# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Evamarie Hey-Hawkins' _publ_contact_author_email HEY@RZ.UNI-LEIPZIG.DE _publ_section_title ; Hydrogen-bonded pillars of alternating chiral complex cations and anions: 1. Synthesis, characterization, X-ray structure and thermal stability of catena-{[Co(H2oxado)3][Cr(C2O4)3]*5H2O} and of its precursor (H3oxado)- [Co(H2oxado)3](SO4)2*2H2O ; loop_ _publ_author_name 'Evamarie Hey-Hawkins' 'Michel M. Belombe' 'Peter Lonnecke' 'Felicite Majoumo-Mbe' ; Y.A.Mbiangue ; 'Justin Nenwa' #------------------------------------------------------------------------------# # DATA BLOCK # #------------------------------------------------------------------------------# data_c1256fin _database_code_depnum_ccdc_archive 'CCDC 700649' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H29 Co N16 O18 S2' _chemical_formula_weight 760.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _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 9.3133(16) _cell_length_b 10.9722(19) _cell_length_c 14.634(3) _cell_angle_alpha 87.182(3) _cell_angle_beta 84.305(4) _cell_angle_gamma 66.336(3) _cell_volume 1362.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 208(2) _cell_measurement_reflns_used 835 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 28.78 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.853 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 0.893 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 208(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 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9165 _diffrn_reflns_av_R_equivalents 0.0229 _diffrn_reflns_av_sigmaI/netI 0.0505 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 29.53 _reflns_number_total 6477 _reflns_number_gt 4977 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick,1997)' _computing_molecular_graphics 'ORTEP3 for Windows (L. J. Farrugia, 1997)' _computing_publication_material 'WINGX (L.J. Farrugia,1999)' _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^)+(0.0289P)^2^+2.8008P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6477 _refine_ls_number_parameters 522 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0811 _refine_ls_R_factor_gt 0.0533 _refine_ls_wR_factor_ref 0.1120 _refine_ls_wR_factor_gt 0.1008 _refine_ls_goodness_of_fit_ref 1.127 _refine_ls_restrained_S_all 1.127 _refine_ls_shift/su_max 0.003 _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 0.75264(5) 0.40927(5) 0.23342(3) 0.01555(11) Uani 1 1 d . . . S1 S 0.73787(10) 0.77596(8) 0.41286(6) 0.01846(18) Uani 1 1 d . . . S2 S 0.73175(10) 0.05251(8) 0.07363(6) 0.01995(18) Uani 1 1 d . . . O1 O 0.8398(3) 0.6346(2) 0.17542(18) 0.0230(5) Uani 1 1 d . . . O2 O 0.4776(3) 0.3753(3) 0.1701(2) 0.0256(6) Uani 1 1 d . . . O3 O 0.4817(3) 0.6286(2) 0.32369(19) 0.0242(6) Uani 1 1 d . . . O4 O 0.8488(3) 0.1255(2) 0.28918(18) 0.0217(5) Uani 1 1 d . . . O5 O 0.9224(3) 0.4243(3) 0.39165(16) 0.0218(5) Uani 1 1 d . . . O6 O 0.9164(3) 0.2837(3) 0.05633(17) 0.0235(5) Uani 1 1 d . . . O7 O 0.1382(4) 0.7711(3) 0.51165(18) 0.0326(7) Uani 1 1 d . . . O8 O 0.0516(3) 0.7728(3) 0.15307(17) 0.0261(6) Uani 1 1 d . . . O9 O 0.7658(3) 0.8975(2) 0.4102(2) 0.0296(6) Uani 1 1 d . . . O10 O 0.5816(3) 0.8013(3) 0.3823(2) 0.0368(7) Uani 1 1 d . . . O11 O 0.8599(3) 0.6758(2) 0.34911(17) 0.0257(6) Uani 1 1 d . . . O12 O 0.7473(3) 0.7155(3) 0.50430(17) 0.0324(6) Uani 1 1 d . . . O13 O 0.5838(3) 0.1161(3) 0.1322(2) 0.0346(7) Uani 1 1 d . . . O14 O 0.7141(3) 0.1114(3) -0.01850(17) 0.0289(6) Uani 1 1 d . . . O15 O 0.7775(3) -0.0919(2) 0.07123(18) 0.0266(6) Uani 1 1 d . . . O16 O 0.8592(3) 0.0765(3) 0.11300(19) 0.0329(6) Uani 1 1 d . . . N1 N 0.7368(3) 0.5710(3) 0.17379(19) 0.0186(6) Uani 1 1 d . . . N2 N 0.5852(3) 0.4357(3) 0.1567(2) 0.0192(6) Uani 1 1 d . . . N3 N 0.5929(4) 0.7460(3) 0.0786(2) 0.0257(7) Uani 1 1 d . . . N4 N 0.3844(4) 0.6041(3) 0.0845(2) 0.0250(7) Uani 1 1 d . . . N5 N 0.5874(3) 0.4956(3) 0.3282(2) 0.0188(6) Uani 1 1 d . . . N6 N 0.7382(3) 0.2570(3) 0.29587(19) 0.0162(6) Uani 1 1 d . . . N7 N 0.3790(4) 0.4643(3) 0.4133(2) 0.0286(7) Uani 1 1 d . . . N8 N 0.5898(4) 0.1822(3) 0.4050(3) 0.0276(7) Uani 1 1 d . . . N9 N 0.9295(3) 0.3905(3) 0.29981(18) 0.0165(6) Uani 1 1 d . . . N10 N 0.9244(3) 0.3075(3) 0.14824(18) 0.0175(6) Uani 1 1 d . . . N11 N 1.1926(4) 0.2502(3) 0.3157(2) 0.0258(7) Uani 1 1 d . . . N12 N 1.1965(4) 0.1910(3) 0.1232(2) 0.0266(7) Uani 1 1 d . . . N13 N 0.1394(4) 0.7544(3) 0.4169(2) 0.0233(6) Uani 1 1 d . . . N14 N 0.0430(4) 0.7990(3) 0.2460(2) 0.0238(7) Uani 1 1 d . . . N15 N 0.1503(5) 0.9676(4) 0.4069(3) 0.0330(8) Uani 1 1 d . . . N16 N 0.2061(4) 0.9095(3) 0.2144(2) 0.0252(7) Uani 1 1 d . . . C1 C 0.6221(4) 0.6306(3) 0.1220(2) 0.0168(6) Uani 1 1 d . . . C2 C 0.5223(4) 0.5539(3) 0.1194(2) 0.0174(7) Uani 1 1 d . . . C3 C 0.5206(4) 0.4203(3) 0.3691(2) 0.0203(7) Uani 1 1 d . . . C4 C 0.6212(4) 0.2766(3) 0.3581(2) 0.0184(7) Uani 1 1 d . . . C5 C 1.0664(4) 0.3020(3) 0.2694(2) 0.0179(7) Uani 1 1 d . . . C6 C 1.0659(4) 0.2635(3) 0.1736(2) 0.0186(7) Uani 1 1 d . . . C7 C 0.1381(4) 0.8596(3) 0.3729(2) 0.0216(7) Uani 1 1 d . . . C8 C 0.1310(4) 0.8558(3) 0.2724(2) 0.0206(7) Uani 1 1 d . . . O17 O 0.4385(3) 0.0032(3) 0.2617(2) 0.0297(6) Uani 1 1 d D . . O18 O 0.8574(5) 0.5057(4) -0.0695(3) 0.0582(10) Uani 1 1 d D . . H1O H 0.842(5) 0.648(4) 0.234(3) 0.030(12) Uiso 1 1 d . . . H2O H 0.525(5) 0.299(5) 0.159(3) 0.031(12) Uiso 1 1 d . . . H3A H 0.657(5) 0.785(4) 0.091(3) 0.036(12) Uiso 1 1 d . . . H3B H 0.511(5) 0.782(4) 0.054(3) 0.023(11) Uiso 1 1 d . . . H3O H 0.520(6) 0.679(5) 0.345(3) 0.046(15) Uiso 1 1 d . . . H4A H 0.327(5) 0.558(4) 0.092(3) 0.028(11) Uiso 1 1 d . . . H4B H 0.358(6) 0.682(5) 0.064(3) 0.044(14) Uiso 1 1 d . . . H4O H 0.848(5) 0.108(4) 0.235(3) 0.025(11) Uiso 1 1 d . . . H5O H 0.897(5) 0.507(5) 0.393(3) 0.042(14) Uiso 1 1 d . . . H6O H 0.893(5) 0.223(4) 0.059(3) 0.027(12) Uiso 1 1 d . . . H7A H 0.317(6) 0.552(6) 0.412(3) 0.054(15) Uiso 1 1 d . . . H7B H 0.345(5) 0.414(4) 0.438(3) 0.029(12) Uiso 1 1 d . . . H7O H 0.136(7) 0.695(6) 0.524(4) 0.072(19) Uiso 1 1 d . . . H8A H 0.648(5) 0.106(5) 0.395(3) 0.031(12) Uiso 1 1 d . . . H8B H 0.523(6) 0.201(5) 0.445(4) 0.054(17) Uiso 1 1 d . . . H8O H -0.035(7) 0.838(6) 0.133(4) 0.08(2) Uiso 1 1 d . . . H11A H 1.184(5) 0.272(4) 0.371(3) 0.031(12) Uiso 1 1 d . . . H11B H 1.272(5) 0.187(4) 0.294(3) 0.016(10) Uiso 1 1 d . . . H12A H 1.194(5) 0.169(4) 0.073(3) 0.029(12) Uiso 1 1 d . . . H12B H 1.280(6) 0.178(5) 0.137(3) 0.048(16) Uiso 1 1 d . . . H14 H -0.011(7) 0.763(6) 0.286(4) 0.071(18) Uiso 1 1 d . . . H15A H 0.152(5) 0.970(5) 0.465(4) 0.040(13) Uiso 1 1 d . . . H15B H 0.102(6) 1.038(5) 0.380(4) 0.052(16) Uiso 1 1 d . . . H16A H 0.194(6) 0.907(6) 0.145(4) 0.075(18) Uiso 1 1 d . . . H16B H 0.267(5) 0.939(5) 0.235(3) 0.038(13) Uiso 1 1 d . . . H17A H 0.506(6) 0.016(6) 0.214(3) 0.09(2) Uiso 1 1 d D . . H17B H 0.490(7) -0.050(6) 0.310(3) 0.10(2) Uiso 1 1 d D . . H18A H 0.878(16) 0.438(10) -0.022(7) 0.28(7) Uiso 1 1 d D . . H18B H 0.946(8) 0.454(9) -0.112(6) 0.19(4) 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 0.0160(2) 0.0140(2) 0.0164(2) 0.00123(16) -0.00103(16) -0.00602(17) S1 0.0199(4) 0.0155(4) 0.0206(4) -0.0007(3) 0.0010(3) -0.0082(3) S2 0.0263(4) 0.0152(4) 0.0180(4) 0.0014(3) -0.0020(3) -0.0081(3) O1 0.0269(14) 0.0254(14) 0.0237(14) 0.0034(11) -0.0039(11) -0.0177(11) O2 0.0180(13) 0.0179(14) 0.0436(17) 0.0010(12) -0.0049(11) -0.0097(11) O3 0.0194(12) 0.0106(12) 0.0394(16) -0.0021(10) -0.0012(11) -0.0028(10) O4 0.0237(13) 0.0128(12) 0.0219(14) -0.0002(10) -0.0011(10) -0.0004(10) O5 0.0291(14) 0.0171(13) 0.0184(12) -0.0024(10) -0.0020(10) -0.0082(11) O6 0.0305(14) 0.0270(14) 0.0172(13) -0.0007(10) -0.0028(10) -0.0158(12) O7 0.0481(18) 0.0321(16) 0.0194(14) 0.0050(12) -0.0028(12) -0.0185(14) O8 0.0268(14) 0.0300(15) 0.0211(13) -0.0015(11) -0.0050(11) -0.0101(12) O9 0.0286(14) 0.0172(13) 0.0443(17) -0.0015(11) 0.0026(12) -0.0117(11) O10 0.0254(15) 0.0246(15) 0.062(2) 0.0009(14) -0.0153(14) -0.0093(12) O11 0.0307(14) 0.0227(13) 0.0225(13) -0.0057(10) 0.0066(11) -0.0108(11) O12 0.0502(18) 0.0375(16) 0.0173(13) 0.0018(11) 0.0019(12) -0.0268(14) O13 0.0352(16) 0.0265(15) 0.0362(16) -0.0019(12) 0.0118(12) -0.0094(12) O14 0.0310(14) 0.0290(15) 0.0218(13) 0.0058(11) -0.0036(11) -0.0071(12) O15 0.0310(14) 0.0167(13) 0.0345(15) 0.0014(11) -0.0044(11) -0.0119(11) O16 0.0429(17) 0.0361(16) 0.0282(15) -0.0013(12) -0.0100(12) -0.0230(14) N1 0.0181(14) 0.0192(14) 0.0215(15) 0.0013(11) -0.0041(11) -0.0100(12) N2 0.0196(14) 0.0184(15) 0.0227(15) 0.0015(11) -0.0033(11) -0.0107(12) N3 0.0249(17) 0.0229(17) 0.0319(18) 0.0099(13) -0.0106(14) -0.0116(14) N4 0.0196(15) 0.0212(17) 0.0359(19) 0.0039(14) -0.0087(13) -0.0089(14) N5 0.0179(14) 0.0146(14) 0.0227(15) 0.0007(11) -0.0004(11) -0.0055(11) N6 0.0175(14) 0.0090(13) 0.0193(14) 0.0007(10) -0.0017(11) -0.0024(11) N7 0.0253(17) 0.0168(16) 0.040(2) -0.0002(14) 0.0100(14) -0.0075(14) N8 0.0286(18) 0.0176(17) 0.0344(19) 0.0003(14) 0.0088(15) -0.0098(14) N9 0.0212(14) 0.0159(14) 0.0112(13) 0.0003(10) -0.0021(10) -0.0060(11) N10 0.0197(14) 0.0198(14) 0.0141(14) -0.0012(11) -0.0017(11) -0.0089(12) N11 0.0214(16) 0.0279(18) 0.0208(17) -0.0050(13) -0.0033(13) -0.0012(14) N12 0.0214(17) 0.0330(19) 0.0224(18) -0.0056(14) 0.0001(13) -0.0078(14) N13 0.0249(16) 0.0248(16) 0.0191(15) 0.0006(12) -0.0016(12) -0.0088(13) N14 0.0259(16) 0.0271(17) 0.0207(16) 0.0026(12) -0.0016(12) -0.0135(14) N15 0.054(2) 0.0274(19) 0.0186(18) 0.0002(14) -0.0017(16) -0.0179(18) N16 0.0300(17) 0.0280(17) 0.0234(17) 0.0030(13) -0.0026(13) -0.0181(14) C1 0.0200(16) 0.0152(16) 0.0147(16) 0.0004(12) -0.0004(12) -0.0068(13) C2 0.0177(16) 0.0184(16) 0.0149(16) -0.0015(12) -0.0024(12) -0.0056(13) C3 0.0218(17) 0.0169(17) 0.0209(17) -0.0018(13) 0.0017(13) -0.0070(14) C4 0.0213(17) 0.0134(16) 0.0206(17) 0.0012(13) -0.0014(13) -0.0073(13) C5 0.0197(16) 0.0164(16) 0.0181(17) 0.0016(12) -0.0015(13) -0.0079(13) C6 0.0207(16) 0.0159(16) 0.0194(17) 0.0015(13) 0.0005(13) -0.0083(13) C7 0.0196(17) 0.0206(17) 0.0220(18) -0.0004(14) 0.0031(13) -0.0065(14) C8 0.0175(16) 0.0184(17) 0.0242(18) 0.0017(13) -0.0036(13) -0.0052(13) O17 0.0218(14) 0.0311(15) 0.0347(16) 0.0015(12) -0.0041(12) -0.0087(12) O18 0.053(2) 0.044(2) 0.074(3) -0.005(2) 0.006(2) -0.0186(18) _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 N1 1.896(3) . ? Co1 N6 1.911(3) . ? Co1 N10 1.915(3) . ? Co1 N5 1.930(3) . ? Co1 N9 1.930(3) . ? Co1 N2 1.931(3) . ? S1 O9 1.455(3) . ? S1 O12 1.459(3) . ? S1 O10 1.479(3) . ? S1 O11 1.502(2) . ? S2 O14 1.461(3) . ? S2 O15 1.468(3) . ? S2 O13 1.474(3) . ? S2 O16 1.488(3) . ? O1 N1 1.397(4) . ? O1 H1O 0.87(4) . ? O2 N2 1.400(4) . ? O2 H2O 0.79(4) . ? O3 N5 1.397(4) . ? O3 H3O 0.85(5) . ? O4 N6 1.397(3) . ? O4 H4O 0.82(4) . ? O5 N9 1.400(4) . ? O5 H5O 0.85(5) . ? O6 N10 1.398(4) . ? O6 H6O 0.77(4) . ? O7 N13 1.406(4) . ? O7 H7O 0.86(6) . ? O8 N14 1.392(4) . ? O8 H8O 0.90(6) . ? N1 C1 1.302(4) . ? N2 C2 1.307(4) . ? N3 C1 1.326(4) . ? N3 H3A 0.90(5) . ? N3 H3B 0.82(4) . ? N4 C2 1.323(4) . ? N4 H4A 0.87(4) . ? N4 H4B 0.84(5) . ? N5 C3 1.311(4) . ? N6 C4 1.303(4) . ? N7 C3 1.319(4) . ? N7 H7A 0.91(5) . ? N7 H7B 0.80(4) . ? N8 C4 1.328(4) . ? N8 H8A 0.80(5) . ? N8 H8B 0.78(5) . ? N9 C5 1.304(4) . ? N10 C6 1.295(4) . ? N11 C5 1.322(4) . ? N11 H11A 0.84(5) . ? N11 H11B 0.83(4) . ? N12 C6 1.326(4) . ? N12 H12A 0.79(5) . ? N12 H12B 0.78(5) . ? N13 C7 1.290(4) . ? N14 C8 1.307(5) . ? N14 H14 0.91(6) . ? N15 C7 1.357(5) . ? N15 H15A 0.85(5) . ? N15 H15B 0.83(5) . ? N16 C8 1.311(5) . ? N16 H16A 1.03(6) . ? N16 H16B 0.84(5) . ? C1 C2 1.486(5) . ? C3 C4 1.483(5) . ? C5 C6 1.485(5) . ? C7 C8 1.482(5) . ? O17 H17A 0.94(2) . ? O17 H17B 0.94(2) . ? O18 H18A 0.97(2) . ? O18 H18B 0.97(2) . ? 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 Co1 N6 172.25(12) . . ? N1 Co1 N10 91.66(12) . . ? N6 Co1 N10 94.50(12) . . ? N1 Co1 N5 94.08(12) . . ? N6 Co1 N5 79.97(12) . . ? N10 Co1 N5 173.82(12) . . ? N1 Co1 N9 95.22(12) . . ? N6 Co1 N9 90.55(12) . . ? N10 Co1 N9 79.18(12) . . ? N5 Co1 N9 98.00(12) . . ? N1 Co1 N2 79.99(12) . . ? N6 Co1 N2 94.54(12) . . ? N10 Co1 N2 97.40(12) . . ? N5 Co1 N2 85.85(12) . . ? N9 Co1 N2 174.10(12) . . ? O9 S1 O12 112.53(17) . . ? O9 S1 O10 111.12(16) . . ? O12 S1 O10 108.33(18) . . ? O9 S1 O11 109.40(15) . . ? O12 S1 O11 107.53(16) . . ? O10 S1 O11 107.74(17) . . ? O14 S2 O15 111.43(16) . . ? O14 S2 O13 109.79(16) . . ? O15 S2 O13 110.42(16) . . ? O14 S2 O16 108.20(17) . . ? O15 S2 O16 107.80(16) . . ? O13 S2 O16 109.13(17) . . ? N1 O1 H1O 105(3) . . ? N2 O2 H2O 107(3) . . ? N5 O3 H3O 110(3) . . ? N6 O4 H4O 102(3) . . ? N9 O5 H5O 107(3) . . ? N10 O6 H6O 104(3) . . ? N13 O7 H7O 92(4) . . ? N14 O8 H8O 104(4) . . ? C1 N1 O1 113.9(3) . . ? C1 N1 Co1 118.7(2) . . ? O1 N1 Co1 127.3(2) . . ? C2 N2 O2 111.5(3) . . ? C2 N2 Co1 115.7(2) . . ? O2 N2 Co1 125.5(2) . . ? C1 N3 H3A 114(3) . . ? C1 N3 H3B 120(3) . . ? H3A N3 H3B 125(4) . . ? C2 N4 H4A 117(3) . . ? C2 N4 H4B 115(3) . . ? H4A N4 H4B 127(4) . . ? C3 N5 O3 111.8(3) . . ? C3 N5 Co1 115.1(2) . . ? O3 N5 Co1 123.8(2) . . ? C4 N6 O4 114.8(3) . . ? C4 N6 Co1 117.8(2) . . ? O4 N6 Co1 127.0(2) . . ? C3 N7 H7A 120(3) . . ? C3 N7 H7B 121(3) . . ? H7A N7 H7B 119(4) . . ? C4 N8 H8A 118(3) . . ? C4 N8 H8B 120(4) . . ? H8A N8 H8B 121(5) . . ? C5 N9 O5 113.4(3) . . ? C5 N9 Co1 116.6(2) . . ? O5 N9 Co1 126.0(2) . . ? C6 N10 O6 114.4(3) . . ? C6 N10 Co1 118.7(2) . . ? O6 N10 Co1 126.7(2) . . ? C5 N11 H11A 118(3) . . ? C5 N11 H11B 120(3) . . ? H11A N11 H11B 121(4) . . ? C6 N12 H12A 121(3) . . ? C6 N12 H12B 122(4) . . ? H12A N12 H12B 115(5) . . ? C7 N13 O7 109.8(3) . . ? C8 N14 O8 118.5(3) . . ? C8 N14 H14 123(4) . . ? O8 N14 H14 117(4) . . ? C7 N15 H15A 117(3) . . ? C7 N15 H15B 114(4) . . ? H15A N15 H15B 118(5) . . ? C8 N16 H16A 119(3) . . ? C8 N16 H16B 118(3) . . ? H16A N16 H16B 123(4) . . ? N1 C1 N3 125.6(3) . . ? N1 C1 C2 111.0(3) . . ? N3 C1 C2 123.4(3) . . ? N2 C2 N4 125.3(3) . . ? N2 C2 C1 112.4(3) . . ? N4 C2 C1 122.3(3) . . ? N5 C3 N7 125.1(3) . . ? N5 C3 C4 112.1(3) . . ? N7 C3 C4 122.7(3) . . ? N6 C4 N8 125.7(3) . . ? N6 C4 C3 111.5(3) . . ? N8 C4 C3 122.8(3) . . ? N9 C5 N11 126.0(3) . . ? N9 C5 C6 111.6(3) . . ? N11 C5 C6 122.4(3) . . ? N10 C6 N12 125.9(3) . . ? N10 C6 C5 111.4(3) . . ? N12 C6 C5 122.6(3) . . ? N13 C7 N15 127.9(3) . . ? N13 C7 C8 114.5(3) . . ? N15 C7 C8 117.5(3) . . ? N14 C8 N16 122.7(4) . . ? N14 C8 C7 115.9(3) . . ? N16 C8 C7 121.4(3) . . ? H17A O17 H17B 114(5) . . ? H18A O18 H18B 96(9) . . ? _diffrn_measured_fraction_theta_max 0.851 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.454 _refine_diff_density_min -0.525 _refine_diff_density_rms 0.094 # Attachment 'c1361fin_excl_H2O.cif' data_c1361fin _database_code_depnum_ccdc_archive 'CCDC 700650' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H24 Co Cr N12 O22.50' _chemical_formula_weight 807.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.8792(8) _cell_length_b 17.7159(14) _cell_length_c 17.6960(14) _cell_angle_alpha 90.00 _cell_angle_beta 102.409(2) _cell_angle_gamma 90.00 _cell_volume 3024.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 208(2) _cell_measurement_reflns_used 4295 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 28.93 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.773 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1644 _exptl_absorpt_coefficient_mu 1.020 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 208(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 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19844 _diffrn_reflns_av_R_equivalents 0.0508 _diffrn_reflns_av_sigmaI/netI 0.0876 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 29.49 _reflns_number_total 7572 _reflns_number_gt 3956 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick,1997)' _computing_molecular_graphics 'ORTEP3 for Windows (L. J. Farrugia, 1997)' _computing_publication_material 'WINGX (L.J. Farrugia,1999)' _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^)+(0.0767P)^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 7572 _refine_ls_number_parameters 533 _refine_ls_number_restraints 45 _refine_ls_R_factor_all 0.1207 _refine_ls_R_factor_gt 0.0507 _refine_ls_wR_factor_ref 0.1529 _refine_ls_wR_factor_gt 0.1314 _refine_ls_goodness_of_fit_ref 0.964 _refine_ls_restrained_S_all 0.962 _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 0.08486(5) 0.31725(3) 0.38149(3) 0.01692(15) Uani 1 1 d . . . Cr1 Cr 0.58367(6) 0.32111(3) 0.38164(4) 0.01978(17) Uani 1 1 d . . . O1 O 0.2930(3) 0.21440(17) 0.47260(19) 0.0340(8) Uani 1 1 d D . . O2 O -0.0635(3) 0.43266(15) 0.45233(17) 0.0256(7) Uani 1 1 d D . . O3 O 0.2702(3) 0.44731(15) 0.43001(17) 0.0257(7) Uani 1 1 d D . . O4 O -0.1424(3) 0.32037(17) 0.24135(17) 0.0287(7) Uani 1 1 d D . . O5 O 0.2088(3) 0.28863(17) 0.24577(17) 0.0272(7) Uani 1 1 d D . . O6 O -0.0632(3) 0.20076(17) 0.45107(18) 0.0303(7) Uani 1 1 d D . . O7 O 0.4392(3) 0.36592(15) 0.29928(16) 0.0236(7) Uani 1 1 d . . . O8 O 0.6834(3) 0.41420(15) 0.36580(16) 0.0241(7) Uani 1 1 d . . . O9 O 0.3920(3) 0.47100(18) 0.2282(2) 0.0402(8) Uani 1 1 d . . . O10 O 0.6464(3) 0.52649(17) 0.30645(18) 0.0362(8) Uani 1 1 d . . . O11 O 0.5033(3) 0.36858(16) 0.46098(16) 0.0241(7) Uani 1 1 d . . . O12 O 0.7290(3) 0.29270(16) 0.47153(16) 0.0255(7) Uani 1 1 d . . . O13 O 0.5669(3) 0.41084(17) 0.58227(17) 0.0339(8) Uani 1 1 d . . . O14 O 0.7892(3) 0.3098(2) 0.59968(19) 0.0444(9) Uani 1 1 d . . . O15 O 0.4792(3) 0.22620(15) 0.38256(16) 0.0241(7) Uani 1 1 d . . . O16 O 0.6681(3) 0.26326(16) 0.30845(16) 0.0260(7) Uani 1 1 d . . . O17 O 0.4582(3) 0.10975(17) 0.3330(2) 0.0411(9) Uani 1 1 d . . . O18 O 0.6533(4) 0.15369(18) 0.24553(19) 0.0405(8) Uani 1 1 d . . . O19 O 0.1828(5) 0.0991(3) 0.5773(3) 0.0995(18) Uani 1 1 d . . . O20 O 0.9285(15) 0.1631(6) 0.6140(5) 0.213(10) Uani 0.701(13) 1 d P . . O20F O 0.730(2) 0.075(2) 0.5826(9) 0.23(2) Uani 0.299(13) 1 d P . . O21 O 0.4517(15) 0.0618(6) 0.4947(6) 0.128(5) Uani 0.50 1 d P . . O22 O 0.5273(6) 0.1963(3) 0.5942(3) 0.1098(19) Uani 1 1 d . . . O23 O -0.0871(18) 0.0321(6) 0.4954(8) 0.074(6) Uani 0.378(16) 1 d P . . O23F O -0.2206(19) 0.0549(9) 0.4591(9) 0.191(8) Uani 0.622(16) 1 d P . . N1 N 0.2189(3) 0.28166(17) 0.46943(19) 0.0204(7) Uani 1 1 d . . . N2 N 0.0173(3) 0.36716(17) 0.46256(19) 0.0193(7) Uani 1 1 d . . . N3 N 0.2736(5) 0.2813(2) 0.6056(2) 0.0363(10) Uani 1 1 d D . . N4 N 0.0985(4) 0.4139(2) 0.5874(2) 0.0307(9) Uani 1 1 d D . . N5 N 0.1760(3) 0.41093(18) 0.37036(19) 0.0204(7) Uani 1 1 d . . . N6 N -0.0443(3) 0.36070(18) 0.29542(19) 0.0212(8) Uani 1 1 d . . . N7 N 0.1387(4) 0.5320(2) 0.3190(2) 0.0278(9) Uani 1 1 d D . . N8 N -0.0745(4) 0.4566(2) 0.2023(2) 0.0339(10) Uani 1 1 d D . . N9 N 0.1535(3) 0.25904(18) 0.30657(19) 0.0214(7) Uani 1 1 d . . . N10 N -0.0126(3) 0.22484(18) 0.38720(19) 0.0205(7) Uani 1 1 d . . . N11 N 0.1052(5) 0.1519(2) 0.2282(2) 0.0333(9) Uani 1 1 d D . . N12 N -0.0087(5) 0.0966(2) 0.3573(3) 0.0376(10) Uani 1 1 d D . . C1 C 0.2063(4) 0.3054(2) 0.5370(3) 0.0229(9) Uani 1 1 d . . . C2 C 0.1020(4) 0.3665(2) 0.5299(2) 0.0206(9) Uani 1 1 d . . . C3 C 0.1098(4) 0.4593(2) 0.3209(2) 0.0186(9) Uani 1 1 d . . . C4 C -0.0125(4) 0.4247(2) 0.2686(2) 0.0208(9) Uani 1 1 d . . . C5 C 0.0970(4) 0.1929(2) 0.2900(2) 0.0219(9) Uani 1 1 d . . . C6 C 0.0186(4) 0.1681(2) 0.3474(2) 0.0217(9) Uani 1 1 d . . . C7 C 0.4667(4) 0.4332(2) 0.2776(2) 0.0243(9) Uani 1 1 d . . . C8 C 0.6112(4) 0.4638(2) 0.3192(2) 0.0252(10) Uani 1 1 d . . . C9 C 0.5857(4) 0.3721(2) 0.5294(2) 0.0238(9) Uani 1 1 d . . . C10 C 0.7139(4) 0.3209(2) 0.5368(3) 0.0256(10) Uani 1 1 d . . . C11 C 0.5091(5) 0.1728(2) 0.3386(3) 0.0277(10) Uani 1 1 d . . . C12 C 0.6206(4) 0.1956(2) 0.2914(2) 0.0260(10) Uani 1 1 d . . . H1N H 0.335(3) 0.254(2) 0.604(2) 0.021(12) Uiso 1 1 d D . . H1O H 0.346(5) 0.219(3) 0.440(3) 0.059(18) Uiso 1 1 d D . . H2N H 0.255(4) 0.295(2) 0.6457(17) 0.024(13) Uiso 1 1 d D . . H2O H -0.147(3) 0.420(3) 0.434(3) 0.055(17) Uiso 1 1 d D . . H3N H 0.170(3) 0.417(3) 0.618(2) 0.046(17) Uiso 1 1 d D . . H3O H 0.334(4) 0.414(2) 0.443(3) 0.060(18) Uiso 1 1 d D . . H4N H 0.046(5) 0.448(2) 0.569(3) 0.056(18) Uiso 1 1 d D . . H4O H -0.202(5) 0.303(3) 0.266(3) 0.065(19) Uiso 1 1 d D . . H5N H 0.201(4) 0.545(3) 0.354(2) 0.035(14) Uiso 1 1 d D . . H5O H 0.277(4) 0.313(3) 0.275(3) 0.055(17) Uiso 1 1 d D . . H6N H 0.090(4) 0.557(2) 0.287(2) 0.028(13) Uiso 1 1 d D . . H6O H -0.115(4) 0.237(2) 0.462(3) 0.045(16) Uiso 1 1 d D . . H7N H -0.045(4) 0.5002(16) 0.195(3) 0.036(14) Uiso 1 1 d D . . H8N H -0.145(3) 0.433(2) 0.177(2) 0.030(13) Uiso 1 1 d D . . H9N H 0.132(5) 0.173(3) 0.191(2) 0.049(17) Uiso 1 1 d D . . H10N H 0.054(4) 0.1148(19) 0.214(3) 0.035(14) Uiso 1 1 d D . . H11N H 0.017(5) 0.061(2) 0.333(3) 0.054(12) Uiso 1 1 d D . . H12N H -0.057(5) 0.089(3) 0.390(2) 0.054(12) 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 0.0178(3) 0.0163(3) 0.0164(3) -0.0007(2) 0.0031(2) -0.0002(2) Cr1 0.0169(3) 0.0208(3) 0.0213(4) -0.0019(3) 0.0032(3) -0.0009(3) O1 0.0392(19) 0.0280(16) 0.039(2) 0.0090(15) 0.0174(16) 0.0153(15) O2 0.0178(15) 0.0219(14) 0.0326(17) -0.0069(13) -0.0048(13) 0.0057(12) O3 0.0229(16) 0.0217(15) 0.0280(16) -0.0041(13) -0.0045(13) -0.0021(13) O4 0.0284(17) 0.0344(17) 0.0210(16) -0.0044(14) -0.0001(13) -0.0142(14) O5 0.0282(17) 0.0365(17) 0.0181(16) -0.0037(13) 0.0077(13) -0.0111(14) O6 0.0342(18) 0.0270(16) 0.0350(18) 0.0047(14) 0.0193(15) 0.0031(14) O7 0.0178(15) 0.0261(15) 0.0244(16) 0.0021(13) -0.0011(12) -0.0061(12) O8 0.0181(14) 0.0245(15) 0.0276(17) 0.0028(13) 0.0002(12) -0.0031(12) O9 0.0293(18) 0.0385(18) 0.046(2) 0.0145(17) -0.0061(16) -0.0007(15) O10 0.0382(19) 0.0284(17) 0.0374(19) 0.0074(15) -0.0022(15) -0.0118(15) O11 0.0195(15) 0.0302(16) 0.0221(16) -0.0046(13) 0.0031(12) 0.0022(13) O12 0.0230(15) 0.0279(15) 0.0243(17) 0.0011(13) 0.0024(13) 0.0031(13) O13 0.048(2) 0.0360(18) 0.0199(16) -0.0043(14) 0.0111(14) -0.0008(15) O14 0.046(2) 0.055(2) 0.0273(19) 0.0041(16) -0.0042(16) 0.0094(18) O15 0.0230(15) 0.0215(14) 0.0289(17) -0.0057(13) 0.0081(13) -0.0027(12) O16 0.0214(15) 0.0288(16) 0.0298(17) -0.0044(13) 0.0095(13) -0.0021(13) O17 0.047(2) 0.0249(16) 0.054(2) -0.0109(16) 0.0167(17) -0.0106(15) O18 0.048(2) 0.0400(19) 0.037(2) -0.0128(16) 0.0175(17) 0.0032(17) O19 0.096(4) 0.087(3) 0.096(4) 0.010(3) -0.025(3) -0.010(3) O20 0.34(2) 0.231(12) 0.116(8) 0.139(8) 0.167(11) 0.237(14) O20F 0.15(2) 0.53(6) 0.024(9) 0.072(18) 0.046(11) 0.23(3) O21 0.250(16) 0.080(7) 0.067(7) 0.011(6) 0.064(8) 0.058(9) O22 0.093(4) 0.136(5) 0.099(4) 0.003(4) 0.016(3) 0.016(4) O23 0.092(13) 0.060(8) 0.071(9) 0.020(6) 0.020(8) -0.026(7) O23F 0.181(19) 0.214(14) 0.167(13) -0.014(11) 0.017(12) -0.066(13) N1 0.0194(17) 0.0170(16) 0.0246(19) 0.0024(14) 0.0042(15) 0.0055(14) N2 0.0172(17) 0.0175(16) 0.0226(19) -0.0026(14) 0.0026(14) 0.0034(14) N3 0.041(3) 0.042(3) 0.022(2) 0.0028(19) -0.0002(19) 0.020(2) N4 0.029(2) 0.035(2) 0.023(2) -0.0061(18) -0.0036(18) 0.0082(19) N5 0.0167(17) 0.0232(17) 0.0202(18) -0.0039(15) 0.0012(14) -0.0040(14) N6 0.0183(18) 0.0235(18) 0.0205(19) -0.0037(14) 0.0015(14) -0.0034(14) N7 0.030(2) 0.0215(19) 0.028(2) 0.0037(17) -0.0039(18) 0.0008(17) N8 0.034(2) 0.028(2) 0.034(2) 0.0077(18) -0.0047(19) -0.0063(19) N9 0.0223(18) 0.0235(18) 0.0206(19) 0.0002(15) 0.0094(15) -0.0034(15) N10 0.0215(18) 0.0212(17) 0.0210(19) 0.0006(14) 0.0091(15) -0.0022(14) N11 0.046(3) 0.028(2) 0.028(2) -0.0098(18) 0.012(2) -0.009(2) N12 0.058(3) 0.0192(19) 0.042(3) -0.0069(18) 0.024(2) -0.0047(19) C1 0.020(2) 0.020(2) 0.028(2) 0.0026(18) 0.0035(18) 0.0021(17) C2 0.017(2) 0.020(2) 0.025(2) -0.0009(17) 0.0038(17) -0.0006(17) C3 0.020(2) 0.0157(19) 0.020(2) -0.0030(17) 0.0034(17) -0.0020(16) C4 0.020(2) 0.023(2) 0.018(2) -0.0002(17) 0.0019(17) 0.0032(17) C5 0.023(2) 0.017(2) 0.025(2) -0.0023(17) 0.0037(18) 0.0014(17) C6 0.021(2) 0.019(2) 0.025(2) -0.0033(17) 0.0048(18) -0.0017(16) C7 0.019(2) 0.030(2) 0.024(2) -0.0026(19) 0.0032(18) -0.0014(18) C8 0.023(2) 0.030(2) 0.023(2) 0.0008(19) 0.0047(19) -0.0033(19) C9 0.026(2) 0.028(2) 0.019(2) 0.0019(18) 0.0059(18) -0.0055(19) C10 0.025(2) 0.027(2) 0.023(2) 0.0026(19) 0.0013(19) -0.0035(19) C11 0.025(2) 0.028(2) 0.027(2) -0.0024(19) -0.0008(19) 0.0035(19) C12 0.025(2) 0.030(2) 0.022(2) -0.0026(19) 0.0038(18) 0.0019(19) _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 N10 1.913(3) . ? Co1 N9 1.915(3) . ? Co1 N5 1.919(3) . ? Co1 N1 1.920(3) . ? Co1 N2 1.923(3) . ? Co1 N6 1.925(3) . ? Cr1 O11 1.946(3) . ? Cr1 O12 1.966(3) . ? Cr1 O16 1.972(3) . ? Cr1 O8 1.972(3) . ? Cr1 O7 1.974(3) . ? Cr1 O15 1.975(3) . ? O1 N1 1.393(4) . ? O1 H1O 0.87(3) . ? O2 N2 1.398(4) . ? O2 H2O 0.85(3) . ? O3 N5 1.404(4) . ? O3 H3O 0.86(3) . ? O4 N6 1.402(4) . ? O4 H4O 0.87(3) . ? O5 N9 1.408(4) . ? O5 H5O 0.87(3) . ? O6 N10 1.397(4) . ? O6 H6O 0.87(3) . ? O7 C7 1.299(5) . ? O8 C8 1.308(5) . ? O9 C7 1.216(5) . ? O10 C8 1.199(5) . ? O11 C9 1.307(5) . ? O12 C10 1.296(5) . ? O13 C9 1.206(5) . ? O14 C10 1.214(5) . ? O15 C11 1.298(5) . ? O16 C12 1.298(5) . ? O17 C11 1.221(5) . ? O18 C12 1.196(5) . ? O23 O23F 1.396(17) . ? N1 C1 1.299(5) . ? N2 C2 1.301(5) . ? N3 C1 1.322(5) . ? N3 H1N 0.78(2) . ? N3 H2N 0.81(2) . ? N4 C2 1.326(5) . ? N4 H3N 0.80(2) . ? N4 H4N 0.82(2) . ? N5 C3 1.298(5) . ? N6 C4 1.293(5) . ? N7 C3 1.321(5) . ? N7 H5N 0.81(2) . ? N7 H6N 0.80(2) . ? N8 C4 1.328(5) . ? N8 H7N 0.85(2) . ? N8 H8N 0.85(2) . ? N9 C5 1.304(5) . ? N10 C6 1.302(5) . ? N11 C5 1.330(5) . ? N11 H9N 0.85(2) . ? N11 H10N 0.84(2) . ? N12 C6 1.315(5) . ? N12 H11N 0.83(2) . ? N12 H12N 0.83(2) . ? C1 C2 1.481(5) . ? C3 C4 1.488(5) . ? C5 C6 1.470(6) . ? C7 C8 1.556(6) . ? C9 C10 1.540(6) . ? C11 C12 1.571(6) . ? 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 N10 Co1 N9 80.38(14) . . ? N10 Co1 N5 176.87(14) . . ? N9 Co1 N5 98.67(14) . . ? N10 Co1 N1 86.76(14) . . ? N9 Co1 N1 95.68(14) . . ? N5 Co1 N1 96.31(13) . . ? N10 Co1 N2 95.43(14) . . ? N9 Co1 N2 174.57(14) . . ? N5 Co1 N2 85.69(14) . . ? N1 Co1 N2 80.56(14) . . ? N10 Co1 N6 97.38(14) . . ? N9 Co1 N6 86.61(14) . . ? N5 Co1 N6 79.57(13) . . ? N1 Co1 N6 175.57(14) . . ? N2 Co1 N6 97.41(14) . . ? O11 Cr1 O12 82.36(12) . . ? O11 Cr1 O16 173.81(12) . . ? O12 Cr1 O16 93.44(12) . . ? O11 Cr1 O8 92.00(12) . . ? O12 Cr1 O8 91.65(11) . . ? O16 Cr1 O8 92.66(12) . . ? O11 Cr1 O7 90.96(12) . . ? O12 Cr1 O7 170.72(12) . . ? O16 Cr1 O7 93.71(12) . . ? O8 Cr1 O7 82.12(11) . . ? O11 Cr1 O15 93.84(12) . . ? O12 Cr1 O15 93.87(12) . . ? O16 Cr1 O15 81.87(12) . . ? O8 Cr1 O15 172.45(12) . . ? O7 Cr1 O15 92.99(11) . . ? N1 O1 H1O 106(4) . . ? N2 O2 H2O 108(4) . . ? N5 O3 H3O 103(4) . . ? N6 O4 H4O 107(4) . . ? N9 O5 H5O 96(4) . . ? N10 O6 H6O 106(3) . . ? C7 O7 Cr1 115.0(2) . . ? C8 O8 Cr1 115.5(2) . . ? C9 O11 Cr1 114.8(3) . . ? C10 O12 Cr1 114.7(3) . . ? C11 O15 Cr1 115.4(3) . . ? C12 O16 Cr1 116.7(3) . . ? C1 N1 O1 113.2(3) . . ? C1 N1 Co1 117.0(3) . . ? O1 N1 Co1 125.3(3) . . ? C2 N2 O2 111.3(3) . . ? C2 N2 Co1 114.9(3) . . ? O2 N2 Co1 124.4(2) . . ? C1 N3 H1N 114(3) . . ? C1 N3 H2N 123(3) . . ? H1N N3 H2N 123(5) . . ? C2 N4 H3N 114(4) . . ? C2 N4 H4N 106(4) . . ? H3N N4 H4N 128(5) . . ? C3 N5 O3 111.1(3) . . ? C3 N5 Co1 117.5(3) . . ? O3 N5 Co1 124.7(2) . . ? C4 N6 O4 112.5(3) . . ? C4 N6 Co1 117.9(3) . . ? O4 N6 Co1 125.4(2) . . ? C3 N7 H5N 113(3) . . ? C3 N7 H6N 117(3) . . ? H5N N7 H6N 129(5) . . ? C4 N8 H7N 115(3) . . ? C4 N8 H8N 115(3) . . ? H7N N8 H8N 129(4) . . ? C5 N9 O5 112.4(3) . . ? C5 N9 Co1 116.2(3) . . ? O5 N9 Co1 125.6(2) . . ? C6 N10 O6 111.7(3) . . ? C6 N10 Co1 116.8(3) . . ? O6 N10 Co1 125.1(2) . . ? C5 N11 H9N 118(3) . . ? C5 N11 H10N 123(3) . . ? H9N N11 H10N 113(5) . . ? C6 N12 H11N 124(4) . . ? C6 N12 H12N 114(4) . . ? H11N N12 H12N 122(5) . . ? N1 C1 N3 127.7(4) . . ? N1 C1 C2 111.2(4) . . ? N3 C1 C2 121.1(4) . . ? N2 C2 N4 125.5(4) . . ? N2 C2 C1 112.5(4) . . ? N4 C2 C1 122.0(4) . . ? N5 C3 N7 125.5(4) . . ? N5 C3 C4 111.8(3) . . ? N7 C3 C4 122.6(4) . . ? N6 C4 N8 126.5(4) . . ? N6 C4 C3 111.3(3) . . ? N8 C4 C3 122.2(4) . . ? N9 C5 N11 125.3(4) . . ? N9 C5 C6 112.2(4) . . ? N11 C5 C6 122.6(4) . . ? N10 C6 N12 126.3(4) . . ? N10 C6 C5 111.3(3) . . ? N12 C6 C5 122.3(4) . . ? O9 C7 O7 125.8(4) . . ? O9 C7 C8 120.0(4) . . ? O7 C7 C8 114.1(4) . . ? O10 C8 O8 126.9(4) . . ? O10 C8 C7 120.5(4) . . ? O8 C8 C7 112.6(3) . . ? O13 C9 O11 125.2(4) . . ? O13 C9 C10 122.0(4) . . ? O11 C9 C10 112.8(4) . . ? O14 C10 O12 126.0(4) . . ? O14 C10 C9 120.3(4) . . ? O12 C10 C9 113.7(4) . . ? O17 C11 O15 124.9(4) . . ? O17 C11 C12 121.0(4) . . ? O15 C11 C12 114.0(4) . . ? O18 C12 O16 126.4(4) . . ? O18 C12 C11 121.6(4) . . ? O16 C12 C11 112.0(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1O O15 0.87(3) 1.82(3) 2.688(4) 172(5) . O2 H2O O8 0.85(3) 1.84(3) 2.656(4) 160(5) 1_455 O3 H3O O11 0.86(3) 1.82(3) 2.648(4) 161(5) . O4 H4O O16 0.87(3) 1.76(3) 2.626(4) 175(6) 1_455 O5 H5O O7 0.87(3) 1.83(3) 2.651(4) 157(5) . O6 H6O O12 0.87(3) 1.87(3) 2.705(4) 161(5) 1_455 N3 H1N O22 0.78(2) 2.20(2) 2.968(7) 169(4) . N4 H4N O2 0.82(2) 2.13(5) 2.597(5) 116(4) . N4 H3N O10 0.80(2) 2.24(3) 2.993(5) 157(5) 3_666 N7 H6N O17 0.80(2) 2.27(3) 2.991(5) 151(4) 2 N8 H7N O17 0.85(2) 2.22(2) 3.063(5) 175(5) 2 N8 H8N O19 0.85(2) 2.25(3) 3.055(6) 159(4) 4_565 N11 H10N O13 0.84(2) 2.40(5) 2.762(5) 107(4) 4_565 N12 H12N O23 0.83(2) 2.20(4) 2.948(12) 149(5) . N12 H11N O9 0.83(2) 2.22(2) 3.053(5) 174(5) 2_545 _diffrn_measured_fraction_theta_max 0.898 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.839 _refine_diff_density_min -0.461 _refine_diff_density_rms 0.110