# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'George Psomas' _publ_contact_author_email GEPSOMAS@CHEM.AUTH.GR _publ_section_title ; Biological evaluation of non-steroidal anti-inflammatory drugs-cobalt(II) complexes ; loop_ _publ_author_name 'George Psomas' 'Filitsa Dimiza' 'Dimitris Kessissoglou' 'Athanasios N. Papadopoulos' 'Vassilis Psycharis' ; C.Raptopoulou ; 'Vassilis Tangoulis' # Attachment 'CCDC-759764.txt' data_ps41 _database_code_depnum_ccdc_archive 'CCDC 759764' #TrackingRef 'CCDC-759764.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H44 Co N4 O6' _chemical_formula_weight 759.74 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 orthorhombic _symmetry_space_group_name_H-M Ic2a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, y+1/2, -z' '-x, y+1/2, z' '-x, y, -z' 'x+1/2, y+1/2, z+1/2' 'x+1/2, y+1, -z+1/2' '-x+1/2, y+1, z+1/2' '-x+1/2, y+1/2, -z+1/2' _cell_length_a 7.21870(10) _cell_length_b 17.6361(3) _cell_length_c 29.6060(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3769.13(10) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 18892 _cell_measurement_theta_min 6.62 _cell_measurement_theta_max 71.80 _exptl_crystal_description parall _exptl_crystal_colour pink _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.339 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1596 _exptl_absorpt_coefficient_mu 4.003 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.726 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'CrystalClear, Rigaku MSC, 2005' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS SPIDER IPDS' _diffrn_measurement_method '\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20358 _diffrn_reflns_av_R_equivalents 0.0399 _diffrn_reflns_av_sigmaI/netI 0.0509 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 7.27 _diffrn_reflns_theta_max 62.99 _reflns_number_total 2940 _reflns_number_gt 2295 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Rigaku MSC, 2005' _computing_cell_refinement 'CrystalClear, Rigaku MSC, 2005' _computing_data_reduction 'CrystalClear, Rigaku MSC, 2005' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0227P)^2^+1.2187P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.017(5) _refine_ls_number_reflns 2940 _refine_ls_number_parameters 295 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0566 _refine_ls_R_factor_gt 0.0351 _refine_ls_wR_factor_ref 0.0818 _refine_ls_wR_factor_gt 0.0689 _refine_ls_goodness_of_fit_ref 1.125 _refine_ls_restrained_S_all 1.124 _refine_ls_shift/su_max 0.002 _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 Co Co 0.0000 0.35132(5) 0.0000 0.0519(3) Uani 1 2 d S . . O1 O 0.3276(4) 0.26367(15) 0.06169(8) 0.0778(9) Uani 1 1 d . . . O2 O 0.1118(4) 0.35171(15) 0.06416(6) 0.0599(6) Uani 1 1 d . . . N1 N 0.0817(5) 0.43950(18) 0.13522(10) 0.0657(11) Uani 1 1 d . . . C1 C 0.2422(6) 0.31484(17) 0.08176(10) 0.0435(9) Uani 1 1 d . . . C2 C 0.2955(4) 0.33367(16) 0.12920(9) 0.0375(8) Uani 1 1 d . . . C3 C 0.4287(5) 0.2886(2) 0.15039(11) 0.0465(9) Uani 1 1 d . . . C4 C 0.4835(6) 0.3006(2) 0.19428(12) 0.0490(9) Uani 1 1 d . . . C5 C 0.3996(5) 0.3590(2) 0.21833(11) 0.0447(9) Uani 1 1 d . . . C6 C 0.2710(5) 0.4047(2) 0.19874(11) 0.0455(10) Uani 1 1 d . . . C7 C 0.2132(5) 0.39320(17) 0.15394(10) 0.0394(8) Uani 1 1 d . . . C8 C -0.0235(6) 0.49594(19) 0.15936(10) 0.0452(9) Uani 1 1 d . . . C9 C -0.1955(6) 0.4763(2) 0.17603(13) 0.0551(11) Uani 1 1 d . . . C10 C -0.3028(7) 0.5312(2) 0.19850(14) 0.0590(11) Uani 1 1 d . . . C11 C -0.2338(6) 0.6032(2) 0.20256(12) 0.0510(9) Uani 1 1 d . . . C12 C -0.0619(5) 0.62340(17) 0.18586(10) 0.0429(9) Uani 1 1 d . . . C13 C 0.0476(5) 0.56845(18) 0.16426(11) 0.0446(9) Uani 1 1 d . . . C14 C 0.2354(5) 0.5877(2) 0.14716(15) 0.0752(13) Uani 1 1 d . . . H14A H 0.2538 0.6427 0.1488 0.098 Uiso 1 1 calc R . . H14B H 0.2471 0.5709 0.1157 0.098 Uiso 1 1 calc R . . H14C H 0.3290 0.5622 0.1657 0.098 Uiso 1 1 calc R . . C15 C 0.0052(6) 0.70418(17) 0.19076(14) 0.0641(12) Uani 1 1 d . . . H15A H 0.1127 0.7054 0.2110 0.083 Uiso 1 1 calc R . . H15B H -0.0942 0.7355 0.2035 0.083 Uiso 1 1 calc R . . H15C H 0.0405 0.7240 0.1611 0.083 Uiso 1 1 calc R . . N21 N 0.1616(5) 0.44520(15) -0.02057(9) 0.0489(8) Uani 1 1 d . . . C21 C 0.0870(5) 0.51357(19) -0.01374(11) 0.0511(10) Uani 1 1 d . . . C22 C 0.1682(9) 0.5781(3) -0.03182(19) 0.0785(16) Uani 1 1 d . . . C23 C 0.3285(9) 0.5711(3) -0.05721(19) 0.0924(18) Uani 1 1 d . . . C24 C 0.4076(8) 0.5026(3) -0.06300(17) 0.0820(14) Uani 1 1 d . . . C25 C 0.3194(7) 0.4399(3) -0.04418(14) 0.0669(13) Uani 1 1 d . . . O31 O 0.1917(7) 0.26869(19) -0.01698(10) 0.1235(19) Uani 1 1 d . . . C31 C 0.2261(6) 0.2269(2) -0.05521(13) 0.0720(13) Uani 1 1 d . . . H31A H 0.1661 0.1773 -0.0526 0.094 Uiso 1 1 calc R . . H31B H 0.3601 0.2200 -0.0587 0.094 Uiso 1 1 calc R . . H31C H 0.1768 0.2536 -0.0816 0.094 Uiso 1 1 calc R . . H3O H 0.259(6) 0.264(2) 0.0051(13) 0.080(15) Uiso 1 1 d . . . H1N H 0.043(5) 0.4265(18) 0.1097(12) 0.059(12) Uiso 1 1 d . . . H3 H 0.482(5) 0.248(2) 0.1328(12) 0.065(11) Uiso 1 1 d . . . H4 H 0.578(5) 0.269(2) 0.2100(12) 0.079(13) Uiso 1 1 d . . . H5 H 0.433(4) 0.3644(17) 0.2467(10) 0.046(9) Uiso 1 1 d . . . H6 H 0.222(4) 0.4430(19) 0.2156(10) 0.047(10) Uiso 1 1 d . . . H9 H -0.238(5) 0.4273(18) 0.1716(11) 0.047(10) Uiso 1 1 d . . . H10 H -0.416(6) 0.523(3) 0.2121(16) 0.12(2) Uiso 1 1 d . . . H11 H -0.306(6) 0.639(2) 0.2208(15) 0.096(15) Uiso 1 1 d . . . H22 H 0.118(6) 0.617(2) -0.0256(15) 0.082(16) Uiso 1 1 d . . . H23 H 0.397(7) 0.615(3) -0.0676(16) 0.120(19) Uiso 1 1 d . . . H24 H 0.545(8) 0.488(3) -0.0788(18) 0.16(3) Uiso 1 1 d . . . H25 H 0.357(6) 0.395(2) -0.0497(14) 0.093(17) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co 0.0923(6) 0.0356(4) 0.0278(3) 0.000 -0.0056(4) 0.000 O1 0.087(2) 0.088(2) 0.0585(16) -0.0332(15) -0.0221(15) 0.0455(17) O2 0.0909(19) 0.0573(13) 0.0315(11) -0.0072(12) -0.0117(12) 0.0299(17) N1 0.100(3) 0.0582(19) 0.0388(17) -0.0183(15) -0.0192(19) 0.041(2) C1 0.059(3) 0.0338(17) 0.0374(18) -0.0008(15) 0.0049(19) 0.0017(17) C2 0.046(2) 0.0345(16) 0.0326(15) 0.0001(13) 0.0025(15) 0.0024(15) C3 0.050(3) 0.0458(19) 0.044(2) -0.0018(17) 0.0054(18) 0.0066(19) C4 0.046(3) 0.057(2) 0.044(2) 0.0079(17) -0.0017(18) 0.011(2) C5 0.046(2) 0.054(2) 0.0337(17) 0.0007(18) -0.0058(16) -0.002(2) C6 0.062(3) 0.0394(19) 0.0352(18) -0.0028(15) 0.0053(18) 0.0026(19) C7 0.050(3) 0.0327(16) 0.0351(17) 0.0016(14) -0.0075(16) 0.0041(16) C8 0.065(3) 0.0412(19) 0.0299(17) -0.0015(14) -0.0069(18) 0.0114(19) C9 0.065(3) 0.042(2) 0.058(2) 0.0037(19) -0.016(2) -0.005(2) C10 0.053(3) 0.063(3) 0.061(3) 0.008(2) -0.001(2) -0.004(2) C11 0.058(3) 0.050(2) 0.0453(19) -0.0008(18) 0.001(2) 0.012(2) C12 0.052(3) 0.042(2) 0.0346(18) -0.0003(14) -0.0035(18) 0.0061(17) C13 0.055(3) 0.0438(19) 0.0354(18) 0.0030(15) -0.0020(18) 0.0053(18) C14 0.067(3) 0.068(3) 0.090(3) 0.032(2) 0.021(2) 0.009(2) C15 0.077(3) 0.044(2) 0.071(3) -0.0016(19) -0.019(2) 0.002(2) N21 0.066(3) 0.0420(16) 0.0391(16) -0.0053(14) -0.0065(17) -0.0008(17) C21 0.061(3) 0.0432(19) 0.049(2) 0.0030(16) -0.0103(18) -0.0075(18) C22 0.094(5) 0.045(3) 0.096(4) 0.009(3) -0.005(3) -0.011(3) C23 0.089(5) 0.089(4) 0.099(4) 0.023(3) 0.002(3) -0.035(4) C24 0.079(4) 0.081(4) 0.086(3) 0.000(3) 0.003(3) -0.022(3) C25 0.080(4) 0.062(3) 0.059(3) -0.008(2) -0.002(3) -0.006(3) O31 0.234(5) 0.096(3) 0.0404(17) -0.0266(17) -0.028(2) 0.094(3) C31 0.091(4) 0.072(3) 0.053(2) -0.024(2) 0.012(2) -0.002(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 Co O2 2.064(2) . ? Co O2 2.064(2) 4 ? Co O31 2.072(3) 4 ? Co O31 2.072(3) . ? Co N21 2.115(3) . ? Co N21 2.115(3) 4 ? O1 C1 1.244(4) . ? O2 C1 1.257(4) . ? N1 C7 1.370(4) . ? N1 C8 1.442(4) . ? N1 H1N 0.84(4) . ? C1 C2 1.494(4) . ? C2 C3 1.396(4) . ? C2 C7 1.411(4) . ? C3 C4 1.375(5) . ? C3 H3 0.97(4) . ? C4 C5 1.392(5) . ? C4 H4 0.99(4) . ? C5 C6 1.359(5) . ? C5 H5 0.88(3) . ? C6 C7 1.405(4) . ? C6 H6 0.91(3) . ? C8 C9 1.380(5) . ? C8 C13 1.386(4) . ? C9 C10 1.407(6) . ? C9 H9 0.93(3) . ? C10 C11 1.369(5) . ? C10 H10 0.92(5) . ? C11 C12 1.382(5) . ? C11 H11 0.98(4) . ? C12 C13 1.405(4) . ? C12 C15 1.512(4) . ? C13 C14 1.486(4) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? N21 C21 1.336(4) . ? N21 C25 1.340(5) . ? C21 C22 1.388(5) . ? C21 C21 1.497(7) 4 ? C22 C23 1.385(7) . ? C22 H22 0.80(4) . ? C23 C24 1.348(7) . ? C23 H23 0.96(5) . ? C24 C25 1.393(6) . ? C24 H24 1.13(6) . ? C25 H25 0.85(4) . ? O31 C31 1.373(4) . ? O31 H3O 0.82(4) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? 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 Co O2 179.62(16) . 4 ? O2 Co O31 92.31(12) . 4 ? O2 Co O31 87.96(12) 4 4 ? O2 Co O31 87.96(12) . . ? O2 Co O31 92.31(12) 4 . ? O31 Co O31 90.6(3) 4 . ? O2 Co N21 92.68(11) . . ? O2 Co N21 87.02(10) 4 . ? O31 Co N21 171.50(18) 4 . ? O31 Co N21 96.45(15) . . ? O2 Co N21 87.02(10) . 4 ? O2 Co N21 92.68(11) 4 4 ? O31 Co N21 96.45(15) 4 4 ? O31 Co N21 171.50(18) . 4 ? N21 Co N21 76.96(18) . 4 ? C1 O2 Co 132.3(2) . . ? C7 N1 C8 125.2(3) . . ? C7 N1 H1N 116(2) . . ? C8 N1 H1N 117(3) . . ? O1 C1 O2 123.3(3) . . ? O1 C1 C2 118.9(3) . . ? O2 C1 C2 117.9(3) . . ? C3 C2 C7 118.7(3) . . ? C3 C2 C1 118.2(3) . . ? C7 C2 C1 123.0(3) . . ? C4 C3 C2 122.4(3) . . ? C4 C3 H3 120(2) . . ? C2 C3 H3 117(2) . . ? C3 C4 C5 118.2(4) . . ? C3 C4 H4 124(2) . . ? C5 C4 H4 118(2) . . ? C6 C5 C4 121.2(3) . . ? C6 C5 H5 122(2) . . ? C4 C5 H5 117(2) . . ? C5 C6 C7 121.4(3) . . ? C5 C6 H6 118(2) . . ? C7 C6 H6 121(2) . . ? N1 C7 C6 120.1(3) . . ? N1 C7 C2 121.7(3) . . ? C6 C7 C2 118.2(3) . . ? C9 C8 C13 121.8(3) . . ? C9 C8 N1 118.5(3) . . ? C13 C8 N1 119.6(4) . . ? C8 C9 C10 119.4(4) . . ? C8 C9 H9 119(2) . . ? C10 C9 H9 122(2) . . ? C11 C10 C9 118.7(4) . . ? C11 C10 H10 115(3) . . ? C9 C10 H10 126(3) . . ? C10 C11 C12 122.3(4) . . ? C10 C11 H11 117(2) . . ? C12 C11 H11 121(2) . . ? C11 C12 C13 119.3(3) . . ? C11 C12 C15 119.8(3) . . ? C13 C12 C15 120.9(3) . . ? C8 C13 C12 118.4(3) . . ? C8 C13 C14 120.9(3) . . ? C12 C13 C14 120.7(3) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C21 N21 C25 119.0(4) . . ? C21 N21 Co 116.2(3) . . ? C25 N21 Co 124.3(3) . . ? N21 C21 C22 120.8(4) . . ? N21 C21 C21 114.9(2) . 4 ? C22 C21 C21 124.3(3) . 4 ? C23 C22 C21 119.3(5) . . ? C23 C22 H22 125(3) . . ? C21 C22 H22 115(3) . . ? C24 C23 C22 120.2(5) . . ? C24 C23 H23 117(3) . . ? C22 C23 H23 122(3) . . ? C23 C24 C25 117.9(6) . . ? C23 C24 H24 129(3) . . ? C25 C24 H24 112(3) . . ? N21 C25 C24 122.8(5) . . ? N21 C25 H25 116(3) . . ? C24 C25 H25 121(3) . . ? C31 O31 Co 134.3(3) . . ? C31 O31 H3O 119(3) . . ? Co O31 H3O 106(3) . . ? O31 C31 H31A 109.5 . . ? O31 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? O31 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 62.99 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.234 _refine_diff_density_min -0.229 _refine_diff_density_rms 0.043 # start Validation Reply Form _vrf_PLAT241_ps41 ; PROBLEM: Check High Ueq as Compared to Neighbors for O31 RESPONSE: There is no disorder or wrong atom type assignment, it is generated because of the small thermal motion of the neighboring atoms. ; # end Validation Reply Form # Attachment 'CCDC-759765.txt' data_psfd27 _database_code_depnum_ccdc_archive 'CCDC 759765' #TrackingRef 'CCDC-759765.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H52 Co N2 O10' _chemical_formula_weight 731.73 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.66020(10) _cell_length_b 7.88870(10) _cell_length_c 15.7633(3) _cell_angle_alpha 90.2790(10) _cell_angle_beta 99.2940(10) _cell_angle_gamma 92.7690(10) _cell_volume 938.88(2) _cell_formula_units_Z 1 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 12175 _cell_measurement_theta_min 6.92 _cell_measurement_theta_max 71.75 _exptl_crystal_description parall _exptl_crystal_colour pink _exptl_crystal_size_max 0.75 _exptl_crystal_size_mid 0.67 _exptl_crystal_size_min 0.31 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.294 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 389 _exptl_absorpt_coefficient_mu 4.053 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.724 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'CrystalClear, Rigaku MSC, 2005' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku, R-AXIS SPIDER IPDS' _diffrn_measurement_method '\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11946 _diffrn_reflns_av_R_equivalents 0.0294 _diffrn_reflns_av_sigmaI/netI 0.0280 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 6.92 _diffrn_reflns_theta_max 65.00 _reflns_number_total 2968 _reflns_number_gt 2743 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Rigaku MSC, 2005' _computing_cell_refinement 'CrystalClear, Rigaku MSC, 2005' _computing_data_reduction 'CrystalClear, Rigaku MSC, 2005' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0686P)^2^+0.8212P] 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 SHELXL _refine_ls_extinction_coef 0.0133(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2968 _refine_ls_number_parameters 270 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0550 _refine_ls_R_factor_gt 0.0523 _refine_ls_wR_factor_ref 0.1365 _refine_ls_wR_factor_gt 0.1344 _refine_ls_goodness_of_fit_ref 1.125 _refine_ls_restrained_S_all 1.125 _refine_ls_shift/su_max 0.002 _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 Co Co 0.0000 0.5000 0.0000 0.0272(3) Uani 1 2 d S . . O1 O 0.0386(3) 0.4615(3) 0.13075(12) 0.0317(5) Uani 1 1 d . . . O21 O 0.2365(5) 0.6469(7) 0.01182(19) 0.1052(18) Uani 1 1 d . . . H21O H 0.283(10) 0.667(10) -0.025(5) 0.137 Uiso 1 1 d . . . O22 O 0.1420(7) 0.2901(6) -0.01671(19) 0.123(2) Uani 1 1 d . . . H22O H 0.206(11) 0.300(11) 0.022(5) 0.160 Uiso 1 1 d . . . O2 O 0.2637(3) 0.2914(3) 0.14652(13) 0.0464(7) Uani 1 1 d . . . N N -0.0553(4) 0.6063(3) 0.26637(16) 0.0289(6) Uani 1 1 d . . . C1 C 0.1615(4) 0.3860(4) 0.17685(18) 0.0264(7) Uani 1 1 d . . . C2 C 0.1851(4) 0.4120(3) 0.27242(17) 0.0216(6) Uani 1 1 d . . . C3 C 0.3182(4) 0.3255(3) 0.32319(18) 0.0240(6) Uani 1 1 d . . . C4 C 0.3505(4) 0.3425(4) 0.41150(19) 0.0267(7) Uani 1 1 d . . . C5 C 0.2466(4) 0.4475(4) 0.45106(18) 0.0272(7) Uani 1 1 d . . . C6 C 0.1138(4) 0.5340(4) 0.40304(18) 0.0243(6) Uani 1 1 d . . . C7 C 0.0786(4) 0.5191(3) 0.31295(17) 0.0218(6) Uani 1 1 d . . . C8 C -0.1695(4) 0.7106(4) 0.30350(17) 0.0243(6) Uani 1 1 d . . . C9 C -0.3435(4) 0.6550(4) 0.30238(19) 0.0279(7) Uani 1 1 d . . . C10 C -0.4574(5) 0.7532(4) 0.3386(2) 0.0313(7) Uani 1 1 d . . . C11 C -0.3961(5) 0.9072(4) 0.3770(2) 0.0320(7) Uani 1 1 d . . . C12 C -0.2217(4) 0.9667(4) 0.3781(2) 0.0329(7) Uani 1 1 d . . . C13 C -0.1073(4) 0.8693(4) 0.3394(2) 0.0309(7) Uani 1 1 d . . . C14 C 0.0793(5) 0.9359(5) 0.3345(3) 0.0515(10) Uani 1 1 d . . . H14A H 0.1530 0.9280 0.3912 0.067 Uiso 1 1 calc R . . H14B H 0.0774 1.0547 0.3166 0.067 Uiso 1 1 calc R . . H14C H 0.1285 0.8681 0.2926 0.067 Uiso 1 1 calc R . . C15 C -0.1581(6) 1.1367(5) 0.4196(3) 0.0599(12) Uani 1 1 d . . . H15A H -0.1258 1.2147 0.3759 0.078 Uiso 1 1 calc R . . H15B H -0.0544 1.1219 0.4638 0.078 Uiso 1 1 calc R . . H15C H -0.2528 1.1836 0.4461 0.078 Uiso 1 1 calc R . . C21 C 0.3480(8) 0.7196(8) 0.0811(3) 0.091(2) Uani 1 1 d . . . H21A H 0.2859 0.7228 0.1308 0.118 Uiso 1 1 calc R . . H21B H 0.3845 0.8354 0.0670 0.118 Uiso 1 1 calc R . . H21C H 0.4528 0.6522 0.0950 0.118 Uiso 1 1 calc R . . C22 C 0.1371(8) 0.1593(6) -0.0682(3) 0.0752(15) Uani 1 1 d . . . H22A H 0.1647 0.0575 -0.0343 0.098 Uiso 1 1 calc R . . H22B H 0.2243 0.1786 -0.1068 0.098 Uiso 1 1 calc R . . H22C H 0.0184 0.1438 -0.1023 0.098 Uiso 1 1 calc R . . CM C 0.3082(7) 0.8137(6) -0.1857(3) 0.0673(13) Uani 1 1 d . . . HCMA H 0.1906 0.8366 -0.1727 0.088 Uiso 1 1 calc R . . HCMB H 0.2962 0.7640 -0.2436 0.088 Uiso 1 1 calc R . . HCMC H 0.3806 0.9200 -0.1828 0.088 Uiso 1 1 calc R . . OM O 0.3875(6) 0.7029(7) -0.1272(3) 0.1041(17) Uani 1 1 d . . . H1N H -0.084(5) 0.577(4) 0.217(2) 0.036(10) Uiso 1 1 d . . . HOM H 0.4613 0.676(6) -0.130(3) 0.056(16) Uiso 1 1 d . . . H3 H 0.387(4) 0.253(4) 0.296(2) 0.029(8) Uiso 1 1 d . . . H4 H 0.444(5) 0.281(4) 0.445(2) 0.038(9) Uiso 1 1 d . . . H5 H 0.266(4) 0.461(4) 0.513(2) 0.028(8) Uiso 1 1 d . . . H6 H 0.045(4) 0.598(4) 0.4276(19) 0.019(7) Uiso 1 1 d . . . H9 H -0.384(4) 0.545(4) 0.2765(19) 0.024(8) Uiso 1 1 d . . . H10 H -0.575(5) 0.714(4) 0.336(2) 0.034(9) Uiso 1 1 d . . . H11 H -0.475(5) 0.981(5) 0.402(2) 0.042(10) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co 0.0285(5) 0.0401(4) 0.0143(3) -0.0001(3) 0.0053(3) 0.0092(3) O1 0.0292(13) 0.0503(13) 0.0170(10) 0.0041(9) 0.0054(9) 0.0110(10) O21 0.074(3) 0.201(5) 0.0304(16) 0.013(2) 0.0015(16) -0.071(3) O22 0.207(5) 0.126(3) 0.0315(16) -0.0330(18) -0.033(2) 0.131(4) O2 0.0556(17) 0.0639(16) 0.0221(11) -0.0047(10) 0.0051(11) 0.0307(13) N 0.0278(16) 0.0421(14) 0.0178(12) 0.0007(11) 0.0040(11) 0.0114(12) C1 0.0241(18) 0.0355(15) 0.0205(14) 0.0011(12) 0.0063(13) 0.0021(13) C2 0.0194(17) 0.0270(14) 0.0184(13) 0.0029(10) 0.0037(12) -0.0026(11) C3 0.0234(18) 0.0258(14) 0.0235(14) 0.0011(11) 0.0056(13) 0.0020(12) C4 0.0239(18) 0.0312(15) 0.0236(14) 0.0042(12) -0.0006(13) 0.0028(13) C5 0.0308(19) 0.0325(15) 0.0177(14) 0.0002(11) 0.0033(13) -0.0034(13) C6 0.0242(18) 0.0282(14) 0.0217(14) -0.0010(11) 0.0074(13) 0.0022(13) C7 0.0200(17) 0.0260(13) 0.0200(13) 0.0036(11) 0.0057(12) -0.0018(12) C8 0.0244(18) 0.0292(14) 0.0197(13) 0.0063(11) 0.0039(12) 0.0054(12) C9 0.0251(19) 0.0278(15) 0.0299(15) 0.0004(12) 0.0020(13) -0.0003(13) C10 0.0199(19) 0.0354(16) 0.0390(17) 0.0037(13) 0.0064(15) -0.0008(14) C11 0.031(2) 0.0321(16) 0.0354(16) 0.0021(13) 0.0085(14) 0.0106(14) C12 0.028(2) 0.0254(15) 0.0433(18) -0.0001(13) -0.0008(15) 0.0035(13) C13 0.0236(19) 0.0287(15) 0.0400(17) 0.0070(13) 0.0039(14) -0.0003(13) C14 0.030(2) 0.0391(19) 0.085(3) 0.0068(19) 0.013(2) -0.0049(16) C15 0.050(3) 0.0352(19) 0.090(3) -0.017(2) -0.004(2) 0.0041(18) C21 0.070(4) 0.129(5) 0.060(3) 0.025(3) -0.019(3) -0.049(4) C22 0.115(4) 0.064(3) 0.046(2) -0.006(2) 0.003(3) 0.036(3) CM 0.073(3) 0.063(3) 0.074(3) 0.004(2) 0.031(3) 0.016(2) OM 0.059(2) 0.187(5) 0.080(3) 0.070(3) 0.039(2) 0.037(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co O1 2.0604(18) 2_565 ? Co O1 2.0604(18) . ? Co O22 2.063(3) 2_565 ? Co O22 2.063(3) . ? Co O21 2.084(3) . ? Co O21 2.084(3) 2_565 ? O1 C1 1.267(4) . ? O21 C21 1.377(6) . ? O21 H21O 0.74(7) . ? O22 C22 1.305(5) . ? O22 H22O 0.73(8) . ? O2 C1 1.254(4) . ? N C7 1.376(4) . ? N C8 1.420(4) . ? N H1N 0.81(4) . ? C1 C2 1.500(4) . ? C2 C3 1.398(4) . ? C2 C7 1.420(4) . ? C3 C4 1.379(4) . ? C3 H3 0.94(3) . ? C4 C5 1.388(4) . ? C4 H4 0.97(4) . ? C5 C6 1.377(4) . ? C5 H5 0.97(3) . ? C6 C7 1.405(4) . ? C6 H6 0.88(3) . ? C8 C9 1.381(4) . ? C8 C13 1.401(4) . ? C9 C10 1.381(4) . ? C9 H9 0.97(3) . ? C10 C11 1.382(5) . ? C10 H10 0.94(4) . ? C11 C12 1.392(5) . ? C11 H11 0.99(4) . ? C12 C13 1.401(4) . ? C12 C15 1.513(5) . ? C13 C14 1.513(5) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? CM OM 1.364(6) . ? CM HCMA 0.9800 . ? CM HCMB 0.9800 . ? CM HCMC 0.9800 . ? OM HOM 0.62(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co O1 180.00(12) 2_565 . ? O1 Co O22 90.16(11) 2_565 2_565 ? O1 Co O22 89.84(11) . 2_565 ? O1 Co O22 89.84(11) 2_565 . ? O1 Co O22 90.16(11) . . ? O22 Co O22 180.00(16) 2_565 . ? O1 Co O21 89.41(10) 2_565 . ? O1 Co O21 90.59(10) . . ? O22 Co O21 91.8(2) 2_565 . ? O22 Co O21 88.2(2) . . ? O1 Co O21 90.59(10) 2_565 2_565 ? O1 Co O21 89.41(10) . 2_565 ? O22 Co O21 88.2(2) 2_565 2_565 ? O22 Co O21 91.8(2) . 2_565 ? O21 Co O21 180.0 . 2_565 ? C1 O1 Co 128.86(17) . . ? C21 O21 Co 133.2(3) . . ? C21 O21 H21O 104(6) . . ? Co O21 H21O 123(6) . . ? C22 O22 Co 140.1(3) . . ? C22 O22 H22O 122(7) . . ? Co O22 H22O 98(7) . . ? C7 N C8 124.2(2) . . ? C7 N H1N 116(3) . . ? C8 N H1N 118(3) . . ? O2 C1 O1 123.3(3) . . ? O2 C1 C2 118.7(3) . . ? O1 C1 C2 118.0(2) . . ? C3 C2 C7 119.1(2) . . ? C3 C2 C1 117.8(2) . . ? C7 C2 C1 123.1(3) . . ? C4 C3 C2 121.9(3) . . ? C4 C3 H3 119(2) . . ? C2 C3 H3 119(2) . . ? C3 C4 C5 118.9(3) . . ? C3 C4 H4 120(2) . . ? C5 C4 H4 121(2) . . ? C6 C5 C4 120.7(3) . . ? C6 C5 H5 118.6(19) . . ? C4 C5 H5 120.7(19) . . ? C5 C6 C7 121.4(3) . . ? C5 C6 H6 121(2) . . ? C7 C6 H6 117(2) . . ? N C7 C6 120.4(3) . . ? N C7 C2 121.7(2) . . ? C6 C7 C2 117.9(3) . . ? C9 C8 C13 120.4(3) . . ? C9 C8 N 119.1(3) . . ? C13 C8 N 120.5(3) . . ? C8 C9 C10 120.5(3) . . ? C8 C9 H9 119.0(19) . . ? C10 C9 H9 120.6(19) . . ? C9 C10 C11 119.7(3) . . ? C9 C10 H10 119(2) . . ? C11 C10 H10 121(2) . . ? C10 C11 C12 120.8(3) . . ? C10 C11 H11 122(2) . . ? C12 C11 H11 117(2) . . ? C11 C12 C13 119.5(3) . . ? C11 C12 C15 119.9(3) . . ? C13 C12 C15 120.6(3) . . ? C8 C13 C12 119.0(3) . . ? C8 C13 C14 120.3(3) . . ? C12 C13 C14 120.6(3) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O21 C21 H21A 109.5 . . ? O21 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O21 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O22 C22 H22A 109.5 . . ? O22 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? O22 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? OM CM HCMA 109.5 . . ? OM CM HCMB 109.5 . . ? HCMA CM HCMB 109.5 . . ? OM CM HCMC 109.5 . . ? HCMA CM HCMC 109.5 . . ? HCMB CM HCMC 109.5 . . ? CM OM HOM 122(5) . . ? _diffrn_measured_fraction_theta_max 0.929 _diffrn_reflns_theta_full 65.00 _diffrn_measured_fraction_theta_full 0.929 _refine_diff_density_max 0.725 _refine_diff_density_min -0.673 _refine_diff_density_rms 0.059 # start Validation Reply Form _vrf_PLAT029_psfd27 ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.93 RESPONSE: This is a usual alert when the data are collected with Cu radiation for triclinic unit cells. No action taken. ; _vrf_PLAT222_psfd27 ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 8.42 Ratio RESPONSE: This is because hydrogen atoms were introduced at calculated positions as riding on bonded atoms and were refined with U equals 1.3 times the Ueq of their respective atom. ; _vrf_PLAT241_psfd27 ; PROBLEM: Check High Ueq as Compared to Neighbors for O22 RESPONSE: There is no disorder or wrong atom type assignement, it is generated because of the small thermal motion of the neighboring atoms. ; _vrf_PLAT242_psfd27 ; PROBLEM: Check Low Ueq as Compared to Neighbors for Co RESPONSE: There is no disorder or wrong atom type assignement, it is generated because of the large thermal motion of the neighboring atoms. ; # end Validation Reply Form