# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author ; R.A. Fischer Lehrstuhl fuer Anorganische Chemie II Ruhr-Universitaet Bochum Universitaetsstrasse 150 44780 Bochum (Germany) ; _publ_contact_author_phone '049 234 32-24174' _publ_contact_author_fax '049 234 321-4174' _publ_contact_author_email roland.fischer@ruhr-uni-bochum.de _publ_requested_coeditor_name ? _publ_contact_letter ; ; #============================================================================== # 2. TITLE AND AUTHOR LIST _publ_section_title ; Zinc-rich Compounds of Iron and Cobalt: Formation of [Fe2Znn] (n = 2-4) and [Co2Zn3] Cores. ; loop_ _publ_author_name _publ_author_address 'Timo Bollermann' ; Lehrstuhl fuer Anorganische Chemie II Ruhr-Universitaet Bochum Universitaetsstrasse 150 44780 Bochum (Germany) ; 'Inke Schwedler' ; Lehrstuhl fuer Anorganische Chemie II Ruhr-Universitaet Bochum Universitaetsstrasse 150 44780 Bochum (Germany) ; 'Mariusz Molon' ; Lehrstuhl fuer Anorganische Chemie II Ruhr-Universitaet Bochum Universitaetsstrasse 150 44780 Bochum (Germany) ; 'Kerstin Freitag' ; Lehrstuhl fuer Anorganische Chemie II Ruhr-Universitaet Bochum Universitaetsstrasse 150 44780 Bochum (Germany) ; 'Christian Gemel' ; Lehrstuhl fuer Anorganische Chemie II Ruhr-Universitaet Bochum Universitaetsstrasse 150 44780 Bochum (Germany) ; 'Ruediger Wolf Seidel' ; Lehrstuhl fuer Analytische Chemie Ruhr-Universitaet Bochum Universitaetsstrasse 150 44780 Bochum (Germany) ; ; R.A.Fischer ; ; Lehrstuhl fuer Anorganische Chemie II Ruhr-Universitaet Bochum Universitaetsstrasse 150 44780 Bochum (Germany) ; #======================================================================= # 4. TEXT _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_experimental ; ; _publ_section_references ; ; _publ_section_figure_captions ; ; _publ_section_acknowledgements; ; ; _publ_contact_author_name 'R.A. Fischer' #==================================================================== data_1 _database_code_depnum_ccdc_archive 'CCDC 836631' #TrackingRef '- 1-5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H32 Fe2 O12 Zn2' _chemical_formula_sum 'C24 H32 Fe2 O12 Zn2' _chemical_formula_weight 754.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 14.7039(6) _cell_length_b 12.3522(5) _cell_length_c 31.5375(11) _cell_angle_alpha 90.00 _cell_angle_beta 93.005(3) _cell_angle_gamma 90.00 _cell_volume 5720.1(4) _cell_formula_units_Z 8 _cell_measurement_temperature 108(2) _cell_measurement_reflns_used 3287 _cell_measurement_theta_min 3.8186 _cell_measurement_theta_max 27.9820 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.753 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3072 _exptl_absorpt_coefficient_mu 2.711 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4504 _exptl_absorpt_correction_T_max 0.6269 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 108(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur^TM^2, Oxford Diffraction' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.4171 _diffrn_reflns_number 13348 _diffrn_reflns_av_R_equivalents 0.0504 _diffrn_reflns_av_sigmaI/netI 0.0804 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 3.83 _diffrn_reflns_theta_max 26.50 _reflns_number_total 5871 _reflns_number_gt 4200 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material 'enCIFer (Allen et al., 2004)' _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^)+(0.0181P)^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_number_reflns 5871 _refine_ls_number_parameters 362 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0760 _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.0787 _refine_ls_wR_factor_gt 0.0668 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.07158(4) 0.60403(5) 0.544746(16) 0.01428(14) Uani 1 1 d . . . Fe2 Fe 0.0000 0.21644(7) 0.2500 0.0154(2) Uani 1 2 d S . . Fe3 Fe 0.0000 -0.12553(7) 0.2500 0.0156(2) Uani 1 2 d S . . Zn1 Zn -0.01149(3) 0.42313(4) 0.530524(13) 0.01399(12) Uani 1 1 d . . . Zn2 Zn 0.06954(3) 0.04653(4) 0.280520(13) 0.01488(12) Uani 1 1 d . . . O1 O 0.06280(18) 0.2879(2) 0.55365(7) 0.0182(7) Uani 1 1 d . . . O2 O -0.10247(18) 0.3915(2) 0.57793(7) 0.0185(7) Uani 1 1 d . . . O3 O 0.2142(2) 0.4501(2) 0.52366(8) 0.0253(7) Uani 1 1 d . . . O4 O 0.1298(2) 0.6267(2) 0.63466(8) 0.0306(8) Uani 1 1 d . . . O5 O 0.12363(19) 0.8146(2) 0.51096(8) 0.0239(7) Uani 1 1 d . . . O6 O -0.1205(2) 0.6436(2) 0.55928(8) 0.0256(7) Uani 1 1 d . . . O7 O 0.21222(18) 0.0433(2) 0.28239(8) 0.0184(6) Uani 1 1 d . . . O8 O 0.08754(18) 0.0523(2) 0.34752(7) 0.0214(7) Uani 1 1 d . . . O9 O 0.1322(2) -0.2627(3) 0.29729(9) 0.0322(8) Uani 1 1 d . . . O10 O 0.1088(2) -0.0747(3) 0.17711(9) 0.0299(8) Uani 1 1 d . . . O11 O 0.0975(2) 0.3521(3) 0.31363(9) 0.0338(8) Uani 1 1 d . . . O12 O 0.1508(2) 0.1618(2) 0.19632(8) 0.0265(7) Uani 1 1 d . . . C1 C -0.1945(3) 0.3542(4) 0.56809(12) 0.0216(10) Uani 1 1 d . . . H1A H -0.1941 0.2787 0.5575 0.026 Uiso 1 1 calc R . . H1B H -0.2251 0.4007 0.5461 0.026 Uiso 1 1 calc R . . C2 C -0.2433(3) 0.3606(4) 0.60898(11) 0.0221(10) Uani 1 1 d . . . H2A H -0.2386 0.2914 0.6248 0.026 Uiso 1 1 calc R . . H2B H -0.3083 0.3792 0.6036 0.026 Uiso 1 1 calc R . . C3 C -0.1920(3) 0.4510(3) 0.63292(11) 0.0189(10) Uani 1 1 d . . . H3A H -0.2135 0.5232 0.6231 0.023 Uiso 1 1 calc R . . H3B H -0.1985 0.4451 0.6639 0.023 Uiso 1 1 calc R . . C4 C -0.0952(3) 0.4308(3) 0.62151(11) 0.0188(10) Uani 1 1 d . . . H4A H -0.0591 0.4984 0.6235 0.023 Uiso 1 1 calc R . . H4B H -0.0659 0.3759 0.6406 0.023 Uiso 1 1 calc R . . C5 C 0.1061(3) 0.2940(4) 0.59604(11) 0.0220(10) Uani 1 1 d . . . H5A H 0.0646 0.2670 0.6174 0.026 Uiso 1 1 calc R . . H5B H 0.1235 0.3695 0.6032 0.026 Uiso 1 1 calc R . . C6 C 0.1893(3) 0.2232(3) 0.59478(12) 0.0226(10) Uani 1 1 d . . . H6A H 0.2059 0.1920 0.6231 0.027 Uiso 1 1 calc R . . H6B H 0.2420 0.2639 0.5846 0.027 Uiso 1 1 calc R . . C7 C 0.1579(3) 0.1361(3) 0.56338(12) 0.0198(10) Uani 1 1 d . . . H7A H 0.2103 0.0992 0.5511 0.024 Uiso 1 1 calc R . . H7B H 0.1193 0.0817 0.5768 0.024 Uiso 1 1 calc R . . C8 C 0.1042(3) 0.2008(3) 0.53026(12) 0.0236(11) Uani 1 1 d . . . H8A H 0.1446 0.2302 0.5089 0.028 Uiso 1 1 calc R . . H8B H 0.0568 0.1553 0.5156 0.028 Uiso 1 1 calc R . . C9 C 0.1558(3) 0.5095(4) 0.53090(11) 0.0166(9) Uani 1 1 d . . . C10 C 0.1075(3) 0.6172(3) 0.59934(12) 0.0185(10) Uani 1 1 d . . . C11 C 0.1043(3) 0.7301(4) 0.52321(11) 0.0181(10) Uani 1 1 d . . . C12 C -0.0448(3) 0.6245(3) 0.55229(11) 0.0191(10) Uani 1 1 d . . . C13 C 0.2733(3) -0.0374(3) 0.26574(13) 0.0228(10) Uani 1 1 d . . . H13A H 0.2539 -0.0565 0.2361 0.027 Uiso 1 1 calc R . . H13B H 0.2735 -0.1039 0.2833 0.027 Uiso 1 1 calc R . . C14 C 0.3667(3) 0.0140(3) 0.26753(12) 0.0219(10) Uani 1 1 d . . . H14A H 0.3803 0.0461 0.2398 0.026 Uiso 1 1 calc R . . H14B H 0.4145 -0.0396 0.2758 0.026 Uiso 1 1 calc R . . C15 C 0.3598(3) 0.1014(3) 0.30157(12) 0.0216(10) Uani 1 1 d . . . H15A H 0.3710 0.0709 0.3304 0.026 Uiso 1 1 calc R . . H15B H 0.4035 0.1609 0.2973 0.026 Uiso 1 1 calc R . . C16 C 0.2631(3) 0.1398(3) 0.29474(12) 0.0210(10) Uani 1 1 d . . . H16A H 0.2407 0.1709 0.3212 0.025 Uiso 1 1 calc R . . H16B H 0.2580 0.1952 0.2721 0.025 Uiso 1 1 calc R . . C17 C 0.0289(3) 0.1076(4) 0.37641(11) 0.0265(11) Uani 1 1 d . . . H17A H -0.0358 0.0890 0.3698 0.032 Uiso 1 1 calc R . . H17B H 0.0362 0.1871 0.3743 0.032 Uiso 1 1 calc R . . C18 C 0.0597(3) 0.0681(4) 0.42043(12) 0.0275(11) Uani 1 1 d . . . H18A H 0.1065 0.1166 0.4338 0.033 Uiso 1 1 calc R . . H18B H 0.0078 0.0629 0.4391 0.033 Uiso 1 1 calc R . . C19 C 0.0988(3) -0.0425(4) 0.41184(12) 0.0281(11) Uani 1 1 d . . . H19A H 0.1429 -0.0651 0.4350 0.034 Uiso 1 1 calc R . . H19B H 0.0502 -0.0977 0.4083 0.034 Uiso 1 1 calc R . . C20 C 0.1454(3) -0.0243(4) 0.37087(12) 0.0257(11) Uani 1 1 d . . . H20A H 0.2073 0.0058 0.3765 0.031 Uiso 1 1 calc R . . H20B H 0.1502 -0.0929 0.3549 0.031 Uiso 1 1 calc R . . C21 C 0.0788(3) -0.2093(3) 0.27829(12) 0.0206(10) Uani 1 1 d . . . C22 C 0.0659(3) -0.0899(3) 0.20645(13) 0.0205(10) Uani 1 1 d . . . C23 C 0.0594(3) 0.3002(3) 0.28820(12) 0.0206(10) Uani 1 1 d . . . C24 C 0.0911(3) 0.1806(3) 0.21766(12) 0.0188(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0143(3) 0.0162(3) 0.0121(3) -0.0005(2) -0.0003(2) -0.0013(3) Fe2 0.0188(5) 0.0125(5) 0.0151(4) 0.000 0.0019(3) 0.000 Fe3 0.0185(5) 0.0131(5) 0.0154(4) 0.000 0.0012(3) 0.000 Zn1 0.0141(3) 0.0160(3) 0.0118(2) 0.00015(19) 0.00037(17) 0.0000(2) Zn2 0.0171(3) 0.0145(3) 0.0131(2) -0.00090(19) 0.00143(17) 0.0004(2) O1 0.0213(18) 0.0210(17) 0.0117(14) -0.0016(12) -0.0038(11) 0.0061(14) O2 0.0159(17) 0.0255(18) 0.0144(14) -0.0042(12) 0.0033(11) -0.0046(14) O3 0.0186(18) 0.0281(19) 0.0296(17) -0.0013(14) 0.0049(13) 0.0045(16) O4 0.041(2) 0.033(2) 0.0173(16) -0.0009(14) -0.0061(13) -0.0019(17) O5 0.0247(19) 0.0209(18) 0.0260(17) 0.0041(14) 0.0006(13) -0.0080(15) O6 0.0186(19) 0.029(2) 0.0295(17) 0.0005(14) 0.0064(13) 0.0048(16) O7 0.0139(16) 0.0173(16) 0.0241(15) -0.0062(12) 0.0012(11) -0.0009(14) O8 0.0255(18) 0.0283(18) 0.0106(14) 0.0005(12) 0.0034(11) 0.0114(15) O9 0.037(2) 0.031(2) 0.0288(18) 0.0073(15) -0.0005(14) 0.0124(17) O10 0.032(2) 0.035(2) 0.0244(17) -0.0013(14) 0.0136(14) 0.0010(16) O11 0.044(2) 0.031(2) 0.0260(17) -0.0078(15) -0.0046(15) -0.0124(17) O12 0.024(2) 0.034(2) 0.0225(17) -0.0006(14) 0.0126(13) 0.0008(16) C1 0.018(3) 0.023(3) 0.024(2) -0.0019(19) 0.0054(17) -0.008(2) C2 0.021(3) 0.029(3) 0.016(2) -0.0005(19) 0.0033(17) -0.003(2) C3 0.023(3) 0.018(2) 0.015(2) -0.0011(18) 0.0006(16) 0.000(2) C4 0.022(3) 0.025(3) 0.0098(19) 0.0015(17) 0.0015(16) -0.003(2) C5 0.029(3) 0.023(3) 0.014(2) -0.0001(18) -0.0036(18) 0.006(2) C6 0.027(3) 0.021(3) 0.019(2) -0.0002(19) -0.0049(18) 0.004(2) C7 0.016(2) 0.021(3) 0.022(2) 0.0004(18) 0.0012(17) 0.007(2) C8 0.029(3) 0.023(3) 0.018(2) -0.0066(19) -0.0038(18) 0.009(2) C9 0.012(2) 0.024(3) 0.013(2) 0.0031(17) -0.0007(16) -0.005(2) C10 0.015(2) 0.019(2) 0.022(2) 0.0014(18) 0.0048(17) 0.001(2) C11 0.017(3) 0.026(3) 0.011(2) -0.0035(18) -0.0010(16) 0.001(2) C12 0.028(3) 0.014(2) 0.015(2) 0.0011(17) -0.0037(18) -0.001(2) C13 0.022(3) 0.019(3) 0.027(2) -0.0079(19) -0.0005(18) 0.006(2) C14 0.019(3) 0.021(3) 0.025(2) -0.0039(19) 0.0001(18) 0.004(2) C15 0.024(3) 0.023(3) 0.018(2) -0.0014(18) 0.0003(17) -0.007(2) C16 0.022(3) 0.015(2) 0.026(2) -0.0074(18) 0.0025(18) -0.007(2) C17 0.031(3) 0.034(3) 0.015(2) -0.0059(19) 0.0068(18) 0.011(2) C18 0.032(3) 0.035(3) 0.015(2) -0.005(2) 0.0037(18) -0.003(2) C19 0.032(3) 0.034(3) 0.019(2) 0.006(2) 0.0011(19) -0.006(2) C20 0.025(3) 0.032(3) 0.020(2) 0.003(2) -0.0017(18) 0.008(2) C21 0.025(3) 0.018(2) 0.020(2) -0.0013(19) 0.0062(18) -0.005(2) C22 0.022(3) 0.013(2) 0.026(2) -0.0036(18) -0.0025(18) -0.001(2) C23 0.026(3) 0.015(2) 0.021(2) 0.0066(18) 0.0086(18) 0.003(2) C24 0.023(3) 0.013(2) 0.019(2) 0.0017(18) -0.0067(18) -0.005(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 Fe1 C12 1.759(5) . ? Fe1 C9 1.773(4) . ? Fe1 C11 1.775(5) . ? Fe1 C10 1.782(4) . ? Fe1 Zn1 2.5116(7) 5_566 ? Fe1 Zn1 2.5746(7) . ? Fe2 C23 1.781(4) 2 ? Fe2 C23 1.781(4) . ? Fe2 C24 1.782(5) . ? Fe2 C24 1.782(5) 2 ? Fe2 Zn2 2.5048(8) 2 ? Fe2 Zn2 2.5048(8) . ? Fe3 C21 1.761(4) . ? Fe3 C21 1.761(4) 2 ? Fe3 C22 1.777(4) . ? Fe3 C22 1.777(4) 2 ? Fe3 Zn2 2.5269(8) 2 ? Fe3 Zn2 2.5270(8) . ? Zn1 O2 2.095(3) . ? Zn1 O1 2.105(3) . ? Zn1 Fe1 2.5116(7) 5_566 ? Zn1 Zn1 2.7378(9) 5_566 ? Zn2 O7 2.096(3) . ? Zn2 O8 2.117(2) . ? Zn2 Zn2 2.7339(8) 2 ? O1 C5 1.452(4) . ? O1 C8 1.456(5) . ? O2 C1 1.448(4) . ? O2 C4 1.456(4) . ? O3 C9 1.162(4) . ? O4 C10 1.151(4) . ? O5 C11 1.153(5) . ? O6 C12 1.170(5) . ? O7 C16 1.449(4) . ? O7 C13 1.457(4) . ? O8 C20 1.448(4) . ? O8 C17 1.457(4) . ? O9 C21 1.166(5) . ? O10 C22 1.162(5) . ? O11 C23 1.150(5) . ? O12 C24 1.157(5) . ? C1 C2 1.510(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.525(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.507(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.506(5) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.518(5) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.506(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C13 C14 1.512(5) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.530(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.504(5) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.518(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.511(6) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.511(5) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C12 Fe1 C9 145.62(19) . . ? C12 Fe1 C11 102.18(19) . . ? C9 Fe1 C11 106.04(19) . . ? C12 Fe1 C10 95.60(17) . . ? C9 Fe1 C10 97.03(17) . . ? C11 Fe1 C10 102.55(18) . . ? C12 Fe1 Zn1 81.40(12) . 5_566 ? C9 Fe1 Zn1 83.96(11) . 5_566 ? C11 Fe1 Zn1 81.06(12) . 5_566 ? C10 Fe1 Zn1 175.78(13) . 5_566 ? C12 Fe1 Zn1 72.08(13) . . ? C9 Fe1 Zn1 73.54(13) . . ? C11 Fe1 Zn1 146.12(12) . . ? C10 Fe1 Zn1 111.18(14) . . ? Zn1 Fe1 Zn1 65.12(2) 5_566 . ? C23 Fe2 C23 109.0(3) 2 . ? C23 Fe2 C24 96.55(18) 2 . ? C23 Fe2 C24 100.06(18) . . ? C23 Fe2 C24 100.06(18) 2 2 ? C23 Fe2 C24 96.55(18) . 2 ? C24 Fe2 C24 151.2(3) . 2 ? C23 Fe2 Zn2 92.92(13) 2 2 ? C23 Fe2 Zn2 157.24(13) . 2 ? C24 Fe2 Zn2 82.86(13) . 2 ? C24 Fe2 Zn2 72.99(13) 2 2 ? C23 Fe2 Zn2 157.24(13) 2 . ? C23 Fe2 Zn2 92.91(13) . . ? C24 Fe2 Zn2 72.99(13) . . ? C24 Fe2 Zn2 82.86(13) 2 . ? Zn2 Fe2 Zn2 66.15(3) 2 . ? C21 Fe3 C21 108.0(3) . 2 ? C21 Fe3 C22 99.55(19) . . ? C21 Fe3 C22 97.18(18) 2 . ? C21 Fe3 C22 97.18(18) . 2 ? C21 Fe3 C22 99.55(19) 2 2 ? C22 Fe3 C22 151.3(3) . 2 ? C21 Fe3 Zn2 158.37(13) . 2 ? C21 Fe3 Zn2 93.38(13) 2 2 ? C22 Fe3 Zn2 73.95(13) . 2 ? C22 Fe3 Zn2 81.95(13) 2 2 ? C21 Fe3 Zn2 93.38(13) . . ? C21 Fe3 Zn2 158.37(13) 2 . ? C22 Fe3 Zn2 81.95(13) . . ? C22 Fe3 Zn2 73.95(13) 2 . ? Zn2 Fe3 Zn2 65.50(3) 2 . ? O2 Zn1 O1 86.79(11) . . ? O2 Zn1 Fe1 116.33(7) . 5_566 ? O1 Zn1 Fe1 111.84(7) . 5_566 ? O2 Zn1 Fe1 110.64(8) . . ? O1 Zn1 Fe1 113.28(8) . . ? Fe1 Zn1 Fe1 114.88(2) 5_566 . ? O2 Zn1 Zn1 137.60(8) . 5_566 ? O1 Zn1 Zn1 135.48(8) . 5_566 ? Fe1 Zn1 Zn1 58.55(2) 5_566 5_566 ? Fe1 Zn1 Zn1 56.33(2) . 5_566 ? O7 Zn2 O8 84.26(10) . . ? O7 Zn2 Fe2 114.50(8) . . ? O8 Zn2 Fe2 112.49(8) . . ? O7 Zn2 Fe3 112.27(8) . . ? O8 Zn2 Fe3 115.82(8) . . ? Fe2 Zn2 Fe3 114.17(2) . . ? O7 Zn2 Zn2 136.92(7) . 2 ? O8 Zn2 Zn2 138.82(8) . 2 ? Fe2 Zn2 Zn2 56.924(15) . 2 ? Fe3 Zn2 Zn2 57.250(15) . 2 ? C5 O1 C8 109.2(3) . . ? C5 O1 Zn1 118.2(2) . . ? C8 O1 Zn1 129.3(2) . . ? C1 O2 C4 109.3(3) . . ? C1 O2 Zn1 122.1(2) . . ? C4 O2 Zn1 126.4(2) . . ? C16 O7 C13 109.9(3) . . ? C16 O7 Zn2 119.6(2) . . ? C13 O7 Zn2 129.6(2) . . ? C20 O8 C17 109.9(3) . . ? C20 O8 Zn2 121.7(2) . . ? C17 O8 Zn2 126.4(2) . . ? O2 C1 C2 106.3(3) . . ? O2 C1 H1A 110.5 . . ? C2 C1 H1A 110.5 . . ? O2 C1 H1B 110.5 . . ? C2 C1 H1B 110.5 . . ? H1A C1 H1B 108.7 . . ? C1 C2 C3 102.5(3) . . ? C1 C2 H2A 111.3 . . ? C3 C2 H2A 111.3 . . ? C1 C2 H2B 111.3 . . ? C3 C2 H2B 111.3 . . ? H2A C2 H2B 109.2 . . ? C4 C3 C2 102.0(3) . . ? C4 C3 H3A 111.4 . . ? C2 C3 H3A 111.4 . . ? C4 C3 H3B 111.4 . . ? C2 C3 H3B 111.4 . . ? H3A C3 H3B 109.2 . . ? O2 C4 C3 104.9(3) . . ? O2 C4 H4A 110.8 . . ? C3 C4 H4A 110.8 . . ? O2 C4 H4B 110.8 . . ? C3 C4 H4B 110.8 . . ? H4A C4 H4B 108.8 . . ? O1 C5 C6 105.3(3) . . ? O1 C5 H5A 110.7 . . ? C6 C5 H5A 110.7 . . ? O1 C5 H5B 110.7 . . ? C6 C5 H5B 110.7 . . ? H5A C5 H5B 108.8 . . ? C5 C6 C7 102.1(3) . . ? C5 C6 H6A 111.4 . . ? C7 C6 H6A 111.4 . . ? C5 C6 H6B 111.4 . . ? C7 C6 H6B 111.4 . . ? H6A C6 H6B 109.2 . . ? C8 C7 C6 101.9(3) . . ? C8 C7 H7A 111.4 . . ? C6 C7 H7A 111.4 . . ? C8 C7 H7B 111.4 . . ? C6 C7 H7B 111.4 . . ? H7A C7 H7B 109.2 . . ? O1 C8 C7 105.0(3) . . ? O1 C8 H8A 110.7 . . ? C7 C8 H8A 110.7 . . ? O1 C8 H8B 110.7 . . ? C7 C8 H8B 110.7 . . ? H8A C8 H8B 108.8 . . ? O3 C9 Fe1 176.1(3) . . ? O4 C10 Fe1 179.0(4) . . ? O5 C11 Fe1 176.5(4) . . ? O6 C12 Fe1 175.4(4) . . ? O7 C13 C14 106.0(3) . . ? O7 C13 H13A 110.5 . . ? C14 C13 H13A 110.5 . . ? O7 C13 H13B 110.5 . . ? C14 C13 H13B 110.5 . . ? H13A C13 H13B 108.7 . . ? C13 C14 C15 103.2(3) . . ? C13 C14 H14A 111.1 . . ? C15 C14 H14A 111.1 . . ? C13 C14 H14B 111.1 . . ? C15 C14 H14B 111.1 . . ? H14A C14 H14B 109.1 . . ? C16 C15 C14 102.7(3) . . ? C16 C15 H15A 111.2 . . ? C14 C15 H15A 111.2 . . ? C16 C15 H15B 111.2 . . ? C14 C15 H15B 111.2 . . ? H15A C15 H15B 109.1 . . ? O7 C16 C15 104.5(3) . . ? O7 C16 H16A 110.9 . . ? C15 C16 H16A 110.9 . . ? O7 C16 H16B 110.9 . . ? C15 C16 H16B 110.9 . . ? H16A C16 H16B 108.9 . . ? O8 C17 C18 105.2(3) . . ? O8 C17 H17A 110.7 . . ? C18 C17 H17A 110.7 . . ? O8 C17 H17B 110.7 . . ? C18 C17 H17B 110.7 . . ? H17A C17 H17B 108.8 . . ? C19 C18 C17 103.0(3) . . ? C19 C18 H18A 111.2 . . ? C17 C18 H18A 111.2 . . ? C19 C18 H18B 111.2 . . ? C17 C18 H18B 111.2 . . ? H18A C18 H18B 109.1 . . ? C20 C19 C18 102.3(3) . . ? C20 C19 H19A 111.3 . . ? C18 C19 H19A 111.3 . . ? C20 C19 H19B 111.3 . . ? C18 C19 H19B 111.3 . . ? H19A C19 H19B 109.2 . . ? O8 C20 C19 104.5(3) . . ? O8 C20 H20A 110.8 . . ? C19 C20 H20A 110.8 . . ? O8 C20 H20B 110.8 . . ? C19 C20 H20B 110.8 . . ? H20A C20 H20B 108.9 . . ? O9 C21 Fe3 178.4(4) . . ? O10 C22 Fe3 174.9(4) . . ? O11 C23 Fe2 178.2(4) . . ? O12 C24 Fe2 177.1(4) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.549 _refine_diff_density_min -0.549 _refine_diff_density_rms 0.121 data_2 _database_code_depnum_ccdc_archive 'CCDC 836632' #TrackingRef '- 1-5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H38 Fe2 O10 Zn4, 2(C4 H8 O)' _chemical_formula_sum 'C32 H54 Fe2 O12 Zn4' _chemical_formula_weight 1003.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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' _symmetry_space_group_name_Hall '-P 2ybc' 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 20.416(5) _cell_length_b 14.321(3) _cell_length_c 14.392(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.34(3) _cell_angle_gamma 90.00 _cell_volume 3945.4(16) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 4451 _cell_measurement_theta_min 2.8387 _cell_measurement_theta_max 29.1766 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.690 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2056 _exptl_absorpt_coefficient_mu 3.164 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5428 _exptl_absorpt_correction_T_max 0.8328 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur^TM^2, Oxford Diffraction' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.4171 _diffrn_reflns_number 41446 _diffrn_reflns_av_R_equivalents 0.1328 _diffrn_reflns_av_sigmaI/netI 0.1143 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6942 _reflns_number_gt 3970 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material 'enCIFer (Allen et al., 2004)' _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^)+(0.0659P)^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_number_reflns 6942 _refine_ls_number_parameters 377 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1158 _refine_ls_R_factor_gt 0.0584 _refine_ls_wR_factor_ref 0.1537 _refine_ls_wR_factor_gt 0.1320 _refine_ls_goodness_of_fit_ref 0.945 _refine_ls_restrained_S_all 0.944 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.01234(4) 0.10090(6) 0.09573(6) 0.0298(2) Uani 1 1 d . . . Zn2 Zn 0.09857(4) -0.04637(6) 0.07100(6) 0.0328(3) Uani 1 1 d . . . Fe1 Fe -0.02336(6) -0.06479(7) 0.06335(8) 0.0287(3) Uani 1 1 d . . . O1 O 0.0257(3) -0.2570(4) 0.0911(4) 0.0437(15) Uani 1 1 d . . . O2 O 0.0075(4) -0.0247(4) 0.2716(4) 0.0567(18) Uani 1 1 d . . . O3 O 0.1682(3) 0.1118(4) -0.0261(5) 0.0624(19) Uani 1 1 d . . . O4 O -0.0612(3) 0.1824(3) 0.1256(4) 0.0374(14) Uani 1 1 d . . . O5 O 0.0891(3) 0.1684(4) 0.2042(4) 0.0445(15) Uani 1 1 d . . . C1 C 0.0079(4) -0.1789(6) 0.0759(6) 0.038(2) Uani 1 1 d . . . C2 C -0.0024(5) -0.0363(5) 0.1875(6) 0.042(2) Uani 1 1 d . . . C3 C 0.1125(5) 0.0859(6) -0.0334(6) 0.045(2) Uani 1 1 d . . . C4 C -0.0701(4) 0.2833(5) 0.1105(7) 0.047(2) Uani 1 1 d . . . H4A H -0.0834 0.2987 0.0393 0.057 Uiso 1 1 calc R . . H4B H -0.0261 0.3164 0.1473 0.057 Uiso 1 1 calc R . . C5 C -0.1264(4) 0.3111(6) 0.1481(7) 0.047(2) Uani 1 1 d . . . H5A H -0.1553 0.3618 0.1073 0.057 Uiso 1 1 calc R . . H5B H -0.1066 0.3323 0.2178 0.057 Uiso 1 1 calc R . . C6 C -0.1691(4) 0.2225(6) 0.1397(8) 0.054(3) Uani 1 1 d . . . H6A H -0.1924 0.2217 0.1896 0.064 Uiso 1 1 calc R . . H6B H -0.2049 0.2165 0.0728 0.064 Uiso 1 1 calc R . . C7 C -0.1168(4) 0.1474(6) 0.1584(6) 0.044(2) Uani 1 1 d . . . H7A H -0.0981 0.1319 0.2299 0.052 Uiso 1 1 calc R . . H7B H -0.1381 0.0905 0.1210 0.052 Uiso 1 1 calc R . . C8 C 0.0862(5) 0.1879(6) 0.3036(6) 0.055(3) Uani 1 1 d . . . H8A H 0.0528 0.1455 0.3186 0.066 Uiso 1 1 calc R . . H8B H 0.0720 0.2533 0.3084 0.066 Uiso 1 1 calc R . . C9 C 0.1592(6) 0.1708(8) 0.3727(7) 0.082(4) Uani 1 1 d . . . H9A H 0.1673 0.1036 0.3888 0.099 Uiso 1 1 calc R . . H9B H 0.1692 0.2066 0.4350 0.099 Uiso 1 1 calc R . . C10 C 0.2028(5) 0.2051(8) 0.3136(7) 0.081(4) Uani 1 1 d . . . H10A H 0.2503 0.1779 0.3385 0.097 Uiso 1 1 calc R . . H10B H 0.2064 0.2741 0.3155 0.097 Uiso 1 1 calc R . . C11 C 0.1616(4) 0.1702(6) 0.2091(6) 0.052(2) Uani 1 1 d . . . H11A H 0.1674 0.2131 0.1585 0.062 Uiso 1 1 calc R . . H11B H 0.1773 0.1071 0.1983 0.062 Uiso 1 1 calc R . . C12 C 0.1917(4) -0.0987(6) 0.1380(6) 0.049(2) Uani 1 1 d . . . H12A H 0.1885 -0.1508 0.1804 0.074 Uiso 1 1 calc R . . H12B H 0.2224 -0.0503 0.1788 0.074 Uiso 1 1 calc R . . H12C H 0.2109 -0.1212 0.0885 0.074 Uiso 1 1 calc R . . Zn3 Zn 0.50418(5) -0.10503(6) 0.41579(7) 0.0358(3) Uani 1 1 d . . . Zn4 Zn 0.40021(5) -0.03773(7) 0.47813(7) 0.0378(3) Uani 1 1 d . . . Fe2 Fe 0.47804(6) 0.06221(8) 0.41185(8) 0.0338(3) Uani 1 1 d . . . O6 O 0.5396(4) 0.0358(5) 0.2615(5) 0.069(2) Uani 1 1 d . . . O7 O 0.3355(3) 0.0731(5) 0.2733(5) 0.067(2) Uani 1 1 d . A . O8 O 0.4981(4) -0.2640(5) 0.5687(5) 0.080(2) Uani 1 1 d . . . O10 O 0.4273(3) -0.1855(4) 0.3191(4) 0.0432(15) Uani 1 1 d . A . C13 C 0.5170(5) 0.0415(6) 0.3255(7) 0.050(2) Uani 1 1 d . A . C14 C 0.3910(5) 0.0650(6) 0.3336(6) 0.047(2) Uani 1 1 d . . . C15 C 0.5067(5) -0.1827(6) 0.5708(6) 0.047(2) Uani 1 1 d . . . O9 O 0.5782(5) -0.1813(7) 0.3862(9) 0.049(3) Uani 0.805(8) 1 d PD A 1 C16 C 0.5702(5) -0.2029(8) 0.2850(7) 0.048(3) Uani 0.805(8) 1 d PD A 1 H16A H 0.5369 -0.1593 0.2388 0.058 Uiso 0.805(8) 1 calc PR A 1 H16B H 0.5529 -0.2675 0.2682 0.058 Uiso 0.805(8) 1 calc PR A 1 C17 C 0.6414(6) -0.1924(9) 0.2790(9) 0.061(4) Uani 0.805(8) 1 d PD A 1 H17A H 0.6512 -0.1267 0.2669 0.073 Uiso 0.805(8) 1 calc PR A 1 H17B H 0.6475 -0.2326 0.2266 0.073 Uiso 0.805(8) 1 calc PR A 1 C18 C 0.6877(6) -0.2253(10) 0.3835(8) 0.057(4) Uani 0.805(8) 1 d PD A 1 H18A H 0.6893 -0.2943 0.3879 0.069 Uiso 0.805(8) 1 calc PR A 1 H18B H 0.7359 -0.2008 0.4014 0.069 Uiso 0.805(8) 1 calc PR A 1 C19 C 0.6509(5) -0.1840(8) 0.4490(8) 0.056(3) Uani 0.805(8) 1 d PD A 1 H19A H 0.6576 -0.2238 0.5079 0.067 Uiso 0.805(8) 1 calc PR A 1 H19B H 0.6686 -0.1205 0.4714 0.067 Uiso 0.805(8) 1 calc PR A 1 O9' O 0.572(2) -0.170(3) 0.364(5) 0.049(3) Uani 0.195(8) 1 d PD A 2 C16' C 0.5848(17) -0.270(3) 0.374(3) 0.048(3) Uani 0.195(8) 1 d PD A 2 H16C H 0.5609 -0.3024 0.3102 0.058 Uiso 0.195(8) 1 calc PR A 2 H16D H 0.5686 -0.2968 0.4255 0.058 Uiso 0.195(8) 1 calc PR A 2 C17' C 0.6636(18) -0.277(3) 0.403(3) 0.061(4) Uani 0.195(8) 1 d PD A 2 H17C H 0.6787 -0.3400 0.3910 0.073 Uiso 0.195(8) 1 calc PR A 2 H17D H 0.6879 -0.2592 0.4733 0.073 Uiso 0.195(8) 1 calc PR A 2 C18' C 0.674(3) -0.203(3) 0.330(4) 0.057(4) Uani 0.195(8) 1 d PD A 2 H18C H 0.7231 -0.1840 0.3493 0.069 Uiso 0.195(8) 1 calc PR A 2 H18D H 0.6573 -0.2271 0.2614 0.069 Uiso 0.195(8) 1 calc PR A 2 C19' C 0.628(2) -0.124(2) 0.342(3) 0.056(3) Uani 0.195(8) 1 d PD A 2 H19C H 0.6547 -0.0816 0.3970 0.067 Uiso 0.195(8) 1 calc PR A 2 H19D H 0.6096 -0.0866 0.2803 0.067 Uiso 0.195(8) 1 calc PR A 2 C20 C 0.4022(5) -0.2769(7) 0.3368(7) 0.062(3) Uani 1 1 d . . . H20A H 0.3881 -0.2748 0.3960 0.074 Uiso 1 1 calc R A . H20B H 0.4394 -0.3244 0.3479 0.074 Uiso 1 1 calc R . . C21 C 0.3420(5) -0.3002(7) 0.2485(8) 0.074(3) Uani 1 1 d . A . H21A H 0.3394 -0.3683 0.2359 0.089 Uiso 1 1 calc R . . H21B H 0.2978 -0.2792 0.2557 0.089 Uiso 1 1 calc R . . C22 C 0.3555(5) -0.2497(7) 0.1690(8) 0.075(4) Uani 1 1 d . . . H22A H 0.3118 -0.2389 0.1123 0.090 Uiso 1 1 calc R A . H22B H 0.3890 -0.2837 0.1457 0.090 Uiso 1 1 calc R . . C23 C 0.3867(5) -0.1573(7) 0.2199(7) 0.064(3) Uani 1 1 d . A . H23A H 0.4166 -0.1278 0.1867 0.076 Uiso 1 1 calc R . . H23B H 0.3495 -0.1130 0.2197 0.076 Uiso 1 1 calc R . . C24 C 0.3037(4) -0.0751(6) 0.4539(7) 0.056(3) Uani 1 1 d . . . H24A H 0.3020 -0.1162 0.5074 0.084 Uiso 1 1 calc R A . H24B H 0.2854 -0.1084 0.3906 0.084 Uiso 1 1 calc R . . H24C H 0.2752 -0.0195 0.4514 0.084 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 0.0282(5) 0.0341(6) 0.0286(5) -0.0017(4) 0.0119(4) 0.0011(4) Zn2 0.0265(5) 0.0381(6) 0.0323(5) 0.0013(4) 0.0084(4) 0.0042(4) Fe1 0.0281(6) 0.0312(7) 0.0289(6) 0.0022(5) 0.0128(5) 0.0019(5) O1 0.059(4) 0.043(4) 0.036(3) 0.006(3) 0.026(3) 0.006(3) O2 0.095(5) 0.053(4) 0.028(3) 0.003(3) 0.029(4) 0.013(3) O3 0.040(4) 0.063(5) 0.093(5) 0.018(4) 0.034(4) -0.001(3) O4 0.033(3) 0.035(3) 0.049(3) -0.002(3) 0.020(3) 0.001(2) O5 0.019(3) 0.066(4) 0.050(4) -0.015(3) 0.015(3) 0.000(3) C1 0.031(5) 0.047(6) 0.035(5) 0.012(4) 0.013(4) 0.003(4) C2 0.055(6) 0.037(5) 0.041(5) 0.003(4) 0.025(5) 0.012(4) C3 0.042(6) 0.052(6) 0.046(5) 0.006(4) 0.020(5) 0.002(4) C4 0.054(6) 0.027(5) 0.073(7) 0.000(4) 0.037(5) 0.006(4) C5 0.040(5) 0.046(6) 0.058(6) 0.003(4) 0.019(5) 0.010(4) C6 0.036(5) 0.043(6) 0.087(7) 0.000(5) 0.028(5) 0.004(4) C7 0.049(6) 0.037(5) 0.056(6) 0.002(4) 0.032(5) -0.001(4) C8 0.052(6) 0.063(7) 0.051(6) -0.017(5) 0.019(5) -0.016(5) C9 0.079(8) 0.101(9) 0.044(6) -0.015(6) -0.009(6) 0.035(7) C10 0.050(7) 0.128(11) 0.065(7) -0.044(7) 0.020(6) -0.001(7) C11 0.041(6) 0.061(6) 0.051(6) -0.023(5) 0.014(5) -0.005(4) C12 0.032(5) 0.067(6) 0.054(6) 0.008(5) 0.021(5) 0.015(4) Zn3 0.0309(6) 0.0377(6) 0.0378(6) -0.0055(4) 0.0109(5) -0.0015(4) Zn4 0.0287(5) 0.0417(6) 0.0422(6) -0.0007(4) 0.0114(5) -0.0044(4) Fe2 0.0323(7) 0.0364(7) 0.0316(6) 0.0015(5) 0.0097(5) -0.0018(5) O6 0.091(6) 0.072(5) 0.065(5) -0.011(4) 0.052(4) -0.025(4) O7 0.039(4) 0.082(5) 0.068(5) 0.018(4) 0.004(4) 0.008(3) O8 0.140(8) 0.041(4) 0.063(5) 0.009(4) 0.038(5) -0.016(4) O10 0.034(3) 0.044(4) 0.048(4) -0.011(3) 0.008(3) -0.006(3) C13 0.059(6) 0.054(6) 0.045(5) 0.000(5) 0.029(5) -0.009(5) C14 0.038(6) 0.059(6) 0.040(5) 0.003(5) 0.009(5) -0.001(5) C15 0.063(7) 0.046(6) 0.033(5) 0.001(4) 0.017(5) 0.001(5) O9 0.025(4) 0.067(6) 0.045(8) -0.013(4) -0.001(4) 0.006(3) C16 0.039(7) 0.065(8) 0.040(7) -0.010(5) 0.013(6) 0.014(6) C17 0.037(7) 0.087(10) 0.053(8) -0.008(7) 0.009(6) -0.015(6) C18 0.035(7) 0.084(10) 0.059(9) -0.031(8) 0.024(7) 0.002(6) C19 0.028(6) 0.068(8) 0.063(8) -0.022(6) 0.005(6) 0.003(5) O9' 0.025(4) 0.067(6) 0.045(8) -0.013(4) -0.001(4) 0.006(3) C16' 0.039(7) 0.065(8) 0.040(7) -0.010(5) 0.013(6) 0.014(6) C17' 0.037(7) 0.087(10) 0.053(8) -0.008(7) 0.009(6) -0.015(6) C18' 0.035(7) 0.084(10) 0.059(9) -0.031(8) 0.024(7) 0.002(6) C19' 0.028(6) 0.068(8) 0.063(8) -0.022(6) 0.005(6) 0.003(5) C20 0.072(7) 0.062(7) 0.054(6) -0.009(5) 0.024(6) -0.019(6) C21 0.047(7) 0.070(8) 0.105(10) -0.041(7) 0.026(7) -0.026(5) C22 0.043(7) 0.091(9) 0.072(8) -0.038(7) -0.005(6) 0.012(6) C23 0.050(6) 0.066(7) 0.046(6) -0.007(5) -0.019(5) 0.001(5) C24 0.042(6) 0.075(7) 0.051(6) 0.008(5) 0.018(5) -0.004(5) _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 O5 2.032(5) . ? Zn1 O4 2.061(5) . ? Zn1 Fe1 2.4327(14) 3 ? Zn1 C2 2.443(8) . ? Zn1 Fe1 2.4785(14) . ? Zn1 Zn2 2.7780(15) 3 ? Zn1 Zn2 2.8477(13) . ? Zn2 C12 1.958(8) . ? Zn2 Fe1 2.4673(15) . ? Zn2 C3 2.494(9) . ? Zn2 Fe1 2.5625(14) 3 ? Zn2 Zn1 2.7780(15) 3 ? Fe1 C2 1.736(9) . ? Fe1 C1 1.741(9) . ? Fe1 C3 1.744(9) 3 ? Fe1 Zn1 2.4327(14) 3 ? Fe1 Zn2 2.5625(14) 3 ? O1 C1 1.172(9) . ? O2 C2 1.167(9) . ? O3 C3 1.167(10) . ? O4 C7 1.462(9) . ? O4 C4 1.463(9) . ? O5 C11 1.457(9) . ? O5 C8 1.479(10) . ? C3 Fe1 1.744(9) 3 ? C4 C5 1.484(11) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.521(11) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.472(11) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.496(12) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.513(15) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.530(12) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? Zn3 O9' 2.02(3) . ? Zn3 O9 2.026(8) . ? Zn3 O10 2.051(5) . ? Zn3 Fe2 2.4502(15) . ? Zn3 Fe2 2.4567(15) 3_656 ? Zn3 C15 2.478(8) . ? Zn3 C13 2.529(9) . ? Zn3 Zn4 2.7502(14) . ? Zn3 Zn4 2.8722(14) 3_656 ? Zn4 C24 1.953(8) . ? Zn4 Fe2 2.4643(17) 3_656 ? Zn4 C14 2.501(9) . ? Zn4 Fe2 2.5566(15) . ? Zn4 Zn3 2.8722(14) 3_656 ? Fe2 C13 1.718(10) . ? Fe2 C14 1.742(9) . ? Fe2 C15 1.756(9) 3_656 ? Fe2 Zn3 2.4567(15) 3_656 ? Fe2 Zn4 2.4642(17) 3_656 ? Fe2 Fe2 2.972(2) 3_656 ? O6 C13 1.167(10) . ? O7 C14 1.169(9) . ? O8 C15 1.176(9) . ? O10 C23 1.438(10) . ? O10 C20 1.461(10) . ? C15 Fe2 1.756(9) 3_656 ? O9 C16 1.441(13) . ? O9 C19 1.447(11) . ? C16 C17 1.493(12) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.546(15) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.515(12) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? O9' C19' 1.448(17) . ? O9' C16' 1.448(17) . ? C16' C17' 1.518(18) . ? C16' H16C 0.9900 . ? C16' H16D 0.9900 . ? C17' C18' 1.55(2) . ? C17' H17C 0.9900 . ? C17' H17D 0.9900 . ? C18' C19' 1.518(18) . ? C18' H18C 0.9900 . ? C18' H18D 0.9900 . ? C19' H19C 0.9900 . ? C19' H19D 0.9900 . ? C20 C21 1.467(12) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.457(14) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.539(12) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Zn1 O4 89.6(2) . . ? O5 Zn1 Fe1 121.68(16) . 3 ? O4 Zn1 Fe1 128.99(15) . 3 ? O5 Zn1 C2 100.0(3) . . ? O4 Zn1 C2 96.1(2) . . ? Fe1 Zn1 C2 114.0(2) 3 . ? O5 Zn1 Fe1 134.25(17) . . ? O4 Zn1 Fe1 113.17(15) . . ? Fe1 Zn1 Fe1 74.74(5) 3 . ? C2 Zn1 Fe1 41.3(2) . . ? O5 Zn1 Zn2 167.70(17) . 3 ? O4 Zn1 Zn2 84.58(15) . 3 ? Fe1 Zn1 Zn2 56.05(4) 3 3 ? C2 Zn1 Zn2 91.4(2) . 3 ? Fe1 Zn1 Zn2 58.02(3) . 3 ? O5 Zn1 Zn2 95.89(15) . . ? O4 Zn1 Zn2 166.42(15) . . ? Fe1 Zn1 Zn2 57.42(4) 3 . ? C2 Zn1 Zn2 70.7(2) . . ? Fe1 Zn1 Zn2 54.66(4) . . ? Zn2 Zn1 Zn2 92.15(4) 3 . ? C12 Zn2 Fe1 140.6(3) . . ? C12 Zn2 C3 107.0(3) . . ? Fe1 Zn2 C3 112.2(2) . . ? C12 Zn2 Fe1 146.5(3) . 3 ? Fe1 Zn2 Fe1 72.67(5) . 3 ? C3 Zn2 Fe1 40.3(2) . 3 ? C12 Zn2 Zn1 132.7(3) . 3 ? Fe1 Zn2 Zn1 54.88(4) . 3 ? C3 Zn2 Zn1 85.5(2) . 3 ? Fe1 Zn2 Zn1 55.12(4) 3 3 ? C12 Zn2 Zn1 139.3(3) . . ? Fe1 Zn2 Zn1 55.03(4) . . ? C3 Zn2 Zn1 73.6(2) . . ? Fe1 Zn2 Zn1 53.13(4) 3 . ? Zn1 Zn2 Zn1 87.85(4) 3 . ? C2 Fe1 C1 99.4(4) . . ? C2 Fe1 C3 99.1(4) . 3 ? C1 Fe1 C3 100.2(4) . 3 ? C2 Fe1 Zn1 161.6(3) . 3 ? C1 Fe1 Zn1 75.4(3) . 3 ? C3 Fe1 Zn1 99.2(3) 3 3 ? C2 Fe1 Zn2 92.6(3) . . ? C1 Fe1 Zn2 76.6(3) . . ? C3 Fe1 Zn2 168.3(3) 3 . ? Zn1 Fe1 Zn2 69.07(5) 3 . ? C2 Fe1 Zn1 68.3(3) . . ? C1 Fe1 Zn1 143.7(3) . . ? C3 Fe1 Zn1 115.2(3) 3 . ? Zn1 Fe1 Zn1 105.26(5) 3 . ? Zn2 Fe1 Zn1 70.31(4) . . ? C2 Fe1 Zn2 120.0(3) . 3 ? C1 Fe1 Zn2 139.8(3) . 3 ? C3 Fe1 Zn2 67.7(3) 3 3 ? Zn1 Fe1 Zn2 69.46(4) 3 3 ? Zn2 Fe1 Zn2 107.33(5) . 3 ? Zn1 Fe1 Zn2 66.86(4) . 3 ? C7 O4 C4 108.4(6) . . ? C7 O4 Zn1 125.3(4) . . ? C4 O4 Zn1 126.2(5) . . ? C11 O5 C8 109.4(6) . . ? C11 O5 Zn1 123.0(5) . . ? C8 O5 Zn1 123.6(5) . . ? O1 C1 Fe1 173.4(7) . . ? O2 C2 Fe1 173.1(8) . . ? O2 C2 Zn1 115.9(6) . . ? Fe1 C2 Zn1 70.4(3) . . ? O3 C3 Fe1 168.2(8) . 3 ? O3 C3 Zn2 119.9(7) . . ? Fe1 C3 Zn2 71.9(3) 3 . ? O4 C4 C5 106.4(7) . . ? O4 C4 H4A 110.4 . . ? C5 C4 H4A 110.4 . . ? O4 C4 H4B 110.4 . . ? C5 C4 H4B 110.4 . . ? H4A C4 H4B 108.6 . . ? C4 C5 C6 104.1(7) . . ? C4 C5 H5A 110.9 . . ? C6 C5 H5A 110.9 . . ? C4 C5 H5B 110.9 . . ? C6 C5 H5B 110.9 . . ? H5A C5 H5B 109.0 . . ? C7 C6 C5 103.6(7) . . ? C7 C6 H6A 111.0 . . ? C5 C6 H6A 111.0 . . ? C7 C6 H6B 111.0 . . ? C5 C6 H6B 111.0 . . ? H6A C6 H6B 109.0 . . ? O4 C7 C6 106.6(7) . . ? O4 C7 H7A 110.4 . . ? C6 C7 H7A 110.4 . . ? O4 C7 H7B 110.4 . . ? C6 C7 H7B 110.4 . . ? H7A C7 H7B 108.6 . . ? O5 C8 C9 104.3(7) . . ? O5 C8 H8A 110.9 . . ? C9 C8 H8A 110.9 . . ? O5 C8 H8B 110.9 . . ? C9 C8 H8B 110.9 . . ? H8A C8 H8B 108.9 . . ? C8 C9 C10 102.6(8) . . ? C8 C9 H9A 111.3 . . ? C10 C9 H9A 111.3 . . ? C8 C9 H9B 111.3 . . ? C10 C9 H9B 111.3 . . ? H9A C9 H9B 109.2 . . ? C9 C10 C11 102.5(8) . . ? C9 C10 H10A 111.3 . . ? C11 C10 H10A 111.3 . . ? C9 C10 H10B 111.3 . . ? C11 C10 H10B 111.3 . . ? H10A C10 H10B 109.2 . . ? O5 C11 C10 104.8(7) . . ? O5 C11 H11A 110.8 . . ? C10 C11 H11A 110.8 . . ? O5 C11 H11B 110.8 . . ? C10 C11 H11B 110.8 . . ? H11A C11 H11B 108.9 . . ? Zn2 C12 H12A 109.5 . . ? Zn2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Zn2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O9' Zn3 O9 9.5(19) . . ? O9' Zn3 O10 87.4(16) . . ? O9 Zn3 O10 90.3(4) . . ? O9' Zn3 Fe2 128.0(12) . . ? O9 Zn3 Fe2 134.0(3) . . ? O10 Zn3 Fe2 115.09(16) . . ? O9' Zn3 Fe2 127.4(18) . 3_656 ? O9 Zn3 Fe2 119.2(3) . 3_656 ? O10 Zn3 Fe2 129.39(17) . 3_656 ? Fe2 Zn3 Fe2 74.57(5) . 3_656 ? O9' Zn3 C15 108.8(15) . . ? O9 Zn3 C15 99.4(4) . . ? O10 Zn3 C15 97.5(3) . . ? Fe2 Zn3 C15 113.3(2) . . ? Fe2 Zn3 C15 41.7(2) 3_656 . ? O9' Zn3 C13 89.3(13) . . ? O9 Zn3 C13 97.0(4) . . ? O10 Zn3 C13 108.0(3) . . ? Fe2 Zn3 C13 40.3(2) . . ? Fe2 Zn3 C13 107.8(2) 3_656 . ? C15 Zn3 C13 149.5(3) . . ? O9' Zn3 Zn4 172.2(13) . . ? O9 Zn3 Zn4 166.9(3) . . ? O10 Zn3 Zn4 85.56(16) . . ? Fe2 Zn3 Zn4 58.56(4) . . ? Fe2 Zn3 Zn4 56.15(4) 3_656 . ? C15 Zn3 Zn4 68.9(2) . . ? C13 Zn3 Zn4 96.1(2) . . ? O9' Zn3 Zn4 95.5(15) . 3_656 ? O9 Zn3 Zn4 94.4(3) . 3_656 ? O10 Zn3 Zn4 168.14(16) . 3_656 ? Fe2 Zn3 Zn4 54.46(4) . 3_656 ? Fe2 Zn3 Zn4 56.70(4) 3_656 3_656 ? C15 Zn3 Zn4 92.5(2) . 3_656 ? C13 Zn3 Zn4 60.7(2) . 3_656 ? Zn4 Zn3 Zn4 92.07(4) . 3_656 ? C24 Zn4 Fe2 143.7(3) . 3_656 ? C24 Zn4 C14 103.5(3) . . ? Fe2 Zn4 C14 112.7(2) 3_656 . ? C24 Zn4 Fe2 143.7(3) . . ? Fe2 Zn4 Fe2 72.57(5) 3_656 . ? C14 Zn4 Fe2 40.3(2) . . ? C24 Zn4 Zn3 133.7(3) . . ? Fe2 Zn4 Zn3 55.89(4) 3_656 . ? C14 Zn4 Zn3 77.2(2) . . ? Fe2 Zn4 Zn3 54.85(4) . . ? C24 Zn4 Zn3 138.4(3) . 3_656 ? Fe2 Zn4 Zn3 54.01(4) 3_656 3_656 ? C14 Zn4 Zn3 82.2(2) . 3_656 ? Fe2 Zn4 Zn3 53.43(4) . 3_656 ? Zn3 Zn4 Zn3 87.93(4) . 3_656 ? C13 Fe2 C14 99.3(4) . . ? C13 Fe2 C15 99.7(4) . 3_656 ? C14 Fe2 C15 99.2(4) . 3_656 ? C13 Fe2 Zn3 72.3(3) . . ? C14 Fe2 Zn3 101.7(3) . . ? C15 Fe2 Zn3 158.6(3) 3_656 . ? C13 Fe2 Zn3 146.1(3) . 3_656 ? C14 Fe2 Zn3 114.0(3) . 3_656 ? C15 Fe2 Zn3 69.8(3) 3_656 3_656 ? Zn3 Fe2 Zn3 105.43(5) . 3_656 ? C13 Fe2 Zn4 79.8(3) . 3_656 ? C14 Fe2 Zn4 173.1(3) . 3_656 ? C15 Fe2 Zn4 87.7(3) 3_656 3_656 ? Zn3 Fe2 Zn4 71.53(4) . 3_656 ? Zn3 Fe2 Zn4 67.95(5) 3_656 3_656 ? C13 Fe2 Zn4 132.6(3) . . ? C14 Fe2 Zn4 68.1(3) . . ? C15 Fe2 Zn4 126.8(3) 3_656 . ? Zn3 Fe2 Zn4 66.60(4) . . ? Zn3 Fe2 Zn4 69.87(5) 3_656 . ? Zn4 Fe2 Zn4 107.43(5) 3_656 . ? C13 Fe2 Fe2 115.8(3) . 3_656 ? C14 Fe2 Fe2 120.2(3) . 3_656 ? C15 Fe2 Fe2 118.8(3) 3_656 3_656 ? Zn3 Fe2 Fe2 52.82(4) . 3_656 ? Zn3 Fe2 Fe2 52.62(4) 3_656 3_656 ? Zn4 Fe2 Fe2 55.15(5) 3_656 3_656 ? Zn4 Fe2 Fe2 52.28(4) . 3_656 ? C23 O10 C20 108.0(6) . . ? C23 O10 Zn3 123.9(5) . . ? C20 O10 Zn3 128.1(5) . . ? O6 C13 Fe2 172.6(9) . . ? O6 C13 Zn3 119.2(7) . . ? Fe2 C13 Zn3 67.4(3) . . ? O7 C14 Fe2 171.7(8) . . ? O7 C14 Zn4 116.7(7) . . ? Fe2 C14 Zn4 71.6(3) . . ? O8 C15 Fe2 173.7(7) . 3_656 ? O8 C15 Zn3 117.7(6) . . ? Fe2 C15 Zn3 68.5(3) 3_656 . ? C16 O9 C19 110.9(8) . . ? C16 O9 Zn3 119.8(7) . . ? C19 O9 Zn3 124.2(8) . . ? O9 C16 C17 105.4(8) . . ? O9 C16 H16A 110.7 . . ? C17 C16 H16A 110.7 . . ? O9 C16 H16B 110.7 . . ? C17 C16 H16B 110.7 . . ? H16A C16 H16B 108.8 . . ? C16 C17 C18 101.1(9) . . ? C16 C17 H17A 111.6 . . ? C18 C17 H17A 111.6 . . ? C16 C17 H17B 111.6 . . ? C18 C17 H17B 111.6 . . ? H17A C17 H17B 109.4 . . ? C19 C18 C17 102.7(9) . . ? C19 C18 H18A 111.2 . . ? C17 C18 H18A 111.2 . . ? C19 C18 H18B 111.2 . . ? C17 C18 H18B 111.2 . . ? H18A C18 H18B 109.2 . . ? O9 C19 C18 104.1(8) . . ? O9 C19 H19A 110.9 . . ? C18 C19 H19A 110.9 . . ? O9 C19 H19B 110.9 . . ? C18 C19 H19B 110.9 . . ? H19A C19 H19B 108.9 . . ? C19' O9' C16' 110.6(18) . . ? C19' O9' Zn3 124(3) . . ? C16' O9' Zn3 123(3) . . ? O9' C16' C17' 103(2) . . ? O9' C16' H16C 111.2 . . ? C17' C16' H16C 111.2 . . ? O9' C16' H16D 111.2 . . ? C17' C16' H16D 111.2 . . ? H16C C16' H16D 109.1 . . ? C16' C17' C18' 98(2) . . ? C16' C17' H17C 112.1 . . ? C18' C17' H17C 112.1 . . ? C16' C17' H17D 112.1 . . ? C18' C17' H17D 112.1 . . ? H17C C17' H17D 109.8 . . ? C19' C18' C17' 102(2) . . ? C19' C18' H18C 111.4 . . ? C17' C18' H18C 111.4 . . ? C19' C18' H18D 111.4 . . ? C17' C18' H18D 111.4 . . ? H18C C18' H18D 109.3 . . ? O9' C19' C18' 103.6(18) . . ? O9' C19' H19C 111.0 . . ? C18' C19' H19C 111.0 . . ? O9' C19' H19D 111.0 . . ? C18' C19' H19D 111.0 . . ? H19C C19' H19D 109.0 . . ? O10 C20 C21 107.0(8) . . ? O10 C20 H20A 110.3 . . ? C21 C20 H20A 110.3 . . ? O10 C20 H20B 110.3 . . ? C21 C20 H20B 110.3 . . ? H20A C20 H20B 108.6 . . ? C22 C21 C20 103.8(8) . . ? C22 C21 H21A 111.0 . . ? C20 C21 H21A 111.0 . . ? C22 C21 H21B 111.0 . . ? C20 C21 H21B 111.0 . . ? H21A C21 H21B 109.0 . . ? C21 C22 C23 102.3(8) . . ? C21 C22 H22A 111.3 . . ? C23 C22 H22A 111.3 . . ? C21 C22 H22B 111.3 . . ? C23 C22 H22B 111.3 . . ? H22A C22 H22B 109.2 . . ? O10 C23 C22 103.4(7) . . ? O10 C23 H23A 111.1 . . ? C22 C23 H23A 111.1 . . ? O10 C23 H23B 111.1 . . ? C22 C23 H23B 111.1 . . ? H23A C23 H23B 109.0 . . ? Zn4 C24 H24A 109.5 . . ? Zn4 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Zn4 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.655 _refine_diff_density_min -0.824 _refine_diff_density_rms 0.152 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.301 0.000 -0.199 488 107 '4 tetrahydrofurane' 2 0.853 0.500 0.853 488 107 '4 tetrahydrofurane' _platon_squeeze_details ; ; data_3 _database_code_depnum_ccdc_archive 'CCDC 836633' #TrackingRef '- 1-5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H30 Fe2 N6 O6 Zn3' _chemical_formula_sum 'C36 H30 Fe2 N6 O6 Zn3' _chemical_formula_weight 950.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 20.0442(8) _cell_length_b 10.0158(4) _cell_length_c 18.6317(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3740.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 10223 _cell_measurement_theta_min 2.8694 _cell_measurement_theta_max 28.9522 _exptl_crystal_description prism _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.688 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1912 _exptl_absorpt_coefficient_mu 2.706 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6562 _exptl_absorpt_correction_T_max 0.7928 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur^TM^2, Oxford Diffraction' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.4171 _diffrn_reflns_number 46685 _diffrn_reflns_av_R_equivalents 0.0801 _diffrn_reflns_av_sigmaI/netI 0.0647 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8459 _reflns_number_gt 6942 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material 'enCIFer (Allen et al, 2004)' _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^)+(0.0259P)^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 0.407(11) _refine_ls_number_reflns 8459 _refine_ls_number_parameters 479 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0603 _refine_ls_R_factor_gt 0.0396 _refine_ls_wR_factor_ref 0.0710 _refine_ls_wR_factor_gt 0.0644 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _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 Fe1 Fe 0.56116(3) 0.55640(6) 0.55055(3) 0.01470(13) Uani 1 1 d . . . Fe2 Fe 0.68552(3) 0.39108(6) 0.59508(3) 0.01507(13) Uani 1 1 d . . . Zn1 Zn 0.58070(2) 0.31533(5) 0.54191(3) 0.01738(11) Uani 1 1 d . . . Zn2 Zn 0.60030(2) 0.49266(5) 0.67023(3) 0.01680(11) Uani 1 1 d . . . Zn3 Zn 0.67868(2) 0.58475(5) 0.51641(3) 0.01865(12) Uani 1 1 d . . . N1 N 0.59150(18) 0.1907(4) 0.4482(2) 0.0221(9) Uani 1 1 d . . . N2 N 0.50593(17) 0.1859(3) 0.5824(2) 0.0202(8) Uani 1 1 d . . . N3 N 0.55951(19) 0.3663(4) 0.7496(2) 0.0209(9) Uani 1 1 d . . . N4 N 0.61711(17) 0.6498(3) 0.74366(19) 0.0181(8) Uani 1 1 d . . . N5 N 0.69134(18) 0.5812(4) 0.3988(2) 0.0219(9) Uani 1 1 d . . . N6 N 0.75099(17) 0.7393(3) 0.5242(2) 0.0224(9) Uani 1 1 d . . . O1 O 0.45827(15) 0.6197(3) 0.65589(17) 0.0283(8) Uani 1 1 d . . . O2 O 0.58237(15) 0.8238(3) 0.49322(17) 0.0236(7) Uani 1 1 d . . . O3 O 0.47762(16) 0.4551(3) 0.43499(18) 0.0303(8) Uani 1 1 d . . . O4 O 0.75762(16) 0.4959(4) 0.71824(17) 0.0343(9) Uani 1 1 d . . . O5 O 0.66919(17) 0.1106(3) 0.63289(19) 0.0346(9) Uani 1 1 d . . . O6 O 0.79332(16) 0.3658(3) 0.49146(17) 0.0304(8) Uani 1 1 d . . . C1 C 0.5030(2) 0.5886(4) 0.6176(2) 0.0201(10) Uani 1 1 d . . . C2 C 0.57928(19) 0.7143(4) 0.5178(2) 0.0189(10) Uani 1 1 d . . . C3 C 0.5151(2) 0.4872(4) 0.4808(2) 0.0217(10) Uani 1 1 d . . . C4 C 0.7256(2) 0.4596(4) 0.6685(3) 0.0211(10) Uani 1 1 d . . . C5 C 0.6717(2) 0.2257(5) 0.6165(2) 0.0233(11) Uani 1 1 d . . . C6 C 0.7473(2) 0.3815(4) 0.5301(2) 0.0189(10) Uani 1 1 d . . . C7 C 0.6514(2) 0.1408(4) 0.4317(3) 0.0230(10) Uani 1 1 d . . . H7A H 0.6867 0.1506 0.4653 0.028 Uiso 1 1 calc R . . C8 C 0.6643(3) 0.0761(5) 0.3681(3) 0.0348(13) Uani 1 1 d . . . H8A H 0.7075 0.0416 0.3581 0.042 Uiso 1 1 calc R . . C9 C 0.6139(3) 0.0624(6) 0.3197(3) 0.0455(16) Uani 1 1 d . . . H9A H 0.6216 0.0181 0.2754 0.055 Uiso 1 1 calc R . . C10 C 0.5520(3) 0.1129(6) 0.3353(3) 0.0489(16) Uani 1 1 d . . . H10A H 0.5163 0.1047 0.3020 0.059 Uiso 1 1 calc R . . C11 C 0.5427(2) 0.1758(5) 0.4003(3) 0.0360(13) Uani 1 1 d . . . H11A H 0.4997 0.2100 0.4114 0.043 Uiso 1 1 calc R . . C12 C 0.5139(2) 0.0558(4) 0.5830(3) 0.0278(11) Uani 1 1 d . . . H12A H 0.5553 0.0206 0.5670 0.033 Uiso 1 1 calc R . . C13 C 0.4656(3) -0.0326(5) 0.6057(3) 0.0327(13) Uani 1 1 d . . . H13A H 0.4739 -0.1260 0.6062 0.039 Uiso 1 1 calc R . . C14 C 0.4054(3) 0.0173(5) 0.6274(3) 0.0311(12) Uani 1 1 d . . . H14A H 0.3706 -0.0411 0.6419 0.037 Uiso 1 1 calc R . . C15 C 0.3960(2) 0.1522(5) 0.6277(3) 0.0283(12) Uani 1 1 d . . . H15A H 0.3548 0.1890 0.6432 0.034 Uiso 1 1 calc R . . C16 C 0.4471(2) 0.2345(5) 0.6053(2) 0.0265(11) Uani 1 1 d . . . H16A H 0.4406 0.3284 0.6061 0.032 Uiso 1 1 calc R . . C17 C 0.5980(3) 0.2720(6) 0.7778(3) 0.0518(17) Uani 1 1 d . . . H17A H 0.6418 0.2609 0.7592 0.062 Uiso 1 1 calc R . . C18 C 0.5776(4) 0.1903(6) 0.8321(4) 0.073(3) Uani 1 1 d . . . H18A H 0.6073 0.1255 0.8513 0.088 Uiso 1 1 calc R . . C19 C 0.5148(3) 0.2015(5) 0.8589(3) 0.0486(16) Uani 1 1 d . . . H19A H 0.4992 0.1434 0.8955 0.058 Uiso 1 1 calc R . . C20 C 0.4750(3) 0.2990(6) 0.8313(3) 0.0381(14) Uani 1 1 d . . . H20A H 0.4311 0.3117 0.8493 0.046 Uiso 1 1 calc R . . C21 C 0.4991(2) 0.3791(5) 0.7768(3) 0.0310(12) Uani 1 1 d . . . H21A H 0.4708 0.4467 0.7580 0.037 Uiso 1 1 calc R . . C22 C 0.6302(3) 0.7694(5) 0.7167(3) 0.0320(12) Uani 1 1 d . . . H22A H 0.6246 0.7831 0.6666 0.038 Uiso 1 1 calc R . . C23 C 0.6517(3) 0.8741(5) 0.7581(3) 0.0392(14) Uani 1 1 d . . . H23A H 0.6602 0.9589 0.7371 0.047 Uiso 1 1 calc R . . C24 C 0.6606(3) 0.8545(5) 0.8298(3) 0.0342(13) Uani 1 1 d . . . H24A H 0.6770 0.9250 0.8591 0.041 Uiso 1 1 calc R . . C25 C 0.6460(2) 0.7333(5) 0.8594(2) 0.0278(12) Uani 1 1 d . . . H25A H 0.6502 0.7190 0.9096 0.033 Uiso 1 1 calc R . . C26 C 0.6251(2) 0.6327(5) 0.8146(2) 0.0260(11) Uani 1 1 d . . . H26A H 0.6160 0.5474 0.8346 0.031 Uiso 1 1 calc R . . C27 C 0.7142(2) 0.6802(5) 0.3571(3) 0.0330(13) Uani 1 1 d . . . H27A H 0.7313 0.7584 0.3792 0.040 Uiso 1 1 calc R . . C28 C 0.7137(2) 0.6725(6) 0.2830(3) 0.0403(15) Uani 1 1 d . . . H28A H 0.7305 0.7441 0.2549 0.048 Uiso 1 1 calc R . . C29 C 0.6890(3) 0.5609(6) 0.2509(3) 0.0447(15) Uani 1 1 d . . . H29A H 0.6881 0.5534 0.2001 0.054 Uiso 1 1 calc R . . C30 C 0.6652(3) 0.4591(5) 0.2936(3) 0.0399(14) Uani 1 1 d . . . H30A H 0.6476 0.3801 0.2728 0.048 Uiso 1 1 calc R . . C31 C 0.6677(3) 0.4744(5) 0.3661(3) 0.0351(13) Uani 1 1 d . . . H31A H 0.6512 0.4036 0.3951 0.042 Uiso 1 1 calc R . . C32 C 0.7366(2) 0.8660(4) 0.5399(3) 0.0254(10) Uani 1 1 d . . . H32A H 0.6916 0.8888 0.5500 0.030 Uiso 1 1 calc R . . C33 C 0.7840(2) 0.9650(4) 0.5422(3) 0.0307(11) Uani 1 1 d . . . H33A H 0.7720 1.0538 0.5545 0.037 Uiso 1 1 calc R . . C34 C 0.8488(2) 0.9339(5) 0.5264(3) 0.0326(13) Uani 1 1 d . . . H34A H 0.8822 1.0013 0.5260 0.039 Uiso 1 1 calc R . . C35 C 0.8649(2) 0.8028(5) 0.5109(3) 0.0363(12) Uani 1 1 d . . . H35A H 0.9097 0.7780 0.5006 0.044 Uiso 1 1 calc R . . C36 C 0.8149(2) 0.7090(5) 0.5107(3) 0.0287(11) Uani 1 1 d . . . H36A H 0.8261 0.6188 0.5006 0.034 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 Fe1 0.0137(3) 0.0163(3) 0.0141(3) -0.0014(3) -0.0006(3) -0.0003(2) Fe2 0.0148(3) 0.0177(3) 0.0127(3) -0.0010(3) 0.0010(3) 0.0010(3) Zn1 0.0172(2) 0.0167(2) 0.0182(3) -0.0030(3) 0.0007(2) -0.0005(2) Zn2 0.0158(2) 0.0211(3) 0.0135(2) -0.0017(2) 0.0010(2) 0.0011(2) Zn3 0.0157(3) 0.0202(3) 0.0201(3) 0.0029(2) 0.0012(2) -0.0005(2) N1 0.024(2) 0.021(2) 0.022(2) -0.0066(18) 0.0054(17) -0.0002(17) N2 0.0174(19) 0.020(2) 0.023(2) 0.0006(18) 0.0027(16) -0.0013(15) N3 0.024(2) 0.022(2) 0.017(2) -0.0025(18) 0.0036(17) -0.0022(17) N4 0.020(2) 0.019(2) 0.015(2) 0.0004(17) 0.0025(15) 0.0002(16) N5 0.018(2) 0.024(2) 0.024(2) 0.0047(18) 0.0049(16) 0.0014(16) N6 0.019(2) 0.025(2) 0.024(2) 0.0024(18) -0.0016(16) -0.0041(15) O1 0.0219(18) 0.035(2) 0.028(2) 0.0003(16) 0.0079(15) 0.0093(15) O2 0.0259(18) 0.0137(16) 0.0310(19) 0.0042(15) -0.0023(15) 0.0008(13) O3 0.030(2) 0.0301(19) 0.030(2) -0.0073(16) -0.0172(16) -0.0033(15) O4 0.0233(19) 0.053(2) 0.026(2) -0.0158(18) -0.0080(15) 0.0070(17) O5 0.039(2) 0.0209(19) 0.044(2) 0.0068(17) -0.0054(17) 0.0018(16) O6 0.0261(19) 0.041(2) 0.0243(19) -0.0004(16) 0.0108(15) 0.0067(15) C1 0.017(2) 0.021(2) 0.023(3) 0.007(2) -0.0060(19) 0.0021(18) C2 0.013(2) 0.026(2) 0.018(2) -0.011(2) -0.0008(18) 0.0032(18) C3 0.018(2) 0.018(2) 0.030(3) 0.002(2) 0.001(2) 0.0016(19) C4 0.015(2) 0.027(3) 0.022(2) 0.000(2) 0.005(2) 0.0077(18) C5 0.022(3) 0.026(3) 0.021(3) -0.007(2) -0.0021(19) 0.004(2) C6 0.022(2) 0.021(2) 0.013(2) -0.0009(19) -0.0025(18) -0.0026(18) C7 0.020(2) 0.026(3) 0.024(3) -0.006(2) 0.0026(19) -0.003(2) C8 0.034(3) 0.038(3) 0.032(3) -0.010(3) 0.012(2) -0.003(2) C9 0.055(4) 0.053(4) 0.029(3) -0.028(3) 0.009(3) 0.001(3) C10 0.041(4) 0.063(4) 0.043(4) -0.028(3) -0.013(3) -0.002(3) C11 0.023(3) 0.042(3) 0.042(3) -0.021(3) -0.002(2) -0.004(2) C12 0.024(3) 0.020(2) 0.040(3) -0.011(2) 0.010(2) 0.000(2) C13 0.033(3) 0.019(2) 0.046(3) 0.000(2) 0.006(2) -0.009(2) C14 0.036(3) 0.034(3) 0.023(3) -0.004(2) 0.004(2) -0.019(2) C15 0.020(3) 0.037(3) 0.028(3) -0.008(2) 0.005(2) -0.007(2) C16 0.032(3) 0.024(3) 0.023(3) -0.004(2) 0.003(2) -0.004(2) C17 0.055(4) 0.051(4) 0.049(4) 0.023(3) 0.027(3) 0.026(3) C18 0.093(6) 0.063(5) 0.063(5) 0.040(4) 0.051(4) 0.052(4) C19 0.075(5) 0.029(3) 0.042(4) 0.005(3) 0.030(3) -0.002(3) C20 0.024(3) 0.057(4) 0.033(3) 0.007(3) 0.008(2) -0.008(3) C21 0.023(3) 0.040(3) 0.030(3) 0.011(3) 0.004(2) 0.006(2) C22 0.045(3) 0.030(3) 0.021(3) 0.003(2) -0.006(2) -0.005(2) C23 0.070(4) 0.021(3) 0.027(3) 0.004(2) -0.014(3) -0.006(3) C24 0.049(4) 0.025(3) 0.029(3) -0.006(2) -0.014(3) -0.007(2) C25 0.037(3) 0.034(3) 0.013(2) -0.003(2) -0.003(2) -0.008(2) C26 0.034(3) 0.026(3) 0.018(3) 0.002(2) 0.005(2) -0.006(2) C27 0.026(3) 0.038(3) 0.035(3) 0.015(3) -0.005(2) -0.008(2) C28 0.026(3) 0.064(4) 0.030(3) 0.027(3) -0.002(2) -0.010(3) C29 0.037(4) 0.075(4) 0.022(3) 0.001(3) 0.005(2) 0.009(3) C30 0.058(4) 0.037(3) 0.025(3) -0.004(3) 0.003(3) 0.000(3) C31 0.052(4) 0.031(3) 0.023(3) 0.002(2) 0.011(2) -0.002(3) C32 0.023(2) 0.026(2) 0.028(3) 0.000(2) 0.000(2) -0.0016(19) C33 0.026(3) 0.028(3) 0.038(3) -0.001(3) -0.008(2) -0.0068(19) C34 0.022(3) 0.032(3) 0.043(4) -0.004(3) -0.001(2) -0.010(2) C35 0.018(2) 0.044(3) 0.047(3) -0.003(3) 0.000(2) -0.002(2) C36 0.016(2) 0.031(3) 0.039(3) 0.003(3) -0.002(2) -0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C2 1.734(5) . ? Fe1 C3 1.738(5) . ? Fe1 C1 1.740(5) . ? Fe1 Zn2 2.4485(8) . ? Fe1 Zn1 2.4513(7) . ? Fe1 Zn3 2.4563(7) . ? Fe2 C5 1.727(5) . ? Fe2 C4 1.728(5) . ? Fe2 C6 1.734(4) . ? Fe2 Zn2 2.4318(8) . ? Fe2 Zn3 2.4352(8) . ? Fe2 Zn1 2.4436(8) . ? Zn1 N2 2.121(3) . ? Zn1 N1 2.158(4) . ? Zn1 C3 2.448(4) . ? Zn1 C5 2.462(5) . ? Zn1 Zn2 3.0042(7) . ? Zn2 N3 2.111(4) . ? Zn2 N4 2.112(4) . ? Zn2 C1 2.385(4) . ? Zn2 C4 2.534(4) . ? Zn3 N6 2.126(3) . ? Zn3 N5 2.205(4) . ? Zn3 C2 2.378(4) . ? Zn3 C6 2.471(4) . ? N1 C11 1.332(6) . ? N1 C7 1.337(5) . ? N2 C12 1.312(5) . ? N2 C16 1.345(6) . ? N3 C21 1.318(6) . ? N3 C17 1.328(6) . ? N4 C22 1.326(6) . ? N4 C26 1.342(6) . ? N5 C31 1.319(6) . ? N5 C27 1.341(6) . ? N6 C32 1.334(5) . ? N6 C36 1.341(5) . ? O1 C1 1.187(5) . ? O2 C2 1.190(5) . ? O3 C3 1.181(5) . ? O4 C4 1.184(5) . ? O5 C5 1.194(6) . ? O6 C6 1.181(5) . ? C7 C8 1.375(7) . ? C7 H7A 0.9500 . ? C8 C9 1.361(7) . ? C8 H8A 0.9500 . ? C9 C10 1.372(8) . ? C9 H9A 0.9500 . ? C10 C11 1.378(7) . ? C10 H10A 0.9500 . ? C11 H11A 0.9500 . ? C12 C13 1.379(6) . ? C12 H12A 0.9500 . ? C13 C14 1.367(7) . ? C13 H13A 0.9500 . ? C14 C15 1.364(7) . ? C14 H14A 0.9500 . ? C15 C16 1.380(6) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C17 C18 1.365(8) . ? C17 H17A 0.9500 . ? C18 C19 1.358(8) . ? C18 H18A 0.9500 . ? C19 C20 1.361(8) . ? C19 H19A 0.9500 . ? C20 C21 1.382(7) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? C22 C23 1.371(7) . ? C22 H22A 0.9500 . ? C23 C24 1.363(7) . ? C23 H23A 0.9500 . ? C24 C25 1.365(6) . ? C24 H24A 0.9500 . ? C25 C26 1.375(6) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? C27 C28 1.383(7) . ? C27 H27A 0.9500 . ? C28 C29 1.361(8) . ? C28 H28A 0.9500 . ? C29 C30 1.377(7) . ? C29 H29A 0.9500 . ? C30 C31 1.361(7) . ? C30 H30A 0.9500 . ? C31 H31A 0.9500 . ? C32 C33 1.374(6) . ? C32 H32A 0.9500 . ? C33 C34 1.368(6) . ? C33 H33A 0.9500 . ? C34 C35 1.383(6) . ? C34 H34A 0.9500 . ? C35 C36 1.373(6) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Fe1 C3 102.2(2) . . ? C2 Fe1 C1 102.9(2) . . ? C3 Fe1 C1 104.8(2) . . ? C2 Fe1 Zn2 119.42(14) . . ? C3 Fe1 Zn2 138.34(14) . . ? C1 Fe1 Zn2 66.96(14) . . ? C2 Fe1 Zn1 147.35(14) . . ? C3 Fe1 Zn1 69.10(14) . . ? C1 Fe1 Zn1 109.70(15) . . ? Zn2 Fe1 Zn1 75.63(2) . . ? C2 Fe1 Zn3 66.58(13) . . ? C3 Fe1 Zn3 111.24(15) . . ? C1 Fe1 Zn3 143.84(15) . . ? Zn2 Fe1 Zn3 87.64(3) . . ? Zn1 Fe1 Zn3 86.77(2) . . ? C5 Fe2 C4 105.9(2) . . ? C5 Fe2 C6 102.9(2) . . ? C4 Fe2 C6 103.99(19) . . ? C5 Fe2 Zn2 98.96(15) . . ? C4 Fe2 Zn2 72.85(14) . . ? C6 Fe2 Zn2 157.92(14) . . ? C5 Fe2 Zn3 153.42(15) . . ? C4 Fe2 Zn3 100.72(15) . . ? C6 Fe2 Zn3 70.39(13) . . ? Zn2 Fe2 Zn3 88.50(3) . . ? C5 Fe2 Zn1 69.97(15) . . ? C4 Fe2 Zn1 147.57(14) . . ? C6 Fe2 Zn1 108.29(14) . . ? Zn2 Fe2 Zn1 76.08(2) . . ? Zn3 Fe2 Zn1 87.41(3) . . ? N2 Zn1 N1 90.30(14) . . ? N2 Zn1 Fe2 130.78(10) . . ? N1 Zn1 Fe2 114.94(10) . . ? N2 Zn1 C3 102.46(14) . . ? N1 Zn1 C3 94.84(15) . . ? Fe2 Zn1 C3 115.61(11) . . ? N2 Zn1 Fe1 117.78(10) . . ? N1 Zn1 Fe1 129.72(10) . . ? Fe2 Zn1 Fe1 78.75(2) . . ? C3 Zn1 Fe1 41.57(11) . . ? N2 Zn1 C5 95.71(15) . . ? N1 Zn1 C5 99.88(14) . . ? Fe2 Zn1 C5 41.21(11) . . ? C3 Zn1 C5 156.51(16) . . ? Fe1 Zn1 C5 116.14(11) . . ? N2 Zn1 Zn2 99.83(10) . . ? N1 Zn1 Zn2 166.69(10) . . ? Fe2 Zn1 Zn2 51.783(19) . . ? C3 Zn1 Zn2 91.40(11) . . ? Fe1 Zn1 Zn2 52.14(2) . . ? C5 Zn1 Zn2 70.71(11) . . ? N3 Zn2 N4 93.13(14) . . ? N3 Zn2 C1 102.28(15) . . ? N4 Zn2 C1 95.53(15) . . ? N3 Zn2 Fe2 115.12(10) . . ? N4 Zn2 Fe2 124.93(10) . . ? C1 Zn2 Fe2 120.43(11) . . ? N3 Zn2 Fe1 132.07(11) . . ? N4 Zn2 Fe1 116.54(10) . . ? C1 Zn2 Fe1 42.16(11) . . ? Fe2 Zn2 Fe1 79.03(3) . . ? N3 Zn2 C4 108.35(15) . . ? N4 Zn2 C4 86.99(14) . . ? C1 Zn2 C4 149.09(16) . . ? Fe2 Zn2 C4 40.67(11) . . ? Fe1 Zn2 C4 109.87(11) . . ? N3 Zn2 Zn1 98.77(10) . . ? N4 Zn2 Zn1 167.63(10) . . ? C1 Zn2 Zn1 78.72(11) . . ? Fe2 Zn2 Zn1 52.139(19) . . ? Fe1 Zn2 Zn1 52.226(19) . . ? C4 Zn2 Zn1 92.41(11) . . ? N6 Zn3 N5 90.09(14) . . ? N6 Zn3 C2 99.98(14) . . ? N5 Zn3 C2 96.67(14) . . ? N6 Zn3 Fe2 120.02(10) . . ? N5 Zn3 Fe2 125.34(10) . . ? C2 Zn3 Fe2 118.38(12) . . ? N6 Zn3 Fe1 136.08(10) . . ? N5 Zn3 Fe1 111.45(10) . . ? C2 Zn3 Fe1 41.99(11) . . ? Fe2 Zn3 Fe1 78.81(2) . . ? N6 Zn3 C6 102.32(14) . . ? N5 Zn3 C6 91.45(14) . . ? C2 Zn3 C6 156.24(15) . . ? Fe2 Zn3 C6 41.40(10) . . ? Fe1 Zn3 C6 114.33(10) . . ? C11 N1 C7 117.6(4) . . ? C11 N1 Zn1 122.2(3) . . ? C7 N1 Zn1 119.5(3) . . ? C12 N2 C16 117.6(4) . . ? C12 N2 Zn1 121.6(3) . . ? C16 N2 Zn1 120.7(3) . . ? C21 N3 C17 116.8(4) . . ? C21 N3 Zn2 124.5(3) . . ? C17 N3 Zn2 118.6(3) . . ? C22 N4 C26 117.7(4) . . ? C22 N4 Zn2 117.3(3) . . ? C26 N4 Zn2 124.2(3) . . ? C31 N5 C27 117.0(4) . . ? C31 N5 Zn3 115.5(3) . . ? C27 N5 Zn3 127.1(3) . . ? C32 N6 C36 117.6(4) . . ? C32 N6 Zn3 124.1(3) . . ? C36 N6 Zn3 118.3(3) . . ? O1 C1 Fe1 170.6(4) . . ? O1 C1 Zn2 118.5(3) . . ? Fe1 C1 Zn2 70.87(15) . . ? O2 C2 Fe1 170.8(4) . . ? O2 C2 Zn3 117.1(3) . . ? Fe1 C2 Zn3 71.43(15) . . ? O3 C3 Fe1 170.5(4) . . ? O3 C3 Zn1 119.1(3) . . ? Fe1 C3 Zn1 69.33(15) . . ? O4 C4 Fe2 173.2(4) . . ? O4 C4 Zn2 119.1(3) . . ? Fe2 C4 Zn2 66.48(14) . . ? O5 C5 Fe2 173.0(4) . . ? O5 C5 Zn1 117.8(3) . . ? Fe2 C5 Zn1 68.82(16) . . ? O6 C6 Fe2 172.3(4) . . ? O6 C6 Zn3 118.8(3) . . ? Fe2 C6 Zn3 68.21(14) . . ? N1 C7 C8 122.9(5) . . ? N1 C7 H7A 118.6 . . ? C8 C7 H7A 118.6 . . ? C9 C8 C7 118.6(5) . . ? C9 C8 H8A 120.7 . . ? C7 C8 H8A 120.7 . . ? C8 C9 C10 119.6(5) . . ? C8 C9 H9A 120.2 . . ? C10 C9 H9A 120.2 . . ? C9 C10 C11 118.5(5) . . ? C9 C10 H10A 120.8 . . ? C11 C10 H10A 120.8 . . ? N1 C11 C10 122.8(5) . . ? N1 C11 H11A 118.6 . . ? C10 C11 H11A 118.6 . . ? N2 C12 C13 123.7(4) . . ? N2 C12 H12A 118.2 . . ? C13 C12 H12A 118.2 . . ? C14 C13 C12 118.4(5) . . ? C14 C13 H13A 120.8 . . ? C12 C13 H13A 120.8 . . ? C15 C14 C13 119.0(5) . . ? C15 C14 H14A 120.5 . . ? C13 C14 H14A 120.5 . . ? C14 C15 C16 119.2(5) . . ? C14 C15 H15A 120.4 . . ? C16 C15 H15A 120.4 . . ? N2 C16 C15 122.1(4) . . ? N2 C16 H16A 119.0 . . ? C15 C16 H16A 119.0 . . ? N3 C17 C18 123.0(5) . . ? N3 C17 H17A 118.5 . . ? C18 C17 H17A 118.5 . . ? C19 C18 C17 120.0(6) . . ? C19 C18 H18A 120.0 . . ? C17 C18 H18A 120.0 . . ? C18 C19 C20 117.6(5) . . ? C18 C19 H19A 121.2 . . ? C20 C19 H19A 121.2 . . ? C19 C20 C21 119.3(5) . . ? C19 C20 H20A 120.4 . . ? C21 C20 H20A 120.4 . . ? N3 C21 C20 123.2(5) . . ? N3 C21 H21A 118.4 . . ? C20 C21 H21A 118.4 . . ? N4 C22 C23 122.7(4) . . ? N4 C22 H22A 118.7 . . ? C23 C22 H22A 118.7 . . ? C24 C23 C22 118.9(5) . . ? C24 C23 H23A 120.6 . . ? C22 C23 H23A 120.6 . . ? C23 C24 C25 119.7(5) . . ? C23 C24 H24A 120.1 . . ? C25 C24 H24A 120.1 . . ? C24 C25 C26 118.1(4) . . ? C24 C25 H25A 120.9 . . ? C26 C25 H25A 120.9 . . ? N4 C26 C25 122.8(4) . . ? N4 C26 H26A 118.6 . . ? C25 C26 H26A 118.6 . . ? N5 C27 C28 122.4(5) . . ? N5 C27 H27A 118.8 . . ? C28 C27 H27A 118.8 . . ? C29 C28 C27 119.1(5) . . ? C29 C28 H28A 120.5 . . ? C27 C28 H28A 120.5 . . ? C28 C29 C30 118.7(5) . . ? C28 C29 H29A 120.6 . . ? C30 C29 H29A 120.6 . . ? C31 C30 C29 118.5(5) . . ? C31 C30 H30A 120.7 . . ? C29 C30 H30A 120.7 . . ? N5 C31 C30 124.3(5) . . ? N5 C31 H31A 117.9 . . ? C30 C31 H31A 117.9 . . ? N6 C32 C33 122.9(4) . . ? N6 C32 H32A 118.5 . . ? C33 C32 H32A 118.5 . . ? C34 C33 C32 119.1(4) . . ? C34 C33 H33A 120.5 . . ? C32 C33 H33A 120.5 . . ? C33 C34 C35 118.9(4) . . ? C33 C34 H34A 120.6 . . ? C35 C34 H34A 120.6 . . ? C36 C35 C34 118.6(4) . . ? C36 C35 H35A 120.7 . . ? C34 C35 H35A 120.7 . . ? N6 C36 C35 122.9(4) . . ? N6 C36 H36A 118.6 . . ? C35 C36 H36A 118.6 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.739 _refine_diff_density_min -0.482 _refine_diff_density_rms 0.103 data_4 _database_code_depnum_ccdc_archive 'CCDC 836634' #TrackingRef '- 1-5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H40 Co2 N2 O6 Zn3, 2(C7 H8)' _chemical_formula_sum 'C50 H56 Co2 N2 O6 Zn3' _chemical_formula_weight 1094.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 '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/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.2422(18) _cell_length_b 14.6947(13) _cell_length_c 19.774(2) _cell_angle_alpha 90.00 _cell_angle_beta 113.370(12) _cell_angle_gamma 90.00 _cell_volume 4599.0(8) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 5133 _cell_measurement_theta_min 2.7667 _cell_measurement_theta_max 29.0184 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.581 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2248 _exptl_absorpt_coefficient_mu 2.300 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6691 _exptl_absorpt_correction_T_max 0.7542 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur^TM^2, Oxford Diffraction' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.4171 _diffrn_reflns_number 50231 _diffrn_reflns_av_R_equivalents 0.0994 _diffrn_reflns_av_sigmaI/netI 0.0865 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8093 _reflns_number_gt 4549 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material 'enCIFer (Allen et al., 2004)' _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^)+(0.1139P)^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_number_reflns 8093 _refine_ls_number_parameters 425 _refine_ls_number_restraints 54 _refine_ls_R_factor_all 0.1345 _refine_ls_R_factor_gt 0.0777 _refine_ls_wR_factor_ref 0.2270 _refine_ls_wR_factor_gt 0.2032 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.078 _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 0.32160(6) 0.92329(7) 0.02393(6) 0.0483(3) Uani 1 1 d . . . Zn2 Zn 0.23481(6) 1.08061(7) -0.09670(5) 0.0479(3) Uani 1 1 d . . . Zn3 Zn 0.24593(6) 1.08227(8) 0.09167(6) 0.0598(4) Uani 1 1 d . . . Co1 Co 0.34499(7) 1.08596(8) 0.02884(6) 0.0443(3) Uani 1 1 d . A . Co2 Co 0.18123(6) 0.99060(7) -0.02154(6) 0.0371(3) Uani 1 1 d . A . O1 O 0.4732(5) 1.0523(6) 0.1745(4) 0.092(2) Uani 1 1 d . A . C1 C 0.4160(6) 1.0649(8) 0.1179(5) 0.074(3) Uani 1 1 d . . . O2 O 0.4518(4) 1.0744(5) -0.0522(4) 0.078(2) Uani 1 1 d . A . C2 C 0.4040(6) 1.0768(6) -0.0225(6) 0.060(3) Uani 1 1 d . . . O3 O 0.3099(7) 1.2814(6) 0.0211(5) 0.120(3) Uani 1 1 d . A . C3 C 0.3221(7) 1.2016(7) 0.0243(5) 0.063(3) Uani 1 1 d . . . O4 O 0.1345(5) 0.8673(5) 0.0706(4) 0.083(2) Uani 1 1 d . A . C4 C 0.1584(6) 0.9185(6) 0.0386(5) 0.055(2) Uani 1 1 d . . . O5 O 0.1351(4) 0.8622(4) -0.1416(4) 0.0649(18) Uani 1 1 d . A . C5 C 0.1581(5) 0.9167(6) -0.0958(5) 0.043(2) Uani 1 1 d . . . O6 O 0.0531(4) 1.1322(5) -0.0628(3) 0.071(2) Uani 1 1 d . A . C6 C 0.1048(6) 1.0774(6) -0.0457(4) 0.052(2) Uani 1 1 d . . . N11 N 0.3476(4) 0.8310(5) -0.0433(4) 0.0525(19) Uani 1 1 d . A . C12 C 0.3133(10) 0.7495(8) -0.0478(8) 0.114(5) Uani 1 1 d . . . H12 H 0.2827 0.7375 -0.0180 0.137 Uiso 1 1 calc R A . C13 C 0.3193(9) 0.6818(9) -0.0926(7) 0.099(4) Uani 1 1 d . A . H13 H 0.2937 0.6238 -0.0957 0.119 Uiso 1 1 calc R . . C14 C 0.3693(11) 0.7068(12) -0.1361(7) 0.129(6) Uani 1 1 d . . . H14 H 0.3806 0.6624 -0.1659 0.155 Uiso 1 1 calc R A . C15 C 0.3983(8) 0.7912(12) -0.1334(7) 0.116(6) Uani 1 1 d . A . H15 H 0.4290 0.8098 -0.1617 0.139 Uiso 1 1 calc R . . C16 C 0.3815(3) 0.8481(3) -0.0882(3) 0.092(4) Uani 1 1 d . . . H16 H 0.3970 0.9098 -0.0900 0.110 Uiso 1 1 calc R A . N21 N 0.3702(3) 0.8367(3) 0.1191(3) 0.071(3) Uani 0.638(11) 1 d PRD A 1 C22 C 0.3191(3) 0.7981(3) 0.1509(3) 0.078(4) Uani 0.638(11) 1 d PRDU A 1 H22 H 0.2594 0.8019 0.1265 0.094 Uiso 0.638(11) 1 calc PR A 1 C23 C 0.3555(3) 0.7539(3) 0.2184(3) 0.082(4) Uani 0.638(11) 1 d PRDU A 1 H23 H 0.3206 0.7275 0.2401 0.098 Uiso 0.638(11) 1 calc PR A 1 C24 C 0.4429(3) 0.7483(3) 0.2541(3) 0.123(10) Uani 0.638(11) 1 d PRD A 1 H24 H 0.4677 0.7181 0.3002 0.147 Uiso 0.638(11) 1 calc PR A 1 C25 C 0.4939(3) 0.7869(3) 0.2222(3) 0.082(4) Uani 0.638(11) 1 d PRDU A 1 H25 H 0.5537 0.7831 0.2466 0.098 Uiso 0.638(11) 1 calc PR A 1 C26 C 0.4576(3) 0.8311(3) 0.1547(3) 0.078(4) Uani 0.638(11) 1 d PRDU A 1 H26 H 0.4925 0.8574 0.1330 0.094 Uiso 0.638(11) 1 calc PR A 1 N21' N 0.3795(3) 0.8451(3) 0.1189(3) 0.071(3) Uani 0.362(11) 1 d PRD A 2 C22' C 0.3460(3) 0.8389(3) 0.1720(3) 0.074(7) Uani 0.362(11) 1 d PRDU A 2 H22' H 0.3074 0.8837 0.1743 0.089 Uiso 0.362(11) 1 calc PR A 2 C23' C 0.3688(3) 0.7671(3) 0.2219(3) 0.114(10) Uani 0.362(11) 1 d PRDU A 2 H23' H 0.3459 0.7629 0.2582 0.136 Uiso 0.362(11) 1 calc PR A 2 C24' C 0.4253(3) 0.7015(3) 0.2186(3) 0.123(10) Uani 0.362(11) 1 d PRD A 2 H24' H 0.4409 0.6524 0.2527 0.147 Uiso 0.362(11) 1 calc PR A 2 C25' C 0.4589(3) 0.7077(3) 0.1654(3) 0.114(10) Uani 0.362(11) 1 d PRDU A 2 H25' H 0.4975 0.6628 0.1632 0.136 Uiso 0.362(11) 1 calc PR A 2 C26' C 0.4360(3) 0.7795(3) 0.1156(3) 0.074(7) Uani 0.362(11) 1 d PRDU A 2 H26' H 0.4590 0.7837 0.0792 0.089 Uiso 0.362(11) 1 calc PR A 2 C31 C 0.2805(6) 1.1879(9) 0.1865(6) 0.068(3) Uani 1 1 d . A . C32 C 0.1944(8) 1.1998(8) 0.1371(6) 0.078(3) Uani 1 1 d . A . C33 C 0.1512(6) 1.1150(7) 0.1446(5) 0.057(3) Uani 1 1 d . A . C34 C 0.2135(8) 1.0658(10) 0.1950(6) 0.086(4) Uani 1 1 d . A . C35 C 0.2875(9) 1.1091(16) 0.2215(7) 0.132(7) Uani 1 1 d . A . C36 C 0.3496(8) 1.2556(11) 0.2041(7) 0.140(7) Uani 1 1 d . . . H36A H 0.3754 1.2656 0.2575 0.210 Uiso 1 1 calc R A . H36B H 0.3266 1.3132 0.1791 0.210 Uiso 1 1 calc R . . H36C H 0.3924 1.2328 0.1874 0.210 Uiso 1 1 calc R . . C37 C 0.1569(8) 1.2798(9) 0.0954(7) 0.110(5) Uani 1 1 d . . . H37A H 0.1216 1.3099 0.1172 0.165 Uiso 1 1 calc R A . H37B H 0.1220 1.2627 0.0444 0.165 Uiso 1 1 calc R . . H37C H 0.2016 1.3216 0.0961 0.165 Uiso 1 1 calc R . . C38 C 0.0586(6) 1.0977(10) 0.1066(7) 0.118(6) Uani 1 1 d . . . H38A H 0.0493 1.0401 0.0796 0.177 Uiso 1 1 calc R A . H38B H 0.0322 1.1474 0.0720 0.177 Uiso 1 1 calc R . . H38C H 0.0336 1.0944 0.1432 0.177 Uiso 1 1 calc R . . C39 C 0.1905(10) 0.9726(11) 0.2241(7) 0.130(5) Uani 1 1 d . . . H39A H 0.2412 0.9479 0.2633 0.194 Uiso 1 1 calc R A . H39B H 0.1692 0.9289 0.1834 0.194 Uiso 1 1 calc R . . H39C H 0.1471 0.9839 0.2434 0.194 Uiso 1 1 calc R . . C40 C 0.3688(8) 1.0706(13) 0.2822(7) 0.150(8) Uani 1 1 d . . . H40A H 0.4183 1.0986 0.2781 0.224 Uiso 1 1 calc R A . H40B H 0.3708 1.0045 0.2762 0.224 Uiso 1 1 calc R . . H40C H 0.3688 1.0842 0.3307 0.224 Uiso 1 1 calc R . . C41 C 0.1188(7) 1.1069(6) -0.2157(5) 0.059(3) Uani 1 1 d . A . C42 C 0.1788(9) 1.0495(8) -0.2316(6) 0.082(3) Uani 1 1 d . A . C43 C 0.2548(9) 1.0959(7) -0.2051(6) 0.075(3) Uani 1 1 d . A . C44 C 0.2451(5) 1.1819(6) -0.1803(5) 0.051(2) Uani 1 1 d . A . C45 C 0.1599(8) 1.1881(7) -0.1848(5) 0.075(3) Uani 1 1 d . A . C46 C 0.0296(6) 1.0755(7) -0.2372(5) 0.067(3) Uani 1 1 d . . . H46A H -0.0028 1.1228 -0.2250 0.101 Uiso 1 1 calc R A . H46B H 0.0291 1.0196 -0.2103 0.101 Uiso 1 1 calc R . . H46C H 0.0040 1.0635 -0.2903 0.101 Uiso 1 1 calc R . . C47 C 0.1696(11) 0.9596(7) -0.2646(7) 0.136(7) Uani 1 1 d . . . H47A H 0.2188 0.9464 -0.2761 0.204 Uiso 1 1 calc R A . H47B H 0.1182 0.9578 -0.3100 0.204 Uiso 1 1 calc R . . H47C H 0.1657 0.9139 -0.2300 0.204 Uiso 1 1 calc R . . C48 C 0.3324(9) 1.0668(10) -0.2200(7) 0.117(5) Uani 1 1 d . . . H48A H 0.3789 1.1096 -0.1959 0.175 Uiso 1 1 calc R A . H48B H 0.3179 1.0668 -0.2732 0.175 Uiso 1 1 calc R . . H48C H 0.3499 1.0055 -0.2003 0.175 Uiso 1 1 calc R . . C49 C 0.3090(10) 1.2521(13) -0.1581(8) 0.198(11) Uani 1 1 d . . . H49A H 0.3582 1.2313 -0.1153 0.297 Uiso 1 1 calc R A . H49B H 0.2861 1.3074 -0.1452 0.297 Uiso 1 1 calc R . . H49C H 0.3260 1.2653 -0.1989 0.297 Uiso 1 1 calc R . . C50 C 0.1154(8) 1.2677(7) -0.1649(5) 0.094(4) Uani 1 1 d . . . H50A H 0.0600 1.2477 -0.1676 0.141 Uiso 1 1 calc R A . H50B H 0.1080 1.3179 -0.1995 0.141 Uiso 1 1 calc R . . H50C H 0.1497 1.2883 -0.1147 0.141 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 0.0308(6) 0.0505(6) 0.0649(7) 0.0171(5) 0.0202(5) 0.0140(5) Zn2 0.0384(6) 0.0613(7) 0.0414(6) 0.0052(5) 0.0130(4) -0.0106(5) Zn3 0.0344(6) 0.0824(8) 0.0682(7) -0.0239(6) 0.0262(5) -0.0086(5) Co1 0.0255(6) 0.0542(7) 0.0500(7) 0.0037(5) 0.0117(5) 0.0007(5) Co2 0.0267(6) 0.0412(6) 0.0444(6) 0.0088(5) 0.0150(5) 0.0065(5) O1 0.053(5) 0.154(7) 0.062(5) 0.000(5) 0.017(4) 0.026(5) C1 0.040(6) 0.129(10) 0.050(6) 0.003(6) 0.016(5) 0.008(6) O2 0.059(5) 0.095(5) 0.102(6) 0.046(4) 0.055(4) 0.033(4) C2 0.037(5) 0.066(6) 0.081(7) 0.034(5) 0.029(5) 0.014(4) O3 0.213(11) 0.061(5) 0.121(7) -0.027(5) 0.102(7) -0.034(6) C3 0.087(8) 0.058(6) 0.056(6) -0.021(5) 0.042(5) -0.033(6) O4 0.088(5) 0.087(5) 0.095(5) 0.046(4) 0.059(5) 0.000(4) C4 0.039(5) 0.068(6) 0.057(6) 0.018(5) 0.019(4) 0.015(5) O5 0.047(4) 0.048(4) 0.084(5) -0.020(4) 0.010(3) 0.000(3) C5 0.028(5) 0.046(5) 0.049(5) 0.001(4) 0.008(4) 0.003(4) O6 0.055(4) 0.094(5) 0.059(4) 0.005(4) 0.019(3) 0.039(4) C6 0.043(5) 0.076(7) 0.042(5) 0.007(5) 0.021(4) 0.024(5) N11 0.047(5) 0.036(4) 0.074(5) 0.011(4) 0.023(4) 0.017(3) C12 0.195(16) 0.065(8) 0.137(12) 0.008(8) 0.124(12) 0.039(9) C13 0.123(11) 0.101(10) 0.088(9) 0.016(7) 0.057(8) 0.001(8) C14 0.155(15) 0.157(14) 0.068(9) -0.032(9) 0.036(9) 0.061(12) C15 0.097(10) 0.183(15) 0.097(10) -0.067(10) 0.070(8) -0.094(10) C16 0.094(9) 0.116(10) 0.092(9) -0.007(8) 0.064(8) -0.029(8) N21 0.029(4) 0.087(6) 0.095(6) 0.053(5) 0.023(4) 0.022(4) C22 0.051(7) 0.091(8) 0.079(7) 0.048(7) 0.010(5) 0.001(6) C23 0.033(6) 0.117(9) 0.084(8) 0.055(7) 0.012(5) 0.001(6) C24 0.075(11) 0.23(3) 0.067(14) 0.090(17) 0.032(11) 0.076(14) C25 0.033(6) 0.117(9) 0.084(8) 0.055(7) 0.012(5) 0.001(6) C26 0.051(7) 0.091(8) 0.079(7) 0.048(7) 0.010(5) 0.001(6) N21' 0.029(4) 0.087(6) 0.095(6) 0.053(5) 0.023(4) 0.022(4) C22' 0.043(10) 0.078(11) 0.101(12) 0.038(10) 0.029(9) 0.025(9) C23' 0.099(14) 0.136(15) 0.122(15) 0.023(11) 0.061(11) 0.021(11) C24' 0.075(11) 0.23(3) 0.067(14) 0.090(17) 0.032(11) 0.076(14) C25' 0.099(14) 0.136(15) 0.122(15) 0.023(11) 0.061(11) 0.021(11) C26' 0.043(10) 0.078(11) 0.101(12) 0.038(10) 0.029(9) 0.025(9) C31 0.034(6) 0.124(10) 0.046(6) -0.026(6) 0.016(5) -0.013(6) C32 0.084(9) 0.090(8) 0.064(7) -0.024(6) 0.033(6) 0.033(7) C33 0.038(5) 0.087(7) 0.054(6) -0.036(5) 0.028(5) -0.027(5) C34 0.057(8) 0.151(12) 0.042(6) -0.030(7) 0.009(5) 0.012(8) C35 0.056(9) 0.29(2) 0.047(8) -0.032(11) 0.016(6) -0.012(12) C36 0.066(9) 0.238(18) 0.114(11) -0.117(12) 0.033(7) -0.064(10) C37 0.092(10) 0.132(12) 0.117(11) -0.065(10) 0.053(9) -0.025(9) C38 0.040(7) 0.217(16) 0.113(10) -0.088(10) 0.047(7) -0.034(8) C39 0.130(13) 0.185(15) 0.089(10) 0.026(10) 0.059(9) -0.015(12) C40 0.063(9) 0.32(2) 0.064(8) -0.011(11) 0.025(7) 0.008(11) C41 0.089(8) 0.049(6) 0.033(5) 0.003(4) 0.018(5) -0.011(5) C42 0.106(10) 0.074(8) 0.062(7) 0.017(6) 0.030(7) 0.010(7) C43 0.113(11) 0.073(7) 0.052(6) -0.001(5) 0.046(7) 0.022(7) C44 0.029(5) 0.052(6) 0.058(6) -0.014(4) 0.003(4) 0.001(4) C45 0.115(10) 0.071(7) 0.028(5) 0.024(5) 0.015(5) 0.037(7) C46 0.071(7) 0.087(7) 0.040(5) 0.003(5) 0.018(5) -0.008(6) C47 0.29(2) 0.050(7) 0.121(11) -0.037(7) 0.132(13) -0.028(10) C48 0.119(12) 0.148(13) 0.101(10) -0.004(9) 0.062(9) 0.029(10) C49 0.107(12) 0.28(2) 0.147(14) 0.147(15) -0.013(10) -0.075(14) C50 0.133(11) 0.064(7) 0.046(6) -0.003(5) -0.006(6) 0.014(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N11 2.069(7) . ? Zn1 N21' 2.087(4) . ? Zn1 N21 2.147(4) . ? Zn1 Co1 2.4197(15) . ? Zn1 Co2 2.4327(14) . ? Zn2 C44 2.282(9) . ? Zn2 C43 2.313(10) . ? Zn2 C45 2.326(8) . ? Zn2 Co2 2.4293(14) . ? Zn2 C41 2.440(9) . ? Zn2 Co1 2.4568(15) . ? Zn2 C42 2.492(11) . ? Zn3 C32 2.284(9) . ? Zn3 C33 2.312(8) . ? Zn3 C31 2.322(10) . ? Zn3 C34 2.334(12) . ? Zn3 C35 2.408(12) . ? Zn3 Co2 2.4676(15) . ? Zn3 Co1 2.4793(15) . ? Co1 C2 1.705(10) . ? Co1 C1 1.728(10) . ? Co1 C3 1.739(11) . ? Co1 Co2 2.9491(15) . ? Co2 C5 1.740(9) . ? Co2 C4 1.750(9) . ? Co2 C6 1.758(9) . ? O1 C1 1.177(11) . ? O2 C2 1.186(10) . ? O3 C3 1.188(12) . ? O4 C4 1.159(10) . ? O5 C5 1.155(9) . ? O6 C6 1.149(9) . ? N11 C16 1.266(8) . ? N11 C12 1.323(14) . ? C12 C13 1.363(15) . ? C12 H12 0.9500 . ? C13 C14 1.49(2) . ? C13 H13 0.9500 . ? C14 C15 1.330(19) . ? C14 H14 0.9500 . ? C15 C16 1.338(15) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? N21 C22 1.3900 . ? N21 C26 1.3900 . ? C22 C23 1.3900 . ? C22 H22 0.9500 . ? C23 C24 1.3900 . ? C23 H23 0.9500 . ? C24 C25 1.3900 . ? C24 H24 0.9500 . ? C25 C26 1.3900 . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? N21' C22' 1.3900 . ? N21' C26' 1.3900 . ? C22' C23' 1.3900 . ? C22' H22' 0.9500 . ? C23' C24' 1.3900 . ? C23' H23' 0.9500 . ? C24' C25' 1.3900 . ? C24' H24' 0.9500 . ? C25' C26' 1.3900 . ? C25' H25' 0.9500 . ? C26' H26' 0.9500 . ? C31 C35 1.33(2) . ? C31 C32 1.427(14) . ? C31 C36 1.484(16) . ? C32 C37 1.435(16) . ? C32 C33 1.488(15) . ? C33 C34 1.349(14) . ? C33 C38 1.492(13) . ? C34 C35 1.333(18) . ? C34 C39 1.594(18) . ? C35 C40 1.546(19) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C45 1.398(14) . ? C41 C42 1.462(15) . ? C41 C46 1.498(14) . ? C42 C43 1.383(16) . ? C42 C47 1.455(15) . ? C43 C44 1.391(12) . ? C43 C48 1.540(16) . ? C44 C45 1.437(14) . ? C44 C49 1.444(16) . ? C45 C50 1.534(14) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N11 Zn1 N21' 93.9(2) . . ? N11 Zn1 N21 93.8(2) . . ? N21' Zn1 N21 5.3 . . ? N11 Zn1 Co1 126.7(2) . . ? N21' Zn1 Co1 119.69(16) . . ? N21 Zn1 Co1 123.34(15) . . ? N11 Zn1 Co2 117.8(2) . . ? N21' Zn1 Co2 127.41(14) . . ? N21 Zn1 Co2 123.37(14) . . ? Co1 Zn1 Co2 74.86(4) . . ? C44 Zn2 C43 35.2(3) . . ? C44 Zn2 C45 36.3(3) . . ? C43 Zn2 C45 58.8(4) . . ? C44 Zn2 Co2 162.8(2) . . ? C43 Zn2 Co2 148.5(3) . . ? C45 Zn2 Co2 126.5(3) . . ? C44 Zn2 C41 57.8(3) . . ? C43 Zn2 C41 57.1(4) . . ? C45 Zn2 C41 34.0(3) . . ? Co2 Zn2 C41 108.1(2) . . ? C44 Zn2 Co1 117.4(2) . . ? C43 Zn2 Co1 126.4(3) . . ? C45 Zn2 Co1 135.4(3) . . ? Co2 Zn2 Co1 74.25(4) . . ? C41 Zn2 Co1 168.2(2) . . ? C44 Zn2 C42 56.9(3) . . ? C43 Zn2 C42 33.2(4) . . ? C45 Zn2 C42 57.2(4) . . ? Co2 Zn2 C42 118.4(3) . . ? C41 Zn2 C42 34.5(3) . . ? Co1 Zn2 C42 154.6(3) . . ? C32 Zn3 C33 37.8(4) . . ? C32 Zn3 C31 36.1(4) . . ? C33 Zn3 C31 59.8(3) . . ? C32 Zn3 C34 57.9(5) . . ? C33 Zn3 C34 33.7(4) . . ? C31 Zn3 C34 55.7(4) . . ? C32 Zn3 C35 56.9(5) . . ? C33 Zn3 C35 56.6(4) . . ? C31 Zn3 C35 32.6(5) . . ? C34 Zn3 C35 32.6(4) . . ? C32 Zn3 Co2 131.6(3) . . ? C33 Zn3 Co2 112.2(2) . . ? C31 Zn3 Co2 167.4(3) . . ? C34 Zn3 Co2 123.9(3) . . ? C35 Zn3 Co2 153.2(5) . . ? C32 Zn3 Co1 129.3(3) . . ? C33 Zn3 Co1 166.6(3) . . ? C31 Zn3 Co1 112.5(3) . . ? C34 Zn3 Co1 153.2(3) . . ? C35 Zn3 Co1 123.9(3) . . ? Co2 Zn3 Co1 73.19(5) . . ? C2 Co1 C1 104.1(5) . . ? C2 Co1 C3 102.9(4) . . ? C1 Co1 C3 106.4(5) . . ? C2 Co1 Zn1 91.6(3) . . ? C1 Co1 Zn1 84.5(4) . . ? C3 Co1 Zn1 158.8(3) . . ? C2 Co1 Zn2 78.5(3) . . ? C1 Co1 Zn2 167.3(4) . . ? C3 Co1 Zn2 84.9(3) . . ? Zn1 Co1 Zn2 83.00(5) . . ? C2 Co1 Zn3 171.7(3) . . ? C1 Co1 Zn3 80.6(3) . . ? C3 Co1 Zn3 81.9(3) . . ? Zn1 Co1 Zn3 82.04(5) . . ? Zn2 Co1 Zn3 95.47(5) . . ? C2 Co1 Co2 118.6(3) . . ? C1 Co1 Co2 117.1(4) . . ? C3 Co1 Co2 106.2(3) . . ? Zn1 Co1 Co2 52.77(4) . . ? Zn2 Co1 Co2 52.45(4) . . ? Zn3 Co1 Co2 53.22(4) . . ? C5 Co2 C4 99.0(4) . . ? C5 Co2 C6 109.1(4) . . ? C4 Co2 C6 106.1(4) . . ? C5 Co2 Zn2 80.8(3) . . ? C4 Co2 Zn2 171.1(3) . . ? C6 Co2 Zn2 82.2(3) . . ? C5 Co2 Zn1 85.4(3) . . ? C4 Co2 Zn1 87.8(3) . . ? C6 Co2 Zn1 157.5(3) . . ? Zn2 Co2 Zn1 83.30(5) . . ? C5 Co2 Zn3 167.3(3) . . ? C4 Co2 Zn3 81.8(3) . . ? C6 Co2 Zn3 82.6(3) . . ? Zn2 Co2 Zn3 96.48(5) . . ? Zn1 Co2 Zn3 82.02(5) . . ? C5 Co2 Co1 116.7(3) . . ? C4 Co2 Co1 120.1(3) . . ? C6 Co2 Co1 105.1(3) . . ? Zn2 Co2 Co1 53.30(4) . . ? Zn1 Co2 Co1 52.37(4) . . ? Zn3 Co2 Co1 53.59(4) . . ? O1 C1 Co1 170.3(9) . . ? O2 C2 Co1 173.1(10) . . ? O3 C3 Co1 177.0(10) . . ? O4 C4 Co2 171.3(9) . . ? O5 C5 Co2 170.6(8) . . ? O6 C6 Co2 177.9(9) . . ? C16 N11 C12 116.8(8) . . ? C16 N11 Zn1 126.8(5) . . ? C12 N11 Zn1 115.6(7) . . ? N11 C12 C13 123.9(12) . . ? N11 C12 H12 118.0 . . ? C13 C12 H12 118.0 . . ? C12 C13 C14 114.0(13) . . ? C12 C13 H13 123.0 . . ? C14 C13 H13 123.0 . . ? C15 C14 C13 120.2(12) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C16 115.6(11) . . ? C14 C15 H15 122.2 . . ? C16 C15 H15 122.2 . . ? N11 C16 C15 128.9(8) . . ? N11 C16 H16 115.6 . . ? C15 C16 H16 115.6 . . ? C22 N21 C26 120.0 . . ? C22 N21 Zn1 122.79(13) . . ? C26 N21 Zn1 116.56(13) . . ? C23 C22 N21 120.0 . . ? C23 C22 H22 120.0 . . ? N21 C22 H22 120.0 . . ? C24 C23 C22 120.0 . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C23 C24 C25 120.0 . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C26 C25 C24 120.0 . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C25 C26 N21 120.0 . . ? C25 C26 H26 120.0 . . ? N21 C26 H26 120.0 . . ? C22' N21' C26' 120.0 . . ? C22' N21' Zn1 121.45(14) . . ? C26' N21' Zn1 115.73(14) . . ? C23' C22' N21' 120.0 . . ? C23' C22' H22' 120.0 . . ? N21' C22' H22' 120.0 . . ? C22' C23' C24' 120.0 . . ? C22' C23' H23' 120.0 . . ? C24' C23' H23' 120.0 . . ? C25' C24' C23' 120.0 . . ? C25' C24' H24' 120.0 . . ? C23' C24' H24' 120.0 . . ? C24' C25' C26' 120.0 . . ? C24' C25' H25' 120.0 . . ? C26' C25' H25' 120.0 . . ? C25' C26' N21' 120.0 . . ? C25' C26' H26' 120.0 . . ? N21' C26' H26' 120.0 . . ? C35 C31 C32 108.5(11) . . ? C35 C31 C36 124.2(12) . . ? C32 C31 C36 126.9(13) . . ? C35 C31 Zn3 77.2(8) . . ? C32 C31 Zn3 70.5(5) . . ? C36 C31 Zn3 124.3(7) . . ? C31 C32 C37 127.0(13) . . ? C31 C32 C33 104.8(10) . . ? C37 C32 C33 127.9(11) . . ? C31 C32 Zn3 73.4(6) . . ? C37 C32 Zn3 123.4(8) . . ? C33 C32 Zn3 72.1(5) . . ? C34 C33 C32 103.8(9) . . ? C34 C33 C38 131.3(12) . . ? C32 C33 C38 124.8(11) . . ? C34 C33 Zn3 74.0(6) . . ? C32 C33 Zn3 70.1(5) . . ? C38 C33 Zn3 122.9(6) . . ? C35 C34 C33 113.1(15) . . ? C35 C34 C39 127.1(14) . . ? C33 C34 C39 119.2(11) . . ? C35 C34 Zn3 76.7(8) . . ? C33 C34 Zn3 72.2(6) . . ? C39 C34 Zn3 125.8(8) . . ? C31 C35 C34 109.6(13) . . ? C31 C35 C40 126.2(15) . . ? C34 C35 C40 124.2(19) . . ? C31 C35 Zn3 70.2(7) . . ? C34 C35 Zn3 70.7(7) . . ? C40 C35 Zn3 124.2(10) . . ? C31 C36 H36A 109.5 . . ? C31 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C31 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C33 C38 H38A 109.5 . . ? C33 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C33 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C34 C39 H39A 109.5 . . ? C34 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C34 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C35 C40 H40A 109.5 . . ? C35 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C35 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C45 C41 C42 107.9(10) . . ? C45 C41 C46 132.3(10) . . ? C42 C41 C46 119.7(9) . . ? C45 C41 Zn2 68.5(5) . . ? C42 C41 Zn2 74.7(6) . . ? C46 C41 Zn2 125.5(6) . . ? C43 C42 C47 122.4(13) . . ? C43 C42 C41 106.2(10) . . ? C47 C42 C41 131.3(13) . . ? C43 C42 Zn2 66.3(6) . . ? C47 C42 Zn2 125.0(8) . . ? C41 C42 Zn2 70.8(6) . . ? C42 C43 C44 110.6(11) . . ? C42 C43 C48 123.7(11) . . ? C44 C43 C48 123.8(12) . . ? C42 C43 Zn2 80.5(7) . . ? C44 C43 Zn2 71.2(6) . . ? C48 C43 Zn2 127.6(8) . . ? C43 C44 C45 107.4(9) . . ? C43 C44 C49 124.8(13) . . ? C45 C44 C49 127.7(12) . . ? C43 C44 Zn2 73.6(6) . . ? C45 C44 Zn2 73.5(5) . . ? C49 C44 Zn2 121.0(7) . . ? C41 C45 C44 107.6(9) . . ? C41 C45 C50 123.0(11) . . ? C44 C45 C50 129.4(11) . . ? C41 C45 Zn2 77.5(5) . . ? C44 C45 Zn2 70.2(5) . . ? C50 C45 Zn2 120.7(6) . . ? C41 C46 H46A 109.5 . . ? C41 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C41 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C42 C47 H47A 109.5 . . ? C42 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C42 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C43 C48 H48A 109.5 . . ? C43 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C43 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C44 C49 H49A 109.5 . . ? C44 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C44 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C45 C50 H50A 109.5 . . ? C45 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C45 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.203 _refine_diff_density_min -0.954 _refine_diff_density_rms 0.121 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.045 0.000 0.500 626 110 '2 toluene' 2 0.901 0.500 0.000 626 110 '2 toluene' _platon_squeeze_details ; ; data_5 _database_code_depnum_ccdc_archive 'CCDC 836635' #TrackingRef '- 1-5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H46 Co2 O8 Zn3, C4 H8 O' _chemical_formula_sum 'C38 H54 Co2 O9 Zn3' _chemical_formula_weight 968.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c n' _symmetry_space_group_name_Hall '-P 2n 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.7762(6) _cell_length_b 17.0143(6) _cell_length_c 14.2531(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4068.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 8198 _cell_measurement_theta_min 2.8525 _cell_measurement_theta_max 28.8397 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.582 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1992 _exptl_absorpt_coefficient_mu 2.592 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6121 _exptl_absorpt_correction_T_max 0.6387 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Xcalibur^TM^2 _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.4171 _diffrn_reflns_number 38397 _diffrn_reflns_av_R_equivalents 0.0708 _diffrn_reflns_av_sigmaI/netI 0.0444 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4660 _reflns_number_gt 3538 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material 'enCIFer (Allen et al., 2004)' _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^)+(0.0245P)^2^+4.5213P] 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 4660 _refine_ls_number_parameters 236 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0578 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0733 _refine_ls_wR_factor_gt 0.0647 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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 Co1 Co 0.03244(2) 0.27726(2) 0.15152(3) 0.01538(10) Uani 1 1 d . . . Zn1 Zn 0.083255(19) 0.200663(19) 0.28454(2) 0.01920(9) Uani 1 1 d . . . Zn2 Zn 0.0000 0.38724(3) 0.2500 0.01540(11) Uani 1 2 d S . . C11 C 0.05399(18) 0.19185(18) 0.0858(2) 0.0228(6) Uani 1 1 d . . . C13 C -0.03818(17) 0.32357(16) 0.0792(2) 0.0189(6) Uani 1 1 d . . . C12 C 0.12354(18) 0.32830(17) 0.1498(2) 0.0218(6) Uani 1 1 d . . . O4 O 0.06917(11) 0.47568(11) 0.30395(14) 0.0191(4) Uani 1 1 d . . . C1 C 0.13226(16) 0.08322(17) 0.3390(2) 0.0210(6) Uani 1 1 d . . . C2 C 0.16782(17) 0.08637(17) 0.2492(2) 0.0215(6) Uani 1 1 d . . . C3 C 0.21903(17) 0.15277(17) 0.2464(2) 0.0221(6) Uani 1 1 d . . . C4 C 0.21471(17) 0.19128(17) 0.3346(2) 0.0231(7) Uani 1 1 d . . . C5 C 0.16165(17) 0.14746(17) 0.3930(2) 0.0209(6) Uani 1 1 d . . . C6 C 0.08238(19) 0.01646(18) 0.3752(3) 0.0339(8) Uani 1 1 d . . . H6A H 0.0646 0.0283 0.4391 0.051 Uiso 1 1 calc R . . H6B H 0.1141 -0.0319 0.3755 0.051 Uiso 1 1 calc R . . H6C H 0.0358 0.0094 0.3345 0.051 Uiso 1 1 calc R . . C7 C 0.1592(2) 0.02534(19) 0.1734(2) 0.0329(8) Uani 1 1 d . . . H7A H 0.1847 -0.0236 0.1937 0.049 Uiso 1 1 calc R . . H7B H 0.1848 0.0442 0.1158 0.049 Uiso 1 1 calc R . . H7C H 0.1025 0.0157 0.1615 0.049 Uiso 1 1 calc R . . C8 C 0.2694(2) 0.1765(2) 0.1642(2) 0.0379(9) Uani 1 1 d . . . H8A H 0.2879 0.2307 0.1728 0.057 Uiso 1 1 calc R . . H8B H 0.2377 0.1731 0.1066 0.057 Uiso 1 1 calc R . . H8C H 0.3155 0.1413 0.1595 0.057 Uiso 1 1 calc R . . C9 C 0.26253(19) 0.26139(19) 0.3654(3) 0.0355(8) Uani 1 1 d . . . H9A H 0.3118 0.2436 0.3957 0.053 Uiso 1 1 calc R . . H9B H 0.2313 0.2925 0.4100 0.053 Uiso 1 1 calc R . . H9C H 0.2757 0.2937 0.3107 0.053 Uiso 1 1 calc R . . C10 C 0.14789(19) 0.1595(2) 0.4958(2) 0.0316(8) Uani 1 1 d . . . H10A H 0.0930 0.1447 0.5116 0.047 Uiso 1 1 calc R . . H10B H 0.1565 0.2149 0.5116 0.047 Uiso 1 1 calc R . . H10C H 0.1851 0.1268 0.5316 0.047 Uiso 1 1 calc R . . O1 O 0.06932(14) 0.14221(13) 0.03456(15) 0.0336(6) Uani 1 1 d . . . O2 O -0.07964(13) 0.35359(12) 0.02573(15) 0.0286(5) Uani 1 1 d . . . O3 O 0.18312(13) 0.36110(14) 0.14066(17) 0.0344(6) Uani 1 1 d . . . C14 C 0.03409(18) 0.53289(16) 0.3680(2) 0.0222(6) Uani 1 1 d . . . H14A H 0.0065 0.5062 0.4206 0.027 Uiso 1 1 calc R . . H14B H -0.0045 0.5670 0.3349 0.027 Uiso 1 1 calc R . . C15 C 0.10426(19) 0.57996(18) 0.4031(2) 0.0288(7) Uani 1 1 d . . . H15A H 0.0935 0.6023 0.4660 0.035 Uiso 1 1 calc R . . H15B H 0.1177 0.6231 0.3593 0.035 Uiso 1 1 calc R . . C16 C 0.17023(19) 0.51944(19) 0.4071(2) 0.0296(7) Uani 1 1 d . . . H16A H 0.2234 0.5447 0.4056 0.036 Uiso 1 1 calc R . . H16B H 0.1659 0.4864 0.4641 0.036 Uiso 1 1 calc R . . C17 C 0.15554(17) 0.47184(18) 0.3194(2) 0.0261(7) Uani 1 1 d . . . H17A H 0.1847 0.4945 0.2654 0.031 Uiso 1 1 calc R . . H17B H 0.1730 0.4168 0.3283 0.031 Uiso 1 1 calc R . . O5 O 0.0000 0.69945(18) 0.2500 0.0409(9) Uani 1 2 d S . . C18 C -0.0128(2) 0.74744(18) 0.3303(2) 0.0286(7) Uani 1 1 d . . . H18A H 0.0341 0.7456 0.3725 0.034 Uiso 1 1 calc R . . H18B H -0.0602 0.7293 0.3656 0.034 Uiso 1 1 calc R . . C19 C -0.0255(2) 0.82992(19) 0.2940(2) 0.0384(9) Uani 1 1 d . . . H19A H -0.0069 0.8697 0.3397 0.046 Uiso 1 1 calc R . . H19B H -0.0823 0.8397 0.2791 0.046 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 Co1 0.01596(19) 0.01420(18) 0.01598(19) -0.00098(15) -0.00001(15) 0.00142(15) Zn1 0.01844(17) 0.02003(17) 0.01914(17) 0.00203(14) -0.00183(14) 0.00427(13) Zn2 0.0173(2) 0.0126(2) 0.0164(2) 0.000 0.00195(19) 0.000 C11 0.0238(16) 0.0228(15) 0.0219(16) 0.0029(14) -0.0030(13) 0.0038(12) C13 0.0215(15) 0.0179(14) 0.0173(14) -0.0046(12) 0.0019(12) -0.0008(12) C12 0.0262(16) 0.0195(14) 0.0197(15) -0.0023(13) 0.0050(13) 0.0033(13) O4 0.0204(11) 0.0159(10) 0.0211(11) -0.0051(8) 0.0013(8) -0.0015(8) C1 0.0151(14) 0.0177(14) 0.0302(17) 0.0059(13) -0.0022(13) 0.0029(11) C2 0.0201(15) 0.0198(14) 0.0246(15) -0.0023(13) -0.0039(13) 0.0056(12) C3 0.0184(14) 0.0229(15) 0.0251(16) 0.0026(13) 0.0020(13) 0.0058(12) C4 0.0158(14) 0.0188(14) 0.0346(18) 0.0015(13) -0.0043(13) 0.0022(11) C5 0.0161(15) 0.0216(15) 0.0249(16) -0.0002(13) -0.0036(12) 0.0061(12) C6 0.0268(18) 0.0266(17) 0.048(2) 0.0127(16) -0.0011(16) -0.0006(14) C7 0.0363(19) 0.0274(17) 0.0350(19) -0.0117(15) -0.0100(16) 0.0096(15) C8 0.0303(19) 0.042(2) 0.041(2) 0.0098(17) 0.0130(16) 0.0045(16) C9 0.0230(17) 0.0274(18) 0.056(2) -0.0044(17) -0.0082(16) -0.0005(14) C10 0.0305(18) 0.039(2) 0.0250(17) -0.0014(15) -0.0053(14) 0.0090(15) O1 0.0450(14) 0.0289(12) 0.0270(12) -0.0137(11) -0.0031(11) 0.0140(11) O2 0.0371(13) 0.0250(11) 0.0237(12) -0.0006(10) -0.0081(10) 0.0088(10) O3 0.0249(12) 0.0390(13) 0.0394(14) -0.0050(11) 0.0108(11) -0.0093(10) C14 0.0251(16) 0.0181(14) 0.0233(16) -0.0058(12) 0.0026(13) 0.0013(12) C15 0.0339(19) 0.0247(16) 0.0278(18) -0.0062(14) 0.0006(14) -0.0071(14) C16 0.0244(17) 0.0300(17) 0.0345(19) -0.0019(15) -0.0034(14) -0.0099(13) C17 0.0170(15) 0.0276(16) 0.0339(18) -0.0021(15) 0.0046(13) -0.0044(13) O5 0.081(3) 0.0172(16) 0.0247(17) 0.000 0.0055(18) 0.000 C18 0.0373(19) 0.0250(16) 0.0235(17) -0.0021(14) 0.0027(14) -0.0021(14) C19 0.058(2) 0.0223(16) 0.035(2) -0.0028(15) 0.0143(18) 0.0015(16) _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 Co1 C13 1.757(3) . ? Co1 C12 1.758(3) . ? Co1 C11 1.767(3) . ? Co1 Zn2 2.4017(5) . ? Co1 Zn1 2.4535(5) . ? Co1 Zn1 2.5093(5) 3 ? Zn1 C5 2.222(3) . ? Zn1 C1 2.296(3) . ? Zn1 C4 2.323(3) . ? Zn1 C2 2.459(3) . ? Zn1 C3 2.479(3) . ? Zn1 Co1 2.5092(5) 3 ? Zn1 Zn1 2.9618(7) 3 ? Zn2 O4 2.0499(19) 3 ? Zn2 O4 2.0499(19) . ? Zn2 Co1 2.4016(5) 3 ? C11 O1 1.145(3) . ? C13 O2 1.152(3) . ? C12 O3 1.152(3) . ? O4 C14 1.459(3) . ? O4 C17 1.467(3) . ? C1 C2 1.413(4) . ? C1 C5 1.425(4) . ? C1 C6 1.502(4) . ? C2 C3 1.420(4) . ? C2 C7 1.505(4) . ? C3 C4 1.419(4) . ? C3 C8 1.500(4) . ? C4 C5 1.429(4) . ? C4 C9 1.503(4) . ? C5 C10 1.498(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C14 C15 1.509(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.513(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.509(4) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? O5 C18 1.422(3) 3 ? O5 C18 1.422(3) . ? C18 C19 1.511(4) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C19 1.519(6) 3 ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C13 Co1 C12 110.89(13) . . ? C13 Co1 C11 101.29(13) . . ? C12 Co1 C11 102.77(14) . . ? C13 Co1 Zn2 80.82(9) . . ? C12 Co1 Zn2 79.65(9) . . ? C11 Co1 Zn2 175.84(10) . . ? C13 Co1 Zn1 157.79(9) . . ? C12 Co1 Zn1 88.34(10) . . ? C11 Co1 Zn1 84.37(9) . . ? Zn2 Co1 Zn1 92.348(16) . . ? C13 Co1 Zn1 85.66(9) . 3 ? C12 Co1 Zn1 159.08(10) . 3 ? C11 Co1 Zn1 85.62(10) . 3 ? Zn2 Co1 Zn1 90.980(16) . 3 ? Zn1 Co1 Zn1 73.274(17) . 3 ? C5 Zn1 C1 36.72(10) . . ? C5 Zn1 C4 36.55(10) . . ? C1 Zn1 C4 59.77(10) . . ? C5 Zn1 Co1 163.63(8) . . ? C1 Zn1 Co1 147.98(8) . . ? C4 Zn1 Co1 127.12(8) . . ? C5 Zn1 C2 58.60(10) . . ? C1 Zn1 C2 34.36(10) . . ? C4 Zn1 C2 57.38(10) . . ? Co1 Zn1 C2 117.52(7) . . ? C5 Zn1 C3 58.32(10) . . ? C1 Zn1 C3 57.25(10) . . ? C4 Zn1 C3 34.17(10) . . ? Co1 Zn1 C3 108.93(7) . . ? C2 Zn1 C3 33.41(9) . . ? C5 Zn1 Co1 114.63(8) . 3 ? C1 Zn1 Co1 127.32(8) . 3 ? C4 Zn1 Co1 131.18(8) . 3 ? Co1 Zn1 Co1 74.694(18) . 3 ? C2 Zn1 Co1 158.64(7) . 3 ? C3 Zn1 Co1 163.92(7) . 3 ? C5 Zn1 Zn1 142.13(8) . 3 ? C1 Zn1 Zn1 116.75(7) . 3 ? C4 Zn1 Zn1 175.78(7) . 3 ? Co1 Zn1 Zn1 54.229(13) . 3 ? C2 Zn1 Zn1 118.42(7) . 3 ? C3 Zn1 Zn1 142.52(7) . 3 ? Co1 Zn1 Zn1 52.498(13) 3 3 ? O4 Zn2 O4 85.54(11) 3 . ? O4 Zn2 Co1 131.52(5) 3 3 ? O4 Zn2 Co1 118.75(6) . 3 ? O4 Zn2 Co1 118.75(6) 3 . ? O4 Zn2 Co1 131.52(5) . . ? Co1 Zn2 Co1 77.64(2) 3 . ? O1 C11 Co1 172.1(3) . . ? O2 C13 Co1 174.1(3) . . ? O3 C12 Co1 174.3(3) . . ? C14 O4 C17 109.5(2) . . ? C14 O4 Zn2 119.76(16) . . ? C17 O4 Zn2 125.64(16) . . ? C2 C1 C5 108.3(3) . . ? C2 C1 C6 125.1(3) . . ? C5 C1 C6 126.0(3) . . ? C2 C1 Zn1 79.17(17) . . ? C5 C1 Zn1 68.83(16) . . ? C6 C1 Zn1 125.1(2) . . ? C1 C2 C3 108.1(3) . . ? C1 C2 C7 125.7(3) . . ? C3 C2 C7 126.0(3) . . ? C1 C2 Zn1 66.48(15) . . ? C3 C2 Zn1 74.07(16) . . ? C7 C2 Zn1 129.6(2) . . ? C4 C3 C2 108.2(3) . . ? C4 C3 C8 126.6(3) . . ? C2 C3 C8 125.2(3) . . ? C4 C3 Zn1 66.87(16) . . ? C2 C3 Zn1 72.51(16) . . ? C8 C3 Zn1 126.9(2) . . ? C3 C4 C5 107.9(3) . . ? C3 C4 C9 126.7(3) . . ? C5 C4 C9 125.2(3) . . ? C3 C4 Zn1 78.96(17) . . ? C5 C4 Zn1 67.87(16) . . ? C9 C4 Zn1 122.8(2) . . ? C1 C5 C4 107.5(3) . . ? C1 C5 C10 125.5(3) . . ? C4 C5 C10 126.5(3) . . ? C1 C5 Zn1 74.45(16) . . ? C4 C5 Zn1 75.58(17) . . ? C10 C5 Zn1 122.3(2) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O4 C14 C15 104.3(2) . . ? O4 C14 H14A 110.9 . . ? C15 C14 H14A 110.9 . . ? O4 C14 H14B 110.9 . . ? C15 C14 H14B 110.9 . . ? H14A C14 H14B 108.9 . . ? C14 C15 C16 102.8(2) . . ? C14 C15 H15A 111.2 . . ? C16 C15 H15A 111.2 . . ? C14 C15 H15B 111.2 . . ? C16 C15 H15B 111.2 . . ? H15A C15 H15B 109.1 . . ? C17 C16 C15 102.4(3) . . ? C17 C16 H16A 111.3 . . ? C15 C16 H16A 111.3 . . ? C17 C16 H16B 111.3 . . ? C15 C16 H16B 111.3 . . ? H16A C16 H16B 109.2 . . ? O4 C17 C16 105.2(2) . . ? O4 C17 H17A 110.7 . . ? C16 C17 H17A 110.7 . . ? O4 C17 H17B 110.7 . . ? C16 C17 H17B 110.7 . . ? H17A C17 H17B 108.8 . . ? C18 O5 C18 109.9(3) 3 . ? O5 C18 C19 106.2(3) . . ? O5 C18 H18A 110.5 . . ? C19 C18 H18A 110.5 . . ? O5 C18 H18B 110.5 . . ? C19 C18 H18B 110.5 . . ? H18A C18 H18B 108.7 . . ? C18 C19 C19 101.7(2) . 3 ? C18 C19 H19A 111.4 . . ? C19 C19 H19A 111.4 3 . ? C18 C19 H19B 111.4 . . ? C19 C19 H19B 111.4 3 . ? H19A C19 H19B 109.3 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.475 _refine_diff_density_min -0.436 _refine_diff_density_rms 0.095