.5981(12) 0.0394(2) 0.036(3) Uani 1 1 d . A . H10A H 0.6723 0.6021 0.0238 0.054 Uiso 1 1 calc R . . H10B H 0.6342 0.7027 0.0423 0.054 Uiso 1 1 calc R . . H10C H 0.6202 0.5220 0.0355 0.054 Uiso 1 1 calc R . . C11 C 0.7145(4) 0.6966(12) 0.0756(2) 0.043(3) Uani 1 1 d . A . H11A H 0.7354 0.6726 0.0928 0.064 Uiso 1 1 calc R . . H11B H 0.6885 0.7807 0.0787 0.064 Uiso 1 1 calc R . . H11C H 0.7390 0.7312 0.0619 0.064 Uiso 1 1 calc R . . C12 C 0.9133(6) 0.2713(18) 0.0480(3) 0.080(5) Uani 1 1 d . A . H12A H 0.9501 0.2294 0.0472 0.121 Uiso 1 1 calc R . . H12B H 0.8870 0.1874 0.0435 0.121 Uiso 1 1 calc R . . H12C H 0.9085 0.3109 0.0664 0.121 Uiso 1 1 calc R . . C13 C 0.9102(5) 0.3338(16) 0.0014(3) 0.068(4) Uani 1 1 d . A . H13A H 0.9061 0.4180 -0.0123 0.103 Uiso 1 1 calc R . . H13B H 0.8820 0.2542 -0.0024 0.103 Uiso 1 1 calc R . . H13C H 0.9459 0.2848 0.0006 0.103 Uiso 1 1 calc R . . C14 C 0.9446(7) 0.5160(17) 0.0413(5) 0.057(5) Uani 0.68(2) 1 d PDU A 1 H14A H 0.9820 0.4757 0.0410 0.069 Uiso 0.68(2) 1 calc PR A 1 H14B H 0.9367 0.5362 0.0605 0.069 Uiso 0.68(2) 1 calc PR A 1 C15 C 0.9377(5) 0.665(2) 0.0244(4) 0.053(5) Uani 0.68(2) 1 d PDU A 1 H15A H 0.9411 0.6400 0.0049 0.064 Uiso 0.68(2) 1 calc PR A 1 H15B H 0.9668 0.7407 0.0303 0.064 Uiso 0.68(2) 1 calc PR A 1 C14X C 0.9423(14) 0.536(3) 0.0229(7) 0.052(7) Uani 0.32(2) 1 d PDU A 2 H14C H 0.9802 0.5000 0.0258 0.063 Uiso 0.32(2) 1 calc PR A 2 H14D H 0.9362 0.5678 0.0035 0.063 Uiso 0.32(2) 1 calc PR A 2 C15X C 0.9347(11) 0.679(4) 0.0407(8) 0.047(8) Uani 0.32(2) 1 d PDU A 2 H15C H 0.9313 0.6496 0.0601 0.056 Uiso 0.32(2) 1 calc PR A 2 H15D H 0.9647 0.7557 0.0396 0.056 Uiso 0.32(2) 1 calc PR A 2 C16 C 0.8723(7) 0.804(2) 0.0537(3) 0.098(6) Uani 1 1 d . A . H16A H 0.9019 0.8746 0.0600 0.146 Uiso 1 1 calc R . . H16B H 0.8697 0.7171 0.0667 0.146 Uiso 1 1 calc R . . H16C H 0.8382 0.8626 0.0522 0.146 Uiso 1 1 calc R . . C17 C 0.8812(4) 0.8604(12) 0.0069(3) 0.050(3) Uani 1 1 d . A . H17A H 0.8973 0.8166 -0.0094 0.060 Uiso 1 1 calc R . . H17B H 0.9039 0.9505 0.0136 0.060 Uiso 1 1 calc R . . C18 C 0.8254(4) 0.9197(12) -0.0014(2) 0.045(3) Uani 1 1 d . A . H18A H 0.8278 0.9992 -0.0161 0.055 Uiso 1 1 calc R . . H18B H 0.8105 0.9726 0.0145 0.055 Uiso 1 1 calc R . . C19 C 0.7338(5) 0.8605(15) -0.0156(3) 0.070(4) Uani 1 1 d . A . H19A H 0.7346 0.9457 -0.0291 0.105 Uiso 1 1 calc R . . H19B H 0.7226 0.9031 0.0017 0.105 Uiso 1 1 calc R . . H19C H 0.7079 0.7796 -0.0224 0.105 Uiso 1 1 calc R . . C20 C 0.8041(6) 0.7274(13) -0.0367(2) 0.056(4) Uani 1 1 d . A . H20A H 0.7748 0.6637 -0.0454 0.085 Uiso 1 1 calc R . . H20B H 0.8361 0.6612 -0.0329 0.085 Uiso 1 1 calc R . . H20C H 0.8128 0.8139 -0.0489 0.085 Uiso 1 1 calc R . . C21 C 0.4415(5) 0.5893(16) 0.1886(2) 0.065(4) Uani 1 1 d . . . H21A H 0.4043 0.5805 0.1939 0.098 Uiso 1 1 calc R . . H21B H 0.4490 0.6989 0.1837 0.098 Uiso 1 1 calc R . . H21C H 0.4666 0.5569 0.2039 0.098 Uiso 1 1 calc R . . C22 C 0.5235(4) 0.4171(11) 0.13882(19) 0.032(2) Uani 1 1 d . . . H22A H 0.5329 0.3049 0.1393 0.048 Uiso 1 1 calc R . . H22B H 0.5520 0.4773 0.1491 0.048 Uiso 1 1 calc R . . H22C H 0.5202 0.4537 0.1198 0.048 Uiso 1 1 calc R . . C23 C 0.3469(4) 0.4295(11) 0.12500(19) 0.033(2) Uani 1 1 d . . . C24 C 0.3744(4) 0.5765(10) 0.1154(2) 0.035(2) Uani 1 1 d . B . H24A H 0.3907 0.6337 0.1313 0.052 Uiso 1 1 calc R . . H24B H 0.3476 0.6440 0.1055 0.052 Uiso 1 1 calc R . . H24C H 0.4025 0.5471 0.1033 0.052 Uiso 1 1 calc R . . C25 C 0.3165(4) 0.3540(12) 0.0990(2) 0.042(3) Uani 1 1 d . B . H25A H 0.3428 0.3200 0.0862 0.063 Uiso 1 1 calc R . . H25B H 0.2920 0.4321 0.0901 0.063 Uiso 1 1 calc R . . H25C H 0.2955 0.2627 0.1045 0.063 Uiso 1 1 calc R . . C26 C 0.3052(4) 0.4829(13) 0.1446(2) 0.044(3) Uani 1 1 d . B . H26A H 0.2761 0.5417 0.1343 0.053 Uiso 1 1 calc R . . H26B H 0.3227 0.5553 0.1584 0.053 Uiso 1 1 calc R . . C27 C 0.2804(4) 0.3425(14) 0.1595(2) 0.050(3) Uani 1 1 d . . . H27A H 0.2550 0.3813 0.1727 0.060 Uiso 1 1 calc R B . H27B H 0.2602 0.2735 0.1460 0.060 Uiso 1 1 calc R . . C28 C 0.3255(5) 0.2522(11) 0.1741(2) 0.037(3) Uani 1 1 d . B . H28A H 0.3101 0.1594 0.1830 0.044 Uiso 1 1 calc R . . H28B H 0.3426 0.3199 0.1888 0.044 Uiso 1 1 calc R . . C29 C 0.3701(4) 0.1947(12) 0.1557(2) 0.037(3) Uani 1 1 d . . . C30 C 0.3486(5) 0.0521(12) 0.1386(2) 0.051(3) Uani 1 1 d . B . H30A H 0.3161 0.0830 0.1274 0.076 Uiso 1 1 calc R . . H30B H 0.3398 -0.0338 0.1509 0.076 Uiso 1 1 calc R . . H30C H 0.3764 0.0166 0.1267 0.076 Uiso 1 1 calc R . . C31 C 0.4181(4) 0.1430(13) 0.1733(2) 0.047(3) Uani 1 1 d . B . H31A H 0.4463 0.1062 0.1617 0.071 Uiso 1 1 calc R . . H31B H 0.4078 0.0570 0.1852 0.071 Uiso 1 1 calc R . . H31C H 0.4319 0.2318 0.1845 0.071 Uiso 1 1 calc R . . C32 C 0.5177(7) -0.1342(15) 0.1312(3) 0.081(5) Uani 1 1 d . B . H32A H 0.4897 -0.2152 0.1283 0.121 Uiso 1 1 calc R . . H32B H 0.5071 -0.0595 0.1452 0.121 Uiso 1 1 calc R . . H32C H 0.5520 -0.1842 0.1374 0.121 Uiso 1 1 calc R . . C33 C 0.5787(5) 0.0084(16) 0.1054(4) 0.091(5) Uani 1 1 d . B . H33A H 0.6038 -0.0802 0.1040 0.137 Uiso 1 1 calc R . . H33B H 0.5881 0.0664 0.1224 0.137 Uiso 1 1 calc R . . H33C H 0.5814 0.0790 0.0897 0.137 Uiso 1 1 calc R . . C34 C 0.5055(7) -0.1762(16) 0.0856(3) 0.033(4) Uani 0.66(2) 1 d PDU B 1 H34A H 0.4707 -0.2207 0.0908 0.039 Uiso 0.66(2) 1 calc PR B 1 H34B H 0.5324 -0.2625 0.0861 0.039 Uiso 0.66(2) 1 calc PR B 1 C35 C 0.4982(6) -0.1113(16) 0.0566(3) 0.031(4) Uani 0.66(2) 1 d PDU B 1 H35A H 0.5327 -0.0648 0.0514 0.037 Uiso 0.66(2) 1 calc PR B 1 H35B H 0.4885 -0.1982 0.0437 0.037 Uiso 0.66(2) 1 calc PR B 1 C34X C 0.5272(11) -0.117(4) 0.0774(4) 0.034(6) Uani 0.34(2) 1 d PDU B 2 H34C H 0.5484 -0.2163 0.0784 0.040 Uiso 0.34(2) 1 calc PR B 2 H34D H 0.5460 -0.0412 0.0660 0.040 Uiso 0.34(2) 1 calc PR B 2 C35X C 0.4709(12) -0.149(2) 0.0645(7) 0.039(7) Uani 0.34(2) 1 d PDU B 2 H35C H 0.4717 -0.2253 0.0492 0.047 Uiso 0.34(2) 1 calc PR B 2 H35D H 0.4466 -0.1894 0.0782 0.047 Uiso 0.34(2) 1 calc PR B 2 C36 C 0.3984(6) -0.0372(13) 0.0548(2) 0.061(4) Uani 1 1 d . B . H36A H 0.3750 0.0557 0.0550 0.092 Uiso 1 1 calc R . . H36B H 0.3938 -0.1010 0.0712 0.092 Uiso 1 1 calc R . . H36C H 0.3887 -0.1002 0.0384 0.092 Uiso 1 1 calc R . . C37 C 0.4639(4) 0.0845(12) 0.0287(2) 0.043(3) Uani 1 1 d . B . H37A H 0.4530 0.0090 0.0139 0.051 Uiso 1 1 calc R . . H37B H 0.5031 0.1040 0.0280 0.051 Uiso 1 1 calc R . . C38 C 0.4338(5) 0.2391(10) 0.0231(2) 0.034(3) Uani 1 1 d . B . H38A H 0.4453 0.2840 0.0058 0.040 Uiso 1 1 calc R . . H38B H 0.3946 0.2160 0.0204 0.040 Uiso 1 1 calc R . . C39 C 0.4061(5) 0.4905(12) 0.0386(2) 0.048(3) Uani 1 1 d . B . H39A H 0.4162 0.5434 0.0219 0.072 Uiso 1 1 calc R . . H39B H 0.4092 0.5648 0.0540 0.072 Uiso 1 1 calc R . . H39C H 0.3686 0.4530 0.0360 0.072 Uiso 1 1 calc R . . C40 C 0.4979(4) 0.4112(12) 0.0470(2) 0.043(3) Uani 1 1 d . B . H40A H 0.5217 0.3225 0.0523 0.065 Uiso 1 1 calc R . . H40B H 0.5020 0.4939 0.0609 0.065 Uiso 1 1 calc R . . H40C H 0.5077 0.4534 0.0293 0.065 Uiso 1 1 calc R . . C41 C 0.1212(5) 0.1656(15) 0.2776(2) 0.057(3) Uani 1 1 d . . . H41A H 0.1085 0.1860 0.2958 0.086 Uiso 1 1 calc R . . H41B H 0.1312 0.0543 0.2762 0.086 Uiso 1 1 calc R . . H41C H 0.0922 0.1903 0.2636 0.086 Uiso 1 1 calc R . . C42 C 0.2214(4) 0.3308(12) 0.23612(18) 0.035(2) Uani 1 1 d . . . H42A H 0.2013 0.2712 0.2216 0.052 Uiso 1 1 calc R . . H42B H 0.2587 0.2926 0.2382 0.052 Uiso 1 1 calc R . . H42C H 0.2212 0.4430 0.2313 0.052 Uiso 1 1 calc R . . C43 C 0.2456(4) 0.3225(11) 0.32533(19) 0.029(2) Uani 1 1 d . . . C44 C 0.2641(4) 0.1757(12) 0.3122(2) 0.040(3) Uani 1 1 d . . . H44A H 0.2327 0.1156 0.3047 0.060 Uiso 1 1 calc R . . H44B H 0.2850 0.1116 0.3258 0.060 Uiso 1 1 calc R . . H44C H 0.2869 0.2032 0.2973 0.060 Uiso 1 1 calc R . . C45 C 0.2962(4) 0.3950(12) 0.3414(2) 0.035(2) Uani 1 1 d . . . H45A H 0.3224 0.4286 0.3285 0.053 Uiso 1 1 calc R . . H45B H 0.3128 0.3157 0.3539 0.053 Uiso 1 1 calc R . . H45C H 0.2851 0.4861 0.3520 0.053 Uiso 1 1 calc R . . C46 C 0.2051(5) 0.2723(12) 0.3466(2) 0.043(3) Uani 1 1 d . . . H46A H 0.1778 0.2000 0.3378 0.052 Uiso 1 1 calc R . . H46B H 0.2248 0.2143 0.3617 0.052 Uiso 1 1 calc R . . C47 C 0.1766(5) 0.4118(13) 0.3582(2) 0.047(3) Uani 1 1 d . . . H47A H 0.2031 0.4798 0.3687 0.056 Uiso 1 1 calc R . . H47B H 0.1496 0.3751 0.3708 0.056 Uiso 1 1 calc R . . C48 C 0.1486(4) 0.5052(12) 0.3346(2) 0.042(3) Uani 1 1 d . . . H48A H 0.1196 0.4393 0.3255 0.051 Uiso 1 1 calc R . . H48B H 0.1314 0.5998 0.3420 0.051 Uiso 1 1 calc R . . C49 C 0.1867(4) 0.5568(12) 0.31328(19) 0.036(2) Uani 1 1 d . . . C50 C 0.1518(4) 0.6143(13) 0.2887(2) 0.044(3) Uani 1 1 d . . . H50A H 0.1725 0.6886 0.2782 0.067 Uiso 1 1 calc R . . H50B H 0.1197 0.6672 0.2949 0.067 Uiso 1 1 calc R . . H50C H 0.1407 0.5243 0.2771 0.067 Uiso 1 1 calc R . . C51 C 0.2208(5) 0.7026(13) 0.3241(2) 0.051(3) Uani 1 1 d . . . H51A H 0.2427 0.6728 0.3408 0.077 Uiso 1 1 calc R . . H51B H 0.1964 0.7888 0.3284 0.077 Uiso 1 1 calc R . . H51C H 0.2445 0.7372 0.3101 0.077 Uiso 1 1 calc R . . C52 C 0.4128(5) 0.2548(11) 0.2990(3) 0.053(4) Uani 1 1 d . . . H52A H 0.4487 0.2088 0.2973 0.080 Uiso 1 1 calc R . . H52B H 0.3850 0.1763 0.2937 0.080 Uiso 1 1 calc R . . H52C H 0.4091 0.2874 0.3180 0.080 Uiso 1 1 calc R . . C53 C 0.4082(5) 0.3388(14) 0.2526(3) 0.060(3) Uani 1 1 d . . . H53A H 0.4009 0.4289 0.2403 0.090 Uiso 1 1 calc R . . H53B H 0.3808 0.2571 0.2486 0.090 Uiso 1 1 calc R . . H53C H 0.4441 0.2960 0.2497 0.090 Uiso 1 1 calc R . . C54 C 0.4484(4) 0.5071(12) 0.2884(3) 0.049(3) Uani 1 1 d . . . H54A H 0.4841 0.4596 0.2856 0.058 Uiso 1 1 calc R . . H54B H 0.4476 0.5328 0.3081 0.058 Uiso 1 1 calc R . . C55 C 0.4429(4) 0.6582(12) 0.2721(2) 0.043(3) Uani 1 1 d . . . H55A H 0.4708 0.7333 0.2795 0.051 Uiso 1 1 calc R . . H55B H 0.4505 0.6350 0.2529 0.051 Uiso 1 1 calc R . . C56 C 0.3820(6) 0.7952(14) 0.2996(2) 0.059(3) Uani 1 1 d . . . H56A H 0.4122 0.8645 0.3055 0.088 Uiso 1 1 calc R . . H56B H 0.3804 0.7065 0.3123 0.088 Uiso 1 1 calc R . . H56C H 0.3481 0.8547 0.2992 0.088 Uiso 1 1 calc R . . C57 C 0.3868(4) 0.8578(13) 0.2515(2) 0.045(3) Uani 1 1 d . . . H57A H 0.3995 0.8149 0.2343 0.053 Uiso 1 1 calc R . . H57B H 0.4114 0.9447 0.2576 0.053 Uiso 1 1 calc R . . C58 C 0.3325(4) 0.9214(12) 0.2460(2) 0.048(3) Uani 1 1 d . . . H58A H 0.3338 1.0011 0.2313 0.057 Uiso 1 1 calc R . . H58B H 0.3221 0.9768 0.2627 0.057 Uiso 1 1 calc R . . C59 C 0.2377(5) 0.8791(14) 0.2373(3) 0.062(3) Uani 1 1 d . . . H59A H 0.2343 0.9564 0.2224 0.093 Uiso 1 1 calc R . . H59B H 0.2332 0.9320 0.2548 0.093 Uiso 1 1 calc R . . H59C H 0.2099 0.7977 0.2343 0.093 Uiso 1 1 calc R . . C60 C 0.2980(6) 0.7431(11) 0.2113(2) 0.046(3) Uani 1 1 d . . . H60A H 0.2917 0.8254 0.1974 0.069 Uiso 1 1 calc R . . H60B H 0.2725 0.6563 0.2075 0.069 Uiso 1 1 calc R . . H60C H 0.3351 0.7036 0.2109 0.069 Uiso 1 1 calc R . . C61 C 0.0534(5) 1.0443(17) 0.0563(3) 0.077(4) Uani 1 1 d . . . H61A H 0.0789 0.9883 0.0453 0.116 Uiso 1 1 calc R . . H61B H 0.0671 1.1506 0.0605 0.116 Uiso 1 1 calc R . . H61C H 0.0181 1.0516 0.0460 0.116 Uiso 1 1 calc R . . C62 C -0.0246(4) 0.9069(14) 0.1110(2) 0.044(3) Uani 1 1 d . . . H62A H -0.0376 0.7978 0.1097 0.066 Uiso 1 1 calc R . . H62B H -0.0520 0.9774 0.1023 0.066 Uiso 1 1 calc R . . H62C H -0.0176 0.9361 0.1303 0.066 Uiso 1 1 calc R . . C63 C 0.1259(4) 0.6728(12) 0.0935(2) 0.038(3) Uani 1 1 d . . . C64 C 0.1489(5) 0.5320(14) 0.1106(3) 0.063(4) Uani 1 1 d . . . H64A H 0.1823 0.5642 0.1210 0.094 Uiso 1 1 calc R . . H64B H 0.1567 0.4447 0.0983 0.094 Uiso 1 1 calc R . . H64C H 0.1223 0.4979 0.1233 0.094 Uiso 1 1 calc R . . C65 C 0.0749(5) 0.6102(13) 0.0779(3) 0.061(4) Uani 1 1 d . . . H65A H 0.0474 0.5880 0.0908 0.092 Uiso 1 1 calc R . . H65B H 0.0835 0.5131 0.0682 0.092 Uiso 1 1 calc R . . H65C H 0.0611 0.6894 0.0646 0.092 Uiso 1 1 calc R . . C66 C 0.1668(5) 0.7210(13) 0.0727(3) 0.047(3) Uani 1 1 d . . . H66A H 0.1797 0.6252 0.0636 0.056 Uiso 1 1 calc R . . H66B H 0.1484 0.7886 0.0584 0.056 Uiso 1 1 calc R . . C67 C 0.2153(5) 0.8099(14) 0.0860(2) 0.051(3) Uani 1 1 d . . . H67A H 0.2402 0.8418 0.0720 0.061 Uiso 1 1 calc R . . H67B H 0.2354 0.7427 0.0997 0.061 Uiso 1 1 calc R . . C68 C 0.1925(4) 0.9556(14) 0.0997(2) 0.052(3) Uani 1 1 d . . . H68A H 0.1740 1.0236 0.0856 0.062 Uiso 1 1 calc R . . H68B H 0.2227 1.0168 0.1088 0.062 Uiso 1 1 calc R . . C69 C 0.1526(4) 0.9109(11) 0.1209(2) 0.035(3) Uani 1 1 d . . . C70 C 0.1833(4) 0.8433(14) 0.1472(2) 0.049(3) Uani 1 1 d . . . H70A H 0.1573 0.8001 0.1594 0.074 Uiso 1 1 calc R . . H70B H 0.2042 0.9277 0.1567 0.074 Uiso 1 1 calc R . . H70C H 0.2080 0.7596 0.1420 0.074 Uiso 1 1 calc R . . C71 C 0.1251(5) 1.0611(13) 0.1298(2) 0.053(3) Uani 1 1 d . . . H71A H 0.1079 1.1141 0.1137 0.079 Uiso 1 1 calc R . . H71B H 0.1522 1.1314 0.1389 0.079 Uiso 1 1 calc R . . H71C H 0.0977 1.0347 0.1425 0.079 Uiso 1 1 calc R . . C72 C 0.0972(5) 0.9893(13) 0.2052(2) 0.057(3) Uani 1 1 d . . . H72A H 0.0929 1.0426 0.2227 0.086 Uiso 1 1 calc R . . H72B H 0.0881 1.0625 0.1901 0.086 Uiso 1 1 calc R . . H72C H 0.1348 0.9544 0.2045 0.086 Uiso 1 1 calc R . . C73 C 0.0056(5) 0.9071(15) 0.2033(3) 0.064(4) Uani 1 1 d . . . H73A H -0.0190 0.8177 0.1998 0.096 Uiso 1 1 calc R . . H73B H -0.0017 0.9880 0.1893 0.096 Uiso 1 1 calc R . . H73C H -0.0001 0.9517 0.2214 0.096 Uiso 1 1 calc R . . C74 C 0.0751(6) 0.7437(11) 0.2241(3) 0.049(3) Uani 1 1 d . . . H74A H 0.0702 0.7955 0.2419 0.059 Uiso 1 1 calc R . . H74B H 0.1139 0.7167 0.2236 0.059 Uiso 1 1 calc R . . C75 C 0.0423(5) 0.5905(13) 0.2228(2) 0.048(3) Uani 1 1 d . . . H75A H 0.0569 0.5187 0.2375 0.057 Uiso 1 1 calc R . . H75B H 0.0043 0.6145 0.2263 0.057 Uiso 1 1 calc R . . C76 C 0.0979(5) 0.4476(14) 0.1931(2) 0.055(3) Uani 1 1 d . . . H76A H 0.1243 0.5334 0.1950 0.083 Uiso 1 1 calc R . . H76B H 0.0989 0.3998 0.1749 0.083 Uiso 1 1 calc R . . H76C H 0.1066 0.3676 0.2072 0.083 Uiso 1 1 calc R . . C77 C 0.0020(5) 0.3845(13) 0.1949(2) 0.049(3) Uani 1 1 d . . . H77A H 0.0141 0.2980 0.2074 0.059 Uiso 1 1 calc R . . H77B H -0.0320 0.4275 0.2013 0.059 Uiso 1 1 calc R . . C78 C -0.0093(5) 0.3185(12) 0.1669(2) 0.048(3) Uani 1 1 d . . . H78A H 0.0233 0.2614 0.1617 0.058 Uiso 1 1 calc R . . H78B H -0.0388 0.2404 0.1675 0.058 Uiso 1 1 calc R . . C79 C -0.0263(5) 0.3514(14) 0.1190(2) 0.065(4) Uani 1 1 d . . . H79A H 0.0085 0.3003 0.1166 0.097 Uiso 1 1 calc R . . H79B H -0.0339 0.4287 0.1044 0.097 Uiso 1 1 calc R . . H79C H -0.0550 0.2716 0.1183 0.097 Uiso 1 1 calc R . . C80 C -0.0774(4) 0.5057(14) 0.1500(3) 0.060(3) Uani 1 1 d . . . H80A H -0.1056 0.4242 0.1492 0.090 Uiso 1 1 calc R . . H80B H -0.0859 0.5837 0.1355 0.090 Uiso 1 1 calc R . . H80C H -0.0760 0.5577 0.1679 0.090 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 0.0227(6) 0.0418(7) 0.0223(6) -0.0071(5) 0.0010(5) -0.0098(6) Zn2 0.0265(6) 0.0391(7) 0.0295(6) -0.0102(5) 0.0025(5) -0.0043(5) Zn3 0.0292(7) 0.0454(7) 0.0199(6) -0.0010(6) 0.0004(5) -0.0029(6) Zn4 0.0257(6) 0.0424(7) 0.0348(7) 0.0058(6) 0.0023(5) 0.0006(5) K1 0.0252(11) 0.0272(11) 0.0334(12) 0.0072(9) 0.0015(9) -0.0061(9) K2 0.0367(14) 0.0317(12) 0.0235(12) -0.0031(10) 0.0018(10) 0.0053(10) K3 0.0274(12) 0.0278(11) 0.0366(12) 0.0049(10) 0.0019(10) -0.0006(9) K4 0.0372(14) 0.0424(13) 0.0286(13) 0.0039(11) 0.0029(11) -0.0104(12) N1 0.020(4) 0.028(4) 0.021(4) -0.001(3) -0.002(3) 0.004(3) N2 0.020(5) 0.044(5) 0.119(10) -0.031(6) -0.008(5) -0.005(4) N3 0.037(6) 0.038(6) 0.083(9) 0.019(5) -0.008(6) -0.012(4) N4 0.037(5) 0.036(5) 0.041(5) 0.001(4) -0.002(4) -0.006(4) N5 0.022(4) 0.019(4) 0.023(4) -0.001(3) 0.001(3) -0.006(3) N6 0.040(5) 0.039(5) 0.033(4) -0.003(4) -0.005(4) 0.011(4) N7 0.062(7) 0.031(5) 0.042(6) -0.013(4) -0.022(5) 0.020(4) N8 0.036(5) 0.033(5) 0.021(4) 0.003(4) -0.005(4) -0.001(4) N9 0.029(4) 0.028(4) 0.018(4) 0.000(3) -0.005(3) 0.005(4) N10 0.024(5) 0.039(5) 0.060(6) -0.008(5) -0.006(4) 0.012(4) N11 0.031(5) 0.027(5) 0.031(5) -0.005(4) -0.001(4) 0.000(4) N12 0.041(6) 0.032(5) 0.034(5) 0.003(4) -0.005(4) 0.000(5) N13 0.022(4) 0.034(5) 0.034(5) 0.009(4) 0.015(4) 0.000(4) N14 0.058(6) 0.036(5) 0.027(5) 0.004(4) 0.000(4) -0.007(5) N15 0.045(6) 0.046(5) 0.036(5) 0.004(4) -0.008(4) -0.005(5) N16 0.038(5) 0.031(5) 0.044(5) 0.013(4) -0.014(4) -0.008(4) C1 0.047(7) 0.062(7) 0.035(6) -0.018(5) 0.005(5) -0.038(6) C2 0.048(7) 0.022(5) 0.022(5) 0.000(4) 0.003(5) 0.000(5) C3 0.028(6) 0.037(6) 0.026(5) 0.001(5) 0.000(4) 0.000(5) C4 0.030(6) 0.055(7) 0.033(6) 0.003(5) -0.006(5) 0.003(5) C5 0.046(7) 0.027(6) 0.050(7) 0.008(5) -0.008(6) -0.008(5) C6 0.024(6) 0.051(7) 0.028(6) 0.021(5) 0.003(5) -0.008(5) C7 0.042(6) 0.061(7) 0.030(6) 0.000(5) 0.016(5) -0.001(6) C8 0.028(5) 0.048(6) 0.035(6) -0.006(5) 0.008(5) 0.012(5) C9 0.023(5) 0.040(6) 0.027(5) -0.006(5) -0.006(4) -0.003(5) C10 0.029(6) 0.041(6) 0.038(6) 0.011(5) 0.001(5) 0.018(5) C11 0.043(7) 0.035(6) 0.049(7) 0.002(6) -0.008(6) 0.002(5) C12 0.055(11) 0.108(13) 0.077(11) -0.016(9) -0.008(9) 0.028(8) C13 0.069(9) 0.069(9) 0.072(9) -0.008(8) 0.030(8) -0.005(7) C14 0.034(9) 0.046(8) 0.087(15) -0.010(9) -0.030(10) -0.003(6) C15 0.025(7) 0.058(9) 0.073(14) 0.001(11) -0.021(9) -0.028(7) C14X 0.031(14) 0.053(13) 0.07(2) -0.022(16) -0.029(16) -0.012(8) C15X 0.038(14) 0.042(12) 0.06(2) -0.009(15) -0.022(15) -0.018(11) C16 0.115(14) 0.103(12) 0.069(11) 0.037(10) -0.035(10) -0.051(11) C17 0.046(7) 0.032(6) 0.071(8) -0.005(6) 0.000(6) -0.012(5) C18 0.045(7) 0.033(6) 0.060(7) 0.004(5) 0.009(6) -0.002(5) C19 0.039(7) 0.068(9) 0.100(11) 0.031(8) -0.018(7) 0.002(6) C20 0.080(10) 0.052(8) 0.036(7) 0.003(6) -0.003(7) -0.031(7) C21 0.037(7) 0.098(10) 0.062(8) -0.039(7) 0.015(6) -0.013(7) C22 0.029(5) 0.033(6) 0.034(6) -0.006(5) -0.007(5) -0.007(5) C23 0.029(5) 0.039(6) 0.032(6) -0.009(5) -0.002(5) 0.011(5) C24 0.037(6) 0.027(5) 0.040(6) 0.010(5) 0.007(5) 0.005(5) C25 0.050(7) 0.049(7) 0.025(6) 0.014(5) -0.007(5) -0.002(6) C26 0.030(6) 0.055(7) 0.046(7) -0.004(6) 0.000(5) 0.008(5) C27 0.025(6) 0.083(9) 0.044(7) -0.005(6) 0.016(5) 0.006(6) C28 0.042(8) 0.038(7) 0.033(6) 0.006(4) 0.015(6) -0.002(5) C29 0.042(7) 0.036(6) 0.034(6) 0.012(5) -0.004(5) -0.003(5) C30 0.060(8) 0.036(7) 0.055(7) -0.007(6) -0.010(6) -0.011(6) C31 0.041(7) 0.057(7) 0.046(7) 0.027(6) 0.015(6) 0.001(6) C32 0.128(13) 0.049(8) 0.070(9) 0.023(7) 0.041(9) 0.030(8) C33 0.059(9) 0.061(9) 0.156(15) -0.022(10) 0.027(10) -0.008(7) C34 0.038(10) 0.026(9) 0.034(8) 0.008(6) -0.002(7) 0.002(7) C35 0.044(10) 0.013(8) 0.034(7) 0.002(6) -0.004(8) 0.001(7) C34X 0.045(14) 0.031(16) 0.025(11) 0.014(11) 0.003(11) 0.009(11) C35X 0.056(16) 0.026(11) 0.034(15) 0.002(11) -0.003(11) -0.005(13) C36 0.104(11) 0.040(7) 0.040(7) 0.001(6) 0.011(7) 0.000(7) C37 0.039(6) 0.052(7) 0.035(6) -0.023(6) -0.005(5) -0.003(6) C38 0.034(7) 0.037(7) 0.029(6) -0.006(4) -0.003(5) -0.007(4) C39 0.059(8) 0.031(6) 0.053(7) 0.017(5) -0.002(6) 0.002(5) C40 0.040(6) 0.043(6) 0.044(7) -0.001(5) -0.013(5) -0.013(5) C41 0.046(7) 0.079(9) 0.045(7) -0.023(7) -0.002(6) -0.035(7) C42 0.028(6) 0.051(7) 0.025(5) -0.007(5) -0.001(4) 0.003(5) C43 0.034(6) 0.026(6) 0.025(5) 0.003(4) 0.002(5) -0.004(5) C44 0.039(7) 0.041(7) 0.039(6) 0.008(5) -0.009(5) 0.000(5) C45 0.027(5) 0.045(6) 0.032(6) 0.006(5) -0.013(4) 0.000(5) C46 0.056(8) 0.046(7) 0.029(6) 0.011(5) 0.002(6) -0.007(6) C47 0.052(7) 0.061(8) 0.029(6) 0.002(6) 0.010(5) -0.012(6) C48 0.044(7) 0.040(6) 0.043(7) -0.013(5) 0.008(5) 0.006(5) C49 0.034(6) 0.044(7) 0.030(6) 0.003(5) 0.002(5) 0.004(5) C50 0.047(7) 0.045(7) 0.042(7) 0.016(5) 0.010(6) 0.022(6) C51 0.064(8) 0.041(6) 0.048(7) -0.017(6) 0.005(6) 0.004(6) C52 0.034(8) 0.025(7) 0.099(11) 0.011(6) -0.010(8) 0.007(5) C53 0.051(8) 0.043(7) 0.086(10) -0.008(7) 0.011(7) -0.003(6) C54 0.031(6) 0.040(7) 0.072(8) 0.003(6) -0.019(6) -0.002(5) C55 0.026(6) 0.048(7) 0.052(7) 0.003(6) -0.007(5) -0.011(5) C56 0.078(10) 0.043(7) 0.056(8) -0.004(6) 0.005(7) -0.008(7) C57 0.033(6) 0.042(6) 0.059(7) 0.009(6) 0.000(6) -0.007(5) C58 0.052(7) 0.035(6) 0.055(7) 0.003(5) 0.000(6) -0.016(6) C59 0.054(8) 0.057(8) 0.077(9) 0.014(7) 0.009(7) 0.007(7) C60 0.066(9) 0.030(6) 0.040(8) -0.010(5) -0.007(7) -0.003(5) C61 0.052(8) 0.101(11) 0.080(10) 0.040(9) 0.016(7) 0.030(8) C62 0.026(6) 0.070(8) 0.036(6) -0.002(6) -0.002(5) 0.014(5) C63 0.029(6) 0.045(7) 0.041(6) -0.003(5) 0.011(5) -0.007(5) C64 0.051(8) 0.055(8) 0.086(10) 0.026(7) 0.021(7) 0.006(6) C65 0.061(8) 0.033(6) 0.085(10) -0.036(6) -0.023(7) 0.016(6) C66 0.049(8) 0.046(7) 0.048(8) -0.005(6) 0.017(6) -0.002(6) C67 0.041(7) 0.057(7) 0.058(8) -0.002(6) 0.034(6) 0.004(6) C68 0.042(7) 0.068(8) 0.044(7) 0.020(6) -0.001(5) -0.031(6) C69 0.027(6) 0.035(6) 0.043(6) 0.001(5) 0.000(5) 0.005(5) C70 0.038(7) 0.066(8) 0.042(7) 0.002(6) -0.011(5) -0.005(6) C71 0.052(7) 0.051(7) 0.054(7) -0.005(6) 0.005(6) -0.006(6) C72 0.091(10) 0.039(7) 0.040(7) -0.015(5) -0.001(7) -0.010(7) C73 0.086(10) 0.055(8) 0.052(8) 0.010(6) 0.013(7) 0.009(7) C74 0.055(9) 0.042(7) 0.050(8) 0.009(5) -0.001(7) -0.003(5) C75 0.051(7) 0.058(7) 0.033(6) 0.019(6) -0.006(5) 0.002(6) C76 0.047(7) 0.056(8) 0.063(8) 0.026(6) 0.010(6) 0.000(6) C77 0.054(7) 0.044(7) 0.050(7) 0.010(6) 0.001(6) -0.009(6) C78 0.049(7) 0.035(6) 0.058(8) -0.002(6) -0.011(6) -0.006(5) C79 0.083(10) 0.059(8) 0.051(8) -0.020(6) 0.001(7) -0.041(7) C80 0.033(7) 0.071(8) 0.076(9) 0.018(7) 0.001(6) 0.002(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N1 2.026(7) . ? Zn1 C1 2.009(9) . ? Zn1 C2 2.033(8) . ? Zn2 N5 2.020(7) . ? Zn2 C21 2.006(10) . ? Zn2 C22 2.050(9) . ? Zn3 N9 2.025(7) . ? Zn3 C41 2.002(10) . ? Zn3 C42 2.034(9) . ? Zn4 N13 2.023(8) . ? Zn4 C61 2.011(12) . ? Zn4 C62 2.040(9) . ? K1 N1 2.758(7) . ? K1 N2 2.862(9) . ? K1 N3 2.808(9) . ? K1 N4 2.824(9) . ? K1 C2 2.987(10) . ? K2 N5 2.758(7) . ? K2 N6 2.876(8) . ? K2 N7 2.822(8) . ? K2 N8 2.918(8) . ? K2 C22 2.973(10) . ? K3 N9 2.773(7) . ? K3 N10 2.902(8) . ? K3 N11 2.849(8) . ? K3 N12 2.872(8) . ? K3 C42 3.003(10) . ? K4 N13 2.756(7) . ? K4 N14 2.882(8) . ? K4 N15 2.834(8) . ? K4 N16 2.877(8) . ? K4 C62 2.971(11) . ? N1 C3 1.472(11) . ? N1 C9 1.483(11) . ? N2 C12 1.454(17) . ? N2 C13 1.444(15) . ? N2 C14 1.501(13) . ? N2 C14X 1.517(16) . ? N3 C15 1.529(13) . ? N3 C15X 1.497(16) . ? N3 C16 1.413(19) . ? N3 C17 1.426(14) . ? N4 C18 1.503(13) . ? N4 C19 1.450(14) . ? N4 C20 1.438(14) . ? N5 C23 1.458(12) . ? N5 C29 1.506(12) . ? N6 C32 1.451(13) . ? N6 C33 1.451(14) . ? N6 C34 1.500(12) . ? N6 C34X 1.502(15) . ? N7 C35 1.510(12) . ? N7 C35X 1.506(15) . ? N7 C36 1.453(15) . ? N7 C37 1.439(13) . ? N8 C38 1.452(12) . ? N8 C39 1.453(12) . ? N8 C40 1.460(12) . ? N9 C43 1.457(11) . ? N9 C49 1.490(12) . ? N10 C52 1.444(13) . ? N10 C53 1.472(14) . ? N10 C54 1.466(13) . ? N11 C55 1.463(13) . ? N11 C56 1.465(14) . ? N11 C57 1.443(13) . ? N12 C58 1.461(13) . ? N12 C59 1.431(13) . ? N12 C60 1.439(13) . ? N13 C63 1.452(13) . ? N13 C69 1.496(13) . ? N14 C72 1.453(13) . ? N14 C73 1.460(14) . ? N14 C74 1.421(14) . ? N15 C75 1.461(13) . ? N15 C76 1.468(13) . ? N15 C77 1.482(13) . ? N16 C78 1.439(13) . ? N16 C79 1.474(13) . ? N16 C80 1.489(13) . ? C1 H1A 0.980 . ? C1 H1B 0.980 . ? C1 H1C 0.980 . ? C2 H2A 0.980 . ? C2 H2B 0.980 . ? C2 H2C 0.980 . ? C3 C4 1.554(13) . ? C3 C5 1.520(14) . ? C3 C6 1.553(13) . ? C4 H4A 0.980 . ? C4 H4B 0.980 . ? C4 H4C 0.980 . ? C5 H5A 0.980 . ? C5 H5B 0.980 . ? C5 H5C 0.980 . ? C6 H6A 0.990 . ? C6 H6B 0.990 . ? C6 C7 1.493(14) . ? C7 H7A 0.990 . ? C7 H7B 0.990 . ? C7 C8 1.503(14) . ? C8 H8A 0.990 . ? C8 H8B 0.990 . ? C8 C9 1.516(13) . ? C9 C10 1.533(13) . ? C9 C11 1.548(13) . ? C10 H10A 0.980 . ? C10 H10B 0.980 . ? C10 H10C 0.980 . ? C11 H11A 0.980 . ? C11 H11B 0.980 . ? C11 H11C 0.980 . ? C12 H12A 0.980 . ? C12 H12B 0.980 . ? C12 H12C 0.980 . ? C13 H13A 0.980 . ? C13 H13B 0.980 . ? C13 H13C 0.980 . ? C14 H14A 0.990 . ? C14 H14B 0.990 . ? C14 C15 1.515(16) . ? C15 H15A 0.990 . ? C15 H15B 0.990 . ? C14X H14C 0.990 . ? C14X H14D 0.990 . ? C14X C15X 1.513(19) . ? C15X H15C 0.990 . ? C15X H15D 0.990 . ? C16 H16A 0.980 . ? C16 H16B 0.980 . ? C16 H16C 0.980 . ? C17 H17A 0.990 . ? C17 H17B 0.990 . ? C17 C18 1.503(15) . ? C18 H18A 0.990 . ? C18 H18B 0.990 . ? C19 H19A 0.980 . ? C19 H19B 0.980 . ? C19 H19C 0.980 . ? C20 H20A 0.980 . ? C20 H20B 0.980 . ? C20 H20C 0.980 . ? C21 H21A 0.980 . ? C21 H21B 0.980 . ? C21 H21C 0.980 . ? C22 H22A 0.980 . ? C22 H22B 0.980 . ? C22 H22C 0.980 . ? C23 C24 1.510(13) . ? C23 C25 1.570(14) . ? C23 C26 1.527(13) . ? C24 H24A 0.980 . ? C24 H24B 0.980 . ? C24 H24C 0.980 . ? C25 H25A 0.980 . ? C25 H25B 0.980 . ? C25 H25C 0.980 . ? C26 H26A 0.990 . ? C26 H26B 0.990 . ? C26 C27 1.544(15) . ? C27 H27A 0.990 . ? C27 H27B 0.990 . ? C27 C28 1.497(15) . ? C28 H28A 0.990 . ? C28 H28B 0.990 . ? C28 C29 1.553(14) . ? C29 C30 1.543(14) . ? C29 C31 1.487(14) . ? C30 H30A 0.980 . ? C30 H30B 0.980 . ? C30 H30C 0.980 . ? C31 H31A 0.980 . ? C31 H31B 0.980 . ? C31 H31C 0.980 . ? C32 H32A 0.980 . ? C32 H32B 0.980 . ? C32 H32C 0.980 . ? C33 H33A 0.980 . ? C33 H33B 0.980 . ? C33 H33C 0.980 . ? C34 H34A 0.990 . ? C34 H34B 0.990 . ? C34 C35 1.519(15) . ? C35 H35A 0.990 . ? C35 H35B 0.990 . ? C34X H34C 0.990 . ? C34X H34D 0.990 . ? C34X C35X 1.516(18) . ? C35X H35C 0.990 . ? C35X H35D 0.990 . ? C36 H36A 0.980 . ? C36 H36B 0.980 . ? C36 H36C 0.980 . ? C37 H37A 0.990 . ? C37 H37B 0.990 . ? C37 C38 1.524(14) . ? C38 H38A 0.990 . ? C38 H38B 0.990 . ? C39 H39A 0.980 . ? C39 H39B 0.980 . ? C39 H39C 0.980 . ? C40 H40A 0.980 . ? C40 H40B 0.980 . ? C40 H40C 0.980 . ? C41 H41A 0.980 . ? C41 H41B 0.980 . ? C41 H41C 0.980 . ? C42 H42A 0.980 . ? C42 H42B 0.980 . ? C42 H42C 0.980 . ? C43 C44 1.489(14) . ? C43 C45 1.561(13) . ? C43 C46 1.555(14) . ? C44 H44A 0.980 . ? C44 H44B 0.980 . ? C44 H44C 0.980 . ? C45 H45A 0.980 . ? C45 H45B 0.980 . ? C45 H45C 0.980 . ? C46 H46A 0.990 . ? C46 H46B 0.990 . ? C46 C47 1.508(15) . ? C47 H47A 0.990 . ? C47 H47B 0.990 . ? C47 C48 1.530(15) . ? C48 H48A 0.990 . ? C48 H48B 0.990 . ? C48 C49 1.518(13) . ? C49 C50 1.514(14) . ? C49 C51 1.569(15) . ? C50 H50A 0.980 . ? C50 H50B 0.980 . ? C50 H50C 0.980 . ? C51 H51A 0.980 . ? C51 H51B 0.980 . ? C51 H51C 0.980 . ? C52 H52A 0.980 . ? C52 H52B 0.980 . ? C52 H52C 0.980 . ? C53 H53A 0.980 . ? C53 H53B 0.980 . ? C53 H53C 0.980 . ? C54 H54A 0.990 . ? C54 H54B 0.990 . ? C54 C55 1.512(14) . ? C55 H55A 0.990 . ? C55 H55B 0.990 . ? C56 H56A 0.980 . ? C56 H56B 0.980 . ? C56 H56C 0.980 . ? C57 H57A 0.990 . ? C57 H57B 0.990 . ? C57 C58 1.457(14) . ? C58 H58A 0.990 . ? C58 H58B 0.990 . ? C59 H59A 0.980 . ? C59 H59B 0.980 . ? C59 H59C 0.980 . ? C60 H60A 0.980 . ? C60 H60B 0.980 . ? C60 H60C 0.980 . ? C61 H61A 0.980 . ? C61 H61B 0.980 . ? C61 H61C 0.980 . ? C62 H62A 0.980 . ? C62 H62B 0.980 . ? C62 H62C 0.980 . ? C63 C64 1.545(15) . ? C63 C65 1.527(15) . ? C63 C66 1.539(14) . ? C64 H64A 0.980 . ? C64 H64B 0.980 . ? C64 H64C 0.980 . ? C65 H65A 0.980 . ? C65 H65B 0.980 . ? C65 H65C 0.980 . ? C66 H66A 0.990 . ? C66 H66B 0.990 . ? C66 C67 1.527(16) . ? C67 H67A 0.990 . ? C67 H67B 0.990 . ? C67 C68 1.533(15) . ? C68 H68A 0.990 . ? C68 H68B 0.990 . ? C68 C69 1.530(13) . ? C69 C70 1.557(14) . ? C69 C71 1.521(14) . ? C70 H70A 0.980 . ? C70 H70B 0.980 . ? C70 H70C 0.980 . ? C71 H71A 0.980 . ? C71 H71B 0.980 . ? C71 H71C 0.980 . ? C72 H72A 0.980 . ? C72 H72B 0.980 . ? C72 H72C 0.980 . ? C73 H73A 0.980 . ? C73 H73B 0.980 . ? C73 H73C 0.980 . ? C74 H74A 0.990 . ? C74 H74B 0.990 . ? C74 C75 1.531(15) . ? C75 H75A 0.990 . ? C75 H75B 0.990 . ? C76 H76A 0.980 . ? C76 H76B 0.980 . ? C76 H76C 0.980 . ? C77 H77A 0.990 . ? C77 H77B 0.990 . ? C77 C78 1.486(15) . ? C78 H78A 0.990 . ? C78 H78B 0.990 . ? C79 H79A 0.980 . ? C79 H79B 0.980 . ? C79 H79C 0.980 . ? C80 H80A 0.980 . ? C80 H80B 0.980 . ? C80 H80C 0.980 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Zn1 C1 120.5(3) . . ? N1 Zn1 C2 115.7(3) . . ? C1 Zn1 C2 123.7(4) . . ? N5 Zn2 C21 120.8(4) . . ? N5 Zn2 C22 114.9(3) . . ? C21 Zn2 C22 124.4(4) . . ? N9 Zn3 C41 119.1(4) . . ? N9 Zn3 C42 114.7(4) . . ? C41 Zn3 C42 126.1(4) . . ? N13 Zn4 C61 120.4(4) . . ? N13 Zn4 C62 114.2(4) . . ? C61 Zn4 C62 125.4(5) . . ? N1 K1 N2 121.0(3) . . ? N1 K1 N3 135.7(3) . . ? N1 K1 N4 124.6(2) . . ? N1 K1 C2 73.4(2) . . ? N2 K1 N3 63.0(3) . . ? N2 K1 N4 113.4(3) . . ? N2 K1 C2 112.2(3) . . ? N3 K1 N4 63.7(3) . . ? N3 K1 C2 150.1(3) . . ? N4 K1 C2 95.9(3) . . ? N5 K2 N6 124.5(2) . . ? N5 K2 N7 140.0(3) . . ? N5 K2 N8 118.0(2) . . ? N5 K2 C22 73.4(2) . . ? N6 K2 N7 63.2(2) . . ? N6 K2 N8 116.4(2) . . ? N6 K2 C22 94.2(3) . . ? N7 K2 N8 62.4(2) . . ? N7 K2 C22 145.9(3) . . ? N8 K2 C22 113.9(2) . . ? N9 K3 N10 116.5(2) . . ? N9 K3 N11 140.9(2) . . ? N9 K3 N12 123.9(2) . . ? N9 K3 C42 72.5(2) . . ? N10 K3 N11 62.5(2) . . ? N10 K3 N12 117.8(3) . . ? N10 K3 C42 114.7(3) . . ? N11 K3 N12 62.2(2) . . ? N11 K3 C42 146.1(3) . . ? N12 K3 C42 96.6(3) . . ? N13 K4 N14 117.0(3) . . ? N13 K4 N15 141.6(3) . . ? N13 K4 N16 124.1(3) . . ? N13 K4 C62 73.0(2) . . ? N14 K4 N15 62.3(2) . . ? N14 K4 N16 117.6(2) . . ? N14 K4 C62 112.3(3) . . ? N15 K4 N16 62.7(2) . . ? N15 K4 C62 145.1(3) . . ? N16 K4 C62 96.8(3) . . ? Zn1 N1 K1 88.4(2) . . ? Zn1 N1 C3 112.1(5) . . ? Zn1 N1 C9 114.9(5) . . ? K1 N1 C3 109.1(5) . . ? K1 N1 C9 113.6(5) . . ? C3 N1 C9 115.5(7) . . ? K1 N2 C12 115.1(8) . . ? K1 N2 C13 101.3(7) . . ? K1 N2 C14 111.9(8) . . ? K1 N2 C14X 106.0(16) . . ? C12 N2 C13 107.4(10) . . ? C12 N2 C14 98.9(11) . . ? C12 N2 C14X 128.8(19) . . ? C13 N2 C14 123.0(13) . . ? C13 N2 C14X 92.5(15) . . ? K1 N3 C15 112.3(8) . . ? K1 N3 C15X 114.8(16) . . ? K1 N3 C16 97.9(8) . . ? K1 N3 C17 114.9(7) . . ? C15 N3 C16 118.1(14) . . ? C15 N3 C17 101.8(10) . . ? C15X N3 C16 87.4(17) . . ? C15X N3 C17 122(2) . . ? C16 N3 C17 112.6(10) . . ? K1 N4 C18 111.1(6) . . ? K1 N4 C19 117.1(7) . . ? K1 N4 C20 100.8(6) . . ? C18 N4 C19 107.6(9) . . ? C18 N4 C20 109.8(8) . . ? C19 N4 C20 110.3(10) . . ? Zn2 N5 K2 88.9(2) . . ? Zn2 N5 C23 113.2(5) . . ? Zn2 N5 C29 113.0(6) . . ? K2 N5 C23 109.0(5) . . ? K2 N5 C29 111.4(5) . . ? C23 N5 C29 117.6(7) . . ? K2 N6 C32 112.9(6) . . ? K2 N6 C33 105.4(7) . . ? K2 N6 C34 110.5(7) . . ? K2 N6 C34X 105.8(12) . . ? C32 N6 C33 109.4(11) . . ? C32 N6 C34 100.1(10) . . ? C32 N6 C34X 128.8(15) . . ? C33 N6 C34 118.8(11) . . ? C33 N6 C34X 90.6(13) . . ? K2 N7 C35 114.9(7) . . ? K2 N7 C35X 109.7(14) . . ? K2 N7 C36 97.8(6) . . ? K2 N7 C37 115.2(6) . . ? C35 N7 C36 118.6(10) . . ? C35 N7 C37 101.2(9) . . ? C35X N7 C36 88.1(13) . . ? C35X N7 C37 127.9(16) . . ? C36 N7 C37 110.1(8) . . ? K2 N8 C38 113.2(5) . . ? K2 N8 C39 121.1(6) . . ? K2 N8 C40 89.8(5) . . ? C38 N8 C39 110.0(8) . . ? C38 N8 C40 111.1(8) . . ? C39 N8 C40 109.7(8) . . ? Zn3 N9 K3 89.5(2) . . ? Zn3 N9 C43 113.0(5) . . ? Zn3 N9 C49 114.1(6) . . ? K3 N9 C43 108.4(5) . . ? K3 N9 C49 111.5(5) . . ? C43 N9 C49 116.9(7) . . ? K3 N10 C52 119.2(7) . . ? K3 N10 C53 92.6(6) . . ? K3 N10 C54 113.3(6) . . ? C52 N10 C53 109.1(9) . . ? C52 N10 C54 110.1(9) . . ? C53 N10 C54 111.2(9) . . ? K3 N11 C55 115.3(5) . . ? K3 N11 C56 94.2(6) . . ? K3 N11 C57 115.2(6) . . ? C55 N11 C56 109.4(9) . . ? C55 N11 C57 109.3(8) . . ? C56 N11 C57 112.7(8) . . ? K3 N12 C58 111.4(6) . . ? K3 N12 C59 113.6(6) . . ? K3 N12 C60 100.7(6) . . ? C58 N12 C59 111.2(9) . . ? C58 N12 C60 110.8(8) . . ? C59 N12 C60 108.7(9) . . ? Zn4 N13 K4 89.5(3) . . ? Zn4 N13 C63 114.1(6) . . ? Zn4 N13 C69 112.6(6) . . ? K4 N13 C63 111.5(5) . . ? K4 N13 C69 111.1(5) . . ? C63 N13 C69 115.2(7) . . ? K4 N14 C72 118.0(6) . . ? K4 N14 C73 93.5(6) . . ? K4 N14 C74 113.3(6) . . ? C72 N14 C73 109.0(9) . . ? C72 N14 C74 110.3(9) . . ? C73 N14 C74 111.6(9) . . ? K4 N15 C75 116.0(6) . . ? K4 N15 C76 94.4(6) . . ? K4 N15 C77 114.9(6) . . ? C75 N15 C76 109.9(9) . . ? C75 N15 C77 109.0(8) . . ? C76 N15 C77 111.9(9) . . ? K4 N16 C78 112.1(6) . . ? K4 N16 C79 114.9(6) . . ? K4 N16 C80 99.5(6) . . ? C78 N16 C79 108.7(8) . . ? C78 N16 C80 111.6(9) . . ? C79 N16 C80 109.7(9) . . ? Zn1 C1 H1A 109.5 . . ? Zn1 C1 H1B 109.5 . . ? Zn1 C1 H1C 109.5 . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Zn1 C2 H2A 109.5 . . ? Zn1 C2 H2B 109.5 . . ? Zn1 C2 H2C 109.5 . . ? H2A C2 H2B 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C3 C4 113.5(8) . . ? N1 C3 C5 107.7(7) . . ? N1 C3 C6 112.7(8) . . ? C4 C3 C5 105.7(8) . . ? C4 C3 C6 108.3(8) . . ? C5 C3 C6 108.6(8) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C6 H6A 109.1 . . ? C3 C6 H6B 109.1 . . ? C3 C6 C7 112.3(8) . . ? H6A C6 H6B 107.9 . . ? H6A C6 C7 109.1 . . ? H6B C6 C7 109.1 . . ? C6 C7 H7A 109.7 . . ? C6 C7 H7B 109.7 . . ? C6 C7 C8 109.7(8) . . ? H7A C7 H7B 108.2 . . ? H7A C7 C8 109.7 . . ? H7B C7 C8 109.7 . . ? C7 C8 H8A 109.1 . . ? C7 C8 H8B 109.1 . . ? C7 C8 C9 112.6(8) . . ? H8A C8 H8B 107.8 . . ? H8A C8 C9 109.1 . . ? H8B C8 C9 109.1 . . ? N1 C9 C8 113.2(8) . . ? N1 C9 C10 105.4(7) . . ? N1 C9 C11 114.0(7) . . ? C8 C9 C10 107.8(8) . . ? C8 C9 C11 110.0(8) . . ? C10 C9 C11 105.8(8) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N2 C12 H12A 109.5 . . ? N2 C12 H12B 109.5 . . ? N2 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N2 C13 H13A 109.5 . . ? N2 C13 H13B 109.5 . . ? N2 C13 H13C 109.5 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N2 C14 H14A 110.5 . . ? N2 C14 H14B 110.5 . . ? N2 C14 C15 106.0(14) . . ? H14A C14 H14B 108.7 . . ? H14A C14 C15 110.5 . . ? H14B C14 C15 110.5 . . ? N3 C15 C14 111.6(13) . . ? N3 C15 H15A 109.3 . . ? N3 C15 H15B 109.3 . . ? C14 C15 H15A 109.3 . . ? C14 C15 H15B 109.3 . . ? H15A C15 H15B 108.0 . . ? N2 C14X H14C 108.7 . . ? N2 C14X H14D 108.7 . . ? N2 C14X C15X 114(2) . . ? H14C C14X H14D 107.6 . . ? H14C C14X C15X 108.7 . . ? H14D C14X C15X 108.7 . . ? N3 C15X C14X 100(2) . . ? N3 C15X H15C 111.7 . . ? N3 C15X H15D 111.7 . . ? N3 C15X C16 44.6(9) . . ? C14X C15X H15C 111.7 . . ? C14X C15X H15D 111.7 . . ? H15C C15X H15D 109.5 . . ? N3 C16 H16A 109.5 . . ? N3 C16 H16B 109.5 . . ? N3 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N3 C17 H17A 108.8 . . ? N3 C17 H17B 108.8 . . ? N3 C17 C18 114.0(9) . . ? H17A C17 H17B 107.7 . . ? H17A C17 C18 108.8 . . ? H17B C17 C18 108.8 . . ? N4 C18 C17 113.2(8) . . ? N4 C18 H18A 108.9 . . ? N4 C18 H18B 108.9 . . ? C17 C18 H18A 108.9 . . ? C17 C18 H18B 108.9 . . ? H18A C18 H18B 107.8 . . ? N4 C19 H19A 109.5 . . ? N4 C19 H19B 109.5 . . ? N4 C19 H19C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N4 C20 H20A 109.5 . . ? N4 C20 H20B 109.5 . . ? N4 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Zn2 C21 H21A 109.5 . . ? Zn2 C21 H21B 109.5 . . ? Zn2 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Zn2 C22 H22A 109.5 . . ? Zn2 C22 H22B 109.5 . . ? Zn2 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N5 C23 C24 107.8(8) . . ? N5 C23 C25 113.9(8) . . ? N5 C23 C26 112.5(8) . . ? C24 C23 C25 106.7(8) . . ? C24 C23 C26 106.8(8) . . ? C25 C23 C26 108.8(8) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.2 . . ? C23 C26 H26B 109.2 . . ? C23 C26 C27 112.1(8) . . ? H26A C26 H26B 107.9 . . ? H26A C26 C27 109.2 . . ? H26B C26 C27 109.2 . . ? C26 C27 H27A 110.1 . . ? C26 C27 H27B 110.1 . . ? C26 C27 C28 108.1(8) . . ? H27A C27 H27B 108.4 . . ? H27A C27 C28 110.1 . . ? H27B C27 C28 110.1 . . ? C27 C28 H28A 108.6 . . ? C27 C28 H28B 108.6 . . ? C27 C28 C29 114.8(9) . . ? H28A C28 H28B 107.5 . . ? H28A C28 C29 108.6 . . ? H28B C28 C29 108.6 . . ? N5 C29 C28 110.3(8) . . ? N5 C29 C30 112.9(8) . . ? N5 C29 C31 106.8(8) . . ? C28 C29 C30 109.2(9) . . ? C28 C29 C31 109.2(9) . . ? C30 C29 C31 108.4(9) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30B 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31B 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N6 C32 H32A 109.5 . . ? N6 C32 H32B 109.5 . . ? N6 C32 H32C 109.5 . . ? H32A C32 H32B 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N6 C33 H33A 109.5 . . ? N6 C33 H33B 109.5 . . ? N6 C33 H33C 109.5 . . ? H33A C33 H33B 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N6 C34 H34A 109.3 . . ? N6 C34 H34B 109.3 . . ? N6 C34 C35 111.6(11) . . ? H34A C34 H34B 108.0 . . ? H34A C34 C35 109.3 . . ? H34B C34 C35 109.3 . . ? N7 C35 C34 110.6(11) . . ? N7 C35 H35A 109.5 . . ? N7 C35 H35B 109.5 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 108.1 . . ? N6 C34X H34C 109.6 . . ? N6 C34X H34D 109.6 . . ? N6 C34X C35X 110(2) . . ? H34C C34X H34D 108.2 . . ? H34C C34X C35X 109.6 . . ? H34D C34X C35X 109.6 . . ? N7 C35X C34X 101.0(18) . . ? N7 C35X H35C 111.6 . . ? N7 C35X H35D 111.6 . . ? C34X C35X H35C 111.6 . . ? C34X C35X H35D 111.6 . . ? H35C C35X H35D 109.4 . . ? N7 C36 H36A 109.5 . . ? N7 C36 H36B 109.5 . . ? N7 C36 H36C 109.5 . . ? H36A C36 H36B 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N7 C37 H37A 108.7 . . ? N7 C37 H37B 108.7 . . ? N7 C37 C38 114.4(8) . . ? H37A C37 H37B 107.6 . . ? H37A C37 C38 108.7 . . ? H37B C37 C38 108.7 . . ? N8 C38 C37 115.1(9) . . ? N8 C38 H38A 108.5 . . ? N8 C38 H38B 108.5 . . ? C37 C38 H38A 108.5 . . ? C37 C38 H38B 108.5 . . ? H38A C38 H38B 107.5 . . ? N8 C39 H39A 109.5 . . ? N8 C39 H39B 109.5 . . ? N8 C39 H39C 109.5 . . ? H39A C39 H39B 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N8 C40 H40A 109.5 . . ? N8 C40 H40B 109.5 . . ? N8 C40 H40C 109.5 . . ? H40A C40 H40B 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? Zn3 C41 H41A 109.5 . . ? Zn3 C41 H41B 109.5 . . ? Zn3 C41 H41C 109.5 . . ? H41A C41 H41B 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? Zn3 C42 H42A 109.5 . . ? Zn3 C42 H42B 109.5 . . ? Zn3 C42 H42C 109.5 . . ? H42A C42 H42B 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N9 C43 C44 108.3(8) . . ? N9 C43 C45 114.8(7) . . ? N9 C43 C46 111.9(8) . . ? C44 C43 C45 106.7(8) . . ? C44 C43 C46 107.1(8) . . ? C45 C43 C46 107.6(8) . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44B 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45B 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C43 C46 H46A 109.2 . . ? C43 C46 H46B 109.2 . . ? C43 C46 C47 112.2(8) . . ? H46A C46 H46B 107.9 . . ? H46A C46 C47 109.2 . . ? H46B C46 C47 109.2 . . ? C46 C47 H47A 110.0 . . ? C46 C47 H47B 110.0 . . ? C46 C47 C48 108.7(8) . . ? H47A C47 H47B 108.3 . . ? H47A C47 C48 110.0 . . ? H47B C47 C48 110.0 . . ? C47 C48 H48A 108.9 . . ? C47 C48 H48B 108.9 . . ? C47 C48 C49 113.4(8) . . ? H48A C48 H48B 107.7 . . ? H48A C48 C49 108.9 . . ? H48B C48 C49 108.9 . . ? N9 C49 C48 112.0(8) . . ? N9 C49 C50 107.7(8) . . ? N9 C49 C51 113.7(8) . . ? C48 C49 C50 106.9(8) . . ? C48 C49 C51 109.9(8) . . ? C50 C49 C51 106.3(9) . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50B 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51B 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? N10 C52 H52A 109.5 . . ? N10 C52 H52B 109.5 . . ? N10 C52 H52C 109.5 . . ? H52A C52 H52B 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N10 C53 H53A 109.5 . . ? N10 C53 H53B 109.5 . . ? N10 C53 H53C 109.5 . . ? H53A C53 H53B 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N10 C54 H54A 108.7 . . ? N10 C54 H54B 108.7 . . ? N10 C54 C55 114.1(9) . . ? H54A C54 H54B 107.6 . . ? H54A C54 C55 108.7 . . ? H54B C54 C55 108.7 . . ? N11 C55 C54 115.4(8) . . ? N11 C55 H55A 108.4 . . ? N11 C55 H55B 108.4 . . ? C54 C55 H55A 108.4 . . ? C54 C55 H55B 108.4 . . ? H55A C55 H55B 107.5 . . ? N11 C56 H56A 109.5 . . ? N11 C56 H56B 109.5 . . ? N11 C56 H56C 109.5 . . ? H56A C56 H56B 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? N11 C57 H57A 108.8 . . ? N11 C57 H57B 108.8 . . ? N11 C57 C58 113.7(9) . . ? H57A C57 H57B 107.7 . . ? H57A C57 C58 108.8 . . ? H57B C57 C58 108.8 . . ? N12 C58 C57 116.3(9) . . ? N12 C58 H58A 108.2 . . ? N12 C58 H58B 108.2 . . ? C57 C58 H58A 108.2 . . ? C57 C58 H58B 108.2 . . ? H58A C58 H58B 107.4 . . ? N12 C59 H59A 109.5 . . ? N12 C59 H59B 109.5 . . ? N12 C59 H59C 109.5 . . ? H59A C59 H59B 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? N12 C60 H60A 109.5 . . ? N12 C60 H60B 109.5 . . ? N12 C60 H60C 109.5 . . ? H60A C60 H60B 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? Zn4 C61 H61A 109.5 . . ? Zn4 C61 H61B 109.5 . . ? Zn4 C61 H61C 109.5 . . ? H61A C61 H61B 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? Zn4 C62 H62A 109.5 . . ? Zn4 C62 H62B 109.5 . . ? Zn4 C62 H62C 109.5 . . ? H62A C62 H62B 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? N13 C63 C64 114.7(9) . . ? N13 C63 C65 105.6(8) . . ? N13 C63 C66 112.7(8) . . ? C64 C63 C65 105.3(9) . . ? C64 C63 C66 109.2(9) . . ? C65 C63 C66 108.8(10) . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64B 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C63 C65 H65A 109.5 . . ? C63 C65 H65B 109.5 . . ? C63 C65 H65C 109.5 . . ? H65A C65 H65B 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C63 C66 H66A 109.1 . . ? C63 C66 H66B 109.1 . . ? C63 C66 C67 112.6(9) . . ? H66A C66 H66B 107.8 . . ? H66A C66 C67 109.1 . . ? H66B C66 C67 109.1 . . ? C66 C67 H67A 110.5 . . ? C66 C67 H67B 110.5 . . ? C66 C67 C68 106.4(9) . . ? H67A C67 H67B 108.6 . . ? H67A C67 C68 110.5 . . ? H67B C67 C68 110.5 . . ? C67 C68 H68A 109.2 . . ? C67 C68 H68B 109.2 . . ? C67 C68 C69 111.9(8) . . ? H68A C68 H68B 107.9 . . ? H68A C68 C69 109.2 . . ? H68B C68 C69 109.2 . . ? N13 C69 C68 112.6(8) . . ? N13 C69 C70 113.2(8) . . ? N13 C69 C71 106.2(8) . . ? C68 C69 C70 110.4(8) . . ? C68 C69 C71 108.0(8) . . ? C70 C69 C71 106.1(9) . . ? C69 C70 H70A 109.5 . . ? C69 C70 H70B 109.5 . . ? C69 C70 H70C 109.5 . . ? H70A C70 H70B 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C69 C71 H71A 109.5 . . ? C69 C71 H71B 109.5 . . ? C69 C71 H71C 109.5 . . ? H71A C71 H71B 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? N14 C72 H72A 109.5 . . ? N14 C72 H72B 109.5 . . ? N14 C72 H72C 109.5 . . ? H72A C72 H72B 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? N14 C73 H73A 109.5 . . ? N14 C73 H73B 109.5 . . ? N14 C73 H73C 109.5 . . ? H73A C73 H73B 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? N14 C74 H74A 108.4 . . ? N14 C74 H74B 108.4 . . ? N14 C74 C75 115.4(10) . . ? H74A C74 H74B 107.5 . . ? H74A C74 C75 108.4 . . ? H74B C74 C75 108.4 . . ? N15 C75 C74 112.8(9) . . ? N15 C75 H75A 109.0 . . ? N15 C75 H75B 109.0 . . ? C74 C75 H75A 109.0 . . ? C74 C75 H75B 109.0 . . ? H75A C75 H75B 107.8 . . ? N15 C76 H76A 109.5 . . ? N15 C76 H76B 109.5 . . ? N15 C76 H76C 109.5 . . ? H76A C76 H76B 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? N15 C77 H77A 108.8 . . ? N15 C77 H77B 108.8 . . ? N15 C77 C78 113.9(9) . . ? H77A C77 H77B 107.7 . . ? H77A C77 C78 108.8 . . ? H77B C77 C78 108.8 . . ? N16 C78 C77 115.6(9) . . ? N16 C78 H78A 108.4 . . ? N16 C78 H78B 108.4 . . ? C77 C78 H78A 108.4 . . ? C77 C78 H78B 108.4 . . ? H78A C78 H78B 107.4 . . ? N16 C79 H79A 109.5 . . ? N16 C79 H79B 109.5 . . ? N16 C79 H79C 109.5 . . ? H79A C79 H79B 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? N16 C80 H80A 109.5 . . ? N16 C80 H80B 109.5 . . ? N16 C80 H80C 109.5 . . ? H80A C80 H80B 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.099 _refine_diff_density_min -1.296 _refine_diff_density_rms 0.101 #===END #------------------------------------------------------------------- #---------------COMPOUND 2------------------------------------------ #-------------------------------------------------------------------- data_pgaben3 _database_code_depnum_ccdc_archive 'CCDC 731815' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H38 Fe K N3 Zn' _chemical_formula_sum 'C21 H38 Fe K N3 Zn' _chemical_formula_weight 492.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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' 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c a 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y, z+1/2' 'x+1/2, -y, z' _cell_length_a 18.2193(7) _cell_length_b 7.5981(4) _cell_length_c 17.7793(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2461.23(19) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 4538 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 30.11 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.330 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 1.743 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.934 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET) (compiled Apr 21 2008,18:23:10) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini S' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14510 _diffrn_reflns_av_R_equivalents 0.0517 _diffrn_reflns_av_sigmaI/netI 0.1075 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 29.00 _reflns_number_total 6300 _reflns_number_gt 4138 _reflns_threshold_expression I>2\s(I) _computing_data_collection CrysAlisPro _computing_cell_refinement CrysAlisPro _computing_data_reduction CrysAlisPro _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material SHELXL97 _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^)+(0.0121P)^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 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 0.010(10) _refine_ls_number_reflns 6300 _refine_ls_number_parameters 270 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0717 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_ref 0.0486 _refine_ls_wR_factor_gt 0.0448 _refine_ls_goodness_of_fit_ref 0.799 _refine_ls_restrained_S_all 0.799 _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 0.353279(17) 0.91881(4) 0.04357(2) 0.02474(8) Uani 1 1 d . . . Fe1 Fe 0.44860(2) 1.15931(6) -0.07810(2) 0.02674(11) Uani 1 1 d . . . K1 K 0.32043(3) 0.48938(8) 0.09328(4) 0.02153(14) Uani 1 1 d . . . N1 N 0.23230(14) 0.5825(5) 0.22206(15) 0.0424(8) Uani 1 1 d . . . N2 N 0.37073(15) 0.3667(4) 0.23714(14) 0.0329(7) Uani 1 1 d . . . N3 N 0.17271(14) 0.3622(4) 0.0960(2) 0.0445(8) Uani 1 1 d . . . C1 C 0.37700(15) 1.1655(4) 0.01243(16) 0.0216(7) Uani 1 1 d . . . C2 C 0.34801(16) 1.2568(4) -0.05233(17) 0.0273(8) Uani 1 1 d . . . H2 H 0.3030 1.2284 -0.0764 0.033 Uiso 1 1 calc R . . C3 C 0.39545(15) 1.3940(4) -0.0752(2) 0.0302(7) Uani 1 1 d . . . H3 H 0.3882 1.4712 -0.1165 0.036 Uiso 1 1 calc R . . C4 C 0.45579(17) 1.3950(4) -0.02503(17) 0.0305(8) Uani 1 1 d . . . H4 H 0.4964 1.4733 -0.0262 0.037 Uiso 1 1 calc R . . C5 C 0.44421(15) 1.2573(4) 0.02724(16) 0.0248(7) Uani 1 1 d . . . H5 H 0.4769 1.2292 0.0671 0.030 Uiso 1 1 calc R . . C10 C 0.5344(3) 0.9852(8) -0.0752(4) 0.0270(15) Uiso 0.60 1 d P . 1 H10 H 0.5632 0.9542 -0.0327 0.032 Uiso 0.60 1 calc PR . 1 C6 C 0.4688(4) 0.8978(8) -0.0979(3) 0.0263(14) Uiso 0.60 1 d P . 1 H6 H 0.4459 0.7995 -0.0747 0.032 Uiso 0.60 1 calc PR . 1 C7 C 0.4446(5) 0.9943(13) -0.1653(6) 0.043(3) Uiso 0.60 1 d P . 1 H7 H 0.4013 0.9673 -0.1928 0.052 Uiso 0.60 1 calc PR . 1 C8 C 0.4912(4) 1.1252(11) -0.1833(4) 0.035(2) Uiso 0.60 1 d P . 1 H8 H 0.4872 1.2029 -0.2250 0.042 Uiso 0.60 1 calc PR . 1 C9 C 0.5503(4) 1.1249(10) -0.1252(4) 0.032(2) Uiso 0.60 1 d P . 1 H9 H 0.5908 1.2034 -0.1224 0.038 Uiso 0.60 1 calc PR . 1 C11 C 0.42743(16) 0.8016(4) 0.11321(17) 0.0338(9) Uani 1 1 d . . . H11A H 0.4675 0.8840 0.1240 0.051 Uiso 1 1 calc R . . H11B H 0.4473 0.6962 0.0888 0.051 Uiso 1 1 calc R . . H11C H 0.4032 0.7683 0.1603 0.051 Uiso 1 1 calc R . . C12 C 0.26520(16) 0.8045(4) -0.00609(17) 0.0337(8) Uani 1 1 d . . . H12A H 0.2461 0.8824 -0.0454 0.050 Uiso 1 1 calc R . . H12B H 0.2270 0.7836 0.0317 0.050 Uiso 1 1 calc R . . H12C H 0.2800 0.6922 -0.0286 0.050 Uiso 1 1 calc R . . C13 C 0.4502(2) 0.3757(5) 0.2420(2) 0.0600(12) Uani 1 1 d . A . H13A H 0.4659 0.3432 0.2929 0.090 Uiso 1 1 calc R . . H13B H 0.4665 0.4958 0.2308 0.090 Uiso 1 1 calc R . . H13C H 0.4719 0.2940 0.2056 0.090 Uiso 1 1 calc R . . C14 C 0.3487(2) 0.1855(5) 0.2450(2) 0.0670(13) Uani 1 1 d . A . H14A H 0.3604 0.1444 0.2958 0.101 Uiso 1 1 calc R . . H14B H 0.3750 0.1133 0.2081 0.101 Uiso 1 1 calc R . . H14C H 0.2957 0.1755 0.2364 0.101 Uiso 1 1 calc R . . C15 C 0.34140(19) 0.4820(5) 0.2948(2) 0.0515(11) Uani 1 1 d . A . H15A H 0.3647 0.5991 0.2894 0.062 Uiso 1 1 calc R . . H15B H 0.3555 0.4347 0.3446 0.062 Uiso 1 1 calc R . . C16 C 0.2602(2) 0.5054(5) 0.2933(2) 0.0502(10) Uani 1 1 d . A . H16A H 0.2366 0.3895 0.3011 0.060 Uiso 1 1 calc R . . H16B H 0.2457 0.5826 0.3356 0.060 Uiso 1 1 calc R . . C17 C 0.2410(2) 0.7710(6) 0.2208(2) 0.0774(14) Uani 1 1 d . A . H17A H 0.2218 0.8176 0.1734 0.116 Uiso 1 1 calc R . . H17B H 0.2932 0.8005 0.2254 0.116 Uiso 1 1 calc R . . H17C H 0.2139 0.8229 0.2630 0.116 Uiso 1 1 calc R . . C18 C 0.1525(5) 0.5048(12) 0.2144(5) 0.030(2) Uiso 0.56 1 d P A 1 H18A H 0.1513 0.3865 0.2377 0.036 Uiso 0.56 1 calc PR A 1 H18B H 0.1179 0.5809 0.2424 0.036 Uiso 0.56 1 calc PR A 1 C19 C 0.1276(3) 0.4908(9) 0.1343(4) 0.0317(15) Uani 0.56 1 d P A 1 H19A H 0.0755 0.4543 0.1325 0.038 Uiso 0.56 1 calc PR A 1 H19B H 0.1321 0.6066 0.1092 0.038 Uiso 0.56 1 calc PR A 1 C20 C 0.1487(4) 0.3804(11) 0.0107(4) 0.041(2) Uani 0.62 1 d P A 1 H20A H 0.0965 0.3512 0.0058 0.062 Uiso 0.62 1 calc PR A 1 H20B H 0.1778 0.2997 -0.0203 0.062 Uiso 0.62 1 calc PR A 1 H20C H 0.1569 0.5016 -0.0062 0.062 Uiso 0.62 1 calc PR A 1 C18A C 0.1561(5) 0.5785(12) 0.2059(6) 0.036(3) Uani 0.44 1 d P A 2 H18C H 0.1442 0.6647 0.1660 0.043 Uiso 0.44 1 calc PR A 2 H18D H 0.1275 0.6087 0.2514 0.043 Uiso 0.44 1 calc PR A 2 C19A C 0.1378(4) 0.3954(10) 0.1803(5) 0.034(2) Uani 0.44 1 d P A 2 H19C H 0.0839 0.3800 0.1787 0.041 Uiso 0.44 1 calc PR A 2 H19D H 0.1583 0.3086 0.2161 0.041 Uiso 0.44 1 calc PR A 2 C20A C 0.1310(6) 0.4240(18) 0.0464(7) 0.043(3) Uani 0.38 1 d P A 2 H20D H 0.0823 0.3702 0.0510 0.064 Uiso 0.38 1 calc PR A 2 H20E H 0.1512 0.3984 -0.0035 0.064 Uiso 0.38 1 calc PR A 2 H20F H 0.1269 0.5517 0.0529 0.064 Uiso 0.38 1 calc PR A 2 C21 C 0.1712(2) 0.1770(6) 0.1070(2) 0.0695(14) Uani 1 1 d . A . H21A H 0.1202 0.1373 0.1112 0.104 Uiso 1 1 calc R . . H21B H 0.1977 0.1474 0.1532 0.104 Uiso 1 1 calc R . . H21C H 0.1946 0.1185 0.0641 0.104 Uiso 1 1 calc R . . C99 C 0.5065(6) 0.9376(12) -0.0826(6) 0.032(2) Uiso 0.40 1 d P . 2 H99 H 0.5217 0.8765 -0.0386 0.038 Uiso 0.40 1 calc PR . 2 C95 C 0.4410(5) 0.9076(13) -0.1226(6) 0.029(2) Uiso 0.40 1 d P . 2 H95 H 0.4045 0.8222 -0.1115 0.035 Uiso 0.40 1 calc PR . 2 C98 C 0.5438(9) 1.0665(18) -0.1169(9) 0.068(5) Uiso 0.40 1 d P . 2 H98 H 0.5905 1.1069 -0.1005 0.081 Uiso 0.40 1 calc PR . 2 C97 C 0.5112(6) 1.1276(16) -0.1720(7) 0.034(3) Uiso 0.40 1 d P . 2 H97 H 0.5279 1.2213 -0.2030 0.041 Uiso 0.40 1 calc PR . 2 C96 C 0.4403(8) 1.0272(17) -0.1813(8) 0.045(5) Uiso 0.40 1 d P . 2 H96 H 0.4037 1.0426 -0.2188 0.054 Uiso 0.40 1 calc PR . 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 Zn1 0.02677(16) 0.02378(18) 0.02366(17) 0.0021(2) 0.0029(2) 0.00094(18) Fe1 0.0309(2) 0.0235(2) 0.0258(2) 0.0024(2) 0.0077(2) 0.0046(2) K1 0.0219(3) 0.0215(4) 0.0211(3) -0.0009(3) 0.0012(3) 0.0018(3) N1 0.0280(16) 0.070(2) 0.0292(17) -0.0105(18) 0.0061(13) 0.0103(17) N2 0.0409(18) 0.0319(19) 0.0257(17) 0.0024(14) -0.0014(13) 0.0137(14) N3 0.0214(15) 0.044(2) 0.068(2) -0.020(2) -0.0073(17) -0.0021(15) C1 0.0219(15) 0.0238(17) 0.0192(17) -0.0064(14) 0.0029(13) 0.0041(14) C2 0.0267(16) 0.0236(18) 0.0316(19) -0.0050(15) -0.0040(16) 0.0012(15) C3 0.0321(17) 0.0251(19) 0.0333(19) 0.007(2) 0.0045(17) 0.0046(14) C4 0.0322(18) 0.0158(19) 0.044(2) -0.0031(17) 0.0059(17) -0.0021(15) C5 0.0277(15) 0.0216(17) 0.0252(19) -0.0033(15) -0.0026(14) 0.0045(14) C11 0.0299(18) 0.036(2) 0.036(2) 0.0027(17) 0.0002(16) -0.0021(16) C12 0.041(2) 0.025(2) 0.034(2) 0.0042(16) -0.0055(16) 0.0037(17) C13 0.049(2) 0.074(3) 0.057(3) 0.023(2) -0.016(2) 0.009(2) C14 0.078(3) 0.041(3) 0.082(3) 0.005(2) -0.031(3) 0.000(3) C15 0.056(3) 0.068(3) 0.030(2) 0.000(2) -0.007(2) 0.010(2) C16 0.045(2) 0.086(3) 0.0202(17) -0.013(3) 0.0045(17) -0.015(2) C17 0.072(3) 0.078(4) 0.082(3) 0.005(3) 0.044(3) 0.015(3) C19 0.017(3) 0.035(4) 0.044(4) 0.004(4) 0.007(3) 0.002(3) C20 0.029(4) 0.053(6) 0.042(5) -0.006(4) -0.011(4) -0.008(4) C18A 0.040(6) 0.028(6) 0.039(6) -0.003(5) 0.027(4) 0.001(5) C19A 0.022(4) 0.031(5) 0.049(5) 0.006(5) 0.009(4) -0.004(4) C20A 0.047(7) 0.048(8) 0.033(8) -0.011(7) 0.019(7) -0.008(6) C21 0.048(3) 0.072(3) 0.089(4) 0.008(3) -0.021(2) -0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 C1 2.002(3) . ? Zn1 C12 2.027(3) . ? Zn1 C11 2.037(3) . ? Fe1 C99 1.989(8) . ? Fe1 C98 1.995(15) . ? Fe1 C7 1.996(9) . ? Fe1 C5 2.017(3) . ? Fe1 C4 2.028(3) . ? Fe1 C2 2.029(3) . ? Fe1 C3 2.030(3) . ? Fe1 C97 2.036(11) . ? Fe1 C8 2.042(8) . ? Fe1 C10 2.048(5) . ? Fe1 C9 2.051(7) . ? Fe1 C6 2.051(6) . ? K1 N3 2.860(3) . ? K1 N2 2.872(3) . ? K1 N1 2.885(3) . ? K1 C1 3.031(3) 1_545 ? K1 C5 3.094(3) 1_545 ? K1 C2 3.175(3) 1_545 ? K1 C4 3.320(3) 1_545 ? K1 C3 3.371(3) 1_545 ? N1 C18A 1.417(10) . ? N1 C17 1.440(4) . ? N1 C16 1.485(4) . ? N1 C18 1.575(9) . ? N2 C14 1.441(4) . ? N2 C15 1.451(4) . ? N2 C13 1.452(4) . ? N3 C20A 1.255(14) . ? N3 C21 1.421(4) . ? N3 C19 1.447(6) . ? N3 C20 1.584(7) . ? N3 C19A 1.648(9) . ? C1 C5 1.434(4) . ? C1 C2 1.444(4) . ? C1 K1 3.031(3) 1_565 ? C2 C3 1.414(4) . ? C2 K1 3.175(3) 1_565 ? C2 H2 0.950 . ? C3 C4 1.415(4) . ? C3 K1 3.371(3) 1_565 ? C3 H3 0.950 . ? C4 C5 1.415(4) . ? C4 K1 3.320(3) 1_565 ? C4 H4 0.950 . ? C5 K1 3.094(3) 1_565 ? C5 H5 0.950 . ? C10 C9 1.415(11) . ? C10 C6 1.425(8) . ? C10 H10 0.950 . ? C6 C7 1.473(11) . ? C6 H6 0.950 . ? C7 C8 1.347(12) . ? C7 H7 0.950 . ? C8 C9 1.492(11) . ? C8 H8 0.950 . ? C9 H9 0.950 . ? C11 H11A 0.980 . ? C11 H11B 0.980 . ? C11 H11C 0.980 . ? C12 H12A 0.980 . ? C12 H12B 0.980 . ? C12 H12C 0.980 . ? C13 H13A 0.980 . ? C13 H13B 0.980 . ? C13 H13C 0.980 . ? C14 H14A 0.980 . ? C14 H14B 0.980 . ? C14 H14C 0.980 . ? C15 C16 1.490(5) . ? C15 H15A 0.990 . ? C15 H15B 0.990 . ? C16 H16A 0.990 . ? C16 H16B 0.990 . ? C17 H17A 0.980 . ? C17 H17B 0.980 . ? C17 H17C 0.980 . ? C18 C19 1.498(10) . ? C18 H18A 0.990 . ? C18 H18B 0.990 . ? C19 H19A 0.990 . ? C19 H19B 0.990 . ? C20 H20A 0.980 . ? C20 H20B 0.980 . ? C20 H20C 0.980 . ? C18A C19A 1.502(12) . ? C18A H18C 0.990 . ? C18A H18D 0.990 . ? C19A H19C 0.990 . ? C19A H19D 0.990 . ? C20A H20D 0.980 . ? C20A H20E 0.980 . ? C20A H20F 0.980 . ? C21 H21A 0.980 . ? C21 H21B 0.980 . ? C21 H21C 0.980 . ? C99 C98 1.340(16) . ? C99 C95 1.408(13) . ? C99 H99 0.950 . ? C95 C96 1.385(17) . ? C95 H95 0.950 . ? C98 C97 1.236(17) . ? C98 H98 0.950 . ? C97 C96 1.509(18) . ? C97 H97 0.950 . ? C96 H96 0.950 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Zn1 C12 116.85(12) . . ? C1 Zn1 C11 115.73(12) . . ? C12 Zn1 C11 127.04(12) . . ? C99 Fe1 C98 39.3(4) . . ? C99 Fe1 C7 57.1(4) . . ? C98 Fe1 C7 62.7(5) . . ? C99 Fe1 C5 111.8(3) . . ? C98 Fe1 C5 119.1(5) . . ? C7 Fe1 C5 162.2(3) . . ? C99 Fe1 C4 137.1(4) . . ? C98 Fe1 C4 114.6(4) . . ? C7 Fe1 C4 156.7(3) . . ? C5 Fe1 C4 40.95(10) . . ? C99 Fe1 C2 142.8(3) . . ? C98 Fe1 C2 172.8(5) . . ? C7 Fe1 C2 111.8(3) . . ? C5 Fe1 C2 67.65(11) . . ? C4 Fe1 C2 68.35(12) . . ? C99 Fe1 C3 176.4(3) . . ? C98 Fe1 C3 137.2(5) . . ? C7 Fe1 C3 123.7(3) . . ? C5 Fe1 C3 68.47(13) . . ? C4 Fe1 C3 40.83(12) . . ? C2 Fe1 C3 40.77(10) . . ? C99 Fe1 C97 64.5(5) . . ? C98 Fe1 C97 35.7(5) . . ? C7 Fe1 C97 46.3(4) . . ? C5 Fe1 C97 145.8(3) . . ? C4 Fe1 C97 116.7(4) . . ? C2 Fe1 C97 137.2(4) . . ? C3 Fe1 C97 113.1(4) . . ? C99 Fe1 C8 69.8(4) . . ? C98 Fe1 C8 46.2(5) . . ? C7 Fe1 C8 39.0(3) . . ? C5 Fe1 C8 155.9(2) . . ? C4 Fe1 C8 120.9(2) . . ? C2 Fe1 C8 126.6(2) . . ? C3 Fe1 C8 108.4(2) . . ? C97 Fe1 C8 11.7(4) . . ? C99 Fe1 C10 18.1(3) . . ? C98 Fe1 C10 28.0(4) . . ? C7 Fe1 C10 69.0(3) . . ? C5 Fe1 C10 104.2(2) . . ? C4 Fe1 C10 120.6(2) . . ? C2 Fe1 C10 156.8(2) . . ? C3 Fe1 C10 158.6(2) . . ? C97 Fe1 C10 61.1(4) . . ? C8 Fe1 C10 69.6(3) . . ? C99 Fe1 C9 52.9(3) . . ? C98 Fe1 C9 13.6(5) . . ? C7 Fe1 C9 68.6(4) . . ? C5 Fe1 C9 117.5(2) . . ? C4 Fe1 C9 104.1(2) . . ? C2 Fe1 C9 162.8(2) . . ? C3 Fe1 C9 123.6(2) . . ? C97 Fe1 C9 31.1(4) . . ? C8 Fe1 C9 42.8(3) . . ? C10 Fe1 C9 40.4(3) . . ? C99 Fe1 C6 22.7(3) . . ? C98 Fe1 C6 56.1(4) . . ? C7 Fe1 C6 42.7(3) . . ? C5 Fe1 C6 121.59(18) . . ? C4 Fe1 C6 157.4(2) . . ? C2 Fe1 C6 123.7(2) . . ? C3 Fe1 C6 160.2(2) . . ? C97 Fe1 C6 69.2(4) . . ? C8 Fe1 C6 69.6(3) . . ? C10 Fe1 C6 40.7(2) . . ? C9 Fe1 C6 69.2(3) . . ? N3 K1 N2 100.13(10) . . ? N3 K1 N1 62.99(9) . . ? N2 K1 N1 63.29(8) . . ? N3 K1 C1 93.07(8) . 1_545 ? N2 K1 C1 92.88(8) . 1_545 ? N1 K1 C1 139.91(9) . 1_545 ? N3 K1 C5 119.98(9) . 1_545 ? N2 K1 C5 85.43(8) . 1_545 ? N1 K1 C5 147.86(9) . 1_545 ? C1 K1 C5 27.04(7) 1_545 1_545 ? N3 K1 C2 88.54(9) . 1_545 ? N2 K1 C2 119.66(8) . 1_545 ? N1 K1 C2 150.69(9) . 1_545 ? C1 K1 C2 26.79(7) 1_545 1_545 ? C5 K1 C2 42.09(7) 1_545 1_545 ? N3 K1 C4 129.54(9) . 1_545 ? N2 K1 C4 104.89(8) . 1_545 ? N1 K1 C4 165.79(8) . 1_545 ? C1 K1 C4 43.23(8) 1_545 1_545 ? C5 K1 C4 25.18(7) 1_545 1_545 ? C2 K1 C4 41.01(8) 1_545 1_545 ? N3 K1 C3 108.89(9) . 1_545 ? N2 K1 C3 126.29(8) . 1_545 ? N1 K1 C3 169.62(8) . 1_545 ? C1 K1 C3 42.79(7) 1_545 1_545 ? C5 K1 C3 40.96(7) 1_545 1_545 ? C2 K1 C3 24.71(6) 1_545 1_545 ? C4 K1 C3 24.41(7) 1_545 1_545 ? C18A N1 C17 97.3(5) . . ? C18A N1 C16 120.0(5) . . ? C17 N1 C16 111.5(3) . . ? C18A N1 C18 21.7(5) . . ? C17 N1 C18 118.2(4) . . ? C16 N1 C18 104.0(4) . . ? C18A N1 K1 112.3(4) . . ? C17 N1 K1 99.8(2) . . ? C16 N1 K1 112.9(2) . . ? C18 N1 K1 110.7(4) . . ? C14 N2 C15 114.0(3) . . ? C14 N2 C13 108.5(3) . . ? C15 N2 C13 107.3(3) . . ? C14 N2 K1 107.9(2) . . ? C15 N2 K1 108.38(18) . . ? C13 N2 K1 110.9(2) . . ? C20A N3 C21 117.1(7) . . ? C20A N3 C19 74.6(6) . . ? C21 N3 C19 126.3(4) . . ? C20A N3 C20 29.3(6) . . ? C21 N3 C20 102.3(4) . . ? C19 N3 C20 103.6(4) . . ? C20A N3 C19A 110.4(6) . . ? C21 N3 C19A 91.1(4) . . ? C19 N3 C19A 41.3(3) . . ? C20 N3 C19A 138.7(4) . . ? C20A N3 K1 115.6(6) . . ? C21 N3 K1 110.8(2) . . ? C19 N3 K1 108.3(3) . . ? C20 N3 K1 102.4(3) . . ? C19A N3 K1 109.0(3) . . ? C5 C1 C2 103.0(3) . . ? C5 C1 Zn1 126.1(2) . . ? C2 C1 Zn1 126.3(2) . . ? C5 C1 Fe1 67.42(15) . . ? C2 C1 Fe1 67.78(16) . . ? Zn1 C1 Fe1 109.24(14) . . ? C5 C1 K1 78.95(16) . 1_565 ? C2 C1 K1 82.17(17) . 1_565 ? Zn1 C1 K1 123.76(12) . 1_565 ? Fe1 C1 K1 126.93(13) . 1_565 ? C3 C2 C1 111.1(3) . . ? C3 C2 Fe1 69.65(16) . . ? C1 C2 Fe1 71.00(16) . . ? C3 C2 K1 85.44(18) . 1_565 ? C1 C2 K1 71.05(16) . 1_565 ? Fe1 C2 K1 122.03(12) . 1_565 ? C3 C2 H2 124.5 . . ? C1 C2 H2 124.5 . . ? Fe1 C2 H2 126.5 . . ? K1 C2 H2 110.9 1_565 . ? C2 C3 C4 107.3(3) . . ? C2 C3 Fe1 69.58(16) . . ? C4 C3 Fe1 69.53(17) . . ? C2 C3 K1 69.85(17) . 1_565 ? C4 C3 K1 75.78(18) . 1_565 ? Fe1 C3 K1 113.90(13) . 1_565 ? C2 C3 H3 126.3 . . ? C4 C3 H3 126.3 . . ? Fe1 C3 H3 126.1 . . ? K1 C3 H3 119.9 1_565 . ? C5 C4 C3 107.1(3) . . ? C5 C4 Fe1 69.09(16) . . ? C3 C4 Fe1 69.64(17) . . ? C5 C4 K1 68.46(16) . 1_565 ? C3 C4 K1 79.81(18) . 1_565 ? Fe1 C4 K1 115.94(12) . 1_565 ? C5 C4 H4 126.5 . . ? C3 C4 H4 126.5 . . ? Fe1 C4 H4 126.4 . . ? K1 C4 H4 117.2 1_565 . ? C4 C5 C1 111.5(3) . . ? C4 C5 Fe1 69.96(17) . . ? C1 C5 Fe1 71.57(16) . . ? C4 C5 K1 86.36(17) . 1_565 ? C1 C5 K1 74.01(15) . 1_565 ? Fe1 C5 K1 126.27(12) . 1_565 ? C4 C5 H5 124.2 . . ? C1 C5 H5 124.2 . . ? Fe1 C5 H5 125.8 . . ? K1 C5 H5 107.5 1_565 . ? C9 C10 C6 110.1(5) . . ? C9 C10 Fe1 69.9(3) . . ? C6 C10 Fe1 69.8(3) . . ? C9 C10 H10 124.9 . . ? C6 C10 H10 124.9 . . ? Fe1 C10 H10 127.0 . . ? C10 C6 C7 104.4(6) . . ? C10 C6 Fe1 69.5(3) . . ? C7 C6 Fe1 66.7(4) . . ? C10 C6 H6 127.8 . . ? C7 C6 H6 127.8 . . ? Fe1 C6 H6 127.5 . . ? C8 C7 C6 111.8(8) . . ? C8 C7 Fe1 72.4(5) . . ? C6 C7 Fe1 70.7(4) . . ? C8 C7 H7 124.1 . . ? C6 C7 H7 124.1 . . ? Fe1 C7 H7 124.4 . . ? C7 C8 C9 106.8(7) . . ? C7 C8 Fe1 68.7(5) . . ? C9 C8 Fe1 68.9(4) . . ? C7 C8 H8 126.6 . . ? C9 C8 H8 126.6 . . ? Fe1 C8 H8 127.4 . . ? C10 C9 C8 106.7(6) . . ? C10 C9 Fe1 69.7(4) . . ? C8 C9 Fe1 68.3(4) . . ? C10 C9 H9 126.6 . . ? C8 C9 H9 126.6 . . ? Fe1 C9 H9 126.9 . . ? Zn1 C11 H11A 109.5 . . ? Zn1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Zn1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Zn1 C12 H12A 109.5 . . ? Zn1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Zn1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N2 C13 H13A 109.5 . . ? N2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N2 C14 H14A 109.5 . . ? N2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N2 C15 C16 115.1(3) . . ? N2 C15 H15A 108.5 . . ? C16 C15 H15A 108.5 . . ? N2 C15 H15B 108.5 . . ? C16 C15 H15B 108.5 . . ? H15A C15 H15B 107.5 . . ? N1 C16 C15 113.7(3) . . ? N1 C16 H16A 108.8 . . ? C15 C16 H16A 108.8 . . ? N1 C16 H16B 108.8 . . ? C15 C16 H16B 108.8 . . ? H16A C16 H16B 107.7 . . ? N1 C17 H17A 109.5 . . ? N1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 N1 112.9(6) . . ? C19 C18 H18A 109.0 . . ? N1 C18 H18A 109.0 . . ? C19 C18 H18B 109.0 . . ? N1 C18 H18B 109.0 . . ? H18A C18 H18B 107.8 . . ? N3 C19 C18 108.9(6) . . ? N3 C19 H19A 109.9 . . ? C18 C19 H19A 109.9 . . ? N3 C19 H19B 109.9 . . ? C18 C19 H19B 109.9 . . ? H19A C19 H19B 108.3 . . ? N3 C20 H20A 109.5 . . ? N3 C20 H20B 109.5 . . ? N3 C20 H20C 109.5 . . ? N1 C18A C19A 107.4(7) . . ? N1 C18A H18C 110.2 . . ? C19A C18A H18C 110.2 . . ? N1 C18A H18D 110.2 . . ? C19A C18A H18D 110.2 . . ? H18C C18A H18D 108.5 . . ? C18A C19A N3 109.4(6) . . ? C18A C19A H19C 109.8 . . ? N3 C19A H19C 109.8 . . ? C18A C19A H19D 109.8 . . ? N3 C19A H19D 109.8 . . ? H19C C19A H19D 108.2 . . ? N3 C20A H20D 109.5 . . ? N3 C20A H20E 109.5 . . ? H20D C20A H20E 109.5 . . ? N3 C20A H20F 109.5 . . ? H20D C20A H20F 109.5 . . ? H20E C20A H20F 109.5 . . ? N3 C21 H21A 109.5 . . ? N3 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N3 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C98 C99 C95 108.5(11) . . ? C98 C99 Fe1 70.6(7) . . ? C95 C99 Fe1 73.0(5) . . ? C98 C99 H99 125.7 . . ? C95 C99 H99 125.7 . . ? Fe1 C99 H99 122.3 . . ? C96 C95 C99 106.4(9) . . ? C96 C95 Fe1 71.5(7) . . ? C99 C95 Fe1 66.5(5) . . ? C96 C95 H95 126.8 . . ? C99 C95 H95 126.8 . . ? Fe1 C95 H95 126.7 . . ? C97 C98 C99 113.1(15) . . ? C97 C98 Fe1 74.0(9) . . ? C99 C98 Fe1 70.1(7) . . ? C97 C98 H98 123.4 . . ? C99 C98 H98 123.4 . . ? Fe1 C98 H98 124.0 . . ? C98 C97 C96 108.0(12) . . ? C98 C97 Fe1 70.3(9) . . ? C96 C97 Fe1 70.8(7) . . ? C98 C97 H97 126.0 . . ? C96 C97 H97 126.0 . . ? Fe1 C97 H97 124.5 . . ? C95 C96 C97 104.0(10) . . ? C95 C96 Fe1 69.7(6) . . ? C97 C96 Fe1 66.4(6) . . ? C95 C96 H96 128.0 . . ? C97 C96 H96 128.0 . . ? Fe1 C96 H96 127.3 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.519 _refine_diff_density_min -0.350 _refine_diff_density_rms 0.066 #===END #------------------------------------------------------------------- #---------------COMPOUND 3------------------------------------------ #-------------------------------------------------------------------- data_jkben4 _database_code_depnum_ccdc_archive 'CCDC 731816' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H76 K2 N6 Ru2 Zn2' _chemical_formula_sum 'C42 H76 K2 N6 Ru2 Zn2' _chemical_formula_weight 1076.17 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 '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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8165(3) _cell_length_b 11.9380(4) _cell_length_c 12.9284(5) _cell_angle_alpha 114.673(4) _cell_angle_beta 95.400(3) _cell_angle_gamma 99.969(3) _cell_volume 1196.61(7) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 14400 _cell_measurement_theta_min 2.68 _cell_measurement_theta_max 30.35 _exptl_crystal_description chip _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.493 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 556 _exptl_absorpt_coefficient_mu 1.817 _exptl_absorpt_correction_T_min 0.848 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET) (compiled Apr 21 2008,18:23:10) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini S' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21909 _diffrn_reflns_av_R_equivalents 0.0246 _diffrn_reflns_av_sigmaI/netI 0.0276 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_theta_max 30.45 _reflns_number_total 6756 _reflns_number_gt 5759 _reflns_threshold_expression I>2\s(I) _computing_data_collection CrysAlisPro _computing_cell_refinement CrysAlisPro _computing_data_reduction CrysAlisPro _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material SHELXL97 _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^)+(0.0269P)^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 6756 _refine_ls_number_parameters 284 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0289 _refine_ls_R_factor_gt 0.0213 _refine_ls_wR_factor_ref 0.0485 _refine_ls_wR_factor_gt 0.0472 _refine_ls_goodness_of_fit_ref 0.990 _refine_ls_restrained_S_all 0.990 _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 K1 K 1.02823(3) 0.71798(3) 0.13700(3) 0.01918(7) Uani 1 1 d . . . Ru1 Ru 1.278091(12) 0.520738(10) -0.348877(10) 0.01534(4) Uani 1 1 d . . . Zn1 Zn 1.086532(19) 0.556942(16) -0.143984(14) 0.01929(4) Uani 1 1 d . . . N6 N 1.29409(13) 0.78938(12) 0.31277(11) 0.0203(3) Uani 1 1 d . . . N5 N 1.24100(14) 0.96571(12) 0.20846(11) 0.0219(3) Uani 1 1 d . . . C61 C 1.41910(16) 0.87725(15) 0.29874(14) 0.0245(3) Uani 1 1 d . . . H61A H 1.4523 0.8318 0.2242 0.029 Uiso 1 1 calc R . . H61B H 1.5104 0.9038 0.3615 0.029 Uiso 1 1 calc R . . N4 N 0.89060(15) 0.92764(12) 0.18835(12) 0.0254(3) Uani 1 1 d . . . C18 C 1.08819(15) 0.41644(13) -0.30017(12) 0.0181(3) Uani 1 1 d . . . C15 C 1.12308(16) 0.35617(14) -0.49328(13) 0.0205(3) Uani 1 1 d . . . H15A H 1.1093 0.3446 -0.5711 0.025 Uiso 1 1 calc R . . C63 C 1.24691(19) 0.84756(17) 0.42486(14) 0.0308(4) Uani 1 1 d . . . H63A H 1.2032 0.9194 0.4299 0.046 Uiso 1 1 calc R . . H63B H 1.3384 0.8775 0.4869 0.046 Uiso 1 1 calc R . . H63C H 1.1675 0.7848 0.4330 0.046 Uiso 1 1 calc R . . C17 C 1.21394(16) 0.35173(13) -0.32328(13) 0.0194(3) Uani 1 1 d . . . H17A H 1.2741 0.3355 -0.2683 0.023 Uiso 1 1 calc R . . C3 C 1.2373(2) 0.55650(18) -0.01490(15) 0.0279(4) Uani 1 1 d . . . C19 C 1.03437(15) 0.41769(14) -0.40837(13) 0.0187(3) Uani 1 1 d . . . H19A H 0.9515 0.4543 -0.4214 0.022 Uiso 1 1 calc R . . C52 C 1.37317(17) 0.99478(15) 0.30085(14) 0.0264(3) Uani 1 1 d . . . H52A H 1.3449 1.0427 0.3768 0.032 Uiso 1 1 calc R . . H52B H 1.4647 1.0498 0.2929 0.032 Uiso 1 1 calc R . . C62 C 1.34903(18) 0.67686(16) 0.30327(15) 0.0284(4) Uani 1 1 d . . . H62A H 1.3809 0.6369 0.2282 0.043 Uiso 1 1 calc R . . H62B H 1.2642 0.6165 0.3097 0.043 Uiso 1 1 calc R . . H62C H 1.4387 0.7020 0.3656 0.043 Uiso 1 1 calc R . . C2 C 0.93864(19) 0.67181(16) -0.13002(15) 0.0262(3) Uani 1 1 d . . . C41 C 0.99250(19) 1.02763(16) 0.17283(15) 0.0291(4) Uani 1 1 d . . . H41A H 0.9458 1.1023 0.1971 0.035 Uiso 1 1 calc R . . H41B H 0.9959 0.9974 0.0894 0.035 Uiso 1 1 calc R . . C16 C 1.23567(16) 0.31543(13) -0.43984(13) 0.0210(3) Uani 1 1 d . . . H16A H 1.3114 0.2721 -0.4752 0.025 Uiso 1 1 calc R . . C51 C 1.15818(19) 1.06884(15) 0.23951(16) 0.0292(4) Uani 1 1 d . . . H51A H 1.2177 1.1376 0.2252 0.035 Uiso 1 1 calc R . . H51B H 1.1556 1.1038 0.3234 0.035 Uiso 1 1 calc R . . C53 C 1.2972(2) 0.94271(18) 0.10003(15) 0.0288(4) Uani 1 1 d . . . C12 C 1.3511(2) 0.71908(15) -0.22218(15) 0.0327(4) Uani 1 1 d . . . H12A H 1.3007 0.7561 -0.1586 0.039 Uiso 1 1 calc R . . C11 C 1.4782(2) 0.66151(17) -0.22241(17) 0.0380(5) Uani 1 1 d . . . H11A H 1.5280 0.6525 -0.1588 0.046 Uiso 1 1 calc R . . C43 C 0.8642(2) 0.97020(18) 0.30697(16) 0.0372(4) Uani 1 1 d . . . H43A H 0.9645 0.9947 0.3596 0.056 Uiso 1 1 calc R . . H43B H 0.7937 0.9013 0.3134 0.056 Uiso 1 1 calc R . . H43C H 0.8168 1.0433 0.3278 0.056 Uiso 1 1 calc R . . C42 C 0.7395(2) 0.88705(19) 0.10980(18) 0.0409(5) Uani 1 1 d . . . H42A H 0.6741 0.8144 0.1141 0.061 Uiso 1 1 calc R . . H42B H 0.7570 0.8625 0.0303 0.061 Uiso 1 1 calc R . . H42C H 0.6864 0.9571 0.1326 0.061 Uiso 1 1 calc R . . C10 C 1.51826(19) 0.62007(17) -0.33232(19) 0.0425(5) Uani 1 1 d . . . H10A H 1.6002 0.5784 -0.3562 0.051 Uiso 1 1 calc R . . C13 C 1.3125(2) 0.71165(16) -0.33362(17) 0.0343(4) Uani 1 1 d . . . H13A H 1.2309 0.7423 -0.3586 0.041 Uiso 1 1 calc R . . C14 C 1.4163(2) 0.65080(17) -0.40119(16) 0.0401(5) Uani 1 1 d . . . H14A H 1.4173 0.6335 -0.4798 0.048 Uiso 1 1 calc R . . H2A H 0.905(2) 0.6703(19) -0.2017(19) 0.046(6) Uiso 1 1 d . . . H2B H 0.841(2) 0.6421(19) -0.1103(18) 0.043(6) Uiso 1 1 d . . . H2C H 0.982(2) 0.7623(18) -0.0736(17) 0.039(5) Uiso 1 1 d . . . H3A H 1.302(2) 0.509(2) -0.0420(19) 0.050(6) Uiso 1 1 d . . . H3B H 1.198(2) 0.5254(18) 0.0349(18) 0.043(6) Uiso 1 1 d . . . H3C H 1.308(2) 0.6414(19) 0.0342(17) 0.037(5) Uiso 1 1 d . . . H53A H 1.347(2) 0.8736(17) 0.0756(16) 0.033(5) Uiso 1 1 d . . . H53B H 1.375(2) 1.0181(17) 0.1062(15) 0.033(5) Uiso 1 1 d . . . H53C H 1.211(2) 0.9205(16) 0.0395(15) 0.027(5) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 K1 0.01990(13) 0.01502(15) 0.01999(15) 0.00644(13) 0.00103(11) 0.00248(11) Ru1 0.01513(5) 0.01395(6) 0.01450(6) 0.00491(5) 0.00279(4) 0.00095(4) Zn1 0.02348(8) 0.01743(9) 0.01738(9) 0.00813(7) 0.00469(7) 0.00428(7) N6 0.0186(5) 0.0211(7) 0.0173(6) 0.0075(5) 0.0003(5) -0.0008(5) N5 0.0234(6) 0.0182(6) 0.0221(6) 0.0086(5) 0.0032(5) 0.0012(5) C61 0.0182(6) 0.0298(9) 0.0221(8) 0.0118(7) 0.0004(6) -0.0020(6) N4 0.0265(6) 0.0230(7) 0.0310(7) 0.0132(6) 0.0127(5) 0.0089(5) C18 0.0164(6) 0.0162(7) 0.0204(7) 0.0086(6) 0.0032(5) -0.0004(5) C15 0.0224(7) 0.0170(7) 0.0162(7) 0.0045(6) 0.0007(5) -0.0007(6) C63 0.0320(8) 0.0307(9) 0.0235(8) 0.0101(7) 0.0065(7) -0.0035(7) C17 0.0220(6) 0.0152(7) 0.0204(7) 0.0086(6) 0.0011(5) 0.0028(5) C3 0.0330(8) 0.0307(10) 0.0202(8) 0.0099(7) 0.0046(7) 0.0117(8) C19 0.0153(6) 0.0168(7) 0.0212(7) 0.0075(6) 0.0011(5) 0.0007(5) C52 0.0250(7) 0.0238(8) 0.0231(8) 0.0089(7) 0.0002(6) -0.0056(6) C62 0.0259(7) 0.0311(9) 0.0281(8) 0.0153(8) -0.0021(6) 0.0048(7) C2 0.0301(8) 0.0239(9) 0.0249(8) 0.0104(7) 0.0037(7) 0.0085(7) C41 0.0365(8) 0.0266(9) 0.0329(9) 0.0177(8) 0.0138(7) 0.0127(7) C16 0.0215(6) 0.0148(7) 0.0216(7) 0.0037(6) 0.0039(6) 0.0034(6) C51 0.0353(8) 0.0164(8) 0.0336(9) 0.0097(7) 0.0086(7) 0.0031(6) C53 0.0291(8) 0.0318(10) 0.0256(8) 0.0139(8) 0.0049(7) 0.0043(7) C12 0.0359(8) 0.0169(8) 0.0298(9) -0.0010(7) 0.0146(7) -0.0072(7) C11 0.0329(9) 0.0276(9) 0.0402(11) 0.0148(8) -0.0156(8) -0.0132(7) C43 0.0468(10) 0.0395(11) 0.0378(10) 0.0232(9) 0.0211(8) 0.0180(9) C42 0.0294(8) 0.0463(12) 0.0453(11) 0.0160(10) 0.0110(8) 0.0139(8) C10 0.0213(8) 0.0242(9) 0.0671(14) 0.0071(9) 0.0175(8) -0.0022(7) C13 0.0337(9) 0.0196(8) 0.0481(11) 0.0183(8) -0.0016(8) -0.0014(7) C14 0.0551(11) 0.0269(9) 0.0269(9) 0.0084(8) 0.0157(8) -0.0135(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag K1 N4 2.8274(13) . ? K1 N6 2.8413(12) . ? K1 N5 2.9310(12) . ? K1 C3 3.1179(19) . ? K1 C2 3.2546(18) . ? K1 C18 3.2775(15) 2_765 ? K1 C3 3.3226(19) 2_765 ? K1 C53 3.4827(18) . ? K1 H2C 2.988(19) . ? K1 H3B 2.88(2) . ? K1 H3C 3.012(19) . ? Ru1 C17 2.1674(14) . ? Ru1 C13 2.1678(16) . ? Ru1 C19 2.1693(13) . ? Ru1 C16 2.1733(14) . ? Ru1 C14 2.1749(17) . ? Ru1 C12 2.1771(16) . ? Ru1 C15 2.1774(14) . ? Ru1 C11 2.1789(15) . ? Ru1 C10 2.1838(16) . ? Ru1 C18 2.2093(14) . ? Zn1 C2 2.0174(16) . ? Zn1 C18 2.0192(15) . ? Zn1 C3 2.0358(17) . ? N6 C63 1.459(2) . ? N6 C61 1.4643(19) . ? N6 C62 1.467(2) . ? N5 C53 1.464(2) . ? N5 C52 1.4687(19) . ? N5 C51 1.471(2) . ? C61 C52 1.517(2) . ? C61 H61A 0.990 . ? C61 H61B 0.990 . ? N4 C43 1.456(2) . ? N4 C41 1.461(2) . ? N4 C42 1.467(2) . ? C18 C19 1.441(2) . ? C18 C17 1.443(2) . ? C18 K1 3.2775(15) 2_765 ? C15 C16 1.420(2) . ? C15 C19 1.430(2) . ? C15 H15A 0.950 . ? C63 H63A 0.980 . ? C63 H63B 0.980 . ? C63 H63C 0.980 . ? C17 C16 1.426(2) . ? C17 H17A 0.950 . ? C3 K1 3.3226(19) 2_765 ? C3 H3A 0.87(2) . ? C3 H3B 0.93(2) . ? C3 H3C 0.994(19) . ? C19 H19A 0.950 . ? C52 H52A 0.990 . ? C52 H52B 0.990 . ? C62 H62A 0.980 . ? C62 H62B 0.980 . ? C62 H62C 0.980 . ? C2 H2A 0.94(2) . ? C2 H2B 0.97(2) . ? C2 H2C 0.995(19) . ? C41 C51 1.510(2) . ? C41 H41A 0.990 . ? C41 H41B 0.990 . ? C16 H16A 0.950 . ? C51 H51A 0.990 . ? C51 H51B 0.990 . ? C53 H53A 0.955(19) . ? C53 H53B 1.002(18) . ? C53 H53C 0.951(17) . ? C12 C13 1.411(3) . ? C12 C11 1.413(3) . ? C12 H12A 0.950 . ? C11 C10 1.399(3) . ? C11 H11A 0.950 . ? C43 H43A 0.980 . ? C43 H43B 0.980 . ? C43 H43C 0.980 . ? C42 H42A 0.980 . ? C42 H42B 0.980 . ? C42 H42C 0.980 . ? C10 C14 1.404(3) . ? C10 H10A 0.950 . ? C13 C14 1.407(3) . ? C13 H13A 0.950 . ? C14 H14A 0.950 . ? 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 N4 K1 N6 108.40(4) . . ? N4 K1 N5 63.08(4) . . ? N6 K1 N5 62.84(4) . . ? N4 K1 C3 146.16(5) . . ? N6 K1 C3 81.62(4) . . ? N5 K1 C3 96.41(5) . . ? N4 K1 C2 84.21(4) . . ? N6 K1 C2 140.58(4) . . ? N5 K1 C2 93.40(4) . . ? C3 K1 C2 69.70(4) . . ? N4 K1 C18 107.05(4) . 2_765 ? N6 K1 C18 75.40(3) . 2_765 ? N5 K1 C18 128.23(4) . 2_765 ? C3 K1 C18 106.75(4) . 2_765 ? C2 K1 C18 137.85(4) . 2_765 ? N4 K1 C3 112.26(4) . 2_765 ? N6 K1 C3 126.94(4) . 2_765 ? N5 K1 C3 169.76(4) . 2_765 ? C3 K1 C3 83.07(5) . 2_765 ? C2 K1 C3 76.80(4) . 2_765 ? C18 K1 C3 61.24(4) 2_765 2_765 ? N4 K1 C53 74.63(4) . . ? N6 K1 C53 75.11(4) . . ? N5 K1 C53 24.50(4) . . ? C3 K1 C53 77.18(5) . . ? C2 K1 C53 72.64(4) . . ? C18 K1 C53 149.26(4) 2_765 . ? C3 K1 C53 147.82(4) 2_765 . ? N4 K1 H2C 71.2(4) . . ? N6 K1 H2C 132.2(4) . . ? N5 K1 H2C 76.9(4) . . ? C3 K1 H2C 78.2(4) . . ? C2 K1 H2C 17.7(4) . . ? C18 K1 H2C 152.2(4) 2_765 . ? C3 K1 H2C 93.0(4) 2_765 . ? C53 K1 H2C 58.3(4) . . ? N4 K1 H3B 163.4(4) . . ? N6 K1 H3B 76.7(4) . . ? N5 K1 H3B 108.0(4) . . ? C3 K1 H3B 17.3(4) . . ? C2 K1 H3B 82.4(4) . . ? C18 K1 H3B 89.5(4) 2_765 . ? C3 K1 H3B 74.0(4) 2_765 . ? C53 K1 H3B 92.0(4) . . ? H2C K1 H3B 93.5(5) . . ? N4 K1 H3C 135.6(4) . . ? N6 K1 H3C 68.8(4) . . ? N5 K1 H3C 78.6(4) . . ? C3 K1 H3C 18.6(4) . . ? C2 K1 H3C 76.2(4) . . ? C18 K1 H3C 114.2(3) 2_765 . ? C3 K1 H3C 101.5(4) 2_765 . ? C53 K1 H3C 61.7(4) . . ? H2C K1 H3C 79.3(5) . . ? H3B K1 H3C 30.4(5) . . ? C17 Ru1 C13 164.30(7) . . ? C17 Ru1 C19 63.20(5) . . ? C13 Ru1 C19 112.51(6) . . ? C17 Ru1 C16 38.36(6) . . ? C13 Ru1 C16 155.70(7) . . ? C19 Ru1 C16 63.87(5) . . ? C17 Ru1 C14 156.60(7) . . ? C13 Ru1 C14 37.81(7) . . ? C19 Ru1 C14 130.58(7) . . ? C16 Ru1 C14 124.35(7) . . ? C17 Ru1 C12 129.84(6) . . ? C13 Ru1 C12 37.89(7) . . ? C19 Ru1 C12 122.80(6) . . ? C16 Ru1 C12 165.31(6) . . ? C14 Ru1 C12 63.13(7) . . ? C17 Ru1 C15 63.69(6) . . ? C13 Ru1 C15 123.45(6) . . ? C19 Ru1 C15 38.40(5) . . ? C16 Ru1 C15 38.11(5) . . ? C14 Ru1 C15 113.51(6) . . ? C12 Ru1 C15 155.05(6) . . ? C17 Ru1 C11 113.59(6) . . ? C13 Ru1 C11 63.19(7) . . ? C19 Ru1 C11 154.84(7) . . ? C16 Ru1 C11 130.79(6) . . ? C14 Ru1 C11 62.82(7) . . ? C12 Ru1 C11 37.84(7) . . ? C15 Ru1 C11 165.69(7) . . ? C17 Ru1 C10 124.81(7) . . ? C13 Ru1 C10 63.09(7) . . ? C19 Ru1 C10 165.87(7) . . ? C16 Ru1 C10 114.02(6) . . ? C14 Ru1 C10 37.58(8) . . ? C12 Ru1 C10 62.99(7) . . ? C15 Ru1 C10 131.06(7) . . ? C11 Ru1 C10 37.40(8) . . ? C17 Ru1 C18 38.48(5) . . ? C13 Ru1 C18 128.46(6) . . ? C19 Ru1 C18 38.42(5) . . ? C16 Ru1 C18 65.17(5) . . ? C14 Ru1 C18 164.28(7) . . ? C12 Ru1 C18 110.96(6) . . ? C15 Ru1 C18 65.07(5) . . ? C11 Ru1 C18 122.53(7) . . ? C10 Ru1 C18 155.17(7) . . ? C2 Zn1 C18 119.91(6) . . ? C2 Zn1 C3 128.00(7) . . ? C18 Zn1 C3 112.02(7) . . ? C63 N6 C61 111.68(12) . . ? C63 N6 C62 108.80(13) . . ? C61 N6 C62 109.34(12) . . ? C63 N6 K1 108.05(9) . . ? C61 N6 K1 108.95(8) . . ? C62 N6 K1 110.00(8) . . ? C53 N5 C52 109.83(13) . . ? C53 N5 C51 110.42(13) . . ? C52 N5 C51 111.24(13) . . ? C53 N5 K1 99.37(9) . . ? C52 N5 K1 113.05(9) . . ? C51 N5 K1 112.33(9) . . ? N6 C61 C52 114.22(12) . . ? N6 C61 H61A 108.7 . . ? C52 C61 H61A 108.7 . . ? N6 C61 H61B 108.7 . . ? C52 C61 H61B 108.7 . . ? H61A C61 H61B 107.6 . . ? C43 N4 C41 111.98(14) . . ? C43 N4 C42 109.14(13) . . ? C41 N4 C42 108.92(14) . . ? C43 N4 K1 107.32(10) . . ? C41 N4 K1 110.19(9) . . ? C42 N4 K1 109.26(10) . . ? C19 C18 C17 103.99(12) . . ? C19 C18 Zn1 123.34(11) . . ? C17 C18 Zn1 123.08(10) . . ? C19 C18 Ru1 69.29(8) . . ? C17 C18 Ru1 69.19(8) . . ? Zn1 C18 Ru1 97.97(6) . . ? C19 C18 K1 139.80(9) . 2_765 ? C17 C18 K1 91.54(9) . 2_765 ? Zn1 C18 K1 72.86(4) . 2_765 ? Ru1 C18 K1 149.99(6) . 2_765 ? C16 C15 C19 107.42(13) . . ? C16 C15 Ru1 70.79(8) . . ? C19 C15 Ru1 70.49(8) . . ? C16 C15 H15A 126.3 . . ? C19 C15 H15A 126.3 . . ? Ru1 C15 H15A 124.1 . . ? N6 C63 H63A 109.5 . . ? N6 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? N6 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C16 C17 C18 110.75(12) . . ? C16 C17 Ru1 71.05(8) . . ? C18 C17 Ru1 72.33(8) . . ? C16 C17 H17A 124.6 . . ? C18 C17 H17A 124.6 . . ? Ru1 C17 H17A 123.6 . . ? Zn1 C3 K1 81.64(6) . . ? Zn1 C3 K1 71.62(5) . 2_765 ? K1 C3 K1 96.93(5) . 2_765 ? Zn1 C3 H3A 111.8(14) . . ? K1 C3 H3A 165.7(14) . . ? K1 C3 H3A 83.4(14) 2_765 . ? Zn1 C3 H3B 119.7(12) . . ? K1 C3 H3B 66.9(12) . . ? K1 C3 H3B 63.4(12) 2_765 . ? H3A C3 H3B 100.9(18) . . ? Zn1 C3 H3C 112.3(10) . . ? K1 C3 H3C 74.7(11) . . ? K1 C3 H3C 169.7(11) 2_765 . ? H3A C3 H3C 103.3(17) . . ? H3B C3 H3C 107.1(16) . . ? C15 C19 C18 110.54(13) . . ? C15 C19 Ru1 71.10(8) . . ? C18 C19 Ru1 72.29(7) . . ? C15 C19 H19A 124.7 . . ? C18 C19 H19A 124.7 . . ? Ru1 C19 H19A 123.5 . . ? N5 C52 C61 113.05(12) . . ? N5 C52 H52A 109.0 . . ? C61 C52 H52A 109.0 . . ? N5 C52 H52B 109.0 . . ? C61 C52 H52B 109.0 . . ? H52A C52 H52B 107.8 . . ? N6 C62 H62A 109.5 . . ? N6 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? N6 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? Zn1 C2 K1 78.39(5) . . ? Zn1 C2 H2A 111.2(13) . . ? K1 C2 H2A 170.2(13) . . ? Zn1 C2 H2B 112.0(11) . . ? K1 C2 H2B 74.5(12) . . ? H2A C2 H2B 102.5(16) . . ? Zn1 C2 H2C 115.2(10) . . ? K1 C2 H2C 65.8(11) . . ? H2A C2 H2C 107.1(16) . . ? H2B C2 H2C 107.8(16) . . ? N4 C41 C51 114.50(13) . . ? N4 C41 H41A 108.6 . . ? C51 C41 H41A 108.6 . . ? N4 C41 H41B 108.6 . . ? C51 C41 H41B 108.6 . . ? H41A C41 H41B 107.6 . . ? C15 C16 C17 107.30(13) . . ? C15 C16 Ru1 71.10(8) . . ? C17 C16 Ru1 70.60(8) . . ? C15 C16 H16A 126.4 . . ? C17 C16 H16A 126.4 . . ? Ru1 C16 H16A 123.6 . . ? N5 C51 C41 113.50(13) . . ? N5 C51 H51A 108.9 . . ? C41 C51 H51A 108.9 . . ? N5 C51 H51B 108.9 . . ? C41 C51 H51B 108.9 . . ? H51A C51 H51B 107.7 . . ? N5 C53 K1 56.14(8) . . ? N5 C53 H53A 112.5(11) . . ? K1 C53 H53A 79.6(11) . . ? N5 C53 H53B 112.4(10) . . ? K1 C53 H53B 168.5(10) . . ? H53A C53 H53B 106.5(15) . . ? N5 C53 H53C 109.8(11) . . ? K1 C53 H53C 77.5(10) . . ? H53A C53 H53C 106.2(15) . . ? H53B C53 H53C 109.2(14) . . ? C13 C12 C11 107.55(16) . . ? C13 C12 Ru1 70.70(9) . . ? C11 C12 Ru1 71.15(9) . . ? C13 C12 H12A 126.2 . . ? C11 C12 H12A 126.2 . . ? Ru1 C12 H12A 123.6 . . ? C10 C11 C12 108.27(16) . . ? C10 C11 Ru1 71.49(10) . . ? C12 C11 Ru1 71.01(9) . . ? C10 C11 H11A 125.9 . . ? C12 C11 H11A 125.9 . . ? Ru1 C11 H11A 123.3 . . ? N4 C43 H43A 109.5 . . ? N4 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? N4 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? N4 C42 H42A 109.5 . . ? N4 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N4 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C11 C10 C14 108.11(16) . . ? C11 C10 Ru1 71.11(9) . . ? C14 C10 Ru1 70.87(9) . . ? C11 C10 H10A 125.9 . . ? C14 C10 H10A 125.9 . . ? Ru1 C10 H10A 123.7 . . ? C14 C13 C12 107.90(16) . . ? C14 C13 Ru1 71.37(10) . . ? C12 C13 Ru1 71.41(10) . . ? C14 C13 H13A 126.1 . . ? C12 C13 H13A 126.1 . . ? Ru1 C13 H13A 122.8 . . ? C10 C14 C13 108.16(16) . . ? C10 C14 Ru1 71.55(10) . . ? C13 C14 Ru1 70.82(10) . . ? C10 C14 H14A 125.9 . . ? C13 C14 H14A 125.9 . . ? Ru1 C14 H14A 123.3 . . ? _diffrn_measured_fraction_theta_max 0.929 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.393 _refine_diff_density_min -0.545 _refine_diff_density_rms 0.064 #===END