Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Parthasarathi Dastidar' _publ_contact_author_address ; Analytical Science Discipline Central Salt & Marine Chemicals Research Institute G B Marg Bhavnagar Gujarat 364002 INDIA ; _publ_contact_author_email PARTHOD123@REDIFFMAIL.COM _publ_section_title ; Exploring Hydrogen bond Functionalized Backbone and Ligating Topologies in Co(II) Coordination Polymers of Mixed Ligand Systems: Conformation Dependent Network Structures and Entrapment of (H2O)14 Water Cluster of an Unprecedented Topology ; loop_ _publ_author_name 'Parthasarathi Dastidar' 'Amitava Das' 'D. Krishna Kumar' data_kkb490em _database_code_depnum_ccdc_archive 'CCDC 644300' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H22 Co N3 O11' _chemical_formula_weight 479.29 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 P2(1)/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 8.3945(8) _cell_length_b 15.8060(16) _cell_length_c 14.8833(15) _cell_angle_alpha 90.00 _cell_angle_beta 100.332(2) _cell_angle_gamma 90.00 _cell_volume 1942.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description PLATE _exptl_crystal_colour PINK _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.639 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 992 _exptl_absorpt_coefficient_mu 0.950 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.7637 _exptl_absorpt_correction_T_max 0.9541 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER CCD AREA DETECTOR' _diffrn_measurement_method 'PHI-OMEGA SCAN' _diffrn_detector_area_resol_mean 3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9725 _diffrn_reflns_av_R_equivalents 0.0333 _diffrn_reflns_av_sigmaI/netI 0.0446 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 25.50 _reflns_number_total 3588 _reflns_number_gt 2554 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER AXS SMART 3' _computing_cell_refinement 'BRUKER AXS SMART 3' _computing_data_reduction 'BRUKER AXS SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'BRUKER SHELXLTL' _computing_publication_material 'MERCURY 1.4' _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^)+(0.0498P)^2^+5.2041P] 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 3588 _refine_ls_number_parameters 302 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0778 _refine_ls_R_factor_gt 0.0531 _refine_ls_wR_factor_ref 0.1298 _refine_ls_wR_factor_gt 0.1179 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.018 _refine_ls_shift/su_mean 0.001 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 0.0000 0.0000 1.0000 0.01595(19) Uani 1 2 d S . . Co2 Co 0.5000 0.0000 0.5000 0.0184(2) Uani 1 2 d S . . N1 N 0.0434(4) 0.1245(2) 0.9484(2) 0.0186(7) Uani 1 1 d . . . C2 C -0.0113(5) 0.1951(3) 0.9816(3) 0.0251(9) Uani 1 1 d . . . H2 H -0.0740 0.1905 1.0286 0.030 Uiso 1 1 calc R . . C3 C 0.0197(6) 0.2746(3) 0.9502(4) 0.0397(12) Uani 1 1 d . . . H3 H -0.0197 0.3239 0.9756 0.048 Uiso 1 1 calc R . . C4 C 0.1102(6) 0.2810(3) 0.8803(3) 0.0462(15) Uani 1 1 d . . . H4 H 0.1334 0.3348 0.8573 0.055 Uiso 1 1 calc R . . C5 C 0.1652(6) 0.2084(3) 0.8455(3) 0.0404(13) Uani 1 1 d . . . C6 C 0.1294(5) 0.1327(3) 0.8811(3) 0.0279(10) Uani 1 1 d . . . H6A H 0.1677 0.0827 0.8567 0.033 Uiso 1 1 calc R . . C8A C 0.2536(6) 0.2524(3) 0.7042(3) 0.0146(11) Uiso 0.69 1 d P . . C8B C 0.1908(16) 0.2537(9) 0.7630(9) 0.026(3) Uiso 0.31 1 d P . . N7A N 0.2736(5) 0.1992(3) 0.7774(3) 0.0166(11) Uiso 0.71 1 d P . . N7B N 0.2997(15) 0.1992(8) 0.7419(9) 0.023(3) Uiso 0.29 1 d P . . O9 O 0.1561(4) 0.31363(18) 0.7019(2) 0.0351(8) Uani 1 1 d . . . C10 C 0.3514(5) 0.2283(4) 0.6355(3) 0.0401(13) Uani 1 1 d . . . C11 C 0.3887(5) 0.2942(3) 0.5820(4) 0.0400(12) Uani 1 1 d . . . H11 H 0.3567 0.3505 0.5925 0.048 Uiso 1 1 calc R . . C12 C 0.4720(5) 0.2767(3) 0.5141(3) 0.0334(11) Uani 1 1 d . . . H12 H 0.5040 0.3212 0.4783 0.040 Uiso 1 1 calc R . . C13 C 0.5099(5) 0.1948(3) 0.4973(3) 0.0258(9) Uani 1 1 d . . . H13 H 0.5667 0.1844 0.4486 0.031 Uiso 1 1 calc R . . N14 N 0.4720(4) 0.1282(2) 0.5451(2) 0.0210(7) Uani 1 1 d . . . C15 C 0.3946(5) 0.1452(3) 0.6144(3) 0.0303(10) Uani 1 1 d . . . H15 H 0.3678 0.0996 0.6506 0.036 Uiso 1 1 calc R . . O16 O 0.7412(4) 0.0306(2) 0.4935(2) 0.0318(7) Uani 1 1 d . . . H16A H 0.7840 0.0549 0.5421 0.048 Uiso 1 1 calc R . . O17 O 0.4247(4) 0.0387(2) 0.36777(19) 0.0331(8) Uani 1 1 d . . . H17A H 0.3711 -0.0002 0.3379 0.050 Uiso 1 1 calc R . . O18 O -0.2371(3) 0.0386(2) 1.0101(2) 0.0261(7) Uani 1 1 d . . . H18A H -0.2439 0.0448 1.0654 0.039 Uiso 1 1 calc R . . O19 O 0.0687(4) 0.0360(2) 1.13303(19) 0.0229(6) Uani 1 1 d . . . H19A H 0.1180 -0.0040 1.1631 0.034 Uiso 1 1 calc R . . O20 O 0.6851(3) 0.43409(17) 0.67706(18) 0.0254(6) Uani 1 1 d . . . C21 C 0.6743(5) 0.3680(3) 0.7226(3) 0.0227(9) Uani 1 1 d . . . O22 O 0.5899(4) 0.3603(2) 0.7848(2) 0.0403(8) Uani 1 1 d . . . C23 C 0.7584(5) 0.2899(3) 0.6982(3) 0.0221(9) Uani 1 1 d . . . H23 H 0.8253 0.2939 0.6532 0.027 Uiso 1 1 calc R . . C24 C 0.7434(5) 0.2160(3) 0.7365(2) 0.0200(8) Uani 1 1 d . . . H24 H 0.6869 0.2144 0.7864 0.024 Uiso 1 1 calc R . . C25 C 0.8081(5) 0.1353(3) 0.7076(3) 0.0210(9) Uani 1 1 d . . . O26 O 0.8932(4) 0.13427(18) 0.6472(2) 0.0315(7) Uani 1 1 d . . . O27 O 0.7645(3) 0.06897(17) 0.74644(17) 0.0215(6) Uani 1 1 d . . . O28 O 0.4780(4) 0.56958(19) 0.65115(19) 0.0234(6) Uani 1 1 d . . . O29 O 0.8914(5) 0.9988(2) 0.3499(3) 0.0477(9) Uani 1 1 d D . . H16B H 0.793(8) 0.014(4) 0.456(4) 0.07(2) Uiso 1 1 d . . . H17B H 0.479(5) 0.066(3) 0.338(3) 0.013(10) Uiso 1 1 d . . . H18B H -0.304(5) 0.051(3) 0.968(3) 0.022(12) Uiso 1 1 d . . . H19B H 0.091(6) 0.079(3) 1.148(4) 0.041(17) Uiso 1 1 d . . . H28A H 0.533(6) 0.530(3) 0.664(3) 0.029(14) Uiso 1 1 d . . . H28B H 0.425(6) 0.573(3) 0.704(3) 0.09(2) Uiso 1 1 d . . . H29A H 0.9566 0.9546 0.3567 0.11(3) Uiso 1 1 d R . . H29B H 0.8612 1.0381 0.3006 0.40(11) Uiso 1 1 d RD . . 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 0.0158(4) 0.0166(4) 0.0151(4) -0.0005(3) 0.0021(3) 0.0008(3) Co2 0.0223(4) 0.0203(4) 0.0128(4) 0.0019(3) 0.0032(3) -0.0053(3) N1 0.0172(17) 0.0207(18) 0.0179(16) 0.0007(14) 0.0027(13) -0.0006(13) C2 0.025(2) 0.025(2) 0.025(2) 0.0000(17) 0.0027(17) 0.0013(18) C3 0.038(3) 0.018(2) 0.054(3) -0.001(2) -0.017(2) 0.002(2) C4 0.051(3) 0.050(3) 0.030(3) 0.026(2) -0.014(2) -0.026(3) C5 0.047(3) 0.051(3) 0.020(2) -0.004(2) 0.000(2) -0.027(3) C6 0.023(2) 0.041(3) 0.020(2) -0.0050(19) 0.0036(17) -0.0156(19) O9 0.0344(17) 0.0190(16) 0.0466(19) 0.0094(14) -0.0069(14) 0.0044(13) C10 0.017(2) 0.063(4) 0.040(3) -0.034(3) 0.0026(19) -0.006(2) C11 0.022(2) 0.030(3) 0.062(3) -0.016(2) -0.010(2) -0.003(2) C12 0.030(2) 0.029(3) 0.034(2) -0.003(2) -0.0118(19) 0.0002(19) C13 0.032(2) 0.024(2) 0.0183(19) -0.0010(18) -0.0023(16) -0.0039(19) N14 0.0219(17) 0.0254(19) 0.0150(16) -0.0016(14) 0.0016(13) -0.0038(14) C15 0.023(2) 0.047(3) 0.020(2) -0.008(2) 0.0026(17) -0.014(2) O16 0.0238(16) 0.040(2) 0.0332(18) -0.0113(15) 0.0087(14) -0.0114(14) O17 0.050(2) 0.0325(18) 0.0145(14) 0.0055(14) 0.0008(14) -0.0153(16) O18 0.0217(15) 0.0370(18) 0.0196(15) 0.0007(14) 0.0032(13) 0.0066(14) O19 0.0328(17) 0.0120(15) 0.0214(15) -0.0009(13) -0.0020(12) 0.0028(13) O20 0.0280(15) 0.0179(15) 0.0332(16) 0.0029(13) 0.0131(13) -0.0009(12) C21 0.028(2) 0.023(2) 0.0159(19) -0.0021(17) 0.0009(16) 0.0002(18) O22 0.063(2) 0.0317(18) 0.0320(17) 0.0029(14) 0.0230(16) 0.0106(16) C23 0.021(2) 0.025(2) 0.021(2) -0.0036(17) 0.0045(16) -0.0002(17) C24 0.021(2) 0.026(2) 0.0143(19) 0.0012(16) 0.0055(15) 0.0038(17) C25 0.017(2) 0.023(2) 0.021(2) -0.0002(17) -0.0012(16) 0.0009(16) O26 0.0363(17) 0.0224(16) 0.0423(18) 0.0030(14) 0.0246(15) 0.0066(13) O27 0.0245(14) 0.0186(14) 0.0210(14) 0.0027(12) 0.0027(11) 0.0001(12) O28 0.0254(16) 0.0190(16) 0.0259(15) 0.0013(13) 0.0053(12) 0.0028(13) O29 0.055(2) 0.037(2) 0.061(2) 0.0090(18) 0.0358(19) 0.0174(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 O19 2.041(3) 3_557 ? Co1 O18 2.113(3) 3_557 ? Co1 N1 2.166(3) 3_557 ? Co2 O17 2.049(3) 3_656 ? Co2 O16 2.101(3) 3_656 ? Co2 N14 2.161(3) 3_656 ? N1 C2 1.336(5) . ? N1 C6 1.343(5) . ? C2 C3 1.382(6) . ? C2 H2 0.9500 . ? C3 C4 1.398(7) . ? C3 H3 0.9500 . ? C4 C5 1.374(8) . ? C4 H4 0.9500 . ? C5 C6 1.363(6) . ? C5 C8B 1.470(14) . ? C5 N7A 1.486(7) . ? C6 H6A 0.9500 . ? C8A N7B 1.045(13) . ? C8A C8B 1.101(14) . ? C8A O9 1.265(6) . ? C8A N7A 1.363(7) . ? C8A C10 1.471(7) . ? C8B N7A 1.105(14) . ? C8B O9 1.309(14) . ? C8B N7B 1.335(19) . ? N7B C10 1.775(15) . ? C10 C11 1.381(7) . ? C10 C15 1.413(7) . ? C11 C12 1.357(7) . ? C11 H11 0.9500 . ? C12 C13 1.366(6) . ? C12 H12 0.9500 . ? C13 N14 1.340(5) . ? C13 H13 0.9500 . ? N14 C15 1.341(5) . ? C15 H15 0.9500 . ? O16 H16A 0.8400 . ? O16 H16B 0.81(6) . ? O17 H17A 0.8400 . ? O17 H17B 0.81(4) . ? O18 H18A 0.8400 . ? O18 H18B 0.79(4) . ? O19 H19A 0.8400 . ? O19 H19B 0.72(5) . ? O20 C21 1.257(5) . ? C21 O22 1.268(5) . ? C21 C23 1.500(5) . ? C23 C24 1.315(5) . ? C23 H23 0.9500 . ? C24 C25 1.480(5) . ? C24 H24 0.9500 . ? C25 O26 1.245(5) . ? C25 O27 1.281(5) . ? O28 H28A 0.78(5) . ? O28 H28B 0.97(5) . ? O29 H29A 0.8821 . ? O29 H29B 0.9608 . ? 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 O19 Co1 O19 180.000(1) 3_557 . ? O19 Co1 O18 87.49(12) 3_557 3_557 ? O19 Co1 O18 92.51(12) 3_557 . ? O18 Co1 O18 180.000(1) 3_557 . ? O19 Co1 N1 86.89(12) 3_557 . ? O19 Co1 N1 93.11(12) . . ? O18 Co1 N1 90.97(12) 3_557 . ? O18 Co1 N1 89.03(12) . . ? O19 Co1 N1 93.11(12) 3_557 3_557 ? O19 Co1 N1 86.89(12) . 3_557 ? O18 Co1 N1 89.03(12) 3_557 3_557 ? O18 Co1 N1 90.97(12) . 3_557 ? N1 Co1 N1 180.00(7) . 3_557 ? O17 Co2 O17 180.00(7) . 3_656 ? O17 Co2 O16 91.22(13) . . ? O17 Co2 O16 88.78(13) 3_656 . ? O17 Co2 O16 91.22(13) 3_656 3_656 ? O16 Co2 O16 180.0 . 3_656 ? O17 Co2 N14 90.78(12) . 3_656 ? O17 Co2 N14 89.22(12) 3_656 3_656 ? O16 Co2 N14 92.44(12) . 3_656 ? O16 Co2 N14 87.56(13) 3_656 3_656 ? O17 Co2 N14 89.22(12) . . ? O17 Co2 N14 90.78(12) 3_656 . ? O16 Co2 N14 87.56(13) . . ? O16 Co2 N14 92.44(13) 3_656 . ? N14 Co2 N14 180.00(15) 3_656 . ? C2 N1 C6 117.5(4) . . ? C2 N1 Co1 122.5(3) . . ? C6 N1 Co1 120.0(3) . . ? N1 C2 C3 122.5(4) . . ? N1 C2 H2 118.7 . . ? C3 C2 H2 118.7 . . ? C2 C3 C4 118.6(5) . . ? C2 C3 H3 120.7 . . ? C4 C3 H3 120.7 . . ? C5 C4 C3 119.0(4) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? C6 C5 C4 118.3(4) . . ? C6 C5 C8B 145.9(7) . . ? C4 C5 C8B 91.0(7) . . ? C6 C5 N7A 112.6(5) . . ? C4 C5 N7A 128.9(4) . . ? N1 C6 C5 124.1(4) . . ? N1 C6 H6A 117.9 . . ? C5 C6 H6A 117.9 . . ? N7B C8A C8B 76.9(11) . . ? N7B C8A O9 143.6(9) . . ? C8B C8A O9 66.8(8) . . ? C8B C8A N7A 52.0(8) . . ? O9 C8A N7A 118.7(5) . . ? N7B C8A C10 88.0(9) . . ? C8B C8A C10 164.7(9) . . ? O9 C8A C10 128.3(5) . . ? N7A C8A C10 113.1(5) . . ? C8A C8B N7A 76.4(10) . . ? C8A C8B O9 62.6(8) . . ? N7A C8B O9 138.9(13) . . ? O9 C8B N7B 112.3(12) . . ? C8A C8B C5 144.8(13) . . ? N7A C8B C5 68.8(8) . . ? O9 C8B C5 152.3(11) . . ? N7B C8B C5 95.2(11) . . ? N7B N7A C8B 98.2(16) . . ? C8B N7A C8A 51.7(8) . . ? N7B N7A C5 162.5(15) . . ? C8B N7A C5 67.3(8) . . ? C8A N7A C5 118.8(5) . . ? N7A N7B C8A 108.2(18) . . ? N7A N7B C8B 55.0(13) . . ? C8A N7B C8B 53.4(9) . . ? N7A N7B C10 163.8(18) . . ? C8A N7B C10 55.9(7) . . ? C8B N7B C10 109.3(10) . . ? C8A O9 C8B 50.6(6) . . ? C11 C10 C15 118.6(4) . . ? C11 C10 C8A 114.7(5) . . ? C15 C10 C8A 126.4(5) . . ? C11 C10 N7B 145.7(6) . . ? C15 C10 N7B 94.1(6) . . ? C12 C11 C10 118.4(4) . . ? C12 C11 H11 120.8 . . ? C10 C11 H11 120.8 . . ? C11 C12 C13 119.9(5) . . ? C11 C12 H12 120.1 . . ? C13 C12 H12 120.1 . . ? N14 C13 C12 124.2(4) . . ? N14 C13 H13 117.9 . . ? C12 C13 H13 117.9 . . ? C13 N14 C15 116.4(4) . . ? C13 N14 Co2 121.5(3) . . ? C15 N14 Co2 121.4(3) . . ? N14 C15 C10 122.4(4) . . ? N14 C15 H15 118.8 . . ? C10 C15 H15 118.8 . . ? Co2 O16 H16A 109.5 . . ? Co2 O16 H16B 127(5) . . ? H16A O16 H16B 122.7 . . ? Co2 O17 H17A 109.5 . . ? Co2 O17 H17B 125(3) . . ? H17A O17 H17B 113.9 . . ? Co1 O18 H18A 109.5 . . ? Co1 O18 H18B 124(3) . . ? H18A O18 H18B 126.5 . . ? Co1 O19 H19A 109.5 . . ? Co1 O19 H19B 125(4) . . ? H19A O19 H19B 117.3 . . ? O20 C21 O22 125.3(4) 1 . ? O20 C21 O22 125.3(4) . . ? O20 C21 C23 118.1(3) 1 . ? O20 C21 C23 118.1(3) . . ? O22 C21 C23 116.5(4) . . ? C24 C23 C21 122.7(4) . . ? C24 C23 H23 118.7 . . ? C21 C23 H23 118.7 . . ? C23 C24 C25 124.8(3) . . ? C23 C24 H24 117.6 . . ? C25 C24 H24 117.6 . . ? O26 C25 O27 124.2(4) 1 . ? O26 C25 O27 124.2(4) . . ? O26 C25 C24 120.6(4) 1 . ? O26 C25 C24 120.6(4) . . ? O27 C25 C24 115.2(3) . . ? H28A O28 H28B 100(4) . . ? H29A O29 H29B 132.3 . . ? 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 O16 H16A O26 0.84 2.08 2.915(4) 169.5 1 O16 H16B O29 0.81(6) 1.93(7) 2.716(5) 165(6) 1_545 O17 H17A O27 0.84 1.88 2.709(4) 167.9 3_656 O17 H17B O22 0.81(4) 1.77(4) 2.571(4) 171(4) 4_565 O18 H18A O20 0.84 1.89 2.714(4) 165.2 4_466 O18 H18B O28 0.79(4) 2.10(5) 2.890(4) 174(4) 2_546 O19 H19A O27 0.84 1.83 2.652(4) 164.1 3_657 O19 H19B O9 0.72(5) 1.92(5) 2.640(4) 173(6) 4_566 O28 H28A O20 0.78(5) 1.97(5) 2.742(4) 170(5) 1 O28 H28B O27 0.97(5) 1.88(5) 2.753(4) 150(4) 2_656 O29 H29A O26 0.88 1.90 2.769(4) 170.4 3_766 O29 H29B O20 0.96 2.19 3.024(5) 144.9 4_575 C13 H13 O22 0.95 2.58 3.461(5) 154.3 4_565 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.172 _refine_diff_density_min -0.342 _refine_diff_density_rms 0.084 # Attachment '2_kb494f2m_FINAL.cif' data_kb494f2m _database_code_depnum_ccdc_archive 'CCDC 644301' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H20 Co N3 O10' _chemical_formula_weight 461.27 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 8.8363(13) _cell_length_b 10.4211(16) _cell_length_c 10.8556(16) _cell_angle_alpha 78.769(3) _cell_angle_beta 75.255(3) _cell_angle_gamma 68.710(3) _cell_volume 894.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description PLATE _exptl_crystal_colour PALE-PINK _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.712 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 476 _exptl_absorpt_coefficient_mu 1.023 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.6504 _exptl_absorpt_correction_T_max 0.9046 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER CCD AREA DETECTOR' _diffrn_measurement_method 'PHI-OMEGA SCAN' _diffrn_detector_area_resol_mean 3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4626 _diffrn_reflns_av_R_equivalents 0.0382 _diffrn_reflns_av_sigmaI/netI 0.1009 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 25.50 _reflns_number_total 3255 _reflns_number_gt 2222 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER AXS SMART 3' _computing_cell_refinement 'BRUKER AXS SMART 3' _computing_data_reduction 'BRUKER AXS SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'BRUKER SHELXLTL' _computing_publication_material 'MERCURY 1.4' _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^)+(0.1051P)^2^+0.1474P] 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 3255 _refine_ls_number_parameters 270 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1037 _refine_ls_R_factor_gt 0.0650 _refine_ls_wR_factor_ref 0.1989 _refine_ls_wR_factor_gt 0.1573 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _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 O27 O 0.9880(6) 0.1517(5) 0.8432(4) 0.0176(10) Uani 1 1 d . . . Co1 Co 0.99522(11) 0.75572(9) 0.79166(8) 0.0117(3) Uani 1 1 d . . . N1 N 0.7502(6) 0.7895(5) 0.9061(5) 0.0128(11) Uani 1 1 d . . . C2 C 0.7111(8) 0.7685(6) 1.0336(6) 0.0156(14) Uani 1 1 d . . . H2 H 0.7978 0.7343 1.0805 0.019 Uiso 1 1 calc R . . C3 C 0.5500(8) 0.7945(7) 1.0999(6) 0.0179(15) Uani 1 1 d . . . C4 C 0.4200(8) 0.8486(7) 1.0312(7) 0.0199(15) Uani 1 1 d . . . H4 H 0.3074 0.8707 1.0747 0.024 Uiso 1 1 calc R . . C5 C 0.4608(8) 0.8684(6) 0.9001(6) 0.0180(15) Uani 1 1 d . . . H5 H 0.3767 0.9055 0.8507 0.022 Uiso 1 1 calc R . . C6 C 0.6265(8) 0.8335(6) 0.8407(6) 0.0162(14) Uani 1 1 d . . . H6 H 0.6542 0.8408 0.7497 0.019 Uiso 1 1 calc R . . N7 N 0.5217(8) 0.7709(7) 1.2369(6) 0.0317(16) Uani 1 1 d . . . H7 H 0.5908 0.7851 1.2743 0.038 Uiso 1 1 calc R . . C8 C 0.4017(9) 0.7299(7) 1.3115(7) 0.0256(17) Uani 1 1 d . . . O9 O 0.2929(6) 0.7055(5) 1.2680(4) 0.0249(11) Uani 1 1 d . . . C10 C 1.4035(9) 0.7054(7) 0.4524(6) 0.0190(15) Uani 1 1 d . . . C11 C 1.5480(8) 0.6579(6) 0.5018(7) 0.0215(16) Uani 1 1 d . . . H11 H 1.6536 0.6387 0.4459 0.026 Uiso 1 1 calc R . . C12 C 1.5351(8) 0.6390(6) 0.6339(7) 0.0183(15) Uani 1 1 d . . . H12 H 1.6314 0.6052 0.6702 0.022 Uiso 1 1 calc R . . C13 C 1.3797(8) 0.6703(7) 0.7108(6) 0.0174(15) Uani 1 1 d . . . H13 H 1.3715 0.6597 0.8009 0.021 Uiso 1 1 calc R . . N14 N 1.2379(7) 0.7153(5) 0.6657(5) 0.0153(12) Uani 1 1 d . . . C15 C 1.2521(8) 0.7301(6) 0.5384(6) 0.0163(14) Uani 1 1 d . . . H14 H 1.1538 0.7590 0.5051 0.020 Uiso 1 1 calc R . . O16 O 0.9439(5) 0.6472(4) 0.6784(4) 0.0148(10) Uani 1 1 d . . . C17 C 1.0211(10) 0.5201(7) 0.6674(6) 0.0250(17) Uani 1 1 d . . . O18 O 1.1237(7) 0.4363(5) 0.7375(5) 0.0340(13) Uani 1 1 d . . . C19 C 1.0129(8) 0.4618(7) 0.5548(6) 0.0171(14) Uani 1 1 d . . . H19 H 1.0267 0.3660 0.5624 0.021 Uiso 1 1 calc R . . O20 O 1.0563(5) 0.8696(4) 0.8991(4) 0.0161(10) Uani 1 1 d . . . O21 O 0.9053(5) 0.9461(4) 0.6745(4) 0.0152(10) Uani 1 1 d . . . O22 O 1.0967(6) 0.5737(4) 0.9170(4) 0.0164(10) Uani 1 1 d . . . O23 O 0.7246(5) 0.8879(5) 0.3172(4) 0.0169(10) Uani 1 1 d . . . C24 C 0.7334(8) 0.9275(6) 0.4171(6) 0.0121(13) Uani 1 1 d . . . O25 O 0.8664(5) 0.9220(4) 0.4433(4) 0.0157(10) Uani 1 1 d . . . C26 C 0.5743(8) 0.9890(6) 0.5099(6) 0.0131(13) Uani 1 1 d . . . H26A H 0.5820 1.0133 0.5875 0.016 Uiso 1 1 calc R . . O28 O 0.3368(7) 0.5335(5) 0.0609(5) 0.0404(15) Uani 1 1 d . . . H20B H 1.0249 0.8380 0.9921 0.05(2) Uiso 1 1 d R . . H27B H 0.9173 0.1955 0.7916 0.02(2) Uiso 1 1 d R . . H21A H 0.8901 0.9284 0.5962 0.03(2) Uiso 1 1 d R . . H21B H 0.9852 0.9863 0.6480 0.022(19) Uiso 1 1 d R . . H27A H 1.0804 0.1343 0.7840 0.07(3) Uiso 1 1 d R . . H20A H 1.0351 0.9658 0.8785 0.03(2) Uiso 1 1 d R . . H28B H 0.3127 0.5964 0.1185 0.050 Uiso 1 1 d R . . H28A H 0.4389 0.5181 0.0195 0.06(3) Uiso 1 1 d R . . H22A H 1.1251 0.5040 0.8641 0.16(6) Uiso 1 1 d 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 O27 0.016(2) 0.025(3) 0.012(2) 0.0025(19) -0.004(2) -0.009(2) Co1 0.0132(5) 0.0136(5) 0.0122(5) -0.0019(3) -0.0012(3) -0.0094(4) N1 0.016(3) 0.014(3) 0.010(3) 0.002(2) -0.004(2) -0.007(2) C2 0.016(3) 0.011(3) 0.022(4) 0.001(3) -0.006(3) -0.006(3) C3 0.020(4) 0.022(4) 0.014(3) -0.007(3) 0.002(3) -0.012(3) C4 0.013(3) 0.018(3) 0.029(4) -0.005(3) 0.001(3) -0.007(3) C5 0.022(4) 0.014(3) 0.023(4) 0.002(3) -0.012(3) -0.009(3) C6 0.023(4) 0.020(3) 0.010(3) 0.001(3) 0.000(3) -0.016(3) N7 0.030(4) 0.058(4) 0.020(3) -0.002(3) -0.003(3) -0.032(4) C8 0.018(4) 0.019(4) 0.033(4) 0.000(3) 0.001(3) -0.004(3) O9 0.024(3) 0.037(3) 0.023(3) 0.000(2) -0.005(2) -0.021(2) C10 0.028(4) 0.014(3) 0.017(3) 0.000(3) -0.001(3) -0.012(3) C11 0.015(4) 0.011(3) 0.032(4) -0.007(3) 0.012(3) -0.005(3) C12 0.015(4) 0.011(3) 0.028(4) -0.003(3) -0.004(3) -0.004(3) C13 0.023(4) 0.020(3) 0.016(3) -0.001(3) -0.004(3) -0.016(3) N14 0.018(3) 0.016(3) 0.012(3) 0.000(2) 0.005(2) -0.011(2) C15 0.019(4) 0.014(3) 0.017(3) 0.000(3) -0.003(3) -0.008(3) O16 0.013(2) 0.013(2) 0.020(2) -0.0072(19) -0.0034(19) -0.0034(19) C17 0.043(5) 0.022(4) 0.017(4) 0.006(3) -0.008(3) -0.020(4) O18 0.053(4) 0.024(3) 0.029(3) -0.003(2) -0.014(3) -0.013(3) C19 0.020(4) 0.015(3) 0.020(3) -0.005(3) -0.003(3) -0.010(3) O20 0.019(3) 0.015(2) 0.016(2) -0.0035(19) -0.002(2) -0.007(2) O21 0.015(2) 0.022(2) 0.014(2) -0.0003(19) -0.0025(19) -0.013(2) O22 0.019(3) 0.014(2) 0.017(2) -0.0024(19) -0.003(2) -0.007(2) O23 0.018(2) 0.024(3) 0.014(2) -0.004(2) -0.004(2) -0.012(2) C24 0.019(3) 0.006(3) 0.014(3) 0.001(2) -0.002(3) -0.009(3) O25 0.012(2) 0.021(2) 0.018(2) -0.0025(19) -0.0048(19) -0.009(2) C26 0.018(3) 0.011(3) 0.013(3) 0.000(3) -0.002(3) -0.009(3) O28 0.032(3) 0.039(3) 0.055(4) -0.024(3) -0.005(3) -0.010(3) _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 O27 H27B 0.8850 . ? O27 H27A 0.8855 . ? Co1 O16 2.049(4) . ? Co1 O20 2.093(4) . ? Co1 O21 2.138(4) . ? Co1 N1 2.145(5) . ? Co1 O22 2.153(4) . ? Co1 N14 2.173(5) . ? N1 C2 1.333(8) . ? N1 C6 1.346(8) . ? C2 C3 1.376(9) . ? C2 H2 0.9500 . ? C3 C4 1.412(10) . ? C3 N7 1.431(8) . ? C4 C5 1.370(9) . ? C4 H4 0.9500 . ? C5 C6 1.384(9) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? N7 C8 1.311(9) . ? N7 H7 0.8800 . ? C8 O9 1.291(9) . ? C8 C10 1.504(10) 1_456 ? C10 C15 1.392(9) . ? C10 C11 1.396(10) . ? C10 C8 1.504(10) 1_654 ? C11 C12 1.390(10) . ? C11 H11 0.9500 . ? C12 C13 1.373(9) . ? C12 H12 0.9500 . ? C13 N14 1.351(8) . ? C13 H13 0.9500 . ? N14 C15 1.339(8) . ? C15 H14 0.9500 . ? O16 C17 1.264(8) . ? C17 O18 1.297(9) . ? C17 C19 1.495(9) . ? C19 C19 1.318(13) 2_766 ? C19 H19 0.9500 . ? O20 H20B 0.9994 . ? O20 H20A 0.9431 . ? O21 H21A 0.9548 . ? O21 H21B 0.9066 . ? O22 H22A 0.9366 . ? O23 C24 1.262(7) . ? C24 O25 1.257(7) . ? C24 C26 1.510(9) . ? C26 C26 1.314(12) 2_676 ? C26 H26A 0.9500 . ? O28 H28B 0.9257 . ? O28 H28A 0.8711 . ? 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 H27B O27 H27A 97.9 . . ? O16 Co1 O20 177.00(17) . . ? O16 Co1 O21 91.57(16) . . ? O20 Co1 O21 86.99(16) . . ? O16 Co1 N1 89.18(18) . . ? O20 Co1 N1 93.45(18) . . ? O21 Co1 N1 89.75(18) . . ? O16 Co1 O22 93.56(17) . . ? O20 Co1 O22 87.82(17) . . ? O21 Co1 O22 174.66(17) . . ? N1 Co1 O22 91.80(18) . . ? O16 Co1 N14 86.61(19) . . ? O20 Co1 N14 90.74(18) . . ? O21 Co1 N14 89.71(18) . . ? N1 Co1 N14 175.7(2) . . ? O22 Co1 N14 89.12(19) . . ? C2 N1 C6 118.1(6) . . ? C2 N1 Co1 126.2(4) . . ? C6 N1 Co1 115.7(4) . . ? N1 C2 C3 122.5(6) . . ? N1 C2 H2 118.8 . . ? C3 C2 H2 118.8 . . ? C2 C3 C4 119.1(6) . . ? C2 C3 N7 117.9(6) . . ? C4 C3 N7 122.9(6) . . ? C5 C4 C3 118.2(6) . . ? C5 C4 H4 120.9 . . ? C3 C4 H4 120.9 . . ? C4 C5 C6 119.0(6) . . ? C4 C5 H5 120.5 . . ? C6 C5 H5 120.5 . . ? N1 C6 C5 123.0(6) . . ? N1 C6 H6 118.5 . . ? C5 C6 H6 118.5 . . ? C8 N7 C3 125.6(6) . . ? C8 N7 H7 117.2 . . ? C3 N7 H7 117.2 . . ? O9 C8 N7 122.9(7) . . ? O9 C8 C10 121.4(6) . 1_456 ? N7 C8 C10 115.5(6) . 1_456 ? C15 C10 C11 118.2(6) . . ? C15 C10 C8 117.9(6) . 1_654 ? C11 C10 C8 123.9(6) . 1_654 ? C12 C11 C10 119.0(6) . . ? C12 C11 H11 120.5 . . ? C10 C11 H11 120.5 . . ? C13 C12 C11 118.4(6) . . ? C13 C12 H12 120.8 . . ? C11 C12 H12 120.8 . . ? N14 C13 C12 123.8(6) . . ? N14 C13 H13 118.1 . . ? C12 C13 H13 118.1 . . ? C15 N14 C13 117.2(6) . . ? C15 N14 Co1 120.3(4) . . ? C13 N14 Co1 122.4(4) . . ? N14 C15 C10 123.2(6) . . ? N14 C15 H14 118.4 . . ? C10 C15 H14 118.4 . . ? C17 O16 Co1 123.2(4) . . ? O16 C17 O18 125.9(6) . . ? O16 C17 C19 118.6(6) . . ? O18 C17 C19 115.0(6) . . ? C19 C19 C17 122.5(8) 2_766 . ? C19 C19 H19 118.7 2_766 . ? C17 C19 H19 118.7 . . ? Co1 O20 H20B 108.7 . . ? Co1 O20 H20A 121.6 . . ? H20B O20 H20A 115.3 . . ? Co1 O21 H21A 110.4 . . ? Co1 O21 H21B 109.3 . . ? H21A O21 H21B 103.1 . . ? Co1 O22 H22A 101.0 . . ? O25 C24 O23 124.2(6) . . ? O25 C24 C26 117.5(5) . . ? O23 C24 C26 118.3(6) . . ? C24 C26 H26A 117.9 . . ? H28B O28 H28A 108.8 . . ? 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 C5 H5 O23 0.95 2.58 3.363(8) 139.8 2_676 C2 H2 O18 0.95 2.45 3.222(8) 138.8 2_767 O28 H28B O9 0.93 2.09 3.007(7) 168.2 1_554 O28 H28A O28 0.87 1.87 2.741(11) 174.2 2_665 O27 H27B O9 0.88 1.97 2.824(7) 160.7 2_667 O27 H27A O25 0.89 2.54 3.177(6) 130.0 2_766 O27 H27A O23 0.89 1.75 2.630(6) 170.4 2_766 O21 H21B O25 0.91 1.87 2.758(6) 166.5 2_776 O21 H21A O25 0.95 1.74 2.689(6) 170.8 1 O20 H20B O27 1.00 1.78 2.701(6) 150.8 2_767 O20 H20A O27 0.94 1.81 2.754(6) 178.0 1_565 N7 H7 O23 0.88 2.04 2.873(7) 157.9 1_556 _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.215 _refine_diff_density_min -0.665 _refine_diff_density_rms 0.180 # Attachment '3_kkb494d_FINAL.cif' data_kkb494d _database_code_depnum_ccdc_archive 'CCDC 644302' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H26 Co N3 O12' _chemical_formula_weight 547.36 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 P2(1)/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 14.8870(13) _cell_length_b 11.8596(10) _cell_length_c 13.9457(12) _cell_angle_alpha 90.00 _cell_angle_beta 115.3440(10) _cell_angle_gamma 90.00 _cell_volume 2225.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description PLATE _exptl_crystal_colour GOLDEN-YELLOW _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.634 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1136 _exptl_absorpt_coefficient_mu 0.844 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.8494 _exptl_absorpt_correction_T_max 0.9751 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER CCD AREA DETECTOR' _diffrn_measurement_method 'PHI-OMEGA SCAN' _diffrn_detector_area_resol_mean 3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12379 _diffrn_reflns_av_R_equivalents 0.0305 _diffrn_reflns_av_sigmaI/netI 0.0418 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 27.00 _reflns_number_total 4792 _reflns_number_gt 4020 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER AXS SMART 3' _computing_cell_refinement 'BRUKER AXS SMART 3' _computing_data_reduction 'BRUKER AXS SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'BRUKER SHELXLTL' _computing_publication_material 'MERCURY 1.4' _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^)+(0.0490P)^2^+1.6339P] 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 4792 _refine_ls_number_parameters 354 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0564 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.1067 _refine_ls_wR_factor_gt 0.1020 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.089 _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 0.64421(2) 0.81729(3) 0.26864(2) 0.01112(11) Uani 1 1 d . . . N1 N 0.80222(15) 0.79690(18) 0.34653(16) 0.0149(4) Uani 1 1 d . . . C2 C 0.83998(19) 0.6933(2) 0.3721(2) 0.0186(6) Uani 1 1 d . . . H2 H 0.7952 0.6316 0.3564 0.022 Uiso 1 1 calc R . . C3 C 0.9413(2) 0.6709(3) 0.4203(2) 0.0257(7) Uani 1 1 d . . . H3 H 0.9651 0.5958 0.4373 0.031 Uiso 1 1 calc R . . C4 C 1.00790(19) 0.7617(3) 0.4435(2) 0.0259(7) Uani 1 1 d . . . C5 C 0.9693(2) 0.8691(3) 0.4170(2) 0.0245(6) Uani 1 1 d . . . H5 H 1.0121 0.9325 0.4308 0.029 Uiso 1 1 calc R . . C6 C 0.8681(2) 0.8825(3) 0.3702(2) 0.0205(6) Uani 1 1 d . . . H6 H 0.8427 0.9569 0.3534 0.025 Uiso 1 1 calc R . . N7A N 1.11244(18) 0.7548(2) 0.49294(19) 0.0121(5) Uiso 0.82 1 d P . . N7B N 1.1804(10) 0.7345(12) 0.5272(11) 0.023(3) Uiso 0.18 1 d P . . C8A C 1.1645(2) 0.6556(3) 0.5260(2) 0.0116(6) Uiso 0.80 1 d P . . C8B C 1.1074(13) 0.6625(13) 0.4941(13) 0.028(3) Uiso 0.20 1 d P . . O9 O 1.12562(13) 0.56201(15) 0.51297(15) 0.0208(4) Uani 1 1 d . . . C10 C 1.27707(19) 0.6721(3) 0.5817(2) 0.0223(6) Uani 1 1 d . . . C11 C 1.33206(19) 0.5787(2) 0.5838(2) 0.0196(6) Uani 1 1 d . . . H11 H 1.3002 0.5115 0.5485 0.024 Uiso 1 1 calc R . . C12 C 1.43432(18) 0.5834(2) 0.6378(2) 0.0164(5) Uani 1 1 d . . . H12 H 1.4713 0.5177 0.6391 0.020 Uiso 1 1 calc R . . N13 N 1.48442(15) 0.67577(18) 0.68868(16) 0.0142(4) Uani 1 1 d . . . C14 C 1.43039(19) 0.7670(2) 0.68677(19) 0.0171(5) Uani 1 1 d . . . H14 H 1.4640 0.8334 0.7220 0.021 Uiso 1 1 calc R . . C15 C 1.3267(2) 0.7683(3) 0.6350(2) 0.0222(6) Uani 1 1 d . . . H15 H 1.2906 0.8339 0.6362 0.027 Uiso 1 1 calc R . . O16 O 0.63186(14) 0.95750(16) 0.35162(16) 0.0186(4) Uani 1 1 d . . . H10 H 0.5794 0.9527 0.3601 0.028 Uiso 1 1 calc R . . O17 O 0.63767(14) 0.70589(17) 0.38039(15) 0.0184(4) Uani 1 1 d . . . H17A H 0.6926 0.7053 0.4341 0.028 Uiso 1 1 calc R . . O18 O 0.63195(13) 0.68954(16) 0.15663(15) 0.0175(4) Uani 1 1 d D . . H18A H 0.6852 0.6858 0.1497 0.026 Uiso 1 1 calc R . . O19 O 0.66212(14) 0.92690(17) 0.15650(15) 0.0175(4) Uani 1 1 d . . . H19A H 0.7014 0.8974 0.1349 0.026 Uiso 1 1 calc R . . O20 O 0.31336(13) 0.65526(15) 0.34398(14) 0.0187(4) Uani 1 1 d . . . C21 C 0.26691(18) 0.7470(2) 0.33162(19) 0.0139(5) Uani 1 1 d . . . O22 O 0.30718(13) 0.84073(15) 0.36745(15) 0.0192(4) Uani 1 1 d . . . C23 C 0.15467(18) 0.7451(2) 0.27089(19) 0.0139(5) Uani 1 1 d . . . C24 C 0.10319(18) 0.8449(2) 0.22825(19) 0.0131(5) Uani 1 1 d . . . H24A H 0.1389 0.9130 0.2348 0.016 Uiso 1 1 calc R . . C25 C 0.00036(19) 0.8450(2) 0.17643(19) 0.0139(5) Uani 1 1 d . . . H25 H -0.0341 0.9127 0.1459 0.017 Uiso 1 1 calc R . . C26 C -0.05272(18) 0.7460(2) 0.16892(19) 0.0132(5) Uani 1 1 d . . . C27 C -0.00120(19) 0.6462(2) 0.2108(2) 0.0158(5) Uani 1 1 d . . . H27 H -0.0370 0.5783 0.2052 0.019 Uiso 1 1 calc R . . C28 C 0.10178(19) 0.6454(2) 0.26037(19) 0.0144(5) Uani 1 1 d . . . H28A H 0.1363 0.5768 0.2872 0.017 Uiso 1 1 calc R . . C29 C -0.16499(18) 0.7484(2) 0.12109(19) 0.0148(5) Uani 1 1 d . . . O30 O -0.20867(13) 0.65711(15) 0.12346(15) 0.0190(4) Uani 1 1 d . . . O31 O -0.20887(13) 0.83944(15) 0.08308(14) 0.0181(4) Uani 1 1 d . . . O32 O 0.46429(13) 0.97660(16) 0.39081(14) 0.0192(4) Uani 1 1 d D . . O33 O 0.50817(16) 0.8159(2) 0.9615(2) 0.0350(5) Uani 1 1 d D . . O34 O 0.21873(14) 0.95863(16) 0.47075(15) 0.0164(4) Uani 1 1 d D . . H16A H 0.678(2) 0.975(3) 0.401(3) 0.021(9) Uiso 1 1 d . . . H17B H 0.594(3) 0.705(3) 0.397(3) 0.039(11) Uiso 1 1 d . . . H18B H 0.600(4) 0.626(3) 0.146(5) 0.13(2) Uiso 1 1 d D . . H19B H 0.672(2) 0.991(3) 0.160(2) 0.018(8) Uiso 1 1 d . . . H32A H 0.4185(15) 0.9265(18) 0.3770(13) 0.023(8) Uiso 1 1 d D . . H32B H 0.4813 0.9912 0.4544 0.050 Uiso 1 1 d RD . . H33A H 0.4436(15) 0.821(3) 0.925(3) 0.060(13) Uiso 1 1 d D . . H33B H 0.529(4) 0.853(5) 1.017(4) 0.13(2) Uiso 1 1 d D . . H34A H 0.250(3) 0.920(3) 0.439(3) 0.048(11) Uiso 1 1 d D . . H34B H 0.201(2) 1.016(2) 0.441(2) 0.017(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 0.00977(17) 0.01235(18) 0.01097(17) -0.00046(13) 0.00418(13) 0.00003(13) N1 0.0125(10) 0.0186(11) 0.0135(10) 0.0002(8) 0.0055(9) -0.0015(8) C2 0.0183(13) 0.0262(15) 0.0146(12) 0.0052(11) 0.0101(11) 0.0054(11) C3 0.0267(15) 0.0371(18) 0.0159(13) 0.0128(12) 0.0117(12) 0.0177(13) C4 0.0119(13) 0.058(2) 0.0091(12) -0.0007(13) 0.0054(10) -0.0023(13) C5 0.0184(14) 0.0391(18) 0.0151(13) -0.0052(12) 0.0062(11) -0.0097(12) C6 0.0198(14) 0.0293(15) 0.0140(12) -0.0041(11) 0.0087(11) -0.0068(11) O9 0.0180(9) 0.0142(9) 0.0287(10) -0.0017(8) 0.0084(8) -0.0002(8) C10 0.0142(13) 0.0431(18) 0.0104(12) 0.0040(12) 0.0061(10) 0.0039(12) C11 0.0144(13) 0.0285(15) 0.0140(12) 0.0009(11) 0.0043(10) -0.0068(11) C12 0.0159(13) 0.0167(13) 0.0160(12) 0.0048(10) 0.0062(10) 0.0007(10) N13 0.0128(10) 0.0163(11) 0.0150(10) 0.0041(9) 0.0074(8) 0.0010(8) C14 0.0223(13) 0.0185(13) 0.0114(12) 0.0032(10) 0.0079(10) 0.0026(11) C15 0.0262(14) 0.0316(16) 0.0121(12) 0.0071(11) 0.0113(11) 0.0138(12) O16 0.0129(10) 0.0231(11) 0.0188(10) -0.0090(8) 0.0060(8) -0.0026(8) O17 0.0114(9) 0.0269(11) 0.0168(10) 0.0051(8) 0.0059(8) 0.0007(8) O18 0.0147(9) 0.0162(10) 0.0249(10) -0.0040(8) 0.0115(8) -0.0037(8) O19 0.0213(10) 0.0115(10) 0.0241(10) 0.0007(8) 0.0139(8) 0.0015(8) O20 0.0169(9) 0.0165(10) 0.0224(10) 0.0017(7) 0.0083(8) 0.0027(7) C21 0.0146(12) 0.0184(13) 0.0110(11) 0.0007(10) 0.0078(10) 0.0009(10) O22 0.0150(9) 0.0178(10) 0.0237(10) -0.0040(8) 0.0073(8) -0.0021(7) C23 0.0162(12) 0.0158(13) 0.0114(11) -0.0010(10) 0.0075(10) -0.0009(10) C24 0.0158(12) 0.0120(12) 0.0122(12) -0.0028(9) 0.0067(10) -0.0033(9) C25 0.0183(13) 0.0140(12) 0.0096(11) 0.0005(9) 0.0060(10) 0.0014(10) C26 0.0147(12) 0.0177(13) 0.0085(11) -0.0028(9) 0.0062(10) 0.0002(10) C27 0.0210(13) 0.0134(12) 0.0163(12) -0.0036(10) 0.0110(11) -0.0033(10) C28 0.0194(13) 0.0120(12) 0.0127(12) -0.0008(9) 0.0078(10) 0.0022(10) C29 0.0167(12) 0.0190(13) 0.0104(12) -0.0044(10) 0.0075(10) -0.0018(10) O30 0.0165(9) 0.0160(10) 0.0263(10) -0.0043(8) 0.0109(8) -0.0027(7) O31 0.0157(9) 0.0189(10) 0.0195(9) 0.0017(8) 0.0073(8) 0.0026(7) O32 0.0164(9) 0.0243(10) 0.0178(9) -0.0006(8) 0.0083(8) -0.0004(8) O33 0.0146(10) 0.0510(15) 0.0377(13) -0.0129(12) 0.0095(10) -0.0009(10) O34 0.0182(10) 0.0142(10) 0.0169(9) -0.0002(8) 0.0077(8) 0.0005(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 O17 2.0769(19) . ? Co1 O16 2.0785(19) . ? Co1 O18 2.1271(19) . ? Co1 O19 2.1362(19) . ? Co1 N1 2.141(2) . ? Co1 N13 2.154(2) 4_475 ? N1 C2 1.335(3) . ? N1 C6 1.351(3) . ? C2 C3 1.389(4) . ? C2 H2 0.9500 . ? C3 C4 1.404(4) . ? C3 H3 0.9500 . ? C4 C5 1.381(5) . ? C4 N7A 1.409(4) . ? C5 C6 1.370(4) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? N7A C8B 1.098(15) . ? N7A C8A 1.376(4) . ? N7B C8B 1.30(2) . ? N7B C10 1.503(14) . ? C8A O9 1.229(4) . ? C8A C10 1.528(4) . ? C8B O9 1.226(15) . ? C10 C11 1.370(4) . ? C10 C15 1.389(4) . ? C11 C12 1.381(4) . ? C11 H11 0.9500 . ? C12 N13 1.344(3) . ? C12 H12 0.9500 . ? N13 C14 1.342(3) . ? C14 C15 1.397(4) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? O16 H10 0.8400 . ? O16 H16A 0.76(3) . ? O17 H17A 0.8400 . ? O17 H17B 0.77(4) . ? O18 H18A 0.8400 . ? O18 H18B 0.86(2) . ? O19 H19A 0.8400 . ? O19 H19B 0.77(3) . ? O20 C21 1.260(3) . ? C21 O22 1.261(3) . ? C21 C23 1.516(3) . ? C23 C28 1.393(4) . ? C23 C24 1.397(3) . ? C24 C25 1.385(4) . ? C24 H24A 0.9500 . ? C25 C26 1.394(3) . ? C25 H25 0.9500 . ? C26 C27 1.395(4) . ? C26 C29 1.512(3) . ? C27 C28 1.386(4) . ? C27 H27 0.9500 . ? C28 H28A 0.9500 . ? C29 O31 1.256(3) . ? C29 O30 1.271(3) . ? O32 H32A 0.861(16) . ? O32 H32B 0.8301 . ? O33 H33A 0.876(19) . ? O33 H33B 0.83(3) . ? O34 H34A 0.90(3) . ? O34 H34B 0.78(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 O17 Co1 O16 92.72(8) . . ? O17 Co1 O18 94.65(8) . . ? O16 Co1 O18 168.08(8) . . ? O17 Co1 O19 175.58(7) . . ? O16 Co1 O19 89.39(8) . . ? O18 Co1 O19 83.92(7) . . ? O17 Co1 N1 86.66(8) . . ? O16 Co1 N1 98.49(8) . . ? O18 Co1 N1 91.28(8) . . ? O19 Co1 N1 89.19(8) . . ? O17 Co1 N13 90.96(8) . 4_475 ? O16 Co1 N13 85.20(8) . 4_475 ? O18 Co1 N13 85.32(7) . 4_475 ? O19 Co1 N13 93.10(8) . 4_475 ? N1 Co1 N13 175.68(8) . 4_475 ? C2 N1 C6 116.6(2) . . ? C2 N1 Co1 119.02(17) . . ? C6 N1 Co1 124.37(18) . . ? N1 C2 C3 123.4(3) . . ? N1 C2 H2 118.3 . . ? C3 C2 H2 118.3 . . ? C2 C3 C4 118.6(3) . . ? C2 C3 H3 120.7 . . ? C4 C3 H3 120.7 . . ? C5 C4 C3 118.3(2) . . ? C5 C4 N7A 115.5(3) . . ? C3 C4 N7A 126.2(3) . . ? C5 C4 C8B 153.4(6) . . ? C3 C4 C8B 88.3(5) . . ? C6 C5 C4 118.7(3) . . ? C6 C5 H5 120.6 . . ? C4 C5 H5 120.6 . . ? N1 C6 C5 124.4(3) . . ? N1 C6 H6 117.8 . . ? C5 C6 H6 117.8 . . ? N7B N7A C8B 78.7(12) . . ? N7B N7A C4 168.4(9) . . ? C8B N7A C4 89.8(9) . . ? C8A N7A C4 124.0(3) . . ? N7A N7B C8A 92.1(12) . . ? N7A N7B C8B 55.8(10) . . ? N7A N7B C10 164.9(14) . . ? C8A N7B C10 72.9(9) . . ? C8B N7B C10 109.3(12) . . ? C8B C8A N7B 96.2(14) . . ? C8B C8A O9 71.3(12) . . ? N7B C8A O9 167.5(9) . . ? C8B C8A N7A 52.9(12) . . ? O9 C8A N7A 124.1(3) . . ? C8B C8A C10 166.1(12) . . ? N7B C8A C10 70.1(9) . . ? O9 C8A C10 122.4(3) . . ? N7A C8A C10 113.5(3) . . ? C8A C8B N7A 92.8(15) . . ? C8A C8B O9 71.8(12) . . ? N7A C8B O9 164.2(17) . . ? O9 C8B N7B 119.1(15) . . ? C8A C8B C4 144.7(16) . . ? N7A C8B C4 52.2(7) . . ? O9 C8B C4 142.8(12) . . ? N7B C8B C4 97.7(11) . . ? C11 C10 C15 118.5(2) . . ? C11 C10 N7B 147.4(6) . . ? C15 C10 N7B 92.4(6) . . ? C11 C10 C8A 115.0(3) . . ? C15 C10 C8A 126.4(3) . . ? C10 C11 C12 119.2(3) . . ? C10 C11 H11 120.4 . . ? C12 C11 H11 120.4 . . ? N13 C12 C11 123.6(2) . . ? N13 C12 H12 118.2 . . ? C11 C12 H12 118.2 . . ? C14 N13 C12 117.0(2) . . ? C14 N13 Co1 119.96(17) . 4_676 ? C12 N13 Co1 123.01(17) . 4_676 ? N13 C14 C15 122.6(3) . . ? N13 C14 H14 118.7 . . ? C15 C14 H14 118.7 . . ? C10 C15 C14 119.0(2) . . ? C10 C15 H15 120.5 . . ? C14 C15 H15 120.5 . . ? Co1 O16 H10 109.5 . . ? Co1 O16 H16A 118(2) . . ? H10 O16 H16A 114.4 . . ? Co1 O17 H17A 109.5 . . ? Co1 O17 H17B 123(3) . . ? H17A O17 H17B 110.7 . . ? Co1 O18 H18A 109.5 . . ? Co1 O18 H18B 128(4) . . ? H18A O18 H18B 114.0 . . ? Co1 O19 H19A 109.5 . . ? Co1 O19 H19B 129(2) . . ? H19A O19 H19B 107.6 . . ? O20 C21 O22 124.5(2) . . ? O20 C21 C23 118.2(2) . . ? O22 C21 C23 117.2(2) . . ? C28 C23 C24 119.5(2) . . ? C28 C23 C21 120.6(2) . . ? C24 C23 C21 119.9(2) . . ? C25 C24 C23 120.3(2) . . ? C25 C24 H24A 119.8 . . ? C23 C24 H24A 119.8 . . ? C24 C25 C26 120.2(2) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C25 C26 C27 119.4(2) . . ? C25 C26 C29 120.1(2) . . ? C27 C26 C29 120.4(2) . . ? C28 C27 C26 120.5(2) . . ? C28 C27 H27 119.8 . . ? C26 C27 H27 119.8 . . ? C27 C28 C23 120.1(2) . . ? C27 C28 H28A 119.9 . . ? C23 C28 H28A 119.9 . . ? O31 C29 O30 124.3(2) . . ? O31 C29 C26 118.7(2) . . ? O30 C29 C26 117.0(2) . . ? H32A O32 H32B 103.5 . . ? H33A O33 H33B 113(5) . . ? H34A O34 H34B 108(3) . . ? 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 C3 H3 O9 0.95 2.57 3.207(4) 124.6 3_766 O34 H34B O30 0.78(3) 1.93(3) 2.669(3) 158(3) 2 O34 H34A O22 0.90(3) 1.82(3) 2.718(3) 177(3) 1 O33 H33B O19 0.83(3) 2.27(4) 3.008(3) 148(6) 1_556 O33 H33A O20 0.876(19) 1.80(2) 2.673(3) 173(4) 4_576 O32 H32A O22 0.861(16) 1.901(17) 2.742(3) 165(2) 1 O19 H19B O20 0.77(3) 1.96(3) 2.733(3) 175(3) 2_655 O19 H19A O31 0.84 1.90 2.738(3) 176.6 1_655 O18 H18B O32 0.86(2) 1.98(2) 2.838(3) 173(6) 2_645 O18 H18A O30 0.84 1.80 2.633(3) 170.8 1_655 O17 H17B O33 0.77(4) 1.87(4) 2.632(3) 167(4) 4_575 O17 H17A O31 0.84 2.04 2.823(3) 156.0 4_676 O16 H16A O34 0.76(3) 1.96(3) 2.712(3) 170(3) 3_676 O16 H10 O32 0.84 1.96 2.782(3) 167.1 1 _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.859 _refine_diff_density_min -0.330 _refine_diff_density_rms 0.093 # Attachment '4_kb537b1m_final.cif' data_kb537b1m _database_code_depnum_ccdc_archive 'CCDC 644303' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H37 Co2 N6 O28' _chemical_formula_weight 1143.60 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 14.228(2) _cell_length_b 14.831(3) _cell_length_c 14.954(3) _cell_angle_alpha 61.237(3) _cell_angle_beta 79.335(3) _cell_angle_gamma 66.117(3) _cell_volume 2529.1(8) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ROD _exptl_crystal_colour GOLDEN-YELLOW _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.502 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1170 _exptl_absorpt_coefficient_mu 0.752 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.7632 _exptl_absorpt_correction_T_max 0.9563 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 CCD AREA DETECTOR' _diffrn_measurement_method 'PHI-OMEGA SCAN' _diffrn_detector_area_resol_mean 3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13220 _diffrn_reflns_av_R_equivalents 0.0411 _diffrn_reflns_av_sigmaI/netI 0.1087 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 25.50 _reflns_number_total 9229 _reflns_number_gt 5577 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER AXS SMART 3' _computing_cell_refinement 'BRUKER AXS SMART 3' _computing_data_reduction 'BRUKER AXS SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'BRUKER SHELXLTL' _computing_publication_material 'MERCURY 1.4' _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^)+(0.1163P)^2^+4.6213P] 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 9229 _refine_ls_number_parameters 692 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1492 _refine_ls_R_factor_gt 0.0913 _refine_ls_wR_factor_ref 0.2563 _refine_ls_wR_factor_gt 0.2158 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.033 _refine_ls_shift/su_mean 0.001 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 1.18434(7) -0.41278(7) 0.73569(7) 0.0288(3) Uani 1 1 d . . . Co2 Co 0.68922(7) 0.59212(7) 0.72785(7) 0.0309(3) Uani 1 1 d . . . N1 N 1.1110(5) -0.2580(5) 0.7505(5) 0.0435(17) Uani 1 1 d . . . C2 C 1.0769(7) -0.2568(7) 0.8370(8) 0.055(2) Uani 1 1 d . . . H2 H 1.0868 -0.3238 0.8952 0.066 Uiso 1 1 calc R . . C3 C 1.0261(7) -0.1595(10) 0.8460(9) 0.072(3) Uani 1 1 d . . . H3 H 1.0042 -0.1618 0.9095 0.087 Uiso 1 1 calc R . . C4 C 1.0080(6) -0.0563(8) 0.7574(11) 0.071(3) Uani 1 1 d . . . C5 C 1.0466(7) -0.0604(8) 0.6703(11) 0.081(4) Uani 1 1 d . . . H5 H 1.0396 0.0049 0.6108 0.097 Uiso 1 1 calc R . . C6 C 1.0957(6) -0.1588(7) 0.6678(8) 0.055(2) Uani 1 1 d . . . H6 H 1.1205 -0.1581 0.6054 0.065 Uiso 1 1 calc R . . N7A N 0.9592(7) 0.0541(7) 0.7427(6) 0.031(2) Uiso 0.67 1 d P . . N7B N 0.9212(13) 0.1238(15) 0.7460(13) 0.030(4) Uiso 0.33 1 d P . . C8A C 0.9089(9) 0.0771(10) 0.8179(8) 0.038(3) Uiso 0.72 1 d P . . C8B C 0.954(2) 0.012(2) 0.8309(19) 0.030(6) Uiso 0.28 1 d P . . O9 O 0.9070(5) 0.0042(5) 0.9084(4) 0.0653(19) Uani 1 1 d . . . C10 C 0.8625(6) 0.2025(7) 0.7839(8) 0.052(2) Uani 1 1 d . . . C11 C 0.8478(7) 0.2289(7) 0.8629(7) 0.050(2) Uani 1 1 d . . . H11 H 0.8719 0.1742 0.9282 0.060 Uiso 1 1 calc R . . C12 C 0.7973(6) 0.3370(6) 0.8445(6) 0.0401(19) Uani 1 1 d . . . H12 H 0.7889 0.3528 0.8993 0.048 Uiso 1 1 calc R . . N13 N 0.7593(5) 0.4209(5) 0.7545(5) 0.0346(15) Uani 1 1 d . . . C14 C 0.7722(6) 0.3945(7) 0.6792(6) 0.043(2) Uani 1 1 d . . . H14 H 0.7451 0.4508 0.6154 0.052 Uiso 1 1 calc R . . C15 C 0.8234(6) 0.2884(8) 0.6891(8) 0.056(3) Uani 1 1 d . . . H15 H 0.8316 0.2749 0.6330 0.067 Uiso 1 1 calc R . . N16 N 0.6221(5) 0.7552(5) 0.7217(5) 0.0383(15) Uani 1 1 d . . . C17 C 0.5964(6) 0.7641(6) 0.8083(6) 0.047(2) Uani 1 1 d . . . H17 H 0.6152 0.6996 0.8695 0.056 Uiso 1 1 calc R . . C18 C 0.5436(7) 0.8629(7) 0.8128(7) 0.056(3) Uani 1 1 d . . . H18 H 0.5275 0.8643 0.8754 0.067 Uiso 1 1 calc R . . C19 C 0.5157(6) 0.9575(7) 0.7249(7) 0.042(2) Uani 1 1 d . . . C20 C 0.5429(6) 0.9519(6) 0.6341(7) 0.051(2) Uani 1 1 d . . . H20 H 0.5260 1.0160 0.5724 0.061 Uiso 1 1 calc R . . C21 C 0.5964(6) 0.8483(6) 0.6358(7) 0.043(2) Uani 1 1 d . . . H21 H 0.6146 0.8449 0.5742 0.051 Uiso 1 1 calc R . . N22 N 0.4567(5) 1.0563(6) 0.7363(5) 0.0519(19) Uani 1 1 d . . . H22 H 0.4453 1.0504 0.7971 0.062 Uiso 1 1 calc R . . C23 C 1.4202(7) -0.8472(8) 0.6609(7) 0.054(2) Uani 1 1 d . . . O24 O 1.4318(5) -0.8240(4) 0.5690(4) 0.0496(15) Uani 1 1 d . . . C25 C 1.3586(6) -0.7531(6) 0.6911(6) 0.041(2) Uani 1 1 d . . . C26 C 1.2831(6) -0.6637(6) 0.6261(6) 0.0415(19) Uani 1 1 d . . . H26 H 1.2650 -0.6632 0.5692 0.050 Uiso 1 1 calc R . . C27 C 1.2342(6) -0.5746(6) 0.6454(6) 0.0405(19) Uani 1 1 d . . . H27 H 1.1823 -0.5150 0.6002 0.049 Uiso 1 1 calc R . . N28 N 1.2545(5) -0.5661(5) 0.7229(5) 0.0344(15) Uani 1 1 d . . . C29 C 1.3300(6) -0.6529(6) 0.7873(6) 0.0403(19) Uani 1 1 d . . . H29 H 1.3471 -0.6489 0.8420 0.048 Uiso 1 1 calc R . . C30 C 1.3836(6) -0.7483(6) 0.7754(7) 0.045(2) Uani 1 1 d . . . H30 H 1.4348 -0.8074 0.8218 0.054 Uiso 1 1 calc R . . O31 O 1.0411(4) -0.4177(4) 0.7283(4) 0.0470(15) Uani 1 1 d . . . H31 H 1.0232 -0.4526 0.7860 0.070 Uiso 1 1 calc R . . O32 O 1.1776(4) -0.3239(4) 0.5774(4) 0.0399(13) Uani 1 1 d . . . H32 H 1.2349 -0.3239 0.5557 0.060 Uiso 1 1 calc R . . O33 O 1.3295(4) -0.4127(4) 0.7362(4) 0.0399(13) Uani 1 1 d . . . H33 H 1.3672 -0.4389 0.6992 0.060 Uiso 1 1 calc R . . O34 O 1.1893(5) -0.5003(4) 0.8945(4) 0.0468(14) Uani 1 1 d . . . H34 H 1.2414 -0.5062 0.9161 0.070 Uiso 1 1 calc R . . O35 O 0.7907(4) 0.6438(4) 0.6126(4) 0.0396(13) Uani 1 1 d . . . H35A H 0.8496 0.5994 0.6303 0.059 Uiso 1 1 calc R . . O36 O 0.7952(4) 0.5544(4) 0.8365(4) 0.0406(13) Uani 1 1 d . . . H36A H 0.7685 0.5388 0.8929 0.061 Uiso 1 1 calc R . . O37 O 0.5772(5) 0.5518(6) 0.8335(5) 0.0523(17) Uani 1 1 d . . . O38 O 0.5971(5) 0.6298(5) 0.6139(5) 0.0518(17) Uani 1 1 d . . . H38 H 0.5747 0.5807 0.6322 0.078 Uiso 1 1 calc R . . O39 O 0.8482(5) -0.2683(4) 0.7863(4) 0.0578(17) Uani 1 1 d . . . C40 C 0.8372(5) -0.1950(6) 0.6964(6) 0.0372(18) Uani 1 1 d . . . O41 O 0.8622(5) -0.2147(5) 0.6208(5) 0.0608(18) Uani 1 1 d . . . C42 C 0.7880(5) -0.0750(6) 0.6761(5) 0.0322(17) Uani 1 1 d . . . C43 C 0.7707(6) 0.0079(6) 0.5777(5) 0.040(2) Uani 1 1 d . . . H43 H 0.7921 -0.0100 0.5237 0.048 Uiso 1 1 calc R . . C44 C 0.7221(6) 0.1173(6) 0.5576(5) 0.0406(19) Uani 1 1 d . . . H44 H 0.7103 0.1719 0.4903 0.049 Uiso 1 1 calc R . . C45 C 0.6903(5) 0.1472(6) 0.6366(5) 0.0291(16) Uani 1 1 d . . . C46 C 0.7083(5) 0.0624(6) 0.7356(5) 0.0341(18) Uani 1 1 d . . . H46 H 0.6870 0.0797 0.7899 0.041 Uiso 1 1 calc R . . C47 C 0.7572(6) -0.0470(6) 0.7553(5) 0.0369(18) Uani 1 1 d . . . H47 H 0.7695 -0.1022 0.8223 0.044 Uiso 1 1 calc R . . C48 C 0.6385(5) 0.2663(6) 0.6143(5) 0.0321(17) Uani 1 1 d . . . O49 O 0.6487(4) 0.3378(4) 0.5274(4) 0.0402(13) Uani 1 1 d . . . O50 O 0.5866(4) 0.2875(4) 0.6834(4) 0.0462(14) Uani 1 1 d . . . O51 O 0.3751(9) 0.6934(6) 0.8772(9) 0.146(5) Uani 1 1 d . . . C52 C 0.3501(8) 0.7706(10) 0.7906(11) 0.074(3) Uani 1 1 d . . . O53 O 0.3669(6) 0.7576(6) 0.7121(8) 0.103(3) Uani 1 1 d . . . C54 C 0.2916(6) 0.8866(7) 0.7768(7) 0.045(2) Uani 1 1 d . . . C55 C 0.2774(6) 0.9743(7) 0.6838(7) 0.045(2) Uani 1 1 d . . . H55 H 0.3070 0.9625 0.6275 0.054 Uiso 1 1 calc R . . C56 C 0.2205(5) 1.0808(7) 0.6693(6) 0.0391(19) Uani 1 1 d . . . H56 H 0.2126 1.1400 0.6045 0.047 Uiso 1 1 calc R . . C57 C 0.1749(5) 1.0985(6) 0.7537(6) 0.0312(17) Uani 1 1 d . . . C58 C 0.1903(6) 1.0102(7) 0.8483(6) 0.045(2) Uani 1 1 d . . . H58 H 0.1608 1.0211 0.9050 0.054 Uiso 1 1 calc R . . C59 C 0.2494(7) 0.9052(7) 0.8602(7) 0.054(2) Uani 1 1 d . . . H59 H 0.2611 0.8459 0.9252 0.064 Uiso 1 1 calc R . . C60 C 0.1082(5) 1.2150(6) 0.7390(6) 0.0371(18) Uani 1 1 d . . . O61 O 0.1001(5) 1.2358(5) 0.8119(5) 0.0548(16) Uani 1 1 d . . . O62 O 0.0619(4) 1.2800(4) 0.6547(5) 0.0529(15) Uani 1 1 d . . . O63 O 0.1429(5) 0.3159(5) 0.0140(4) 0.0572(16) Uani 1 1 d . . . O64 O 0.2175(4) 0.1343(5) 0.9773(4) 0.0545(16) Uani 1 1 d . . . O65 O 0.0017(4) 0.7776(4) 0.4648(4) 0.0463(14) Uani 1 1 d . . . O66 O 0.3406(6) 0.5030(7) 0.9713(5) 0.086(2) Uani 1 1 d . . . O67 O 0.5375(6) 0.3635(5) 0.9537(5) 0.075(2) Uani 1 1 d . . . O68 O 0.4890(4) 0.5078(4) 0.6281(4) 0.0400(13) Uani 1 1 d . . . O69 O 0.4102(6) 0.7947(6) 0.1072(5) 0.075(2) Uani 1 1 d . . . O70 O 0.9704(6) 0.4933(5) 0.5989(7) 0.107(3) Uani 1 1 d . . . O71 O 0.9910(5) 0.3979(5) 0.8660(5) 0.0609(17) Uani 1 1 d . . . O72 O 0.4189(5) 0.9954(5) 0.9616(4) 0.0541(16) Uani 1 1 d . . . H35B H 0.803(6) 0.696(7) 0.621(6) 0.05(3) Uiso 1 1 d . . . H36B H 0.809(4) 0.622(5) 0.821(4) 0.013(15) Uiso 1 1 d . . . H37A H 0.526(7) 0.604(7) 0.811(6) 0.05(3) Uiso 1 1 d . . . H37B H 0.569(8) 0.481(10) 0.863(8) 0.10(4) Uiso 1 1 d . . . H38A H 0.572(6) 0.676(7) 0.567(6) 0.04(3) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0304(5) 0.0185(5) 0.0357(5) -0.0158(4) 0.0089(4) -0.0064(4) Co2 0.0337(6) 0.0193(5) 0.0396(6) -0.0176(4) 0.0077(4) -0.0074(4) N1 0.039(4) 0.029(4) 0.067(5) -0.029(3) 0.024(3) -0.018(3) C2 0.054(5) 0.040(5) 0.079(6) -0.042(5) 0.030(5) -0.018(4) C3 0.049(6) 0.094(9) 0.116(9) -0.090(8) 0.029(6) -0.025(6) C4 0.025(5) 0.041(6) 0.166(12) -0.068(7) 0.005(6) -0.006(4) C5 0.055(6) 0.030(5) 0.153(11) -0.048(7) 0.019(7) -0.010(5) C6 0.049(5) 0.028(5) 0.086(7) -0.030(5) 0.016(5) -0.015(4) O9 0.117(6) 0.034(3) 0.039(3) -0.021(3) 0.031(3) -0.029(3) C10 0.031(4) 0.038(5) 0.099(7) -0.048(5) 0.002(5) -0.004(4) C11 0.053(5) 0.034(5) 0.060(5) -0.021(4) -0.001(4) -0.012(4) C12 0.050(5) 0.031(4) 0.046(5) -0.030(4) 0.011(4) -0.012(4) N13 0.045(4) 0.025(3) 0.040(4) -0.022(3) 0.011(3) -0.013(3) C14 0.036(4) 0.050(5) 0.051(5) -0.031(4) -0.001(4) -0.011(4) C15 0.035(5) 0.065(6) 0.100(8) -0.074(6) -0.003(5) 0.000(4) N16 0.042(4) 0.025(4) 0.049(4) -0.022(3) 0.011(3) -0.011(3) C17 0.062(6) 0.029(4) 0.043(5) -0.016(4) 0.020(4) -0.019(4) C18 0.068(6) 0.030(5) 0.071(6) -0.032(5) 0.028(5) -0.019(4) C19 0.029(4) 0.039(5) 0.079(6) -0.047(5) 0.009(4) -0.009(4) C20 0.048(5) 0.019(4) 0.073(6) -0.014(4) -0.016(5) -0.001(4) C21 0.048(5) 0.032(5) 0.058(5) -0.032(4) -0.001(4) -0.009(4) N22 0.060(5) 0.048(5) 0.044(4) -0.020(4) 0.005(4) -0.019(4) C23 0.052(6) 0.047(6) 0.060(6) -0.017(5) 0.002(5) -0.025(5) O24 0.075(4) 0.023(3) 0.033(3) -0.013(2) 0.005(3) -0.003(3) C25 0.042(5) 0.031(5) 0.061(5) -0.033(4) 0.014(4) -0.015(4) C26 0.046(5) 0.032(4) 0.059(5) -0.032(4) 0.004(4) -0.012(4) C27 0.039(5) 0.029(4) 0.058(5) -0.027(4) -0.007(4) -0.005(4) N28 0.036(4) 0.024(3) 0.041(3) -0.020(3) 0.005(3) -0.004(3) C29 0.043(5) 0.025(4) 0.048(5) -0.020(4) 0.003(4) -0.006(4) C30 0.028(4) 0.018(4) 0.066(6) -0.007(4) -0.002(4) 0.000(3) O31 0.025(3) 0.032(3) 0.074(4) -0.017(3) 0.003(3) -0.011(2) O32 0.039(3) 0.035(3) 0.035(3) -0.010(2) 0.009(2) -0.014(3) O33 0.040(3) 0.040(3) 0.046(3) -0.030(3) 0.014(2) -0.013(3) O34 0.071(4) 0.036(3) 0.038(3) -0.021(3) 0.014(3) -0.023(3) O35 0.042(3) 0.031(3) 0.053(3) -0.026(3) 0.009(3) -0.014(3) O36 0.058(4) 0.025(3) 0.040(3) -0.018(3) 0.007(3) -0.014(3) O37 0.049(4) 0.036(4) 0.077(5) -0.036(3) 0.030(4) -0.019(3) O38 0.056(4) 0.036(4) 0.056(4) -0.009(3) -0.018(3) -0.016(3) O39 0.089(5) 0.024(3) 0.056(4) -0.018(3) -0.031(3) -0.004(3) C40 0.027(4) 0.028(4) 0.056(5) -0.025(4) -0.004(4) -0.001(3) O41 0.081(4) 0.049(4) 0.075(4) -0.051(3) 0.047(4) -0.037(3) C42 0.033(4) 0.031(4) 0.039(4) -0.022(3) 0.005(3) -0.012(3) C43 0.069(6) 0.039(5) 0.027(4) -0.024(4) 0.021(4) -0.030(4) C44 0.061(5) 0.030(4) 0.026(4) -0.011(3) 0.008(4) -0.018(4) C45 0.026(4) 0.025(4) 0.032(4) -0.012(3) 0.001(3) -0.009(3) C46 0.042(4) 0.032(4) 0.032(4) -0.022(3) 0.004(3) -0.007(3) C47 0.051(5) 0.022(4) 0.031(4) -0.012(3) -0.006(3) -0.005(4) C48 0.026(4) 0.028(4) 0.034(4) -0.013(3) -0.002(3) -0.002(3) O49 0.042(3) 0.024(3) 0.038(3) -0.009(2) 0.005(2) -0.005(2) O50 0.053(3) 0.029(3) 0.043(3) -0.017(3) 0.017(3) -0.009(3) O51 0.192(11) 0.035(5) 0.199(10) -0.036(6) -0.143(9) 0.013(5) C52 0.053(6) 0.070(8) 0.135(11) -0.068(8) -0.011(7) -0.023(6) O53 0.085(6) 0.074(5) 0.193(10) -0.097(6) 0.056(6) -0.047(5) C54 0.031(4) 0.035(5) 0.082(7) -0.039(5) -0.014(4) -0.002(4) C55 0.033(4) 0.054(6) 0.066(6) -0.048(5) 0.005(4) -0.009(4) C56 0.030(4) 0.049(5) 0.038(4) -0.018(4) -0.001(3) -0.016(4) C57 0.020(4) 0.033(4) 0.047(4) -0.024(4) 0.002(3) -0.010(3) C58 0.056(5) 0.042(5) 0.048(5) -0.029(4) 0.008(4) -0.021(4) C59 0.060(6) 0.034(5) 0.060(6) -0.012(4) -0.014(5) -0.017(4) C60 0.025(4) 0.031(4) 0.057(5) -0.023(4) -0.004(4) -0.006(3) O61 0.062(4) 0.044(4) 0.066(4) -0.039(3) 0.001(3) -0.009(3) O62 0.057(4) 0.033(3) 0.063(4) -0.023(3) -0.015(3) -0.004(3) O63 0.084(5) 0.040(3) 0.046(3) -0.011(3) -0.001(3) -0.031(3) O64 0.058(4) 0.047(4) 0.057(4) -0.027(3) 0.002(3) -0.015(3) O65 0.038(3) 0.052(4) 0.038(3) -0.013(3) 0.001(2) -0.016(3) O66 0.113(6) 0.106(6) 0.056(4) -0.033(4) -0.005(4) -0.058(5) O67 0.108(6) 0.051(4) 0.067(4) -0.025(4) 0.009(4) -0.036(4) O68 0.036(3) 0.033(3) 0.054(3) -0.027(3) 0.003(2) -0.009(2) O69 0.100(5) 0.067(5) 0.065(4) -0.031(4) -0.003(4) -0.035(4) O70 0.091(6) 0.037(4) 0.133(7) -0.027(4) 0.046(5) -0.001(4) O71 0.062(4) 0.042(4) 0.076(4) -0.036(3) -0.005(3) -0.003(3) O72 0.077(4) 0.047(4) 0.038(3) -0.020(3) 0.006(3) -0.023(3) _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 O33 2.068(5) . ? Co1 O32 2.080(5) . ? Co1 O34 2.085(5) . ? Co1 O31 2.093(5) . ? Co1 N28 2.172(6) . ? Co1 N1 2.207(6) . ? Co2 O38 2.062(6) . ? Co2 O37 2.080(6) . ? Co2 O35 2.085(5) . ? Co2 O36 2.139(6) . ? Co2 N16 2.173(6) . ? Co2 N13 2.173(6) . ? N1 C2 1.301(10) . ? N1 C6 1.353(10) . ? C2 C3 1.390(12) . ? C2 H2 0.9300 . ? C3 C4 1.421(15) . ? C3 H3 0.9300 . ? C4 C5 1.337(16) . ? C4 N7A 1.415(12) . ? C5 C6 1.355(12) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? N7A C8B 1.16(3) . ? N7A C8A 1.329(14) . ? N7B C10 1.433(19) . ? N7B C8B 1.47(3) . ? C8A O9 1.265(12) . ? C8A C10 1.540(14) . ? C8B O9 1.20(3) . ? C10 C11 1.372(12) . ? C10 C15 1.386(13) . ? C11 C12 1.370(10) . ? C11 H11 0.9300 . ? C12 N13 1.328(9) . ? C12 H12 0.9300 . ? N13 C14 1.322(9) . ? C14 C15 1.384(11) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? N16 C21 1.322(10) . ? N16 C17 1.333(10) . ? C17 C18 1.379(11) . ? C17 H17 0.9300 . ? C18 C19 1.350(12) . ? C18 H18 0.9300 . ? C19 C20 1.374(12) . ? C19 N22 1.439(10) . ? C20 C21 1.402(10) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? N22 C23 1.286(10) 1_475 ? N22 H22 0.8600 . ? C23 O24 1.242(10) . ? C23 C25 1.545(11) . ? C25 C26 1.360(11) . ? C25 C30 1.413(12) . ? C26 C27 1.365(10) . ? C26 H26 0.9300 . ? C27 N28 1.317(9) . ? C27 H27 0.9300 . ? N28 C29 1.344(9) . ? C29 C30 1.390(10) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? O31 H31 0.8200 . ? O32 H32 0.8200 . ? O33 H33 0.8200 . ? O34 H34 0.8200 . ? O35 H35A 0.8200 . ? O35 H35B 0.92(9) . ? O36 H36A 0.8200 . ? O36 H36B 1.01(6) . ? O37 H37A 0.79(8) . ? O37 H37B 0.97(12) . ? O38 H38 0.8200 . ? O38 H38A 0.73(7) . ? O39 C40 1.244(9) . ? C40 O41 1.255(9) . ? C40 C42 1.516(10) . ? C42 C43 1.374(10) . ? C42 C47 1.378(10) . ? C43 C44 1.378(10) . ? C43 H43 0.9300 . ? C44 C45 1.394(10) . ? C44 H44 0.9300 . ? C45 C46 1.388(9) . ? C45 C48 1.497(10) . ? C46 C47 1.381(10) . ? C46 H46 0.9300 . ? C47 H47 0.9300 . ? C48 O50 1.247(8) . ? C48 O49 1.251(8) . ? O51 C52 1.236(15) . ? C52 O53 1.244(14) . ? C52 C54 1.502(13) . ? C54 C55 1.348(12) . ? C54 C59 1.384(12) . ? C55 C56 1.378(11) . ? C55 H55 0.9300 . ? C56 C57 1.400(10) . ? C56 H56 0.9300 . ? C57 C58 1.366(11) . ? C57 C60 1.522(10) . ? C58 C59 1.376(11) . ? C58 H58 0.9300 . ? C59 H59 0.9300 . ? C60 O61 1.242(9) . ? C60 O62 1.256(9) . ? 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 O33 Co1 O32 90.2(2) . . ? O33 Co1 O34 90.3(2) . . ? O32 Co1 O34 179.2(2) . . ? O33 Co1 O31 176.1(2) . . ? O32 Co1 O31 87.6(2) . . ? O34 Co1 O31 92.0(2) . . ? O33 Co1 N28 89.0(2) . . ? O32 Co1 N28 89.8(2) . . ? O34 Co1 N28 90.8(2) . . ? O31 Co1 N28 87.7(2) . . ? O33 Co1 N1 91.7(2) . . ? O32 Co1 N1 90.8(2) . . ? O34 Co1 N1 88.6(2) . . ? O31 Co1 N1 91.5(2) . . ? N28 Co1 N1 179.0(2) . . ? O38 Co2 O37 89.3(3) . . ? O38 Co2 O35 86.5(3) . . ? O37 Co2 O35 174.8(3) . . ? O38 Co2 O36 175.0(2) . . ? O37 Co2 O36 95.6(3) . . ? O35 Co2 O36 88.7(2) . . ? O38 Co2 N16 95.4(3) . . ? O37 Co2 N16 87.3(2) . . ? O35 Co2 N16 90.1(2) . . ? O36 Co2 N16 85.6(2) . . ? O38 Co2 N13 90.7(3) . . ? O37 Co2 N13 88.9(2) . . ? O35 Co2 N13 94.1(2) . . ? O36 Co2 N13 88.6(2) . . ? N16 Co2 N13 172.7(2) . . ? C2 N1 C6 116.8(7) . . ? C2 N1 Co1 122.3(6) . . ? C6 N1 Co1 120.8(6) . . ? N1 C2 C3 122.7(9) . . ? N1 C2 H2 118.6 . . ? C3 C2 H2 118.6 . . ? C2 C3 C4 119.3(10) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C5 C4 N7A 111.3(11) . . ? C5 C4 C3 116.4(8) . . ? N7A C4 C3 132.2(11) . . ? C5 C4 C8B 152.7(13) . . ? N7A C4 C8B 42.1(9) . . ? C3 C4 C8B 90.2(12) . . ? C4 C5 C6 120.6(11) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C5 C6 N1 124.0(10) . . ? C5 C6 H6 118.0 . . ? N1 C6 H6 118.0 . . ? N7B N7A C8B 86.4(18) . . ? N7B N7A C4 169.0(15) . . ? C8B N7A C4 83.0(16) . . ? C8A N7A C4 121.1(10) . . ? N7A N7B C8A 85.2(17) . . ? N7A N7B C10 161.7(19) . . ? C8A N7B C10 76.5(14) . . ? N7A N7B C8B 52.1(14) . . ? C10 N7B C8B 109.9(16) . . ? C8B C8A N7B 104(2) . . ? C8B C8A O9 65.8(19) . . ? N7B C8A O9 169.9(17) . . ? C8B C8A N7A 59.3(19) . . ? O9 C8A N7A 123.7(11) . . ? C8B C8A C10 160(2) . . ? N7B C8A C10 64.8(13) . . ? O9 C8A C10 124.4(10) . . ? N7A C8A C10 111.7(9) . . ? C8A C8B N7A 81(2) . . ? C8A C8B O9 73(2) . . ? N7A C8B O9 151(3) . . ? O9 C8B N7B 114(2) . . ? C8A C8B C4 133(3) . . ? N7A C8B C4 54.9(12) . . ? O9 C8B C4 142(2) . . ? N7B C8B C4 96.4(16) . . ? C8B O9 C8A 40.9(12) . . ? C11 C10 C15 117.1(7) . . ? C11 C10 N7B 146.3(11) . . ? C15 C10 N7B 94.8(10) . . ? C11 C10 C8A 113.4(9) . . ? C15 C10 C8A 129.0(9) . . ? C10 C11 C12 119.2(8) . . ? C10 C11 H11 120.4 . . ? C12 C11 H11 120.4 . . ? N13 C12 C11 125.0(7) . . ? N13 C12 H12 117.5 . . ? C11 C12 H12 117.5 . . ? C14 N13 C12 115.4(6) . . ? C14 N13 Co2 121.2(5) . . ? C12 N13 Co2 123.3(5) . . ? N13 C14 C15 124.2(8) . . ? N13 C14 H14 117.9 . . ? C15 C14 H14 117.9 . . ? C14 C15 C10 119.1(8) . . ? C14 C15 H15 120.5 . . ? C10 C15 H15 120.5 . . ? C21 N16 C17 116.8(6) . . ? C21 N16 Co2 123.6(5) . . ? C17 N16 Co2 119.3(5) . . ? N16 C17 C18 124.1(8) . . ? N16 C17 H17 118.0 . . ? C18 C17 H17 118.0 . . ? C19 C18 C17 119.0(8) . . ? C19 C18 H18 120.5 . . ? C17 C18 H18 120.5 . . ? C18 C19 C20 118.6(7) . . ? C18 C19 N22 115.4(8) . . ? C20 C19 N22 126.0(8) . . ? C19 C20 C21 119.0(8) . . ? C19 C20 H20 120.5 . . ? C21 C20 H20 120.5 . . ? N16 C21 C20 122.5(8) . . ? N16 C21 H21 118.7 . . ? C20 C21 H21 118.7 . . ? C23 N22 C19 123.7(8) 1_475 . ? C23 N22 H22 118.2 1_475 . ? C19 N22 H22 118.2 . . ? O24 C23 N22 126.3(9) . 1_635 ? O24 C23 C25 118.9(8) . . ? N22 C23 C25 114.8(8) 1_635 . ? C26 C25 C30 117.8(7) . . ? C26 C25 C23 117.8(7) . . ? C30 C25 C23 124.0(7) . . ? C25 C26 C27 119.2(8) . . ? C25 C26 H26 120.4 . . ? C27 C26 H26 120.4 . . ? N28 C27 C26 125.3(7) . . ? N28 C27 H27 117.3 . . ? C26 C27 H27 117.3 . . ? C27 N28 C29 116.5(6) . . ? C27 N28 Co1 121.9(5) . . ? C29 N28 Co1 121.2(5) . . ? N28 C29 C30 122.8(8) . . ? N28 C29 H29 118.6 . . ? C30 C29 H29 118.6 . . ? C29 C30 C25 118.4(7) . . ? C29 C30 H30 120.8 . . ? C25 C30 H30 120.8 . . ? Co1 O31 H31 109.5 . . ? Co1 O32 H32 109.5 . . ? Co1 O33 H33 109.5 . . ? Co1 O34 H34 109.5 . . ? Co2 O35 H35A 109.5 . . ? Co2 O35 H35B 106(5) . . ? H35A O35 H35B 92.2 . . ? Co2 O36 H36A 109.5 . . ? Co2 O36 H36B 111(3) . . ? H36A O36 H36B 103.7 . . ? Co2 O37 H37A 105(6) . . ? Co2 O37 H37B 124(7) . . ? H37A O37 H37B 114(9) . . ? Co2 O38 H38 109.5 . . ? Co2 O38 H38A 140(7) . . ? H38 O38 H38A 109.9 . . ? O39 C40 O41 123.5(7) . . ? O39 C40 C42 118.7(7) . . ? O41 C40 C42 117.7(7) . . ? C43 C42 C47 118.8(7) . . ? C43 C42 C40 120.2(7) . . ? C47 C42 C40 121.0(7) . . ? C42 C43 C44 121.1(7) . . ? C42 C43 H43 119.5 . . ? C44 C43 H43 119.5 . . ? C43 C44 C45 121.0(7) . . ? C43 C44 H44 119.5 . . ? C45 C44 H44 119.5 . . ? C46 C45 C44 117.2(6) . . ? C46 C45 C48 122.0(6) . . ? C44 C45 C48 120.8(6) . . ? C47 C46 C45 121.6(7) . . ? C47 C46 H46 119.2 . . ? C45 C46 H46 119.2 . . ? C46 C47 C42 120.4(7) . . ? C46 C47 H47 119.8 . . ? C42 C47 H47 119.8 . . ? O50 C48 O49 124.3(7) . . ? O50 C48 C45 117.7(6) . . ? O49 C48 C45 118.0(6) . . ? O51 C52 O53 123.4(11) . . ? O51 C52 C54 120.0(12) . . ? O53 C52 C54 116.6(12) . . ? C55 C54 C59 118.5(7) . . ? C55 C54 C52 121.4(9) . . ? C59 C54 C52 120.1(9) . . ? C54 C55 C56 122.1(8) . . ? C54 C55 H55 118.9 . . ? C56 C55 H55 118.9 . . ? C55 C56 C57 119.0(7) . . ? C55 C56 H56 120.5 . . ? C57 C56 H56 120.5 . . ? C58 C57 C56 119.1(7) . . ? C58 C57 C60 120.9(7) . . ? C56 C57 C60 120.0(7) . . ? C57 C58 C59 120.3(8) . . ? C57 C58 H58 119.9 . . ? C59 C58 H58 119.9 . . ? C54 C59 C58 120.9(8) . . ? C54 C59 H59 119.5 . . ? C58 C59 H59 119.5 . . ? O61 C60 O62 126.0(7) . . ? O61 C60 C57 118.1(7) . . ? O62 C60 C57 115.9(7) . . ? 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 N22 H22 O72 0.86 2.20 3.041(9) 166.3 1 O31 H31 O71 0.82 2.15 2.801(8) 136.2 1_545 O32 H32 O49 0.82 1.88 2.659(7) 158.1 2_756 O33 H33 O68 0.82 1.94 2.732(7) 160.9 1_645 O34 H34 O66 0.82 1.84 2.648(9) 168.4 1_645 O35 H35A O70 0.82 1.97 2.680(8) 144.7 1 O35 H35B O41 0.92(9) 1.84(9) 2.735(8) 163(8) 1_565 O36 H36A O66 0.82 2.31 3.104(9) 164.5 2_667 O36 H36B O39 1.01(6) 1.74(6) 2.746(8) 172(5) 1_565 O37 H37A O51 0.79(8) 2.35(9) 2.972(13) 136(8) 1 O37 H37A O53 0.79(8) 2.52(9) 3.293(12) 169(9) 1 O37 H37B O67 0.97(12) 1.79(12) 2.725(9) 160(10) 1 O38 H38 O68 0.82 1.95 2.729(8) 157.5 1 O38 H38A O24 0.73(7) 2.14(8) 2.796(8) 150(9) 2_756 C21 H21 O24 0.93 2.54 3.362(10) 147.9 2_756 _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.024 _refine_diff_density_min -0.622 _refine_diff_density_rms 0.193