# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email wyaoyu@nwu.edu.cn _publ_contact_author_name 'Yao-Yu Wang' loop_ _publ_author_name 'Bo Liu' 'Lei Hou' 'Yao-Yu Wang' 'Qi-Zhen Shi' data_Complex_1 _database_code_depnum_ccdc_archive 'CCDC 848094' #TrackingRef 'web_deposit_cif_file_0_BoLiu_1318311692.1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum C18H13CoN2O5 _chemical_formula_weight 396.22 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/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 13.1622(15) _cell_length_b 7.2427(8) _cell_length_c 17.7408(19) _cell_angle_alpha 90.00 _cell_angle_beta 103.584(2) _cell_angle_gamma 90.00 _cell_volume 1643.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2647 _cell_measurement_theta_min 2.823 _cell_measurement_theta_max 26.492 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.593 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 800 _exptl_absorpt_coefficient_mu 1.077 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8216 _exptl_absorpt_correction_T_max 0.8466 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8007 _diffrn_reflns_av_R_equivalents 0.0297 _diffrn_reflns_av_sigmaI/netI 0.0320 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 25.10 _reflns_number_total 2928 _reflns_number_gt 2499 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0449P)^2^+1.0322P] 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 2928 _refine_ls_number_parameters 236 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0424 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.0942 _refine_ls_wR_factor_gt 0.0901 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 0.21497(3) 0.42354(5) 0.40245(2) 0.03114(14) Uani 1 1 d . . . O1 O 0.26732(16) 0.2774(3) 0.49644(11) 0.0450(5) Uani 1 1 d . . . O2 O 0.15403(16) 0.0745(3) 0.43256(11) 0.0436(5) Uani 1 1 d . . . O3 O 0.37307(17) -0.3454(4) 0.81214(13) 0.0658(7) Uani 1 1 d . . . O4 O 0.20236(15) -0.3389(3) 0.79660(11) 0.0452(5) Uani 1 1 d . . . N1 N 0.31714(16) 0.6397(3) 0.43396(12) 0.0312(5) Uani 1 1 d . . . N2 N -0.06286(17) -0.5111(3) 0.61100(13) 0.0335(5) Uani 1 1 d . . . C1 C 0.2179(2) 0.1236(4) 0.49168(16) 0.0339(6) Uani 1 1 d . . . C2 C 0.24013(19) 0.0043(4) 0.56254(15) 0.0289(6) Uani 1 1 d . . . C3 C 0.3216(2) 0.0444(4) 0.62621(16) 0.0343(6) Uani 1 1 d . . . H3 H 0.3651 0.1449 0.6248 0.041 Uiso 1 1 calc R . . C4 C 0.3376(2) -0.0657(4) 0.69131(16) 0.0359(6) Uani 1 1 d . . . H4 H 0.3936 -0.0407 0.7329 0.043 Uiso 1 1 calc R . . C5 C 0.27138(19) -0.2142(4) 0.69630(14) 0.0300(6) Uani 1 1 d . . . C6 C 0.18994(18) -0.2571(3) 0.63182(14) 0.0271(5) Uani 1 1 d . . . C7 C 0.17671(18) -0.1466(3) 0.56581(14) 0.0284(5) Uani 1 1 d . . . H7 H 0.1237 -0.1752 0.5227 0.034 Uiso 1 1 calc R . . C8 C 0.2852(2) -0.3096(4) 0.77361(15) 0.0363(6) Uani 1 1 d . . . C9 C 0.1169(2) -0.4136(3) 0.63212(14) 0.0280(6) Uani 1 1 d . . . C10 C 0.01056(19) -0.3800(4) 0.61104(15) 0.0317(6) Uani 1 1 d . . . H10 H -0.0118 -0.2609 0.5961 0.038 Uiso 1 1 calc R . . C11 C -0.0295(2) -0.6827(4) 0.63207(17) 0.0419(7) Uani 1 1 d . . . H11 H -0.0787 -0.7744 0.6327 0.050 Uiso 1 1 calc R . . C12 C 0.0749(2) -0.7284(4) 0.65276(18) 0.0459(8) Uani 1 1 d . . . H12 H 0.0955 -0.8491 0.6664 0.055 Uiso 1 1 calc R . . C13 C 0.1489(2) -0.5927(4) 0.65301(18) 0.0400(7) Uani 1 1 d . . . H13 H 0.2197 -0.6213 0.6671 0.048 Uiso 1 1 calc R . . C14 C 0.3843(2) 0.6330(4) 0.50397(17) 0.0382(7) Uani 1 1 d . . . H14 H 0.3814 0.5321 0.5358 0.046 Uiso 1 1 calc R . . C15 C 0.4572(2) 0.7686(4) 0.53065(16) 0.0391(7) Uani 1 1 d . . . H15 H 0.5029 0.7566 0.5791 0.047 Uiso 1 1 calc R . . C16 C 0.46288(19) 0.9226(3) 0.48575(15) 0.0290(6) Uani 1 1 d . . . C17 C 0.3948(2) 0.9271(4) 0.41331(17) 0.0422(7) Uani 1 1 d . . . H17 H 0.3964 1.0262 0.3803 0.051 Uiso 1 1 calc R . . C18 C 0.3246(2) 0.7853(4) 0.38987(17) 0.0441(7) Uani 1 1 d . . . H18 H 0.2802 0.7917 0.3407 0.053 Uiso 1 1 calc R . . O1W O 0.5000 0.6111(9) 0.2500 0.195(4) Uani 1 2 d S . . O2W O 0.0000 0.0841(6) 0.2500 0.0939(14) Uani 1 2 d S . . 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 0.0310(2) 0.0325(2) 0.0291(2) -0.00402(15) 0.00544(15) -0.01156(15) O1 0.0563(13) 0.0338(11) 0.0435(12) 0.0073(9) 0.0091(10) -0.0145(10) O2 0.0476(12) 0.0408(12) 0.0383(12) 0.0087(9) 0.0021(10) -0.0026(9) O3 0.0447(13) 0.0941(19) 0.0482(14) 0.0265(13) -0.0100(11) -0.0095(13) O4 0.0476(12) 0.0562(13) 0.0347(11) 0.0121(10) 0.0159(9) 0.0081(10) N1 0.0315(11) 0.0281(11) 0.0333(12) -0.0043(10) 0.0060(9) -0.0082(9) N2 0.0334(12) 0.0320(12) 0.0357(12) -0.0060(10) 0.0093(10) -0.0098(10) C1 0.0354(15) 0.0303(14) 0.0380(16) 0.0034(12) 0.0130(12) -0.0005(12) C2 0.0305(13) 0.0268(13) 0.0313(14) 0.0003(11) 0.0110(11) -0.0013(11) C3 0.0298(14) 0.0343(15) 0.0396(15) -0.0022(12) 0.0096(12) -0.0089(11) C4 0.0296(14) 0.0427(16) 0.0318(15) -0.0023(12) -0.0002(11) -0.0089(12) C5 0.0279(13) 0.0336(14) 0.0281(13) -0.0009(11) 0.0056(10) -0.0001(11) C6 0.0251(12) 0.0275(13) 0.0291(13) -0.0026(11) 0.0075(10) -0.0012(10) C7 0.0265(13) 0.0312(13) 0.0255(13) -0.0017(11) 0.0021(10) -0.0023(11) C8 0.0415(16) 0.0338(15) 0.0295(14) -0.0017(12) 0.0005(12) -0.0023(12) C9 0.0337(14) 0.0255(13) 0.0256(13) -0.0010(10) 0.0088(11) -0.0038(10) C10 0.0321(14) 0.0279(14) 0.0343(15) 0.0012(11) 0.0059(11) -0.0062(11) C11 0.0488(18) 0.0337(16) 0.0465(17) -0.0059(13) 0.0180(14) -0.0134(13) C12 0.0571(19) 0.0221(14) 0.062(2) 0.0023(13) 0.0208(16) 0.0002(13) C13 0.0383(16) 0.0316(15) 0.0506(18) -0.0010(13) 0.0114(13) 0.0025(12) C14 0.0386(15) 0.0288(14) 0.0428(17) 0.0031(12) 0.0008(13) -0.0062(12) C15 0.0348(15) 0.0320(15) 0.0428(16) 0.0013(13) -0.0062(12) -0.0081(12) C16 0.0248(13) 0.0261(13) 0.0369(14) -0.0048(11) 0.0089(11) -0.0050(10) C17 0.0489(17) 0.0382(16) 0.0376(16) 0.0040(13) 0.0060(13) -0.0181(13) C18 0.0505(18) 0.0436(17) 0.0330(15) -0.0005(13) -0.0005(13) -0.0180(14) O1W 0.169(6) 0.114(5) 0.338(12) 0.000 0.132(7) 0.000 O2W 0.128(4) 0.070(3) 0.084(3) 0.000 0.026(3) 0.000 _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 O4 1.9451(19) 4 ? Co1 O1 1.958(2) . ? Co1 N1 2.054(2) . ? Co1 N2 2.060(2) 3_556 ? O1 C1 1.283(3) . ? O2 C1 1.233(3) . ? O3 C8 1.225(3) . ? O4 C8 1.268(3) . ? O4 Co1 1.9451(19) 4_556 ? N1 C18 1.330(4) . ? N1 C14 1.346(3) . ? N2 C11 1.342(4) . ? N2 C10 1.355(3) . ? N2 Co1 2.060(2) 3_556 ? C1 C2 1.496(4) . ? C2 C7 1.385(4) . ? C2 C3 1.393(4) . ? C3 C4 1.378(4) . ? C4 C5 1.400(4) . ? C5 C6 1.406(3) . ? C5 C8 1.508(4) . ? C6 C7 1.395(3) . ? C6 C9 1.487(3) . ? C9 C10 1.383(4) . ? C9 C13 1.387(4) . ? C11 C12 1.377(4) . ? C12 C13 1.383(4) . ? C14 C15 1.377(4) . ? C15 C16 1.383(4) . ? C16 C17 1.384(4) . ? C16 C16 1.495(5) 3_676 ? C17 C18 1.379(4) . ? 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 O4 Co1 O1 125.79(9) 4 . ? O4 Co1 N1 113.89(9) 4 . ? O1 Co1 N1 95.92(8) . . ? O4 Co1 N2 97.18(9) 4 3_556 ? O1 Co1 N2 113.78(9) . 3_556 ? N1 Co1 N2 110.69(9) . 3_556 ? C1 O1 Co1 109.98(17) . . ? C8 O4 Co1 118.58(18) . 4_556 ? C18 N1 C14 116.6(2) . . ? C18 N1 Co1 125.32(18) . . ? C14 N1 Co1 118.06(18) . . ? C11 N2 C10 117.5(2) . . ? C11 N2 Co1 124.30(18) . 3_556 ? C10 N2 Co1 117.26(18) . 3_556 ? O2 C1 O1 122.7(3) . . ? O2 C1 C2 120.5(2) . . ? O1 C1 C2 116.7(2) . . ? C7 C2 C3 119.2(2) . . ? C7 C2 C1 119.3(2) . . ? C3 C2 C1 121.5(2) . . ? C4 C3 C2 119.7(2) . . ? C3 C4 C5 121.5(2) . . ? C4 C5 C6 119.0(2) . . ? C4 C5 C8 117.8(2) . . ? C6 C5 C8 123.0(2) . . ? C7 C6 C5 118.5(2) . . ? C7 C6 C9 119.1(2) . . ? C5 C6 C9 122.4(2) . . ? C2 C7 C6 122.0(2) . . ? O3 C8 O4 123.7(3) . . ? O3 C8 C5 120.0(3) . . ? O4 C8 C5 116.1(2) . . ? C10 C9 C13 117.5(2) . . ? C10 C9 C6 118.7(2) . . ? C13 C9 C6 123.9(2) . . ? N2 C10 C9 123.6(2) . . ? N2 C11 C12 122.6(3) . . ? C11 C12 C13 119.2(3) . . ? C12 C13 C9 119.6(3) . . ? N1 C14 C15 123.1(3) . . ? C14 C15 C16 120.3(3) . . ? C15 C16 C17 116.3(2) . . ? C15 C16 C16 122.0(3) . 3_676 ? C17 C16 C16 121.7(3) . 3_676 ? C18 C17 C16 120.3(3) . . ? N1 C18 C17 123.4(3) . . ? 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 O4 Co1 O1 C1 -52.5(2) 4 . . . ? N1 Co1 O1 C1 -177.74(18) . . . . ? N2 Co1 O1 C1 66.5(2) 3_556 . . . ? O4 Co1 N1 C18 42.4(3) 4 . . . ? O1 Co1 N1 C18 176.0(2) . . . . ? N2 Co1 N1 C18 -65.8(2) 3_556 . . . ? O4 Co1 N1 C14 -135.7(2) 4 . . . ? O1 Co1 N1 C14 -2.2(2) . . . . ? N2 Co1 N1 C14 116.0(2) 3_556 . . . ? Co1 O1 C1 O2 5.9(3) . . . . ? Co1 O1 C1 C2 -173.40(17) . . . . ? O2 C1 C2 C7 -10.5(4) . . . . ? O1 C1 C2 C7 168.8(2) . . . . ? O2 C1 C2 C3 171.2(3) . . . . ? O1 C1 C2 C3 -9.5(4) . . . . ? C7 C2 C3 C4 -0.3(4) . . . . ? C1 C2 C3 C4 178.0(2) . . . . ? C2 C3 C4 C5 -2.2(4) . . . . ? C3 C4 C5 C6 3.2(4) . . . . ? C3 C4 C5 C8 -171.3(3) . . . . ? C4 C5 C6 C7 -1.6(4) . . . . ? C8 C5 C6 C7 172.6(2) . . . . ? C4 C5 C6 C9 179.4(2) . . . . ? C8 C5 C6 C9 -6.4(4) . . . . ? C3 C2 C7 C6 1.9(4) . . . . ? C1 C2 C7 C6 -176.5(2) . . . . ? C5 C6 C7 C2 -0.9(4) . . . . ? C9 C6 C7 C2 178.1(2) . . . . ? Co1 O4 C8 O3 6.0(4) 4_556 . . . ? Co1 O4 C8 C5 -170.00(17) 4_556 . . . ? C4 C5 C8 O3 -43.5(4) . . . . ? C6 C5 C8 O3 142.2(3) . . . . ? C4 C5 C8 O4 132.7(3) . . . . ? C6 C5 C8 O4 -41.6(4) . . . . ? C7 C6 C9 C10 -51.2(3) . . . . ? C5 C6 C9 C10 127.8(3) . . . . ? C7 C6 C9 C13 129.3(3) . . . . ? C5 C6 C9 C13 -51.7(4) . . . . ? C11 N2 C10 C9 -0.6(4) . . . . ? Co1 N2 C10 C9 168.9(2) 3_556 . . . ? C13 C9 C10 N2 1.1(4) . . . . ? C6 C9 C10 N2 -178.4(2) . . . . ? C10 N2 C11 C12 -0.4(4) . . . . ? Co1 N2 C11 C12 -169.1(2) 3_556 . . . ? N2 C11 C12 C13 0.9(5) . . . . ? C11 C12 C13 C9 -0.3(4) . . . . ? C10 C9 C13 C12 -0.6(4) . . . . ? C6 C9 C13 C12 178.9(3) . . . . ? C18 N1 C14 C15 0.7(4) . . . . ? Co1 N1 C14 C15 179.0(2) . . . . ? N1 C14 C15 C16 1.2(4) . . . . ? C14 C15 C16 C17 -2.2(4) . . . . ? C14 C15 C16 C16 176.8(3) . . . 3_676 ? C15 C16 C17 C18 1.4(4) . . . . ? C16 C16 C17 C18 -177.6(3) 3_676 . . . ? C14 N1 C18 C17 -1.5(4) . . . . ? Co1 N1 C18 C17 -179.7(2) . . . . ? C16 C17 C18 N1 0.4(5) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.466 _refine_diff_density_min -0.468 _refine_diff_density_rms 0.057 # Attachment 'web_deposit_cif_file_1_BoLiu_1318311692.2.cif' data_Complex_2 _database_code_depnum_ccdc_archive 'CCDC 848095' #TrackingRef 'web_deposit_cif_file_1_BoLiu_1318311692.2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum C18H17CoN2O7 _chemical_formula_weight 432.23 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' Co Co 0.3494 0.9721 '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' _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 17.795(2) _cell_length_b 14.8776(19) _cell_length_c 16.052(2) _cell_angle_alpha 90.00 _cell_angle_beta 109.140(2) _cell_angle_gamma 90.00 _cell_volume 4014.8(8) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1388 _cell_measurement_theta_min 2.493 _cell_measurement_theta_max 21.492 _exptl_crystal_description rod _exptl_crystal_colour red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.417 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1744 _exptl_absorpt_coefficient_mu 0.895 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8555 _exptl_absorpt_correction_T_max 0.8849 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10042 _diffrn_reflns_av_R_equivalents 0.0499 _diffrn_reflns_av_sigmaI/netI 0.0604 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 25.09 _reflns_number_total 3578 _reflns_number_gt 2664 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1116P)^2^+7.2055P] 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 3578 _refine_ls_number_parameters 253 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0793 _refine_ls_R_factor_gt 0.0611 _refine_ls_wR_factor_ref 0.1984 _refine_ls_wR_factor_gt 0.1845 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.087 _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 -0.13285(4) 0.40671(4) -0.04604(4) 0.0226(3) Uani 1 1 d . . . N1 N -0.1689(2) 0.5401(3) -0.0323(3) 0.0269(9) Uani 1 1 d . . . N2 N 0.1983(2) 0.3637(3) 0.4615(3) 0.0287(9) Uani 1 1 d . . . O1 O -0.0576(2) 0.2880(2) -0.0251(2) 0.0347(9) Uani 1 1 d . . . O2 O -0.02335(19) 0.4030(2) 0.0645(2) 0.0293(8) Uani 1 1 d . . . O3 O 0.2941(3) 0.0706(3) 0.2315(3) 0.0557(13) Uani 1 1 d . . . O4 O 0.27163(19) 0.1264(2) 0.3502(2) 0.0291(8) Uani 1 1 d . . . C1 C -0.0107(3) 0.3236(3) 0.0424(3) 0.0266(11) Uani 1 1 d . . . C2 C 0.0595(3) 0.2721(3) 0.1000(3) 0.0266(11) Uani 1 1 d . . . C3 C 0.0840(3) 0.1923(3) 0.0710(3) 0.0301(11) Uani 1 1 d . . . H3 H 0.0564 0.1700 0.0152 0.036 Uiso 1 1 calc R . . C4 C 0.1490(3) 0.1467(3) 0.1252(3) 0.0298(11) Uani 1 1 d . . . H4 H 0.1659 0.0945 0.1049 0.036 Uiso 1 1 calc R . . C5 C 0.1900(3) 0.1774(3) 0.2103(3) 0.0248(10) Uani 1 1 d . . . C6 C 0.1664(3) 0.2574(3) 0.2402(3) 0.0246(10) Uani 1 1 d . . . C7 C 0.1010(3) 0.3038(3) 0.1839(3) 0.0259(11) Uani 1 1 d . . . H7 H 0.0848 0.3572 0.2031 0.031 Uiso 1 1 calc R . . C8 C 0.2587(3) 0.1204(3) 0.2681(3) 0.0292(11) Uani 1 1 d . . . C9 C 0.2090(3) 0.3006(3) 0.3273(3) 0.0243(10) Uani 1 1 d . . . C10 C 0.1673(3) 0.3209(3) 0.3842(3) 0.0292(11) Uani 1 1 d . . . H10 H 0.1142 0.3037 0.3676 0.035 Uiso 1 1 calc R . . C11 C 0.2758(3) 0.3865(4) 0.4841(4) 0.0341(12) Uani 1 1 d . . . H11 H 0.2997 0.4146 0.5381 0.041 Uiso 1 1 calc R . . C12 C 0.3203(3) 0.3699(4) 0.4314(4) 0.0387(13) Uani 1 1 d . . . H12 H 0.3732 0.3883 0.4489 0.046 Uiso 1 1 calc R . . C13 C 0.2874(3) 0.3260(4) 0.3523(4) 0.0355(13) Uani 1 1 d . . . H13 H 0.3178 0.3138 0.3163 0.043 Uiso 1 1 calc R . . C14 C -0.1442(3) 0.5828(3) 0.0450(4) 0.0388(13) Uani 1 1 d . . . H14 H -0.1048 0.5559 0.0915 0.047 Uiso 1 1 calc R . . C15 C -0.1737(3) 0.6641(4) 0.0598(4) 0.0416(14) Uani 1 1 d . . . H15 H -0.1537 0.6912 0.1149 0.050 Uiso 1 1 calc R . . C16 C -0.2326(3) 0.7057(3) -0.0065(3) 0.0270(11) Uani 1 1 d . . . C17 C -0.2588(3) 0.6615(3) -0.0868(3) 0.0362(13) Uani 1 1 d . . . H17 H -0.2994 0.6862 -0.1336 0.043 Uiso 1 1 calc R . . C18 C -0.2251(3) 0.5815(3) -0.0972(4) 0.0380(13) Uani 1 1 d . . . H18 H -0.2423 0.5544 -0.1525 0.046 Uiso 1 1 calc R . . O1W O -0.0706(2) 0.4488(2) -0.1327(2) 0.0341(8) Uani 1 1 d D . . H1WB H -0.0439 0.4962 -0.1129 0.041 Uiso 1 1 d RD . . H1WC H -0.1034 0.4602 -0.1836 0.041 Uiso 1 1 d RD . . O2W O 0.5381(7) 0.5104(7) 0.7876(9) 0.253(7) Uani 1 1 d . . . O3W O 0.9433(5) 0.2459(6) 0.7902(5) 0.144(3) Uani 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 0.0209(4) 0.0197(4) 0.0226(4) -0.0002(2) 0.0008(3) 0.0011(2) N1 0.029(2) 0.020(2) 0.029(2) 0.0023(17) 0.0052(18) 0.0034(17) N2 0.027(2) 0.029(2) 0.026(2) -0.0034(17) 0.0025(18) 0.0003(18) O1 0.0279(19) 0.031(2) 0.033(2) -0.0004(15) -0.0058(16) 0.0020(15) O2 0.0230(17) 0.026(2) 0.0322(19) -0.0018(14) -0.0005(15) 0.0043(14) O3 0.056(3) 0.076(3) 0.030(2) 0.001(2) 0.007(2) 0.044(2) O4 0.0284(18) 0.034(2) 0.0201(17) 0.0035(14) 0.0017(14) 0.0065(15) C1 0.019(2) 0.031(3) 0.026(3) 0.005(2) 0.003(2) -0.003(2) C2 0.020(2) 0.031(3) 0.026(3) 0.005(2) 0.004(2) 0.003(2) C3 0.025(3) 0.036(3) 0.024(3) 0.000(2) 0.000(2) 0.001(2) C4 0.031(3) 0.028(3) 0.027(3) -0.001(2) 0.007(2) 0.008(2) C5 0.023(2) 0.026(3) 0.023(2) 0.0051(19) 0.003(2) 0.003(2) C6 0.024(2) 0.029(3) 0.020(2) 0.0007(19) 0.008(2) 0.003(2) C7 0.024(3) 0.024(3) 0.026(3) 0.0010(19) 0.005(2) 0.006(2) C8 0.026(3) 0.027(3) 0.030(3) 0.001(2) 0.003(2) 0.002(2) C9 0.023(2) 0.022(3) 0.024(2) 0.0008(19) 0.002(2) 0.0043(19) C10 0.022(2) 0.032(3) 0.029(3) -0.003(2) 0.002(2) 0.001(2) C11 0.029(3) 0.036(3) 0.032(3) -0.010(2) 0.003(2) 0.000(2) C12 0.023(3) 0.045(3) 0.045(3) -0.013(3) 0.006(2) -0.007(2) C13 0.030(3) 0.039(3) 0.038(3) -0.003(2) 0.012(2) 0.004(2) C14 0.041(3) 0.029(3) 0.037(3) -0.001(2) 0.001(3) 0.009(2) C15 0.047(3) 0.035(3) 0.036(3) -0.009(2) 0.005(3) 0.016(3) C16 0.030(3) 0.021(3) 0.032(3) 0.001(2) 0.013(2) 0.002(2) C17 0.046(3) 0.025(3) 0.031(3) 0.000(2) 0.003(2) 0.011(2) C18 0.048(3) 0.026(3) 0.033(3) -0.004(2) 0.004(3) 0.002(2) O1W 0.0288(19) 0.036(2) 0.034(2) -0.0047(16) 0.0069(16) -0.0065(16) O2W 0.191(12) 0.148(10) 0.310(18) 0.060(9) -0.065(10) -0.040(7) O3W 0.166(7) 0.159(7) 0.155(7) -0.073(6) 0.119(6) -0.055(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O4 2.013(3) 8_455 ? Co1 N1 2.119(4) . ? Co1 O1W 2.138(3) . ? Co1 N2 2.155(4) 2 ? Co1 O2 2.164(3) . ? Co1 O1 2.176(4) . ? N1 C18 1.335(7) . ? N1 C14 1.335(6) . ? N2 C10 1.342(6) . ? N2 C11 1.348(6) . ? N2 Co1 2.155(4) 2 ? O1 C1 1.248(6) . ? O2 C1 1.275(6) . ? O3 C8 1.238(6) . ? O4 C8 1.264(6) . ? O4 Co1 2.013(3) 8_556 ? C1 C2 1.499(6) . ? C2 C7 1.389(7) . ? C2 C3 1.395(7) . ? C3 C4 1.376(7) . ? C3 H3 0.9300 . ? C4 C5 1.398(7) . ? C4 H4 0.9300 . ? C5 C6 1.398(7) . ? C5 C8 1.527(6) . ? C6 C7 1.400(6) . ? C6 C9 1.499(6) . ? C7 H7 0.9300 . ? C9 C13 1.372(7) . ? C9 C10 1.385(7) . ? C10 H10 0.9300 . ? C11 C12 1.358(7) . ? C11 H11 0.9300 . ? C12 C13 1.377(7) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C15 1.369(7) . ? C14 H14 0.9300 . ? C15 C16 1.373(7) . ? C15 H15 0.9300 . ? C16 C17 1.385(7) . ? C16 C16 1.499(9) 7_465 ? C17 C18 1.368(7) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? O1W H1WB 0.8500 . ? O1W H1WC 0.8501 . ? O2W O2W 1.491(19) 2_656 ? 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 O4 Co1 N1 96.46(15) 8_455 . ? O4 Co1 O1W 90.58(13) 8_455 . ? N1 Co1 O1W 91.87(15) . . ? O4 Co1 N2 87.96(14) 8_455 2 ? N1 Co1 N2 88.13(16) . 2 ? O1W Co1 N2 178.53(14) . 2 ? O4 Co1 O2 164.12(14) 8_455 . ? N1 Co1 O2 99.24(14) . . ? O1W Co1 O2 91.24(13) . . ? N2 Co1 O2 90.20(14) 2 . ? O4 Co1 O1 103.86(13) 8_455 . ? N1 Co1 O1 159.46(14) . . ? O1W Co1 O1 85.08(14) . . ? N2 Co1 O1 95.42(15) 2 . ? O2 Co1 O1 60.61(12) . . ? C18 N1 C14 116.1(4) . . ? C18 N1 Co1 121.7(3) . . ? C14 N1 Co1 121.6(3) . . ? C10 N2 C11 116.2(4) . . ? C10 N2 Co1 125.4(3) . 2 ? C11 N2 Co1 118.2(3) . 2 ? C1 O1 Co1 89.5(3) . . ? C1 O2 Co1 89.4(3) . . ? C8 O4 Co1 131.4(3) . 8_556 ? O1 C1 O2 120.4(4) . . ? O1 C1 C2 120.2(5) . . ? O2 C1 C2 119.4(4) . . ? C7 C2 C3 119.3(4) . . ? C7 C2 C1 119.6(4) . . ? C3 C2 C1 121.1(4) . . ? C4 C3 C2 119.8(5) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C3 C4 C5 121.2(5) . . ? C3 C4 H4 119.4 . . ? C5 C4 H4 119.4 . . ? C4 C5 C6 119.6(4) . . ? C4 C5 C8 118.0(4) . . ? C6 C5 C8 122.4(4) . . ? C5 C6 C7 118.5(4) . . ? C5 C6 C9 124.6(4) . . ? C7 C6 C9 116.8(4) . . ? C2 C7 C6 121.6(4) . . ? C2 C7 H7 119.2 . . ? C6 C7 H7 119.2 . . ? O3 C8 O4 126.1(5) . . ? O3 C8 C5 118.4(4) . . ? O4 C8 C5 115.5(4) . . ? C13 C9 C10 117.5(5) . . ? C13 C9 C6 123.0(4) . . ? C10 C9 C6 119.4(4) . . ? N2 C10 C9 124.5(4) . . ? N2 C10 H10 117.8 . . ? C9 C10 H10 117.8 . . ? N2 C11 C12 122.7(5) . . ? N2 C11 H11 118.6 . . ? C12 C11 H11 118.6 . . ? C11 C12 C13 120.2(5) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C9 C13 C12 118.9(5) . . ? C9 C13 H13 120.6 . . ? C12 C13 H13 120.6 . . ? N1 C14 C15 123.6(5) . . ? N1 C14 H14 118.2 . . ? C15 C14 H14 118.2 . . ? C14 C15 C16 120.2(5) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C15 C16 C17 116.5(5) . . ? C15 C16 C16 122.3(6) . 7_465 ? C17 C16 C16 121.3(6) . 7_465 ? C18 C17 C16 120.0(5) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? N1 C18 C17 123.5(5) . . ? N1 C18 H18 118.2 . . ? C17 C18 H18 118.2 . . ? Co1 O1W H1WB 110.1 . . ? Co1 O1W H1WC 110.1 . . ? H1WB O1W H1WC 108.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.09 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.248 _refine_diff_density_min -0.373 _refine_diff_density_rms 0.133