# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 1350 loop_ _publ_author_name 'Ming-Liang Tong' 'Zhuo-jia Lin' 'Wen-Ting Liu' 'Yong-Cong Ou' _publ_contact_author_name 'Ming-Liang Tong' _publ_contact_author_email TONGML@MAIL.SYSU.EDU.CN _publ_section_title ; Coordination polymers of the conformation-flexible 1,2,4,5-cyclohexanete- tracarboxylate. Synthesis, structures and transforming mechanism studies ; # Attachment 'cif.cif' data_compound1 _database_code_depnum_ccdc_archive 'CCDC 768141' #TrackingRef 'cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H28 Co2 N3 O12' _chemical_formula_weight 680.36 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2183(13) _cell_length_b 11.3812(14) _cell_length_c 12.9323(16) _cell_angle_alpha 113.731(2) _cell_angle_beta 94.737(3) _cell_angle_gamma 101.552(2) _cell_volume 1326.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour purple _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.704 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 698 _exptl_absorpt_coefficient_mu 1.323 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8132 _exptl_absorpt_correction_T_max 0.9626 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6937 _diffrn_reflns_av_R_equivalents 0.0287 _diffrn_reflns_av_sigmaI/netI 0.0715 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5077 _reflns_number_gt 3926 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 1998)' _computing_cell_refinement 'Bruker SMART (Bruker, 1998)' _computing_data_reduction 'Bruker SAINT + & SHELXTL (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0558P)^2^+0.6987P] 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 5077 _refine_ls_number_parameters 379 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0755 _refine_ls_R_factor_gt 0.0553 _refine_ls_wR_factor_ref 0.1288 _refine_ls_wR_factor_gt 0.1175 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.027 _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 0.23584(5) 0.52095(5) 0.32737(5) 0.01855(16) Uani 1 1 d . . . Co2 Co 0.29336(6) -0.01538(6) -0.11772(5) 0.02572(18) Uani 1 1 d . . . O1 O 0.4560(3) 0.5637(3) 0.3500(2) 0.0259(7) Uani 1 1 d . . . O2 O 0.3288(3) 0.4759(3) 0.1798(2) 0.0241(6) Uani 1 1 d . . . O3 O 0.4445(3) 0.2348(3) 0.1409(3) 0.0344(8) Uani 1 1 d . . . O4 O 0.3853(3) 0.1779(3) -0.0457(3) 0.0350(8) Uani 1 1 d . . . O5 O 0.6946(3) 0.1209(3) 0.0059(3) 0.0333(8) Uani 1 1 d . . . O6 O 0.7885(3) 0.2242(3) 0.1863(3) 0.0330(8) Uani 1 1 d . . . O7 O 1.0369(3) 0.4581(3) 0.2360(2) 0.0220(6) Uani 1 1 d . . . O8 O 0.9397(3) 0.5465(3) 0.3874(3) 0.0339(8) Uani 1 1 d . . . O1W O 0.1884(3) 0.5938(3) 0.4917(2) 0.0278(7) Uani 1 1 d D . . H1WA H 0.1052 0.5780 0.4621 0.033 Uiso 1 1 d RD . . H1WB H 0.1919 0.5552 0.5360 0.033 Uiso 1 1 d RD . . O2W O 0.1234(4) 0.0446(4) -0.0343(4) 0.0554(11) Uani 1 1 d D . . H2WA H 0.1021 0.1139 -0.0316 0.067 Uiso 1 1 d RD . . H2WB H 0.1413 0.0542 0.0345 0.067 Uiso 1 1 d RD . . O3W O 0.4754(3) -0.0430(3) -0.1742(3) 0.0376(8) Uani 1 1 d D . . H3WA H 0.4960 -0.1102 -0.1708 0.045 Uiso 1 1 d RD . . H3WB H 0.5332 0.0273 -0.1265 0.045 Uiso 1 1 d RD . . O4W O 0.1070(3) 0.3012(4) 0.0126(3) 0.0510(10) Uani 1 1 d D . . H4WA H 0.1904 0.3409 0.0392 0.061 Uiso 1 1 d RD . . H4WB H 0.0598 0.3368 0.0618 0.061 Uiso 1 1 d RD . . N1 N 0.2385(3) 0.3366(3) 0.3326(3) 0.0237(8) Uani 1 1 d . . . N2 N 0.2466(4) -0.2861(3) 0.3310(3) 0.0261(8) Uani 1 1 d . . . N3 N 0.1984(4) -0.0051(4) -0.2642(3) 0.0283(8) Uani 1 1 d . . . C1 C 0.5690(4) 0.5010(4) 0.1858(3) 0.0201(9) Uani 1 1 d . . . H1A H 0.6002 0.5833 0.1773 0.024 Uiso 1 1 calc R . . C2 C 0.5319(4) 0.3882(4) 0.0644(3) 0.0196(9) Uani 1 1 d . . . H2A H 0.4756 0.4165 0.0184 0.024 Uiso 1 1 calc R . . C3 C 0.6586(4) 0.3696(4) 0.0089(3) 0.0210(9) Uani 1 1 d . . . H3A H 0.6328 0.2894 -0.0625 0.025 Uiso 1 1 calc R . . H3B H 0.6908 0.4437 -0.0095 0.025 Uiso 1 1 calc R . . C4 C 0.7759(4) 0.3598(4) 0.0855(4) 0.0205(9) Uani 1 1 d . . . H4A H 0.8556 0.3660 0.0489 0.025 Uiso 1 1 calc R . . C5 C 0.8105(4) 0.4804(4) 0.2023(3) 0.0185(8) Uani 1 1 d . . . H5A H 0.8316 0.5579 0.1854 0.022 Uiso 1 1 calc R . . C6 C 0.6866(4) 0.4924(4) 0.2615(4) 0.0226(9) Uani 1 1 d . . . H6A H 0.6579 0.4158 0.2775 0.027 Uiso 1 1 calc R . . H6B H 0.7113 0.5711 0.3341 0.027 Uiso 1 1 calc R . . C7 C 0.4448(4) 0.5135(4) 0.2424(4) 0.0204(9) Uani 1 1 d . . . C8 C 0.4473(4) 0.2569(4) 0.0549(4) 0.0213(9) Uani 1 1 d . . . C9 C 0.7502(4) 0.2272(4) 0.0934(4) 0.0220(9) Uani 1 1 d . . . C10 C 0.9371(4) 0.4931(4) 0.2813(4) 0.0210(9) Uani 1 1 d . . . C11 C 0.1530(5) 0.2240(5) 0.2595(4) 0.0413(13) Uani 1 1 d . . . H11A H 0.0852 0.2276 0.2091 0.050 Uiso 1 1 calc R . . C12 C 0.1584(5) 0.1006(5) 0.2532(5) 0.0457(14) Uani 1 1 d . . . H12A H 0.0963 0.0241 0.1991 0.055 Uiso 1 1 calc R . . C13 C 0.2565(4) 0.0922(4) 0.3280(4) 0.0251(10) Uani 1 1 d . . . C14 C 0.3429(5) 0.2094(5) 0.4065(5) 0.0384(12) Uani 1 1 d . . . H14A H 0.4089 0.2096 0.4606 0.046 Uiso 1 1 calc R . . C15 C 0.3307(5) 0.3269(4) 0.4043(4) 0.0370(12) Uani 1 1 d . . . H15A H 0.3918 0.4049 0.4572 0.044 Uiso 1 1 calc R . . C16 C 0.2596(4) -0.0394(4) 0.3266(4) 0.0254(10) Uani 1 1 d . . . C17 C 0.1921(5) -0.1570(4) 0.2344(4) 0.0339(11) Uani 1 1 d . . . H17A H 0.1493 -0.1560 0.1686 0.041 Uiso 1 1 calc R . . C18 C 0.1879(5) -0.2759(4) 0.2396(4) 0.0323(11) Uani 1 1 d . . . H18A H 0.1417 -0.3536 0.1760 0.039 Uiso 1 1 calc R . . C19 C 0.3139(5) -0.1729(5) 0.4194(4) 0.0357(12) Uani 1 1 d . . . H19A H 0.3571 -0.1773 0.4834 0.043 Uiso 1 1 calc R . . C20 C 0.3233(5) -0.0485(4) 0.4215(4) 0.0365(12) Uani 1 1 d . . . H20A H 0.3716 0.0278 0.4855 0.044 Uiso 1 1 calc R . . C21 C 0.1291(6) -0.1166(5) -0.3539(4) 0.0413(13) Uani 1 1 d . . . H21A H 0.1337 -0.1973 -0.3536 0.050 Uiso 1 1 calc R . . C22 C 0.0510(6) -0.1189(5) -0.4472(4) 0.0426(13) Uani 1 1 d . . . H22A H 0.0045 -0.1995 -0.5076 0.051 Uiso 1 1 calc R . . C23 C 0.0420(4) -0.0003(4) -0.4506(4) 0.0269(10) Uani 1 1 d . . . C24 C 0.1140(5) 0.1134(5) -0.3587(4) 0.0413(13) Uani 1 1 d . . . H24A H 0.1119 0.1953 -0.3574 0.050 Uiso 1 1 calc R . . C25 C 0.1898(5) 0.1087(5) -0.2676(4) 0.0442(13) Uani 1 1 d . . . H25A H 0.2368 0.1882 -0.2062 0.053 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0166(3) 0.0167(3) 0.0249(3) 0.0106(3) 0.0039(2) 0.0060(2) Co2 0.0276(3) 0.0196(3) 0.0273(4) 0.0114(3) -0.0059(3) 0.0023(3) O1 0.0225(16) 0.0305(17) 0.0225(17) 0.0084(14) 0.0026(13) 0.0091(13) O2 0.0155(14) 0.0269(16) 0.0286(17) 0.0105(14) 0.0020(12) 0.0067(12) O3 0.049(2) 0.0275(17) 0.036(2) 0.0199(16) 0.0135(16) 0.0132(15) O4 0.0357(19) 0.0237(17) 0.036(2) 0.0114(16) -0.0087(15) -0.0043(14) O5 0.0407(19) 0.0202(16) 0.0325(19) 0.0065(15) -0.0011(15) 0.0074(14) O6 0.0399(19) 0.0256(17) 0.0336(19) 0.0184(15) -0.0078(15) 0.0026(14) O7 0.0152(14) 0.0221(15) 0.0279(17) 0.0094(13) 0.0027(12) 0.0064(12) O8 0.0268(17) 0.049(2) 0.0210(18) 0.0091(16) 0.0032(13) 0.0134(15) O1W 0.0311(17) 0.0325(17) 0.0232(17) 0.0134(14) 0.0049(13) 0.0121(14) O2W 0.057(2) 0.046(2) 0.077(3) 0.033(2) 0.034(2) 0.019(2) O3W 0.0316(18) 0.0321(18) 0.055(2) 0.0235(18) 0.0054(16) 0.0104(15) O4W 0.037(2) 0.054(2) 0.044(2) 0.0054(19) -0.0006(17) 0.0105(18) N1 0.0229(19) 0.0224(19) 0.028(2) 0.0129(17) 0.0014(16) 0.0077(15) N2 0.027(2) 0.0205(19) 0.038(2) 0.0170(18) 0.0087(17) 0.0095(16) N3 0.035(2) 0.028(2) 0.024(2) 0.0130(18) 0.0001(17) 0.0115(17) C1 0.017(2) 0.020(2) 0.024(2) 0.0103(19) 0.0020(17) 0.0047(17) C2 0.017(2) 0.022(2) 0.022(2) 0.0134(19) -0.0025(17) 0.0049(17) C3 0.024(2) 0.021(2) 0.019(2) 0.0094(18) 0.0031(17) 0.0058(18) C4 0.015(2) 0.023(2) 0.025(2) 0.0113(19) 0.0042(17) 0.0059(17) C5 0.018(2) 0.016(2) 0.024(2) 0.0103(18) 0.0026(17) 0.0040(16) C6 0.018(2) 0.024(2) 0.023(2) 0.0065(19) -0.0001(17) 0.0074(18) C7 0.021(2) 0.016(2) 0.028(3) 0.0126(19) 0.0035(18) 0.0063(17) C8 0.017(2) 0.020(2) 0.029(3) 0.011(2) 0.0041(18) 0.0085(17) C9 0.013(2) 0.021(2) 0.029(3) 0.009(2) 0.0017(17) 0.0050(17) C10 0.017(2) 0.016(2) 0.031(3) 0.0120(19) -0.0003(18) 0.0028(17) C11 0.046(3) 0.031(3) 0.047(3) 0.022(3) -0.017(2) 0.008(2) C12 0.054(3) 0.022(3) 0.055(4) 0.016(3) -0.013(3) 0.008(2) C13 0.028(2) 0.017(2) 0.034(3) 0.013(2) 0.0059(19) 0.0080(18) C14 0.037(3) 0.026(3) 0.050(3) 0.020(2) -0.014(2) 0.004(2) C15 0.039(3) 0.021(2) 0.040(3) 0.009(2) -0.013(2) 0.003(2) C16 0.025(2) 0.020(2) 0.037(3) 0.015(2) 0.0099(19) 0.0080(18) C17 0.054(3) 0.025(2) 0.027(3) 0.015(2) 0.005(2) 0.013(2) C18 0.044(3) 0.020(2) 0.032(3) 0.010(2) 0.006(2) 0.009(2) C19 0.032(3) 0.030(3) 0.044(3) 0.019(2) -0.011(2) 0.007(2) C20 0.036(3) 0.021(2) 0.047(3) 0.016(2) -0.013(2) 0.002(2) C21 0.070(4) 0.030(3) 0.029(3) 0.013(2) -0.001(2) 0.025(3) C22 0.071(4) 0.027(3) 0.024(3) 0.004(2) -0.010(2) 0.021(3) C23 0.033(2) 0.030(2) 0.020(2) 0.011(2) 0.0048(19) 0.014(2) C24 0.056(3) 0.024(3) 0.039(3) 0.015(2) -0.016(2) 0.005(2) C25 0.059(3) 0.028(3) 0.036(3) 0.012(2) -0.015(2) 0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1W 2.086(3) . ? Co1 O7 2.093(3) 1_455 ? Co1 O2 2.125(3) . ? Co1 N1 2.131(3) . ? Co1 N2 2.158(3) 1_565 ? Co1 O1 2.173(3) . ? Co1 C7 2.482(4) . ? Co2 O4 1.992(3) . ? Co2 O3W 2.090(3) . ? Co2 N3 2.113(3) . ? Co2 O6 2.126(3) 2_655 ? Co2 O2W 2.199(3) . ? Co2 O5 2.231(3) 2_655 ? Co2 C9 2.512(4) 2_655 ? O1 C7 1.258(5) . ? O2 C7 1.267(5) . ? O3 C8 1.237(5) . ? O4 C8 1.263(5) . ? O5 C9 1.259(5) . ? O5 Co2 2.231(3) 2_655 ? O6 C9 1.248(5) . ? O6 Co2 2.126(3) 2_655 ? O7 C10 1.271(5) . ? O7 Co1 2.093(3) 1_655 ? O8 C10 1.253(5) . ? O1W H1WA 0.8555 . ? O1W H1WB 0.8520 . ? O2W H2WA 0.8474 . ? O2W H2WB 0.8500 . ? O3W H3WA 0.8489 . ? O3W H3WB 0.8502 . ? O4W H4WA 0.8496 . ? O4W H4WB 0.8511 . ? N1 C15 1.318(5) . ? N1 C11 1.319(6) . ? N2 C19 1.331(6) . ? N2 C18 1.338(6) . ? N2 Co1 2.158(3) 1_545 ? N3 C25 1.333(6) . ? N3 C21 1.334(6) . ? C1 C7 1.520(5) . ? C1 C6 1.530(5) . ? C1 C2 1.530(6) . ? C1 H1A 0.9800 . ? C2 C8 1.521(5) . ? C2 C3 1.542(5) . ? C2 H2A 0.9800 . ? C3 C4 1.542(5) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C9 1.525(5) . ? C4 C5 1.529(6) . ? C4 H4A 0.9800 . ? C5 C10 1.526(5) . ? C5 C6 1.534(5) . ? C5 H5A 0.9800 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C9 Co2 2.512(4) 2_655 ? C11 C12 1.387(6) . ? C11 H11A 0.9300 . ? C12 C13 1.379(6) . ? C12 H12A 0.9300 . ? C13 C14 1.371(6) . ? C13 C16 1.497(5) . ? C14 C15 1.380(6) . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? C16 C17 1.378(6) . ? C16 C20 1.392(6) . ? C17 C18 1.373(6) . ? C17 H17A 0.9300 . ? C18 H18A 0.9300 . ? C19 C20 1.389(6) . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? C21 C22 1.378(6) . ? C21 H21A 0.9300 . ? C22 C23 1.389(6) . ? C22 H22A 0.9300 . ? C23 C24 1.366(6) . ? C23 C23 1.482(8) 2_554 ? C24 C25 1.380(6) . ? C24 H24A 0.9300 . ? C25 H25A 0.9300 . ? 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 O1W Co1 O7 97.05(11) . 1_455 ? O1W Co1 O2 166.89(12) . . ? O7 Co1 O2 95.19(11) 1_455 . ? O1W Co1 N1 90.61(12) . . ? O7 Co1 N1 95.77(12) 1_455 . ? O2 Co1 N1 92.81(12) . . ? O1W Co1 N2 88.11(13) . 1_565 ? O7 Co1 N2 88.26(12) 1_455 1_565 ? O2 Co1 N2 87.60(12) . 1_565 ? N1 Co1 N2 175.90(14) . 1_565 ? O1W Co1 O1 106.49(11) . . ? O7 Co1 O1 156.24(11) 1_455 . ? O2 Co1 O1 61.09(11) . . ? N1 Co1 O1 87.24(12) . . ? N2 Co1 O1 89.39(12) 1_565 . ? O1W Co1 C7 136.92(13) . . ? O7 Co1 C7 125.87(13) 1_455 . ? O2 Co1 C7 30.70(12) . . ? N1 Co1 C7 88.64(12) . . ? N2 Co1 C7 89.64(13) 1_565 . ? O1 Co1 C7 30.45(12) . . ? O4 Co2 O3W 85.95(13) . . ? O4 Co2 N3 92.15(13) . . ? O3W Co2 N3 96.99(13) . . ? O4 Co2 O6 174.52(12) . 2_655 ? O3W Co2 O6 90.70(12) . 2_655 ? N3 Co2 O6 92.56(13) . 2_655 ? O4 Co2 O2W 85.41(13) . . ? O3W Co2 O2W 170.27(14) . . ? N3 Co2 O2W 87.78(15) . . ? O6 Co2 O2W 97.57(13) 2_655 . ? O4 Co2 O5 116.17(12) . 2_655 ? O3W Co2 O5 94.65(12) . 2_655 ? N3 Co2 O5 150.06(13) . 2_655 ? O6 Co2 O5 59.74(11) 2_655 2_655 ? O2W Co2 O5 85.19(13) . 2_655 ? O4 Co2 C9 145.90(14) . 2_655 ? O3W Co2 C9 91.91(12) . 2_655 ? N3 Co2 C9 121.84(14) . 2_655 ? O6 Co2 C9 29.75(12) 2_655 2_655 ? O2W Co2 C9 92.76(13) . 2_655 ? O5 Co2 C9 30.03(12) 2_655 2_655 ? C7 O1 Co1 88.5(2) . . ? C7 O2 Co1 90.4(2) . . ? C8 O4 Co2 132.4(3) . . ? C9 O5 Co2 87.4(2) . 2_655 ? C9 O6 Co2 92.5(3) . 2_655 ? C10 O7 Co1 123.5(3) . 1_655 ? Co1 O1W H1WA 89.6 . . ? Co1 O1W H1WB 123.8 . . ? H1WA O1W H1WB 108.3 . . ? Co2 O2W H2WA 120.0 . . ? Co2 O2W H2WB 107.1 . . ? H2WA O2W H2WB 107.3 . . ? Co2 O3W H3WA 112.7 . . ? Co2 O3W H3WB 102.7 . . ? H3WA O3W H3WB 109.6 . . ? H4WA O4W H4WB 109.2 . . ? C15 N1 C11 115.9(4) . . ? C15 N1 Co1 122.1(3) . . ? C11 N1 Co1 121.9(3) . . ? C19 N2 C18 116.4(4) . . ? C19 N2 Co1 123.4(3) . 1_545 ? C18 N2 Co1 120.2(3) . 1_545 ? C25 N3 C21 116.7(4) . . ? C25 N3 Co2 123.3(3) . . ? C21 N3 Co2 119.5(3) . . ? C7 C1 C6 112.2(3) . . ? C7 C1 C2 111.2(3) . . ? C6 C1 C2 113.6(3) . . ? C7 C1 H1A 106.4 . . ? C6 C1 H1A 106.4 . . ? C2 C1 H1A 106.4 . . ? C8 C2 C1 114.9(3) . . ? C8 C2 C3 111.1(3) . . ? C1 C2 C3 111.5(3) . . ? C8 C2 H2A 106.2 . . ? C1 C2 H2A 106.2 . . ? C3 C2 H2A 106.2 . . ? C4 C3 C2 113.9(3) . . ? C4 C3 H3A 108.8 . . ? C2 C3 H3A 108.8 . . ? C4 C3 H3B 108.8 . . ? C2 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? C9 C4 C5 113.8(3) . . ? C9 C4 C3 113.3(3) . . ? C5 C4 C3 109.5(3) . . ? C9 C4 H4A 106.6 . . ? C5 C4 H4A 106.6 . . ? C3 C4 H4A 106.6 . . ? C10 C5 C4 115.1(3) . . ? C10 C5 C6 112.9(3) . . ? C4 C5 C6 111.6(3) . . ? C10 C5 H5A 105.4 . . ? C4 C5 H5A 105.4 . . ? C6 C5 H5A 105.4 . . ? C1 C6 C5 111.0(3) . . ? C1 C6 H6A 109.4 . . ? C5 C6 H6A 109.4 . . ? C1 C6 H6B 109.4 . . ? C5 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? O1 C7 O2 119.8(4) . . ? O1 C7 C1 121.1(4) . . ? O2 C7 C1 119.1(4) . . ? O1 C7 Co1 61.1(2) . . ? O2 C7 Co1 58.9(2) . . ? C1 C7 Co1 176.8(3) . . ? O3 C8 O4 125.8(4) . . ? O3 C8 C2 120.2(4) . . ? O4 C8 C2 113.9(4) . . ? O6 C9 O5 120.1(4) . . ? O6 C9 C4 119.6(4) . . ? O5 C9 C4 120.2(4) . . ? O6 C9 Co2 57.7(2) . 2_655 ? O5 C9 Co2 62.5(2) . 2_655 ? C4 C9 Co2 176.8(3) . 2_655 ? O8 C10 O7 124.1(4) . . ? O8 C10 C5 117.6(4) . . ? O7 C10 C5 118.0(4) . . ? N1 C11 C12 123.9(4) . . ? N1 C11 H11A 118.1 . . ? C12 C11 H11A 118.1 . . ? C13 C12 C11 119.4(5) . . ? C13 C12 H12A 120.3 . . ? C11 C12 H12A 120.3 . . ? C14 C13 C12 116.9(4) . . ? C14 C13 C16 122.8(4) . . ? C12 C13 C16 120.2(4) . . ? C13 C14 C15 119.2(4) . . ? C13 C14 H14A 120.4 . . ? C15 C14 H14A 120.4 . . ? N1 C15 C14 124.7(4) . . ? N1 C15 H15A 117.7 . . ? C14 C15 H15A 117.7 . . ? C17 C16 C20 116.9(4) . . ? C17 C16 C13 121.6(4) . . ? C20 C16 C13 121.4(4) . . ? C18 C17 C16 120.1(4) . . ? C18 C17 H17A 119.9 . . ? C16 C17 H17A 119.9 . . ? N2 C18 C17 123.7(4) . . ? N2 C18 H18A 118.2 . . ? C17 C18 H18A 118.2 . . ? N2 C19 C20 123.7(4) . . ? N2 C19 H19A 118.2 . . ? C20 C19 H19A 118.2 . . ? C19 C20 C16 119.2(4) . . ? C19 C20 H20A 120.4 . . ? C16 C20 H20A 120.4 . . ? N3 C21 C22 123.5(4) . . ? N3 C21 H21A 118.2 . . ? C22 C21 H21A 118.2 . . ? C21 C22 C23 119.8(5) . . ? C21 C22 H22A 120.1 . . ? C23 C22 H22A 120.1 . . ? C24 C23 C22 116.3(4) . . ? C24 C23 C23 122.8(5) . 2_554 ? C22 C23 C23 120.9(5) . 2_554 ? C23 C24 C25 121.1(4) . . ? C23 C24 H24A 119.5 . . ? C25 C24 H24A 119.5 . . ? N3 C25 C24 122.7(5) . . ? N3 C25 H25A 118.6 . . ? C24 C25 H25A 118.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1W Co1 O1 C7 -178.2(2) . . . . ? O7 Co1 O1 C7 -6.1(4) 1_455 . . . ? O2 Co1 O1 C7 -2.7(2) . . . . ? N1 Co1 O1 C7 92.0(2) . . . . ? N2 Co1 O1 C7 -90.3(2) 1_565 . . . ? O1W Co1 O2 C7 22.4(6) . . . . ? O7 Co1 O2 C7 -178.6(2) 1_455 . . . ? N1 Co1 O2 C7 -82.6(2) . . . . ? N2 Co1 O2 C7 93.4(2) 1_565 . . . ? O1 Co1 O2 C7 2.7(2) . . . . ? O3W Co2 O4 C8 -96.1(4) . . . . ? N3 Co2 O4 C8 167.0(4) . . . . ? O6 Co2 O4 C8 -43.7(16) 2_655 . . . ? O2W Co2 O4 C8 79.4(4) . . . . ? O5 Co2 O4 C8 -2.9(4) 2_655 . . . ? C9 Co2 O4 C8 -8.7(5) 2_655 . . . ? O1W Co1 N1 C15 -66.5(4) . . . . ? O7 Co1 N1 C15 -163.6(4) 1_455 . . . ? O2 Co1 N1 C15 100.9(4) . . . . ? N2 Co1 N1 C15 5(2) 1_565 . . . ? O1 Co1 N1 C15 40.0(4) . . . . ? C7 Co1 N1 C15 70.4(4) . . . . ? O1W Co1 N1 C11 117.7(4) . . . . ? O7 Co1 N1 C11 20.5(4) 1_455 . . . ? O2 Co1 N1 C11 -75.0(4) . . . . ? N2 Co1 N1 C11 -170.6(17) 1_565 . . . ? O1 Co1 N1 C11 -135.8(4) . . . . ? C7 Co1 N1 C11 -105.4(4) . . . . ? O4 Co2 N3 C25 -15.4(4) . . . . ? O3W Co2 N3 C25 -101.5(4) . . . . ? O6 Co2 N3 C25 167.4(4) 2_655 . . . ? O2W Co2 N3 C25 70.0(4) . . . . ? O5 Co2 N3 C25 146.3(4) 2_655 . . . ? C9 Co2 N3 C25 161.8(4) 2_655 . . . ? O4 Co2 N3 C21 172.8(4) . . . . ? O3W Co2 N3 C21 86.6(4) . . . . ? O6 Co2 N3 C21 -4.4(4) 2_655 . . . ? O2W Co2 N3 C21 -101.9(4) . . . . ? O5 Co2 N3 C21 -25.5(5) 2_655 . . . ? C9 Co2 N3 C21 -10.0(4) 2_655 . . . ? C7 C1 C2 C8 -49.2(4) . . . . ? C6 C1 C2 C8 78.5(4) . . . . ? C7 C1 C2 C3 -176.7(3) . . . . ? C6 C1 C2 C3 -49.1(4) . . . . ? C8 C2 C3 C4 -79.6(4) . . . . ? C1 C2 C3 C4 50.0(4) . . . . ? C2 C3 C4 C9 74.1(4) . . . . ? C2 C3 C4 C5 -54.1(4) . . . . ? C9 C4 C5 C10 59.8(4) . . . . ? C3 C4 C5 C10 -172.3(3) . . . . ? C9 C4 C5 C6 -70.6(4) . . . . ? C3 C4 C5 C6 57.3(4) . . . . ? C7 C1 C6 C5 -179.8(3) . . . . ? C2 C1 C6 C5 53.1(4) . . . . ? C10 C5 C6 C1 171.1(3) . . . . ? C4 C5 C6 C1 -57.4(4) . . . . ? Co1 O1 C7 O2 4.6(4) . . . . ? Co1 O1 C7 C1 -177.3(3) . . . . ? Co1 O2 C7 O1 -4.8(4) . . . . ? Co1 O2 C7 C1 177.2(3) . . . . ? C6 C1 C7 O1 26.5(5) . . . . ? C2 C1 C7 O1 154.9(3) . . . . ? C6 C1 C7 O2 -155.5(4) . . . . ? C2 C1 C7 O2 -27.1(5) . . . . ? C6 C1 C7 Co1 -106(5) . . . . ? C2 C1 C7 Co1 22(5) . . . . ? O1W Co1 C7 O1 2.5(3) . . . . ? O7 Co1 C7 O1 176.99(19) 1_455 . . . ? O2 Co1 C7 O1 175.3(4) . . . . ? N1 Co1 C7 O1 -86.9(2) . . . . ? N2 Co1 C7 O1 89.4(2) 1_565 . . . ? O1W Co1 C7 O2 -172.7(2) . . . . ? O7 Co1 C7 O2 1.7(3) 1_455 . . . ? N1 Co1 C7 O2 97.8(2) . . . . ? N2 Co1 C7 O2 -85.9(2) 1_565 . . . ? O1 Co1 C7 O2 -175.3(4) . . . . ? O1W Co1 C7 C1 137(5) . . . . ? O7 Co1 C7 C1 -49(5) 1_455 . . . ? O2 Co1 C7 C1 -51(5) . . . . ? N1 Co1 C7 C1 47(5) . . . . ? N2 Co1 C7 C1 -137(5) 1_565 . . . ? O1 Co1 C7 C1 134(5) . . . . ? Co2 O4 C8 O3 -13.9(6) . . . . ? Co2 O4 C8 C2 165.4(3) . . . . ? C1 C2 C8 O3 -19.9(5) . . . . ? C3 C2 C8 O3 107.8(4) . . . . ? C1 C2 C8 O4 160.7(3) . . . . ? C3 C2 C8 O4 -71.6(4) . . . . ? Co2 O6 C9 O5 -4.2(4) 2_655 . . . ? Co2 O6 C9 C4 178.0(3) 2_655 . . . ? Co2 O5 C9 O6 4.0(4) 2_655 . . . ? Co2 O5 C9 C4 -178.2(3) 2_655 . . . ? C5 C4 C9 O6 -16.6(5) . . . . ? C3 C4 C9 O6 -142.6(4) . . . . ? C5 C4 C9 O5 165.5(3) . . . . ? C3 C4 C9 O5 39.6(5) . . . . ? C5 C4 C9 Co2 16(5) . . . 2_655 ? C3 C4 C9 Co2 -110(5) . . . 2_655 ? Co1 O7 C10 O8 -14.5(5) 1_655 . . . ? Co1 O7 C10 C5 160.0(3) 1_655 . . . ? C4 C5 C10 O8 -149.1(4) . . . . ? C6 C5 C10 O8 -19.3(5) . . . . ? C4 C5 C10 O7 36.1(5) . . . . ? C6 C5 C10 O7 165.9(3) . . . . ? C15 N1 C11 C12 -1.8(8) . . . . ? Co1 N1 C11 C12 174.3(4) . . . . ? N1 C11 C12 C13 1.0(8) . . . . ? C11 C12 C13 C14 1.1(8) . . . . ? C11 C12 C13 C16 176.9(5) . . . . ? C12 C13 C14 C15 -2.2(7) . . . . ? C16 C13 C14 C15 -177.9(4) . . . . ? C11 N1 C15 C14 0.5(7) . . . . ? Co1 N1 C15 C14 -175.6(4) . . . . ? C13 C14 C15 N1 1.6(8) . . . . ? C14 C13 C16 C17 -166.7(5) . . . . ? C12 C13 C16 C17 17.7(7) . . . . ? C14 C13 C16 C20 17.6(7) . . . . ? C12 C13 C16 C20 -158.0(5) . . . . ? C20 C16 C17 C18 1.1(7) . . . . ? C13 C16 C17 C18 -174.8(4) . . . . ? C19 N2 C18 C17 -1.2(7) . . . . ? Co1 N2 C18 C17 -178.9(4) 1_545 . . . ? C16 C17 C18 N2 0.1(7) . . . . ? C18 N2 C19 C20 1.2(7) . . . . ? Co1 N2 C19 C20 178.8(4) 1_545 . . . ? N2 C19 C20 C16 0.0(8) . . . . ? C17 C16 C20 C19 -1.1(7) . . . . ? C13 C16 C20 C19 174.8(4) . . . . ? C25 N3 C21 C22 -0.2(8) . . . . ? Co2 N3 C21 C22 172.2(4) . . . . ? N3 C21 C22 C23 0.1(8) . . . . ? C21 C22 C23 C24 0.3(7) . . . . ? C21 C22 C23 C23 -179.6(5) . . . 2_554 ? C22 C23 C24 C25 -0.7(8) . . . . ? C23 C23 C24 C25 179.3(5) 2_554 . . . ? C21 N3 C25 C24 -0.1(8) . . . . ? Co2 N3 C25 C24 -172.2(4) . . . . ? C23 C24 C25 N3 0.6(9) . . . . ? 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 O1W H1WA O8 0.86 1.77 2.622(4) 173.7 1_455 O1W H1WA O7 0.86 2.64 3.131(4) 117.8 1_455 O1W H1WB O8 0.85 2.16 2.866(4) 140.6 2_666 O2W H2WA O4W 0.85 1.96 2.777(5) 161.3 . O2W H2WB O5 0.85 2.78 2.998(5) 96.8 2_655 O3W H3WA O3 0.85 1.81 2.652(4) 170.7 2_655 O3W H3WB O5 0.85 2.04 2.808(5) 150.6 . O4W H4WA O2 0.85 2.03 2.773(4) 145.6 . O4W H4WB O7 0.85 2.18 2.959(5) 152.2 1_455 _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.656 _refine_diff_density_min -0.487 _refine_diff_density_rms 0.099 #=================================================END data_compound2 _database_code_depnum_ccdc_archive 'CCDC 768142' #TrackingRef 'cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H54 Co4 N6 O23' _chemical_formula_weight 1342.71 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.741(13) _cell_length_b 11.376(5) _cell_length_c 19.605(9) _cell_angle_alpha 90.00 _cell_angle_beta 114.165(9) _cell_angle_gamma 90.00 _cell_volume 5238(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.703 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2752 _exptl_absorpt_coefficient_mu 1.338 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8246 _exptl_absorpt_correction_T_max 0.9005 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11231 _diffrn_reflns_av_R_equivalents 0.0992 _diffrn_reflns_av_sigmaI/netI 0.1975 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5019 _reflns_number_gt 2139 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 1998)' _computing_cell_refinement 'Bruker SMART (Bruker, 1998)' _computing_data_reduction 'Bruker SAINT + & SHELXTL (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0123P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5019 _refine_ls_number_parameters 379 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1566 _refine_ls_R_factor_gt 0.0575 _refine_ls_wR_factor_ref 0.1113 _refine_ls_wR_factor_gt 0.0829 _refine_ls_goodness_of_fit_ref 0.821 _refine_ls_restrained_S_all 0.829 _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 0.55464(4) 0.55482(8) 0.70327(5) 0.0238(3) Uani 1 1 d . . . Co2 Co 0.72473(4) 0.15721(9) 1.09865(6) 0.0331(3) Uani 1 1 d . . . N1 N 0.5539(3) 0.7455(5) 0.7027(3) 0.0287(15) Uani 1 1 d . . . N2 N 0.5530(2) 1.3688(5) 0.7094(3) 0.0263(15) Uani 1 1 d . . . N3 N 0.6435(3) 0.0964(6) 1.0869(4) 0.0395(18) Uani 1 1 d . . . O1 O 0.60422(19) 0.5675(4) 0.8140(2) 0.0311(13) Uani 1 1 d . . . O2 O 0.53033(19) 0.5530(4) 0.8445(3) 0.0354(13) Uani 1 1 d . . . O3 O 0.7511(2) 0.5163(4) 0.9143(3) 0.0445(15) Uani 1 1 d . . . O4 O 0.6910(2) 0.3925(4) 0.9279(3) 0.0464(16) Uani 1 1 d . . . O5 O 0.7024(2) 0.3331(4) 1.1035(3) 0.0384(13) Uani 1 1 d . . . O6 O 0.7829(2) 0.4161(4) 1.1128(3) 0.0473(16) Uani 1 1 d . . . O7 O 0.5740(2) 0.4521(4) 1.1118(3) 0.0347(13) Uani 1 1 d . . . O8 O 0.6569(2) 0.4917(4) 1.2017(3) 0.0402(15) Uani 1 1 d . . . O1W O 0.7674(2) 0.1565(4) 1.2120(2) 0.0493(15) Uani 1 1 d . . . H1WB H 0.7784 0.0884 1.2298 0.059 Uiso 1 1 d RD . . H1WA H 0.7489 0.1893 1.2342 0.059 Uiso 1 1 d RD . . O2W O 0.68356(19) 0.1821(4) 0.9839(2) 0.0426(15) Uani 1 1 d . . . H2WA H 0.6830 0.2558 0.9765 0.051 Uiso 1 1 d RD . . H2WB H 0.6994 0.1447 0.9600 0.051 Uiso 1 1 d RD . . O3W O 0.7373(2) 0.3259(5) 1.2902(3) 0.0678(18) Uani 1 1 d . . . H3WA H 0.7277 0.3767 1.2554 0.081 Uiso 1 1 d RD . . H3WB H 0.7609 0.3415 1.3345 0.081 Uiso 1 1 d RD . . O4W O 0.6361(6) -0.0827(12) 0.9241(8) 0.124(6) Uani 0.50 1 d P . . H4WA H 0.6574 -0.0367 0.9130 0.149 Uiso 0.50 1 d PRD . . H4WB H 0.6434 -0.0766 0.9703 0.149 Uiso 0.50 1 d PRD . . C1 C 0.6213(3) 0.5885(6) 0.9427(4) 0.0238(18) Uani 1 1 d . . . H1 H 0.6112 0.6677 0.9528 0.029 Uiso 1 1 calc R . . C2 C 0.6843(3) 0.5963(6) 0.9587(4) 0.0266(18) Uani 1 1 d . . . H2 H 0.6883 0.6662 0.9320 0.032 Uiso 1 1 calc R . . C3 C 0.7192(3) 0.6217(6) 1.0420(4) 0.032(2) Uani 1 1 d . . . H3A H 0.7128 0.7028 1.0516 0.038 Uiso 1 1 calc R . . H3B H 0.7593 0.6138 1.0523 0.038 Uiso 1 1 calc R . . C4 C 0.7066(3) 0.5434(6) 1.0974(4) 0.0274(18) Uani 1 1 d . . . H4 H 0.7251 0.5805 1.1467 0.033 Uiso 1 1 calc R . . C5 C 0.6422(3) 0.5454(6) 1.0766(4) 0.0265(17) Uani 1 1 d . . . H5 H 0.6333 0.6289 1.0775 0.032 Uiso 1 1 calc R . . C6 C 0.6079(3) 0.5089(6) 0.9960(3) 0.0310(19) Uani 1 1 d . . . H6A H 0.5676 0.5133 0.9848 0.037 Uiso 1 1 calc R . . H6B H 0.6169 0.4281 0.9891 0.037 Uiso 1 1 calc R . . C7 C 0.5827(3) 0.5663(6) 0.8605(4) 0.0234(17) Uani 1 1 d . . . C8 C 0.7091(3) 0.4958(7) 0.9313(4) 0.0313(19) Uani 1 1 d . . . C9 C 0.7320(3) 0.4216(6) 1.1043(4) 0.0286(19) Uani 1 1 d . . . C10 C 0.6245(3) 0.4899(6) 1.1342(5) 0.032(2) Uani 1 1 d . . . C11 C 0.5063(3) 0.8066(7) 0.6690(4) 0.037(2) Uani 1 1 d . . . H11 H 0.4724 0.7664 0.6434 0.044 Uiso 1 1 calc R . . C12 C 0.5055(3) 0.9276(7) 0.6705(4) 0.035(2) Uani 1 1 d . . . H12 H 0.4713 0.9674 0.6463 0.042 Uiso 1 1 calc R . . C13 C 0.5545(3) 0.9898(6) 0.7072(4) 0.0248(17) Uani 1 1 d . . . C14 C 0.6043(3) 0.9271(6) 0.7418(4) 0.037(2) Uani 1 1 d . . . H14 H 0.6388 0.9656 0.7671 0.045 Uiso 1 1 calc R . . C15 C 0.6019(3) 0.8042(6) 0.7381(4) 0.036(2) Uani 1 1 d . . . H15 H 0.6355 0.7619 0.7615 0.043 Uiso 1 1 calc R . . C16 C 0.5541(3) 1.1216(6) 0.7087(4) 0.0257(18) Uani 1 1 d . . . C17 C 0.5087(3) 1.1848(6) 0.6598(4) 0.037(2) Uani 1 1 d . . . H17 H 0.4770 1.1457 0.6257 0.044 Uiso 1 1 calc R . . C18 C 0.5100(3) 1.3065(6) 0.6610(4) 0.037(2) Uani 1 1 d . . . H18 H 0.4792 1.3468 0.6261 0.044 Uiso 1 1 calc R . . C19 C 0.5964(3) 1.3079(6) 0.7582(4) 0.032(2) Uani 1 1 d . . . H19 H 0.6267 1.3487 0.7936 0.038 Uiso 1 1 calc R . . C20 C 0.5983(3) 1.1852(6) 0.7583(4) 0.034(2) Uani 1 1 d . . . H20 H 0.6301 1.1465 0.7926 0.041 Uiso 1 1 calc R . . C21 C 0.5999(3) 0.1715(7) 1.0630(4) 0.043(2) Uani 1 1 d . . . H21 H 0.6081 0.2515 1.0689 0.052 Uiso 1 1 calc R . . C22 C 0.5439(3) 0.1386(7) 1.0302(4) 0.044(2) Uani 1 1 d . . . H22 H 0.5153 0.1952 1.0161 0.053 Uiso 1 1 calc R . . C23 C 0.5300(3) 0.0201(7) 1.0181(4) 0.035(2) Uani 1 1 d . . . C24 C 0.5748(3) -0.0591(7) 1.0445(4) 0.048(2) Uani 1 1 d . . . H24 H 0.5679 -0.1396 1.0399 0.058 Uiso 1 1 calc R . . C25 C 0.6297(3) -0.0171(7) 1.0778(5) 0.056(3) Uani 1 1 d . . . H25 H 0.6591 -0.0717 1.0950 0.068 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0290(5) 0.0221(6) 0.0220(6) -0.0013(5) 0.0119(5) -0.0003(5) Co2 0.0320(6) 0.0331(7) 0.0346(7) 0.0021(6) 0.0141(5) -0.0010(6) N1 0.045(4) 0.019(4) 0.026(4) 0.002(3) 0.019(4) 0.002(3) N2 0.026(3) 0.028(4) 0.023(4) 0.002(3) 0.009(3) 0.002(3) N3 0.035(4) 0.046(5) 0.041(5) 0.007(4) 0.019(4) 0.005(4) O1 0.037(3) 0.038(3) 0.020(3) 0.002(3) 0.014(3) -0.001(3) O2 0.026(3) 0.028(3) 0.045(3) 0.001(3) 0.007(3) 0.002(3) O3 0.043(3) 0.053(4) 0.048(4) -0.002(3) 0.030(3) 0.007(3) O4 0.065(4) 0.026(3) 0.042(4) -0.004(3) 0.016(3) 0.002(3) O5 0.052(4) 0.025(3) 0.038(3) 0.001(3) 0.018(3) 0.000(3) O6 0.036(3) 0.060(4) 0.044(4) -0.006(3) 0.014(3) 0.009(3) O7 0.045(3) 0.032(3) 0.038(3) -0.003(3) 0.029(3) -0.009(3) O8 0.060(4) 0.036(4) 0.030(3) 0.001(3) 0.023(3) -0.001(3) O1W 0.059(4) 0.047(4) 0.042(3) 0.008(3) 0.020(3) 0.019(3) O2W 0.053(4) 0.039(4) 0.046(4) 0.005(3) 0.030(3) 0.007(3) O3W 0.084(5) 0.068(5) 0.037(4) 0.002(3) 0.010(4) 0.018(4) O4W 0.106(13) 0.165(16) 0.123(13) -0.035(12) 0.068(12) -0.044(11) C1 0.026(4) 0.025(5) 0.024(5) 0.002(4) 0.014(4) -0.001(3) C2 0.037(5) 0.011(4) 0.032(5) 0.002(4) 0.016(4) 0.004(3) C3 0.033(4) 0.035(5) 0.031(5) -0.010(4) 0.017(4) -0.010(4) C4 0.037(4) 0.028(5) 0.018(4) -0.003(4) 0.013(4) -0.004(4) C5 0.029(4) 0.027(4) 0.026(5) 0.000(4) 0.015(4) 0.000(4) C6 0.032(4) 0.042(5) 0.021(4) 0.004(4) 0.013(4) -0.006(4) C7 0.029(4) 0.010(4) 0.031(5) 0.006(4) 0.012(4) 0.005(3) C8 0.034(5) 0.040(5) 0.013(4) -0.003(4) 0.002(4) 0.007(4) C9 0.033(5) 0.031(5) 0.014(4) -0.002(4) 0.001(4) 0.002(4) C10 0.048(5) 0.021(5) 0.037(5) 0.003(4) 0.027(5) 0.007(4) C11 0.030(5) 0.042(6) 0.034(5) -0.001(4) 0.009(4) -0.001(4) C12 0.038(5) 0.034(5) 0.031(5) -0.002(5) 0.013(4) 0.001(4) C13 0.035(4) 0.014(4) 0.027(5) 0.008(4) 0.014(4) 0.005(4) C14 0.038(5) 0.024(5) 0.049(6) -0.008(4) 0.016(5) -0.013(4) C15 0.031(5) 0.026(5) 0.050(6) 0.004(4) 0.015(4) 0.001(4) C16 0.030(4) 0.025(5) 0.023(5) 0.000(4) 0.012(4) -0.001(4) C17 0.041(5) 0.027(5) 0.033(5) -0.008(4) 0.007(4) -0.011(4) C18 0.039(5) 0.022(5) 0.042(6) 0.001(4) 0.009(5) 0.002(4) C19 0.033(5) 0.022(5) 0.040(5) -0.003(4) 0.016(4) -0.004(4) C20 0.033(5) 0.030(5) 0.038(5) 0.003(4) 0.013(4) 0.006(4) C21 0.057(6) 0.036(6) 0.047(6) 0.005(5) 0.030(5) -0.007(5) C22 0.040(5) 0.054(6) 0.047(6) -0.006(5) 0.025(5) -0.006(5) C23 0.034(5) 0.044(6) 0.033(5) 0.005(4) 0.018(5) -0.007(4) C24 0.036(5) 0.032(5) 0.074(7) 0.002(5) 0.021(5) -0.007(4) C25 0.042(5) 0.039(6) 0.093(8) 0.003(6) 0.033(6) -0.003(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O2 1.996(5) 2_656 ? Co1 O1 2.023(5) . ? Co1 O7 2.048(4) 6_565 ? Co1 N2 2.121(6) 1_545 ? Co1 N1 2.170(6) . ? Co2 O1W 2.037(5) . ? Co2 O2W 2.077(5) . ? Co2 O5 2.095(5) . ? Co2 O3 2.116(5) 7_657 ? Co2 N3 2.122(6) . ? N1 C15 1.322(8) . ? N1 C11 1.325(8) . ? N2 C19 1.329(8) . ? N2 C18 1.329(8) . ? N2 Co1 2.121(6) 1_565 ? N3 C25 1.332(9) . ? N3 C21 1.334(9) . ? O1 C7 1.245(6) . ? O2 C7 1.263(7) . ? O2 Co1 1.996(5) 2_656 ? O3 C8 1.275(7) . ? O3 Co2 2.116(5) 7_657 ? O4 C8 1.256(8) . ? O5 C9 1.259(8) . ? O6 C9 1.252(8) . ? O7 C10 1.267(8) . ? O7 Co1 2.048(4) 6_566 ? O8 C10 1.243(8) . ? O1W H1WB 0.8500 . ? O1W H1WA 0.8500 . ? O2W H2WA 0.8500 . ? O2W H2WB 0.8498 . ? O3W H3WA 0.8500 . ? O3W H3WB 0.8501 . ? O4W H4WA 0.8501 . ? O4W H4WB 0.8500 . ? C1 C2 1.524(8) . ? C1 C6 1.526(7) . ? C1 C7 1.528(9) . ? C1 H1 0.9800 . ? C2 C8 1.510(8) . ? C2 C3 1.535(9) . ? C2 H2 0.9800 . ? C3 C4 1.538(8) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C9 1.513(9) . ? C4 C5 1.538(8) . ? C4 H4 0.9800 . ? C5 C10 1.517(8) . ? C5 C6 1.518(8) . ? C5 H5 0.9800 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C11 C12 1.377(9) . ? C11 H11 0.9300 . ? C12 C13 1.365(9) . ? C12 H12 0.9300 . ? C13 C14 1.379(9) . ? C13 C16 1.501(8) . ? C14 C15 1.401(9) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C20 1.364(9) . ? C16 C17 1.372(9) . ? C17 C18 1.385(8) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.396(8) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.370(10) . ? C21 H21 0.9300 . ? C22 C23 1.390(10) . ? C22 H22 0.9300 . ? C23 C24 1.385(10) . ? C23 C23 1.485(13) 5_657 ? C24 C25 1.375(10) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Co1 O1 126.36(18) 2_656 . ? O2 Co1 O7 101.60(19) 2_656 6_565 ? O1 Co1 O7 131.99(19) . 6_565 ? O2 Co1 N2 88.5(2) 2_656 1_545 ? O1 Co1 N2 91.6(2) . 1_545 ? O7 Co1 N2 91.68(19) 6_565 1_545 ? O2 Co1 N1 90.1(2) 2_656 . ? O1 Co1 N1 86.2(2) . . ? O7 Co1 N1 92.2(2) 6_565 . ? N2 Co1 N1 176.1(2) 1_545 . ? O1W Co2 O2W 172.3(2) . . ? O1W Co2 O5 89.38(19) . . ? O2W Co2 O5 83.76(18) . . ? O1W Co2 O3 94.2(2) . 7_657 ? O2W Co2 O3 92.40(19) . 7_657 ? O5 Co2 O3 174.98(18) . 7_657 ? O1W Co2 N3 100.6(2) . . ? O2W Co2 N3 83.3(2) . . ? O5 Co2 N3 92.3(2) . . ? O3 Co2 N3 90.5(2) 7_657 . ? C15 N1 C11 118.1(6) . . ? C15 N1 Co1 119.8(5) . . ? C11 N1 Co1 122.1(5) . . ? C19 N2 C18 116.4(6) . . ? C19 N2 Co1 122.0(5) . 1_565 ? C18 N2 Co1 121.4(5) . 1_565 ? C25 N3 C21 115.6(7) . . ? C25 N3 Co2 121.9(5) . . ? C21 N3 Co2 118.6(5) . . ? C7 O1 Co1 120.7(4) . . ? C7 O2 Co1 165.8(5) . 2_656 ? C8 O3 Co2 100.6(5) . 7_657 ? C9 O5 Co2 126.1(5) . . ? C10 O7 Co1 107.1(5) . 6_566 ? Co2 O1W H1WB 113.0 . . ? Co2 O1W H1WA 113.1 . . ? H1WB O1W H1WA 110.7 . . ? Co2 O2W H2WA 106.5 . . ? Co2 O2W H2WB 112.4 . . ? H2WA O2W H2WB 112.3 . . ? H3WA O3W H3WB 122.0 . . ? H4WA O4W H4WB 109.8 . . ? C2 C1 C6 114.4(6) . . ? C2 C1 C7 113.8(5) . . ? C6 C1 C7 113.1(5) . . ? C2 C1 H1 104.7 . . ? C6 C1 H1 104.7 . . ? C7 C1 H1 104.7 . . ? C8 C2 C1 116.9(6) . . ? C8 C2 C3 111.8(6) . . ? C1 C2 C3 109.8(5) . . ? C8 C2 H2 105.8 . . ? C1 C2 H2 105.8 . . ? C3 C2 H2 105.8 . . ? C2 C3 C4 116.3(6) . . ? C2 C3 H3A 108.2 . . ? C4 C3 H3A 108.2 . . ? C2 C3 H3B 108.2 . . ? C4 C3 H3B 108.2 . . ? H3A C3 H3B 107.4 . . ? C9 C4 C5 114.6(6) . . ? C9 C4 C3 112.7(5) . . ? C5 C4 C3 108.6(6) . . ? C9 C4 H4 106.8 . . ? C5 C4 H4 106.8 . . ? C3 C4 H4 106.8 . . ? C10 C5 C6 115.9(6) . . ? C10 C5 C4 114.5(6) . . ? C6 C5 C4 112.1(5) . . ? C10 C5 H5 104.2 . . ? C6 C5 H5 104.2 . . ? C4 C5 H5 104.2 . . ? C5 C6 C1 110.6(6) . . ? C5 C6 H6A 109.5 . . ? C1 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? O1 C7 O2 124.6(7) . . ? O1 C7 C1 118.6(6) . . ? O2 C7 C1 116.7(6) . . ? O4 C8 O3 119.5(7) . . ? O4 C8 C2 121.7(7) . . ? O3 C8 C2 118.8(7) . . ? O6 C9 O5 123.8(7) . . ? O6 C9 C4 116.5(6) . . ? O5 C9 C4 119.6(6) . . ? O8 C10 O7 121.3(7) . . ? O8 C10 C5 120.8(7) . . ? O7 C10 C5 117.5(7) . . ? N1 C11 C12 122.1(7) . . ? N1 C11 H11 118.9 . . ? C12 C11 H11 118.9 . . ? C13 C12 C11 120.7(7) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C12 C13 C14 117.6(7) . . ? C12 C13 C16 121.0(7) . . ? C14 C13 C16 121.3(7) . . ? C13 C14 C15 118.5(7) . . ? C13 C14 H14 120.7 . . ? C15 C14 H14 120.7 . . ? N1 C15 C14 122.9(7) . . ? N1 C15 H15 118.5 . . ? C14 C15 H15 118.5 . . ? C20 C16 C17 116.4(7) . . ? C20 C16 C13 122.3(7) . . ? C17 C16 C13 121.4(7) . . ? C16 C17 C18 120.3(7) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? N2 C18 C17 123.5(7) . . ? N2 C18 H18 118.2 . . ? C17 C18 H18 118.2 . . ? N2 C19 C20 122.8(7) . . ? N2 C19 H19 118.6 . . ? C20 C19 H19 118.6 . . ? C16 C20 C19 120.7(7) . . ? C16 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? N3 C21 C22 124.3(8) . . ? N3 C21 H21 117.8 . . ? C22 C21 H21 117.8 . . ? C21 C22 C23 119.5(8) . . ? C21 C22 H22 120.3 . . ? C23 C22 H22 120.3 . . ? C24 C23 C22 116.8(7) . . ? C24 C23 C23 121.5(9) . 5_657 ? C22 C23 C23 121.6(9) . 5_657 ? C25 C24 C23 119.1(8) . . ? C25 C24 H24 120.4 . . ? C23 C24 H24 120.4 . . ? N3 C25 C24 124.6(8) . . ? N3 C25 H25 117.7 . . ? C24 C25 H25 117.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Co1 N1 C15 171.7(5) 2_656 . . . ? O1 Co1 N1 C15 45.2(5) . . . . ? O7 Co1 N1 C15 -86.7(5) 6_565 . . . ? N2 Co1 N1 C15 103(4) 1_545 . . . ? O2 Co1 N1 C11 -7.0(6) 2_656 . . . ? O1 Co1 N1 C11 -133.4(6) . . . . ? O7 Co1 N1 C11 94.6(5) 6_565 . . . ? N2 Co1 N1 C11 -76(4) 1_545 . . . ? O1W Co2 N3 C25 -92.8(7) . . . . ? O2W Co2 N3 C25 93.9(7) . . . . ? O5 Co2 N3 C25 177.4(7) . . . . ? O3 Co2 N3 C25 1.6(7) 7_657 . . . ? O1W Co2 N3 C21 110.2(6) . . . . ? O2W Co2 N3 C21 -63.0(6) . . . . ? O5 Co2 N3 C21 20.4(6) . . . . ? O3 Co2 N3 C21 -155.4(6) 7_657 . . . ? O2 Co1 O1 C7 5.5(6) 2_656 . . . ? O7 Co1 O1 C7 -177.6(4) 6_565 . . . ? N2 Co1 O1 C7 -83.8(5) 1_545 . . . ? N1 Co1 O1 C7 92.8(5) . . . . ? O1W Co2 O5 C9 86.0(6) . . . . ? O2W Co2 O5 C9 -90.4(6) . . . . ? O3 Co2 O5 C9 -50(3) 7_657 . . . ? N3 Co2 O5 C9 -173.5(6) . . . . ? C6 C1 C2 C8 79.6(8) . . . . ? C7 C1 C2 C8 -52.7(8) . . . . ? C6 C1 C2 C3 -49.1(8) . . . . ? C7 C1 C2 C3 178.6(5) . . . . ? C8 C2 C3 C4 -82.4(7) . . . . ? C1 C2 C3 C4 49.0(8) . . . . ? C2 C3 C4 C9 75.7(8) . . . . ? C2 C3 C4 C5 -52.4(8) . . . . ? C9 C4 C5 C10 63.4(8) . . . . ? C3 C4 C5 C10 -169.6(6) . . . . ? C9 C4 C5 C6 -71.4(8) . . . . ? C3 C4 C5 C6 55.6(7) . . . . ? C10 C5 C6 C1 168.2(6) . . . . ? C4 C5 C6 C1 -57.7(8) . . . . ? C2 C1 C6 C5 54.7(8) . . . . ? C7 C1 C6 C5 -172.7(5) . . . . ? Co1 O1 C7 O2 2.8(9) . . . . ? Co1 O1 C7 C1 -173.9(4) . . . . ? Co1 O2 C7 O1 -35(2) 2_656 . . . ? Co1 O2 C7 C1 141.6(17) 2_656 . . . ? C2 C1 C7 O1 -6.5(9) . . . . ? C6 C1 C7 O1 -139.4(6) . . . . ? C2 C1 C7 O2 176.5(6) . . . . ? C6 C1 C7 O2 43.6(8) . . . . ? Co2 O3 C8 O4 -7.4(8) 7_657 . . . ? Co2 O3 C8 C2 169.7(5) 7_657 . . . ? C1 C2 C8 O4 -32.0(10) . . . . ? C3 C2 C8 O4 95.8(8) . . . . ? C1 C2 C8 O3 150.9(6) . . . . ? C3 C2 C8 O3 -81.3(8) . . . . ? Co2 O5 C9 O6 -10.5(11) . . . . ? Co2 O5 C9 C4 171.8(4) . . . . ? C5 C4 C9 O6 172.2(6) . . . . ? C3 C4 C9 O6 47.3(9) . . . . ? C5 C4 C9 O5 -9.9(10) . . . . ? C3 C4 C9 O5 -134.8(7) . . . . ? Co1 O7 C10 O8 15.4(9) 6_566 . . . ? Co1 O7 C10 C5 -158.0(5) 6_566 . . . ? C6 C5 C10 O8 163.2(7) . . . . ? C4 C5 C10 O8 30.2(10) . . . . ? C6 C5 C10 O7 -23.3(9) . . . . ? C4 C5 C10 O7 -156.4(6) . . . . ? C15 N1 C11 C12 -0.7(11) . . . . ? Co1 N1 C11 C12 178.0(5) . . . . ? N1 C11 C12 C13 0.2(11) . . . . ? C11 C12 C13 C14 0.4(11) . . . . ? C11 C12 C13 C16 179.6(6) . . . . ? C12 C13 C14 C15 -0.6(11) . . . . ? C16 C13 C14 C15 -179.7(6) . . . . ? C11 N1 C15 C14 0.5(11) . . . . ? Co1 N1 C15 C14 -178.2(5) . . . . ? C13 C14 C15 N1 0.1(11) . . . . ? C12 C13 C16 C20 164.0(7) . . . . ? C14 C13 C16 C20 -16.9(11) . . . . ? C12 C13 C16 C17 -15.9(11) . . . . ? C14 C13 C16 C17 163.3(7) . . . . ? C20 C16 C17 C18 1.8(10) . . . . ? C13 C16 C17 C18 -178.3(6) . . . . ? C19 N2 C18 C17 0.3(10) . . . . ? Co1 N2 C18 C17 175.8(5) 1_565 . . . ? C16 C17 C18 N2 -2.1(11) . . . . ? C18 N2 C19 C20 1.6(9) . . . . ? Co1 N2 C19 C20 -173.8(5) 1_565 . . . ? C17 C16 C20 C19 0.0(10) . . . . ? C13 C16 C20 C19 -179.9(6) . . . . ? N2 C19 C20 C16 -1.8(10) . . . . ? C25 N3 C21 C22 -0.5(12) . . . . ? Co2 N3 C21 C22 157.8(6) . . . . ? N3 C21 C22 C23 -2.1(12) . . . . ? C21 C22 C23 C24 3.7(11) . . . . ? C21 C22 C23 C23 -179.2(8) . . . 5_657 ? C22 C23 C24 C25 -2.7(12) . . . . ? C23 C23 C24 C25 -179.9(8) 5_657 . . . ? C21 N3 C25 C24 1.6(13) . . . . ? Co2 N3 C25 C24 -156.0(6) . . . . ? C23 C24 C25 N3 0.1(13) . . . . ? 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 O1W H1WB O8 0.85 1.99 2.735(7) 145.9 4_647 O1W H1WA O3W 0.85 1.99 2.763(6) 149.8 . O2W H2WA O4 0.85 1.88 2.673(7) 154.8 . O2W H2WB O6 0.85 1.81 2.633(6) 163.9 7_657 O3W H3WA O8 0.85 2.14 2.812(7) 136.0 . O3W H3WB O3 0.85 2.34 2.926(7) 126.9 6_566 O4W H4WA O6 0.85 2.27 3.116(13) 177.9 7_657 _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.113 _refine_diff_density_min -0.380 _refine_diff_density_rms 0.095 #=================================================END data_compound3 _database_code_depnum_ccdc_archive 'CCDC 768143' #TrackingRef 'cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H28 Co2 N4 O10' _chemical_formula_weight 722.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co -2.3653 3.6143 '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 7.3292(6) _cell_length_b 20.3154(14) _cell_length_c 9.9169(8) _cell_angle_alpha 90.00 _cell_angle_beta 99.256(8) _cell_angle_gamma 90.00 _cell_volume 1457.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1232 _cell_measurement_theta_min 4.5241 _cell_measurement_theta_max 62.2636 _exptl_crystal_description sheet _exptl_crystal_colour amaranth _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.646 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 740 _exptl_absorpt_coefficient_mu 9.503 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3298 _exptl_absorpt_correction_T_max 0.7024 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Goniometer Xcalibur, detector: Sapphire3 (Gemini ultra Cu)' _diffrn_measurement_method '\w and \p scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3527 _diffrn_reflns_av_R_equivalents 0.0425 _diffrn_reflns_av_sigmaI/netI 0.0938 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 5.02 _diffrn_reflns_theta_max 59.99 _reflns_number_total 2117 _reflns_number_gt 1408 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0413P)^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 2117 _refine_ls_number_parameters 211 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0691 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.0907 _refine_ls_wR_factor_gt 0.0860 _refine_ls_goodness_of_fit_ref 0.853 _refine_ls_restrained_S_all 0.853 _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 0.04927(9) 0.60891(3) 0.36005(7) 0.0207(2) Uani 1 1 d . . . N1 N -0.1265(5) 0.64370(17) 0.4970(4) 0.0249(9) Uani 1 1 d . . . N2 N 0.0899(5) 0.71147(17) 0.3587(4) 0.0250(9) Uani 1 1 d . . . O1 O 0.2285(4) 0.59229(14) 0.2272(3) 0.0288(8) Uani 1 1 d . . . O1W O 0.2355(4) 0.57441(14) 0.5256(3) 0.0225(7) Uani 1 1 d . . . H1WA H 0.1917 0.5459 0.5745 0.027 Uiso 1 1 d R . . H1WB H 0.3146 0.5575 0.4820 0.027 Uiso 1 1 d R . . O2 O 0.4494(4) 0.53170(16) 0.3501(3) 0.0325(8) Uani 1 1 d . . . O3 O 0.8916(4) 0.51805(14) 0.3113(3) 0.0252(7) Uani 1 1 d . . . O4 O 0.8089(4) 0.60779(15) 0.1934(3) 0.0282(7) Uani 1 1 d . . . C1 C 0.4465(6) 0.5436(2) 0.1074(5) 0.0307(12) Uani 1 1 d . . . H1A H 0.469(6) 0.594(2) 0.057(5) 0.037 Uiso 1 1 d . . . C2 C 0.6345(5) 0.5097(2) 0.1277(5) 0.0256(11) Uani 1 1 d . . . H2A H 0.6228 0.4675 0.1692 0.031 Uiso 1 1 d R . . C3 C 0.6945(6) 0.4976(2) -0.0125(5) 0.0256(10) Uani 1 1 d . . . H3A H 0.7107 0.5405 -0.0564 0.038 Uiso 1 1 calc R . . H3B H 0.8153 0.4747 0.0013 0.038 Uiso 1 1 calc R . . C4 C 0.3719(6) 0.5556(2) 0.2404(5) 0.0228(10) Uani 1 1 d . . . C5 C 0.7845(6) 0.5480(2) 0.2163(5) 0.0229(11) Uani 1 1 d . . . C6 C -0.2330(6) 0.6060(2) 0.5646(4) 0.0271(10) Uani 1 1 d . . . H6A H -0.2297 0.5595 0.5540 0.033 Uiso 1 1 calc R . . C7 C -0.3471(6) 0.6325(2) 0.6491(5) 0.0337(12) Uani 1 1 d . . . H7A H -0.4207 0.6047 0.6956 0.040 Uiso 1 1 calc R . . C8 C -0.3520(6) 0.6995(2) 0.6645(5) 0.0340(12) Uani 1 1 d . . . H8A H -0.4277 0.7185 0.7234 0.041 Uiso 1 1 calc R . . C9 C -0.2466(6) 0.7394(2) 0.5943(5) 0.0310(12) Uani 1 1 d . . . H9A H -0.2511 0.7859 0.6024 0.037 Uiso 1 1 calc R . . C10 C -0.1340(6) 0.7099(2) 0.5115(5) 0.0243(11) Uani 1 1 d . . . C11 C -0.0122(6) 0.7483(2) 0.4337(5) 0.0248(11) Uani 1 1 d . . . C12 C -0.0042(7) 0.8164(2) 0.4338(5) 0.0323(12) Uani 1 1 d . . . H12A H -0.0678 0.8414 0.4926 0.039 Uiso 1 1 calc R . . C13 C 0.0982(7) 0.8476(2) 0.3467(5) 0.0361(13) Uani 1 1 d . . . H13A H 0.0984 0.8942 0.3405 0.043 Uiso 1 1 calc R . . C14 C 0.2005(6) 0.8103(2) 0.2684(5) 0.0313(12) Uani 1 1 d . . . H14A H 0.2728 0.8308 0.2090 0.038 Uiso 1 1 calc R . . C15 C 0.1946(6) 0.7419(2) 0.2794(5) 0.0302(12) Uani 1 1 d . . . H15A H 0.2675 0.7160 0.2286 0.036 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0190(3) 0.0205(4) 0.0243(4) 0.0005(4) 0.0084(3) -0.0002(4) N1 0.023(2) 0.022(2) 0.031(2) -0.0005(17) 0.0071(17) 0.0005(17) N2 0.024(2) 0.025(2) 0.028(2) 0.0025(18) 0.0106(19) -0.0035(17) O1 0.0254(16) 0.0321(19) 0.0308(18) 0.0051(14) 0.0106(14) 0.0083(15) O1W 0.0238(16) 0.0252(16) 0.0202(16) 0.0021(13) 0.0086(14) 0.0042(14) O2 0.0309(18) 0.0393(19) 0.0297(19) 0.0016(16) 0.0117(16) 0.0088(16) O3 0.0214(17) 0.0255(17) 0.0296(18) 0.0046(14) 0.0068(15) 0.0015(14) O4 0.0303(17) 0.0232(17) 0.0321(18) 0.0040(16) 0.0084(15) -0.0006(16) C1 0.023(3) 0.042(3) 0.030(3) -0.005(2) 0.014(2) 0.004(2) C2 0.013(2) 0.036(3) 0.029(3) -0.004(2) 0.0053(19) 0.002(2) C3 0.016(2) 0.032(3) 0.029(3) -0.005(2) 0.006(2) -0.001(2) C4 0.021(3) 0.026(3) 0.022(3) -0.003(2) 0.002(2) -0.009(2) C5 0.017(2) 0.029(3) 0.026(3) -0.013(2) 0.012(2) -0.007(2) C6 0.028(2) 0.026(2) 0.030(3) -0.005(2) 0.012(2) -0.008(2) C7 0.029(3) 0.039(3) 0.037(3) -0.006(2) 0.019(2) -0.009(2) C8 0.026(3) 0.037(3) 0.043(3) -0.012(2) 0.018(2) 0.001(2) C9 0.026(3) 0.030(3) 0.039(3) -0.006(2) 0.011(2) 0.005(2) C10 0.022(2) 0.020(2) 0.030(3) -0.005(2) 0.004(2) -0.001(2) C11 0.023(2) 0.023(2) 0.029(3) -0.001(2) 0.007(2) 0.001(2) C12 0.038(3) 0.021(2) 0.040(3) 0.002(2) 0.012(3) 0.000(2) C13 0.039(3) 0.020(3) 0.049(3) 0.000(2) 0.008(3) -0.007(2) C14 0.032(3) 0.025(3) 0.037(3) 0.006(2) 0.006(2) -0.010(2) C15 0.024(3) 0.032(3) 0.036(3) 0.003(2) 0.008(2) -0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 2.032(3) . ? Co1 O1W 2.081(3) . ? Co1 N2 2.105(4) . ? Co1 N1 2.136(3) . ? Co1 O3 2.190(3) 1_455 ? Co1 O4 2.213(3) 1_455 ? N1 C6 1.347(5) . ? N1 C10 1.354(6) . ? N2 C15 1.335(6) . ? N2 C11 1.361(5) . ? O1 C4 1.278(5) . ? O1W H1WA 0.8501 . ? O1W H1WB 0.8500 . ? O2 C4 1.242(5) . ? O3 C5 1.279(6) . ? O3 Co1 2.190(3) 1_655 ? O4 C5 1.254(5) . ? O4 Co1 2.213(3) 1_655 ? C1 C4 1.526(6) . ? C1 C2 1.526(6) . ? C1 C3 1.531(7) 3_665 ? C1 H1A 1.17(5) . ? C2 C5 1.509(6) . ? C2 C3 1.543(6) . ? C2 H2A 0.9608 . ? C3 C1 1.531(7) 3_665 ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C6 C7 1.385(6) . ? C6 H6A 0.9500 . ? C7 C8 1.370(6) . ? C7 H7A 0.9500 . ? C8 C9 1.383(7) . ? C8 H8A 0.9500 . ? C9 C10 1.389(6) . ? C9 H9A 0.9500 . ? C10 C11 1.491(6) . ? C11 C12 1.386(6) . ? C12 C13 1.385(6) . ? C12 H12A 0.9500 . ? C13 C14 1.387(7) . ? C13 H13A 0.9500 . ? C14 C15 1.396(6) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 O1W 92.59(12) . . ? O1 Co1 N2 93.06(13) . . ? O1W Co1 N2 105.24(14) . . ? O1 Co1 N1 170.18(13) . . ? O1W Co1 N1 89.76(13) . . ? N2 Co1 N1 77.12(13) . . ? O1 Co1 O3 95.16(12) . 1_455 ? O1W Co1 O3 98.40(12) . 1_455 ? N2 Co1 O3 154.55(14) . 1_455 ? N1 Co1 O3 93.93(12) . 1_455 ? O1 Co1 O4 91.97(12) . 1_455 ? O1W Co1 O4 158.13(12) . 1_455 ? N2 Co1 O4 95.85(14) . 1_455 ? N1 Co1 O4 89.37(13) . 1_455 ? O3 Co1 O4 59.88(11) 1_455 1_455 ? C6 N1 C10 118.3(4) . . ? C6 N1 Co1 125.8(3) . . ? C10 N1 Co1 115.8(3) . . ? C15 N2 C11 119.1(4) . . ? C15 N2 Co1 123.9(3) . . ? C11 N2 Co1 116.7(3) . . ? C4 O1 Co1 129.6(3) . . ? Co1 O1W H1WA 114.8 . . ? Co1 O1W H1WB 98.6 . . ? H1WA O1W H1WB 111.4 . . ? C5 O3 Co1 90.1(2) . 1_655 ? C5 O4 Co1 89.7(3) . 1_655 ? C4 C1 C2 113.6(4) . . ? C4 C1 C3 108.6(3) . 3_665 ? C2 C1 C3 109.9(4) . 3_665 ? C4 C1 H1A 109(2) . . ? C2 C1 H1A 105(2) . . ? C3 C1 H1A 110(2) 3_665 . ? C5 C2 C1 113.7(4) . . ? C5 C2 C3 108.7(3) . . ? C1 C2 C3 109.6(4) . . ? C5 C2 H2A 108.6 . . ? C1 C2 H2A 108.6 . . ? C3 C2 H2A 107.6 . . ? C1 C3 C2 112.3(3) 3_665 . ? C1 C3 H3A 109.2 3_665 . ? C2 C3 H3A 109.2 . . ? C1 C3 H3B 109.2 3_665 . ? C2 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? O2 C4 O1 124.7(4) . . ? O2 C4 C1 121.2(4) . . ? O1 C4 C1 114.1(4) . . ? O4 C5 O3 120.4(4) . . ? O4 C5 C2 120.4(4) . . ? O3 C5 C2 119.1(4) . . ? N1 C6 C7 122.3(4) . . ? N1 C6 H6A 118.8 . . ? C7 C6 H6A 118.8 . . ? C8 C7 C6 118.9(4) . . ? C8 C7 H7A 120.6 . . ? C6 C7 H7A 120.6 . . ? C7 C8 C9 119.9(4) . . ? C7 C8 H8A 120.0 . . ? C9 C8 H8A 120.0 . . ? C8 C9 C10 118.6(4) . . ? C8 C9 H9A 120.7 . . ? C10 C9 H9A 120.7 . . ? N1 C10 C9 121.9(4) . . ? N1 C10 C11 115.2(4) . . ? C9 C10 C11 122.8(4) . . ? N2 C11 C12 121.5(4) . . ? N2 C11 C10 115.1(4) . . ? C12 C11 C10 123.5(4) . . ? C13 C12 C11 118.9(4) . . ? C13 C12 H12A 120.6 . . ? C11 C12 H12A 120.6 . . ? C12 C13 C14 119.7(4) . . ? C12 C13 H13A 120.1 . . ? C14 C13 H13A 120.1 . . ? C13 C14 C15 118.3(4) . . ? C13 C14 H14A 120.9 . . ? C15 C14 H14A 120.9 . . ? N2 C15 C14 122.3(4) . . ? N2 C15 H15A 118.8 . . ? C14 C15 H15A 118.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Co1 N1 C6 -178.0(7) . . . . ? O1W Co1 N1 C6 -74.0(4) . . . . ? N2 Co1 N1 C6 -179.7(4) . . . . ? O3 Co1 N1 C6 24.4(4) 1_455 . . . ? O4 Co1 N1 C6 84.1(4) 1_455 . . . ? O1 Co1 N1 C10 4.5(11) . . . . ? O1W Co1 N1 C10 108.5(3) . . . . ? N2 Co1 N1 C10 2.7(3) . . . . ? O3 Co1 N1 C10 -153.1(3) 1_455 . . . ? O4 Co1 N1 C10 -93.4(3) 1_455 . . . ? O1 Co1 N2 C15 4.2(4) . . . . ? O1W Co1 N2 C15 97.8(4) . . . . ? N1 Co1 N2 C15 -176.1(4) . . . . ? O3 Co1 N2 C15 -104.5(4) 1_455 . . . ? O4 Co1 N2 C15 -88.0(4) 1_455 . . . ? O1 Co1 N2 C11 177.5(3) . . . . ? O1W Co1 N2 C11 -89.0(3) . . . . ? N1 Co1 N2 C11 -2.8(3) . . . . ? O3 Co1 N2 C11 68.7(5) 1_455 . . . ? O4 Co1 N2 C11 85.2(3) 1_455 . . . ? O1W Co1 O1 C4 18.4(4) . . . . ? N2 Co1 O1 C4 123.9(4) . . . . ? N1 Co1 O1 C4 122.1(8) . . . . ? O3 Co1 O1 C4 -80.2(4) 1_455 . . . ? O4 Co1 O1 C4 -140.2(4) 1_455 . . . ? C4 C1 C2 C5 -60.2(5) . . . . ? C3 C1 C2 C5 178.0(4) 3_665 . . . ? C4 C1 C2 C3 178.0(4) . . . . ? C3 C1 C2 C3 56.2(5) 3_665 . . . ? C5 C2 C3 C1 177.6(4) . . . 3_665 ? C1 C2 C3 C1 -57.6(6) . . . 3_665 ? Co1 O1 C4 O2 -14.1(6) . . . . ? Co1 O1 C4 C1 166.9(3) . . . . ? C2 C1 C4 O2 -8.7(6) . . . . ? C3 C1 C4 O2 113.8(5) 3_665 . . . ? C2 C1 C4 O1 170.4(4) . . . . ? C3 C1 C4 O1 -67.1(5) 3_665 . . . ? Co1 O4 C5 O3 0.2(4) 1_655 . . . ? Co1 O4 C5 C2 -176.7(3) 1_655 . . . ? Co1 O3 C5 O4 -0.2(4) 1_655 . . . ? Co1 O3 C5 C2 176.8(3) 1_655 . . . ? C1 C2 C5 O4 -49.5(5) . . . . ? C3 C2 C5 O4 72.8(5) . . . . ? C1 C2 C5 O3 133.6(4) . . . . ? C3 C2 C5 O3 -104.1(4) . . . . ? C10 N1 C6 C7 -0.8(7) . . . . ? Co1 N1 C6 C7 -178.3(4) . . . . ? N1 C6 C7 C8 0.0(8) . . . . ? C6 C7 C8 C9 1.2(8) . . . . ? C7 C8 C9 C10 -1.5(8) . . . . ? C6 N1 C10 C9 0.4(7) . . . . ? Co1 N1 C10 C9 178.2(4) . . . . ? C6 N1 C10 C11 180.0(4) . . . . ? Co1 N1 C10 C11 -2.3(5) . . . . ? C8 C9 C10 N1 0.7(8) . . . . ? C8 C9 C10 C11 -178.8(5) . . . . ? C15 N2 C11 C12 -2.7(7) . . . . ? Co1 N2 C11 C12 -176.3(4) . . . . ? C15 N2 C11 C10 176.1(4) . . . . ? Co1 N2 C11 C10 2.5(5) . . . . ? N1 C10 C11 N2 0.0(6) . . . . ? C9 C10 C11 N2 179.5(5) . . . . ? N1 C10 C11 C12 178.7(5) . . . . ? C9 C10 C11 C12 -1.8(8) . . . . ? N2 C11 C12 C13 5.5(8) . . . . ? C10 C11 C12 C13 -173.1(5) . . . . ? C11 C12 C13 C14 -4.4(8) . . . . ? C12 C13 C14 C15 0.8(8) . . . . ? C11 N2 C15 C14 -1.2(7) . . . . ? Co1 N2 C15 C14 171.9(4) . . . . ? C13 C14 C15 N2 2.2(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 O1W H1WA O3 0.85 1.89 2.738(4) 176.7 3_666 O1W H1WB O2 0.85 1.84 2.668(4) 165.1 . _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 59.99 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.463 _refine_diff_density_min -0.375 _refine_diff_density_rms 0.070 #=================================================END data_compound4 _database_code_depnum_ccdc_archive 'CCDC 768144' #TrackingRef 'cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H36 Co2 N4 O14' _chemical_formula_weight 842.53 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)/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 6.5613(13) _cell_length_b 24.646(5) _cell_length_c 11.088(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.26(3) _cell_angle_gamma 90.00 _cell_volume 1769.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.581 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 868 _exptl_absorpt_coefficient_mu 1.013 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8386 _exptl_absorpt_correction_T_max 0.9511 _exptl_absorpt_process_details '(ABSCOR; Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS SPIDER IP' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14158 _diffrn_reflns_av_R_equivalents 0.0900 _diffrn_reflns_av_sigmaI/netI 0.0771 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 27.00 _reflns_number_total 3802 _reflns_number_gt 1984 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'PROCESS-AUTO (Rigaku, 1998)' _computing_cell_refinement 'PROCESS-AUTO (Rigaku, 1998)' _computing_data_reduction 'PROCESS-AUTO (Rigaku, 1998)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0816P)^2^+0.8302P] 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 3802 _refine_ls_number_parameters 244 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.1324 _refine_ls_R_factor_gt 0.0634 _refine_ls_wR_factor_ref 0.1840 _refine_ls_wR_factor_gt 0.1450 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.046 _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 0.59638(11) 0.12696(3) 0.76601(7) 0.0489(3) Uani 1 1 d . . . N1 N 0.8398(6) 0.17636(16) 0.8569(4) 0.0485(10) Uani 1 1 d . . . N2 N 0.4642(7) 0.20387(17) 0.7411(4) 0.0506(11) Uani 1 1 d . . . O1 O 0.3327(6) 0.08905(15) 0.6799(4) 0.0626(10) Uani 1 1 d . . . O2 O 0.3165(7) 0.02385(18) 0.8150(4) 0.0831(14) Uani 1 1 d . . . O3 O -0.2059(7) 0.06128(15) 0.7344(4) 0.0691(11) Uani 1 1 d . . . O4 O -0.2509(6) 0.12701(15) 0.6028(4) 0.0679(11) Uani 1 1 d . . . O1W O 0.5365(6) 0.10169(14) 0.9352(4) 0.0630(10) Uani 1 1 d D . . H1WA H 0.6487 0.0992 0.9853 0.076 Uiso 1 1 d RD . . H1WB H 0.4786 0.0707 0.9289 0.076 Uiso 1 1 d RD . . O2W O 0.8511(8) 0.06453(18) 1.1027(5) 0.1024(17) Uani 1 1 d D . . H2WA H 0.9545 0.0557 1.0697 0.123 Uiso 1 1 d RD . . H2WB H 0.7985 0.0363 1.1294 0.123 Uiso 1 1 d RD . . O3W O 1.2661(11) 0.0418(2) 1.1625(9) 0.170(4) Uani 1 1 d D . . H3WA H 1.3924 0.0479 1.1587 0.204 Uiso 1 1 d RD . . H3WB H 1.2684 0.0110 1.1975 0.204 Uiso 1 1 d RD . . C1 C 0.1047(8) 0.0145(2) 0.6236(6) 0.0587(15) Uani 1 1 d . . . H1A H 0.0323 -0.0111 0.6694 0.070 Uiso 1 1 calc R . . C2 C -0.0555(9) 0.0516(2) 0.5530(5) 0.0568(14) Uani 1 1 d . . . H2A H 0.0140 0.0774 0.5061 0.068 Uiso 1 1 calc R . . C3 C -0.2122(8) 0.0179(2) 0.4630(6) 0.0641(16) Uani 1 1 d . . . H3A H -0.2867 -0.0066 0.5089 0.077 Uiso 1 1 calc R . . H3B H -0.3118 0.0421 0.4164 0.077 Uiso 1 1 calc R . . C4 C 0.2610(9) 0.0445(2) 0.7143(6) 0.0597(15) Uani 1 1 d . . . C5 C -0.1769(9) 0.0827(2) 0.6339(5) 0.0541(14) Uani 1 1 d . . . C6 C 1.0226(9) 0.1619(2) 0.9148(5) 0.0580(14) Uani 1 1 d . . . H6 H 1.0425 0.1279 0.9122 0.070 Uiso 1 1 d R . . C7 C 1.1669(9) 0.1983(2) 0.9715(6) 0.0643(16) Uani 1 1 d . . . H7 H 1.2935 0.1861 1.0125 0.077 Uiso 1 1 calc R . . C8 C 1.1214(10) 0.2527(2) 0.9667(6) 0.0690(18) Uani 1 1 d . . . H8 H 1.1999 0.2769 1.0038 0.083 Uiso 1 1 d R . . C9 C 0.9297(10) 0.2701(2) 0.9048(5) 0.0585(15) Uani 1 1 d . . . C10 C 0.7905(9) 0.2302(2) 0.8515(5) 0.0496(13) Uani 1 1 d . . . C11 C 0.5915(9) 0.2447(2) 0.7881(5) 0.0523(13) Uani 1 1 d . . . C12 C 0.5335(11) 0.2995(2) 0.7760(6) 0.0640(17) Uani 1 1 d . . . C13 C 0.3368(12) 0.3103(3) 0.7115(7) 0.083(2) Uani 1 1 d . . . H13 H 0.3038 0.3437 0.7077 0.099 Uiso 1 1 d R . . C14 C 0.2116(12) 0.2691(3) 0.6650(6) 0.082(2) Uani 1 1 d . . . H14 H 0.0800 0.2764 0.6231 0.098 Uiso 1 1 calc R . . C15 C 0.2804(9) 0.2164(2) 0.6803(6) 0.0634(16) Uani 1 1 d . . . H15 H 0.1931 0.1916 0.6567 0.076 Uiso 1 1 d R . . C16 C 0.8659(12) 0.3259(2) 0.8901(7) 0.077(2) Uani 1 1 d . . . H16 H 0.9556 0.3532 0.9233 0.093 Uiso 1 1 calc R . . C17 C 0.6784(13) 0.3392(2) 0.8288(7) 0.078(2) Uani 1 1 d . . . H17 H 0.6423 0.3756 0.8208 0.093 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0476(4) 0.0486(4) 0.0470(5) -0.0059(3) -0.0023(3) 0.0036(3) N1 0.046(3) 0.049(2) 0.049(3) -0.0039(19) 0.001(2) 0.0015(18) N2 0.052(3) 0.061(3) 0.039(3) -0.003(2) 0.006(2) 0.008(2) O1 0.057(2) 0.070(2) 0.054(3) -0.0063(19) -0.011(2) 0.004(2) O2 0.083(3) 0.084(3) 0.073(3) 0.009(2) -0.018(3) -0.029(2) O3 0.076(3) 0.057(2) 0.069(3) -0.003(2) -0.006(2) 0.015(2) O4 0.074(3) 0.062(2) 0.067(3) 0.000(2) 0.008(2) 0.020(2) O1W 0.062(3) 0.066(2) 0.056(3) -0.0006(19) -0.005(2) -0.0135(19) O2W 0.100(4) 0.086(3) 0.109(4) 0.030(3) -0.020(3) -0.017(3) O3W 0.131(6) 0.096(4) 0.302(11) 0.040(5) 0.091(7) 0.025(4) C1 0.045(3) 0.060(3) 0.066(4) -0.019(3) -0.006(3) 0.007(2) C2 0.056(3) 0.060(3) 0.052(4) -0.007(3) 0.001(3) 0.010(3) C3 0.041(3) 0.082(4) 0.063(4) -0.025(3) -0.010(3) 0.012(3) C4 0.047(3) 0.058(3) 0.069(4) -0.009(3) -0.005(3) -0.005(3) C5 0.053(3) 0.065(3) 0.040(3) -0.010(3) -0.007(3) -0.001(3) C6 0.052(3) 0.062(3) 0.056(4) -0.008(3) -0.003(3) -0.001(3) C7 0.050(3) 0.082(4) 0.058(4) -0.011(3) -0.001(3) -0.011(3) C8 0.069(4) 0.073(4) 0.065(4) -0.014(3) 0.011(4) -0.024(3) C9 0.072(4) 0.061(3) 0.045(3) -0.009(3) 0.017(3) -0.013(3) C10 0.066(4) 0.050(3) 0.035(3) -0.005(2) 0.014(3) -0.006(2) C11 0.061(4) 0.056(3) 0.042(3) 0.005(2) 0.013(3) 0.008(3) C12 0.091(5) 0.041(3) 0.064(4) 0.005(3) 0.025(4) 0.005(3) C13 0.101(6) 0.071(4) 0.080(5) 0.022(4) 0.025(5) 0.045(4) C14 0.090(5) 0.085(5) 0.066(5) 0.012(4) 0.001(4) 0.030(4) C15 0.051(4) 0.076(4) 0.059(4) 0.008(3) -0.003(3) 0.014(3) C16 0.110(6) 0.051(3) 0.074(5) -0.011(3) 0.026(5) -0.022(4) C17 0.114(6) 0.046(3) 0.078(5) 0.004(3) 0.029(5) 0.009(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 2.061(4) . ? Co1 O1W 2.073(4) . ? Co1 N2 2.084(4) . ? Co1 N1 2.128(4) . ? Co1 O3 2.138(4) 1_655 ? Co1 O4 2.205(4) 1_655 ? Co1 C5 2.500(6) 1_655 ? N1 C6 1.315(7) . ? N1 C10 1.365(6) . ? N2 C15 1.320(7) . ? N2 C11 1.358(7) . ? O1 C4 1.276(7) . ? O2 C4 1.228(7) . ? O3 C5 1.275(7) . ? O3 Co1 2.138(4) 1_455 ? O4 C5 1.222(6) . ? O4 Co1 2.205(4) 1_455 ? O1W H1WA 0.8500 . ? O1W H1WB 0.8500 . ? O2W H2WA 0.8501 . ? O2W H2WB 0.8499 . ? O3W H3WA 0.8500 . ? O3W H3WB 0.8501 . ? C1 C3 1.508(7) 3_556 ? C1 C4 1.509(8) . ? C1 C2 1.512(7) . ? C1 H1A 0.9800 . ? C2 C5 1.502(8) . ? C2 C3 1.554(7) . ? C2 H2A 0.9800 . ? C3 C1 1.508(7) 3_556 ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C5 Co1 2.500(6) 1_455 ? C6 C7 1.380(7) . ? C6 H6 0.8500 . ? C7 C8 1.372(8) . ? C7 H7 0.9300 . ? C8 C9 1.400(9) . ? C8 H8 0.8500 . ? C9 C10 1.407(7) . ? C9 C16 1.438(8) . ? C10 C11 1.425(8) . ? C11 C12 1.403(7) . ? C12 C13 1.397(10) . ? C12 C17 1.423(9) . ? C13 C14 1.354(10) . ? C13 H13 0.8498 . ? C14 C15 1.377(8) . ? C14 H14 0.9300 . ? C15 H15 0.8497 . ? C16 C17 1.346(10) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 O1W 90.90(16) . . ? O1 Co1 N2 92.90(16) . . ? O1W Co1 N2 104.94(16) . . ? O1 Co1 N1 171.41(15) . . ? O1W Co1 N1 88.89(16) . . ? N2 Co1 N1 78.87(16) . . ? O1 Co1 O3 93.85(15) . 1_655 ? O1W Co1 O3 97.43(17) . 1_655 ? N2 Co1 O3 156.51(18) . 1_655 ? N1 Co1 O3 94.69(16) . 1_655 ? O1 Co1 O4 94.50(16) . 1_655 ? O1W Co1 O4 156.94(15) . 1_655 ? N2 Co1 O4 97.17(15) . 1_655 ? N1 Co1 O4 89.01(16) . 1_655 ? O3 Co1 O4 59.88(16) 1_655 1_655 ? O1 Co1 C5 93.73(16) . 1_655 ? O1W Co1 C5 128.06(18) . 1_655 ? N2 Co1 C5 126.37(19) . 1_655 ? N1 Co1 C5 93.16(17) . 1_655 ? O3 Co1 C5 30.66(16) 1_655 1_655 ? O4 Co1 C5 29.26(16) 1_655 1_655 ? C6 N1 C10 118.4(5) . . ? C6 N1 Co1 129.2(4) . . ? C10 N1 Co1 112.4(3) . . ? C15 N2 C11 118.6(5) . . ? C15 N2 Co1 127.3(4) . . ? C11 N2 Co1 114.0(3) . . ? C4 O1 Co1 125.0(4) . . ? C5 O3 Co1 90.6(3) . 1_455 ? C5 O4 Co1 88.9(4) . 1_455 ? Co1 O1W H1WA 110.0 . . ? Co1 O1W H1WB 110.1 . . ? H1WA O1W H1WB 108.5 . . ? H2WA O2W H2WB 109.7 . . ? H3WA O3W H3WB 103.6 . . ? C3 C1 C4 110.2(5) 3_556 . ? C3 C1 C2 110.4(5) 3_556 . ? C4 C1 C2 113.0(5) . . ? C3 C1 H1A 107.7 3_556 . ? C4 C1 H1A 107.7 . . ? C2 C1 H1A 107.7 . . ? C5 C2 C1 113.0(5) . . ? C5 C2 C3 107.3(4) . . ? C1 C2 C3 110.0(4) . . ? C5 C2 H2A 108.8 . . ? C1 C2 H2A 108.8 . . ? C3 C2 H2A 108.8 . . ? C1 C3 C2 111.3(4) 3_556 . ? C1 C3 H3A 109.4 3_556 . ? C2 C3 H3A 109.4 . . ? C1 C3 H3B 109.4 3_556 . ? C2 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? O2 C4 O1 124.0(5) . . ? O2 C4 C1 118.3(5) . . ? O1 C4 C1 117.8(6) . . ? O4 C5 O3 120.5(5) . . ? O4 C5 C2 120.8(6) . . ? O3 C5 C2 118.6(5) . . ? O4 C5 Co1 61.9(3) . 1_455 ? O3 C5 Co1 58.8(3) . 1_455 ? C2 C5 Co1 174.4(4) . 1_455 ? N1 C6 C7 123.5(5) . . ? N1 C6 H6 112.6 . . ? C7 C6 H6 124.0 . . ? C8 C7 C6 119.2(6) . . ? C8 C7 H7 120.4 . . ? C6 C7 H7 120.4 . . ? C7 C8 C9 119.5(5) . . ? C7 C8 H8 123.7 . . ? C9 C8 H8 116.7 . . ? C8 C9 C10 117.5(5) . . ? C8 C9 C16 124.8(6) . . ? C10 C9 C16 117.6(6) . . ? N1 C10 C9 121.9(5) . . ? N1 C10 C11 117.2(5) . . ? C9 C10 C11 120.8(5) . . ? N2 C11 C12 122.4(6) . . ? N2 C11 C10 117.5(5) . . ? C12 C11 C10 120.1(6) . . ? C13 C12 C11 116.5(6) . . ? C13 C12 C17 125.5(6) . . ? C11 C12 C17 118.0(6) . . ? C14 C13 C12 120.4(6) . . ? C14 C13 H13 124.9 . . ? C12 C13 H13 114.6 . . ? C13 C14 C15 119.6(7) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? N2 C15 C14 122.5(6) . . ? N2 C15 H15 120.3 . . ? C14 C15 H15 116.8 . . ? C17 C16 C9 121.0(6) . . ? C17 C16 H16 119.5 . . ? C9 C16 H16 119.5 . . ? C16 C17 C12 122.4(6) . . ? C16 C17 H17 118.8 . . ? C12 C17 H17 118.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Co1 N1 C6 162.2(10) . . . . ? O1W Co1 N1 C6 73.5(5) . . . . ? N2 Co1 N1 C6 179.0(5) . . . . ? O3 Co1 N1 C6 -23.9(5) 1_655 . . . ? O4 Co1 N1 C6 -83.5(5) 1_655 . . . ? C5 Co1 N1 C6 -54.6(5) 1_655 . . . ? O1 Co1 N1 C10 -17.7(13) . . . . ? O1W Co1 N1 C10 -106.4(4) . . . . ? N2 Co1 N1 C10 -0.9(3) . . . . ? O3 Co1 N1 C10 156.3(4) 1_655 . . . ? O4 Co1 N1 C10 96.6(4) 1_655 . . . ? C5 Co1 N1 C10 125.6(4) 1_655 . . . ? O1 Co1 N2 C15 -4.6(5) . . . . ? O1W Co1 N2 C15 -96.4(5) . . . . ? N1 Co1 N2 C15 177.8(5) . . . . ? O3 Co1 N2 C15 101.9(6) 1_655 . . . ? O4 Co1 N2 C15 90.3(5) 1_655 . . . ? C5 Co1 N2 C15 92.1(5) 1_655 . . . ? O1 Co1 N2 C11 179.4(4) . . . . ? O1W Co1 N2 C11 87.7(4) . . . . ? N1 Co1 N2 C11 1.9(3) . . . . ? O3 Co1 N2 C11 -74.0(6) 1_655 . . . ? O4 Co1 N2 C11 -85.7(4) 1_655 . . . ? C5 Co1 N2 C11 -83.8(4) 1_655 . . . ? O1W Co1 O1 C4 -35.1(5) . . . . ? N2 Co1 O1 C4 -140.1(5) . . . . ? N1 Co1 O1 C4 -123.6(11) . . . . ? O3 Co1 O1 C4 62.4(5) 1_655 . . . ? O4 Co1 O1 C4 122.5(5) 1_655 . . . ? C5 Co1 O1 C4 93.2(5) 1_655 . . . ? C3 C1 C2 C5 176.6(5) 3_556 . . . ? C4 C1 C2 C5 -59.4(7) . . . . ? C3 C1 C2 C3 56.8(7) 3_556 . . . ? C4 C1 C2 C3 -179.3(5) . . . . ? C5 C2 C3 C1 179.4(5) . . . 3_556 ? C1 C2 C3 C1 -57.3(7) . . . 3_556 ? Co1 O1 C4 O2 14.5(9) . . . . ? Co1 O1 C4 C1 -163.1(3) . . . . ? C3 C1 C4 O2 -96.6(7) 3_556 . . . ? C2 C1 C4 O2 139.4(6) . . . . ? C3 C1 C4 O1 81.1(7) 3_556 . . . ? C2 C1 C4 O1 -42.9(7) . . . . ? Co1 O4 C5 O3 -3.8(5) 1_455 . . . ? Co1 O4 C5 C2 174.4(5) 1_455 . . . ? Co1 O3 C5 O4 3.9(6) 1_455 . . . ? Co1 O3 C5 C2 -174.3(4) 1_455 . . . ? C1 C2 C5 O4 151.9(5) . . . . ? C3 C2 C5 O4 -86.7(6) . . . . ? C1 C2 C5 O3 -29.9(7) . . . . ? C3 C2 C5 O3 91.5(6) . . . . ? C1 C2 C5 Co1 -91(4) . . . 1_455 ? C3 C2 C5 Co1 31(5) . . . 1_455 ? C10 N1 C6 C7 0.6(8) . . . . ? Co1 N1 C6 C7 -179.3(4) . . . . ? N1 C6 C7 C8 -1.0(9) . . . . ? C6 C7 C8 C9 0.2(9) . . . . ? C7 C8 C9 C10 0.9(8) . . . . ? C7 C8 C9 C16 -178.0(6) . . . . ? C6 N1 C10 C9 0.6(8) . . . . ? Co1 N1 C10 C9 -179.5(4) . . . . ? C6 N1 C10 C11 180.0(5) . . . . ? Co1 N1 C10 C11 -0.1(6) . . . . ? C8 C9 C10 N1 -1.4(8) . . . . ? C16 C9 C10 N1 177.7(5) . . . . ? C8 C9 C10 C11 179.3(5) . . . . ? C16 C9 C10 C11 -1.7(8) . . . . ? C15 N2 C11 C12 0.9(8) . . . . ? Co1 N2 C11 C12 177.3(4) . . . . ? C15 N2 C11 C10 -178.9(5) . . . . ? Co1 N2 C11 C10 -2.6(6) . . . . ? N1 C10 C11 N2 1.8(7) . . . . ? C9 C10 C11 N2 -178.8(5) . . . . ? N1 C10 C11 C12 -178.0(5) . . . . ? C9 C10 C11 C12 1.3(8) . . . . ? N2 C11 C12 C13 -0.6(8) . . . . ? C10 C11 C12 C13 179.3(5) . . . . ? N2 C11 C12 C17 180.0(5) . . . . ? C10 C11 C12 C17 -0.2(8) . . . . ? C11 C12 C13 C14 0.5(10) . . . . ? C17 C12 C13 C14 180.0(7) . . . . ? C12 C13 C14 C15 -0.9(11) . . . . ? C11 N2 C15 C14 -1.3(9) . . . . ? Co1 N2 C15 C14 -177.1(5) . . . . ? C13 C14 C15 N2 1.3(11) . . . . ? C8 C9 C16 C17 179.9(6) . . . . ? C10 C9 C16 C17 0.9(9) . . . . ? C9 C16 C17 C12 0.2(10) . . . . ? C13 C12 C17 C16 180.0(7) . . . . ? C11 C12 C17 C16 -0.6(10) . . . . ? 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 O1W H1WA O2W 0.85 1.91 2.705(6) 156.0 . O1W H1WB O2 0.85 1.91 2.631(5) 142.4 . O2W H2WA O3W 0.85 2.16 2.755(9) 126.5 . O2W H2WB O2 0.85 1.82 2.666(6) 179.3 3_657 O3W H3WA O2 0.85 2.58 3.156(8) 125.6 3_757 O3W H3WB O3 0.85 2.00 2.839(7) 167.2 3_657 _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.479 _refine_diff_density_min -0.492 _refine_diff_density_rms 0.089 #_eof #End of Crystallographic Information File