# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Debajit Sarma' _publ_contact_author_email debajit@sscu.iisc.ernet.in _publ_author_name 'Srinivasan Natarajan' data_CompoundI _database_code_depnum_ccdc_archive 'CCDC 849287' #TrackingRef 'CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Co-Nitroisophthalate _chemical_melting_point ? _chemical_formula_moiety 'C36 H16 Co5 N10 O30' _chemical_formula_sum 'C36 H16 Co5 N10 O30' _chemical_formula_weight 1363.24 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' _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 9.5395(2) _cell_length_b 11.7926(2) _cell_length_c 11.8861(2) _cell_angle_alpha 110.2040(10) _cell_angle_beta 111.3290(10) _cell_angle_gamma 90.9080(10) _cell_volume 1153.50(4) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4514 _cell_measurement_theta_min 1.86 _cell_measurement_theta_max 26.00 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.962 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 677 _exptl_absorpt_coefficient_mu 1.876 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7533 _exptl_absorpt_correction_T_max 0.9287 _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 Smart CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16645 _diffrn_reflns_av_R_equivalents 0.0200 _diffrn_reflns_av_sigmaI/netI 0.0171 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4514 _reflns_number_gt 4211 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SAINT (Bruker, 2000)' _computing_data_reduction SAINT _computing_structure_solution 'SIR92 (Altomare et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1999) and CAMERON (Watkin et al., 1993)' _computing_publication_material 'PLATON (Spek, 2003)' _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^)+(0.0435P)^2^+0.9400P] 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 4514 _refine_ls_number_parameters 367 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0264 _refine_ls_R_factor_gt 0.0245 _refine_ls_wR_factor_ref 0.0747 _refine_ls_wR_factor_gt 0.0737 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.35510(3) 0.63078(2) 0.73759(3) 0.01783(8) Uani 1 1 d . . . Co2 Co 0.0000 0.5000 0.5000 0.01395(9) Uani 1 2 d S . . Co3 Co 0.60882(3) 0.83865(2) 0.70784(3) 0.01753(8) Uani 1 1 d . . . O1 O 0.42724(18) 0.36354(16) 1.15943(18) 0.0362(4) Uani 1 1 d . . . O2 O 0.26846(18) 0.55287(15) 0.82859(15) 0.0285(4) Uani 1 1 d . . . O3 O 0.15795(16) 0.68039(13) 0.61070(14) 0.0189(3) Uani 1 1 d . . . O4 O 0.3619(2) 0.80952(15) 0.88625(16) 0.0322(4) Uani 1 1 d . . . O5 O 0.37947(16) 0.75150(13) 0.62657(14) 0.0212(3) Uani 1 1 d . . . O6 O 0.03227(17) 0.48420(15) 0.67475(14) 0.0257(3) Uani 1 1 d . . . O7 O 0.27169(18) 0.20722(15) 1.13599(15) 0.0280(3) Uani 1 1 d . . . O8 O 0.38766(18) 1.03429(15) 0.38043(16) 0.0290(4) Uani 1 1 d . . . O9 O 0.54326(19) 0.97545(14) 0.84334(16) 0.0297(4) Uani 1 1 d . . . O10 O 0.17011(18) 1.05549(15) 0.24784(16) 0.0289(4) Uani 1 1 d . . . O11 O -0.2803(2) 0.21914(19) 0.9096(2) 0.0425(5) Uani 1 1 d . . . O12 O -0.3441(2) 0.3284(2) 0.7938(3) 0.0646(7) Uani 1 1 d . . . O13 O -0.3051(2) 0.8871(2) 0.2353(2) 0.0526(6) Uani 1 1 d . . . O14 O -0.3070(2) 0.7902(3) 0.3578(3) 0.0663(7) Uani 1 1 d . . . O100 O 0.1262(3) 0.9350(2) 0.9086(2) 0.0611(6) Uani 1 1 d . . . N1 N 0.33204(19) 0.46986(15) 0.58203(17) 0.0195(3) Uani 1 1 d . . . N2 N 0.18723(19) 0.42550(16) 0.48732(17) 0.0198(3) Uani 1 1 d . . . N3 N 0.3424(2) 0.30837(16) 0.42113(18) 0.0226(4) Uani 1 1 d . . . N4 N -0.2496(2) 0.28808(18) 0.86309(19) 0.0263(4) Uani 1 1 d . . . N5 N -0.2411(2) 0.84235(18) 0.3155(2) 0.0300(4) Uani 1 1 d . . . C1 C 0.1364(2) 0.49416(18) 0.78071(19) 0.0193(4) Uani 1 1 d . . . C2 C 0.0982(2) 0.42794(18) 0.85624(19) 0.0182(4) Uani 1 1 d . . . C3 C 0.2125(2) 0.39889(18) 0.94974(19) 0.0191(4) Uani 1 1 d . . . H3 H 0.3143 0.4269 0.9718 0.023 Uiso 1 1 calc R . . C4 C 0.1752(2) 0.32807(18) 1.01056(19) 0.0188(4) Uani 1 1 d . . . C5 C 0.0233(2) 0.28835(19) 0.9810(2) 0.0198(4) Uani 1 1 d . . . H5 H -0.0029 0.2393 1.0194 0.024 Uiso 1 1 calc R . . C6 C -0.0877(2) 0.32446(18) 0.89246(19) 0.0192(4) Uani 1 1 d . . . C7 C -0.0541(2) 0.39168(18) 0.82824(19) 0.0191(4) Uani 1 1 d . . . H7 H -0.1316 0.4123 0.7675 0.023 Uiso 1 1 calc R . . C8 C 0.3017(2) 0.29635(19) 1.10999(19) 0.0200(4) Uani 1 1 d . . . C9 C 0.2369(2) 0.74402(17) 0.58112(18) 0.0160(4) Uani 1 1 d . . . C10 C 0.1581(2) 0.80966(18) 0.49391(19) 0.0177(4) Uani 1 1 d . . . C11 C 0.2396(2) 0.87874(18) 0.4560(2) 0.0188(4) Uani 1 1 d . . . H11 H 0.3453 0.8870 0.4871 0.023 Uiso 1 1 calc R . . C12 C 0.1609(2) 0.93548(18) 0.3710(2) 0.0194(4) Uani 1 1 d . . . C13 C 0.0030(2) 0.92288(19) 0.3242(2) 0.0217(4) Uani 1 1 d . . . H13 H -0.0500 0.9593 0.2668 0.026 Uiso 1 1 calc R . . C14 C -0.0735(2) 0.85524(19) 0.3646(2) 0.0203(4) Uani 1 1 d . . . C15 C 0.0000(2) 0.79924(18) 0.4493(2) 0.0195(4) Uani 1 1 d . . . H15 H -0.0548 0.7555 0.4761 0.023 Uiso 1 1 calc R . . C16 C 0.2451(2) 1.01197(19) 0.3305(2) 0.0216(4) Uani 1 1 d . . . C17 C 0.1991(2) 0.33059(19) 0.3945(2) 0.0234(4) Uani 1 1 d . . . H17 H 0.1167 0.2838 0.3184 0.028 Uiso 1 1 calc R . . C18 C 0.4199(2) 0.39714(19) 0.5386(2) 0.0233(4) Uani 1 1 d . . . H18 H 0.5245 0.4063 0.5844 0.028 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01368(14) 0.02148(15) 0.01802(15) 0.01212(11) 0.00163(11) -0.00059(11) Co2 0.01005(18) 0.01880(19) 0.01525(18) 0.01040(15) 0.00366(14) 0.00283(14) Co3 0.01504(15) 0.02026(15) 0.02131(15) 0.01276(12) 0.00689(11) 0.00295(11) O1 0.0170(8) 0.0434(10) 0.0432(10) 0.0298(8) -0.0060(7) -0.0040(7) O2 0.0242(8) 0.0360(9) 0.0266(8) 0.0194(7) 0.0046(7) -0.0065(7) O3 0.0170(7) 0.0214(7) 0.0216(7) 0.0136(6) 0.0060(6) 0.0013(5) O4 0.0357(9) 0.0344(9) 0.0246(8) 0.0077(7) 0.0134(7) -0.0034(7) O5 0.0127(7) 0.0255(7) 0.0267(8) 0.0147(6) 0.0046(6) 0.0028(6) O6 0.0227(8) 0.0374(9) 0.0221(8) 0.0208(7) 0.0053(6) 0.0024(7) O7 0.0249(8) 0.0341(8) 0.0300(8) 0.0250(7) 0.0041(7) 0.0029(7) O8 0.0201(8) 0.0369(9) 0.0393(9) 0.0270(8) 0.0099(7) 0.0030(7) O9 0.0311(9) 0.0267(8) 0.0310(9) 0.0086(7) 0.0141(7) 0.0042(7) O10 0.0250(8) 0.0339(9) 0.0336(9) 0.0254(7) 0.0061(7) 0.0004(7) O11 0.0271(9) 0.0593(12) 0.0552(12) 0.0378(10) 0.0167(8) -0.0010(8) O12 0.0169(9) 0.1012(19) 0.0957(18) 0.0778(16) 0.0055(10) 0.0071(10) O13 0.0245(9) 0.0807(15) 0.0730(14) 0.0604(13) 0.0114(9) 0.0189(10) O14 0.0204(10) 0.1088(19) 0.0996(18) 0.0818(17) 0.0164(11) 0.0040(11) O100 0.0482(13) 0.0704(15) 0.0510(13) 0.0200(12) 0.0068(10) 0.0230(11) N1 0.0122(8) 0.0221(9) 0.0219(9) 0.0101(7) 0.0026(7) 0.0012(7) N2 0.0126(8) 0.0237(9) 0.0206(8) 0.0089(7) 0.0035(7) 0.0030(7) N3 0.0178(9) 0.0251(9) 0.0272(9) 0.0117(8) 0.0096(7) 0.0066(7) N4 0.0172(9) 0.0330(10) 0.0285(10) 0.0146(8) 0.0059(8) -0.0003(8) N5 0.0178(9) 0.0357(11) 0.0394(11) 0.0219(9) 0.0072(8) 0.0051(8) C1 0.0212(10) 0.0213(10) 0.0190(10) 0.0117(8) 0.0080(8) 0.0045(8) C2 0.0197(10) 0.0195(9) 0.0165(9) 0.0100(8) 0.0055(8) 0.0018(8) C3 0.0148(9) 0.0230(10) 0.0192(10) 0.0104(8) 0.0043(8) 0.0001(8) C4 0.0181(10) 0.0213(10) 0.0171(9) 0.0104(8) 0.0041(8) 0.0028(8) C5 0.0189(10) 0.0226(10) 0.0199(10) 0.0117(8) 0.0066(8) 0.0003(8) C6 0.0140(9) 0.0224(10) 0.0195(10) 0.0084(8) 0.0045(8) 0.0001(8) C7 0.0163(10) 0.0230(10) 0.0167(9) 0.0106(8) 0.0021(8) 0.0038(8) C8 0.0182(10) 0.0254(10) 0.0178(10) 0.0119(8) 0.0048(8) 0.0049(8) C9 0.0161(9) 0.0155(9) 0.0159(9) 0.0068(7) 0.0049(8) 0.0015(7) C10 0.0177(10) 0.0180(9) 0.0183(9) 0.0094(8) 0.0057(8) 0.0025(7) C11 0.0152(9) 0.0207(10) 0.0217(10) 0.0112(8) 0.0056(8) 0.0012(8) C12 0.0198(10) 0.0191(9) 0.0220(10) 0.0115(8) 0.0078(8) 0.0007(8) C13 0.0215(10) 0.0221(10) 0.0232(10) 0.0140(9) 0.0054(8) 0.0047(8) C14 0.0142(10) 0.0217(10) 0.0250(10) 0.0114(8) 0.0054(8) 0.0030(8) C15 0.0173(10) 0.0195(9) 0.0238(10) 0.0114(8) 0.0075(8) 0.0007(8) C16 0.0234(11) 0.0210(10) 0.0240(10) 0.0125(9) 0.0095(9) 0.0027(8) C17 0.0164(10) 0.0270(11) 0.0237(11) 0.0082(9) 0.0056(9) 0.0037(8) C18 0.0133(9) 0.0271(11) 0.0305(11) 0.0139(9) 0.0069(8) 0.0054(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 1.9758(16) 2_667 ? Co1 O2 2.0024(15) . ? Co1 N1 2.0822(17) . ? Co1 O3 2.1760(14) . ? Co1 O4 2.2156(17) . ? Co1 O5 2.3091(14) . ? Co2 N2 2.0344(17) 2_566 ? Co2 N2 2.0344(17) . ? Co2 O6 2.0610(14) 2_566 ? Co2 O6 2.0610(14) . ? Co2 O3 2.2472(14) . ? Co2 O3 2.2472(14) 2_566 ? Co3 O7 2.0522(15) 2_667 ? Co3 N3 2.0690(18) 2_666 ? Co3 O8 2.1112(15) 2_676 ? Co3 O5 2.1170(14) . ? Co3 O9 2.1349(16) . ? Co3 O10 2.2221(16) 2_676 ? Co3 C16 2.488(2) 2_676 ? O1 C8 1.243(3) . ? O1 Co1 1.9758(16) 2_667 ? O2 C1 1.252(3) . ? O3 C9 1.269(2) . ? O5 C9 1.257(2) . ? O6 C1 1.253(3) . ? O7 C8 1.249(3) . ? O7 Co3 2.0522(15) 2_667 ? O8 C16 1.251(3) . ? O8 Co3 2.1112(15) 2_676 ? O10 C16 1.261(3) . ? O10 Co3 2.2221(16) 2_676 ? O11 N4 1.214(3) . ? O12 N4 1.209(3) . ? O13 N5 1.223(3) . ? O14 N5 1.207(3) . ? N1 C18 1.318(3) . ? N1 N2 1.374(2) . ? N2 C17 1.313(3) . ? N3 C17 1.339(3) . ? N3 C18 1.344(3) . ? N3 Co3 2.0690(18) 2_666 ? N4 C6 1.475(3) . ? N5 C14 1.473(3) . ? C1 C2 1.504(3) . ? C2 C3 1.391(3) . ? C2 C7 1.391(3) . ? C3 C4 1.393(3) . ? C4 C5 1.392(3) . ? C4 C8 1.508(3) . ? C5 C6 1.387(3) . ? C6 C7 1.379(3) . ? C9 C10 1.498(3) . ? C10 C15 1.393(3) . ? C10 C11 1.399(3) . ? C11 C12 1.401(3) . ? C12 C13 1.388(3) . ? C12 C16 1.500(3) . ? C13 C14 1.379(3) . ? C14 C15 1.379(3) . ? C16 Co3 2.488(2) 2_676 ? 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 O1 Co1 O2 97.38(7) 2_667 . ? O1 Co1 N1 96.21(7) 2_667 . ? O2 Co1 N1 96.19(7) . . ? O1 Co1 O3 157.26(6) 2_667 . ? O2 Co1 O3 103.87(6) . . ? N1 Co1 O3 89.53(6) . . ? O1 Co1 O4 89.03(7) 2_667 . ? O2 Co1 O4 87.05(7) . . ? N1 Co1 O4 173.42(7) . . ? O3 Co1 O4 84.12(6) . . ? O1 Co1 O5 99.62(6) 2_667 . ? O2 Co1 O5 159.96(6) . . ? N1 Co1 O5 92.45(6) . . ? O3 Co1 O5 58.05(5) . . ? O4 Co1 O5 82.72(6) . . ? N2 Co2 N2 180.000(1) 2_566 . ? N2 Co2 O6 94.13(7) 2_566 2_566 ? N2 Co2 O6 85.87(7) . 2_566 ? N2 Co2 O6 85.87(7) 2_566 . ? N2 Co2 O6 94.13(7) . . ? O6 Co2 O6 180.0 2_566 . ? N2 Co2 O3 94.05(6) 2_566 . ? N2 Co2 O3 85.95(6) . . ? O6 Co2 O3 90.84(6) 2_566 . ? O6 Co2 O3 89.16(6) . . ? N2 Co2 O3 85.95(6) 2_566 2_566 ? N2 Co2 O3 94.05(6) . 2_566 ? O6 Co2 O3 89.16(6) 2_566 2_566 ? O6 Co2 O3 90.84(6) . 2_566 ? O3 Co2 O3 180.0 . 2_566 ? O7 Co3 N3 92.64(7) 2_667 2_666 ? O7 Co3 O8 143.68(6) 2_667 2_676 ? N3 Co3 O8 98.19(7) 2_666 2_676 ? O7 Co3 O5 108.45(6) 2_667 . ? N3 Co3 O5 89.83(6) 2_666 . ? O8 Co3 O5 106.15(6) 2_676 . ? O7 Co3 O9 84.88(7) 2_667 . ? N3 Co3 O9 173.50(7) 2_666 . ? O8 Co3 O9 87.29(7) 2_676 . ? O5 Co3 O9 85.28(6) . . ? O7 Co3 O10 85.50(6) 2_667 2_676 ? N3 Co3 O10 88.49(7) 2_666 2_676 ? O8 Co3 O10 60.42(6) 2_676 2_676 ? O5 Co3 O10 166.01(6) . 2_676 ? O9 Co3 O10 97.29(6) . 2_676 ? O7 Co3 C16 115.49(7) 2_667 2_676 ? N3 Co3 C16 91.87(7) 2_666 2_676 ? O8 Co3 C16 30.15(7) 2_676 2_676 ? O5 Co3 C16 135.89(6) . 2_676 ? O9 Co3 C16 94.62(7) . 2_676 ? O10 Co3 C16 30.38(6) 2_676 2_676 ? C8 O1 Co1 140.94(15) . 2_667 ? C1 O2 Co1 124.95(14) . . ? C9 O3 Co1 94.22(12) . . ? C9 O3 Co2 133.82(13) . . ? Co1 O3 Co2 101.27(5) . . ? C9 O5 Co3 156.23(13) . . ? C9 O5 Co1 88.43(11) . . ? Co3 O5 Co1 109.18(6) . . ? C1 O6 Co2 140.99(14) . . ? C8 O7 Co3 129.45(14) . 2_667 ? C16 O8 Co3 91.85(12) . 2_676 ? C16 O10 Co3 86.57(13) . 2_676 ? C18 N1 N2 105.46(17) . . ? C18 N1 Co1 138.55(15) . . ? N2 N1 Co1 115.77(12) . . ? C17 N2 N1 106.25(16) . . ? C17 N2 Co2 129.94(14) . . ? N1 N2 Co2 123.81(13) . . ? C17 N3 C18 102.55(17) . . ? C17 N3 Co3 120.47(15) . 2_666 ? C18 N3 Co3 136.96(14) . 2_666 ? O12 N4 O11 123.8(2) . . ? O12 N4 C6 118.09(19) . . ? O11 N4 C6 118.14(18) . . ? O14 N5 O13 123.8(2) . . ? O14 N5 C14 118.52(19) . . ? O13 N5 C14 117.68(19) . . ? O2 C1 O6 126.31(19) . . ? O2 C1 C2 117.39(18) . . ? O6 C1 C2 116.29(18) . . ? C3 C2 C7 119.89(18) . . ? C3 C2 C1 120.96(18) . . ? C7 C2 C1 119.11(17) . . ? C2 C3 C4 120.27(19) . . ? C5 C4 C3 120.46(18) . . ? C5 C4 C8 120.47(18) . . ? C3 C4 C8 119.06(18) . . ? C6 C5 C4 117.68(18) . . ? C7 C6 C5 123.05(19) . . ? C7 C6 N4 117.93(18) . . ? C5 C6 N4 119.02(18) . . ? C6 C7 C2 118.53(18) . . ? O1 C8 O7 126.10(19) . . ? O1 C8 C4 115.78(18) . . ? O7 C8 C4 118.11(18) . . ? O5 C9 O3 119.28(17) . . ? O5 C9 C10 121.42(18) . . ? O3 C9 C10 119.29(17) . . ? C15 C10 C11 120.20(18) . . ? C15 C10 C9 118.27(18) . . ? C11 C10 C9 121.52(18) . . ? C10 C11 C12 119.62(19) . . ? C13 C12 C11 120.22(19) . . ? C13 C12 C16 118.89(18) . . ? C11 C12 C16 120.89(19) . . ? C14 C13 C12 118.66(19) . . ? C13 C14 C15 122.83(19) . . ? C13 C14 N5 118.69(18) . . ? C15 C14 N5 118.48(18) . . ? C14 C15 C10 118.45(19) . . ? O8 C16 O10 120.67(19) . . ? O8 C16 C12 120.27(18) . . ? O10 C16 C12 119.04(19) . . ? O8 C16 Co3 58.00(11) . 2_676 ? O10 C16 Co3 63.05(11) . 2_676 ? C12 C16 Co3 172.25(15) . 2_676 ? N2 C17 N3 112.83(19) . . ? N1 C18 N3 112.92(19) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.685 _refine_diff_density_min -0.385 _refine_diff_density_rms 0.069 ######END####### data_CompoundIa _database_code_depnum_ccdc_archive 'CCDC 849288' #TrackingRef 'CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Co-Nitroisophthalate _chemical_melting_point ? _chemical_formula_moiety 'C36 H16 Co5 N10 O24' _chemical_formula_sum 'C36 H16 Co5 N10 O24' _chemical_formula_weight 1267.24 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' _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 9.259(3) _cell_length_b 11.177(4) _cell_length_c 12.131(4) _cell_angle_alpha 108.02(3) _cell_angle_beta 91.64(3) _cell_angle_gamma 105.27(3) _cell_volume 1143.4(6) _cell_formula_units_Z 1 _cell_measurement_temperature 503(2) _cell_measurement_reflns_used 4478 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 26.00 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.840 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 629 _exptl_absorpt_coefficient_mu 1.876 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7534 _exptl_absorpt_correction_T_max 0.9287 _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 503(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 Smart CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18322 _diffrn_reflns_av_R_equivalents 0.1847 _diffrn_reflns_av_sigmaI/netI 0.1633 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4478 _reflns_number_gt 1854 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SAINT (Bruker, 2000)' _computing_data_reduction SAINT _computing_structure_solution 'SIR92 (Altomare et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1999) and CAMERON (Watkin et al., 1993)' _computing_publication_material 'PLATON (Spek, 2003)' _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^)+(0.2000P)^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 4478 _refine_ls_number_parameters 340 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2335 _refine_ls_R_factor_gt 0.1316 _refine_ls_wR_factor_ref 0.3833 _refine_ls_wR_factor_gt 0.3108 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 0.988 _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 0.15651(19) 0.26358(19) 0.37692(16) 0.0592(7) Uani 1 1 d . . . Co2 Co 0.5000 0.5000 0.5000 0.0512(7) Uani 1 2 d S . . Co3 Co -0.0808(2) 0.3103(2) 0.17214(17) 0.0630(7) Uani 1 1 d . . . O1 O 0.0493(10) -0.1478(11) 0.6373(9) 0.083(3) Uani 1 1 d . . . O2 O 0.2700(9) 0.1698(9) 0.4404(8) 0.060(2) Uani 1 1 d . . . O3 O 0.3605(8) 0.3886(9) 0.3271(7) 0.056(2) Uani 1 1 d . . . O5 O 0.1376(8) 0.3453(8) 0.2362(7) 0.049(2) Uani 1 1 d . . . O6 O 0.4853(10) 0.3233(9) 0.5292(8) 0.062(2) Uani 1 1 d . . . O7 O 0.1736(12) -0.1427(11) 0.7952(8) 0.079(3) Uani 1 1 d . . . O8 O 0.1008(9) 0.6252(10) -0.0352(8) 0.062(2) Uani 1 1 d . . . O10 O 0.3137(11) 0.7203(11) -0.0880(10) 0.089(4) Uani 1 1 d . . . O11 O 0.7297(14) 0.0199(17) 0.8145(13) 0.129(6) Uani 1 1 d . . . O12 O 0.8255(12) 0.1568(16) 0.7310(14) 0.130(6) Uani 1 1 d . . . O13 O 0.7945(11) 0.7579(14) 0.1075(11) 0.102(4) Uani 1 1 d . . . O14 O 0.8095(11) 0.6594(14) 0.2297(13) 0.114(5) Uani 1 1 d . . . N1 N 0.1641(12) 0.4135(11) 0.5232(10) 0.058(3) Uani 1 1 d . . . N2 N 0.2998(11) 0.5135(11) 0.5639(10) 0.057(3) Uani 1 1 d . . . N3 N 0.1328(13) 0.5633(12) 0.6792(10) 0.062(3) Uani 1 1 d . . . N4 N 0.7177(15) 0.0820(16) 0.7523(14) 0.091(4) Uani 1 1 d . . . N5 N 0.7387(13) 0.6886(13) 0.1636(11) 0.072(3) Uani 1 1 d . . . C1 C 0.3904(15) 0.2193(13) 0.5129(13) 0.059(3) Uani 1 1 d . . . C2 C 0.4141(13) 0.1343(12) 0.5830(11) 0.050(3) Uani 1 1 d . . . C3 C 0.2847(13) 0.0446(13) 0.6042(12) 0.057(3) Uani 1 1 d . . . H3 H 0.1901 0.0321 0.5669 0.068 Uiso 1 1 calc R . . C4 C 0.2989(14) -0.0231(12) 0.6791(12) 0.053(3) Uani 1 1 d . . . C5 C 0.4447(14) -0.0077(13) 0.7314(11) 0.056(3) Uani 1 1 d . . . H5 H 0.4555 -0.0519 0.7832 0.067 Uiso 1 1 calc R . . C6 C 0.5707(16) 0.0730(15) 0.7054(13) 0.069(4) Uani 1 1 d . . . C7 C 0.5521(16) 0.1500(12) 0.6333(11) 0.056(3) Uani 1 1 d . . . H7 H 0.6354 0.2106 0.6215 0.067 Uiso 1 1 calc R . . C8 C 0.1605(17) -0.1115(16) 0.7073(13) 0.066(4) Uani 1 1 d . . . C9 C 0.2804(13) 0.4059(12) 0.2535(10) 0.048(3) Uani 1 1 d . . . C10 C 0.3469(13) 0.4978(13) 0.1880(11) 0.053(3) Uani 1 1 d . . . C11 C 0.2623(13) 0.5339(12) 0.1129(10) 0.045(3) Uani 1 1 d . . . H11 H 0.1581 0.4978 0.1007 0.055 Uiso 1 1 calc R . . C12 C 0.3270(15) 0.6212(18) 0.0559(11) 0.074(5) Uani 1 1 d . . . C13 C 0.4891(13) 0.6724(12) 0.0700(10) 0.049(3) Uani 1 1 d . . . H13 H 0.5373 0.7304 0.0327 0.058 Uiso 1 1 calc R . . C14 C 0.5701(13) 0.6306(13) 0.1421(10) 0.049(3) Uani 1 1 d . . . C15 C 0.5041(13) 0.5518(12) 0.2039(10) 0.049(3) Uani 1 1 d . . . H15 H 0.5632 0.5339 0.2565 0.059 Uiso 1 1 calc R . . C16 C 0.2457(16) 0.6620(14) -0.0248(11) 0.061(4) Uani 1 1 d . . . C17 C 0.2738(13) 0.6004(14) 0.6565(12) 0.054(3) Uani 1 1 d . . . H17 H 0.3452 0.6781 0.7004 0.065 Uiso 1 1 calc R . . C18 C 0.0692(15) 0.4531(14) 0.5973(13) 0.060(4) Uani 1 1 d . . . H18 H -0.0318 0.4066 0.5908 0.072 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0517(10) 0.0657(14) 0.0650(12) 0.0405(10) -0.0032(8) 0.0031(9) Co2 0.0428(13) 0.0556(16) 0.0663(16) 0.0392(13) 0.0058(11) 0.0095(11) Co3 0.0538(11) 0.0803(15) 0.0687(13) 0.0493(11) 0.0009(8) 0.0132(9) O1 0.055(6) 0.097(8) 0.102(8) 0.071(7) -0.015(5) -0.012(5) O2 0.053(5) 0.052(6) 0.072(6) 0.032(5) -0.011(4) -0.003(4) O3 0.038(4) 0.073(6) 0.067(6) 0.041(5) -0.004(4) 0.010(4) O5 0.032(4) 0.058(6) 0.057(5) 0.029(4) -0.001(3) -0.001(4) O6 0.060(5) 0.051(6) 0.093(7) 0.048(5) 0.013(5) 0.014(5) O7 0.097(7) 0.080(8) 0.054(6) 0.040(5) -0.004(5) -0.002(6) O8 0.043(5) 0.079(7) 0.066(6) 0.033(5) -0.007(4) 0.009(4) O10 0.079(7) 0.102(9) 0.095(8) 0.071(7) -0.015(6) -0.004(6) O11 0.088(9) 0.207(17) 0.147(12) 0.133(13) -0.004(8) 0.048(10) O12 0.041(6) 0.166(14) 0.203(15) 0.119(13) -0.006(7) -0.002(7) O13 0.061(6) 0.147(12) 0.127(10) 0.099(10) 0.015(6) 0.012(7) O14 0.054(6) 0.146(12) 0.165(12) 0.121(11) -0.013(7) -0.012(7) N1 0.052(6) 0.055(7) 0.068(7) 0.025(6) 0.004(5) 0.012(5) N2 0.053(6) 0.063(7) 0.074(8) 0.047(6) 0.005(5) 0.017(6) N3 0.068(7) 0.065(8) 0.077(8) 0.052(7) 0.012(6) 0.025(6) N4 0.061(8) 0.102(12) 0.111(12) 0.042(10) -0.006(8) 0.019(8) N5 0.056(7) 0.086(10) 0.091(9) 0.055(8) -0.005(6) 0.021(6) C1 0.059(8) 0.038(8) 0.089(10) 0.030(7) 0.028(7) 0.018(7) C2 0.042(6) 0.045(7) 0.059(8) 0.014(6) -0.003(5) 0.014(6) C3 0.046(7) 0.050(8) 0.079(9) 0.040(7) -0.011(6) 0.002(6) C4 0.054(7) 0.033(7) 0.072(9) 0.025(6) 0.006(6) 0.003(6) C5 0.060(8) 0.055(8) 0.062(8) 0.029(7) -0.004(6) 0.023(7) C6 0.065(9) 0.066(10) 0.078(10) 0.032(8) -0.015(7) 0.015(8) C7 0.079(9) 0.033(7) 0.055(8) 0.015(6) 0.002(6) 0.016(6) C8 0.069(9) 0.090(12) 0.071(10) 0.050(9) 0.027(8) 0.046(9) C9 0.054(7) 0.045(7) 0.049(7) 0.030(6) 0.008(5) 0.003(6) C10 0.052(7) 0.055(8) 0.054(7) 0.039(6) 0.009(6) -0.005(6) C11 0.051(6) 0.043(7) 0.047(7) 0.028(6) 0.006(5) 0.005(5) C12 0.051(7) 0.129(14) 0.042(7) 0.043(8) -0.006(6) 0.011(8) C13 0.060(7) 0.055(8) 0.041(6) 0.032(6) 0.006(5) 0.015(6) C14 0.044(6) 0.056(8) 0.049(7) 0.020(6) 0.003(5) 0.016(6) C15 0.043(6) 0.056(8) 0.050(7) 0.023(6) -0.009(5) 0.014(6) C16 0.078(9) 0.060(9) 0.053(8) 0.034(7) -0.012(7) 0.017(7) C17 0.047(7) 0.066(9) 0.068(9) 0.048(8) 0.017(6) 0.014(6) C18 0.050(7) 0.052(9) 0.083(10) 0.037(8) 0.000(7) 0.007(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 O2 1.957(9) . ? Co1 O1 1.969(9) 2_556 ? Co1 N1 2.013(12) . ? Co1 O5 2.194(8) . ? Co1 O3 2.255(8) . ? Co2 N2 2.054(11) 2_666 ? Co2 N2 2.054(11) . ? Co2 O6 2.083(8) 2_666 ? Co2 O6 2.083(8) . ? Co2 O3 2.236(8) . ? Co2 O3 2.236(8) 2_666 ? Co3 O7 2.009(10) 2_556 ? Co3 O8 2.026(9) 2_565 ? Co3 O5 2.038(7) . ? Co3 N3 2.077(12) 2_566 ? Co3 O10 2.253(10) 2_565 ? Co3 C16 2.461(12) 2_565 ? O1 C8 1.209(16) . ? O1 Co1 1.969(9) 2_556 ? O2 C1 1.281(16) . ? O3 C9 1.236(14) . ? O5 C9 1.294(14) . ? O6 C1 1.213(15) . ? O7 C8 1.232(15) . ? O7 Co3 2.009(10) 2_556 ? O8 C16 1.286(16) . ? O8 Co3 2.026(9) 2_565 ? O10 C16 1.237(16) . ? O10 Co3 2.253(10) 2_565 ? O11 N4 1.193(18) . ? O12 N4 1.212(19) . ? O13 N5 1.211(15) . ? O14 N5 1.193(14) . ? N1 C18 1.334(17) . ? N1 N2 1.398(14) . ? N2 C17 1.314(16) . ? N3 C18 1.296(17) . ? N3 C17 1.326(15) . ? N3 Co3 2.077(12) 2_566 ? N4 C6 1.426(17) . ? N5 C14 1.504(15) . ? C1 C2 1.507(18) . ? C2 C7 1.344(16) . ? C2 C3 1.432(17) . ? C3 C4 1.374(17) . ? C4 C5 1.419(17) . ? C4 C8 1.518(19) . ? C5 C6 1.385(19) . ? C6 C7 1.439(18) . ? C9 C10 1.505(15) . ? C10 C11 1.400(17) . ? C10 C15 1.403(16) . ? C11 C12 1.386(18) . ? C12 C13 1.443(17) . ? C12 C16 1.465(17) . ? C13 C14 1.394(16) . ? C14 C15 1.365(17) . ? C16 Co3 2.461(12) 2_565 ? 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 O2 Co1 O1 99.7(4) . 2_556 ? O2 Co1 N1 99.3(4) . . ? O1 Co1 N1 102.3(5) 2_556 . ? O2 Co1 O5 144.0(4) . . ? O1 Co1 O5 101.8(3) 2_556 . ? N1 Co1 O5 103.8(4) . . ? O2 Co1 O3 94.7(3) . . ? O1 Co1 O3 159.1(4) 2_556 . ? N1 Co1 O3 90.1(4) . . ? O5 Co1 O3 58.5(3) . . ? N2 Co2 N2 180.000(2) 2_666 . ? N2 Co2 O6 93.4(4) 2_666 2_666 ? N2 Co2 O6 86.6(4) . 2_666 ? N2 Co2 O6 86.6(4) 2_666 . ? N2 Co2 O6 93.4(4) . . ? O6 Co2 O6 180.000(1) 2_666 . ? N2 Co2 O3 94.2(4) 2_666 . ? N2 Co2 O3 85.8(4) . . ? O6 Co2 O3 90.4(3) 2_666 . ? O6 Co2 O3 89.6(3) . . ? N2 Co2 O3 85.8(4) 2_666 2_666 ? N2 Co2 O3 94.2(4) . 2_666 ? O6 Co2 O3 89.6(3) 2_666 2_666 ? O6 Co2 O3 90.4(3) . 2_666 ? O3 Co2 O3 180.000(2) . 2_666 ? O7 Co3 O8 134.8(4) 2_556 2_565 ? O7 Co3 O5 99.5(4) 2_556 . ? O8 Co3 O5 113.1(3) 2_565 . ? O7 Co3 N3 97.1(4) 2_556 2_566 ? O8 Co3 N3 109.7(4) 2_565 2_566 ? O5 Co3 N3 95.1(4) . 2_566 ? O7 Co3 O10 85.0(4) 2_556 2_565 ? O8 Co3 O10 61.4(3) 2_565 2_565 ? O5 Co3 O10 174.5(4) . 2_565 ? N3 Co3 O10 87.5(5) 2_566 2_565 ? O7 Co3 C16 110.9(4) 2_556 2_565 ? O8 Co3 C16 31.4(4) 2_565 2_565 ? O5 Co3 C16 144.5(4) . 2_565 ? N3 Co3 C16 98.8(5) 2_566 2_565 ? O10 Co3 C16 30.0(4) 2_565 2_565 ? C8 O1 Co1 134.4(10) . 2_556 ? C1 O2 Co1 127.5(8) . . ? C9 O3 Co2 140.0(9) . . ? C9 O3 Co1 90.9(7) . . ? Co2 O3 Co1 102.0(3) . . ? C9 O5 Co3 154.2(8) . . ? C9 O5 Co1 92.1(6) . . ? Co3 O5 Co1 112.4(3) . . ? C1 O6 Co2 137.5(9) . . ? C8 O7 Co3 131.4(11) . 2_556 ? C16 O8 Co3 93.3(7) . 2_565 ? C16 O10 Co3 84.3(8) . 2_565 ? C18 N1 N2 104.0(11) . . ? C18 N1 Co1 137.8(9) . . ? N2 N1 Co1 118.2(9) . . ? C17 N2 N1 106.3(10) . . ? C17 N2 Co2 129.7(9) . . ? N1 N2 Co2 123.3(9) . . ? C18 N3 C17 105.7(12) . . ? C18 N3 Co3 139.6(10) . 2_566 ? C17 N3 Co3 114.8(10) . 2_566 ? O11 N4 O12 122.6(14) . . ? O11 N4 C6 118.9(16) . . ? O12 N4 C6 118.4(15) . . ? O14 N5 O13 124.0(12) . . ? O14 N5 C14 118.9(12) . . ? O13 N5 C14 116.9(11) . . ? O6 C1 O2 127.6(13) . . ? O6 C1 C2 118.1(13) . . ? O2 C1 C2 114.3(11) . . ? C7 C2 C3 120.3(12) . . ? C7 C2 C1 120.9(12) . . ? C3 C2 C1 118.6(10) . . ? C4 C3 C2 120.6(11) . . ? C3 C4 C5 119.1(12) . . ? C3 C4 C8 120.5(11) . . ? C5 C4 C8 120.3(12) . . ? C6 C5 C4 120.2(12) . . ? C5 C6 N4 120.1(13) . . ? C5 C6 C7 119.5(12) . . ? N4 C6 C7 120.4(14) . . ? C2 C7 C6 119.9(13) . . ? O1 C8 O7 126.9(15) . . ? O1 C8 C4 115.4(12) . . ? O7 C8 C4 117.7(13) . . ? O3 C9 O5 118.3(11) . . ? O3 C9 C10 120.7(11) . . ? O5 C9 C10 120.9(10) . . ? C11 C10 C15 117.8(10) . . ? C11 C10 C9 124.4(11) . . ? C15 C10 C9 117.9(11) . . ? C12 C11 C10 122.9(11) . . ? C11 C12 C13 118.7(11) . . ? C11 C12 C16 125.7(12) . . ? C13 C12 C16 115.5(12) . . ? C14 C13 C12 116.8(11) . . ? C15 C14 C13 123.6(11) . . ? C15 C14 N5 118.2(10) . . ? C13 C14 N5 117.8(11) . . ? C14 C15 C10 120.0(11) . . ? O10 C16 O8 120.9(11) . . ? O10 C16 C12 121.0(13) . . ? O8 C16 C12 117.8(12) . . ? O10 C16 Co3 65.7(7) . 2_565 ? O8 C16 Co3 55.3(6) . 2_565 ? C12 C16 Co3 169.8(11) . 2_565 ? N2 C17 N3 111.3(13) . . ? N3 C18 N1 112.8(12) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.585 _refine_diff_density_min -0.771 _refine_diff_density_rms 0.213 ######END####### data_CompoundIb _database_code_depnum_ccdc_archive 'CCDC 849289' #TrackingRef 'CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Co-Nitroisophthalate _chemical_melting_point ? _chemical_formula_moiety 'C36 H16 Co5 N10 O26' _chemical_formula_sum 'C36 H16 Co5 N10 O26' _chemical_formula_weight 1299.24 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' _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 9.202(3) _cell_length_b 11.088(4) _cell_length_c 11.992(3) _cell_angle_alpha 108.58(3) _cell_angle_beta 91.40(2) _cell_angle_gamma 104.71(3) _cell_volume 1114.3(6) _cell_formula_units_Z 1 _cell_measurement_temperature 423(2) _cell_measurement_reflns_used 4281 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 26.00 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.936 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 645 _exptl_absorpt_coefficient_mu 1.931 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7475 _exptl_absorpt_correction_T_max 0.9268 _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 423(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 Smart CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7158 _diffrn_reflns_av_R_equivalents 0.0986 _diffrn_reflns_av_sigmaI/netI 0.1937 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4281 _reflns_number_gt 1736 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SAINT (Bruker, 2000)' _computing_data_reduction SAINT _computing_structure_solution 'SIR92 (Altomare et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1999) and CAMERON (Watkin et al., 1993)' _computing_publication_material 'PLATON (Spek, 2003)' _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^)+(0.1737P)^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 4281 _refine_ls_number_parameters 349 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2368 _refine_ls_R_factor_gt 0.1211 _refine_ls_wR_factor_ref 0.3461 _refine_ls_wR_factor_gt 0.2804 _refine_ls_goodness_of_fit_ref 0.952 _refine_ls_restrained_S_all 0.952 _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 0.15461(19) 0.26731(19) 0.38008(18) 0.0524(7) Uani 1 1 d . . . Co2 Co 0.5000 0.5000 0.5000 0.0436(7) Uani 1 2 d S . . Co3 Co -0.0809(2) 0.2996(2) 0.16360(19) 0.0596(7) Uani 1 1 d . . . O1 O 0.0491(10) -0.1563(9) 0.6252(9) 0.062(3) Uani 1 1 d . . . O2 O 0.2713(10) 0.1738(9) 0.4377(9) 0.055(3) Uani 1 1 d . . . O3 O 0.3592(9) 0.3902(9) 0.3311(8) 0.049(2) Uani 1 1 d . . . O5 O 0.1401(8) 0.3449(9) 0.2393(7) 0.046(2) Uani 1 1 d . . . O6 O 0.4866(10) 0.3222(9) 0.5299(10) 0.061(3) Uani 1 1 d . . . O7 O 0.1703(11) -0.1379(10) 0.7938(9) 0.065(3) Uani 1 1 d . . . O8 O 0.0966(10) 0.6160(10) -0.0373(9) 0.060(3) Uani 1 1 d . . . O9 O -0.018(3) 0.140(3) 0.007(3) 0.269(15) Uani 1 1 d . . . O10 O 0.3059(11) 0.7277(11) -0.0762(10) 0.082(4) Uani 1 1 d . . . O11 O 0.7250(13) 0.0155(16) 0.8139(11) 0.106(5) Uani 1 1 d . . . O12 O 0.8249(12) 0.1591(15) 0.7355(15) 0.122(6) Uani 1 1 d . . . O13 O 0.7898(12) 0.7564(13) 0.1090(11) 0.091(4) Uani 1 1 d . . . O14 O 0.8027(12) 0.6589(13) 0.2299(12) 0.095(4) Uani 1 1 d . . . N1 N 0.1623(12) 0.4218(11) 0.5296(9) 0.043(3) Uani 1 1 d . . . N2 N 0.2992(11) 0.5165(12) 0.5727(10) 0.046(3) Uani 1 1 d . . . N3 N 0.1356(12) 0.5761(14) 0.6895(12) 0.060(4) Uani 1 1 d . . . N4 N 0.7187(15) 0.0825(15) 0.7547(14) 0.079(4) Uani 1 1 d . . . N5 N 0.7350(13) 0.6899(12) 0.1650(12) 0.061(3) Uani 1 1 d . . . C1 C 0.3848(15) 0.2157(13) 0.5108(14) 0.051(4) Uani 1 1 d . . . C2 C 0.4106(13) 0.1351(12) 0.5828(11) 0.044(3) Uani 1 1 d . . . C3 C 0.2863(14) 0.0446(11) 0.5994(12) 0.044(3) Uani 1 1 d . . . H3 H 0.1917 0.0298 0.5601 0.053 Uiso 1 1 calc R . . C4 C 0.3038(15) -0.0244(15) 0.6755(13) 0.057(4) Uani 1 1 d . . . C5 C 0.4395(15) -0.0076(13) 0.7301(13) 0.056(4) Uani 1 1 d . . . H5 H 0.4479 -0.0474 0.7866 0.067 Uiso 1 1 calc R . . C6 C 0.5658(14) 0.0684(14) 0.7028(13) 0.053(4) Uani 1 1 d . . . C7 C 0.5509(15) 0.1453(13) 0.6344(13) 0.050(3) Uani 1 1 d . . . H7 H 0.6362 0.2044 0.6230 0.061 Uiso 1 1 calc R . . C8 C 0.1629(15) -0.1105(15) 0.7050(14) 0.054(4) Uani 1 1 d . . . C9 C 0.2821(14) 0.4076(12) 0.2559(11) 0.042(3) Uani 1 1 d . . . C10 C 0.3504(13) 0.4966(12) 0.1884(11) 0.036(3) Uani 1 1 d . . . C11 C 0.2568(15) 0.5349(13) 0.1170(12) 0.050(4) Uani 1 1 d . . . H11 H 0.1519 0.5050 0.1102 0.061 Uiso 1 1 calc R . . C12 C 0.3276(14) 0.6174(13) 0.0588(11) 0.044(3) Uani 1 1 d . . . C13 C 0.4848(14) 0.6712(13) 0.0739(11) 0.049(4) Uani 1 1 d . . . H13 H 0.5305 0.7308 0.0370 0.059 Uiso 1 1 calc R . . C14 C 0.5707(13) 0.6319(13) 0.1467(11) 0.041(3) Uani 1 1 d . . . C15 C 0.5030(13) 0.5493(12) 0.2052(11) 0.040(3) Uani 1 1 d . . . H15 H 0.5617 0.5288 0.2570 0.048 Uiso 1 1 calc R . . C16 C 0.2403(16) 0.6603(13) -0.0216(11) 0.050(4) Uani 1 1 d . . . C17 C 0.2801(14) 0.6062(14) 0.6615(13) 0.048(4) Uani 1 1 d . . . H17 H 0.3549 0.6834 0.7028 0.057 Uiso 1 1 calc R . . C18 C 0.0696(15) 0.4615(16) 0.6030(15) 0.060(4) Uani 1 1 d . . . H18 H -0.0317 0.4155 0.5965 0.072 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0474(10) 0.0495(12) 0.0662(14) 0.0381(12) -0.0035(9) 0.0007(8) Co2 0.0362(12) 0.0393(15) 0.0653(18) 0.0331(15) 0.0044(11) 0.0081(10) Co3 0.0497(11) 0.0741(15) 0.0718(15) 0.0538(13) 0.0019(9) 0.0094(10) O1 0.049(5) 0.047(6) 0.090(8) 0.041(6) -0.013(5) -0.005(4) O2 0.052(5) 0.039(6) 0.075(7) 0.026(6) -0.002(5) 0.007(4) O3 0.049(5) 0.042(5) 0.061(6) 0.029(5) -0.009(4) 0.007(4) O5 0.035(4) 0.057(6) 0.047(6) 0.025(5) 0.001(4) 0.007(4) O6 0.051(5) 0.042(6) 0.105(9) 0.046(6) 0.010(5) 0.009(4) O7 0.076(7) 0.057(7) 0.050(6) 0.022(6) -0.011(5) -0.009(5) O8 0.045(5) 0.079(8) 0.073(7) 0.048(7) 0.004(5) 0.017(5) O9 0.34(4) 0.33(4) 0.24(3) 0.17(3) 0.10(3) 0.18(3) O10 0.075(7) 0.078(8) 0.109(10) 0.074(8) -0.015(6) -0.006(6) O11 0.080(8) 0.171(15) 0.094(10) 0.073(11) -0.016(7) 0.048(9) O12 0.048(7) 0.128(13) 0.212(17) 0.106(13) -0.004(8) 0.002(7) O13 0.062(7) 0.114(11) 0.119(11) 0.083(10) 0.014(6) 0.007(7) O14 0.064(7) 0.113(11) 0.135(11) 0.088(10) 0.002(7) 0.016(7) N1 0.048(6) 0.045(7) 0.046(7) 0.020(6) 0.013(5) 0.025(5) N2 0.045(6) 0.042(7) 0.044(7) 0.017(6) -0.010(5) -0.002(5) N3 0.042(6) 0.082(10) 0.072(9) 0.052(9) 0.004(6) 0.013(6) N4 0.066(9) 0.070(10) 0.093(12) 0.023(9) -0.024(8) 0.011(8) N5 0.054(7) 0.053(8) 0.080(10) 0.035(8) -0.002(6) 0.005(6) C1 0.053(8) 0.035(8) 0.080(11) 0.031(8) 0.019(8) 0.018(6) C2 0.045(7) 0.038(8) 0.053(9) 0.024(7) 0.005(6) 0.007(6) C3 0.051(7) 0.018(6) 0.054(9) 0.006(7) -0.006(6) 0.002(5) C4 0.056(8) 0.063(11) 0.065(10) 0.040(9) 0.004(7) 0.012(7) C5 0.062(8) 0.039(8) 0.082(11) 0.039(9) 0.005(8) 0.014(7) C6 0.047(7) 0.044(9) 0.063(10) 0.019(8) -0.010(7) 0.004(6) C7 0.057(8) 0.030(7) 0.064(10) 0.013(8) 0.015(7) 0.015(6) C8 0.050(8) 0.064(10) 0.074(11) 0.045(9) 0.019(7) 0.031(7) C9 0.051(7) 0.036(7) 0.045(8) 0.019(7) 0.024(6) 0.015(6) C10 0.049(7) 0.032(7) 0.033(7) 0.013(6) 0.015(5) 0.018(5) C11 0.056(8) 0.041(8) 0.048(9) 0.022(7) -0.009(6) -0.006(6) C12 0.054(7) 0.042(8) 0.039(8) 0.017(7) 0.009(6) 0.012(6) C13 0.063(8) 0.051(9) 0.037(8) 0.026(7) -0.008(6) 0.011(7) C14 0.037(6) 0.050(8) 0.046(8) 0.021(7) 0.008(6) 0.019(6) C15 0.043(7) 0.032(7) 0.047(8) 0.016(7) 0.001(6) 0.011(6) C16 0.078(10) 0.047(9) 0.036(8) 0.022(7) 0.000(7) 0.027(7) C17 0.047(8) 0.038(8) 0.058(10) 0.027(8) 0.003(7) -0.001(6) C18 0.040(7) 0.074(11) 0.088(13) 0.058(11) 0.011(8) 0.016(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O2 1.922(8) . ? Co1 O1 1.951(8) 2_556 ? Co1 N1 2.033(12) . ? Co1 O5 2.140(7) . ? Co1 O3 2.238(8) . ? Co2 N2 2.087(11) 2_666 ? Co2 N2 2.087(11) . ? Co2 O6 2.088(7) . ? Co2 O6 2.088(7) 2_666 ? Co2 O3 2.182(9) . ? Co2 O3 2.182(9) 2_666 ? Co3 O7 2.002(9) 2_556 ? Co3 N3 2.025(15) 2_566 ? Co3 O8 2.037(8) 2_565 ? Co3 O5 2.077(8) . ? Co3 O10 2.202(10) 2_565 ? Co3 O9 2.34(3) . ? Co3 C16 2.437(11) 2_565 ? O1 C8 1.282(16) . ? O1 Co1 1.951(8) 2_556 ? O2 C1 1.235(16) . ? O3 C9 1.225(14) . ? O5 C9 1.292(14) . ? O6 C1 1.257(15) . ? O7 C8 1.202(15) . ? O7 Co3 2.002(9) 2_556 ? O8 C16 1.275(15) . ? O8 Co3 2.037(8) 2_565 ? O10 C16 1.205(15) . ? O10 Co3 2.202(10) 2_565 ? O11 N4 1.190(16) . ? O12 N4 1.201(17) . ? O13 N5 1.179(13) . ? O14 N5 1.170(13) . ? N1 C18 1.295(16) . ? N1 N2 1.381(14) . ? N2 C17 1.256(16) . ? N3 C18 1.34(2) . ? N3 C17 1.365(15) . ? N3 Co3 2.025(15) 2_566 ? N4 C6 1.474(17) . ? N5 C14 1.465(15) . ? C1 C2 1.480(15) . ? C2 C7 1.380(17) . ? C2 C3 1.382(16) . ? C3 C4 1.394(16) . ? C4 C5 1.337(18) . ? C4 C8 1.525(18) . ? C5 C6 1.366(17) . ? C6 C7 1.386(16) . ? C9 C10 1.498(14) . ? C10 C15 1.359(15) . ? C10 C11 1.427(16) . ? C11 C12 1.369(15) . ? C12 C13 1.401(17) . ? C12 C16 1.500(15) . ? C13 C14 1.400(14) . ? C14 C15 1.364(15) . ? C16 Co3 2.437(11) 2_565 ? 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 O2 Co1 O1 100.0(4) . 2_556 ? O2 Co1 N1 101.0(4) . . ? O1 Co1 N1 100.1(4) 2_556 . ? O2 Co1 O5 140.5(4) . . ? O1 Co1 O5 104.7(3) 2_556 . ? N1 Co1 O5 104.4(4) . . ? O2 Co1 O3 92.5(3) . . ? O1 Co1 O3 162.3(4) 2_556 . ? N1 Co1 O3 89.6(4) . . ? O5 Co1 O3 58.3(3) . . ? N2 Co2 N2 180.000(2) 2_666 . ? N2 Co2 O6 87.4(4) 2_666 . ? N2 Co2 O6 92.6(4) . . ? N2 Co2 O6 92.6(4) 2_666 2_666 ? N2 Co2 O6 87.4(4) . 2_666 ? O6 Co2 O6 180.00(10) . 2_666 ? N2 Co2 O3 93.6(4) 2_666 . ? N2 Co2 O3 86.4(4) . . ? O6 Co2 O3 89.8(4) . . ? O6 Co2 O3 90.2(4) 2_666 . ? N2 Co2 O3 86.4(4) 2_666 2_666 ? N2 Co2 O3 93.6(4) . 2_666 ? O6 Co2 O3 90.2(4) . 2_666 ? O6 Co2 O3 89.8(4) 2_666 2_666 ? O3 Co2 O3 180.000(1) . 2_666 ? O7 Co3 N3 93.9(4) 2_556 2_566 ? O7 Co3 O8 142.8(4) 2_556 2_565 ? N3 Co3 O8 104.2(4) 2_566 2_565 ? O7 Co3 O5 99.0(4) 2_556 . ? N3 Co3 O5 91.9(4) 2_566 . ? O8 Co3 O5 112.4(3) 2_565 . ? O7 Co3 O10 87.9(4) 2_556 2_565 ? N3 Co3 O10 87.8(5) 2_566 2_565 ? O8 Co3 O10 61.1(3) 2_565 2_565 ? O5 Co3 O10 173.1(3) . 2_565 ? O7 Co3 O9 80.1(7) 2_556 . ? N3 Co3 O9 173.4(6) 2_566 . ? O8 Co3 O9 82.4(6) 2_565 . ? O5 Co3 O9 86.3(8) . . ? O10 Co3 O9 94.7(8) 2_565 . ? O7 Co3 C16 115.4(4) 2_556 2_565 ? N3 Co3 C16 96.3(4) 2_566 2_565 ? O8 Co3 C16 31.5(4) 2_565 2_565 ? O5 Co3 C16 143.9(4) . 2_565 ? O10 Co3 C16 29.6(4) 2_565 2_565 ? O9 Co3 C16 88.9(7) . 2_565 ? C8 O1 Co1 131.2(8) . 2_556 ? C1 O2 Co1 130.5(9) . . ? C9 O3 Co2 140.6(9) . . ? C9 O3 Co1 91.4(7) . . ? Co2 O3 Co1 103.6(3) . . ? C9 O5 Co3 153.0(7) . . ? C9 O5 Co1 94.1(6) . . ? Co3 O5 Co1 112.4(3) . . ? C1 O6 Co2 135.0(8) . . ? C8 O7 Co3 134.3(11) . 2_556 ? C16 O8 Co3 91.8(6) . 2_565 ? C16 O10 Co3 86.1(8) . 2_565 ? C18 N1 N2 104.7(12) . . ? C18 N1 Co1 137.5(11) . . ? N2 N1 Co1 117.8(9) . . ? C17 N2 N1 108.5(11) . . ? C17 N2 Co2 128.3(9) . . ? N1 N2 Co2 123.2(10) . . ? C18 N3 C17 102.6(13) . . ? C18 N3 Co3 138.7(10) . 2_566 ? C17 N3 Co3 118.7(12) . 2_566 ? O11 N4 O12 125.5(14) . . ? O11 N4 C6 115.5(14) . . ? O12 N4 C6 119.0(13) . . ? O14 N5 O13 124.9(12) . . ? O14 N5 C14 116.1(10) . . ? O13 N5 C14 118.9(11) . . ? O2 C1 O6 126.1(11) . . ? O2 C1 C2 119.2(12) . . ? O6 C1 C2 114.6(13) . . ? C7 C2 C3 118.3(10) . . ? C7 C2 C1 123.9(11) . . ? C3 C2 C1 117.8(11) . . ? C2 C3 C4 119.5(12) . . ? C5 C4 C3 121.2(12) . . ? C5 C4 C8 119.8(11) . . ? C3 C4 C8 118.8(11) . . ? C4 C5 C6 119.8(12) . . ? C5 C6 C7 119.6(12) . . ? C5 C6 N4 121.8(12) . . ? C7 C6 N4 118.3(12) . . ? C2 C7 C6 120.6(12) . . ? O7 C8 O1 125.8(13) . . ? O7 C8 C4 119.0(13) . . ? O1 C8 C4 115.0(11) . . ? O3 C9 O5 115.9(9) . . ? O3 C9 C10 121.3(11) . . ? O5 C9 C10 122.7(10) . . ? C15 C10 C11 120.8(10) . . ? C15 C10 C9 118.2(10) . . ? C11 C10 C9 120.8(11) . . ? C12 C11 C10 117.3(12) . . ? C11 C12 C13 122.5(11) . . ? C11 C12 C16 121.8(12) . . ? C13 C12 C16 115.7(10) . . ? C14 C13 C12 117.5(10) . . ? C15 C14 C13 121.1(11) . . ? C15 C14 N5 120.9(10) . . ? C13 C14 N5 117.8(10) . . ? C10 C15 C14 120.6(10) . . ? O10 C16 O8 121.0(10) . . ? O10 C16 C12 120.3(13) . . ? O8 C16 C12 118.5(11) . . ? O10 C16 Co3 64.3(7) . 2_565 ? O8 C16 Co3 56.7(5) . 2_565 ? C12 C16 Co3 172.7(10) . 2_565 ? N2 C17 N3 111.3(13) . . ? N1 C18 N3 112.6(13) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 1.676 _refine_diff_density_min -1.234 _refine_diff_density_rms 0.197 ######END####### data_CompoundII _database_code_depnum_ccdc_archive 'CCDC 849290' #TrackingRef 'CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Co-Nitroisophthalate _chemical_melting_point ? _chemical_formula_moiety 'C10 H7 Co2 N5 O9' _chemical_formula_sum 'C10 H7 Co2 N5 O9' _chemical_formula_weight 459.07 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M ' P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.5193(2) _cell_length_b 12.5170(2) _cell_length_c 11.5835(2) _cell_angle_alpha 90.00 _cell_angle_beta 103.7230(10) _cell_angle_gamma 90.00 _cell_volume 1481.66(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3301 _cell_measurement_theta_min 2.86 _cell_measurement_theta_max 27.56 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.058 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 912 _exptl_absorpt_coefficient_mu 2.303 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6559 _exptl_absorpt_correction_T_max 0.9135 _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 Smart CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11859 _diffrn_reflns_av_R_equivalents 0.0196 _diffrn_reflns_av_sigmaI/netI 0.0174 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.86 _diffrn_reflns_theta_max 27.56 _reflns_number_total 3301 _reflns_number_gt 3134 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SAINT (Bruker, 2000)' _computing_data_reduction SAINT _computing_structure_solution 'SIR92 (Altomare et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1999) and CAMERON (Watkin et al., 1993)' _computing_publication_material 'PLATON (Spek, 2003)' _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^)+(0.0373P)^2^+1.2883P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3301 _refine_ls_number_parameters 239 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0276 _refine_ls_R_factor_gt 0.0261 _refine_ls_wR_factor_ref 0.0686 _refine_ls_wR_factor_gt 0.0677 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.56971(2) 0.112186(18) 0.01223(2) 0.01615(8) Uani 1 1 d . . . Co2 Co 0.46289(2) 0.062529(18) 0.25104(2) 0.01607(8) Uani 1 1 d . . . O1 O 0.42381(12) 0.03265(10) 0.07309(11) 0.0161(2) Uani 1 1 d D . . O2 O 0.7226(2) 0.1737(2) -0.05537(19) 0.0646(7) Uani 1 1 d . . . O3 O 0.72245(16) 0.05278(13) 0.16095(15) 0.0331(3) Uani 1 1 d . . . O4 O 0.65683(15) 0.08399(16) 0.32754(15) 0.0357(4) Uani 1 1 d . . . O5 O 1.34076(15) 0.10521(13) 0.35741(18) 0.0364(4) Uani 1 1 d . . . O6 O 0.9563(2) 0.1820(2) 0.6873(2) 0.0638(7) Uani 1 1 d . . . O7 O 1.1617(2) 0.1817(2) 0.7036(2) 0.0614(6) Uani 1 1 d . . . O8 O 1.2101(2) 0.0439(2) 0.1970(2) 0.0642(6) Uani 1 1 d . . . O100 O 0.9675(9) 0.1052(5) -0.0381(8) 0.222(4) Uani 1 1 d . . . N1 N 0.53811(17) 0.24640(12) 0.10837(14) 0.0218(3) Uani 1 1 d . . . N2 N 0.42375(16) 0.33504(13) 0.35261(14) 0.0200(3) Uani 1 1 d . . . H2A H 0.3968 0.2808 0.3857 0.024 Uiso 1 1 calc R . . H2B H 0.4217 0.3978 0.3824 0.024 Uiso 1 1 calc R . . N3 N 0.52304(17) 0.40142(12) 0.19822(15) 0.0216(3) Uani 1 1 d . . . N4 N 0.47689(16) 0.22736(12) 0.20012(14) 0.0200(3) Uani 1 1 d . . . N5 N 1.0509(2) 0.17160(17) 0.64555(19) 0.0367(4) Uani 1 1 d . . . C1 C 0.74319(19) 0.07535(15) 0.26971(19) 0.0238(4) Uani 1 1 d . . . C2 C 0.88164(19) 0.09394(16) 0.33843(18) 0.0227(4) Uani 1 1 d . . . C3 C 0.9868(2) 0.08153(17) 0.2865(2) 0.0261(4) Uani 1 1 d . . . H3 H 0.9723 0.0618 0.2070 0.031 Uiso 1 1 calc R . . C4 C 1.1144(2) 0.09859(17) 0.3529(2) 0.0272(4) Uani 1 1 d . . . C5 C 1.1370(2) 0.13007(17) 0.4706(2) 0.0286(4) Uani 1 1 d . . . H5 H 1.2215 0.1430 0.5152 0.034 Uiso 1 1 calc R . . C6 C 1.0304(2) 0.14166(17) 0.52012(19) 0.0259(4) Uani 1 1 d . . . C7 C 0.90362(19) 0.12351(16) 0.45668(19) 0.0238(4) Uani 1 1 d . . . H7 H 0.8341 0.1310 0.4928 0.029 Uiso 1 1 calc R . . C8 C 1.2285(2) 0.08137(19) 0.2969(2) 0.0357(5) Uani 1 1 d . . . C9 C 0.47120(17) 0.32120(14) 0.24992(16) 0.0178(3) Uani 1 1 d . . . C10 C 0.5624(2) 0.34964(15) 0.11025(17) 0.0227(4) Uani 1 1 d . . . H10 H 0.6024 0.3834 0.0567 0.027 Uiso 1 1 calc R . . H1A H 0.3506(16) 0.063(2) 0.048(2) 0.037(8) Uiso 1 1 d 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 Co1 0.02179(14) 0.01311(13) 0.01487(13) -0.00180(8) 0.00693(9) -0.00251(8) Co2 0.02152(13) 0.01300(13) 0.01478(13) -0.00037(8) 0.00647(9) -0.00083(8) O1 0.0184(6) 0.0147(6) 0.0161(6) -0.0017(5) 0.0059(5) 0.0002(5) O2 0.0529(12) 0.0939(18) 0.0446(11) 0.0183(11) 0.0068(9) -0.0450(13) O3 0.0291(8) 0.0327(8) 0.0326(8) -0.0063(7) -0.0023(6) 0.0036(6) O4 0.0180(7) 0.0529(10) 0.0356(9) 0.0101(8) 0.0051(6) -0.0017(7) O5 0.0228(8) 0.0295(8) 0.0636(12) 0.0089(8) 0.0235(8) 0.0040(6) O6 0.0558(13) 0.0931(19) 0.0471(12) -0.0347(12) 0.0212(10) -0.0086(12) O7 0.0421(11) 0.0871(17) 0.0450(11) -0.0236(11) -0.0097(9) 0.0035(11) O8 0.0502(12) 0.0944(18) 0.0602(14) -0.0174(13) 0.0371(11) 0.0011(12) O100 0.307(10) 0.140(5) 0.289(9) -0.033(5) 0.211(9) 0.014(5) N1 0.0348(9) 0.0157(7) 0.0176(7) -0.0018(6) 0.0116(7) -0.0018(6) N2 0.0275(8) 0.0155(7) 0.0188(7) -0.0031(6) 0.0089(6) -0.0032(6) N3 0.0334(9) 0.0139(7) 0.0189(8) -0.0024(6) 0.0093(7) -0.0028(6) N4 0.0297(8) 0.0154(7) 0.0165(7) -0.0013(6) 0.0089(6) -0.0020(6) N5 0.0370(10) 0.0347(10) 0.0363(11) -0.0110(8) 0.0044(8) 0.0004(8) C1 0.0206(9) 0.0192(9) 0.0301(10) 0.0042(7) 0.0028(8) 0.0006(7) C2 0.0184(9) 0.0208(9) 0.0289(10) 0.0004(8) 0.0058(7) 0.0003(7) C3 0.0265(10) 0.0261(9) 0.0281(10) -0.0007(8) 0.0111(8) 0.0011(8) C4 0.0215(9) 0.0247(9) 0.0392(12) 0.0018(9) 0.0148(9) 0.0012(7) C5 0.0178(9) 0.0270(10) 0.0406(12) -0.0008(9) 0.0061(8) -0.0004(7) C6 0.0238(9) 0.0235(9) 0.0300(10) -0.0047(8) 0.0055(8) 0.0002(7) C7 0.0182(8) 0.0235(9) 0.0312(10) -0.0028(8) 0.0089(8) 0.0017(7) C8 0.0285(11) 0.0304(11) 0.0561(15) 0.0058(10) 0.0257(11) 0.0042(9) C9 0.0216(8) 0.0149(8) 0.0165(8) -0.0007(6) 0.0037(7) -0.0019(6) C10 0.0338(10) 0.0177(8) 0.0187(8) -0.0011(7) 0.0105(8) -0.0034(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 2.0736(12) 3_655 ? Co1 N1 2.0853(15) . ? Co1 O1 2.0874(12) . ? Co1 O2 2.0954(19) . ? Co1 O3 2.1883(16) . ? Co1 N2 2.2058(16) 4_565 ? Co2 O1 2.0386(13) . ? Co2 O4 2.0400(15) . ? Co2 O5 2.0507(16) 1_455 ? Co2 N3 2.0959(16) 2_645 ? Co2 N4 2.1605(16) . ? O1 Co1 2.0736(12) 3_655 ? O3 C1 1.259(3) . ? O4 C1 1.255(3) . ? O5 C8 1.258(3) . ? O5 Co2 2.0507(16) 1_655 ? O6 N5 1.213(3) . ? O7 N5 1.206(3) . ? O8 C8 1.220(4) . ? N1 C10 1.316(2) . ? N1 N4 1.388(2) . ? N2 C9 1.406(2) . ? N2 Co1 2.2058(16) 4_566 ? N3 C9 1.349(2) . ? N3 C10 1.353(2) . ? N3 Co2 2.0959(16) 2_655 ? N4 C9 1.316(2) . ? N5 C6 1.466(3) . ? C1 C2 1.503(3) . ? C2 C7 1.384(3) . ? C2 C3 1.388(3) . ? C3 C4 1.396(3) . ? C4 C5 1.385(3) . ? C4 C8 1.509(3) . ? C5 C6 1.382(3) . ? C6 C7 1.380(3) . ? 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 O1 Co1 N1 170.49(6) 3_655 . ? O1 Co1 O1 81.60(5) 3_655 . ? N1 Co1 O1 88.90(6) . . ? O1 Co1 O2 91.61(9) 3_655 . ? N1 Co1 O2 97.90(9) . . ? O1 Co1 O2 173.00(9) . . ? O1 Co1 O3 88.69(6) 3_655 . ? N1 Co1 O3 91.93(6) . . ? O1 Co1 O3 91.92(6) . . ? O2 Co1 O3 86.20(8) . . ? O1 Co1 N2 87.55(5) 3_655 4_565 ? N1 Co1 N2 92.23(6) . 4_565 ? O1 Co1 N2 90.26(5) . 4_565 ? O2 Co1 N2 91.16(7) . 4_565 ? O3 Co1 N2 175.34(6) . 4_565 ? O1 Co2 O4 113.85(6) . . ? O1 Co2 O5 130.58(6) . 1_455 ? O4 Co2 O5 114.16(7) . 1_455 ? O1 Co2 N3 95.22(6) . 2_645 ? O4 Co2 N3 90.46(7) . 2_645 ? O5 Co2 N3 95.44(6) 1_455 2_645 ? O1 Co2 N4 84.81(6) . . ? O4 Co2 N4 82.35(7) . . ? O5 Co2 N4 90.47(6) 1_455 . ? N3 Co2 N4 172.12(7) 2_645 . ? Co2 O1 Co1 128.37(6) . 3_655 ? Co2 O1 Co1 105.42(6) . . ? Co1 O1 Co1 98.40(5) 3_655 . ? C1 O3 Co1 129.22(14) . . ? C1 O4 Co2 122.20(15) . . ? C8 O5 Co2 104.03(16) . 1_655 ? C10 N1 N4 106.22(15) . . ? C10 N1 Co1 138.14(13) . . ? N4 N1 Co1 115.62(11) . . ? C9 N2 Co1 115.46(12) . 4_566 ? C9 N3 C10 101.88(15) . . ? C9 N3 Co2 126.93(13) . 2_655 ? C10 N3 Co2 131.18(13) . 2_655 ? C9 N4 N1 105.07(14) . . ? C9 N4 Co2 136.01(12) . . ? N1 N4 Co2 116.56(11) . . ? O7 N5 O6 122.8(2) . . ? O7 N5 C6 118.4(2) . . ? O6 N5 C6 118.8(2) . . ? O4 C1 O3 125.3(2) . . ? O4 C1 C2 115.93(19) . . ? O3 C1 C2 118.75(18) . . ? C7 C2 C3 119.72(19) . . ? C7 C2 C1 118.61(17) . . ? C3 C2 C1 121.67(19) . . ? C2 C3 C4 120.3(2) . . ? C5 C4 C3 120.33(18) . . ? C5 C4 C8 119.7(2) . . ? C3 C4 C8 119.9(2) . . ? C6 C5 C4 118.1(2) . . ? C7 C6 C5 122.6(2) . . ? C7 C6 N5 117.78(18) . . ? C5 C6 N5 119.65(19) . . ? C6 C7 C2 118.96(18) . . ? O8 C8 O5 122.4(2) . . ? O8 C8 C4 120.0(2) . . ? O5 C8 C4 117.6(2) . . ? N4 C9 N3 113.86(16) . . ? N4 C9 N2 122.89(16) . . ? N3 C9 N2 123.11(16) . . ? N1 C10 N3 112.96(17) . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 1.262 _refine_diff_density_min -0.648 _refine_diff_density_rms 0.072 ######END####### data_CompoundIII _database_code_depnum_ccdc_archive 'CCDC 849291' #TrackingRef 'CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Co-Nitroisophthalate _chemical_melting_point ? _chemical_formula_moiety 'C10 H11 Co2 N6 O9' _chemical_formula_sum 'C10 H11 Co2 N6 O9' _chemical_formula_weight 477.11 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M ' P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.0633(6) _cell_length_b 12.5347(5) _cell_length_c 11.1579(7) _cell_angle_alpha 90.00 _cell_angle_beta 104.120(6) _cell_angle_gamma 90.00 _cell_volume 1500.57(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2960 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 26.00 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.112 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 956 _exptl_absorpt_coefficient_mu 2.280 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8753 _exptl_absorpt_correction_T_max 0.9558 _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 Smart CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15573 _diffrn_reflns_av_R_equivalents 0.0806 _diffrn_reflns_av_sigmaI/netI 0.0633 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 26.00 _reflns_number_total 2960 _reflns_number_gt 2143 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SAINT (Bruker, 2000)' _computing_data_reduction SAINT _computing_structure_solution 'SIR92 (Altomare et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1999) and CAMERON (Watkin et al., 1993)' _computing_publication_material 'PLATON (Spek, 2003)' _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^)+(0.0869P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2960 _refine_ls_number_parameters 256 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0830 _refine_ls_R_factor_gt 0.0541 _refine_ls_wR_factor_ref 0.1534 _refine_ls_wR_factor_gt 0.1391 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.048 _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 -0.00643(6) 0.06602(6) 0.77804(6) 0.0178(2) Uani 1 1 d . . . Co2 Co 0.06737(7) 0.10887(6) 0.50728(6) 0.0187(2) Uani 1 1 d . . . O1 O 0.8330(4) 0.0933(3) 0.8328(4) 0.0293(10) Uani 1 1 d . . . O2 O 0.1848(4) 0.0720(3) 0.8071(4) 0.0318(10) Uani 1 1 d . . . O3 O 0.0601(3) -0.0298(3) 0.4099(3) 0.0178(8) Uani 1 1 d D . . O4 O 0.2384(4) 0.0535(3) 0.6302(4) 0.0293(10) Uani 1 1 d . . . O5 O 0.2055(4) 0.1869(4) 0.4281(4) 0.0401(11) Uani 1 1 d D . . O6 O 0.4729(5) 0.1784(4) 1.1750(4) 0.0522(14) Uani 1 1 d . . . O7 O 0.6695(5) 0.1769(4) 1.1905(4) 0.0580(15) Uani 1 1 d . . . O8 O 0.7014(5) 0.0646(6) 0.6511(5) 0.086(2) Uani 1 1 d . . . O100 O 0.4435(9) 0.1159(6) 0.4436(7) 0.116(3) Uani 1 1 d . . . N1 N -0.0054(4) 0.4008(3) 0.6748(4) 0.0172(9) Uani 1 1 d . . . H1 H -0.0154 0.4685 0.6805 0.021 Uiso 1 1 calc R . . N2 N -0.0088(4) 0.2261(3) 0.7117(4) 0.0189(10) Uani 1 1 d . . . N3 N 0.0450(4) 0.2424(3) 0.6108(4) 0.0205(10) Uani 1 1 d . . . N4 N -0.0830(4) 0.3371(3) 0.8489(4) 0.0178(9) Uani 1 1 d . . . H4A H -0.0940 0.2836 0.8933 0.021 Uiso 1 1 calc R . . H4B H -0.1006 0.4005 0.8688 0.021 Uiso 1 1 calc R . . N5 N 0.0894(4) 0.3960(4) 0.5040(4) 0.0250(11) Uani 1 1 d . . . H5A H 0.1198 0.3584 0.4539 0.030 Uiso 1 1 calc R . . H5B H 0.0870 0.4644 0.4975 0.030 Uiso 1 1 calc R . . N6 C 0.5632(5) 0.1669(4) 1.1303(5) 0.0219(12) Uani 1 1 d . . . C1 C 0.2630(5) 0.0701(4) 0.7431(5) 0.0225(12) Uani 1 1 d . . . C2 C 0.3959(5) 0.0906(4) 0.8119(5) 0.0230(12) Uani 1 1 d . . . C3 C 0.4196(5) 0.1206(4) 0.9359(5) 0.0252(13) Uani 1 1 d . . . H3 H 0.3547 0.1277 0.9749 0.030 Uiso 1 1 calc R . . C4 C 0.5403(5) 0.1393(5) 0.9990(5) 0.0253(13) Uani 1 1 d . . . C5 C 0.6403(5) 0.1265(5) 0.9477(6) 0.0305(14) Uani 1 1 d . . . H5 H 0.7214 0.1369 0.9943 0.037 Uiso 1 1 calc R . . C6 C 0.6165(5) 0.0976(5) 0.8241(6) 0.0287(14) Uani 1 1 d . . . C7 C 0.4956(5) 0.0809(5) 0.7567(6) 0.0300(14) Uani 1 1 d . . . H7 H 0.4805 0.0629 0.6735 0.036 Uiso 1 1 calc R . . C8 N 0.7238(6) 0.0830(5) 0.7614(6) 0.0555(17) Uani 1 1 d . . . C9 C 0.0446(5) 0.3467(4) 0.5948(4) 0.0190(11) Uani 1 1 d . . . C10 C -0.0363(5) 0.3210(4) 0.7441(5) 0.0198(12) Uani 1 1 d . . . H51 H 0.284(4) 0.156(6) 0.463(7) 0.08(3) Uiso 1 1 d D . . H52 H 0.161(8) 0.201(8) 0.346(3) 0.13(4) Uiso 1 1 d D . . H3A H 0.131(4) -0.059(6) 0.428(8) 0.09(3) Uiso 1 1 d 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 Co1 0.0157(4) 0.0179(4) 0.0208(4) 0.0005(3) 0.0066(3) -0.0003(3) Co2 0.0193(4) 0.0191(4) 0.0184(4) -0.0012(3) 0.0058(3) -0.0010(3) O1 0.012(2) 0.041(3) 0.035(2) 0.0054(19) 0.0064(17) 0.0036(17) O2 0.019(2) 0.055(3) 0.022(2) -0.0003(19) 0.0068(17) -0.0055(19) O3 0.017(2) 0.0168(19) 0.0197(19) -0.0039(15) 0.0055(15) 0.0018(15) O4 0.019(2) 0.041(3) 0.026(2) -0.0035(18) 0.0025(17) 0.0041(18) O5 0.029(3) 0.055(3) 0.036(3) 0.008(2) 0.006(2) -0.011(2) O6 0.048(3) 0.069(4) 0.037(3) -0.018(3) 0.006(2) -0.001(3) O7 0.035(3) 0.092(4) 0.041(3) -0.022(3) -0.004(2) 0.006(3) O8 0.028(3) 0.193(7) 0.039(3) -0.053(4) 0.008(2) -0.012(4) O100 0.192(10) 0.087(6) 0.079(5) -0.005(4) 0.048(5) 0.035(5) N1 0.024(3) 0.012(2) 0.018(2) 0.0023(18) 0.0089(19) 0.0009(18) N2 0.022(3) 0.018(2) 0.017(2) -0.0017(18) 0.0070(18) -0.0059(18) N3 0.026(3) 0.019(2) 0.019(2) -0.0017(19) 0.0088(18) 0.0003(19) N4 0.025(3) 0.014(2) 0.015(2) 0.0005(17) 0.0063(18) -0.0017(18) N5 0.035(3) 0.017(2) 0.025(3) 0.0040(19) 0.012(2) 0.002(2) N6 0.019(3) 0.029(3) 0.016(3) -0.008(2) 0.002(2) 0.002(2) C1 0.014(3) 0.025(3) 0.027(3) -0.003(2) 0.002(2) 0.000(2) C2 0.016(3) 0.028(3) 0.026(3) 0.003(2) 0.006(2) -0.001(2) C3 0.020(3) 0.033(3) 0.024(3) 0.002(3) 0.008(2) 0.004(2) C4 0.024(3) 0.025(3) 0.027(3) -0.007(2) 0.007(2) 0.002(2) C5 0.017(3) 0.034(3) 0.039(3) 0.003(3) 0.003(3) 0.001(2) C6 0.020(3) 0.035(3) 0.033(3) -0.001(3) 0.010(3) 0.000(3) C7 0.021(3) 0.043(4) 0.027(3) -0.002(3) 0.008(2) 0.004(3) C8 0.034(4) 0.072(5) 0.062(4) -0.010(3) 0.015(3) 0.000(3) C9 0.021(3) 0.022(3) 0.012(2) 0.000(2) 0.000(2) -0.001(2) C10 0.017(3) 0.024(3) 0.018(3) 0.000(2) 0.004(2) -0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 2.043(4) 1_455 ? Co1 O2 2.062(4) . ? Co1 O3 2.085(4) 3_556 ? Co1 N1 2.133(4) 2_546 ? Co1 N2 2.137(4) . ? Co2 O3 2.042(4) . ? Co2 N3 2.083(4) . ? Co2 O3 2.112(4) 3_556 ? Co2 O4 2.163(4) . ? Co2 O5 2.175(5) . ? Co2 N4 2.217(4) 4_565 ? O1 C8 1.281(7) . ? O1 Co1 2.043(4) 1_655 ? O2 C1 1.249(7) . ? O3 Co1 2.085(4) 3_556 ? O3 Co2 2.112(4) 3_556 ? O4 C1 1.240(6) . ? O6 N6 1.229(7) . ? O7 N6 1.210(7) . ? O8 C8 1.217(8) . ? N1 C9 1.342(7) . ? N1 C10 1.358(7) . ? N1 Co1 2.133(4) 2_556 ? N2 C10 1.301(7) . ? N2 N3 1.411(6) . ? N3 C9 1.319(7) . ? N4 C10 1.404(7) . ? N4 Co2 2.217(4) 4_566 ? N5 C9 1.378(7) . ? N6 C4 1.467(7) . ? C1 C2 1.506(7) . ? C2 C7 1.393(8) . ? C2 C3 1.396(8) . ? C3 C4 1.369(8) . ? C4 C5 1.374(8) . ? C5 C6 1.387(8) . ? C6 C7 1.382(8) . ? C6 C8 1.529(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 O1 Co1 O2 151.67(17) 1_455 . ? O1 Co1 O3 106.37(16) 1_455 3_556 ? O2 Co1 O3 101.30(15) . 3_556 ? O1 Co1 N1 95.40(16) 1_455 2_546 ? O2 Co1 N1 89.84(17) . 2_546 ? O3 Co1 N1 91.28(15) 3_556 2_546 ? O1 Co1 N2 90.51(16) 1_455 . ? O2 Co1 N2 86.90(17) . . ? O3 Co1 N2 83.07(15) 3_556 . ? N1 Co1 N2 172.79(17) 2_546 . ? O3 Co2 N3 170.17(17) . . ? O3 Co2 O3 83.69(15) . 3_556 ? N3 Co2 O3 87.25(15) . 3_556 ? O3 Co2 O4 88.78(15) . . ? N3 Co2 O4 96.33(16) . . ? O3 Co2 O4 98.40(15) 3_556 . ? O3 Co2 O5 96.13(17) . . ? N3 Co2 O5 93.10(18) . . ? O3 Co2 O5 177.39(16) 3_556 . ? O4 Co2 O5 78.99(17) . . ? O3 Co2 N4 84.92(15) . 4_565 ? N3 Co2 N4 91.67(17) . 4_565 ? O3 Co2 N4 92.33(15) 3_556 4_565 ? O4 Co2 N4 166.89(16) . 4_565 ? O5 Co2 N4 90.24(16) . 4_565 ? C8 O1 Co1 123.6(4) . 1_655 ? C1 O2 Co1 137.4(4) . . ? Co2 O3 Co1 133.25(18) . 3_556 ? Co2 O3 Co2 96.31(15) . 3_556 ? Co1 O3 Co2 106.33(16) 3_556 3_556 ? C1 O4 Co2 122.1(4) . . ? C9 N1 C10 102.0(4) . . ? C9 N1 Co1 130.1(4) . 2_556 ? C10 N1 Co1 125.7(3) . 2_556 ? C10 N2 N3 105.2(4) . . ? C10 N2 Co1 138.2(4) . . ? N3 N2 Co1 116.2(3) . . ? C9 N3 N2 105.2(4) . . ? C9 N3 Co2 136.0(4) . . ? N2 N3 Co2 117.1(3) . . ? C10 N4 Co2 110.5(3) . 4_566 ? O7 N6 O6 122.6(5) . . ? O7 N6 C4 119.1(5) . . ? O6 N6 C4 118.3(5) . . ? O4 C1 O2 125.0(5) . . ? O4 C1 C2 119.4(5) . . ? O2 C1 C2 115.6(5) . . ? C7 C2 C3 119.0(5) . . ? C7 C2 C1 122.6(5) . . ? C3 C2 C1 118.4(5) . . ? C4 C3 C2 118.6(5) . . ? C3 C4 C5 123.4(5) . . ? C3 C4 N6 117.6(5) . . ? C5 C4 N6 118.9(5) . . ? C4 C5 C6 117.9(5) . . ? C7 C6 C5 120.4(6) . . ? C7 C6 C8 119.3(6) . . ? C5 C6 C8 120.4(5) . . ? C6 C7 C2 120.7(6) . . ? O8 C8 O1 125.2(6) . . ? O8 C8 C6 119.8(6) . . ? O1 C8 C6 115.0(6) . . ? N3 C9 N1 113.5(5) . . ? N3 C9 N5 123.6(5) . . ? N1 C9 N5 122.9(5) . . ? N2 C10 N1 114.0(5) . . ? N2 C10 N4 121.5(5) . . ? N1 C10 N4 124.3(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.137 _refine_diff_density_min -0.690 _refine_diff_density_rms 0.150