# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 loop_ _publ_author_name _publ_author_address S.M.Cohen ; Department of Chemistry and Biochemistry University of California, San Diego La Jolla CA 92093-0358 USA ; S.J.Garibay ; Department of Chemistry and Biochemistry University of California, San Diego La Jolla CA 92093-0358 USA ; J.R.Stork ; Department of Chemistry and Biochemistry University of California, San Diego La Jolla CA 92093-0358 USA ; Z.Wang ; Department of Chemistry and Biochemistry University of California, San Diego La Jolla CA 92093-0358 USA ; S.Telfer ; MacDiarmid Institute for Advanced Materials and Nanotechnology Institute of Fundamental Sciences Massey University Palmerston North New Zealand ; _publ_contact_author ; Seth M. Cohen Department of Chemistry and Biochemistry University of California, San Diego La Jolla CA 92093-0358 USA ; _publ_contact_author_email scohen@ucsd.edu _publ_section_title ; Enantiopure vs. Racemic Metalloligands: Impact on Metal-Organic Framework Structure and Synthesis ; _publ_contact_author_name 'Seth M. Cohen' # Attachment 'New-MOF-Co-Zn-5a-and-5b.cif' data_sjg02 _database_code_depnum_ccdc_archive 'CCDC 656116' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common MOF-Co/Zn-5a _chemical_melting_point ? _chemical_formula_moiety 'C48 H30.5 Co N6 O8.25 Zn2, C5 H11 N O, O0.25' _chemical_formula_sum 'C53 H41.50 Co N7 O9.50 Zn2' _chemical_formula_weight 1118.10 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' 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 15.229(4) _cell_length_b 8.796(2) _cell_length_c 38.650(11) _cell_angle_alpha 90.00 _cell_angle_beta 89.977(5) _cell_angle_gamma 90.00 _cell_volume 5177(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 977 _cell_measurement_theta_min 2.80 _cell_measurement_theta_max 22.8 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.434 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2286 _exptl_absorpt_coefficient_mu 1.299 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.74449 _exptl_absorpt_correction_T_max 0.96078 _exptl_absorpt_process_details 'SADABS 2.10 (Sheldrick, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43650 _diffrn_reflns_av_R_equivalents 0.0841 _diffrn_reflns_av_sigmaI/netI 0.0842 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 26.37 _reflns_number_total 10531 _reflns_number_gt 7689 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART 5.054 (Bruker, 2003)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT 6.45A (Bruker, 2003)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5.1 (Sheldrick, 1994)' _computing_publication_material SHELXL97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The \b angle is 89.98 degrees. Attempts to integrate and refine the data as orthorhombic were unsuccessful. The structure was refined as a twinned monoclinic crystal via 180 degree rotation about the 0 0 1 reciprocal axis direction. The major twin component refined to 51.90(18) %. The model contains an infinite zinc-oxo cluster. This cluster is disordered about a screw axis, resulting in 50 % occupancy for the Zn atoms. The cluster has three unique \m-2- and \m-3-O atoms. These O atoms are disordered both by the screw axis and by general disorder. The assign- ment of the \m-O atoms to specific Zn atoms was determined on the basis of reasonable bond distances. The \m-3-O atom (O8) was set at an assumed occupancy of 50 %. The \m-2-O atoms (O7 and O9), which are near each other in the idealized cluster but bridge different Zn atoms, were assigned assumed occupancies of 25 %. The thermal parameters of the three \m-O atoms were set mutually equal, and the atoms were left isor. The structure has a disordered solvent region, which appears to contain a mixture of coordinated and free ethanol. Satisfactory atomic positions for the solvent molecules could not be determined, and treating the solvent as a diffuse contribution was unsuccessful, so a single Fourier peak was assigned as an isolated, 25 %-occupied oxygen atom. A DEF solvent molecule displays thermal parameters indicative of wagging about the central N atom. Independent positions for the peripheral DEF atoms could not be determined. The slight unresolved disorder likely contributes to a short O14 ... O12 distance (2.41 ang.) H atoms of the tris-(dipyrrinato)cobalt(III) complex and the DEF solvent molecule were located in a difference map, placed in calculated positions, and treated with a riding model. The model includes three partially occupied and disordered water molecules coordinated to the infinite zinc- oxo cluster in addition to the isolated O atom. Only one H atom was found for these water molecules. The remaining water H atoms were not included in the structural model. ; _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^)+(0.1422P)^2^+2.8876P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 10531 _refine_ls_number_parameters 690 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1109 _refine_ls_R_factor_gt 0.0787 _refine_ls_wR_factor_ref 0.2285 _refine_ls_wR_factor_gt 0.2051 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 0.76003(17) -0.0916(4) 0.24968(6) 0.0618(7) Uani 0.50 1 d P . 1 Zn2 Zn 0.5959(2) 0.2246(3) 0.25247(9) 0.0564(7) Uani 0.50 1 d P . 1 Zn3 Zn 0.75849(15) -0.4948(3) 0.25120(5) 0.0478(6) Uani 0.50 1 d P . 1 Zn4 Zn 0.94567(17) -0.2906(5) 0.24402(8) 0.0592(9) Uani 0.50 1 d P . 1 Co1 Co 0.74218(6) 0.01750(8) 0.54862(2) 0.0254(2) Uani 1 1 d . . . C1 C 0.8219(5) 0.2489(7) 0.59469(18) 0.0303(15) Uani 1 1 d . . . H1 H 0.7954 0.3319 0.5829 0.036 Uiso 1 1 calc R . . C2 C 0.8672(5) 0.2616(7) 0.6249(2) 0.0376(18) Uani 1 1 d . . . H2 H 0.8775 0.3537 0.6371 0.045 Uiso 1 1 calc R . . C3 C 0.8955(5) 0.1203(8) 0.6351(2) 0.0387(17) Uani 1 1 d . . . H3 H 0.9270 0.0946 0.6555 0.046 Uiso 1 1 calc R . . C4 C 0.8671(5) 0.0207(7) 0.60823(19) 0.0305(15) Uani 1 1 d . . . C5 C 0.8873(4) -0.1344(7) 0.60443(17) 0.0274(13) Uani 1 1 d . . . C6 C 0.8627(4) -0.2211(7) 0.57560(18) 0.0266(14) Uani 1 1 d . . . C7 C 0.8907(4) -0.3700(7) 0.56741(19) 0.0322(15) Uani 1 1 d . . . H7 H 0.9266 -0.4337 0.5813 0.039 Uiso 1 1 calc R . . C8 C 0.8555(5) -0.4060(7) 0.53495(18) 0.0322(15) Uani 1 1 d . . . H8 H 0.8636 -0.4977 0.5224 0.039 Uiso 1 1 calc R . . C9 C 0.8054(5) -0.2777(7) 0.52463(18) 0.0302(14) Uani 1 1 d . . . H9 H 0.7737 -0.2711 0.5035 0.036 Uiso 1 1 calc R . . C10 C 0.9378(5) -0.2059(7) 0.63264(18) 0.0346(16) Uani 1 1 d . . . C11 C 0.9002(6) -0.3230(8) 0.6514(2) 0.0425(18) Uani 1 1 d . . . H11 H 0.8430 -0.3578 0.6457 0.051 Uiso 1 1 calc R . . C12 C 0.9465(6) -0.3907(9) 0.6789(2) 0.047(2) Uani 1 1 d . . . H12 H 0.9192 -0.4688 0.6921 0.056 Uiso 1 1 calc R . . C13 C 1.0300(6) -0.3461(9) 0.6871(2) 0.053(2) Uani 1 1 d . . . C14 C 1.0691(6) -0.2318(11) 0.6672(2) 0.059(3) Uani 1 1 d . . . H14 H 1.1279 -0.2023 0.6719 0.071 Uiso 1 1 calc R . . C15 C 1.0231(5) -0.1600(9) 0.6403(2) 0.0415(18) Uani 1 1 d . . . H15 H 1.0500 -0.0805 0.6275 0.050 Uiso 1 1 calc R . . C16 C 1.0827(8) -0.4245(15) 0.7149(2) 0.069(3) Uani 1 1 d . . . C17 C 0.8998(4) 0.1390(7) 0.51631(19) 0.0319(15) Uani 1 1 d . . . H17 H 0.9290 0.1455 0.5380 0.038 Uiso 1 1 calc R . . C18 C 0.9377(5) 0.1833(8) 0.48360(19) 0.0383(16) Uani 1 1 d . . . H18 H 0.9946 0.2235 0.4796 0.046 Uiso 1 1 calc R . . C19 C 0.8737(5) 0.1547(8) 0.4596(2) 0.0391(17) Uani 1 1 d . . . H19 H 0.8781 0.1751 0.4355 0.047 Uiso 1 1 calc R . . C20 C 0.8010(4) 0.0911(7) 0.47605(17) 0.0288(14) Uani 1 1 d . . . C21 C 0.7222(4) 0.0332(7) 0.46149(19) 0.0330(15) Uani 1 1 d . . . C22 C 0.6571(4) -0.0421(7) 0.47999(18) 0.0295(14) Uani 1 1 d . . . C23 C 0.5806(5) -0.1152(7) 0.46519(19) 0.0341(15) Uani 1 1 d . . . H23 H 0.5636 -0.1168 0.4416 0.041 Uiso 1 1 calc R . . C24 C 0.5382(5) -0.1813(7) 0.49245(19) 0.0347(16) Uani 1 1 d . . . H24 H 0.4862 -0.2408 0.4913 0.042 Uiso 1 1 calc R . . C25 C 0.5859(4) -0.1450(7) 0.52277(19) 0.0332(15) Uani 1 1 d . . . H25 H 0.5688 -0.1757 0.5454 0.040 Uiso 1 1 calc R . . C26 C 0.7103(5) 0.0516(7) 0.4235(2) 0.0381(17) Uani 1 1 d . . . C27 C 0.7674(5) -0.0171(8) 0.40049(19) 0.0403(16) Uani 1 1 d . . . H27 H 0.8154 -0.0752 0.4090 0.048 Uiso 1 1 calc R . . C28 C 0.7554(6) -0.0019(8) 0.36563(19) 0.0452(18) Uani 1 1 d . . . H28 H 0.7949 -0.0506 0.3501 0.054 Uiso 1 1 calc R . . C29 C 0.6863(6) 0.0838(10) 0.3525(2) 0.049(2) Uani 1 1 d . . . C30 C 0.6276(6) 0.1562(9) 0.3748(2) 0.049(2) Uani 1 1 d . . . H30 H 0.5803 0.2151 0.3661 0.058 Uiso 1 1 calc R . . C31 C 0.6403(5) 0.1397(8) 0.4102(2) 0.0409(17) Uani 1 1 d . . . H31 H 0.6013 0.1886 0.4257 0.049 Uiso 1 1 calc R . . C32 C 0.6748(8) 0.0939(13) 0.3132(2) 0.066(3) Uani 1 1 d . . . C33 C 0.6820(5) 0.3188(7) 0.5253(2) 0.0321(15) Uani 1 1 d . . . H33 H 0.7151 0.3127 0.5045 0.039 Uiso 1 1 calc R . . C34 C 0.6331(5) 0.4472(7) 0.5355(2) 0.0354(16) Uani 1 1 d . . . H34 H 0.6260 0.5393 0.5230 0.042 Uiso 1 1 calc R . . C35 C 0.5984(5) 0.4129(7) 0.5666(2) 0.0397(18) Uani 1 1 d . . . H35 H 0.5626 0.4776 0.5803 0.048 Uiso 1 1 calc R . . C36 C 0.6251(4) 0.2615(7) 0.5753(2) 0.0315(15) Uani 1 1 d . . . C37 C 0.6036(5) 0.1775(7) 0.60470(19) 0.0337(15) Uani 1 1 d . . . C38 C 0.6248(5) 0.0254(7) 0.6102(2) 0.0328(16) Uani 1 1 d . . . C39 C 0.5980(5) -0.0713(8) 0.6373(2) 0.0377(16) Uani 1 1 d . . . H39 H 0.5659 -0.0420 0.6573 0.045 Uiso 1 1 calc R . . C40 C 0.6265(5) -0.2138(8) 0.6297(2) 0.0381(17) Uani 1 1 d . . . H40 H 0.6172 -0.3033 0.6430 0.046 Uiso 1 1 calc R . . C41 C 0.6720(4) -0.2026(7) 0.59843(18) 0.0309(14) Uani 1 1 d . . . H41 H 0.6987 -0.2861 0.5869 0.037 Uiso 1 1 calc R . . C42 C 0.5529(5) 0.2564(8) 0.6325(2) 0.0374(17) Uani 1 1 d . . . C43 C 0.5905(6) 0.3697(8) 0.6519(2) 0.0451(19) Uani 1 1 d . . . H43 H 0.6486 0.4011 0.6466 0.054 Uiso 1 1 calc R . . C44 C 0.5471(6) 0.4397(8) 0.6788(2) 0.047(2) Uani 1 1 d . . . H44 H 0.5750 0.5166 0.6921 0.056 Uiso 1 1 calc R . . C45 C 0.4625(6) 0.3958(9) 0.6860(2) 0.050(2) Uani 1 1 d . . . C46 C 0.4221(6) 0.2810(9) 0.6670(3) 0.054(2) Uani 1 1 d . . . H46 H 0.3642 0.2486 0.6725 0.065 Uiso 1 1 calc R . . C47 C 0.4671(6) 0.2151(9) 0.6400(2) 0.0467(19) Uani 1 1 d . . . H47 H 0.4390 0.1399 0.6263 0.056 Uiso 1 1 calc R . . C48 C 0.4137(7) 0.4759(10) 0.7147(2) 0.054(2) Uani 1 1 d . . . N1 N 0.8193(3) 0.1041(5) 0.58365(14) 0.0266(11) Uani 1 1 d . . . N2 N 0.8085(3) -0.1669(5) 0.54854(14) 0.0263(11) Uani 1 1 d . . . N3 N 0.8186(4) 0.0880(6) 0.51203(15) 0.0287(12) Uani 1 1 d . . . N4 N 0.6575(4) -0.0627(5) 0.51595(15) 0.0285(12) Uani 1 1 d . . . N5 N 0.6761(4) 0.2074(5) 0.54834(14) 0.0285(11) Uani 1 1 d . . . N6 N 0.6733(3) -0.0616(5) 0.58695(15) 0.0268(12) Uani 1 1 d . . . O1 O 1.0445(8) -0.5274(15) 0.7321(3) 0.130(4) Uani 1 1 d . . . O2 O 1.1603(5) -0.3855(11) 0.7181(2) 0.092(3) Uani 1 1 d . . . O3 O 0.6044(5) 0.1662(9) 0.30346(17) 0.074(2) Uani 1 1 d . . . O4 O 0.7323(5) 0.0324(10) 0.29540(17) 0.079(2) Uani 1 1 d . . . O5 O 0.4562(5) 0.5693(10) 0.73319(19) 0.080(2) Uani 1 1 d . . . O6 O 0.3338(5) 0.4480(8) 0.71740(18) 0.0702(19) Uani 1 1 d . . . O7 O 0.7216(11) 0.112(2) 0.2439(5) 0.0273(16) Uiso 0.25 1 d P . 1 O8 O 0.8139(6) -0.2750(11) 0.2634(2) 0.0273(16) Uiso 0.50 1 d P . 1 O9 O 0.7087(12) -0.705(2) 0.2328(5) 0.0273(16) Uiso 0.25 1 d P . 1 O10 O 1.0776(12) -0.308(2) 0.2283(4) 0.092(5) Uiso 0.50 1 d P A 1 H1WA H 1.0910 -0.4007 0.2265 0.138 Uiso 0.50 1 d PR A 1 O11 O 1.235(3) -0.648(6) 0.2112(12) 0.140(15) Uiso 0.25 1 d P . . O12 O 0.544(6) 0.345(3) 0.2051(9) 0.106(16) Uani 0.37(7) 1 d P B 1 O13 O 1.003(3) -0.226(8) 0.2908(6) 0.09(2) Uani 0.38(7) 1 d P B 1 C49 C 0.6711(11) 0.1277(16) 0.1471(3) 0.097(4) Uani 1 1 d . . . H49 H 0.7226 0.1203 0.1608 0.116 Uiso 1 1 calc R . . C50 C 0.7464(8) -0.0278(12) 0.1073(4) 0.089(4) Uani 1 1 d . . . H50A H 0.7277 -0.1326 0.1015 0.107 Uiso 1 1 calc R . . H50B H 0.7879 -0.0345 0.1269 0.107 Uiso 1 1 calc R . . C51 C 0.7934(10) 0.0352(15) 0.0773(6) 0.148(8) Uani 1 1 d . . . H51A H 0.7523 0.0484 0.0580 0.222 Uiso 1 1 calc R . . H51B H 0.8404 -0.0345 0.0704 0.222 Uiso 1 1 calc R . . H51C H 0.8188 0.1339 0.0835 0.222 Uiso 1 1 calc R . . C52 C 0.5928(7) 0.0436(13) 0.0981(3) 0.080(3) Uani 1 1 d . . . H52A H 0.5422 0.0353 0.1141 0.096 Uiso 1 1 calc R . . H52B H 0.5959 -0.0526 0.0848 0.096 Uiso 1 1 calc R . . C53 C 0.5748(9) 0.1681(15) 0.0736(4) 0.111(6) Uani 1 1 d . . . H53A H 0.5574 0.2594 0.0864 0.166 Uiso 1 1 calc R . . H53B H 0.5272 0.1381 0.0579 0.166 Uiso 1 1 calc R . . H53C H 0.6278 0.1898 0.0600 0.166 Uiso 1 1 calc R . . N7 N 0.6708(5) 0.0565(8) 0.11828(18) 0.0483(16) Uani 1 1 d . . . O14 O 0.6107(10) 0.2045(14) 0.1586(4) 0.164(7) 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 Zn1 0.0469(14) 0.102(2) 0.0366(11) -0.0083(14) 0.0042(10) -0.0182(15) Zn2 0.074(2) 0.0478(12) 0.0476(16) -0.0152(10) -0.0164(19) 0.0011(16) Zn3 0.0343(11) 0.0812(17) 0.0278(9) 0.0130(11) 0.0027(8) -0.0046(12) Zn4 0.0352(14) 0.111(2) 0.0315(12) 0.0146(12) -0.0035(13) -0.0039(15) Co1 0.0269(4) 0.0170(3) 0.0324(4) 0.0007(3) -0.0008(4) -0.0019(3) C1 0.031(3) 0.025(3) 0.035(4) -0.001(3) 0.001(3) -0.008(3) C2 0.048(5) 0.014(3) 0.051(5) -0.005(3) -0.002(4) -0.007(3) C3 0.043(4) 0.028(3) 0.045(4) 0.003(3) -0.011(3) -0.002(3) C4 0.036(4) 0.017(3) 0.038(4) -0.002(3) 0.002(3) -0.002(3) C5 0.024(3) 0.022(3) 0.035(4) -0.002(3) 0.000(3) -0.005(2) C6 0.026(3) 0.022(3) 0.033(4) 0.007(3) 0.000(3) -0.003(2) C7 0.026(3) 0.026(3) 0.045(4) 0.004(3) 0.005(3) 0.003(3) C8 0.035(4) 0.023(3) 0.039(4) -0.005(3) 0.003(3) 0.004(3) C9 0.037(4) 0.025(3) 0.028(4) 0.001(3) 0.003(3) -0.005(3) C10 0.041(4) 0.025(3) 0.038(4) -0.004(3) -0.012(3) 0.001(3) C11 0.051(5) 0.030(4) 0.046(4) 0.009(3) -0.004(4) -0.003(3) C12 0.064(6) 0.040(4) 0.036(4) 0.013(3) -0.004(4) 0.008(4) C13 0.070(6) 0.039(4) 0.050(5) 0.000(4) -0.006(4) 0.017(4) C14 0.047(5) 0.066(6) 0.064(6) -0.024(5) -0.024(5) 0.019(4) C15 0.044(4) 0.038(4) 0.043(4) 0.003(3) -0.008(3) -0.006(3) C16 0.077(8) 0.099(8) 0.030(5) -0.015(5) -0.008(5) 0.020(6) C17 0.031(4) 0.029(3) 0.036(4) 0.006(3) 0.003(3) -0.008(3) C18 0.035(4) 0.039(4) 0.041(4) 0.006(3) 0.004(3) -0.005(3) C19 0.041(4) 0.032(4) 0.044(4) 0.004(3) 0.001(3) -0.001(3) C20 0.032(4) 0.020(3) 0.034(4) 0.001(3) 0.005(3) 0.004(3) C21 0.031(4) 0.026(3) 0.042(4) 0.003(3) 0.000(3) 0.002(3) C22 0.029(4) 0.026(3) 0.034(4) 0.001(3) -0.004(3) 0.001(3) C23 0.032(4) 0.032(3) 0.038(4) -0.006(3) -0.006(3) 0.003(3) C24 0.035(4) 0.027(3) 0.042(4) -0.006(3) -0.007(3) -0.005(3) C25 0.034(4) 0.019(3) 0.047(4) 0.001(3) 0.000(3) -0.004(3) C26 0.049(4) 0.022(3) 0.043(4) 0.003(3) -0.006(3) -0.008(3) C27 0.047(4) 0.033(3) 0.041(4) -0.001(3) -0.005(4) -0.003(3) C28 0.045(4) 0.049(4) 0.041(4) 0.000(3) 0.005(4) -0.015(4) C29 0.053(5) 0.059(5) 0.035(4) 0.008(4) -0.007(4) -0.025(4) C30 0.047(5) 0.048(5) 0.051(5) 0.021(4) -0.017(4) -0.013(4) C31 0.039(4) 0.038(4) 0.046(4) 0.008(3) -0.004(3) -0.002(3) C32 0.079(7) 0.085(7) 0.034(5) 0.010(5) -0.017(5) -0.046(6) C33 0.029(3) 0.020(3) 0.047(4) 0.005(3) -0.002(3) -0.006(3) C34 0.037(4) 0.018(3) 0.051(5) 0.003(3) -0.010(3) -0.003(3) C35 0.032(4) 0.020(3) 0.066(5) -0.002(3) -0.011(4) 0.006(3) C36 0.031(4) 0.015(3) 0.048(4) 0.001(3) -0.001(3) 0.000(2) C37 0.034(4) 0.023(3) 0.044(4) -0.007(3) -0.002(3) -0.002(3) C38 0.030(3) 0.029(4) 0.040(4) -0.002(3) 0.007(3) -0.008(3) C39 0.042(4) 0.030(4) 0.041(4) 0.009(3) 0.013(3) -0.002(3) C40 0.044(4) 0.029(4) 0.042(4) 0.007(3) 0.012(3) 0.002(3) C41 0.034(3) 0.021(3) 0.038(4) 0.002(3) 0.000(3) -0.004(3) C42 0.043(4) 0.024(3) 0.045(4) 0.001(3) 0.010(4) -0.003(3) C43 0.054(5) 0.028(4) 0.054(5) -0.004(3) 0.012(4) -0.009(3) C44 0.060(5) 0.031(4) 0.050(5) -0.007(3) 0.015(4) -0.006(4) C45 0.065(6) 0.042(5) 0.043(5) 0.001(4) 0.013(4) 0.007(4) C46 0.047(5) 0.039(4) 0.076(6) -0.006(4) 0.012(5) -0.009(4) C47 0.050(5) 0.035(4) 0.056(5) -0.006(4) 0.014(4) -0.005(4) C48 0.066(6) 0.046(5) 0.050(5) 0.008(4) 0.018(5) 0.002(4) N1 0.031(3) 0.014(2) 0.034(3) -0.001(2) -0.004(2) 0.000(2) N2 0.029(3) 0.025(2) 0.025(3) 0.002(2) -0.001(2) -0.004(2) N3 0.031(3) 0.020(2) 0.035(3) 0.004(2) -0.007(2) -0.006(2) N4 0.026(3) 0.020(2) 0.039(3) 0.004(2) -0.002(2) -0.002(2) N5 0.034(3) 0.024(2) 0.028(3) 0.001(2) -0.001(3) 0.004(2) N6 0.025(3) 0.016(2) 0.039(3) -0.001(2) 0.001(2) 0.000(2) O1 0.126(9) 0.185(11) 0.078(6) 0.065(7) -0.017(6) 0.038(8) O2 0.070(5) 0.125(7) 0.082(5) 0.013(5) -0.036(4) 0.022(5) O3 0.090(5) 0.084(5) 0.049(4) 0.019(3) -0.029(4) -0.030(4) O4 0.073(5) 0.132(6) 0.033(3) 0.006(4) -0.003(3) -0.033(5) O5 0.067(5) 0.106(6) 0.067(5) -0.039(4) 0.004(4) 0.007(4) O6 0.070(5) 0.082(5) 0.058(4) -0.006(4) 0.027(4) -0.012(4) O12 0.18(4) 0.056(16) 0.085(18) -0.021(12) -0.02(2) 0.00(2) O13 0.08(2) 0.14(4) 0.044(12) 0.023(16) -0.029(12) -0.07(2) C49 0.113(11) 0.106(10) 0.072(8) 0.000(7) 0.023(7) -0.059(9) C50 0.064(7) 0.060(5) 0.143(11) 0.023(6) -0.012(8) 0.010(6) C51 0.116(12) 0.070(7) 0.26(2) 0.003(11) 0.118(14) 0.029(8) C52 0.067(7) 0.074(7) 0.099(9) 0.021(6) -0.034(6) -0.025(5) C53 0.084(9) 0.101(9) 0.148(12) 0.062(9) -0.060(9) -0.053(7) N7 0.051(4) 0.052(4) 0.042(4) 0.000(3) -0.002(3) -0.004(3) O14 0.194(13) 0.128(9) 0.169(12) -0.052(8) 0.131(11) -0.059(9) _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 O8 1.886(10) . ? Zn1 O7 1.90(2) . ? Zn1 O2 1.958(7) 4 ? Zn1 O6 2.101(7) 4_665 ? Zn1 O4 2.119(8) . ? Zn2 O9 1.98(2) 1_565 ? Zn2 O3 2.041(7) . ? Zn2 O5 2.055(9) 3_666 ? Zn2 O1 2.059(10) 4 ? Zn2 O7 2.180(19) . ? Zn2 O12 2.26(3) . ? Zn3 O4 1.822(7) 2_645 ? Zn3 O6 1.902(7) 3_656 ? Zn3 O2 2.011(7) 3_746 ? Zn3 O9 2.12(2) . ? Zn3 O8 2.161(10) . ? Zn4 O1 1.853(11) 3_746 ? Zn4 O5 1.997(9) 4_665 ? Zn4 O3 2.023(7) 2_645 ? Zn4 O13 2.08(2) . ? Zn4 O10 2.105(18) . ? Zn4 O8 2.145(10) . ? Co1 N2 1.911(5) . ? Co1 N3 1.934(6) . ? Co1 N4 1.938(6) . ? Co1 N6 1.943(6) . ? Co1 N1 1.947(5) . ? Co1 N5 1.950(5) . ? C1 N1 1.344(8) . ? C1 C2 1.363(10) . ? C1 H1 0.9500 . ? C2 C3 1.373(10) . ? C2 H2 0.9500 . ? C3 C4 1.426(10) . ? C3 H3 0.9500 . ? C4 N1 1.404(9) . ? C4 C5 1.406(8) . ? C5 C6 1.402(9) . ? C5 C10 1.475(9) . ? C6 C7 1.413(9) . ? C6 N2 1.414(8) . ? C7 C8 1.401(10) . ? C7 H7 0.9500 . ? C8 C9 1.420(9) . ? C8 H8 0.9500 . ? C9 N2 1.344(8) . ? C9 H9 0.9500 . ? C10 C11 1.384(10) . ? C10 C15 1.393(11) . ? C11 C12 1.408(11) . ? C11 H11 0.9500 . ? C12 C13 1.368(13) . ? C12 H12 0.9500 . ? C13 C14 1.400(14) . ? C13 C16 1.508(13) . ? C14 C15 1.402(12) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 O2 1.237(14) . ? C16 O1 1.266(16) . ? C17 N3 1.325(9) . ? C17 C18 1.443(10) . ? C17 H17 0.9500 . ? C18 C19 1.368(11) . ? C18 H18 0.9500 . ? C19 C20 1.394(10) . ? C19 H19 0.9500 . ? C20 N3 1.417(9) . ? C20 C21 1.420(10) . ? C21 C22 1.391(10) . ? C21 C26 1.489(11) . ? C22 N4 1.402(9) . ? C22 C23 1.448(9) . ? C23 C24 1.366(10) . ? C23 H23 0.9500 . ? C24 C25 1.415(10) . ? C24 H24 0.9500 . ? C25 N4 1.336(8) . ? C25 H25 0.9500 . ? C26 C27 1.382(11) . ? C26 C31 1.415(10) . ? C27 C28 1.366(11) . ? C27 H27 0.9500 . ? C28 C29 1.391(13) . ? C28 H28 0.9500 . ? C29 C30 1.396(13) . ? C29 C32 1.531(12) . ? C30 C31 1.386(11) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 O4 1.239(14) . ? C32 O3 1.302(14) . ? C33 N5 1.326(8) . ? C33 C34 1.410(10) . ? C33 H33 0.9500 . ? C34 C35 1.345(11) . ? C34 H34 0.9500 . ? C35 C36 1.433(9) . ? C35 H35 0.9500 . ? C36 N5 1.383(9) . ? C36 C37 1.395(10) . ? C37 C38 1.393(10) . ? C37 C42 1.493(10) . ? C38 N6 1.391(9) . ? C38 C39 1.411(10) . ? C39 C40 1.359(10) . ? C39 H39 0.9500 . ? C40 C41 1.396(10) . ? C40 H40 0.9500 . ? C41 N6 1.318(8) . ? C41 H41 0.9500 . ? C42 C43 1.373(11) . ? C42 C47 1.387(11) . ? C43 C44 1.377(11) . ? C43 H43 0.9500 . ? C44 C45 1.373(12) . ? C44 H44 0.9500 . ? C45 C46 1.393(12) . ? C45 C48 1.510(12) . ? C46 C47 1.375(12) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? C48 O6 1.246(12) . ? C48 O5 1.266(12) . ? O1 Zn4 1.853(11) 3_746 ? O1 Zn2 2.059(10) 4_656 ? O2 Zn1 1.958(7) 4_656 ? O2 Zn3 2.011(7) 3_746 ? O3 Zn4 2.023(7) 2_655 ? O4 Zn3 1.822(7) 2_655 ? O5 Zn4 1.997(9) 4_566 ? O5 Zn2 2.055(9) 3_666 ? O6 Zn3 1.902(7) 3_656 ? O6 Zn1 2.101(7) 4_566 ? O7 Zn3 1.005(19) 2_655 ? O8 Zn2 1.503(10) 2_645 ? O9 Zn1 1.294(19) 2_645 ? O9 Zn2 1.98(2) 1_545 ? O10 H1WA 0.8400 . ? C49 O14 1.224(19) . ? C49 N7 1.277(14) . ? C49 H49 0.9500 . ? C50 N7 1.434(14) . ? C50 C51 1.470(18) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 N7 1.426(12) . ? C52 C53 1.474(15) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 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 O8 Zn1 O7 167.1(6) . . ? O8 Zn1 O2 115.1(4) . 4 ? O7 Zn1 O2 77.6(6) . 4 ? O8 Zn1 O6 116.6(4) . 4_665 ? O7 Zn1 O6 61.8(6) . 4_665 ? O2 Zn1 O6 96.1(4) 4 4_665 ? O8 Zn1 O4 107.0(4) . . ? O7 Zn1 O4 63.3(6) . . ? O2 Zn1 O4 114.7(4) 4 . ? O6 Zn1 O4 107.0(3) 4_665 . ? O9 Zn2 O3 113.2(6) 1_565 . ? O9 Zn2 O5 99.3(6) 1_565 3_666 ? O3 Zn2 O5 89.2(4) . 3_666 ? O9 Zn2 O1 116.6(6) 1_565 4 ? O3 Zn2 O1 100.4(4) . 4 ? O5 Zn2 O1 134.4(4) 3_666 4 ? O9 Zn2 O7 47.3(7) 1_565 . ? O3 Zn2 O7 88.6(6) . . ? O5 Zn2 O7 141.3(5) 3_666 . ? O1 Zn2 O7 83.9(6) 4 . ? O9 Zn2 O12 81(2) 1_565 . ? O3 Zn2 O12 157.4(17) . . ? O5 Zn2 O12 70.7(9) 3_666 . ? O1 Zn2 O12 87.2(13) 4 . ? O7 Zn2 O12 113(2) . . ? O4 Zn3 O6 131.2(4) 2_645 3_656 ? O4 Zn3 O2 127.2(4) 2_645 3_746 ? O6 Zn3 O2 101.0(4) 3_656 3_746 ? O4 Zn3 O9 79.0(6) 2_645 . ? O6 Zn3 O9 98.0(6) 3_656 . ? O2 Zn3 O9 87.8(6) 3_746 . ? O4 Zn3 O8 93.9(4) 2_645 . ? O6 Zn3 O8 87.5(3) 3_656 . ? O2 Zn3 O8 95.7(4) 3_746 . ? O9 Zn3 O8 172.9(6) . . ? O1 Zn4 O5 160.0(5) 3_746 4_665 ? O1 Zn4 O3 108.6(5) 3_746 2_645 ? O5 Zn4 O3 91.3(3) 4_665 2_645 ? O1 Zn4 O13 76.6(19) 3_746 . ? O5 Zn4 O13 83.3(18) 4_665 . ? O3 Zn4 O13 174.2(13) 2_645 . ? O1 Zn4 O10 90.1(6) 3_746 . ? O5 Zn4 O10 86.3(5) 4_665 . ? O3 Zn4 O10 94.9(5) 2_645 . ? O13 Zn4 O10 82.7(16) . . ? O1 Zn4 O8 87.6(5) 3_746 . ? O5 Zn4 O8 94.9(4) 4_665 . ? O3 Zn4 O8 88.6(3) 2_645 . ? O13 Zn4 O8 94.0(15) . . ? O10 Zn4 O8 176.3(6) . . ? N2 Co1 N3 87.3(2) . . ? N2 Co1 N4 92.4(2) . . ? N3 Co1 N4 92.3(2) . . ? N2 Co1 N6 89.0(2) . . ? N3 Co1 N6 175.5(2) . . ? N4 Co1 N6 90.4(2) . . ? N2 Co1 N1 90.8(2) . . ? N3 Co1 N1 91.1(2) . . ? N4 Co1 N1 175.4(2) . . ? N6 Co1 N1 86.3(2) . . ? N2 Co1 N5 179.0(2) . . ? N3 Co1 N5 91.8(2) . . ? N4 Co1 N5 88.0(2) . . ? N6 Co1 N5 91.9(2) . . ? N1 Co1 N5 88.8(2) . . ? N1 C1 C2 111.4(6) . . ? N1 C1 H1 124.3 . . ? C2 C1 H1 124.3 . . ? C1 C2 C3 109.3(6) . . ? C1 C2 H2 125.4 . . ? C3 C2 H2 125.4 . . ? C2 C3 C4 104.7(6) . . ? C2 C3 H3 127.7 . . ? C4 C3 H3 127.7 . . ? N1 C4 C5 123.3(6) . . ? N1 C4 C3 109.2(5) . . ? C5 C4 C3 127.3(6) . . ? C6 C5 C4 123.5(6) . . ? C6 C5 C10 119.7(5) . . ? C4 C5 C10 116.8(6) . . ? C5 C6 C7 127.0(6) . . ? C5 C6 N2 124.1(5) . . ? C7 C6 N2 108.8(6) . . ? C8 C7 C6 107.1(6) . . ? C8 C7 H7 126.4 . . ? C6 C7 H7 126.4 . . ? C7 C8 C9 106.1(6) . . ? C7 C8 H8 126.9 . . ? C9 C8 H8 126.9 . . ? N2 C9 C8 111.3(6) . . ? N2 C9 H9 124.3 . . ? C8 C9 H9 124.3 . . ? C11 C10 C15 119.3(7) . . ? C11 C10 C5 119.3(6) . . ? C15 C10 C5 121.4(7) . . ? C10 C11 C12 120.3(8) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C13 C12 C11 121.3(8) . . ? C13 C12 H12 119.4 . . ? C11 C12 H12 119.4 . . ? C12 C13 C14 118.3(8) . . ? C12 C13 C16 121.9(9) . . ? C14 C13 C16 119.6(9) . . ? C13 C14 C15 121.3(9) . . ? C13 C14 H14 119.4 . . ? C15 C14 H14 119.4 . . ? C10 C15 C14 119.6(8) . . ? C10 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? O2 C16 O1 125.8(11) . . ? O2 C16 C13 117.0(11) . . ? O1 C16 C13 117.2(10) . . ? N3 C17 C18 110.8(6) . . ? N3 C17 H17 124.6 . . ? C18 C17 H17 124.6 . . ? C19 C18 C17 105.0(6) . . ? C19 C18 H18 127.5 . . ? C17 C18 H18 127.5 . . ? C18 C19 C20 109.3(7) . . ? C18 C19 H19 125.3 . . ? C20 C19 H19 125.3 . . ? C19 C20 N3 107.7(6) . . ? C19 C20 C21 129.4(7) . . ? N3 C20 C21 122.9(6) . . ? C22 C21 C20 124.7(7) . . ? C22 C21 C26 118.2(6) . . ? C20 C21 C26 117.1(6) . . ? C21 C22 N4 124.6(6) . . ? C21 C22 C23 125.6(7) . . ? N4 C22 C23 109.8(6) . . ? C24 C23 C22 105.3(6) . . ? C24 C23 H23 127.3 . . ? C22 C23 H23 127.3 . . ? C23 C24 C25 107.5(6) . . ? C23 C24 H24 126.3 . . ? C25 C24 H24 126.3 . . ? N4 C25 C24 112.2(6) . . ? N4 C25 H25 123.9 . . ? C24 C25 H25 123.9 . . ? C27 C26 C31 118.7(7) . . ? C27 C26 C21 120.7(6) . . ? C31 C26 C21 120.7(7) . . ? C28 C27 C26 120.5(7) . . ? C28 C27 H27 119.8 . . ? C26 C27 H27 119.8 . . ? C27 C28 C29 120.9(8) . . ? C27 C28 H28 119.6 . . ? C29 C28 H28 119.6 . . ? C28 C29 C30 120.5(7) . . ? C28 C29 C32 118.7(9) . . ? C30 C29 C32 120.9(9) . . ? C31 C30 C29 118.1(8) . . ? C31 C30 H30 121.0 . . ? C29 C30 H30 121.0 . . ? C30 C31 C26 121.4(8) . . ? C30 C31 H31 119.3 . . ? C26 C31 H31 119.3 . . ? O4 C32 O3 129.3(9) . . ? O4 C32 C29 116.5(10) . . ? O3 C32 C29 114.2(10) . . ? N5 C33 C34 111.6(7) . . ? N5 C33 H33 124.2 . . ? C34 C33 H33 124.2 . . ? C35 C34 C33 106.1(6) . . ? C35 C34 H34 126.9 . . ? C33 C34 H34 126.9 . . ? C34 C35 C36 107.8(7) . . ? C34 C35 H35 126.1 . . ? C36 C35 H35 126.1 . . ? N5 C36 C37 124.3(6) . . ? N5 C36 C35 107.6(6) . . ? C37 C36 C35 128.1(7) . . ? C38 C37 C36 125.3(7) . . ? C38 C37 C42 117.2(6) . . ? C36 C37 C42 117.5(6) . . ? N6 C38 C37 123.6(7) . . ? N6 C38 C39 107.6(6) . . ? C37 C38 C39 128.7(7) . . ? C40 C39 C38 107.6(7) . . ? C40 C39 H39 126.2 . . ? C38 C39 H39 126.2 . . ? C39 C40 C41 106.3(6) . . ? C39 C40 H40 126.8 . . ? C41 C40 H40 126.8 . . ? N6 C41 C40 111.4(6) . . ? N6 C41 H41 124.3 . . ? C40 C41 H41 124.3 . . ? C43 C42 C47 117.9(7) . . ? C43 C42 C37 121.0(7) . . ? C47 C42 C37 121.0(7) . . ? C42 C43 C44 122.5(8) . . ? C42 C43 H43 118.8 . . ? C44 C43 H43 118.8 . . ? C45 C44 C43 118.6(8) . . ? C45 C44 H44 120.7 . . ? C43 C44 H44 120.7 . . ? C44 C45 C46 120.7(8) . . ? C44 C45 C48 118.6(8) . . ? C46 C45 C48 120.6(8) . . ? C47 C46 C45 119.0(8) . . ? C47 C46 H46 120.5 . . ? C45 C46 H46 120.5 . . ? C46 C47 C42 121.2(8) . . ? C46 C47 H47 119.4 . . ? C42 C47 H47 119.4 . . ? O6 C48 O5 125.5(9) . . ? O6 C48 C45 116.7(9) . . ? O5 C48 C45 117.8(9) . . ? C1 N1 C4 105.4(5) . . ? C1 N1 Co1 127.5(4) . . ? C4 N1 Co1 125.4(4) . . ? C9 N2 C6 106.5(5) . . ? C9 N2 Co1 126.7(5) . . ? C6 N2 Co1 126.4(4) . . ? C17 N3 C20 107.0(6) . . ? C17 N3 Co1 125.3(5) . . ? C20 N3 Co1 127.6(4) . . ? C25 N4 C22 105.1(6) . . ? C25 N4 Co1 127.8(5) . . ? C22 N4 Co1 127.1(4) . . ? C33 N5 C36 106.8(5) . . ? C33 N5 Co1 127.0(5) . . ? C36 N5 Co1 125.5(4) . . ? C41 N6 C38 107.0(6) . . ? C41 N6 Co1 127.0(5) . . ? C38 N6 Co1 125.5(4) . . ? C16 O1 Zn4 147.4(10) . 3_746 ? C16 O1 Zn2 129.0(9) . 4_656 ? C16 O2 Zn1 140.8(8) . 4_656 ? C16 O2 Zn3 120.1(9) . 3_746 ? C32 O3 Zn4 131.7(7) . 2_655 ? C32 O3 Zn2 117.1(7) . . ? C32 O4 Zn3 131.4(7) . 2_655 ? C32 O4 Zn1 146.0(6) . . ? C48 O5 Zn4 135.2(7) . 4_566 ? C48 O5 Zn2 121.8(7) . 3_666 ? C48 O6 Zn3 137.0(7) . 3_656 ? C48 O6 Zn1 116.9(6) . 4_566 ? Zn3 O7 Zn2 131.4(13) 2_655 . ? Zn1 O7 Zn2 133.0(9) . . ? Zn2 O8 Zn1 106.6(5) 2_645 . ? Zn1 O8 Zn4 111.3(4) . . ? Zn2 O8 Zn3 105.5(5) 2_645 . ? Zn1 O8 Zn3 122.3(5) . . ? Zn4 O8 Zn3 103.4(4) . . ? Zn1 O9 Zn2 111.1(11) 2_645 1_545 ? Zn2 O9 Zn3 117.1(9) 1_545 . ? Zn4 O10 H1WA 109.1 . . ? O14 C49 N7 125.8(16) . . ? O14 C49 H49 117.1 . . ? N7 C49 H49 117.1 . . ? N7 C50 C51 115.4(9) . . ? N7 C50 H50A 108.4 . . ? C51 C50 H50A 108.4 . . ? N7 C50 H50B 108.4 . . ? C51 C50 H50B 108.4 . . ? H50A C50 H50B 107.5 . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? N7 C52 C53 116.6(8) . . ? N7 C52 H52A 108.1 . . ? C53 C52 H52A 108.1 . . ? N7 C52 H52B 108.1 . . ? C53 C52 H52B 108.1 . . ? H52A C52 H52B 107.3 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C49 N7 C52 121.3(11) . . ? C49 N7 C50 120.6(11) . . ? C52 N7 C50 117.7(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -0.8(9) . . . . ? C1 C2 C3 C4 2.1(9) . . . . ? C2 C3 C4 N1 -2.6(8) . . . . ? C2 C3 C4 C5 173.0(7) . . . . ? N1 C4 C5 C6 0.8(10) . . . . ? C3 C4 C5 C6 -174.3(7) . . . . ? N1 C4 C5 C10 -179.8(6) . . . . ? C3 C4 C5 C10 5.1(11) . . . . ? C4 C5 C6 C7 170.2(7) . . . . ? C10 C5 C6 C7 -9.3(10) . . . . ? C4 C5 C6 N2 -5.7(10) . . . . ? C10 C5 C6 N2 174.9(6) . . . . ? C5 C6 C7 C8 -175.0(6) . . . . ? N2 C6 C7 C8 1.4(7) . . . . ? C6 C7 C8 C9 -1.1(7) . . . . ? C7 C8 C9 N2 0.4(8) . . . . ? C6 C5 C10 C11 -63.3(9) . . . . ? C4 C5 C10 C11 117.3(7) . . . . ? C6 C5 C10 C15 115.5(8) . . . . ? C4 C5 C10 C15 -63.9(10) . . . . ? C15 C10 C11 C12 2.6(12) . . . . ? C5 C10 C11 C12 -178.6(7) . . . . ? C10 C11 C12 C13 -1.9(12) . . . . ? C11 C12 C13 C14 -0.6(13) . . . . ? C11 C12 C13 C16 -175.8(8) . . . . ? C12 C13 C14 C15 2.5(13) . . . . ? C16 C13 C14 C15 177.8(8) . . . . ? C11 C10 C15 C14 -0.7(11) . . . . ? C5 C10 C15 C14 -179.5(7) . . . . ? C13 C14 C15 C10 -1.9(12) . . . . ? C12 C13 C16 O2 173.2(9) . . . . ? C14 C13 C16 O2 -1.9(14) . . . . ? C12 C13 C16 O1 -4.6(15) . . . . ? C14 C13 C16 O1 -179.7(10) . . . . ? N3 C17 C18 C19 -0.2(8) . . . . ? C17 C18 C19 C20 -2.0(8) . . . . ? C18 C19 C20 N3 3.5(8) . . . . ? C18 C19 C20 C21 -175.0(6) . . . . ? C19 C20 C21 C22 173.2(7) . . . . ? N3 C20 C21 C22 -5.0(10) . . . . ? C19 C20 C21 C26 -5.1(10) . . . . ? N3 C20 C21 C26 176.7(6) . . . . ? C20 C21 C22 N4 4.4(10) . . . . ? C26 C21 C22 N4 -177.4(6) . . . . ? C20 C21 C22 C23 -173.4(6) . . . . ? C26 C21 C22 C23 4.8(10) . . . . ? C21 C22 C23 C24 176.5(6) . . . . ? N4 C22 C23 C24 -1.6(7) . . . . ? C22 C23 C24 C25 1.9(7) . . . . ? C23 C24 C25 N4 -1.7(8) . . . . ? C22 C21 C26 C27 -115.8(7) . . . . ? C20 C21 C26 C27 62.6(8) . . . . ? C22 C21 C26 C31 64.2(9) . . . . ? C20 C21 C26 C31 -117.4(7) . . . . ? C31 C26 C27 C28 -1.1(10) . . . . ? C21 C26 C27 C28 178.9(7) . . . . ? C26 C27 C28 C29 0.6(11) . . . . ? C27 C28 C29 C30 0.0(11) . . . . ? C27 C28 C29 C32 -178.6(7) . . . . ? C28 C29 C30 C31 -0.2(11) . . . . ? C32 C29 C30 C31 178.5(7) . . . . ? C29 C30 C31 C26 -0.3(11) . . . . ? C27 C26 C31 C30 0.9(11) . . . . ? C21 C26 C31 C30 -179.1(7) . . . . ? C28 C29 C32 O4 -4.8(12) . . . . ? C30 C29 C32 O4 176.6(8) . . . . ? C28 C29 C32 O3 174.8(7) . . . . ? C30 C29 C32 O3 -3.9(11) . . . . ? N5 C33 C34 C35 1.9(8) . . . . ? C33 C34 C35 C36 -0.9(8) . . . . ? C34 C35 C36 N5 -0.3(8) . . . . ? C34 C35 C36 C37 -178.8(7) . . . . ? N5 C36 C37 C38 -4.7(11) . . . . ? C35 C36 C37 C38 173.6(7) . . . . ? N5 C36 C37 C42 175.9(6) . . . . ? C35 C36 C37 C42 -5.8(11) . . . . ? C36 C37 C38 N6 2.1(11) . . . . ? C42 C37 C38 N6 -178.5(6) . . . . ? C36 C37 C38 C39 -172.8(8) . . . . ? C42 C37 C38 C39 6.6(12) . . . . ? N6 C38 C39 C40 -2.6(8) . . . . ? C37 C38 C39 C40 172.9(7) . . . . ? C38 C39 C40 C41 1.3(9) . . . . ? C39 C40 C41 N6 0.5(9) . . . . ? C38 C37 C42 C43 111.7(8) . . . . ? C36 C37 C42 C43 -68.9(10) . . . . ? C38 C37 C42 C47 -66.7(10) . . . . ? C36 C37 C42 C47 112.7(8) . . . . ? C47 C42 C43 C44 1.8(12) . . . . ? C37 C42 C43 C44 -176.8(7) . . . . ? C42 C43 C44 C45 -1.1(13) . . . . ? C43 C44 C45 C46 1.2(13) . . . . ? C43 C44 C45 C48 -178.0(8) . . . . ? C44 C45 C46 C47 -2.1(14) . . . . ? C48 C45 C46 C47 177.2(8) . . . . ? C45 C46 C47 C42 2.7(14) . . . . ? C43 C42 C47 C46 -2.6(13) . . . . ? C37 C42 C47 C46 175.9(8) . . . . ? C44 C45 C48 O6 170.4(8) . . . . ? C46 C45 C48 O6 -8.8(13) . . . . ? C44 C45 C48 O5 -7.1(13) . . . . ? C46 C45 C48 O5 173.7(9) . . . . ? C2 C1 N1 C4 -0.9(8) . . . . ? C2 C1 N1 Co1 164.6(5) . . . . ? C5 C4 N1 C1 -173.7(6) . . . . ? C3 C4 N1 C1 2.2(8) . . . . ? C5 C4 N1 Co1 20.4(9) . . . . ? C3 C4 N1 Co1 -163.7(5) . . . . ? N2 Co1 N1 C1 169.9(6) . . . . ? N3 Co1 N1 C1 82.6(6) . . . . ? N6 Co1 N1 C1 -101.1(6) . . . . ? N5 Co1 N1 C1 -9.1(6) . . . . ? N2 Co1 N1 C4 -27.2(6) . . . . ? N3 Co1 N1 C4 -114.6(6) . . . . ? N6 Co1 N1 C4 61.7(5) . . . . ? N5 Co1 N1 C4 153.7(6) . . . . ? C8 C9 N2 C6 0.4(7) . . . . ? C8 C9 N2 Co1 -172.9(4) . . . . ? C5 C6 N2 C9 175.4(6) . . . . ? C7 C6 N2 C9 -1.1(7) . . . . ? C5 C6 N2 Co1 -11.2(9) . . . . ? C7 C6 N2 Co1 172.3(4) . . . . ? N3 Co1 N2 C9 -74.0(5) . . . . ? N4 Co1 N2 C9 18.2(6) . . . . ? N6 Co1 N2 C9 108.6(5) . . . . ? N1 Co1 N2 C9 -165.1(5) . . . . ? N3 Co1 N2 C6 113.9(5) . . . . ? N4 Co1 N2 C6 -153.9(5) . . . . ? N6 Co1 N2 C6 -63.5(5) . . . . ? N1 Co1 N2 C6 22.8(5) . . . . ? C18 C17 N3 C20 2.3(7) . . . . ? C18 C17 N3 Co1 -179.6(4) . . . . ? C19 C20 N3 C17 -3.5(7) . . . . ? C21 C20 N3 C17 175.1(6) . . . . ? C19 C20 N3 Co1 178.4(4) . . . . ? C21 C20 N3 Co1 -3.0(9) . . . . ? N2 Co1 N3 C17 -77.3(5) . . . . ? N4 Co1 N3 C17 -169.6(5) . . . . ? N1 Co1 N3 C17 13.4(5) . . . . ? N5 Co1 N3 C17 102.3(5) . . . . ? N2 Co1 N3 C20 100.4(5) . . . . ? N4 Co1 N3 C20 8.1(5) . . . . ? N1 Co1 N3 C20 -168.8(5) . . . . ? N5 Co1 N3 C20 -79.9(5) . . . . ? C24 C25 N4 C22 0.6(7) . . . . ? C24 C25 N4 Co1 178.8(4) . . . . ? C21 C22 N4 C25 -177.5(6) . . . . ? C23 C22 N4 C25 0.6(7) . . . . ? C21 C22 N4 Co1 4.3(9) . . . . ? C23 C22 N4 Co1 -177.6(4) . . . . ? N2 Co1 N4 C25 86.1(5) . . . . ? N3 Co1 N4 C25 173.5(5) . . . . ? N6 Co1 N4 C25 -2.9(5) . . . . ? N5 Co1 N4 C25 -94.8(5) . . . . ? N2 Co1 N4 C22 -96.2(5) . . . . ? N3 Co1 N4 C22 -8.8(5) . . . . ? N6 Co1 N4 C22 174.8(5) . . . . ? N5 Co1 N4 C22 83.0(5) . . . . ? C34 C33 N5 C36 -2.0(7) . . . . ? C34 C33 N5 Co1 -172.4(4) . . . . ? C37 C36 N5 C33 180.0(7) . . . . ? C35 C36 N5 C33 1.4(7) . . . . ? C37 C36 N5 Co1 -9.5(9) . . . . ? C35 C36 N5 Co1 171.9(4) . . . . ? N3 Co1 N5 C33 9.6(6) . . . . ? N4 Co1 N5 C33 -82.6(6) . . . . ? N6 Co1 N5 C33 -173.0(6) . . . . ? N1 Co1 N5 C33 100.8(6) . . . . ? N3 Co1 N5 C36 -159.0(5) . . . . ? N4 Co1 N5 C36 108.8(5) . . . . ? N6 Co1 N5 C36 18.4(5) . . . . ? N1 Co1 N5 C36 -67.9(5) . . . . ? C40 C41 N6 C38 -2.2(8) . . . . ? C40 C41 N6 Co1 170.2(5) . . . . ? C37 C38 N6 C41 -172.9(7) . . . . ? C39 C38 N6 C41 2.9(8) . . . . ? C37 C38 N6 Co1 14.5(10) . . . . ? C39 C38 N6 Co1 -169.6(5) . . . . ? N2 Co1 N6 C41 -12.3(6) . . . . ? N4 Co1 N6 C41 80.1(6) . . . . ? N1 Co1 N6 C41 -103.2(6) . . . . ? N5 Co1 N6 C41 168.1(6) . . . . ? N2 Co1 N6 C38 158.8(5) . . . . ? N4 Co1 N6 C38 -108.8(5) . . . . ? N1 Co1 N6 C38 67.9(5) . . . . ? N5 Co1 N6 C38 -20.8(6) . . . . ? O2 C16 O1 Zn4 -29(3) . . . 3_746 ? C13 C16 O1 Zn4 148.2(15) . . . 3_746 ? O2 C16 O1 Zn2 -31.8(19) . . . 4_656 ? C13 C16 O1 Zn2 145.8(9) . . . 4_656 ? O1 C16 O2 Zn1 -14(2) . . . 4_656 ? C13 C16 O2 Zn1 168.6(8) . . . 4_656 ? O1 C16 O2 Zn3 7.6(17) . . . 3_746 ? C13 C16 O2 Zn3 -170.0(6) . . . 3_746 ? O4 C32 O3 Zn4 1.3(15) . . . 2_655 ? C29 C32 O3 Zn4 -178.1(6) . . . 2_655 ? O4 C32 O3 Zn2 -13.0(14) . . . . ? C29 C32 O3 Zn2 167.5(5) . . . . ? O9 Zn2 O3 C32 -39.7(9) 1_565 . . . ? O5 Zn2 O3 C32 -139.5(7) 3_666 . . . ? O1 Zn2 O3 C32 85.4(8) 4 . . . ? O7 Zn2 O3 C32 1.9(8) . . . . ? O12 Zn2 O3 C32 -166(5) . . . . ? O9 Zn2 O3 Zn4 175.4(9) 1_565 . . 2_655 ? O5 Zn2 O3 Zn4 75.6(6) 3_666 . . 2_655 ? O1 Zn2 O3 Zn4 -59.5(6) 4 . . 2_655 ? O7 Zn2 O3 Zn4 -143.0(7) . . . 2_655 ? O12 Zn2 O3 Zn4 49(5) . . . 2_655 ? O3 C32 O4 Zn3 -4.2(16) . . . 2_655 ? C29 C32 O4 Zn3 175.2(6) . . . 2_655 ? O3 C32 O4 Zn1 -35(2) . . . . ? C29 C32 O4 Zn1 144.0(9) . . . . ? O8 Zn1 O4 C32 -121.9(13) . . . . ? O7 Zn1 O4 C32 67.4(14) . . . . ? O2 Zn1 O4 C32 7.2(14) 4 . . . ? O6 Zn1 O4 C32 112.4(13) 4_665 . . . ? O8 Zn1 O4 Zn3 170.9(4) . . . 2_655 ? O7 Zn1 O4 Zn3 0.1(6) . . . 2_655 ? O2 Zn1 O4 Zn3 -60.1(4) 4 . . 2_655 ? O6 Zn1 O4 Zn3 45.2(4) 4_665 . . 2_655 ? O6 C48 O5 Zn4 -56.6(15) . . . 4_566 ? C45 C48 O5 Zn4 120.6(9) . . . 4_566 ? O6 C48 O5 Zn2 -39.8(14) . . . 3_666 ? C45 C48 O5 Zn2 137.5(7) . . . 3_666 ? O5 C48 O6 Zn3 -9.3(17) . . . 3_656 ? C45 C48 O6 Zn3 173.4(7) . . . 3_656 ? O5 C48 O6 Zn1 10.2(13) . . . 4_566 ? C45 C48 O6 Zn1 -167.1(6) . . . 4_566 ? O8 Zn1 O7 Zn3 -44(8) . . . 2_655 ? O2 Zn1 O7 Zn3 125(7) 4 . . 2_655 ? O6 Zn1 O7 Zn3 -131(7) 4_665 . . 2_655 ? O4 Zn1 O7 Zn3 -1(6) . . . 2_655 ? O8 Zn1 O7 Zn2 -113(3) . . . . ? O2 Zn1 O7 Zn2 56.6(11) 4 . . . ? O6 Zn1 O7 Zn2 160.6(14) 4_665 . . . ? O4 Zn1 O7 Zn2 -69.6(11) . . . . ? O9 Zn2 O7 Zn3 180.0(10) 1_565 . . 2_655 ? O3 Zn2 O7 Zn3 56.0(18) . . . 2_655 ? O5 Zn2 O7 Zn3 143.0(14) 3_666 . . 2_655 ? O1 Zn2 O7 Zn3 -44.7(17) 4 . . 2_655 ? O12 Zn2 O7 Zn3 -129(2) . . . 2_655 ? O9 Zn2 O7 Zn1 -175.0(17) 1_565 . . . ? O3 Zn2 O7 Zn1 61.0(12) . . . . ? O5 Zn2 O7 Zn1 148.1(9) 3_666 . . . ? O1 Zn2 O7 Zn1 -39.6(12) 4 . . . ? O12 Zn2 O7 Zn1 -123.8(19) . . . . ? O7 Zn1 O8 Zn2 -79(3) . . . 2_645 ? O2 Zn1 O8 Zn2 112.6(5) 4 . . 2_645 ? O6 Zn1 O8 Zn2 1.1(6) 4_665 . . 2_645 ? O4 Zn1 O8 Zn2 -118.6(5) . . . 2_645 ? O7 Zn1 O8 Zn4 -77(3) . . . . ? O2 Zn1 O8 Zn4 114.3(5) 4 . . . ? O6 Zn1 O8 Zn4 2.8(6) 4_665 . . . ? O4 Zn1 O8 Zn4 -116.9(4) . . . . ? O7 Zn1 O8 Zn3 160(3) . . . . ? O2 Zn1 O8 Zn3 -8.5(7) 4 . . . ? O6 Zn1 O8 Zn3 -120.0(5) 4_665 . . . ? O4 Zn1 O8 Zn3 120.3(5) . . . . ? O1 Zn4 O8 Zn2 -164(3) 3_746 . . 2_645 ? O5 Zn4 O8 Zn2 36(3) 4_665 . . 2_645 ? O3 Zn4 O8 Zn2 -56(3) 2_645 . . 2_645 ? O13 Zn4 O8 Zn2 119(3) . . . 2_645 ? O1 Zn4 O8 Zn1 176.8(6) 3_746 . . . ? O5 Zn4 O8 Zn1 16.7(5) 4_665 . . . ? O3 Zn4 O8 Zn1 -74.5(5) 2_645 . . . ? O13 Zn4 O8 Zn1 100(2) . . . . ? O1 Zn4 O8 Zn3 -50.1(5) 3_746 . . . ? O5 Zn4 O8 Zn3 149.8(4) 4_665 . . . ? O3 Zn4 O8 Zn3 58.6(4) 2_645 . . . ? O13 Zn4 O8 Zn3 -127(2) . . . . ? O4 Zn3 O8 Zn2 -59.4(5) 2_645 . . 2_645 ? O6 Zn3 O8 Zn2 169.5(5) 3_656 . . 2_645 ? O2 Zn3 O8 Zn2 68.6(5) 3_746 . . 2_645 ? O4 Zn3 O8 Zn1 62.3(6) 2_645 . . . ? O6 Zn3 O8 Zn1 -68.9(5) 3_656 . . . ? O2 Zn3 O8 Zn1 -169.7(5) 3_746 . . . ? O4 Zn3 O8 Zn4 -64.1(4) 2_645 . . . ? O6 Zn3 O8 Zn4 164.7(4) 3_656 . . . ? O2 Zn3 O8 Zn4 63.9(4) 3_746 . . . ? O4 Zn3 O9 Zn1 165.7(17) 2_645 . . 2_645 ? O6 Zn3 O9 Zn1 -63.7(17) 3_656 . . 2_645 ? O2 Zn3 O9 Zn1 37.1(16) 3_746 . . 2_645 ? O4 Zn3 O9 Zn2 -131.0(9) 2_645 . . 1_545 ? O6 Zn3 O9 Zn2 -0.4(9) 3_656 . . 1_545 ? O2 Zn3 O9 Zn2 100.4(9) 3_746 . . 1_545 ? O14 C49 N7 C52 -8.5(18) . . . . ? O14 C49 N7 C50 178.8(12) . . . . ? C53 C52 N7 C49 87.3(15) . . . . ? C53 C52 N7 C50 -99.8(14) . . . . ? C51 C50 N7 C49 -111.2(15) . . . . ? C51 C50 N7 C52 75.8(15) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.369 _refine_diff_density_min -0.634 _refine_diff_density_rms 0.146 #===END data_sqz _database_code_depnum_ccdc_archive 'CCDC 656117' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common MOF-Co/Zn-5b _chemical_melting_point ? _chemical_formula_moiety 'C53 H41 Co N7 O7 Zn1.5,2.5(C5 H11 N O)' _chemical_formula_sum 'C65.50 H68.50 Co N9.50 O9.50 Zn1.50' _chemical_formula_weight 1297.78 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' 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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.626(3) _cell_length_b 14.766(3) _cell_length_c 17.357(4) _cell_angle_alpha 81.062(4) _cell_angle_beta 81.660(4) _cell_angle_gamma 75.534(4) _cell_volume 3319.8(12) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 5482 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 28.0 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.298 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1352 _exptl_absorpt_coefficient_mu 0.849 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8989 _exptl_absorpt_correction_T_max 0.9679 _exptl_absorpt_process_details 'SADABS 2.10 (Sheldrick, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX' _diffrn_measurement_method \w\f _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36922 _diffrn_reflns_av_R_equivalents 0.0800 _diffrn_reflns_av_sigmaI/netI 0.0903 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.19 _diffrn_reflns_theta_max 26.37 _reflns_number_total 13380 _reflns_number_gt 8288 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART 5.054 (Bruker, 2003)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT 6.45A (Bruker, 2003)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5.1 (Sheldrick, 1994)' _computing_publication_material SHELXL97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. All H atoms were located in a difference map, placed in optimized positions, and treated with a riding model The model included four DEF solvent molecules. One was disordered over a special position. That molecule was assigned an occupancy of 50 percent. Its aldehyde H atom could not be located and was omitted from the refinement. Another DEF molecule was coordinated to a zinc atom. That DEF molecule was also disordered over two general positions with assumed occupancies of 50 percent. The remaining two DEF molecules were severely disordered and satisfactory atomic positions could not be determined. These severely disordered solvent molecules were treated as a diffuse contribution using the program SQUEEZE (A. Spek, Platon Library). SQUEEZE found 998.7 ang.^3^ void space per cell and 224.1 electrons. Four molecules of DEF requires 184 electrons, giving an additional two DEF molecules per formula unit. These two DEF molecules were included in the moiety and sum formulas and in the associated calculated values. The DEF molecule including atoms c49 through O8 is disordered over two positions resulting in some irregularities in the refinement. Independent positions were located for all of the disordered DEF atoms except for the aldehyde groups. The associated DEF atoms have generally larger thermal parameters than the rest of the main residue. The asymmetric unit includes one full cobalt dipyrrinato complex, two disordered DEF molecules and one and one-half zn atoms for a z of 2. ; _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^)+(0.0897P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13380 _refine_ls_number_parameters 736 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0905 _refine_ls_R_factor_gt 0.0605 _refine_ls_wR_factor_ref 0.1642 _refine_ls_wR_factor_gt 0.1507 _refine_ls_goodness_of_fit_ref 0.906 _refine_ls_restrained_S_all 0.906 _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 1.0000 0.5000 0.0000 0.03428(16) Uani 1 2 d S . . Zn2 Zn 0.81871(3) 0.42746(3) -0.08334(2) 0.04156(14) Uani 1 1 d . . . Co1 Co 0.61816(4) 0.16703(3) 0.57819(3) 0.03735(15) Uani 1 1 d . . . C1 C 0.8139(3) 0.2150(4) 0.5699(3) 0.0699(15) Uani 1 1 d . . . H1 H 0.8165 0.1975 0.6241 0.084 Uiso 1 1 calc R . . C2 C 0.8941(3) 0.2433(4) 0.5176(3) 0.0773(16) Uani 1 1 d . . . H2 H 0.9564 0.2498 0.5307 0.093 Uiso 1 1 calc R . . C3 C 0.8630(3) 0.2589(3) 0.4453(2) 0.0569(12) Uani 1 1 d . . . H3 H 0.9008 0.2759 0.3979 0.068 Uiso 1 1 calc R . . C4 C 0.7633(3) 0.2451(2) 0.4541(2) 0.0413(9) Uani 1 1 d . . . C5 C 0.6999(3) 0.2590(3) 0.3960(2) 0.0426(9) Uani 1 1 d . . . C6 C 0.6006(3) 0.2413(3) 0.4084(2) 0.0419(9) Uani 1 1 d . . . C7 C 0.5238(3) 0.2675(3) 0.3558(2) 0.0491(10) Uani 1 1 d . . . H7 H 0.5298 0.2986 0.3044 0.059 Uiso 1 1 calc R . . C8 C 0.4406(3) 0.2389(3) 0.3943(2) 0.0517(10) Uani 1 1 d . . . H8 H 0.3782 0.2461 0.3743 0.062 Uiso 1 1 calc R . . C9 C 0.4647(3) 0.1967(3) 0.4691(2) 0.0435(9) Uani 1 1 d . . . H9 H 0.4196 0.1717 0.5078 0.052 Uiso 1 1 calc R . . C10 C 0.7343(3) 0.2969(3) 0.3145(2) 0.0436(9) Uani 1 1 d . . . C11 C 0.7315(4) 0.2506(3) 0.2514(2) 0.0646(13) Uani 1 1 d . . . H11 H 0.7091 0.1942 0.2603 0.077 Uiso 1 1 calc R . . C12 C 0.7614(4) 0.2867(3) 0.1749(2) 0.0557(11) Uani 1 1 d . . . H12 H 0.7581 0.2555 0.1325 0.067 Uiso 1 1 calc R . . C13 C 0.7961(3) 0.3692(3) 0.1621(2) 0.0402(9) Uani 1 1 d . . . C14 C 0.8000(3) 0.4154(3) 0.2248(2) 0.0413(9) Uani 1 1 d . . . H14 H 0.8235 0.4712 0.2160 0.050 Uiso 1 1 calc R . . C15 C 0.7692(3) 0.3792(3) 0.3001(2) 0.0418(9) Uani 1 1 d . . . H15 H 0.7719 0.4110 0.3424 0.050 Uiso 1 1 calc R . . C16 C 0.8239(3) 0.4103(3) 0.0784(2) 0.0399(9) Uani 1 1 d . . . C17 C 0.7156(3) 0.0130(3) 0.4856(2) 0.0572(12) Uani 1 1 d . . . H17 H 0.6973 0.0498 0.4383 0.069 Uiso 1 1 calc R . . C18 C 0.7649(4) -0.0835(3) 0.4924(3) 0.0692(15) Uani 1 1 d . . . H18 H 0.7859 -0.1210 0.4512 0.083 Uiso 1 1 calc R . . C19 C 0.7763(3) -0.1120(3) 0.5690(3) 0.0609(13) Uani 1 1 d . . . H19 H 0.8055 -0.1733 0.5913 0.073 Uiso 1 1 calc R . . C20 C 0.7361(3) -0.0320(3) 0.6094(2) 0.0461(10) Uani 1 1 d . . . C21 C 0.7317(3) -0.0252(3) 0.6890(2) 0.0485(10) Uani 1 1 d . . . C22 C 0.6989(3) 0.0564(3) 0.7237(2) 0.0480(10) Uani 1 1 d . . . C23 C 0.7005(4) 0.0687(4) 0.8026(3) 0.0677(14) Uani 1 1 d . . . H23 H 0.7214 0.0207 0.8432 0.081 Uiso 1 1 calc R . . C24 C 0.6664(4) 0.1631(4) 0.8095(3) 0.0707(14) Uani 1 1 d . . . H24 H 0.6603 0.1924 0.8549 0.085 Uiso 1 1 calc R . . C25 C 0.6428(3) 0.2064(3) 0.7348(2) 0.0532(11) Uani 1 1 d . . . H25 H 0.6170 0.2716 0.7224 0.064 Uiso 1 1 calc R . . C26 C 0.7632(3) -0.1168(3) 0.7423(2) 0.0527(11) Uani 1 1 d . . . C27 C 0.6980(3) -0.1769(3) 0.7590(2) 0.0509(10) Uani 1 1 d . . . H27 H 0.6347 -0.1597 0.7387 0.061 Uiso 1 1 calc R . . C28 C 0.7248(3) -0.2627(3) 0.8055(2) 0.0487(10) Uani 1 1 d . . . H28 H 0.6801 -0.3034 0.8161 0.058 Uiso 1 1 calc R . . C29 C 0.8175(3) -0.2884(3) 0.8364(2) 0.0483(10) Uani 1 1 d . . . C30 C 0.8825(4) -0.2285(4) 0.8211(4) 0.0879(19) Uani 1 1 d . . . H30 H 0.9448 -0.2448 0.8428 0.105 Uiso 1 1 calc R . . C31 C 0.8550(4) -0.1424(4) 0.7728(4) 0.097(2) Uani 1 1 d . . . H31 H 0.9001 -0.1020 0.7612 0.116 Uiso 1 1 calc R . . C32 C 0.8467(3) -0.3823(3) 0.8863(2) 0.0495(10) Uani 1 1 d . . . C33 C 0.5025(3) 0.0184(3) 0.6244(2) 0.0443(9) Uani 1 1 d . . . H33 H 0.5514 -0.0254 0.5966 0.053 Uiso 1 1 calc R . . C34 C 0.4159(3) -0.0019(3) 0.6703(2) 0.0546(11) Uani 1 1 d . . . H34 H 0.3970 -0.0600 0.6790 0.065 Uiso 1 1 calc R . . C35 C 0.3640(3) 0.0792(3) 0.7002(2) 0.0501(10) Uani 1 1 d . . . H35 H 0.3026 0.0871 0.7338 0.060 Uiso 1 1 calc R . . C36 C 0.4195(3) 0.1490(3) 0.6717(2) 0.0416(9) Uani 1 1 d . . . C37 C 0.3920(3) 0.2439(3) 0.6796(2) 0.0419(9) Uani 1 1 d . . . C38 C 0.4460(3) 0.3113(3) 0.6460(2) 0.0412(9) Uani 1 1 d . . . C39 C 0.4173(3) 0.4093(3) 0.6484(2) 0.0561(11) Uani 1 1 d . . . H39 H 0.3577 0.4421 0.6758 0.067 Uiso 1 1 calc R . . C40 C 0.4917(4) 0.4486(3) 0.6037(2) 0.0585(12) Uani 1 1 d . . . H40 H 0.4935 0.5127 0.5949 0.070 Uiso 1 1 calc R . . C41 C 0.5642(3) 0.3733(3) 0.5742(2) 0.0493(10) Uani 1 1 d . . . H41 H 0.6236 0.3798 0.5408 0.059 Uiso 1 1 calc R . . C42 C 0.2917(3) 0.2781(3) 0.7274(2) 0.0434(9) Uani 1 1 d . . . C43 C 0.2018(3) 0.2942(4) 0.6960(3) 0.0675(14) Uani 1 1 d . . . H43 H 0.2021 0.2854 0.6435 0.081 Uiso 1 1 calc R . . C44 C 0.1104(3) 0.3235(4) 0.7410(2) 0.0652(14) Uani 1 1 d . . . H44 H 0.0489 0.3324 0.7192 0.078 Uiso 1 1 calc R . . C45 C 0.1076(3) 0.3399(3) 0.8173(2) 0.0452(10) Uani 1 1 d . . . C46 C 0.1966(3) 0.3239(3) 0.8485(2) 0.0520(11) Uani 1 1 d . . . H46 H 0.1958 0.3339 0.9008 0.062 Uiso 1 1 calc R . . C47 C 0.2897(3) 0.2928(3) 0.8040(2) 0.0514(10) Uani 1 1 d . . . H47 H 0.3511 0.2820 0.8264 0.062 Uiso 1 1 calc R . . C48 C 0.0094(3) 0.3710(3) 0.8667(2) 0.0479(10) Uani 1 1 d . . . N1 N 0.7360(2) 0.2162(2) 0.53330(17) 0.0430(8) Uani 1 1 d . . . N2 N 0.5610(2) 0.1966(2) 0.47823(16) 0.0377(7) Uani 1 1 d . . . N3 N 0.6982(2) 0.0450(2) 0.55512(18) 0.0460(8) Uani 1 1 d . . . N4 N 0.6612(2) 0.1445(2) 0.68303(18) 0.0445(8) Uani 1 1 d . . . N5 N 0.5078(2) 0.1081(2) 0.62460(16) 0.0387(7) Uani 1 1 d . . . N6 N 0.5391(2) 0.2912(2) 0.59887(16) 0.0385(7) Uani 1 1 d . . . O1 O 0.86671(19) 0.47703(17) 0.06783(14) 0.0430(6) Uani 1 1 d . . . O2 O 0.7990(2) 0.3732(2) 0.02497(15) 0.0483(7) Uani 1 1 d . . . O3 O 0.9269(2) -0.39907(19) 0.91856(17) 0.0572(8) Uani 1 1 d . . . O4 O 0.7876(2) -0.43675(19) 0.88967(17) 0.0561(8) Uani 1 1 d . . . O5 O 0.0077(2) 0.38981(19) 0.93387(16) 0.0511(7) Uani 1 1 d . . . O6 O -0.0725(2) 0.3775(2) 0.83622(17) 0.0685(9) Uani 1 1 d . . . C49 C 0.6290(4) 0.3729(4) -0.0661(3) 0.0781(16) Uani 0.50 1 d P A 1 H49 H 0.6559 0.3263 -0.0263 0.094 Uiso 0.50 1 calc PR A 1 C50 C 0.485(3) 0.440(3) -0.140(2) 0.25(3) Uani 0.50 1 d P A 1 H50A H 0.5295 0.4074 -0.1820 0.300 Uiso 0.50 1 calc PR A 1 H50B H 0.4155 0.4322 -0.1418 0.300 Uiso 0.50 1 calc PR A 1 C51 C 0.4844(19) 0.5378(14) -0.1545(19) 0.134(13) Uani 0.50 1 d P A 1 H51A H 0.4644 0.5634 -0.2063 0.200 Uiso 0.50 1 calc PR A 1 H51B H 0.5522 0.5457 -0.1513 0.200 Uiso 0.50 1 calc PR A 1 H51C H 0.4365 0.5709 -0.1154 0.200 Uiso 0.50 1 calc PR A 1 C52 C 0.4513(11) 0.3630(10) 0.0003(7) 0.089(4) Uani 0.50 1 d P A 1 H52A H 0.3907 0.4139 0.0094 0.107 Uiso 0.50 1 calc PR A 1 H52B H 0.4858 0.3476 0.0481 0.107 Uiso 0.50 1 calc PR A 1 C53 C 0.4162(15) 0.2748(13) -0.0133(10) 0.103(6) Uani 0.50 1 d P A 1 H53A H 0.3689 0.2584 0.0309 0.154 Uiso 0.50 1 calc PR A 1 H53B H 0.4751 0.2224 -0.0185 0.154 Uiso 0.50 1 calc PR A 1 H53C H 0.3829 0.2887 -0.0609 0.154 Uiso 0.50 1 calc PR A 1 N7 N 0.5196(7) 0.3973(9) -0.0640(7) 0.066(3) Uani 0.50 1 d P A 1 O7 O 0.6915(2) 0.4054(2) -0.11348(17) 0.0633(8) Uani 0.50 1 d P A 1 C54 C 0.6290(4) 0.3729(4) -0.0661(3) 0.0781(16) Uani 0.50 1 d P A 2 H54 H 0.6376 0.3551 -0.0126 0.094 Uiso 0.50 1 calc PR A 2 C55 C 0.5139(17) 0.4217(13) -0.1669(13) 0.079(5) Uani 0.50 1 d P A 2 H55A H 0.5695 0.4107 -0.2095 0.095 Uiso 0.50 1 calc PR A 2 H55B H 0.4591 0.3962 -0.1795 0.095 Uiso 0.50 1 calc PR A 2 C56 C 0.4783(19) 0.516(2) -0.1690(17) 0.128(12) Uani 0.50 1 d P A 2 H56A H 0.4611 0.5430 -0.2213 0.192 Uiso 0.50 1 calc PR A 2 H56B H 0.5303 0.5435 -0.1556 0.192 Uiso 0.50 1 calc PR A 2 H56C H 0.4179 0.5294 -0.1316 0.192 Uiso 0.50 1 calc PR A 2 C57 C 0.4868(9) 0.3031(10) -0.0498(8) 0.091(4) Uani 0.50 1 d P A 2 H57A H 0.4786 0.2586 -0.0834 0.110 Uiso 0.50 1 calc PR A 2 H57B H 0.5225 0.2664 -0.0058 0.110 Uiso 0.50 1 calc PR A 2 C58 C 0.3893(13) 0.3524(17) -0.0202(10) 0.120(7) Uani 0.50 1 d P A 2 H58A H 0.3513 0.3078 0.0083 0.180 Uiso 0.50 1 calc PR A 2 H58B H 0.3531 0.3884 -0.0634 0.180 Uiso 0.50 1 calc PR A 2 H58C H 0.3966 0.3948 0.0149 0.180 Uiso 0.50 1 calc PR A 2 N8 N 0.5512(8) 0.3654(8) -0.0957(6) 0.064(3) Uani 0.50 1 d P A 2 O8 O 0.6915(2) 0.4054(2) -0.11348(17) 0.0633(8) Uani 0.50 1 d P A 2 C59 C 0.8807(10) 0.0449(10) 0.2950(8) 0.096(4) Uani 0.50 1 d P B -1 C60 C 1.0026(8) 0.0107(7) 0.3746(6) 0.069(3) Uani 0.50 1 d P B -1 H60A H 0.9972 0.0786 0.3612 0.083 Uiso 0.50 1 calc PR B -1 H60B H 1.0741 -0.0208 0.3612 0.083 Uiso 0.50 1 calc PR B -1 C61 C 0.9784(10) -0.0084(9) 0.4617(7) 0.093(4) Uani 0.50 1 d P B -1 H61A H 1.0249 0.0135 0.4877 0.139 Uiso 0.50 1 calc PR B -1 H61B H 0.9858 -0.0756 0.4768 0.139 Uiso 0.50 1 calc PR B -1 H61C H 0.9089 0.0245 0.4769 0.139 Uiso 0.50 1 calc PR B -1 C62 C 0.9630(7) -0.1108(7) 0.3108(6) 0.066(3) Uani 0.50 1 d P B -1 H62A H 0.8987 -0.1237 0.3019 0.079 Uiso 0.50 1 calc PR B -1 H62B H 0.9863 -0.1521 0.3577 0.079 Uiso 0.50 1 calc PR B -1 C63 C 1.0418(9) -0.1361(10) 0.2408(8) 0.099(4) Uani 0.50 1 d P B -1 H63A H 1.0500 -0.2019 0.2347 0.148 Uiso 0.50 1 calc PR B -1 H63B H 1.1066 -0.1256 0.2496 0.148 Uiso 0.50 1 calc PR B -1 H63C H 1.0189 -0.0968 0.1936 0.148 Uiso 0.50 1 calc PR B -1 N9 N 0.9441(6) -0.0162(5) 0.3256(4) 0.057(2) Uani 0.50 1 d P B -1 O9 O 0.8184(7) 0.0344(5) 0.2400(8) 0.137(4) Uani 0.50 1 d P B -1 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 0.0322(3) 0.0342(3) 0.0285(3) 0.0062(2) 0.0054(2) -0.0042(2) Zn2 0.0348(3) 0.0467(3) 0.0338(2) 0.00508(19) 0.00577(18) -0.00372(19) Co1 0.0367(3) 0.0342(3) 0.0298(3) 0.0057(2) 0.0081(2) 0.0002(2) C1 0.045(3) 0.103(4) 0.045(2) 0.029(3) -0.007(2) -0.010(3) C2 0.039(3) 0.118(4) 0.065(3) 0.027(3) -0.001(2) -0.026(3) C3 0.042(2) 0.065(3) 0.050(2) 0.015(2) 0.0130(19) -0.010(2) C4 0.044(2) 0.034(2) 0.0351(19) 0.0049(16) 0.0092(17) -0.0037(17) C5 0.051(2) 0.035(2) 0.0343(19) 0.0015(16) 0.0095(17) -0.0075(17) C6 0.052(2) 0.038(2) 0.0287(18) 0.0001(15) 0.0099(17) -0.0089(18) C7 0.067(3) 0.050(2) 0.0300(19) 0.0067(17) -0.0072(19) -0.019(2) C8 0.051(3) 0.055(3) 0.046(2) 0.0038(19) -0.0017(19) -0.013(2) C9 0.043(2) 0.043(2) 0.039(2) 0.0029(17) 0.0029(17) -0.0089(18) C10 0.055(2) 0.038(2) 0.035(2) 0.0012(16) 0.0072(17) -0.0141(18) C11 0.108(4) 0.047(3) 0.041(2) -0.0003(19) 0.016(2) -0.039(3) C12 0.082(3) 0.052(2) 0.037(2) -0.0045(18) 0.011(2) -0.033(2) C13 0.040(2) 0.042(2) 0.0326(19) 0.0086(16) 0.0041(16) -0.0099(17) C14 0.046(2) 0.035(2) 0.039(2) 0.0041(16) 0.0038(17) -0.0128(17) C15 0.045(2) 0.039(2) 0.0364(19) -0.0039(16) 0.0075(17) -0.0077(17) C16 0.033(2) 0.043(2) 0.0338(19) 0.0034(17) 0.0055(16) -0.0018(17) C17 0.068(3) 0.041(2) 0.044(2) 0.0047(18) 0.021(2) 0.001(2) C18 0.078(3) 0.042(2) 0.065(3) -0.001(2) 0.037(3) 0.000(2) C19 0.052(3) 0.037(2) 0.072(3) 0.009(2) 0.018(2) 0.0069(19) C20 0.034(2) 0.038(2) 0.053(2) 0.0132(18) 0.0002(18) 0.0033(17) C21 0.038(2) 0.044(2) 0.053(2) 0.0212(19) -0.0019(18) -0.0067(18) C22 0.047(2) 0.048(2) 0.040(2) 0.0190(19) -0.0077(18) -0.0081(19) C23 0.080(3) 0.074(3) 0.045(2) 0.025(2) -0.020(2) -0.024(3) C24 0.093(4) 0.076(4) 0.042(2) 0.004(2) -0.011(2) -0.021(3) C25 0.056(3) 0.053(3) 0.043(2) 0.001(2) 0.000(2) -0.006(2) C26 0.042(2) 0.051(2) 0.054(2) 0.018(2) -0.0051(19) -0.0039(19) C27 0.053(3) 0.051(2) 0.043(2) 0.0130(19) -0.0097(19) -0.009(2) C28 0.048(2) 0.046(2) 0.044(2) 0.0159(18) -0.0046(19) -0.0106(19) C29 0.042(2) 0.045(2) 0.048(2) 0.0139(18) -0.0007(18) -0.0040(18) C30 0.057(3) 0.072(3) 0.123(5) 0.053(3) -0.033(3) -0.020(3) C31 0.069(4) 0.072(4) 0.138(5) 0.061(4) -0.036(4) -0.026(3) C32 0.046(3) 0.047(2) 0.043(2) 0.0122(18) 0.0041(19) -0.003(2) C33 0.050(2) 0.033(2) 0.042(2) -0.0007(16) 0.0082(18) -0.0062(17) C34 0.067(3) 0.047(2) 0.047(2) 0.0037(19) 0.008(2) -0.022(2) C35 0.051(2) 0.054(3) 0.040(2) 0.0027(19) 0.0104(19) -0.016(2) C36 0.041(2) 0.043(2) 0.0310(18) 0.0024(16) 0.0054(16) -0.0014(17) C37 0.040(2) 0.046(2) 0.0326(19) -0.0043(16) 0.0035(16) -0.0001(17) C38 0.041(2) 0.040(2) 0.0350(19) -0.0025(16) 0.0050(16) -0.0015(17) C39 0.060(3) 0.042(2) 0.051(2) -0.0012(19) 0.007(2) 0.009(2) C40 0.075(3) 0.035(2) 0.055(3) 0.0014(19) 0.012(2) -0.008(2) C41 0.057(3) 0.041(2) 0.042(2) 0.0016(18) 0.0104(19) -0.0102(19) C42 0.038(2) 0.048(2) 0.039(2) -0.0078(17) 0.0083(17) -0.0060(18) C43 0.047(3) 0.106(4) 0.038(2) -0.022(2) 0.001(2) 0.010(3) C44 0.036(2) 0.107(4) 0.044(2) -0.021(2) 0.0007(19) 0.004(2) C45 0.037(2) 0.051(2) 0.039(2) -0.0039(18) 0.0078(17) -0.0013(18) C46 0.054(3) 0.063(3) 0.037(2) -0.0156(19) 0.0134(19) -0.014(2) C47 0.041(2) 0.064(3) 0.045(2) -0.013(2) -0.0007(18) -0.002(2) C48 0.040(2) 0.045(2) 0.050(2) -0.0035(19) 0.0147(19) -0.0060(18) N1 0.0371(18) 0.0456(18) 0.0341(16) 0.0097(14) 0.0042(14) -0.0006(14) N2 0.0406(18) 0.0328(16) 0.0304(15) 0.0029(12) 0.0078(13) -0.0021(13) N3 0.0467(19) 0.0380(17) 0.0380(17) 0.0050(14) 0.0139(15) 0.0019(14) N4 0.0414(19) 0.0431(18) 0.0382(17) 0.0091(15) 0.0049(14) -0.0038(15) N5 0.0375(17) 0.0351(16) 0.0314(15) 0.0048(13) 0.0123(13) -0.0006(13) N6 0.0381(17) 0.0343(16) 0.0348(16) 0.0011(13) 0.0048(13) -0.0015(13) O1 0.0442(15) 0.0398(14) 0.0380(14) 0.0037(11) 0.0140(12) -0.0125(12) O2 0.0485(17) 0.0617(18) 0.0328(14) 0.0049(13) 0.0058(12) -0.0215(14) O3 0.0492(18) 0.0512(17) 0.0603(18) 0.0247(14) -0.0111(15) -0.0082(14) O4 0.0519(18) 0.0439(16) 0.0618(18) 0.0169(14) -0.0053(14) -0.0060(14) O5 0.0576(18) 0.0494(16) 0.0421(16) -0.0118(13) 0.0195(13) -0.0153(14) O6 0.0426(18) 0.093(3) 0.0546(19) -0.0114(17) 0.0162(15) 0.0011(16) C49 0.084(4) 0.078(4) 0.084(4) 0.021(3) -0.033(3) -0.046(3) C50 0.22(4) 0.29(5) 0.25(4) 0.20(4) -0.12(3) -0.17(4) C51 0.105(15) 0.052(8) 0.24(3) 0.057(14) -0.093(16) -0.019(8) C52 0.072(8) 0.121(10) 0.088(9) -0.053(8) 0.048(7) -0.056(8) C53 0.095(12) 0.159(15) 0.075(8) -0.004(11) -0.003(8) -0.079(13) N7 0.032(5) 0.090(8) 0.068(7) -0.013(5) 0.008(4) -0.008(5) O7 0.058(2) 0.078(2) 0.0523(18) 0.0019(16) -0.0070(15) -0.0187(17) C54 0.084(4) 0.078(4) 0.084(4) 0.021(3) -0.033(3) -0.046(3) C55 0.100(10) 0.059(8) 0.105(11) 0.005(8) -0.062(9) -0.047(7) C56 0.066(11) 0.23(4) 0.112(14) -0.043(17) -0.011(10) -0.063(16) C57 0.076(8) 0.101(10) 0.091(9) 0.010(8) -0.005(7) -0.025(7) C58 0.067(11) 0.23(2) 0.093(11) -0.059(15) 0.033(8) -0.085(15) N8 0.045(6) 0.080(8) 0.073(7) 0.008(5) -0.012(5) -0.034(5) O8 0.058(2) 0.078(2) 0.0523(18) 0.0019(16) -0.0070(15) -0.0187(17) C59 0.067(8) 0.120(11) 0.110(10) -0.027(9) 0.010(7) -0.041(8) C60 0.068(7) 0.060(6) 0.077(7) -0.004(5) 0.003(6) -0.018(5) C61 0.086(9) 0.079(8) 0.116(11) -0.031(7) 0.012(7) -0.028(7) C62 0.049(6) 0.070(7) 0.079(7) -0.011(5) -0.017(5) -0.008(5) C63 0.075(8) 0.113(10) 0.109(10) -0.029(8) -0.002(7) -0.019(7) N9 0.046(4) 0.054(5) 0.058(4) 0.013(4) -0.005(4) 0.001(4) O9 0.078(6) 0.052(5) 0.264(13) 0.029(6) -0.012(7) -0.019(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O3 2.055(3) 1_564 ? Zn1 O3 2.055(3) 2_756 ? Zn1 O1 2.089(2) 2_765 ? Zn1 O1 2.089(2) . ? Zn1 O5 2.106(3) 1_654 ? Zn1 O5 2.106(3) 2_666 ? Zn2 O2 1.934(2) . ? Zn2 O4 1.939(3) 1_564 ? Zn2 O6 1.966(3) 1_654 ? Zn2 O7 1.996(3) . ? Zn2 C48 2.586(4) 1_654 ? Co1 N3 1.927(3) . ? Co1 N5 1.937(3) . ? Co1 N6 1.938(3) . ? Co1 N1 1.939(3) . ? Co1 N4 1.947(3) . ? Co1 N2 1.948(3) . ? C1 N1 1.309(5) . ? C1 C2 1.419(6) . ? C1 H1 0.9400 . ? C2 C3 1.351(6) . ? C2 H2 0.9400 . ? C3 C4 1.406(5) . ? C3 H3 0.9400 . ? C4 C5 1.382(5) . ? C4 N1 1.399(4) . ? C5 C6 1.420(5) . ? C5 C10 1.492(5) . ? C6 N2 1.392(4) . ? C6 C7 1.429(5) . ? C7 C8 1.357(5) . ? C7 H7 0.9400 . ? C8 C9 1.397(5) . ? C8 H8 0.9400 . ? C9 N2 1.344(5) . ? C9 H9 0.9400 . ? C10 C11 1.388(6) . ? C10 C15 1.388(5) . ? C11 C12 1.394(5) . ? C11 H11 0.9400 . ? C12 C13 1.389(5) . ? C12 H12 0.9400 . ? C13 C14 1.385(5) . ? C13 C16 1.517(5) . ? C14 C15 1.381(5) . ? C14 H14 0.9400 . ? C15 H15 0.9400 . ? C16 O1 1.243(4) . ? C16 O2 1.272(5) . ? C17 N3 1.332(5) . ? C17 C18 1.410(6) . ? C17 H17 0.9400 . ? C18 C19 1.350(6) . ? C18 H18 0.9400 . ? C19 C20 1.417(6) . ? C19 H19 0.9400 . ? C20 C21 1.393(6) . ? C20 N3 1.401(5) . ? C21 C22 1.376(6) . ? C21 C26 1.517(5) . ? C22 N4 1.393(5) . ? C22 C23 1.412(6) . ? C23 C24 1.373(7) . ? C23 H23 0.9400 . ? C24 C25 1.399(6) . ? C24 H24 0.9400 . ? C25 N4 1.334(5) . ? C25 H25 0.9400 . ? C26 C31 1.372(6) . ? C26 C27 1.379(6) . ? C27 C28 1.387(5) . ? C27 H27 0.9400 . ? C28 C29 1.386(5) . ? C28 H28 0.9400 . ? C29 C30 1.373(6) . ? C29 C32 1.511(5) . ? C30 C31 1.407(6) . ? C30 H30 0.9400 . ? C31 H31 0.9400 . ? C32 O3 1.252(5) . ? C32 O4 1.263(5) . ? C33 N5 1.345(5) . ? C33 C34 1.396(5) . ? C33 H33 0.9400 . ? C34 C35 1.367(6) . ? C34 H34 0.9400 . ? C35 C36 1.415(5) . ? C35 H35 0.9400 . ? C36 C37 1.381(5) . ? C36 N5 1.409(4) . ? C37 C38 1.390(5) . ? C37 C42 1.505(5) . ? C38 N6 1.397(4) . ? C38 C39 1.407(5) . ? C39 C40 1.377(6) . ? C39 H39 0.9400 . ? C40 C41 1.399(6) . ? C40 H40 0.9400 . ? C41 N6 1.331(5) . ? C41 H41 0.9400 . ? C42 C43 1.365(6) . ? C42 C47 1.376(5) . ? C43 C44 1.379(6) . ? C43 H43 0.9400 . ? C44 C45 1.376(6) . ? C44 H44 0.9400 . ? C45 C46 1.351(6) . ? C45 C48 1.490(5) . ? C46 C47 1.397(5) . ? C46 H46 0.9400 . ? C47 H47 0.9400 . ? C48 O5 1.236(5) . ? C48 O6 1.279(5) . ? C48 Zn2 2.586(4) 1_456 ? O3 Zn1 2.055(3) 1_546 ? O4 Zn2 1.939(3) 1_546 ? O5 Zn1 2.106(3) 1_456 ? O6 Zn2 1.966(3) 1_456 ? C49 O7 1.230(6) . ? C49 N7 1.440(11) . ? C49 H49 0.9400 . ? C50 C51 1.43(5) . ? C50 N7 1.47(3) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C51 H51C 0.9700 . ? C52 N7 1.459(14) . ? C52 C53 1.554(19) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C53 H53C 0.9700 . ? C55 C56 1.35(4) . ? C55 N8 1.46(2) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C56 H56C 0.9700 . ? C57 C58 1.41(2) . ? C57 N8 1.491(15) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? C58 H58C 0.9700 . ? C59 N9 1.199(15) . ? C59 O9 1.415(16) . ? C60 N9 1.406(12) . ? C60 C61 1.498(15) . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C61 H61C 0.9700 . ? C62 N9 1.412(12) . ? C62 C63 1.527(14) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C63 H63A 0.9700 . ? C63 H63B 0.9700 . ? C63 H63C 0.9700 . ? 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 O3 Zn1 O3 179.998(1) 1_564 2_756 ? O3 Zn1 O1 84.61(10) 1_564 2_765 ? O3 Zn1 O1 95.39(10) 2_756 2_765 ? O3 Zn1 O1 95.39(10) 1_564 . ? O3 Zn1 O1 84.61(10) 2_756 . ? O1 Zn1 O1 180.0 2_765 . ? O3 Zn1 O5 93.01(12) 1_564 1_654 ? O3 Zn1 O5 86.99(12) 2_756 1_654 ? O1 Zn1 O5 87.69(10) 2_765 1_654 ? O1 Zn1 O5 92.32(10) . 1_654 ? O3 Zn1 O5 86.99(12) 1_564 2_666 ? O3 Zn1 O5 93.01(12) 2_756 2_666 ? O1 Zn1 O5 92.31(10) 2_765 2_666 ? O1 Zn1 O5 87.69(10) . 2_666 ? O5 Zn1 O5 179.999(1) 1_654 2_666 ? O2 Zn2 O4 120.01(13) . 1_564 ? O2 Zn2 O6 126.52(13) . 1_654 ? O4 Zn2 O6 105.66(13) 1_564 1_654 ? O2 Zn2 O7 95.49(12) . . ? O4 Zn2 O7 97.37(13) 1_564 . ? O6 Zn2 O7 105.24(14) 1_654 . ? O2 Zn2 C48 107.67(13) . 1_654 ? O4 Zn2 C48 105.15(12) 1_564 1_654 ? O6 Zn2 C48 28.73(13) 1_654 1_654 ? O7 Zn2 C48 132.65(14) . 1_654 ? N3 Co1 N5 88.65(13) . . ? N3 Co1 N6 178.55(12) . . ? N5 Co1 N6 92.49(12) . . ? N3 Co1 N1 87.15(13) . . ? N5 Co1 N1 175.42(12) . . ? N6 Co1 N1 91.74(13) . . ? N3 Co1 N4 91.22(14) . . ? N5 Co1 N4 86.15(13) . . ? N6 Co1 N4 89.76(13) . . ? N1 Co1 N4 92.12(13) . . ? N3 Co1 N2 93.72(13) . . ? N5 Co1 N2 90.35(13) . . ? N6 Co1 N2 85.38(12) . . ? N1 Co1 N2 91.73(13) . . ? N4 Co1 N2 173.89(13) . . ? N1 C1 C2 111.7(4) . . ? N1 C1 H1 124.1 . . ? C2 C1 H1 124.1 . . ? C3 C2 C1 106.1(4) . . ? C3 C2 H2 126.9 . . ? C1 C2 H2 126.9 . . ? C2 C3 C4 107.2(4) . . ? C2 C3 H3 126.4 . . ? C4 C3 H3 126.4 . . ? C5 C4 N1 124.2(3) . . ? C5 C4 C3 127.0(3) . . ? N1 C4 C3 108.8(3) . . ? C4 C5 C6 124.2(3) . . ? C4 C5 C10 119.5(4) . . ? C6 C5 C10 116.2(4) . . ? N2 C6 C5 123.7(3) . . ? N2 C6 C7 108.2(3) . . ? C5 C6 C7 128.1(3) . . ? C8 C7 C6 107.0(3) . . ? C8 C7 H7 126.5 . . ? C6 C7 H7 126.5 . . ? C7 C8 C9 107.4(4) . . ? C7 C8 H8 126.3 . . ? C9 C8 H8 126.3 . . ? N2 C9 C8 111.0(3) . . ? N2 C9 H9 124.5 . . ? C8 C9 H9 124.5 . . ? C11 C10 C15 118.6(3) . . ? C11 C10 C5 120.6(3) . . ? C15 C10 C5 120.8(3) . . ? C10 C11 C12 120.9(4) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? C13 C12 C11 119.4(4) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C14 C13 C12 120.1(3) . . ? C14 C13 C16 120.8(3) . . ? C12 C13 C16 119.1(4) . . ? C15 C14 C13 119.8(3) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C14 C15 C10 121.2(4) . . ? C14 C15 H15 119.4 . . ? C10 C15 H15 119.4 . . ? O1 C16 O2 125.9(3) . . ? O1 C16 C13 118.4(4) . . ? O2 C16 C13 115.7(3) . . ? N3 C17 C18 110.9(4) . . ? N3 C17 H17 124.6 . . ? C18 C17 H17 124.5 . . ? C19 C18 C17 107.3(4) . . ? C19 C18 H18 126.4 . . ? C17 C18 H18 126.4 . . ? C18 C19 C20 107.1(4) . . ? C18 C19 H19 126.5 . . ? C20 C19 H19 126.5 . . ? C21 C20 N3 122.7(4) . . ? C21 C20 C19 128.9(4) . . ? N3 C20 C19 108.5(4) . . ? C22 C21 C20 125.9(3) . . ? C22 C21 C26 117.4(4) . . ? C20 C21 C26 116.6(4) . . ? C21 C22 N4 123.7(4) . . ? C21 C22 C23 128.4(4) . . ? N4 C22 C23 107.9(4) . . ? C24 C23 C22 108.1(4) . . ? C24 C23 H23 125.9 . . ? C22 C23 H23 125.9 . . ? C23 C24 C25 105.4(4) . . ? C23 C24 H24 127.3 . . ? C25 C24 H24 127.3 . . ? N4 C25 C24 112.1(4) . . ? N4 C25 H25 123.9 . . ? C24 C25 H25 123.9 . . ? C31 C26 C27 119.1(4) . . ? C31 C26 C21 122.2(4) . . ? C27 C26 C21 118.6(4) . . ? C26 C27 C28 120.7(4) . . ? C26 C27 H27 119.7 . . ? C28 C27 H27 119.7 . . ? C29 C28 C27 120.1(4) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? C30 C29 C28 119.7(4) . . ? C30 C29 C32 120.4(4) . . ? C28 C29 C32 119.8(4) . . ? C29 C30 C31 119.6(5) . . ? C29 C30 H30 120.2 . . ? C31 C30 H30 120.2 . . ? C26 C31 C30 120.8(5) . . ? C26 C31 H31 119.6 . . ? C30 C31 H31 119.6 . . ? O3 C32 O4 126.8(4) . . ? O3 C32 C29 117.6(4) . . ? O4 C32 C29 115.6(4) . . ? N5 C33 C34 112.0(3) . . ? N5 C33 H33 124.0 . . ? C34 C33 H33 124.0 . . ? C35 C34 C33 106.5(4) . . ? C35 C34 H34 126.7 . . ? C33 C34 H34 126.7 . . ? C34 C35 C36 107.6(4) . . ? C34 C35 H35 126.2 . . ? C36 C35 H35 126.2 . . ? C37 C36 N5 122.8(3) . . ? C37 C36 C35 128.5(4) . . ? N5 C36 C35 108.4(3) . . ? C36 C37 C38 126.5(3) . . ? C36 C37 C42 116.5(3) . . ? C38 C37 C42 116.9(3) . . ? C37 C38 N6 123.9(3) . . ? C37 C38 C39 128.2(4) . . ? N6 C38 C39 107.9(3) . . ? C40 C39 C38 108.1(4) . . ? C40 C39 H39 126.0 . . ? C38 C39 H39 126.0 . . ? C39 C40 C41 105.5(4) . . ? C39 C40 H40 127.2 . . ? C41 C40 H40 127.2 . . ? N6 C41 C40 111.9(4) . . ? N6 C41 H41 124.0 . . ? C40 C41 H41 124.0 . . ? C43 C42 C47 119.0(4) . . ? C43 C42 C37 120.9(3) . . ? C47 C42 C37 120.0(4) . . ? C42 C43 C44 120.2(4) . . ? C42 C43 H43 119.9 . . ? C44 C43 H43 119.9 . . ? C45 C44 C43 121.2(4) . . ? C45 C44 H44 119.4 . . ? C43 C44 H44 119.4 . . ? C46 C45 C44 118.6(4) . . ? C46 C45 C48 119.6(4) . . ? C44 C45 C48 121.7(4) . . ? C45 C46 C47 120.8(4) . . ? C45 C46 H46 119.6 . . ? C47 C46 H46 119.6 . . ? C42 C47 C46 120.0(4) . . ? C42 C47 H47 120.0 . . ? C46 C47 H47 120.0 . . ? O5 C48 O6 121.9(4) . . ? O5 C48 C45 121.2(4) . . ? O6 C48 C45 116.9(4) . . ? O5 C48 Zn2 74.3(2) . 1_456 ? O6 C48 Zn2 47.61(18) . 1_456 ? C45 C48 Zn2 164.3(3) . 1_456 ? C1 N1 C4 106.0(3) . . ? C1 N1 Co1 125.8(3) . . ? C4 N1 Co1 127.4(3) . . ? C9 N2 C6 106.4(3) . . ? C9 N2 Co1 124.8(2) . . ? C6 N2 Co1 127.3(3) . . ? C17 N3 C20 106.2(3) . . ? C17 N3 Co1 126.3(3) . . ? C20 N3 Co1 126.8(3) . . ? C25 N4 C22 106.4(3) . . ? C25 N4 Co1 126.9(3) . . ? C22 N4 Co1 125.5(3) . . ? C33 N5 C36 105.5(3) . . ? C33 N5 Co1 127.8(2) . . ? C36 N5 Co1 126.5(3) . . ? C41 N6 C38 106.6(3) . . ? C41 N6 Co1 127.2(3) . . ? C38 N6 Co1 126.2(2) . . ? C16 O1 Zn1 132.9(2) . . ? C16 O2 Zn2 119.5(2) . . ? C32 O3 Zn1 137.6(3) . 1_546 ? C32 O4 Zn2 127.4(3) . 1_546 ? C48 O5 Zn1 143.7(3) . 1_456 ? C48 O6 Zn2 103.7(3) . 1_456 ? O7 C49 N7 127.9(6) . . ? O7 C49 H49 116.0 . . ? N7 C49 H49 116.0 . . ? C51 C50 N7 111(3) . . ? C51 C50 H50A 109.4 . . ? N7 C50 H50A 109.4 . . ? C51 C50 H50B 109.4 . . ? N7 C50 H50B 109.4 . . ? H50A C50 H50B 108.0 . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? N7 C52 C53 114.8(11) . . ? N7 C52 H52A 108.6 . . ? C53 C52 H52A 108.6 . . ? N7 C52 H52B 108.6 . . ? C53 C52 H52B 108.6 . . ? H52A C52 H52B 107.6 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C49 N7 C52 123.6(11) . . ? C49 N7 C50 113.0(17) . . ? C52 N7 C50 121.8(17) . . ? C49 O7 Zn2 123.0(3) . . ? C56 C55 N8 120.1(18) . . ? C56 C55 H55A 107.3 . . ? N8 C55 H55A 107.3 . . ? C56 C55 H55B 107.3 . . ? N8 C55 H55B 107.3 . . ? H55A C55 H55B 106.9 . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C58 C57 N8 113.8(15) . . ? C58 C57 H57A 108.8 . . ? N8 C57 H57A 108.8 . . ? C58 C57 H57B 108.8 . . ? N8 C57 H57B 108.8 . . ? H57A C57 H57B 107.7 . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C55 N8 C57 117.1(11) . . ? N9 C59 O9 126.4(13) . . ? N9 C60 C61 118.7(9) . . ? N9 C60 H60A 107.6 . . ? C61 C60 H60A 107.6 . . ? N9 C60 H60B 107.6 . . ? C61 C60 H60B 107.6 . . ? H60A C60 H60B 107.1 . . ? C60 C61 H61A 109.5 . . ? C60 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C60 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? N9 C62 C63 114.8(9) . . ? N9 C62 H62A 108.6 . . ? C63 C62 H62A 108.6 . . ? N9 C62 H62B 108.6 . . ? C63 C62 H62B 108.6 . . ? H62A C62 H62B 107.5 . . ? C62 C63 H63A 109.5 . . ? C62 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C62 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C59 N9 C60 117.2(10) . . ? C59 N9 C62 121.9(10) . . ? C60 N9 C62 120.8(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -2.3(6) . . . . ? C1 C2 C3 C4 3.0(6) . . . . ? C2 C3 C4 C5 175.9(4) . . . . ? C2 C3 C4 N1 -2.8(5) . . . . ? N1 C4 C5 C6 -3.2(6) . . . . ? C3 C4 C5 C6 178.2(4) . . . . ? N1 C4 C5 C10 175.4(3) . . . . ? C3 C4 C5 C10 -3.1(6) . . . . ? C4 C5 C6 N2 -8.6(6) . . . . ? C10 C5 C6 N2 172.7(3) . . . . ? C4 C5 C6 C7 168.9(4) . . . . ? C10 C5 C6 C7 -9.8(6) . . . . ? N2 C6 C7 C8 0.2(4) . . . . ? C5 C6 C7 C8 -177.6(4) . . . . ? C6 C7 C8 C9 0.5(5) . . . . ? C7 C8 C9 N2 -1.0(5) . . . . ? C4 C5 C10 C11 127.8(5) . . . . ? C6 C5 C10 C11 -53.5(5) . . . . ? C4 C5 C10 C15 -52.7(5) . . . . ? C6 C5 C10 C15 126.1(4) . . . . ? C15 C10 C11 C12 -1.0(7) . . . . ? C5 C10 C11 C12 178.5(4) . . . . ? C10 C11 C12 C13 1.1(7) . . . . ? C11 C12 C13 C14 -0.6(7) . . . . ? C11 C12 C13 C16 -177.3(4) . . . . ? C12 C13 C14 C15 -0.1(6) . . . . ? C16 C13 C14 C15 176.6(3) . . . . ? C13 C14 C15 C10 0.1(6) . . . . ? C11 C10 C15 C14 0.4(6) . . . . ? C5 C10 C15 C14 -179.1(4) . . . . ? C14 C13 C16 O1 12.2(5) . . . . ? C12 C13 C16 O1 -171.1(4) . . . . ? C14 C13 C16 O2 -166.7(3) . . . . ? C12 C13 C16 O2 10.0(5) . . . . ? N3 C17 C18 C19 1.2(6) . . . . ? C17 C18 C19 C20 -1.4(5) . . . . ? C18 C19 C20 C21 -179.0(4) . . . . ? C18 C19 C20 N3 1.2(5) . . . . ? N3 C20 C21 C22 -5.8(7) . . . . ? C19 C20 C21 C22 174.5(4) . . . . ? N3 C20 C21 C26 172.4(4) . . . . ? C19 C20 C21 C26 -7.4(6) . . . . ? C20 C21 C22 N4 2.6(7) . . . . ? C26 C21 C22 N4 -175.5(4) . . . . ? C20 C21 C22 C23 -174.3(4) . . . . ? C26 C21 C22 C23 7.5(7) . . . . ? C21 C22 C23 C24 176.1(4) . . . . ? N4 C22 C23 C24 -1.2(5) . . . . ? C22 C23 C24 C25 1.0(6) . . . . ? C23 C24 C25 N4 -0.5(6) . . . . ? C22 C21 C26 C31 -76.8(6) . . . . ? C20 C21 C26 C31 104.9(6) . . . . ? C22 C21 C26 C27 104.6(5) . . . . ? C20 C21 C26 C27 -73.7(5) . . . . ? C31 C26 C27 C28 -0.5(7) . . . . ? C21 C26 C27 C28 178.1(4) . . . . ? C26 C27 C28 C29 0.6(7) . . . . ? C27 C28 C29 C30 0.3(7) . . . . ? C27 C28 C29 C32 -179.4(4) . . . . ? C28 C29 C30 C31 -1.4(9) . . . . ? C32 C29 C30 C31 178.3(5) . . . . ? C27 C26 C31 C30 -0.5(9) . . . . ? C21 C26 C31 C30 -179.1(6) . . . . ? C29 C30 C31 C26 1.5(10) . . . . ? C30 C29 C32 O3 6.4(7) . . . . ? C28 C29 C32 O3 -173.9(4) . . . . ? C30 C29 C32 O4 -172.3(5) . . . . ? C28 C29 C32 O4 7.4(6) . . . . ? N5 C33 C34 C35 0.5(5) . . . . ? C33 C34 C35 C36 0.4(5) . . . . ? C34 C35 C36 C37 173.0(4) . . . . ? C34 C35 C36 N5 -1.1(5) . . . . ? N5 C36 C37 C38 -2.1(6) . . . . ? C35 C36 C37 C38 -175.4(4) . . . . ? N5 C36 C37 C42 175.8(3) . . . . ? C35 C36 C37 C42 2.5(6) . . . . ? C36 C37 C38 N6 -0.8(6) . . . . ? C42 C37 C38 N6 -178.6(3) . . . . ? C36 C37 C38 C39 175.4(4) . . . . ? C42 C37 C38 C39 -2.5(6) . . . . ? C37 C38 C39 C40 -176.8(4) . . . . ? N6 C38 C39 C40 -0.2(5) . . . . ? C38 C39 C40 C41 0.6(5) . . . . ? C39 C40 C41 N6 -0.8(5) . . . . ? C36 C37 C42 C43 -79.1(5) . . . . ? C38 C37 C42 C43 99.0(5) . . . . ? C36 C37 C42 C47 100.4(5) . . . . ? C38 C37 C42 C47 -81.5(5) . . . . ? C47 C42 C43 C44 -1.0(7) . . . . ? C37 C42 C43 C44 178.5(5) . . . . ? C42 C43 C44 C45 2.0(8) . . . . ? C43 C44 C45 C46 -2.0(8) . . . . ? C43 C44 C45 C48 -179.7(5) . . . . ? C44 C45 C46 C47 1.0(7) . . . . ? C48 C45 C46 C47 178.7(4) . . . . ? C43 C42 C47 C46 -0.1(7) . . . . ? C37 C42 C47 C46 -179.5(4) . . . . ? C45 C46 C47 C42 0.0(7) . . . . ? C46 C45 C48 O5 5.8(6) . . . . ? C44 C45 C48 O5 -176.5(4) . . . . ? C46 C45 C48 O6 -174.4(4) . . . . ? C44 C45 C48 O6 3.2(6) . . . . ? C46 C45 C48 Zn2 176.0(9) . . . 1_456 ? C44 C45 C48 Zn2 -6.3(13) . . . 1_456 ? C2 C1 N1 C4 0.5(6) . . . . ? C2 C1 N1 Co1 171.1(3) . . . . ? C5 C4 N1 C1 -177.4(4) . . . . ? C3 C4 N1 C1 1.4(5) . . . . ? C5 C4 N1 Co1 12.3(5) . . . . ? C3 C4 N1 Co1 -169.0(3) . . . . ? N3 Co1 N1 C1 -83.2(4) . . . . ? N6 Co1 N1 C1 97.7(4) . . . . ? N4 Co1 N1 C1 7.9(4) . . . . ? N2 Co1 N1 C1 -176.8(4) . . . . ? N3 Co1 N1 C4 85.4(3) . . . . ? N6 Co1 N1 C4 -93.7(3) . . . . ? N4 Co1 N1 C4 176.5(3) . . . . ? N2 Co1 N1 C4 -8.3(3) . . . . ? C8 C9 N2 C6 1.1(4) . . . . ? C8 C9 N2 Co1 167.9(3) . . . . ? C5 C6 N2 C9 177.1(4) . . . . ? C7 C6 N2 C9 -0.8(4) . . . . ? C5 C6 N2 Co1 10.8(5) . . . . ? C7 C6 N2 Co1 -167.1(3) . . . . ? N3 Co1 N2 C9 106.1(3) . . . . ? N5 Co1 N2 C9 17.4(3) . . . . ? N6 Co1 N2 C9 -75.1(3) . . . . ? N1 Co1 N2 C9 -166.7(3) . . . . ? N3 Co1 N2 C6 -89.9(3) . . . . ? N5 Co1 N2 C6 -178.6(3) . . . . ? N6 Co1 N2 C6 88.9(3) . . . . ? N1 Co1 N2 C6 -2.7(3) . . . . ? C18 C17 N3 C20 -0.4(5) . . . . ? C18 C17 N3 Co1 -171.6(3) . . . . ? C21 C20 N3 C17 179.7(4) . . . . ? C19 C20 N3 C17 -0.5(5) . . . . ? C21 C20 N3 Co1 -9.1(6) . . . . ? C19 C20 N3 Co1 170.7(3) . . . . ? N5 Co1 N3 C17 102.0(4) . . . . ? N1 Co1 N3 C17 -79.8(4) . . . . ? N4 Co1 N3 C17 -171.9(4) . . . . ? N2 Co1 N3 C17 11.7(4) . . . . ? N5 Co1 N3 C20 -67.4(3) . . . . ? N1 Co1 N3 C20 110.8(3) . . . . ? N4 Co1 N3 C20 18.7(3) . . . . ? N2 Co1 N3 C20 -157.7(3) . . . . ? C24 C25 N4 C22 -0.2(5) . . . . ? C24 C25 N4 Co1 168.0(3) . . . . ? C21 C22 N4 C25 -176.6(4) . . . . ? C23 C22 N4 C25 0.9(5) . . . . ? C21 C22 N4 Co1 14.9(6) . . . . ? C23 C22 N4 Co1 -167.6(3) . . . . ? N3 Co1 N4 C25 172.5(3) . . . . ? N5 Co1 N4 C25 -98.9(3) . . . . ? N6 Co1 N4 C25 -6.4(3) . . . . ? N1 Co1 N4 C25 85.3(3) . . . . ? N3 Co1 N4 C22 -21.3(3) . . . . ? N5 Co1 N4 C22 67.2(3) . . . . ? N6 Co1 N4 C22 159.7(3) . . . . ? N1 Co1 N4 C22 -108.5(3) . . . . ? C34 C33 N5 C36 -1.2(4) . . . . ? C34 C33 N5 Co1 174.0(3) . . . . ? C37 C36 N5 C33 -173.1(4) . . . . ? C35 C36 N5 C33 1.4(4) . . . . ? C37 C36 N5 Co1 11.7(5) . . . . ? C35 C36 N5 Co1 -173.8(3) . . . . ? N3 Co1 N5 C33 -7.0(3) . . . . ? N6 Co1 N5 C33 172.1(3) . . . . ? N4 Co1 N5 C33 -98.3(3) . . . . ? N2 Co1 N5 C33 86.7(3) . . . . ? N3 Co1 N5 C36 167.1(3) . . . . ? N6 Co1 N5 C36 -13.8(3) . . . . ? N4 Co1 N5 C36 75.8(3) . . . . ? N2 Co1 N5 C36 -99.2(3) . . . . ? C40 C41 N6 C38 0.7(5) . . . . ? C40 C41 N6 Co1 -176.7(3) . . . . ? C37 C38 N6 C41 176.5(4) . . . . ? C39 C38 N6 C41 -0.3(4) . . . . ? C37 C38 N6 Co1 -6.1(5) . . . . ? C39 C38 N6 Co1 177.1(3) . . . . ? N5 Co1 N6 C41 -172.1(3) . . . . ? N1 Co1 N6 C41 9.6(3) . . . . ? N4 Co1 N6 C41 101.8(3) . . . . ? N2 Co1 N6 C41 -82.0(3) . . . . ? N5 Co1 N6 C38 11.0(3) . . . . ? N1 Co1 N6 C38 -167.2(3) . . . . ? N4 Co1 N6 C38 -75.1(3) . . . . ? N2 Co1 N6 C38 101.2(3) . . . . ? O2 C16 O1 Zn1 -53.5(5) . . . . ? C13 C16 O1 Zn1 127.8(3) . . . . ? O3 Zn1 O1 C16 108.9(3) 1_564 . . . ? O3 Zn1 O1 C16 -71.1(3) 2_756 . . . ? O5 Zn1 O1 C16 15.7(3) 1_654 . . . ? O5 Zn1 O1 C16 -164.3(3) 2_666 . . . ? O1 C16 O2 Zn2 -4.6(5) . . . . ? C13 C16 O2 Zn2 174.1(2) . . . . ? O4 Zn2 O2 C16 -40.8(3) 1_564 . . . ? O6 Zn2 O2 C16 103.8(3) 1_654 . . . ? O7 Zn2 O2 C16 -142.6(3) . . . . ? C48 Zn2 O2 C16 79.2(3) 1_654 . . . ? O4 C32 O3 Zn1 -10.0(7) . . . 1_546 ? C29 C32 O3 Zn1 171.4(3) . . . 1_546 ? O3 C32 O4 Zn2 -20.4(6) . . . 1_546 ? C29 C32 O4 Zn2 158.2(3) . . . 1_546 ? O6 C48 O5 Zn1 -87.3(6) . . . 1_456 ? C45 C48 O5 Zn1 92.4(5) . . . 1_456 ? Zn2 C48 O5 Zn1 -84.8(4) 1_456 . . 1_456 ? O5 C48 O6 Zn2 3.3(5) . . . 1_456 ? C45 C48 O6 Zn2 -176.5(3) . . . 1_456 ? O7 C49 N7 C52 -172.2(9) . . . . ? O7 C49 N7 C50 22(2) . . . . ? C53 C52 N7 C49 -96.3(16) . . . . ? C53 C52 N7 C50 68(3) . . . . ? C51 C50 N7 C49 -81(3) . . . . ? C51 C50 N7 C52 113(3) . . . . ? N7 C49 O7 Zn2 143.3(7) . . . . ? O2 Zn2 O7 C49 4.4(4) . . . . ? O4 Zn2 O7 C49 -116.9(4) 1_564 . . . ? O6 Zn2 O7 C49 134.6(4) 1_654 . . . ? C48 Zn2 O7 C49 124.6(4) 1_654 . . . ? C56 C55 N8 C57 108.4(19) . . . . ? C58 C57 N8 C55 -62.2(19) . . . . ? O9 C59 N9 C60 175.6(11) . . . . ? O9 C59 N9 C62 -1.5(18) . . . . ? C61 C60 N9 C59 103.3(12) . . . . ? C61 C60 N9 C62 -79.5(13) . . . . ? C63 C62 N9 C59 88.4(13) . . . . ? C63 C62 N9 C60 -88.7(11) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.811 _refine_diff_density_min -0.413 _refine_diff_density_rms 0.092 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.012 0.000 0.000 545.7 125.7 2 0.000 0.500 0.500 453.0 98.4 _platon_squeeze_details ; ;