data_global #------------------ AUTHOR DETAILS -------------------------------------------# # Name and address of author for correspondence _publ_contact_author ; 'Radovanovi\'c, Lidija' Innovation Centre, Faculty of Technology and Metallurgy University of Belgrade Karnegijeva 4 11000 Belgrade Serbia ; _publ_contact_author_phone '+381 11 3303 784' _publ_contact_author_fax '+381 11 3370 387' _publ_contact_author_email 'lradovanovic@tmf.bg.ac.rs' _publ_requested_journal '' _publ_contact_letter ; The manuscript will be submited for publication in the Zeitschrift für Anorganische und Allgemeine Chemie. Could you, please, assign CCDC reference number for the structure included. ; # TITLE AND AUTHOR LIST _publ_section_title ; Diaquabis(2,2'-dipyridylamine)M(II) terephthalate dihydrates, M(II) = Ni, Co: synthesis, crystal structures, thermal and magnetic properties ; loop_ _publ_author_name _publ_author_address 'Radovanovi\'c, Lidija' ; Innovation Centre, Faculty of Technology and Metallurgy University of Belgrade Karnegijeva 4 11000 Belgrade Serbia ; 'Rogan, Jelena' ; Department of General and Inorganic Chemistry Faculty of Technology and Metallurgy University of Belgrade Karnegijeva 4 11000 Belgrade Serbia ; 'Poleti, Dejan' ; Department of General and Inorganic Chemistry Faculty of Technology and Metallurgy University of Belgrade Karnegijeva 4 11000 Belgrade Serbia ; 'Rodi\'c, Marko' ; Faculty of Sciences University of Novi Sad Trg Dositeja Obradovi\'ca 3 21000 Novi Sad Serbia ; 'Jagli\ 2\s(I)' _computing_data_collection 'CrysAlisPro' _computing_cell_refinement 'CrysAlisPro' _computing_data_reduction 'CrysAlisPro' _computing_structure_solution 'SIR-2014' _computing_structure_refinement 'SHELXL-2014/7' _computing_molecular_graphics 'Mercury' _computing_publication_material 'WinGX' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0341P)^2^+1.9123P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary direct _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5603 _refine_ls_number_parameters 420 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0478 _refine_ls_R_factor_gt 0.0395 _refine_ls_wR_factor_ref 0.092 _refine_ls_wR_factor_gt 0.0882 _refine_ls_goodness_of_fit_ref 1.121 _refine_ls_restrained_S_all 1.121 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1188(3) 0.2175(3) 0.18008(9) 0.0419(6) Uani 1 1 d . . . . . H1 H 0.0338 0.2514 0.1862 0.05 Uiso 1 1 calc R U . . . C2 C 0.1585(3) 0.0915(3) 0.19574(10) 0.0517(7) Uani 1 1 d . . . . . H2 H 0.1019 0.0405 0.212 0.062 Uiso 1 1 calc R U . . . C3 C 0.2852(3) 0.0410(3) 0.18685(11) 0.0539(8) Uani 1 1 d . . . . . H3 H 0.3141 -0.0457 0.1966 0.065 Uiso 1 1 calc R U . . . C4 C 0.3677(3) 0.1195(3) 0.16367(9) 0.0444(6) Uani 1 1 d . . . . . H4 H 0.4534 0.0871 0.1576 0.053 Uiso 1 1 calc R U . . . C5 C 0.3215(2) 0.2485(2) 0.14930(8) 0.0312(5) Uani 1 1 d . . . . . C6 C 0.4209(2) 0.4686(2) 0.12771(7) 0.0289(5) Uani 1 1 d . . . . . C7 C 0.5488(2) 0.5252(3) 0.11987(8) 0.0388(6) Uani 1 1 d . . . . . H7 H 0.6191 0.47 0.1116 0.047 Uiso 1 1 calc R U . . . C8 C 0.5676(3) 0.6625(3) 0.12469(9) 0.0444(7) Uani 1 1 d . . . . . H8 H 0.651 0.7021 0.1194 0.053 Uiso 1 1 calc R U . . . C9 C 0.4623(3) 0.7430(3) 0.13741(9) 0.0423(6) Uani 1 1 d . . . . . H9 H 0.4755 0.8359 0.1426 0.051 Uiso 1 1 calc R U . . . C10 C 0.3382(3) 0.6820(3) 0.14208(8) 0.0353(6) Uani 1 1 d . . . . . H10 H 0.2665 0.7363 0.1498 0.042 Uiso 1 1 calc R U . . . C11 C 0.1532(3) 0.2744(3) 0.05476(9) 0.0383(6) Uani 1 1 d . . . . . H11 H 0.1196 0.2142 0.0746 0.046 Uiso 1 1 calc R U . . . C12 C 0.2138(3) 0.2206(3) 0.02039(9) 0.0488(7) Uani 1 1 d . . . . . H12 H 0.2225 0.1267 0.0172 0.059 Uiso 1 1 calc R U . . . C13 C 0.2616(3) 0.3095(3) -0.00936(10) 0.0525(8) Uani 1 1 d . . . . . H13 H 0.306 0.2761 -0.0326 0.063 Uiso 1 1 calc R U . . . C14 C 0.2438(3) 0.4460(3) -0.00473(9) 0.0447(7) Uani 1 1 d . . . . . H14 H 0.2733 0.5068 -0.0252 0.054 Uiso 1 1 calc R U . . . C15 C 0.1800(2) 0.4945(2) 0.03138(8) 0.0294(5) Uani 1 1 d . . . . . C16 C 0.0860(2) 0.7110(2) 0.06045(8) 0.0286(5) Uani 1 1 d . . . . . C17 C 0.0625(3) 0.8480(3) 0.04830(9) 0.0392(6) Uani 1 1 d . . . . . H17 H 0.101 0.8842 0.0243 0.047 Uiso 1 1 calc R U . . . C18 C -0.0168(3) 0.9276(3) 0.07171(10) 0.0479(7) Uani 1 1 d . . . . . H18 H -0.0328 1.0186 0.064 0.058 Uiso 1 1 calc R U . . . C19 C -0.0735(3) 0.8710(3) 0.10731(10) 0.0485(7) Uani 1 1 d . . . . . H19 H -0.1302 0.9225 0.1234 0.058 Uiso 1 1 calc R U . . . C20 C -0.0442(3) 0.7384(3) 0.11798(9) 0.0396(6) Uani 1 1 d . . . . . H20 H -0.082 0.7012 0.142 0.048 Uiso 1 1 calc R U . . . C21 C 0.2415(2) 0.4421(3) 0.28883(8) 0.0365(6) Uani 1 1 d . . . . . C22 C 0.3755(2) 0.4428(3) 0.26825(7) 0.0329(5) Uani 1 1 d . . . . . C23 C 0.4375(3) 0.5646(3) 0.25871(9) 0.0403(6) Uani 1 1 d . . . . . H23 H 0.395 0.647 0.2641 0.048 Uiso 1 1 calc R U . . . C24 C 0.4386(3) 0.3210(3) 0.25949(9) 0.0398(6) Uani 1 1 d . . . . . H24 H 0.3986 0.2387 0.2663 0.048 Uiso 1 1 calc R U . . . C25 C 0.3246(2) 0.8170(2) -0.05849(8) 0.0298(5) Uani 1 1 d . . . . . C26 C 0.4146(2) 0.9109(2) -0.02768(8) 0.0285(5) Uani 1 1 d . . . . . C27 C 0.4285(3) 0.8970(3) 0.01823(8) 0.0352(6) Uani 1 1 d . . . . . H27 H 0.3807 0.828 0.0308 0.042 Uiso 1 1 calc R U . . . C28 C 0.4873(3) 1.0154(3) -0.04539(8) 0.0356(6) Uani 1 1 d . . . . . H28 H 0.4792 1.0264 -0.0761 0.043 Uiso 1 1 calc R U . . . N1 N 0.1963(2) 0.2962(2) 0.15606(6) 0.0311(4) Uani 1 1 d . . . . . N2 N 0.31446(19) 0.54721(19) 0.13612(6) 0.0276(4) Uani 1 1 d . . . . . N3 N 0.4081(2) 0.3283(2) 0.12684(7) 0.0333(5) Uani 1 1 d . . . . . H3A H 0.4597 0.2853 0.1105 0.04 Uiso 1 1 calc R U . . . N4 N 0.13893(19) 0.40975(19) 0.06173(6) 0.0283(4) Uani 1 1 d . . . . . N5 N 0.03677(18) 0.6569(2) 0.09586(6) 0.0282(4) Uani 1 1 d . . . . . N6 N 0.1633(2) 0.6336(2) 0.03460(7) 0.0336(5) Uani 1 1 d . . . . . H6 H 0.2092 0.6805 0.0174 0.04 Uiso 1 1 calc R U . . . O1 O -0.09179(18) 0.3958(2) 0.11718(7) 0.0371(4) Uani 1 1 d . . . . . O2 O 0.0745(2) 0.5445(2) 0.18758(6) 0.0387(4) Uani 1 1 d . . . . . O3 O 0.20888(19) 0.3368(2) 0.30790(6) 0.0468(5) Uani 1 1 d . . . . . O4 O 0.17106(19) 0.5507(2) 0.28560(7) 0.0544(6) Uani 1 1 d . . . . . O5 O 0.22310(19) 0.75933(19) -0.04404(6) 0.0446(5) Uani 1 1 d . . . . . O6 O 0.35401(19) 0.8030(2) -0.09711(6) 0.0503(5) Uani 1 1 d . . . . . O7 O 0.1432(4) -0.1661(3) 0.26815(13) 0.1012(11) Uani 1 1 d . . . . . O8A O 0.2591(13) 0.0628(12) 0.3203(4) 0.081(2) Uani 0.599(17) 1 d D . P . . O8B O 0.3032(18) 0.0135(16) 0.3241(6) 0.081(2) Uani 0.401(17) 1 d D . P . . Ni1 Ni 0.10996(3) 0.47314(3) 0.12572(2) 0.02543(9) Uani 1 1 d . . . . . H30 H -0.130(3) 0.371(3) 0.1399(11) 0.060(10) Uiso 1 1 d . . . . . H29 H -0.123(3) 0.345(3) 0.0976(12) 0.062(11) Uiso 1 1 d . . . . . H31 H -0.003(4) 0.543(3) 0.1950(11) 0.065(11) Uiso 1 1 d . . . . . H32 H 0.128(4) 0.538(4) 0.2072(13) 0.079(14) Uiso 1 1 d . . . . . H35 H 0.242(4) -0.015(3) 0.3055(13) 0.118 Uiso 1 1 d D U . . . H36 H 0.304(5) 0.071(4) 0.3454(9) 0.118 Uiso 1 1 d D U . . . H34 H 0.143(5) -0.210(5) 0.2420(17) 0.118 Uiso 1 1 d . U . . . H33 H 0.164(5) -0.245(5) 0.2802(16) 0.118 Uiso 1 1 d . U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0380(14) 0.0450(15) 0.0448(15) 0.0110(12) 0.0129(12) -0.0023(12) C2 0.0562(18) 0.0439(16) 0.0576(19) 0.0148(14) 0.0175(14) -0.0059(14) C3 0.069(2) 0.0322(14) 0.0607(19) 0.0077(14) 0.0100(16) 0.0054(14) C4 0.0479(16) 0.0348(14) 0.0513(17) -0.0032(12) 0.0095(13) 0.0063(12) C5 0.0331(12) 0.0318(12) 0.0288(12) -0.0045(10) 0.0046(10) -0.0021(10) C6 0.0269(11) 0.0368(13) 0.0229(11) 0.0009(10) 0.0035(9) 0.0001(10) C7 0.0239(12) 0.0539(16) 0.0396(14) 0.0051(13) 0.0082(10) -0.0007(12) C8 0.0293(13) 0.0553(17) 0.0494(16) 0.0099(14) 0.0079(11) -0.0135(12) C9 0.0396(14) 0.0374(14) 0.0492(16) 0.0020(12) 0.0033(12) -0.0113(12) C10 0.0325(13) 0.0355(13) 0.0375(14) -0.0025(11) 0.0031(10) -0.0025(11) C11 0.0456(15) 0.0315(13) 0.0359(14) -0.0027(11) -0.0025(11) -0.0030(12) C12 0.0613(18) 0.0380(15) 0.0441(16) -0.0109(13) -0.0041(14) 0.0101(14) C13 0.0573(18) 0.0604(19) 0.0411(16) -0.0108(14) 0.0107(14) 0.0146(15) C14 0.0504(16) 0.0529(17) 0.0335(14) -0.0001(12) 0.0160(12) 0.0034(13) C15 0.0260(11) 0.0335(13) 0.0284(12) -0.0007(10) 0.0025(9) -0.0017(10) C16 0.0250(11) 0.0316(12) 0.0293(12) -0.0003(10) 0.0034(9) -0.0035(10) C17 0.0415(14) 0.0344(13) 0.0420(15) 0.0066(11) 0.0061(11) -0.0062(12) C18 0.0521(17) 0.0304(13) 0.0608(19) -0.0003(13) 0.0053(14) 0.0050(13) C19 0.0468(16) 0.0453(16) 0.0547(18) -0.0073(14) 0.0117(13) 0.0118(13) C20 0.0346(13) 0.0473(15) 0.0391(14) 0.0015(12) 0.0126(11) 0.0059(12) C21 0.0287(12) 0.0558(17) 0.0261(12) 0.0024(11) 0.0073(10) 0.0011(12) C22 0.0270(12) 0.0509(15) 0.0216(11) 0.0022(10) 0.0061(9) 0.0006(11) C23 0.0376(14) 0.0480(15) 0.0380(14) -0.0010(12) 0.0152(11) 0.0042(12) C24 0.0368(13) 0.0491(16) 0.0358(14) 0.0028(12) 0.0137(11) -0.0039(12) C25 0.0307(12) 0.0284(12) 0.0304(13) -0.0025(10) 0.0048(10) -0.0001(10) C26 0.0277(11) 0.0295(12) 0.0286(12) -0.0020(10) 0.0053(9) -0.0005(10) C27 0.0378(13) 0.0355(13) 0.0336(13) 0.0022(11) 0.0091(10) -0.0115(11) C28 0.0405(13) 0.0411(14) 0.0257(12) 0.0012(11) 0.0058(10) -0.0087(12) N1 0.0311(10) 0.0345(11) 0.0288(10) 0.0046(8) 0.0076(8) -0.0010(9) N2 0.0244(9) 0.0329(11) 0.0259(10) -0.0017(8) 0.0049(7) -0.0011(8) N3 0.0293(10) 0.0364(11) 0.0359(11) -0.0033(9) 0.0110(9) 0.0024(9) N4 0.0271(10) 0.0294(10) 0.0282(10) -0.0007(8) 0.0031(8) -0.0043(8) N5 0.0241(9) 0.0341(10) 0.0270(10) 0.0014(8) 0.0060(8) 0.0005(8) N6 0.0390(11) 0.0341(11) 0.0307(11) 0.0033(9) 0.0157(9) -0.0045(9) O1 0.0308(9) 0.0514(12) 0.0304(10) -0.0042(9) 0.0089(8) -0.0168(8) O2 0.0297(10) 0.0594(13) 0.0278(10) -0.0035(9) 0.0069(8) -0.0012(9) O3 0.0453(11) 0.0524(11) 0.0482(11) 0.0058(9) 0.0264(9) -0.0001(9) O4 0.0362(10) 0.0638(13) 0.0675(14) 0.0256(11) 0.0234(9) 0.0137(10) O5 0.0483(11) 0.0535(11) 0.0324(10) -0.0019(8) 0.0068(8) -0.0248(9) O6 0.0446(11) 0.0726(14) 0.0361(10) -0.0214(10) 0.0146(8) -0.0135(10) O7 0.128(3) 0.0515(16) 0.116(3) 0.0140(17) -0.017(2) -0.0103(17) O8A 0.091(6) 0.074(6) 0.078(3) -0.011(4) 0.010(4) -0.029(4) O8B 0.091(6) 0.074(6) 0.078(3) -0.011(4) 0.010(4) -0.029(4) Ni1 0.02177(15) 0.03066(16) 0.02472(15) 0.00133(12) 0.00629(11) -0.00261(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.353(3) . ? C1 C2 1.360(4) . ? C1 H1 0.93 . ? C2 C3 1.384(4) . ? C2 H2 0.93 . ? C3 C4 1.368(4) . ? C3 H3 0.93 . ? C4 C5 1.392(3) . ? C4 H4 0.93 . ? C5 N1 1.343(3) . ? C5 N3 1.389(3) . ? C6 N2 1.339(3) . ? C6 N3 1.380(3) . ? C6 C7 1.408(3) . ? C7 C8 1.362(4) . ? C7 H7 0.93 . ? C8 C9 1.384(4) . ? C8 H8 0.93 . ? C9 C10 1.368(3) . ? C9 H9 0.93 . ? C10 N2 1.348(3) . ? C10 H10 0.93 . ? C11 N4 1.353(3) . ? C11 C12 1.366(4) . ? C11 H11 0.93 . ? C12 C13 1.377(4) . ? C12 H12 0.93 . ? C13 C14 1.358(4) . ? C13 H13 0.93 . ? C14 C15 1.407(3) . ? C14 H14 0.93 . ? C15 N4 1.337(3) . ? C15 N6 1.377(3) . ? C16 N5 1.339(3) . ? C16 N6 1.380(3) . ? C16 C17 1.402(3) . ? C17 C18 1.358(4) . ? C17 H17 0.93 . ? C18 C19 1.388(4) . ? C18 H18 0.93 . ? C19 C20 1.359(4) . ? C19 H19 0.93 . ? C20 N5 1.356(3) . ? C20 H20 0.93 . ? C21 O3 1.243(3) . ? C21 O4 1.261(3) . ? C21 C22 1.514(3) . ? C22 C24 1.381(4) . ? C22 C23 1.384(4) . ? C23 C23 1.383(5) 2_655 ? C23 H23 0.93 . ? C24 C24 1.389(5) 2_655 ? C24 H24 0.93 . ? C25 O6 1.248(3) . ? C25 O5 1.262(3) . ? C25 C26 1.507(3) . ? C26 C27 1.387(3) . ? C26 C28 1.389(3) . ? C27 C28 1.381(3) 3_675 ? C27 H27 0.93 . ? C28 C27 1.381(3) 3_675 ? C28 H28 0.93 . ? N1 Ni1 2.086(2) . ? N2 Ni1 2.0984(19) . ? N3 H3A 0.86 . ? N4 Ni1 2.0893(19) . ? N5 Ni1 2.0972(19) . ? N6 H6 0.86 . ? O1 Ni1 2.0843(17) . ? O1 H30 0.86(3) . ? O1 H29 0.80(3) . ? O2 Ni1 2.0703(19) . ? O2 H31 0.82(4) . ? O2 H32 0.74(4) . ? O7 H34 0.90(5) . ? O7 H33 0.87(5) . ? O8A O8B 0.646(14) . ? O8A H35 0.891(19) . ? O8A H36 0.830(19) . ? O8B H35 0.817(19) . ? O8B H36 0.855(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 123.6(2) . . ? N1 C1 H1 118.2 . . ? C2 C1 H1 118.2 . . ? C1 C2 C3 118.4(3) . . ? C1 C2 H2 120.8 . . ? C3 C2 H2 120.8 . . ? C4 C3 C2 119.5(3) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C3 C4 C5 119.0(3) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? N1 C5 N3 119.7(2) . . ? N1 C5 C4 122.0(2) . . ? N3 C5 C4 118.3(2) . . ? N2 C6 N3 120.4(2) . . ? N2 C6 C7 121.6(2) . . ? N3 C6 C7 117.9(2) . . ? C8 C7 C6 118.6(2) . . ? C8 C7 H7 120.7 . . ? C6 C7 H7 120.7 . . ? C7 C8 C9 119.9(2) . . ? C7 C8 H8 120 . . ? C9 C8 H8 120 . . ? C10 C9 C8 118.1(2) . . ? C10 C9 H9 120.9 . . ? C8 C9 H9 120.9 . . ? N2 C10 C9 123.5(2) . . ? N2 C10 H10 118.3 . . ? C9 C10 H10 118.3 . . ? N4 C11 C12 124.0(2) . . ? N4 C11 H11 118 . . ? C12 C11 H11 118 . . ? C11 C12 C13 118.1(3) . . ? C11 C12 H12 121 . . ? C13 C12 H12 121 . . ? C14 C13 C12 119.8(3) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C13 C14 C15 119.1(3) . . ? C13 C14 H14 120.4 . . ? C15 C14 H14 120.4 . . ? N4 C15 N6 121.1(2) . . ? N4 C15 C14 121.7(2) . . ? N6 C15 C14 117.1(2) . . ? N5 C16 N6 120.9(2) . . ? N5 C16 C17 121.8(2) . . ? N6 C16 C17 117.3(2) . . ? C18 C17 C16 119.7(2) . . ? C18 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? C17 C18 C19 119.0(3) . . ? C17 C18 H18 120.5 . . ? C19 C18 H18 120.5 . . ? C20 C19 C18 118.3(2) . . ? C20 C19 H19 120.8 . . ? C18 C19 H19 120.8 . . ? N5 C20 C19 124.1(2) . . ? N5 C20 H20 117.9 . . ? C19 C20 H20 117.9 . . ? O3 C21 O4 124.6(2) . . ? O3 C21 C22 118.6(2) . . ? O4 C21 C22 116.8(2) . . ? C24 C22 C23 119.3(2) . . ? C24 C22 C21 120.1(2) . . ? C23 C22 C21 120.6(2) . . ? C23 C23 C22 120.39(14) 2_655 . ? C23 C23 H23 119.8 2_655 . ? C22 C23 H23 119.8 . . ? C22 C24 C24 120.32(14) . 2_655 ? C22 C24 H24 119.8 . . ? C24 C24 H24 119.8 2_655 . ? O6 C25 O5 124.0(2) . . ? O6 C25 C26 117.6(2) . . ? O5 C25 C26 118.3(2) . . ? C27 C26 C28 118.1(2) . . ? C27 C26 C25 122.3(2) . . ? C28 C26 C25 119.5(2) . . ? C28 C27 C26 120.7(2) 3_675 . ? C28 C27 H27 119.7 3_675 . ? C26 C27 H27 119.7 . . ? C27 C28 C26 121.2(2) 3_675 . ? C27 C28 H28 119.4 3_675 . ? C26 C28 H28 119.4 . . ? C5 N1 C1 117.4(2) . . ? C5 N1 Ni1 122.83(15) . . ? C1 N1 Ni1 119.40(16) . . ? C6 N2 C10 117.7(2) . . ? C6 N2 Ni1 120.71(15) . . ? C10 N2 Ni1 120.05(15) . . ? C6 N3 C5 127.63(19) . . ? C6 N3 H3A 116.2 . . ? C5 N3 H3A 116.2 . . ? C15 N4 C11 117.1(2) . . ? C15 N4 Ni1 122.81(15) . . ? C11 N4 Ni1 117.71(16) . . ? C16 N5 C20 116.9(2) . . ? C16 N5 Ni1 123.33(15) . . ? C20 N5 Ni1 118.51(16) . . ? C15 N6 C16 131.45(19) . . ? C15 N6 H6 114.3 . . ? C16 N6 H6 114.3 . . ? Ni1 O1 H30 120(2) . . ? Ni1 O1 H29 125(2) . . ? H30 O1 H29 105(3) . . ? Ni1 O2 H31 121(2) . . ? Ni1 O2 H32 121(3) . . ? H31 O2 H32 111(4) . . ? H34 O7 H33 85(4) . . ? O8B O8A H35 62(2) . . ? O8B O8A H36 70(2) . . ? H35 O8A H36 126(3) . . ? O8A O8B H35 74(2) . . ? O8A O8B H36 65(2) . . ? H35 O8B H36 133(4) . . ? O2 Ni1 O1 88.39(8) . . ? O2 Ni1 N1 89.16(8) . . ? O1 Ni1 N1 94.01(8) . . ? O2 Ni1 N4 176.89(8) . . ? O1 Ni1 N4 90.78(8) . . ? N1 Ni1 N4 93.88(8) . . ? O2 Ni1 N5 90.82(8) . . ? O1 Ni1 N5 89.90(8) . . ? N1 Ni1 N5 176.08(7) . . ? N4 Ni1 N5 86.18(7) . . ? O2 Ni1 N2 90.68(8) . . ? O1 Ni1 N2 178.19(8) . . ? N1 Ni1 N2 84.42(8) . . ? N4 Ni1 N2 90.23(8) . . ? N5 Ni1 N2 91.66(7) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.529 _refine_diff_density_min -0.382 _refine_diff_density_rms 0.048 #-----------------------------------------------------------------------------# data_2 _audit_creation_method 'WinGX routine CIF_UPDATE' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H22 Co N6 O2, C8 H4 O4, 2(H2 O)' _chemical_formula_sum 'C28 H30 Co N6 O8' _chemical_formula_weight 637.51 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 0 '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 0.006 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2/c' _symmetry_space_group_name_Hall '-P 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 9.7461(19) _cell_length_b 9.797(2) _cell_length_c 30.287(6) _cell_angle_alpha 90 _cell_angle_beta 97.40(3) _cell_angle_gamma 90 _cell_volume 2867.9(10) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 16802 _cell_measurement_theta_min 3.1160 _cell_measurement_theta_max 28.9080 _exptl_crystal_description 'block' _exptl_crystal_colour orange _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.477 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1324 _exptl_absorpt_coefficient_mu 0.659 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.99092 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.3280 _diffrn_standards_number 0 _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_decay_% ? _diffrn_reflns_number 29474 _diffrn_reflns_av_R_equivalents 0.0234 _diffrn_reflns_av_unetI/netI 0.017 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.909 _diffrn_reflns_theta_max 26.019 _reflns_number_total 5630 _reflns_number_gt 5260 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'CrysAlisPro' _computing_cell_refinement 'CrysAlisPro' _computing_data_reduction 'CrysAlisPro' _computing_structure_solution 'SIR-2014' _computing_structure_refinement 'SHELXL-2014/7' _computing_molecular_graphics 'Mercury' _computing_publication_material 'WinGX' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0337P)^2^+1.6366P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary direct _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5630 _refine_ls_number_parameters 420 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0388 _refine_ls_R_factor_gt 0.0354 _refine_ls_wR_factor_ref 0.0851 _refine_ls_wR_factor_gt 0.0833 _refine_ls_goodness_of_fit_ref 1.152 _refine_ls_restrained_S_all 1.153 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1231(2) 0.2134(2) 0.18106(8) 0.0417(5) Uani 1 1 d . . . . . H1 H 0.039 0.2475 0.1876 0.05 Uiso 1 1 calc R U . . . C2 C 0.1626(3) 0.0872(3) 0.19642(9) 0.0512(6) Uani 1 1 d . . . . . H2 H 0.1065 0.036 0.2127 0.061 Uiso 1 1 calc R U . . . C3 C 0.2883(3) 0.0367(2) 0.18718(9) 0.0522(6) Uani 1 1 d . . . . . H3 H 0.3172 -0.05 0.1969 0.063 Uiso 1 1 calc R U . . . C4 C 0.3699(2) 0.1151(2) 0.16363(8) 0.0433(5) Uani 1 1 d . . . . . H4 H 0.4546 0.0825 0.1571 0.052 Uiso 1 1 calc R U . . . C5 C 0.3236(2) 0.2448(2) 0.14961(6) 0.0303(4) Uani 1 1 d . . . . . C6 C 0.42331(19) 0.4644(2) 0.12783(6) 0.0275(4) Uani 1 1 d . . . . . C7 C 0.5509(2) 0.5199(2) 0.11998(7) 0.0374(5) Uani 1 1 d . . . . . H7 H 0.6205 0.4641 0.1117 0.045 Uiso 1 1 calc R U . . . C8 C 0.5710(2) 0.6570(3) 0.12465(8) 0.0443(6) Uani 1 1 d . . . . . H8 H 0.6546 0.6958 0.1195 0.053 Uiso 1 1 calc R U . . . C9 C 0.4662(2) 0.7385(2) 0.13713(8) 0.0426(5) Uani 1 1 d . . . . . H9 H 0.4797 0.8315 0.1421 0.051 Uiso 1 1 calc R U . . . C10 C 0.3426(2) 0.6784(2) 0.14201(7) 0.0351(5) Uani 1 1 d . . . . . H10 H 0.2715 0.7334 0.1496 0.042 Uiso 1 1 calc R U . . . C11 C 0.1570(2) 0.2761(2) 0.05301(7) 0.0377(5) Uani 1 1 d . . . . . H11 H 0.1244 0.215 0.0727 0.045 Uiso 1 1 calc R U . . . C12 C 0.2194(3) 0.2242(2) 0.01891(8) 0.0468(6) Uani 1 1 d . . . . . H12 H 0.2304 0.1306 0.0158 0.056 Uiso 1 1 calc R U . . . C13 C 0.2657(3) 0.3143(3) -0.01075(8) 0.0508(6) Uani 1 1 d . . . . . H13 H 0.3108 0.2823 -0.0339 0.061 Uiso 1 1 calc R U . . . C14 C 0.2450(2) 0.4505(2) -0.00593(7) 0.0443(5) Uani 1 1 d . . . . . H14 H 0.2735 0.5121 -0.0262 0.053 Uiso 1 1 calc R U . . . C15 C 0.18010(19) 0.4970(2) 0.03003(6) 0.0275(4) Uani 1 1 d . . . . . C16 C 0.08521(18) 0.71294(19) 0.05962(6) 0.0266(4) Uani 1 1 d . . . . . C17 C 0.0623(2) 0.8501(2) 0.04739(7) 0.0380(5) Uani 1 1 d . . . . . H17 H 0.1001 0.8859 0.0232 0.046 Uiso 1 1 calc R U . . . C18 C -0.0156(2) 0.9303(2) 0.07115(8) 0.0459(6) Uani 1 1 d . . . . . H18 H -0.0315 1.0213 0.0634 0.055 Uiso 1 1 calc R U . . . C19 C -0.0708(2) 0.8744(2) 0.10712(8) 0.0479(6) Uani 1 1 d . . . . . H19 H -0.1259 0.9265 0.1236 0.057 Uiso 1 1 calc R U . . . C20 C -0.0423(2) 0.7416(2) 0.11767(7) 0.0395(5) Uani 1 1 d . . . . . H20 H -0.0796 0.7045 0.1418 0.047 Uiso 1 1 calc R U . . . C21 C 0.2425(2) 0.4390(2) 0.28855(6) 0.0343(5) Uani 1 1 d . . . . . C22 C 0.37604(19) 0.4389(2) 0.26808(6) 0.0312(4) Uani 1 1 d . . . . . C23 C 0.4375(2) 0.5610(2) 0.25867(7) 0.0378(5) Uani 1 1 d . . . . . H23 H 0.3949 0.6432 0.264 0.045 Uiso 1 1 calc R U . . . C24 C 0.4389(2) 0.3173(2) 0.25941(7) 0.0371(5) Uani 1 1 d . . . . . H24 H 0.399 0.235 0.2662 0.045 Uiso 1 1 calc R U . . . C25 C 0.32394(19) 0.82003(19) -0.05917(6) 0.0280(4) Uani 1 1 d . . . . . C26 C 0.41426(18) 0.91258(19) -0.02798(6) 0.0264(4) Uani 1 1 d . . . . . C27 C 0.4283(2) 0.8967(2) 0.01797(6) 0.0327(4) Uani 1 1 d . . . . . H27 H 0.3805 0.8274 0.0303 0.039 Uiso 1 1 calc R U . . . C28 C 0.4872(2) 1.0170(2) -0.04545(6) 0.0329(4) Uani 1 1 d . . . . . H28 H 0.479 1.029 -0.0761 0.04 Uiso 1 1 calc R U . . . N1 N 0.19963(16) 0.29214(17) 0.15681(5) 0.0314(4) Uani 1 1 d . . . . . N2 N 0.31826(16) 0.54359(16) 0.13638(5) 0.0277(3) Uani 1 1 d . . . . . N3 N 0.40954(16) 0.32437(17) 0.12706(5) 0.0322(4) Uani 1 1 d . . . . . H3A H 0.4605 0.2811 0.1106 0.039 Uiso 1 1 calc R U . . . N4 N 0.13943(16) 0.41083(16) 0.05996(5) 0.0277(3) Uani 1 1 d . . . . . N5 N 0.03716(15) 0.65969(17) 0.09523(5) 0.0287(3) Uani 1 1 d . . . . . N6 N 0.16095(17) 0.63584(17) 0.03333(5) 0.0315(4) Uani 1 1 d . . . . . H6 H 0.2044 0.6833 0.0157 0.038 Uiso 1 1 calc R U . . . O2 O 0.07138(17) 0.54368(18) 0.18843(5) 0.0373(4) Uani 1 1 d . . . . . O1 O -0.09122(15) 0.38815(17) 0.11777(6) 0.0369(4) Uani 1 1 d . . . . . O3 O 0.20933(16) 0.33402(17) 0.30762(5) 0.0451(4) Uani 1 1 d . . . . . O4 O 0.17305(16) 0.54782(17) 0.28510(6) 0.0503(4) Uani 1 1 d . . . . . O5 O 0.22218(16) 0.76333(16) -0.04493(5) 0.0413(4) Uani 1 1 d . . . . . O6 O 0.35314(16) 0.80676(18) -0.09771(5) 0.0472(4) Uani 1 1 d . . . . . O7 O 0.1419(3) 0.8309(3) 0.26852(11) 0.0990(10) Uani 1 1 d . . . . . O8A O 0.2585(9) 0.0593(8) 0.3199(3) 0.0739(16) Uani 0.596(12) 1 d D . P . . O8B O 0.3047(12) 0.0103(12) 0.3238(4) 0.0739(16) Uani 0.404(12) 1 d D . P . . Co1 Co 0.10804(2) 0.47132(3) 0.12586(2) 0.02435(8) Uani 1 1 d . . . . . H29 H -0.126(3) 0.342(3) 0.0973(9) 0.045(7) Uiso 1 1 d . . . . . H30 H -0.130(3) 0.367(3) 0.1390(10) 0.063(9) Uiso 1 1 d . . . . . H31 H -0.008(3) 0.541(3) 0.1963(10) 0.066(9) Uiso 1 1 d . . . . . H32 H 0.122(3) 0.543(3) 0.2087(11) 0.069(10) Uiso 1 1 d . . . . . H35 H 0.303(4) 0.070(3) 0.3443(8) 0.103 Uiso 1 1 d D U . . . H36 H 0.245(3) -0.021(3) 0.3058(11) 0.103 Uiso 1 1 d D U . . . H33 H 0.142(5) 0.797(4) 0.2438(13) 0.103 Uiso 1 1 d . U . . . H34 H 0.164(4) 0.754(4) 0.2786(13) 0.103 Uiso 1 1 d . U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0381(11) 0.0435(13) 0.0458(13) 0.0123(10) 0.0140(10) -0.0014(10) C2 0.0580(15) 0.0425(13) 0.0557(15) 0.0160(12) 0.0166(12) -0.0044(12) C3 0.0674(16) 0.0296(12) 0.0599(16) 0.0075(11) 0.0093(13) 0.0040(11) C4 0.0449(12) 0.0328(12) 0.0529(14) -0.0037(10) 0.0087(10) 0.0076(10) C5 0.0315(10) 0.0309(10) 0.0285(10) -0.0038(8) 0.0035(8) -0.0015(8) C6 0.0241(9) 0.0371(11) 0.0215(9) 0.0014(8) 0.0031(7) -0.0006(8) C7 0.0255(10) 0.0503(13) 0.0376(11) 0.0042(10) 0.0089(8) 0.0001(9) C8 0.0311(11) 0.0554(15) 0.0473(13) 0.0087(11) 0.0081(9) -0.0157(10) C9 0.0418(12) 0.0353(12) 0.0500(13) 0.0036(10) 0.0037(10) -0.0119(10) C10 0.0320(10) 0.0344(11) 0.0386(11) -0.0011(9) 0.0034(8) -0.0015(9) C11 0.0469(12) 0.0297(11) 0.0341(11) -0.0020(9) -0.0035(9) -0.0039(9) C12 0.0593(14) 0.0353(12) 0.0428(13) -0.0111(10) -0.0048(11) 0.0114(11) C13 0.0586(15) 0.0563(15) 0.0392(13) -0.0101(11) 0.0127(11) 0.0164(12) C14 0.0513(13) 0.0497(14) 0.0352(12) 0.0011(10) 0.0183(10) 0.0065(11) C15 0.0250(9) 0.0321(10) 0.0255(9) -0.0011(8) 0.0037(7) 0.0002(8) C16 0.0228(9) 0.0290(10) 0.0276(9) -0.0003(8) 0.0023(7) -0.0029(7) C17 0.0424(12) 0.0317(11) 0.0403(12) 0.0057(9) 0.0072(9) -0.0033(9) C18 0.0508(13) 0.0276(11) 0.0587(15) -0.0012(10) 0.0054(11) 0.0060(10) C19 0.0482(13) 0.0428(13) 0.0544(14) -0.0068(11) 0.0131(11) 0.0139(11) C20 0.0373(11) 0.0464(13) 0.0370(11) 0.0018(10) 0.0130(9) 0.0109(10) C21 0.0281(10) 0.0508(13) 0.0250(10) 0.0016(9) 0.0073(8) 0.0003(9) C22 0.0250(9) 0.0482(12) 0.0209(9) 0.0020(8) 0.0047(7) 0.0007(8) C23 0.0345(11) 0.0427(12) 0.0383(11) 0.0003(9) 0.0128(9) 0.0037(9) C24 0.0347(11) 0.0429(12) 0.0358(11) 0.0032(9) 0.0127(9) -0.0030(9) C25 0.0287(9) 0.0256(9) 0.0298(10) -0.0022(8) 0.0045(8) 0.0007(8) C26 0.0260(9) 0.0260(9) 0.0280(9) -0.0016(7) 0.0059(7) 0.0000(7) C27 0.0369(10) 0.0312(10) 0.0310(10) 0.0035(8) 0.0083(8) -0.0094(9) C28 0.0393(11) 0.0369(11) 0.0231(9) 0.0023(8) 0.0060(8) -0.0078(9) N1 0.0288(8) 0.0341(9) 0.0323(9) 0.0062(7) 0.0082(7) 0.0004(7) N2 0.0243(8) 0.0309(9) 0.0284(8) -0.0007(7) 0.0052(6) -0.0017(6) N3 0.0285(8) 0.0340(9) 0.0361(9) -0.0039(7) 0.0117(7) 0.0025(7) N4 0.0276(8) 0.0288(8) 0.0268(8) -0.0022(7) 0.0035(6) -0.0032(7) N5 0.0244(8) 0.0331(9) 0.0297(8) 0.0020(7) 0.0074(6) 0.0026(7) N6 0.0373(9) 0.0293(9) 0.0306(9) 0.0032(7) 0.0153(7) -0.0035(7) O2 0.0278(8) 0.0582(11) 0.0266(8) -0.0040(7) 0.0065(6) -0.0008(7) O1 0.0305(7) 0.0518(10) 0.0296(8) -0.0043(7) 0.0084(6) -0.0163(7) O3 0.0439(9) 0.0491(9) 0.0472(9) 0.0056(8) 0.0255(7) 0.0002(7) O4 0.0330(8) 0.0578(11) 0.0639(11) 0.0217(8) 0.0207(7) 0.0119(7) O5 0.0463(9) 0.0460(9) 0.0321(8) -0.0011(7) 0.0070(6) -0.0216(7) O6 0.0400(8) 0.0688(11) 0.0354(8) -0.0214(8) 0.0144(7) -0.0126(8) O7 0.129(2) 0.0485(13) 0.110(2) 0.0130(14) -0.0197(19) -0.0134(14) O8A 0.081(4) 0.066(4) 0.075(2) -0.012(3) 0.010(3) -0.024(3) O8B 0.081(4) 0.066(4) 0.075(2) -0.012(3) 0.010(3) -0.024(3) Co1 0.02081(13) 0.02817(14) 0.02497(14) 0.00228(10) 0.00632(9) -0.00147(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.353(3) . ? C1 C2 1.359(3) . ? C1 H1 0.93 . ? C2 C3 1.382(4) . ? C2 H2 0.93 . ? C3 C4 1.370(3) . ? C3 H3 0.93 . ? C4 C5 1.396(3) . ? C4 H4 0.93 . ? C5 N1 1.339(2) . ? C5 N3 1.387(2) . ? C6 N2 1.336(2) . ? C6 N3 1.378(3) . ? C6 C7 1.406(3) . ? C7 C8 1.362(3) . ? C7 H7 0.93 . ? C8 C9 1.387(3) . ? C8 H8 0.93 . ? C9 C10 1.366(3) . ? C9 H9 0.93 . ? C10 N2 1.349(3) . ? C10 H10 0.93 . ? C11 N4 1.351(3) . ? C11 C12 1.363(3) . ? C11 H11 0.93 . ? C12 C13 1.377(4) . ? C12 H12 0.93 . ? C13 C14 1.360(3) . ? C13 H13 0.93 . ? C14 C15 1.404(3) . ? C14 H14 0.93 . ? C15 N4 1.336(2) . ? C15 N6 1.379(2) . ? C16 N5 1.336(2) . ? C16 N6 1.379(2) . ? C16 C17 1.404(3) . ? C17 C18 1.361(3) . ? C17 H17 0.93 . ? C18 C19 1.388(3) . ? C18 H18 0.93 . ? C19 C20 1.361(3) . ? C19 H19 0.93 . ? C20 N5 1.356(3) . ? C20 H20 0.93 . ? C21 O3 1.242(3) . ? C21 O4 1.260(3) . ? C21 C22 1.512(3) . ? C22 C24 1.380(3) . ? C22 C23 1.383(3) . ? C23 C23 1.388(4) 2_655 ? C23 H23 0.93 . ? C24 C24 1.385(4) 2_655 ? C24 H24 0.93 . ? C25 O6 1.243(2) . ? C25 O5 1.260(2) . ? C25 C26 1.508(3) . ? C26 C28 1.388(3) . ? C26 C27 1.390(3) . ? C27 C28 1.382(3) 3_675 ? C27 H27 0.93 . ? C28 C27 1.382(3) 3_675 ? C28 H28 0.93 . ? N1 Co1 2.1313(17) . ? N2 Co1 2.1523(16) . ? N3 H3A 0.86 . ? N4 Co1 2.1413(16) . ? N5 Co1 2.1397(17) . ? N6 H6 0.86 . ? O2 Co1 2.0966(16) . ? O2 H31 0.84(3) . ? O2 H32 0.73(3) . ? O1 Co1 2.0911(15) . ? O1 H29 0.81(3) . ? O1 H30 0.81(3) . ? O7 H33 0.82(4) . ? O7 H34 0.83(4) . ? O8A O8B 0.659(9) . ? O8A H35 0.814(18) . ? O8A H36 0.901(18) . ? O8B H35 0.853(18) . ? O8B H36 0.804(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 123.6(2) . . ? N1 C1 H1 118.2 . . ? C2 C1 H1 118.2 . . ? C1 C2 C3 118.4(2) . . ? C1 C2 H2 120.8 . . ? C3 C2 H2 120.8 . . ? C4 C3 C2 119.6(2) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C3 C4 C5 118.9(2) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? N1 C5 N3 120.02(18) . . ? N1 C5 C4 121.93(19) . . ? N3 C5 C4 118.04(18) . . ? N2 C6 N3 120.38(16) . . ? N2 C6 C7 121.65(19) . . ? N3 C6 C7 117.96(18) . . ? C8 C7 C6 118.8(2) . . ? C8 C7 H7 120.6 . . ? C6 C7 H7 120.6 . . ? C7 C8 C9 119.7(2) . . ? C7 C8 H8 120.2 . . ? C9 C8 H8 120.2 . . ? C10 C9 C8 118.2(2) . . ? C10 C9 H9 120.9 . . ? C8 C9 H9 120.9 . . ? N2 C10 C9 123.5(2) . . ? N2 C10 H10 118.2 . . ? C9 C10 H10 118.2 . . ? N4 C11 C12 124.1(2) . . ? N4 C11 H11 117.9 . . ? C12 C11 H11 117.9 . . ? C11 C12 C13 118.1(2) . . ? C11 C12 H12 121 . . ? C13 C12 H12 121 . . ? C14 C13 C12 119.6(2) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? C13 C14 C15 119.3(2) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? N4 C15 N6 121.30(17) . . ? N4 C15 C14 121.61(19) . . ? N6 C15 C14 117.08(18) . . ? N5 C16 N6 121.45(17) . . ? N5 C16 C17 121.78(18) . . ? N6 C16 C17 116.77(17) . . ? C18 C17 C16 119.6(2) . . ? C18 C17 H17 120.2 . . ? C16 C17 H17 120.2 . . ? C17 C18 C19 119.1(2) . . ? C17 C18 H18 120.5 . . ? C19 C18 H18 120.5 . . ? C20 C19 C18 118.2(2) . . ? C20 C19 H19 120.9 . . ? C18 C19 H19 120.9 . . ? N5 C20 C19 124.1(2) . . ? N5 C20 H20 117.9 . . ? C19 C20 H20 117.9 . . ? O3 C21 O4 124.72(18) . . ? O3 C21 C22 118.66(19) . . ? O4 C21 C22 116.62(19) . . ? C24 C22 C23 119.50(18) . . ? C24 C22 C21 120.34(19) . . ? C23 C22 C21 120.15(19) . . ? C22 C23 C23 120.16(12) . 2_655 ? C22 C23 H23 119.9 . . ? C23 C23 H23 119.9 2_655 . ? C22 C24 C24 120.31(12) . 2_655 ? C22 C24 H24 119.8 . . ? C24 C24 H24 119.8 2_655 . ? O6 C25 O5 124.09(18) . . ? O6 C25 C26 117.72(17) . . ? O5 C25 C26 118.18(16) . . ? C28 C26 C27 118.34(18) . . ? C28 C26 C25 119.36(17) . . ? C27 C26 C25 122.30(17) . . ? C28 C27 C26 120.60(18) 3_675 . ? C28 C27 H27 119.7 3_675 . ? C26 C27 H27 119.7 . . ? C27 C28 C26 121.07(18) 3_675 . ? C27 C28 H28 119.5 3_675 . ? C26 C28 H28 119.5 . . ? C5 N1 C1 117.57(18) . . ? C5 N1 Co1 123.35(13) . . ? C1 N1 Co1 118.65(14) . . ? C6 N2 C10 117.78(17) . . ? C6 N2 Co1 121.25(13) . . ? C10 N2 Co1 119.32(13) . . ? C6 N3 C5 127.97(16) . . ? C6 N3 H3A 116 . . ? C5 N3 H3A 116 . . ? C15 N4 C11 117.19(17) . . ? C15 N4 Co1 123.25(13) . . ? C11 N4 Co1 116.86(13) . . ? C16 N5 C20 117.10(17) . . ? C16 N5 Co1 124.03(12) . . ? C20 N5 Co1 117.78(13) . . ? C15 N6 C16 132.07(16) . . ? C15 N6 H6 114 . . ? C16 N6 H6 114 . . ? Co1 O2 H31 121(2) . . ? Co1 O2 H32 125(2) . . ? H31 O2 H32 108(3) . . ? Co1 O1 H29 126.8(18) . . ? Co1 O1 H30 122(2) . . ? H29 O1 H30 106(3) . . ? H33 O7 H34 87(4) . . ? O8B O8A H35 70(2) . . ? O8B O8A H36 59.7(17) . . ? H35 O8A H36 125(3) . . ? O8A O8B H35 63.6(19) . . ? O8A O8B H36 75(2) . . ? H35 O8B H36 133(3) . . ? O1 Co1 O2 88.50(7) . . ? O1 Co1 N1 93.47(7) . . ? O2 Co1 N1 89.50(7) . . ? O1 Co1 N5 92.42(6) . . ? O2 Co1 N5 90.98(6) . . ? N1 Co1 N5 174.10(6) . . ? O1 Co1 N4 91.43(7) . . ? O2 Co1 N4 175.90(6) . . ? N1 Co1 N4 94.59(6) . . ? N5 Co1 N4 84.93(6) . . ? O1 Co1 N2 175.94(6) . . ? O2 Co1 N2 91.41(7) . . ? N1 Co1 N2 82.47(6) . . ? N5 Co1 N2 91.64(6) . . ? N4 Co1 N2 88.94(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.318 _refine_diff_density_min -0.391 _refine_diff_density_rms 0.043 # END of CIF