# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 1350 loop_ _publ_author_name 'Burrows, Andrew' _publ_contact_author_name 'Burrows, Andrew' _publ_contact_author_email a.d.burrows@bath.ac.uk _publ_section_title ; The synthesis, structures and reactions of zinc and cobalt metal-organic frameworks incorporating an alkyne-based dicarboxylate linker ; # Attachment '- hodgson.cif' data_k08adb13 _database_code_depnum_ccdc_archive 'CCDC 839201' #TrackingRef '- hodgson.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H35 N3 O10.50 Zn2' _chemical_formula_weight 772.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnmn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y, z' _cell_length_a 19.8070(3) _cell_length_b 27.7140(5) _cell_length_c 27.8470(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 15286.1(5) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 138395 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 21.967 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.671 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3184 _exptl_absorpt_coefficient_mu 0.655 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.54 _exptl_absorpt_correction_T_max 0.75 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 117607 _diffrn_reflns_av_R_equivalents 0.1865 _diffrn_reflns_av_sigmaI/netI 0.0792 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.58 _diffrn_reflns_theta_max 21.92 _reflns_number_total 9432 _reflns_number_gt 5767 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The asymmetric unit in this structure consists of 1 full zinc, one full dicarboxylate ligand, 2 half-occupancy zincs (located at special positions coincident with a crystallographic mirror plane in the space group symmetry), one half of a dicarboxylate ligand (wherein O6, O7, O8, C18-26, C29, C30, O8 -- and associated hydrogens where relevent also lie on the mirror plane), 2 half water molecules (O9, O10 -- also on the mirror symmetry element), and approximately 3 DMF molecules. The water hydrogens could not be located reliably, and hence were omitted from the final least squares refinement. The DMF was very diffuse / disordered. Hence the data were subjected to the PLATON SQUEEZE routine, from which the estimate of 3 molecules per asymmetric unit arose. This solvent was accounted for in the unit cell contents during the final least squares cycles. Data collection for this crystal structure involved several heroic efforts, and it is a miracle all round that severe mental illness was not contracted by some of the parties involved. Early batches of crystals obtained would have been perfectly respectable size-wise had this been a molecular structure determination. However, such samples are generally poor candidates for 3-D MOF data collections, where diffraction intensity falls off quickly - and this sample was no exception. Thus, the first goal was to produce larger crystals -- not easy, as crystalline material cannot be readily recrystallised. This is quite simply a function of a MOF being a covalently bonded 3-D polymer. Valiant efforts by the (now permanently worried and fretful) student eventually yielded 'blocky' crystals, which looked excellent under the microscope, a feature that did not follow through to yield and excellent diffraction pattern. Elation when, at last, a decent crystal was mounted (diffraction to 20o approx) rapidly turned to despair when it was note that the sample degraded in the X-ray beam, and also seemed to undergo a possible phase transition. Several trials later, an optimum temperature of 200 K for data collection was settled upon, and low sigmas on the intensity data were sacrificed in order to get a 'complete' data set before degradation of the sample. This was the correct decision, although it adversely affected R(int), such that data were truncated to 22o. Ultimately then, a very fine result indeed, as presented here. As for myself (MFM), ADB, and his group- well - all things heal, and therapy is helped a lot! ; _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^)+(0.0976P)^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 9432 _refine_ls_number_parameters 331 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1209 _refine_ls_R_factor_gt 0.0602 _refine_ls_wR_factor_ref 0.1769 _refine_ls_wR_factor_gt 0.1523 _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_restrained_S_all 0.985 _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 0.68856(3) 0.05763(2) 0.381992(19) 0.0550(2) Uani 1 1 d . . . Zn2 Zn 0.80041(3) 0.0000 0.43794(2) 0.0440(2) Uani 1 2 d S . . Zn3 Zn 0.80124(4) 0.0000 0.32423(3) 0.0594(3) Uani 1 2 d S . . O1 O 0.74407(19) 0.0000 0.38170(13) 0.0454(11) Uani 1 2 d S . . O2 O 0.68989(18) 0.08457(15) 0.44813(15) 0.0857(13) Uani 1 1 d . . . O3 O 0.7824(2) 0.05424(14) 0.48100(12) 0.0781(11) Uani 1 1 d . . . O4 O 0.7948(2) 0.4001(2) 0.8295(2) 0.148(2) Uani 1 1 d . . . O5 O 0.7034(3) 0.4382(3) 0.7959(3) 0.197(4) Uani 1 1 d . . . O6 O 0.8959(2) 0.0000 0.34774(17) 0.0730(16) Uani 1 2 d S . . O7 O 0.8978(2) 0.0000 0.42907(16) 0.0605(14) Uani 1 2 d S . . O8 O 1.59241(15) -0.04037(13) 0.37688(12) 0.0659(10) Uani 1 1 d . . . O9 O 0.7002(5) 0.0000 0.2803(5) 0.402(14) Uani 1 2 d S . . O10 O 0.8545(8) 0.0000 0.2520(4) 0.374(11) Uani 1 2 d S . . C1 C 0.7340(3) 0.0827(2) 0.4794(2) 0.0730(17) Uani 1 1 d . . . C2 C 0.7291(3) 0.1177(2) 0.5202(2) 0.0806(18) Uani 1 1 d . . . C3 C 0.6770(4) 0.1492(3) 0.5242(3) 0.141(3) Uani 1 1 d . . . H3 H 0.6419 0.1485 0.5010 0.170 Uiso 1 1 calc R . . C4 C 0.6737(5) 0.1830(3) 0.5618(3) 0.171(4) Uani 1 1 d . . . H4 H 0.6363 0.2044 0.5635 0.205 Uiso 1 1 calc R . . C5 C 0.7237(5) 0.1855(3) 0.5964(3) 0.132(3) Uani 1 1 d . . . C6 C 0.7713(5) 0.1525(3) 0.5928(3) 0.146(4) Uani 1 1 d . . . H6 H 0.8053 0.1524 0.6169 0.176 Uiso 1 1 calc R . . C7 C 0.7765(4) 0.1172(3) 0.5561(3) 0.129(3) Uani 1 1 d . . . H7 H 0.8117 0.0939 0.5563 0.154 Uiso 1 1 calc R . . C8 C 0.7236(4) 0.2204(4) 0.6310(3) 0.162(4) Uani 1 1 d . . . C9 C 0.7246(5) 0.2509(4) 0.6612(4) 0.170(4) Uani 1 1 d . . . C10 C 0.7300(5) 0.2883(4) 0.6980(4) 0.172(4) Uani 1 1 d . . . C11 C 0.7785(5) 0.2898(4) 0.7305(4) 0.189(5) Uani 1 1 d . . . H11 H 0.8101 0.2641 0.7317 0.226 Uiso 1 1 calc R . . C12 C 0.7854(4) 0.3278(4) 0.7632(3) 0.181(5) Uani 1 1 d . . . H12 H 0.8227 0.3288 0.7846 0.217 Uiso 1 1 calc R . . C13 C 0.7398(4) 0.3620(4) 0.7640(4) 0.189(5) Uani 1 1 d . . . C14 C 0.6922(5) 0.3644(4) 0.7298(5) 0.259(8) Uani 1 1 d . . . H14 H 0.6627 0.3914 0.7278 0.311 Uiso 1 1 calc R . . C15 C 0.6872(5) 0.3266(5) 0.6974(5) 0.265(8) Uani 1 1 d . . . H15 H 0.6524 0.3275 0.6739 0.318 Uiso 1 1 calc R . . C16 C 0.7458(4) 0.4065(5) 0.7958(4) 0.208(6) Uani 1 1 d . . . C17 C 0.9245(3) 0.0000 0.3885(3) 0.0570(19) Uani 1 2 d S . . C18 C 1.0024(3) 0.0000 0.3888(3) 0.063(2) Uani 1 2 d S . . C19 C 1.0343(4) 0.0000 0.3452(4) 0.137(5) Uani 1 2 d S . . H19 H 1.0084 0.0000 0.3165 0.164 Uiso 1 2 calc SR . . C20 C 1.1045(4) 0.0000 0.3427(3) 0.168(6) Uani 1 2 d S . . H20 H 1.1264 0.0000 0.3124 0.201 Uiso 1 2 calc SR . . C21 C 1.1428(4) 0.0000 0.3851(3) 0.087(3) Uani 1 2 d S . . C22 C 1.1074(4) 0.0000 0.4272(3) 0.095(3) Uani 1 2 d S . . H22 H 1.1316 0.0000 0.4566 0.114 Uiso 1 2 calc SR . . C23 C 1.0376(4) 0.0000 0.4285(3) 0.082(3) Uani 1 2 d S . . H23 H 1.0150 0.0000 0.4586 0.098 Uiso 1 2 calc SR . . C24 C 1.2151(4) 0.0000 0.3844(3) 0.105(3) Uani 1 2 d S . . C25 C 1.2747(4) 0.0000 0.3816(3) 0.102(3) Uani 1 2 d S . . C26 C 1.3470(4) 0.0000 0.3792(3) 0.083(3) Uani 1 2 d S . . C27 C 1.3817(3) -0.0436(3) 0.3782(2) 0.110(2) Uani 1 1 d . . . H27 H 1.3580 -0.0734 0.3782 0.132 Uiso 1 1 calc R . . C28 C 1.4513(3) -0.0427(3) 0.3772(2) 0.096(2) Uani 1 1 d . . . H28 H 1.4754 -0.0723 0.3779 0.115 Uiso 1 1 calc R . . C29 C 1.4870(3) 0.0000 0.3752(2) 0.066(2) Uani 1 2 d S . . C30 C 1.5646(3) 0.0000 0.3764(2) 0.0525(19) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0376(3) 0.0730(5) 0.0544(4) 0.0053(3) 0.0012(3) 0.0088(3) Zn2 0.0306(4) 0.0531(6) 0.0484(5) 0.000 -0.0014(3) 0.000 Zn3 0.0391(5) 0.0754(7) 0.0638(6) 0.000 0.0108(4) 0.000 O1 0.032(2) 0.051(3) 0.053(2) 0.000 0.003(2) 0.000 O2 0.043(2) 0.105(3) 0.109(3) -0.047(3) -0.010(2) 0.013(2) O3 0.080(3) 0.074(3) 0.080(3) -0.033(2) -0.007(2) 0.014(2) O4 0.080(4) 0.187(6) 0.178(5) -0.128(4) 0.012(3) -0.002(4) O5 0.070(4) 0.211(7) 0.311(9) -0.192(7) -0.023(4) 0.029(4) O6 0.034(3) 0.124(5) 0.061(3) 0.000 0.002(2) 0.000 O7 0.035(3) 0.093(4) 0.053(3) 0.000 0.001(2) 0.000 O8 0.0314(19) 0.078(3) 0.088(2) -0.004(2) -0.0047(16) 0.0013(19) O9 0.124(9) 0.86(5) 0.216(12) 0.000 -0.023(8) 0.000 O10 0.273(16) 0.68(3) 0.174(10) 0.000 -0.055(10) 0.000 C1 0.040(4) 0.086(5) 0.093(4) -0.044(4) 0.007(3) 0.001(3) C2 0.056(4) 0.081(5) 0.105(5) -0.041(4) -0.005(3) 0.022(4) C3 0.085(5) 0.172(8) 0.167(7) -0.104(7) -0.045(5) 0.038(5) C4 0.142(8) 0.174(9) 0.196(9) -0.133(8) -0.054(7) 0.075(7) C5 0.105(6) 0.124(7) 0.166(8) -0.094(6) -0.026(6) 0.022(5) C6 0.143(7) 0.176(9) 0.120(6) -0.092(6) -0.050(6) 0.043(7) C7 0.119(6) 0.130(7) 0.138(6) -0.074(6) -0.047(5) 0.049(5) C8 0.141(7) 0.173(9) 0.173(8) -0.127(7) -0.030(6) 0.044(7) C9 0.138(7) 0.189(10) 0.185(8) -0.128(8) -0.030(6) 0.026(7) C10 0.126(8) 0.193(11) 0.196(9) -0.139(8) -0.049(7) 0.038(8) C11 0.145(8) 0.194(10) 0.227(10) -0.139(9) -0.069(8) 0.068(8) C12 0.110(7) 0.220(11) 0.212(9) -0.172(9) -0.061(6) 0.056(7) C13 0.091(6) 0.219(11) 0.258(10) -0.218(9) -0.044(7) 0.049(7) C14 0.145(9) 0.265(13) 0.367(16) -0.271(13) -0.133(10) 0.095(8) C15 0.163(10) 0.288(15) 0.344(16) -0.254(14) -0.120(10) 0.106(10) C16 0.047(5) 0.303(15) 0.273(12) -0.221(11) -0.031(7) 0.007(7) C17 0.044(4) 0.064(5) 0.063(5) 0.000 -0.001(4) 0.000 C18 0.022(4) 0.105(7) 0.064(5) 0.000 0.008(4) 0.000 C19 0.035(5) 0.278(16) 0.098(8) 0.000 -0.005(5) 0.000 C20 0.030(5) 0.39(2) 0.082(7) 0.000 -0.004(5) 0.000 C21 0.028(4) 0.124(8) 0.110(7) 0.000 0.010(5) 0.000 C22 0.035(5) 0.174(10) 0.076(6) 0.000 -0.014(4) 0.000 C23 0.042(5) 0.153(9) 0.051(5) 0.000 -0.011(4) 0.000 C24 0.031(6) 0.173(11) 0.111(7) 0.000 0.001(5) 0.000 C25 0.030(5) 0.168(10) 0.108(7) 0.000 0.005(5) 0.000 C26 0.026(5) 0.125(9) 0.099(6) 0.000 0.004(4) 0.000 C27 0.030(4) 0.117(6) 0.184(7) -0.010(5) -0.001(4) -0.009(4) C28 0.030(3) 0.095(5) 0.162(6) -0.014(5) 0.005(3) -0.006(3) C29 0.023(4) 0.111(7) 0.063(5) 0.000 0.001(3) 0.000 C30 0.030(4) 0.079(6) 0.049(4) 0.000 0.000(3) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O4 1.903(4) 2_654 ? Zn1 O1 1.939(2) . ? Zn1 O8 1.969(3) 8_455 ? Zn1 O2 1.987(4) . ? Zn2 O1 1.923(4) . ? Zn2 O7 1.946(4) . ? Zn2 O3 1.956(3) 8 ? Zn2 O3 1.956(3) . ? Zn2 Zn1 3.1442(8) 8 ? Zn3 O5 1.888(5) 2_654 ? Zn3 O5 1.888(5) 7_755 ? Zn3 O1 1.960(4) . ? Zn3 O6 1.986(5) . ? Zn3 O10 2.270(14) . ? Zn3 O9 2.345(11) . ? O1 Zn1 1.939(2) 8 ? O2 C1 1.236(6) . ? O3 C1 1.242(6) . ? O4 C16 1.361(11) . ? O4 Zn1 1.903(4) 2_655 ? O5 C16 1.216(11) . ? O5 Zn3 1.888(5) 2_655 ? O6 C17 1.268(8) . ? O7 C17 1.247(7) . ? O8 C30 1.247(4) . ? O8 Zn1 1.969(3) 8_655 ? C1 C2 1.496(7) . ? C2 C3 1.355(8) . ? C2 C7 1.371(8) . ? C3 C4 1.406(9) . ? C3 H3 0.9500 . ? C4 C5 1.383(10) . ? C4 H4 0.9500 . ? C5 C6 1.319(10) . ? C5 C8 1.365(10) . ? C6 C7 1.420(9) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C9 1.192(9) . ? C9 C10 1.461(10) . ? C10 C11 1.321(10) . ? C10 C15 1.358(12) . ? C11 C12 1.399(10) . ? C11 H11 0.9500 . ? C12 C13 1.310(10) . ? C12 H12 0.9500 . ? C13 C14 1.343(11) . ? C13 C16 1.522(10) . ? C14 C15 1.386(11) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C17 C18 1.544(9) . ? C18 C23 1.306(9) . ? C18 C19 1.369(10) . ? C19 C20 1.392(11) . ? C19 H19 0.9500 . ? C20 C21 1.402(11) . ? C20 H20 0.9500 . ? C21 C22 1.367(10) . ? C21 C24 1.431(11) . ? C22 C23 1.384(10) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C25 1.182(10) . ? C25 C26 1.436(11) . ? C26 C27 1.390(7) 8 ? C26 C27 1.390(7) . ? C27 C28 1.379(7) . ? C27 H27 0.9500 . ? C28 C29 1.379(7) . ? C28 H28 0.9500 . ? C29 C28 1.379(7) 8 ? C29 C30 1.537(9) . ? C30 O8 1.247(4) 8 ? 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 O4 Zn1 O1 114.0(2) 2_654 . ? O4 Zn1 O8 105.16(17) 2_654 8_455 ? O1 Zn1 O8 110.36(14) . 8_455 ? O4 Zn1 O2 118.6(3) 2_654 . ? O1 Zn1 O2 107.81(16) . . ? O8 Zn1 O2 99.85(14) 8_455 . ? O1 Zn2 O7 118.18(17) . . ? O1 Zn2 O3 113.17(13) . 8 ? O7 Zn2 O3 105.00(15) . 8 ? O1 Zn2 O3 113.17(13) . . ? O7 Zn2 O3 105.00(15) . . ? O3 Zn2 O3 100.5(2) 8 . ? O1 Zn2 Zn1 35.67(6) . 8 ? O7 Zn2 Zn1 129.49(10) . 8 ? O3 Zn2 Zn1 77.57(12) 8 8 ? O3 Zn2 Zn1 124.45(12) . 8 ? O5 Zn3 O5 130.2(6) 2_654 7_755 ? O5 Zn3 O1 108.2(2) 2_654 . ? O5 Zn3 O1 108.2(2) 7_755 . ? O5 Zn3 O6 100.6(2) 2_654 . ? O5 Zn3 O6 100.6(2) 7_755 . ? O1 Zn3 O6 106.04(17) . . ? O5 Zn3 O10 69.7(2) 2_654 . ? O5 Zn3 O10 69.7(2) 7_755 . ? O1 Zn3 O10 172.4(4) . . ? O6 Zn3 O10 81.6(4) . . ? O5 Zn3 O9 75.0(2) 2_654 . ? O5 Zn3 O9 75.0(2) 7_755 . ? O1 Zn3 O9 86.2(3) . . ? O6 Zn3 O9 167.8(3) . . ? O10 Zn3 O9 86.3(4) . . ? Zn2 O1 Zn1 109.00(13) . 8 ? Zn2 O1 Zn1 109.00(13) . . ? Zn1 O1 Zn1 110.91(18) 8 . ? Zn2 O1 Zn3 109.25(18) . . ? Zn1 O1 Zn3 109.32(13) 8 . ? Zn1 O1 Zn3 109.33(13) . . ? C1 O2 Zn1 130.4(4) . . ? C1 O3 Zn2 127.4(4) . . ? C16 O4 Zn1 124.9(5) . 2_655 ? C16 O5 Zn3 133.6(5) . 2_655 ? C17 O6 Zn3 135.7(4) . . ? C17 O7 Zn2 122.3(4) . . ? C30 O8 Zn1 130.3(4) . 8_655 ? O2 C1 O3 126.6(5) . . ? O2 C1 C2 117.5(6) . . ? O3 C1 C2 115.9(5) . . ? C3 C2 C7 117.9(6) . . ? C3 C2 C1 122.0(6) . . ? C7 C2 C1 120.0(6) . . ? C2 C3 C4 121.7(7) . . ? C2 C3 H3 119.2 . . ? C4 C3 H3 119.2 . . ? C5 C4 C3 121.3(7) . . ? C5 C4 H4 119.3 . . ? C3 C4 H4 119.3 . . ? C6 C5 C8 123.1(8) . . ? C6 C5 C4 115.0(7) . . ? C8 C5 C4 121.8(8) . . ? C5 C6 C7 125.8(7) . . ? C5 C6 H6 117.1 . . ? C7 C6 H6 117.1 . . ? C2 C7 C6 117.9(7) . . ? C2 C7 H7 121.1 . . ? C6 C7 H7 121.1 . . ? C9 C8 C5 179.0(10) . . ? C8 C9 C10 176.7(11) . . ? C11 C10 C15 115.9(8) . . ? C11 C10 C9 123.8(10) . . ? C15 C10 C9 120.1(9) . . ? C10 C11 C12 122.8(9) . . ? C10 C11 H11 118.6 . . ? C12 C11 H11 118.6 . . ? C13 C12 C11 119.2(8) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? C12 C13 C14 120.6(7) . . ? C12 C13 C16 122.8(8) . . ? C14 C13 C16 115.3(9) . . ? C13 C14 C15 118.3(9) . . ? C13 C14 H14 120.8 . . ? C15 C14 H14 120.8 . . ? C10 C15 C14 122.6(9) . . ? C10 C15 H15 118.7 . . ? C14 C15 H15 118.7 . . ? O5 C16 O4 125.9(7) . . ? O5 C16 C13 122.1(8) . . ? O4 C16 C13 110.5(10) . . ? O7 C17 O6 128.5(6) . . ? O7 C17 C18 114.7(6) . . ? O6 C17 C18 116.8(7) . . ? C23 C18 C19 120.4(7) . . ? C23 C18 C17 122.6(7) . . ? C19 C18 C17 117.1(7) . . ? C18 C19 C20 120.2(8) . . ? C18 C19 H19 119.9 . . ? C20 C19 H19 119.9 . . ? C19 C20 C21 120.0(8) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C22 C21 C20 116.3(7) . . ? C22 C21 C24 121.7(8) . . ? C20 C21 C24 122.0(8) . . ? C21 C22 C23 122.4(7) . . ? C21 C22 H22 118.8 . . ? C23 C22 H22 118.8 . . ? C18 C23 C22 120.7(7) . . ? C18 C23 H23 119.6 . . ? C22 C23 H23 119.6 . . ? C25 C24 C21 177.1(10) . . ? C24 C25 C26 179.0(10) . . ? C27 C26 C27 120.8(7) 8 . ? C27 C26 C25 119.6(4) 8 . ? C27 C26 C25 119.6(4) . . ? C28 C27 C26 118.5(7) . . ? C28 C27 H27 120.7 . . ? C26 C27 H27 120.7 . . ? C29 C28 C27 122.0(7) . . ? C29 C28 H28 119.0 . . ? C27 C28 H28 119.0 . . ? C28 C29 C28 118.1(7) 8 . ? C28 C29 C30 120.8(3) 8 . ? C28 C29 C30 120.8(3) . . ? O8 C30 O8 127.5(6) 8 . ? O8 C30 C29 116.2(3) 8 . ? O8 C30 C29 116.2(3) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 21.92 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.549 _refine_diff_density_min -0.481 _refine_diff_density_rms 0.049 # 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 -0.007 -0.007 -0.004 11911.8 991.1 _platon_squeeze_details ; ; #===end data_k08adb18 _database_code_depnum_ccdc_archive 'CCDC 839202' #TrackingRef '- hodgson.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33.90 H35.10 Co1.50 N3.30 O9.30' _chemical_formula_weight 725.95 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 15.3310(2) _cell_length_b 17.9570(3) _cell_length_c 16.5330(3) _cell_angle_alpha 90.00 _cell_angle_beta 117.704(1) _cell_angle_gamma 90.00 _cell_volume 4029.73(11) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 103071 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Pale-pink _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.197 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1506 _exptl_absorpt_coefficient_mu 0.674 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.65 _exptl_absorpt_correction_T_max 0.70 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 76129 _diffrn_reflns_av_R_equivalents 0.1353 _diffrn_reflns_av_sigmaI/netI 0.0992 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.59 _diffrn_reflns_theta_max 27.60 _reflns_number_total 9233 _reflns_number_gt 5204 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Asymmetric unit consists of 1.5 cobalt centres, 1 full ligand molecule, one half of a ligand molecule, 1 DMF ligand and 2 areas of free solvent. The latter comprises of one DMF fragment with 50% occupancy plus one DMF fragment with 80%. The partial solvent was resfined subjects to similarity restraints for the bond distances and ADPs therein. There was clearly some disorder in these 2 areas, which is not unsurprising, but this could not be readily modelled. The largest difference peak in the electron density map is associated with the free solvent. ; _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^)+(0.1452P)^2^+3.1865P] 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 9233 _refine_ls_number_parameters 451 _refine_ls_number_restraints 53 _refine_ls_R_factor_all 0.1507 _refine_ls_R_factor_gt 0.0775 _refine_ls_wR_factor_ref 0.2547 _refine_ls_wR_factor_gt 0.2087 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.050 _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 Co1 Co 0.76893(4) -0.05885(3) -0.16769(4) 0.0273(2) Uani 1 1 d . . . Co2 Co 1.0000 0.0000 0.0000 0.0221(2) Uani 1 2 d S . . O1 O 0.7367(2) 0.01819(19) -0.0946(2) 0.0344(8) Uani 1 1 d . . . O2 O 0.8865(2) 0.03371(19) 0.0261(2) 0.0320(8) Uani 1 1 d . . . O3 O 0.2711(3) 0.4640(2) 0.2473(2) 0.0443(9) Uani 1 1 d . . . O4 O 0.4061(2) 0.51162(18) 0.3564(2) 0.0300(7) Uani 1 1 d . . . O5 O 0.8215(2) -0.13624(17) -0.0675(2) 0.0362(8) Uani 1 1 d . . . O6 O 0.9831(2) -0.11203(17) 0.0163(2) 0.0306(7) Uani 1 1 d . . . O7 O 0.6219(3) -0.0849(2) -0.2319(3) 0.0421(9) Uani 1 1 d . . . O8 O 0.7898(3) -0.1406(2) -0.2528(3) 0.0536(11) Uani 1 1 d D . . O9 O -0.0153(9) 0.1515(8) -0.6497(10) 0.129(3) Uani 0.50 1 d PDU . . O10 O 0.6332(8) -0.1212(6) 0.1942(7) 0.140(2) Uiso 0.80 1 d PDU . . N1 N 0.4668(4) -0.0392(4) -0.3013(4) 0.0718(17) Uani 1 1 d . . . N2 N 0.8886(5) -0.2385(3) -0.2479(4) 0.0721(17) Uani 1 1 d D . . N3 N 0.1446(12) 0.1256(9) -0.5567(11) 0.128(3) Uani 0.50 1 d PDU . . N4 N 0.6646(8) -0.1613(6) 0.0881(8) 0.117(2) Uiso 0.80 1 d PDU . . C1 C 0.7953(4) 0.0435(3) -0.0174(4) 0.0308(11) Uani 1 1 d . . . C2 C 0.7498(4) 0.0908(3) 0.0290(4) 0.0368(12) Uani 1 1 d . . . C3 C 0.6502(4) 0.1046(3) -0.0132(4) 0.0437(13) Uani 1 1 d . . . H3 H 0.6098 0.0841 -0.0719 0.052 Uiso 1 1 calc R . . C4 C 0.6077(4) 0.1480(4) 0.0282(4) 0.0545(16) Uani 1 1 d . . . H4 H 0.5387 0.1568 -0.0016 0.065 Uiso 1 1 calc R . . C5 C 0.6672(5) 0.1791(4) 0.1147(5) 0.0576(17) Uani 1 1 d . . . C6 C 0.7659(5) 0.1631(5) 0.1571(5) 0.076(2) Uani 1 1 d . . . H6 H 0.8068 0.1825 0.2164 0.092 Uiso 1 1 calc R . . C7 C 0.8074(5) 0.1186(4) 0.1142(5) 0.0643(19) Uani 1 1 d . . . H7 H 0.8759 0.1078 0.1447 0.077 Uiso 1 1 calc R . . C8 C 0.6232(5) 0.2267(4) 0.1550(5) 0.0630(19) Uani 1 1 d . . . C9 C 0.5830(5) 0.2670(4) 0.1844(5) 0.066(2) Uani 1 1 d . . . C10 C 0.5301(4) 0.3143(4) 0.2176(4) 0.0563(17) Uani 1 1 d . . . C11 C 0.4344(5) 0.2956(4) 0.2010(4) 0.0592(18) Uani 1 1 d . . . H11 H 0.4059 0.2498 0.1723 0.071 Uiso 1 1 calc R . . C12 C 0.3817(4) 0.3444(4) 0.2266(4) 0.0546(16) Uani 1 1 d . . . H12 H 0.3161 0.3324 0.2136 0.066 Uiso 1 1 calc R . . C13 C 0.4238(4) 0.4105(3) 0.2711(3) 0.0393(12) Uani 1 1 d . . . C14 C 0.5197(4) 0.4263(3) 0.2923(4) 0.0455(14) Uani 1 1 d . . . H14 H 0.5498 0.4703 0.3255 0.055 Uiso 1 1 calc R . . C15 C 0.5728(4) 0.3790(4) 0.2658(4) 0.0553(16) Uani 1 1 d . . . H15 H 0.6390 0.3908 0.2806 0.066 Uiso 1 1 calc R . . C16 C 0.3629(4) 0.4639(3) 0.2924(3) 0.0366(12) Uani 1 1 d . . . C17 C 0.9103(4) -0.1545(2) -0.0192(3) 0.0294(10) Uani 1 1 d . . . C18 C 0.9307(4) -0.2374(3) -0.0056(3) 0.0323(11) Uani 1 1 d . . . C19 C 0.8572(4) -0.2880(3) -0.0548(4) 0.0440(14) Uani 1 1 d . . . H19 H 0.7916 -0.2709 -0.0908 0.053 Uiso 1 1 calc R . . C20 C 0.8774(4) -0.3632(3) -0.0524(4) 0.0484(15) Uani 1 1 d . . . H20 H 0.8265 -0.3970 -0.0886 0.058 Uiso 1 1 calc R . . C21 C 0.9714(4) -0.3893(3) 0.0021(3) 0.0402(13) Uani 1 1 d . . . C22 C 1.0468(4) -0.3391(3) 0.0556(4) 0.0452(14) Uani 1 1 d . . . H22 H 1.1113 -0.3568 0.0948 0.054 Uiso 1 1 calc R . . C23 C 1.0262(4) -0.2637(3) 0.0506(4) 0.0384(12) Uani 1 1 d . . . H23 H 1.0772 -0.2295 0.0855 0.046 Uiso 1 1 calc R . . C24 C 0.9921(4) -0.4673(3) 0.0016(4) 0.0428(13) Uani 1 1 d . . . C25 C 0.5637(5) -0.0333(4) -0.2680(5) 0.0599(17) Uani 1 1 d . . . H25 H 0.5897 0.0136 -0.2724 0.072 Uiso 1 1 calc R . . C26 C 0.3991(7) 0.0226(6) -0.3502(7) 0.103(3) Uani 1 1 d . . . H26A H 0.4369 0.0648 -0.3551 0.155 Uiso 1 1 calc R . . H26B H 0.3639 0.0380 -0.3164 0.155 Uiso 1 1 calc R . . H26C H 0.3515 0.0060 -0.4115 0.155 Uiso 1 1 calc R . . C27 C 0.4219(7) -0.1075(6) -0.3015(8) 0.122(4) Uani 1 1 d . . . H27A H 0.4689 -0.1481 -0.2900 0.183 Uiso 1 1 calc R . . H27B H 0.3642 -0.1149 -0.3611 0.183 Uiso 1 1 calc R . . H27C H 0.4012 -0.1071 -0.2536 0.183 Uiso 1 1 calc R . . C28 C 0.8711(5) -0.1717(3) -0.2220(4) 0.0566(16) Uani 1 1 d D . . H28 H 0.9259 -0.1460 -0.1759 0.068 Uiso 1 1 calc R . . C29 C 0.9821(6) -0.2714(5) -0.2057(6) 0.092(3) Uani 1 1 d D . . H29A H 1.0228 -0.2465 -0.1473 0.138 Uiso 1 1 calc R . . H29B H 1.0133 -0.2664 -0.2454 0.138 Uiso 1 1 calc R . . H29C H 0.9757 -0.3243 -0.1948 0.138 Uiso 1 1 calc R . . C30 C 0.8104(6) -0.2848(5) -0.3110(7) 0.101(3) Uani 1 1 d D . . H30A H 0.7472 -0.2663 -0.3178 0.152 Uiso 1 1 calc R . . H30B H 0.8206 -0.3361 -0.2879 0.152 Uiso 1 1 calc R . . H30C H 0.8099 -0.2839 -0.3705 0.152 Uiso 1 1 calc R . . C33 C 0.1576(13) 0.0550(9) -0.5826(14) 0.128(4) Uani 0.50 1 d PDU . . H33A H 0.1562 0.0184 -0.5392 0.191 Uiso 0.50 1 calc PR . . H33B H 0.2212 0.0524 -0.5831 0.191 Uiso 0.50 1 calc PR . . H33C H 0.1045 0.0441 -0.6439 0.191 Uiso 0.50 1 calc PR . . C32 C 0.2232(12) 0.1602(11) -0.4847(12) 0.127(4) Uani 0.50 1 d PDU . . H32A H 0.2247 0.2129 -0.4993 0.191 Uiso 0.50 1 calc PR . . H32B H 0.2849 0.1363 -0.4747 0.191 Uiso 0.50 1 calc PR . . H32C H 0.2154 0.1559 -0.4293 0.191 Uiso 0.50 1 calc PR . . C34 C 0.6487(10) -0.1703(8) 0.1584(9) 0.120(2) Uiso 0.80 1 d PDU . . H34 H 0.6500 -0.2193 0.1807 0.144 Uiso 0.80 1 calc PR . . C36 C 0.6666(10) -0.1029(7) 0.0368(8) 0.118(2) Uiso 0.80 1 d PDU . . H36A H 0.6571 -0.0564 0.0628 0.177 Uiso 0.80 1 calc PR . . H36B H 0.6138 -0.1085 -0.0259 0.177 Uiso 0.80 1 calc PR . . H36C H 0.7304 -0.1016 0.0366 0.177 Uiso 0.80 1 calc PR . . C35 C 0.6887(11) -0.2309(7) 0.0603(9) 0.124(3) Uiso 0.80 1 d PDU . . H35A H 0.7605 -0.2356 0.0867 0.186 Uiso 0.80 1 calc PR . . H35B H 0.6593 -0.2325 -0.0065 0.186 Uiso 0.80 1 calc PR . . H35C H 0.6629 -0.2721 0.0817 0.186 Uiso 0.80 1 calc PR . . C31 C 0.0595(11) 0.1663(11) -0.5942(13) 0.128(3) Uani 0.50 1 d PDU . . H31 H 0.0648 0.2147 -0.5691 0.154 Uiso 0.50 1 calc PR . . 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 0.0274(4) 0.0247(4) 0.0311(4) -0.0009(3) 0.0148(3) -0.0012(2) Co2 0.0248(5) 0.0144(4) 0.0297(5) -0.0005(3) 0.0149(4) 0.0005(3) O1 0.0331(19) 0.0313(19) 0.039(2) -0.0037(15) 0.0168(17) 0.0054(15) O2 0.0286(18) 0.0313(18) 0.0407(19) -0.0026(15) 0.0201(16) 0.0038(14) O3 0.032(2) 0.055(2) 0.044(2) -0.0172(18) 0.0156(18) 0.0050(17) O4 0.0298(17) 0.0297(19) 0.0327(17) -0.0010(14) 0.0164(15) 0.0025(14) O5 0.0322(19) 0.0197(17) 0.055(2) 0.0050(15) 0.0184(17) 0.0021(14) O6 0.0342(18) 0.0148(16) 0.0397(18) 0.0001(13) 0.0144(15) -0.0013(13) O7 0.033(2) 0.039(2) 0.052(2) 0.0008(17) 0.0175(18) 0.0008(17) O8 0.044(2) 0.063(3) 0.055(2) -0.025(2) 0.024(2) -0.007(2) O9 0.089(6) 0.149(7) 0.114(7) 0.049(6) 0.017(5) -0.005(6) N1 0.046(3) 0.087(5) 0.076(4) -0.005(3) 0.023(3) 0.007(3) N2 0.082(4) 0.057(4) 0.098(5) -0.012(3) 0.059(4) 0.006(3) N3 0.090(6) 0.148(7) 0.112(7) 0.048(6) 0.019(5) -0.002(6) C1 0.038(3) 0.020(2) 0.044(3) 0.003(2) 0.027(3) 0.003(2) C2 0.034(3) 0.030(3) 0.053(3) -0.005(2) 0.025(3) 0.002(2) C3 0.038(3) 0.046(3) 0.048(3) -0.009(3) 0.021(3) 0.008(2) C4 0.038(3) 0.058(4) 0.071(4) -0.016(3) 0.028(3) 0.011(3) C5 0.048(4) 0.061(4) 0.072(4) -0.019(3) 0.035(3) 0.011(3) C6 0.050(4) 0.100(6) 0.078(5) -0.044(4) 0.028(4) 0.008(4) C7 0.044(3) 0.077(5) 0.069(4) -0.032(4) 0.024(3) 0.008(3) C8 0.054(4) 0.075(5) 0.072(4) -0.020(4) 0.039(4) 0.010(3) C9 0.056(4) 0.070(5) 0.075(5) -0.032(4) 0.032(4) 0.001(3) C10 0.048(4) 0.070(4) 0.058(4) -0.022(3) 0.030(3) 0.009(3) C11 0.048(4) 0.062(4) 0.064(4) -0.030(3) 0.022(3) 0.006(3) C12 0.039(3) 0.061(4) 0.062(4) -0.020(3) 0.022(3) 0.005(3) C13 0.035(3) 0.046(3) 0.038(3) -0.010(2) 0.017(2) 0.006(2) C14 0.040(3) 0.057(4) 0.041(3) -0.018(3) 0.020(3) 0.000(3) C15 0.043(3) 0.067(4) 0.064(4) -0.018(3) 0.032(3) 0.002(3) C16 0.036(3) 0.039(3) 0.037(3) -0.003(2) 0.018(2) 0.005(2) C17 0.038(3) 0.017(2) 0.036(3) 0.003(2) 0.020(2) 0.001(2) C18 0.037(3) 0.019(2) 0.036(3) 0.002(2) 0.013(2) -0.002(2) C19 0.037(3) 0.023(3) 0.058(4) 0.001(2) 0.010(3) 0.001(2) C20 0.048(3) 0.023(3) 0.056(3) -0.001(2) 0.009(3) -0.006(2) C21 0.055(3) 0.019(3) 0.040(3) -0.002(2) 0.016(3) -0.001(2) C22 0.043(3) 0.024(3) 0.054(3) 0.006(2) 0.011(3) 0.006(2) C23 0.046(3) 0.019(3) 0.048(3) 0.000(2) 0.020(3) -0.001(2) C24 0.054(3) 0.024(2) 0.042(3) 0.001(2) 0.015(3) 0.003(2) C25 0.049(4) 0.067(5) 0.066(4) -0.010(4) 0.029(3) -0.005(3) C26 0.069(6) 0.107(7) 0.125(8) 0.005(6) 0.038(6) 0.030(5) C27 0.068(6) 0.131(9) 0.185(11) 0.062(8) 0.073(7) 0.008(6) C28 0.057(4) 0.051(4) 0.067(4) -0.009(3) 0.033(3) 0.007(3) C29 0.105(7) 0.086(6) 0.110(7) 0.015(5) 0.072(6) 0.049(5) C30 0.094(6) 0.104(7) 0.128(8) -0.070(6) 0.070(6) -0.044(5) C33 0.090(6) 0.149(8) 0.112(7) 0.048(6) 0.020(5) -0.003(6) C32 0.090(6) 0.148(8) 0.112(7) 0.047(6) 0.020(5) 0.000(6) C31 0.089(6) 0.148(7) 0.112(7) 0.048(6) 0.019(5) -0.002(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O5 2.021(3) . ? Co1 O1 2.042(3) . ? Co1 O7 2.050(4) . ? Co1 O4 2.127(3) 4_665 ? Co1 O8 2.157(4) . ? Co1 O3 2.218(4) 4_665 ? Co1 C16 2.511(5) 4_665 ? Co2 O6 2.062(3) . ? Co2 O6 2.062(3) 3_755 ? Co2 O2 2.067(3) . ? Co2 O2 2.067(3) 3_755 ? Co2 O4 2.139(3) 2_645 ? Co2 O4 2.139(3) 4_665 ? O1 C1 1.256(6) . ? O2 C1 1.252(6) . ? O3 C16 1.250(6) . ? O3 Co1 2.218(4) 4_566 ? O4 C16 1.282(6) . ? O4 Co1 2.127(3) 4_566 ? O4 Co2 2.139(3) 2_655 ? O5 C17 1.260(6) . ? O6 C17 1.249(6) . ? O7 C25 1.231(8) . ? O8 C28 1.240(7) . ? O9 C31 1.118(14) . ? O10 C34 1.147(12) . ? N1 C25 1.327(8) . ? N1 C27 1.406(11) . ? N1 C26 1.477(10) . ? N2 C28 1.341(8) . ? N2 C29 1.400(8) . ? N2 C30 1.435(9) . ? N3 C31 1.368(19) . ? N3 C33 1.381(14) . ? N3 C32 1.386(13) . ? N4 C34 1.303(14) . ? N4 C36 1.358(11) . ? N4 C35 1.440(11) . ? C1 C2 1.515(7) . ? C2 C7 1.363(8) . ? C2 C3 1.374(7) . ? C3 C4 1.384(7) . ? C4 C5 1.405(9) . ? C5 C6 1.370(9) . ? C5 C8 1.430(8) . ? C6 C7 1.403(9) . ? C8 C9 1.192(8) . ? C9 C10 1.446(8) . ? C10 C15 1.388(9) . ? C10 C11 1.402(9) . ? C11 C12 1.384(8) . ? C12 C13 1.388(8) . ? C13 C14 1.374(8) . ? C13 C16 1.489(7) . ? C14 C15 1.382(8) . ? C16 Co1 2.511(5) 4_566 ? C17 C18 1.516(6) . ? C18 C19 1.381(7) . ? C18 C23 1.402(7) . ? C19 C20 1.381(7) . ? C20 C21 1.379(8) . ? C21 C22 1.407(7) . ? C21 C24 1.437(7) . ? C22 C23 1.383(7) . ? C24 C24 1.205(11) 3_745 ? 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 Co1 O1 95.45(14) . . ? O5 Co1 O7 101.01(14) . . ? O1 Co1 O7 87.17(14) . . ? O5 Co1 O4 97.93(13) . 4_665 ? O1 Co1 O4 96.26(13) . 4_665 ? O7 Co1 O4 160.34(14) . 4_665 ? O5 Co1 O8 86.74(16) . . ? O1 Co1 O8 175.15(14) . . ? O7 Co1 O8 88.16(15) . . ? O4 Co1 O8 87.70(14) 4_665 . ? O5 Co1 O3 158.40(14) . 4_665 ? O1 Co1 O3 86.18(15) . 4_665 ? O7 Co1 O3 100.58(14) . 4_665 ? O4 Co1 O3 60.51(13) 4_665 4_665 ? O8 Co1 O3 93.37(17) . 4_665 ? O5 Co1 C16 128.60(15) . 4_665 ? O1 Co1 C16 91.24(16) . 4_665 ? O7 Co1 C16 130.24(16) . 4_665 ? O4 Co1 C16 30.68(14) 4_665 4_665 ? O8 Co1 C16 90.76(17) . 4_665 ? O3 Co1 C16 29.83(15) 4_665 4_665 ? O6 Co2 O6 180.0(2) . 3_755 ? O6 Co2 O2 95.10(13) . . ? O6 Co2 O2 84.90(13) 3_755 . ? O6 Co2 O2 84.90(13) . 3_755 ? O6 Co2 O2 95.10(13) 3_755 3_755 ? O2 Co2 O2 180.0(2) . 3_755 ? O6 Co2 O4 90.60(12) . 2_645 ? O6 Co2 O4 89.40(12) 3_755 2_645 ? O2 Co2 O4 86.40(13) . 2_645 ? O2 Co2 O4 93.60(13) 3_755 2_645 ? O6 Co2 O4 89.40(12) . 4_665 ? O6 Co2 O4 90.60(12) 3_755 4_665 ? O2 Co2 O4 93.60(13) . 4_665 ? O2 Co2 O4 86.40(13) 3_755 4_665 ? O4 Co2 O4 180.00(11) 2_645 4_665 ? C1 O1 Co1 126.2(3) . . ? C1 O2 Co2 138.1(3) . . ? C16 O3 Co1 88.2(3) . 4_566 ? C16 O4 Co1 91.5(3) . 4_566 ? C16 O4 Co2 132.4(3) . 2_655 ? Co1 O4 Co2 110.08(14) 4_566 2_655 ? C17 O5 Co1 126.9(3) . . ? C17 O6 Co2 132.3(3) . . ? C25 O7 Co1 117.0(4) . . ? C28 O8 Co1 117.7(4) . . ? C25 N1 C27 121.6(7) . . ? C25 N1 C26 122.2(7) . . ? C27 N1 C26 115.8(7) . . ? C28 N2 C29 121.9(7) . . ? C28 N2 C30 121.8(6) . . ? C29 N2 C30 115.7(7) . . ? C31 N3 C33 126.5(13) . . ? C31 N3 C32 114.4(13) . . ? C33 N3 C32 119.0(14) . . ? C34 N4 C36 136.1(11) . . ? C34 N4 C35 111.1(10) . . ? C36 N4 C35 112.8(10) . . ? O2 C1 O1 127.8(4) . . ? O2 C1 C2 116.3(4) . . ? O1 C1 C2 115.9(4) . . ? C7 C2 C3 119.4(5) . . ? C7 C2 C1 120.0(5) . . ? C3 C2 C1 120.6(5) . . ? C2 C3 C4 121.2(5) . . ? C3 C4 C5 119.7(5) . . ? C6 C5 C4 118.6(5) . . ? C6 C5 C8 122.3(6) . . ? C4 C5 C8 119.1(5) . . ? C5 C6 C7 120.8(6) . . ? C2 C7 C6 120.3(6) . . ? C9 C8 C5 176.9(8) . . ? C8 C9 C10 177.4(7) . . ? C15 C10 C11 118.9(5) . . ? C15 C10 C9 120.7(6) . . ? C11 C10 C9 120.4(6) . . ? C12 C11 C10 119.7(6) . . ? C11 C12 C13 120.7(6) . . ? C14 C13 C12 119.4(5) . . ? C14 C13 C16 121.4(5) . . ? C12 C13 C16 119.2(5) . . ? C13 C14 C15 120.7(5) . . ? C14 C15 C10 120.4(6) . . ? O3 C16 O4 119.8(4) . . ? O3 C16 C13 121.1(5) . . ? O4 C16 C13 119.1(4) . . ? O3 C16 Co1 62.0(3) . 4_566 ? O4 C16 Co1 57.8(2) . 4_566 ? C13 C16 Co1 176.6(4) . 4_566 ? O6 C17 O5 127.2(4) . . ? O6 C17 C18 116.8(4) . . ? O5 C17 C18 115.9(4) . . ? C19 C18 C23 118.9(4) . . ? C19 C18 C17 120.2(4) . . ? C23 C18 C17 120.7(4) . . ? C18 C19 C20 121.0(5) . . ? C21 C20 C19 120.2(5) . . ? C20 C21 C22 119.8(5) . . ? C20 C21 C24 119.6(5) . . ? C22 C21 C24 120.6(5) . . ? C23 C22 C21 119.4(5) . . ? C22 C23 C18 120.6(5) . . ? C24 C24 C21 178.0(8) 3_745 . ? O7 C25 N1 124.1(7) . . ? O8 C28 N2 125.8(6) . . ? O10 C34 N4 122.3(13) . . ? O9 C31 N3 130.1(17) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.60 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.566 _refine_diff_density_min -1.049 _refine_diff_density_rms 0.118 #===end