Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Ciani, Gianfranco' 'Banfi, Stefano' 'Carlucci, Lucia' 'Caruso, Enrico' 'Proserpio, D. M.' _publ_contact_author_name 'Prof Gianfranco Ciani' _publ_contact_author_address ; DCSSI universita' di Milano via venezian 21 milano 20133 ITALY ; _publ_contact_author_email 'DAVIDE@CSMTBO.MI.CNR.IT' _publ_section_title ; Using long bis(4-pyridyl) ligands designed for the self-assembly of coordination frameworks and architectures. ; data_1 _database_code_CSD 173813 _diffrn_measurement_domega 0.30 _diffrn_measurement_rtime 43 _chemical_formula_sum 'C56 H46 F6 N6 O17 S2 Zn' _chemical_formula_weight 1318.48 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 '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' #(#2) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.323(2) _cell_length_b 11.113(2) _cell_length_c 14.306(2) _cell_angle_alpha 93.260(10) _cell_angle_beta 93.420(10) _cell_angle_gamma 97.110(10) _cell_volume 1465.1(5) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 3. _cell_measurement_theta_max 29. _exptl_crystal_description column _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.494 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 676 _exptl_absorpt_coefficient_mu 0.585 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.90 _exptl_absorpt_correction_T_max 1.00 _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 SMART _diffrn_detector_type CCD_plate _diffrn_measurement_method omega-scan _diffrn_standards_decay_% 0 _diffrn_reflns_number 19777 _diffrn_reflns_av_R_equivalents 0.0353 _diffrn_reflns_av_sigmaI/netI 0.0498 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 29.64 _reflns_number_total 7249 _reflns_number_observed 5058 _reflns_observed_criterion >2sigma(I) _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SCHAKAL _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^)+(0.0572P)^2^+0.8882P] 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_number_reflns 7249 _refine_ls_number_parameters 475 _refine_ls_number_restraints 157 _refine_ls_R_factor_all 0.0940 _refine_ls_R_factor_obs 0.0587 _refine_ls_wR_factor_all 0.1396 _refine_ls_wR_factor_obs 0.1243 _refine_ls_goodness_of_fit_all 1.020 _refine_ls_restrained_S_all 1.083 _refine_ls_shift/su_max 0.034 _refine_ls_shift/su_mean 0.002 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 O3W O 0.4536(9) 0.4885(8) 0.0453(6) 0.126(3) Uiso 0.50 1 d P . . Zn Zn 0.0000 0.5000 0.0000 0.03762(15) Uani 1 2 d S . . O1W O 0.2096(2) 0.5909(2) -0.01095(15) 0.0555(6) Uani 1 1 d . . . H111 H 0.2768 0.6123 0.0316 0.117(18) Uiso 1 1 d R . . H112 H 0.2274 0.6365 -0.0558 0.075(12) Uiso 1 1 d R . . O2W O -0.0731(2) 0.67069(19) 0.02735(13) 0.0498(5) Uani 1 1 d . . . H211 H -0.0078 0.7288 0.0436 0.062(11) Uiso 1 1 d R . . H212 H -0.1459 0.6771 0.0592 0.060(11) Uiso 1 1 d R . . N11 N 0.1170(4) 0.8618(3) 0.1170(2) 0.0777(9) Uani 1 1 d . . . C11 C 0.1481(5) 0.8173(4) 0.1983(3) 0.0847(13) Uani 1 1 d . . . H11 H 0.1200 0.7350 0.2041 0.102 Uiso 1 1 calc R . . C12 C 0.2194(4) 0.8842(3) 0.2754(2) 0.0646(9) Uani 1 1 d . . . H12 H 0.2385 0.8478 0.3310 0.077 Uiso 1 1 calc R . . C13 C 0.2611(4) 1.0055(3) 0.2679(2) 0.0527(8) Uani 1 1 d . . . C14 C 0.2300(5) 1.0537(4) 0.1831(3) 0.0744(11) Uani 1 1 d . . . H14 H 0.2571 1.1357 0.1754 0.089 Uiso 1 1 calc R . . C15 C 0.1591(5) 0.9795(4) 0.1106(3) 0.0816(12) Uani 1 1 d . . . H15 H 0.1393 1.0135 0.0541 0.098 Uiso 1 1 calc R . . C16 C 0.3311(4) 1.0877(3) 0.3494(2) 0.0610(9) Uani 1 1 d . . . C17 C 0.4177(3) 1.0396(3) 0.4258(2) 0.0477(7) Uani 1 1 d . . . C18 C 0.4926(4) 0.9409(3) 0.4116(2) 0.0533(8) Uani 1 1 d . . . H18 H 0.4884 0.9008 0.3525 0.064 Uiso 1 1 calc R . . C19 C 0.5734(4) 0.9020(3) 0.4851(2) 0.0551(8) Uani 1 1 d . . . H19 H 0.6231 0.8353 0.4750 0.066 Uiso 1 1 calc R . . O11 O 0.3111(4) 1.1930(3) 0.3523(2) 0.1137(13) Uani 1 1 d . . . N21 N 0.0576(2) 0.4827(2) 0.14623(14) 0.0392(5) Uani 1 1 d . . . C21 C -0.0184(3) 0.5165(3) 0.21755(18) 0.0430(6) Uani 1 1 d . . . H21 H -0.1047 0.5479 0.2037 0.052 Uiso 1 1 calc R . . C22 C 0.0247(3) 0.5072(3) 0.31073(18) 0.0433(6) Uani 1 1 d . . . H22 H -0.0322 0.5303 0.3581 0.052 Uiso 1 1 calc R . . C23 C 0.1544(3) 0.4626(2) 0.33227(17) 0.0383(6) Uani 1 1 d . . . C24 C 0.2340(3) 0.4280(3) 0.25901(18) 0.0425(6) Uani 1 1 d . . . H24 H 0.3216 0.3980 0.2711 0.051 Uiso 1 1 calc R . . C25 C 0.1821(3) 0.4384(3) 0.16820(18) 0.0430(6) Uani 1 1 d . . . H25 H 0.2359 0.4135 0.1196 0.052 Uiso 1 1 calc R . . C26 C 0.2002(3) 0.4443(3) 0.43263(18) 0.0417(6) Uani 1 1 d . . . C27 C 0.3552(3) 0.4747(2) 0.46613(17) 0.0372(6) Uani 1 1 d . . . C28 C 0.4529(3) 0.5517(2) 0.42008(17) 0.0414(6) Uani 1 1 d . . . H28 H 0.4211 0.5871 0.3665 0.050 Uiso 1 1 calc R . . C29 C 0.5959(3) 0.5762(2) 0.45308(17) 0.0390(6) Uani 1 1 d . . . H29 H 0.6603 0.6270 0.4212 0.047 Uiso 1 1 calc R . . O21 O 0.1102(2) 0.4019(2) 0.48298(15) 0.0633(6) Uani 1 1 d . . . N31 N -0.2507(4) 0.2772(3) 0.1662(2) 0.0756(9) Uani 1 1 d . . . C31 C -0.1389(5) 0.2211(3) 0.1906(3) 0.0698(10) Uani 1 1 d . . . H31 H -0.0787 0.2012 0.1442 0.084 Uiso 1 1 calc R . . C32 C -0.1055(4) 0.1901(3) 0.2802(2) 0.0618(9) Uani 1 1 d . . . H32 H -0.0254 0.1502 0.2933 0.074 Uiso 1 1 calc R . . C33 C -0.1934(4) 0.2194(3) 0.3508(2) 0.0537(8) Uani 1 1 d . . . C34 C -0.3108(4) 0.2785(4) 0.3266(3) 0.0675(10) Uani 1 1 d . . . H34 H -0.3728 0.2999 0.3716 0.081 Uiso 1 1 calc R . . C35 C -0.3343(4) 0.3053(4) 0.2343(3) 0.0809(12) Uani 1 1 d . . . H35 H -0.4133 0.3455 0.2188 0.097 Uiso 1 1 calc R . . C36 C -0.1611(4) 0.1954(3) 0.4513(2) 0.0534(8) Uani 1 1 d . . . C37 C -0.0749(3) 0.0949(3) 0.4737(2) 0.0498(7) Uani 1 1 d . . . C38 C -0.0951(4) -0.0152(3) 0.4208(2) 0.0545(8) Uani 1 1 d . . . H38 H -0.1585 -0.0256 0.3675 0.065 Uiso 1 1 calc R . . C39 C -0.0205(4) -0.1096(3) 0.4476(2) 0.0544(8) Uani 1 1 d . . . H39 H -0.0349 -0.1834 0.4122 0.065 Uiso 1 1 calc R . . O31 O -0.2043(3) 0.2578(2) 0.51334(17) 0.0706(7) Uani 1 1 d . . . S1A S 0.6436(5) 0.7418(3) 0.1962(2) 0.0712(9) Uani 0.479(6) 1 d PDU A 1 O1A O 0.7512(11) 0.7761(9) 0.2677(6) 0.146(4) Uani 0.479(6) 1 d PDU A 1 O2A O 0.4981(8) 0.7150(7) 0.2273(7) 0.097(3) Uani 0.479(6) 1 d PDU A 1 O3A O 0.6802(12) 0.6448(14) 0.1358(9) 0.074(3) Uani 0.479(6) 1 d PDU A 1 C1A C 0.6183(18) 0.8612(13) 0.1147(10) 0.163(12) Uani 0.479(6) 1 d PDU A 1 F1A F 0.7513(14) 0.9158(14) 0.1412(10) 0.179(6) Uani 0.479(6) 1 d PDU A 1 F2A F 0.5254(13) 0.9364(11) 0.1370(10) 0.167(4) Uani 0.479(6) 1 d PDU A 1 F3A F 0.6051(15) 0.8419(10) 0.0250(6) 0.171(4) Uani 0.479(6) 1 d PDU A 1 S1B S 0.5782(3) 0.7177(3) 0.1659(2) 0.0612(7) Uani 0.521(6) 1 d PDU A 2 O1B O 0.6005(12) 0.7509(8) 0.2643(5) 0.120(3) Uani 0.521(6) 1 d PDU A 2 O2B O 0.4396(8) 0.6701(9) 0.1350(7) 0.153(4) Uani 0.521(6) 1 d PDU A 2 O3B O 0.6903(14) 0.6708(15) 0.1237(10) 0.120(6) Uani 0.521(6) 1 d PDU A 2 C1B C 0.6182(11) 0.8737(8) 0.1288(7) 0.086(4) Uani 0.521(6) 1 d PDU A 2 F1B F 0.6001(10) 0.9648(6) 0.1905(6) 0.124(3) Uani 0.521(6) 1 d PDU A 2 F2B F 0.5132(14) 0.8586(11) 0.0639(9) 0.196(5) Uani 0.521(6) 1 d PDU A 2 F3B F 0.7398(12) 0.9051(11) 0.0915(9) 0.158(4) Uani 0.521(6) 1 d PDU A 2 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 Zn 0.0399(3) 0.0522(3) 0.0217(2) 0.00294(18) -0.00384(16) 0.0121(2) O1W 0.0459(12) 0.0764(15) 0.0442(12) 0.0174(11) -0.0017(10) 0.0039(11) O2W 0.0512(13) 0.0565(13) 0.0413(11) -0.0077(9) -0.0046(10) 0.0136(11) N11 0.081(2) 0.087(2) 0.0576(19) -0.0086(17) -0.0091(16) -0.0046(19) C11 0.099(3) 0.067(3) 0.078(3) 0.002(2) -0.011(2) -0.016(2) C12 0.075(2) 0.061(2) 0.0536(19) 0.0066(16) -0.0014(17) -0.0079(18) C13 0.0528(18) 0.0544(19) 0.0497(17) 0.0024(14) 0.0010(14) 0.0036(15) C14 0.088(3) 0.064(2) 0.065(2) 0.0115(18) -0.014(2) -0.007(2) C15 0.089(3) 0.094(3) 0.057(2) 0.013(2) -0.009(2) -0.004(2) C16 0.077(2) 0.0442(19) 0.060(2) 0.0009(15) -0.0064(17) 0.0077(16) C17 0.0495(17) 0.0422(16) 0.0496(17) -0.0015(13) 0.0022(13) 0.0006(13) C18 0.062(2) 0.0505(18) 0.0456(16) -0.0116(14) 0.0023(14) 0.0063(15) C19 0.060(2) 0.0442(17) 0.061(2) -0.0080(15) -0.0020(16) 0.0157(15) O11 0.182(4) 0.0538(17) 0.100(2) -0.0092(15) -0.062(2) 0.0334(19) N21 0.0407(12) 0.0516(14) 0.0263(10) 0.0025(9) -0.0029(9) 0.0120(10) C21 0.0418(15) 0.0546(17) 0.0340(13) 0.0042(12) -0.0020(11) 0.0141(13) C22 0.0448(16) 0.0553(17) 0.0301(13) 0.0011(12) 0.0026(11) 0.0082(13) C23 0.0421(15) 0.0434(15) 0.0281(12) 0.0034(11) -0.0047(11) 0.0032(12) C24 0.0426(15) 0.0521(17) 0.0335(13) 0.0026(12) -0.0066(11) 0.0128(13) C25 0.0456(16) 0.0551(17) 0.0294(13) 0.0011(12) -0.0002(11) 0.0125(13) C26 0.0477(16) 0.0499(16) 0.0278(12) 0.0050(12) -0.0019(12) 0.0080(13) C27 0.0477(16) 0.0377(14) 0.0255(12) 0.0002(10) -0.0044(11) 0.0064(12) C28 0.0540(17) 0.0420(15) 0.0281(12) 0.0086(11) -0.0064(12) 0.0072(13) C29 0.0511(16) 0.0383(14) 0.0264(12) 0.0064(10) -0.0033(11) 0.0017(12) O21 0.0569(14) 0.0937(18) 0.0398(11) 0.0204(12) 0.0026(10) 0.0052(12) N31 0.076(2) 0.086(2) 0.066(2) 0.0322(17) -0.0009(17) 0.0029(18) C31 0.087(3) 0.066(2) 0.058(2) 0.0181(18) 0.0196(19) 0.006(2) C32 0.067(2) 0.061(2) 0.063(2) 0.0213(17) 0.0133(17) 0.0158(17) C33 0.0529(19) 0.0516(18) 0.0595(19) 0.0192(15) 0.0110(15) 0.0081(15) C34 0.055(2) 0.080(3) 0.073(2) 0.030(2) 0.0128(17) 0.0190(18) C35 0.059(2) 0.102(3) 0.086(3) 0.042(2) 0.001(2) 0.014(2) C36 0.0526(18) 0.0551(19) 0.0558(19) 0.0179(15) 0.0129(15) 0.0084(15) C37 0.0513(18) 0.0509(18) 0.0508(17) 0.0184(14) 0.0129(14) 0.0092(14) C38 0.0533(19) 0.059(2) 0.0527(18) 0.0167(15) 0.0026(14) 0.0059(15) C39 0.061(2) 0.0502(18) 0.0524(18) 0.0100(14) 0.0070(15) 0.0058(15) O31 0.0787(17) 0.0779(17) 0.0644(15) 0.0170(13) 0.0207(13) 0.0327(14) S1A 0.085(2) 0.0747(16) 0.0564(16) -0.0083(12) 0.0071(15) 0.0256(16) O1A 0.151(7) 0.151(7) 0.126(6) -0.031(5) -0.045(5) 0.021(6) O2A 0.090(5) 0.094(5) 0.118(6) 0.022(4) 0.065(5) 0.025(4) O3A 0.075(5) 0.062(5) 0.091(5) 0.005(4) 0.032(4) 0.022(4) C1A 0.149(14) 0.170(14) 0.176(14) -0.014(9) 0.056(10) 0.036(9) F1A 0.200(9) 0.144(7) 0.186(9) -0.010(7) 0.025(7) -0.012(6) F2A 0.185(8) 0.134(7) 0.201(9) 0.050(7) 0.028(7) 0.078(6) F3A 0.197(8) 0.200(8) 0.130(6) 0.090(6) 0.020(6) 0.035(7) S1B 0.0520(14) 0.0747(14) 0.0586(15) 0.0043(11) 0.0106(11) 0.0123(11) O1B 0.175(8) 0.123(6) 0.066(4) -0.002(4) 0.027(5) 0.035(6) O2B 0.101(5) 0.174(7) 0.169(7) 0.047(6) -0.042(5) -0.032(5) O3B 0.124(8) 0.096(9) 0.151(9) -0.005(6) 0.073(6) 0.031(5) C1B 0.090(7) 0.089(7) 0.095(6) 0.038(5) 0.057(6) 0.035(5) F1B 0.156(6) 0.082(4) 0.145(6) 0.019(4) 0.059(5) 0.029(4) F2B 0.229(9) 0.204(8) 0.161(8) 0.038(7) -0.029(7) 0.057(7) F3B 0.176(7) 0.137(6) 0.174(8) 0.047(6) 0.111(6) 0.009(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 Zn O1W 2.104(2) . ? Zn O1W 2.104(2) 2_565 ? Zn O2W 2.117(2) 2_565 ? Zn O2W 2.117(2) . ? Zn N21 2.154(2) 2_565 ? Zn N21 2.154(2) . ? N11 C11 1.320(5) . ? N11 C15 1.329(5) . ? C11 C12 1.382(5) . ? C12 C13 1.368(5) . ? C13 C14 1.382(5) . ? C13 C16 1.504(5) . ? C14 C15 1.371(5) . ? C16 O11 1.206(4) . ? C16 C17 1.484(5) . ? C17 C18 1.383(4) . ? C17 C19 1.389(4) 2_676 ? C18 C19 1.378(4) . ? C19 C17 1.389(4) 2_676 ? N21 C21 1.339(3) . ? N21 C25 1.344(3) . ? C21 C22 1.383(4) . ? C22 C23 1.387(4) . ? C23 C24 1.383(4) . ? C23 C26 1.505(3) . ? C24 C25 1.375(4) . ? C26 O21 1.207(3) . ? C26 C27 1.487(4) . ? C27 C29 1.392(3) 2_666 ? C27 C28 1.393(4) . ? C28 C29 1.377(4) . ? C29 C27 1.392(3) 2_666 ? N31 C31 1.318(5) . ? N31 C35 1.331(5) . ? C31 C32 1.374(5) . ? C32 C33 1.387(5) . ? C33 C34 1.381(5) . ? C33 C36 1.496(4) . ? C34 C35 1.381(5) . ? C36 O31 1.214(4) . ? C36 C37 1.493(4) . ? C37 C39 1.382(4) 2_556 ? C37 C38 1.387(5) . ? C38 C39 1.387(4) . ? C39 C37 1.382(4) 2_556 ? S1A O1A 1.391(8) . ? S1A O3A 1.431(9) . ? S1A O2A 1.454(7) . ? S1A C1A 1.844(10) . ? C1A F3A 1.284(12) . ? C1A F2A 1.316(12) . ? C1A F1A 1.335(13) . ? S1B O2B 1.372(7) . ? S1B O3B 1.380(9) . ? S1B O1B 1.431(7) . ? S1B C1B 1.842(8) . ? C1B F2B 1.297(11) . ? C1B F3B 1.299(10) . ? C1B F1B 1.338(11) . ? 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 Zn O1W 180.00(11) . 2_565 ? O1W Zn O2W 91.17(9) . 2_565 ? O1W Zn O2W 88.83(9) 2_565 2_565 ? O1W Zn O2W 88.83(9) . . ? O1W Zn O2W 91.17(9) 2_565 . ? O2W Zn O2W 180.0 2_565 . ? O1W Zn N21 91.85(8) . 2_565 ? O1W Zn N21 88.15(8) 2_565 2_565 ? O2W Zn N21 92.55(8) 2_565 2_565 ? O2W Zn N21 87.45(8) . 2_565 ? O1W Zn N21 88.15(8) . . ? O1W Zn N21 91.85(8) 2_565 . ? O2W Zn N21 87.45(8) 2_565 . ? O2W Zn N21 92.55(8) . . ? N21 Zn N21 180.00(12) 2_565 . ? C11 N11 C15 116.2(3) . . ? N11 C11 C12 124.8(4) . . ? C13 C12 C11 118.2(3) . . ? C12 C13 C14 117.9(3) . . ? C12 C13 C16 122.3(3) . . ? C14 C13 C16 119.7(3) . . ? C15 C14 C13 119.4(4) . . ? N11 C15 C14 123.4(4) . . ? O11 C16 C17 121.0(3) . . ? O11 C16 C13 118.0(3) . . ? C17 C16 C13 120.9(3) . . ? C18 C17 C19 118.7(3) . 2_676 ? C18 C17 C16 122.8(3) . . ? C19 C17 C16 118.5(3) 2_676 . ? C19 C18 C17 120.0(3) . . ? C18 C19 C17 121.3(3) . 2_676 ? C21 N21 C25 117.1(2) . . ? C21 N21 Zn 125.19(17) . . ? C25 N21 Zn 117.66(17) . . ? N21 C21 C22 123.3(3) . . ? C21 C22 C23 118.8(3) . . ? C24 C23 C22 118.2(2) . . ? C24 C23 C26 121.5(2) . . ? C22 C23 C26 120.1(2) . . ? C25 C24 C23 119.3(3) . . ? N21 C25 C24 123.2(3) . . ? O21 C26 C27 121.8(2) . . ? O21 C26 C23 118.8(3) . . ? C27 C26 C23 119.3(2) . . ? C29 C27 C28 118.9(2) 2_666 . ? C29 C27 C26 118.4(2) 2_666 . ? C28 C27 C26 122.7(2) . . ? C29 C28 C27 120.7(2) . . ? C28 C29 C27 120.4(3) . 2_666 ? C31 N31 C35 116.5(3) . . ? N31 C31 C32 124.3(4) . . ? C31 C32 C33 118.8(3) . . ? C34 C33 C32 117.7(3) . . ? C34 C33 C36 119.6(3) . . ? C32 C33 C36 122.6(3) . . ? C35 C34 C33 118.6(4) . . ? N31 C35 C34 124.0(4) . . ? O31 C36 C37 120.9(3) . . ? O31 C36 C33 119.9(3) . . ? C37 C36 C33 119.2(3) . . ? C39 C37 C38 119.5(3) 2_556 . ? C39 C37 C36 118.9(3) 2_556 . ? C38 C37 C36 121.5(3) . . ? C37 C38 C39 119.9(3) . . ? C37 C39 C38 120.6(3) 2_556 . ? O1A S1A O3A 111.3(6) . . ? O1A S1A O2A 115.0(6) . . ? O3A S1A O2A 111.5(7) . . ? O1A S1A C1A 114.0(7) . . ? O3A S1A C1A 102.8(9) . . ? O2A S1A C1A 101.2(6) . . ? F3A C1A F2A 106.9(11) . . ? F3A C1A F1A 109.8(12) . . ? F2A C1A F1A 108.0(12) . . ? F3A C1A S1A 123.6(10) . . ? F2A C1A S1A 116.5(10) . . ? F1A C1A S1A 89.7(10) . . ? O2B S1B O3B 117.5(7) . . ? O2B S1B O1B 115.6(6) . . ? O3B S1B O1B 116.6(8) . . ? O2B S1B C1B 110.1(5) . . ? O3B S1B C1B 96.9(8) . . ? O1B S1B C1B 95.3(5) . . ? F2B C1B F3B 109.4(10) . . ? F2B C1B F1B 110.3(9) . . ? F3B C1B F1B 106.6(9) . . ? F2B C1B S1B 93.1(8) . . ? F3B C1B S1B 119.1(8) . . ? F1B C1B S1B 117.4(6) . . ? 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 H112 N31 0.85 1.90 2.750(4) 172.4 2_565 O2W H211 N11 0.84 1.97 2.790(4) 163.1 . _diffrn_measured_fraction_theta_max 0.878 _diffrn_reflns_theta_full 29.64 _diffrn_measured_fraction_theta_full 0.878 _refine_diff_density_max 0.369 _refine_diff_density_min -0.401 _refine_diff_density_rms 0.053 data_2 _database_code_CSD 173814 _diffrn_measurement_domega 0.30 _diffrn_measurement_rtime 20 _chemical_formula_sum 'C22 H18 Co N6 O10' _chemical_formula_weight 585.35 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' #(#2) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.359(2) _cell_length_b 11.765(2) _cell_length_c 11.928(2) _cell_angle_alpha 112.498(2) _cell_angle_beta 93.738(2) _cell_angle_gamma 112.770(2) _cell_volume 1314.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1622 _cell_measurement_theta_min 3. _cell_measurement_theta_max 23. _exptl_crystal_description column _exptl_crystal_colour pink _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 1.479 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 598 _exptl_absorpt_coefficient_mu 0.718 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.79 _exptl_absorpt_correction_T_max 1.00 _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 SMART _diffrn_detector_type CCD_plate _diffrn_measurement_method omega-scan _diffrn_standards_decay_% 0 _diffrn_reflns_number 10202 _diffrn_reflns_av_R_equivalents 0.0442 _diffrn_reflns_av_sigmaI/netI 0.0551 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 24.28 _reflns_number_total 3368 _reflns_number_observed 2702 _reflns_observed_criterion >2sigma(I) _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SCHAKAL _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^)+(0.1036P)^2^+34.4743P] 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_number_reflns 3368 _refine_ls_number_parameters 352 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.1378 _refine_ls_R_factor_obs 0.1202 _refine_ls_wR_factor_all 0.3533 _refine_ls_wR_factor_obs 0.3453 _refine_ls_goodness_of_fit_all 1.123 _refine_ls_restrained_S_all 1.122 _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 Co Co -0.11032(18) 0.34747(17) 0.70951(17) 0.0331(6) Uani 1 1 d . . . N1 N -0.2107(12) 0.1293(11) 0.6053(11) 0.044(3) Uani 1 1 d . . . C2 C -0.3225(19) 0.0523(17) 0.6204(18) 0.073(6) Uani 1 1 d . . . H2 H -0.3571 0.0958 0.6823 0.088 Uiso 1 1 calc R . . C3 C -0.3929(18) -0.0901(17) 0.5500(17) 0.073(6) Uani 1 1 d . . . H3 H -0.4708 -0.1408 0.5650 0.088 Uiso 1 1 calc R . . C4 C -0.3415(16) -0.1512(14) 0.4578(14) 0.047(4) Uani 1 1 d . . . C5 C -0.230(2) -0.0753(15) 0.436(2) 0.086(8) Uani 1 1 d U . . H5 H -0.1953 -0.1160 0.3727 0.103 Uiso 1 1 calc R . . C6 C -0.1693(16) 0.0656(16) 0.5107(16) 0.064(5) Uani 1 1 d . . . H6 H -0.0947 0.1187 0.4932 0.077 Uiso 1 1 calc R . . C7 C -0.4714(13) -0.3536(14) 0.2743(14) 0.039(3) Uani 1 1 d . . . C8 C -0.5292(13) -0.5089(13) 0.2166(13) 0.039(3) Uani 1 1 d . . . C9 C -0.4893(15) -0.5737(14) 0.2778(14) 0.047(4) Uani 1 1 d . . . H9 H -0.4266 -0.5224 0.3543 0.056 Uiso 1 1 calc R . . C10 C -0.5452(15) -0.7146(14) 0.2222(14) 0.046(4) Uani 1 1 d . . . H10 H -0.5181 -0.7596 0.2598 0.055 Uiso 1 1 calc R . . C11 C -0.6419(14) -0.7907(13) 0.1098(14) 0.043(4) Uani 1 1 d . . . C12 C -0.6809(15) -0.7276(14) 0.0495(14) 0.048(4) Uani 1 1 d . . . H12 H -0.7452 -0.7794 -0.0259 0.057 Uiso 1 1 calc R . . C13 C -0.6219(14) -0.5840(14) 0.1038(15) 0.045(4) Uani 1 1 d . . . H13 H -0.6454 -0.5393 0.0635 0.054 Uiso 1 1 calc R . . C14 C -0.6977(17) -0.9431(16) 0.0571(16) 0.054(4) Uani 1 1 d . . . C15 C -0.8677(17) -1.1534(14) -0.0979(15) 0.051(4) Uani 1 1 d . . . C16 C -0.9511(17) -1.2131(16) -0.0386(16) 0.059(5) Uani 1 1 d . . . H16 H -0.9624 -1.1616 0.0377 0.071 Uiso 1 1 calc R . . C17 C -1.0173(16) -1.3533(14) -0.0977(14) 0.048(4) Uani 1 1 d . . . H17 H -1.0747 -1.3959 -0.0582 0.057 Uiso 1 1 calc R . . C18 C -0.9231(15) -1.3690(15) -0.2601(14) 0.048(4) Uani 1 1 d . . . H18 H -0.9122 -1.4224 -0.3357 0.058 Uiso 1 1 calc R . . C19 C -0.8519(17) -1.2273(15) -0.2095(14) 0.054(4) Uani 1 1 d . . . H19 H -0.7962 -1.1852 -0.2503 0.065 Uiso 1 1 calc R . . N21 N -0.2458(10) 0.3499(9) 0.5235(10) 0.022(2) Uani 1 1 d . . . O1 O -0.4838(10) -0.2907(9) 0.2179(10) 0.050(3) Uani 1 1 d . . . O2 O -0.6639(13) -1.0067(11) 0.1018(12) 0.080(4) Uani 1 1 d . . . O3 O -0.4012(11) -0.2946(9) 0.3939(9) 0.054(3) Uani 1 1 d . . . O4 O -0.8018(12) -1.0101(9) -0.0464(9) 0.056(3) Uani 1 1 d . . . N71 N -0.2074(13) 0.3420(12) 0.8535(12) 0.042(3) Uani 1 1 d D . . C72 C -0.2638(15) 0.3267(15) 0.9219(15) 0.045(4) Uani 1 1 d D . . C73 C -0.3465(16) 0.3051(17) 1.0097(16) 0.054(4) Uani 1 1 d D . . H73A H -0.4301 0.3004 0.9814 0.080 Uiso 1 1 calc R . . H73B H -0.3030 0.3803 1.0918 0.080 Uiso 1 1 calc R . . H73C H -0.3601 0.2207 1.0128 0.080 Uiso 1 1 calc R . . N81 N 0.032(3) -0.962(2) 0.255(3) 0.196(17) Uani 1 1 d D . . C82 C 0.101(2) -0.854(2) 0.310(2) 0.090(7) Uani 1 1 d D . . C83 C 0.178(2) -0.7043(18) 0.3881(19) 0.090(7) Uani 1 1 d D . . H83A H 0.1328 -0.6733 0.4499 0.135 Uiso 1 1 calc R . . H83B H 0.1861 -0.6578 0.3360 0.135 Uiso 1 1 calc R . . H83C H 0.2636 -0.6844 0.4292 0.135 Uiso 1 1 calc R . . N11 N 0.1235(13) 0.3455(12) 0.7682(13) 0.047(3) Uani 1 1 d . . . O11 O 0.0395(11) 0.3468(11) 0.8371(14) 0.074(4) Uani 1 1 d . . . O12 O 0.0857(12) 0.3435(11) 0.6621(12) 0.065(3) Uani 1 1 d . . . O13 O 0.2255(11) 0.3491(12) 0.8053(13) 0.068(4) Uani 1 1 d . . . N20 N -1.0072(12) -1.4333(11) -0.2052(11) 0.039(3) Uani 1 1 d . . . O21 O -0.2810(11) 0.3577(11) 0.6226(10) 0.057(3) Uani 1 1 d . . . O22 O -0.1321(11) 0.3516(10) 0.5256(9) 0.051(3) Uani 1 1 d . . . O23 O -0.3070(14) 0.3514(16) 0.4366(13) 0.093(5) 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 Co 0.0364(11) 0.0167(9) 0.0343(11) 0.0071(8) 0.0039(8) 0.0055(8) N1 0.049(8) 0.024(6) 0.042(7) 0.008(6) 0.008(6) 0.006(6) C2 0.073(13) 0.038(10) 0.071(13) 0.003(9) 0.036(10) 0.006(9) C3 0.059(12) 0.039(10) 0.062(12) -0.010(9) 0.024(10) -0.004(8) C4 0.055(10) 0.022(8) 0.039(9) 0.000(7) -0.006(7) 0.010(7) C5 0.089(14) 0.016(8) 0.104(16) -0.013(9) 0.061(13) 0.009(9) C6 0.048(10) 0.037(9) 0.064(11) -0.002(8) 0.028(9) -0.001(8) C7 0.026(8) 0.026(7) 0.045(9) 0.008(7) -0.001(7) 0.000(6) C8 0.034(8) 0.025(7) 0.043(9) 0.005(6) 0.002(7) 0.009(6) C9 0.042(9) 0.030(8) 0.044(9) 0.016(7) -0.007(7) -0.004(7) C10 0.050(9) 0.023(7) 0.042(9) 0.009(7) -0.014(7) 0.004(7) C11 0.044(9) 0.017(7) 0.057(10) 0.013(7) 0.010(8) 0.008(6) C12 0.045(9) 0.022(7) 0.048(9) 0.000(7) -0.011(7) 0.007(7) C13 0.041(9) 0.024(7) 0.068(11) 0.024(7) -0.008(8) 0.011(7) C14 0.059(11) 0.030(8) 0.054(10) 0.004(8) 0.003(9) 0.018(8) C15 0.063(11) 0.024(8) 0.044(10) 0.004(7) -0.006(8) 0.012(8) C16 0.066(12) 0.038(9) 0.046(10) 0.004(8) 0.011(9) 0.013(9) C17 0.064(11) 0.023(8) 0.038(9) 0.006(7) 0.019(8) 0.009(7) C18 0.052(10) 0.038(9) 0.036(8) 0.007(7) 0.011(7) 0.011(8) C19 0.074(12) 0.027(8) 0.038(9) 0.007(7) 0.013(8) 0.008(8) N21 0.029(6) 0.010(5) 0.025(6) 0.012(4) 0.001(5) 0.003(4) O1 0.053(7) 0.019(5) 0.059(7) 0.009(5) -0.007(5) 0.009(5) O2 0.095(10) 0.022(6) 0.077(9) -0.006(6) -0.037(7) 0.019(6) O3 0.071(8) 0.017(5) 0.044(6) 0.005(5) -0.008(6) 0.003(5) O4 0.086(8) 0.019(5) 0.037(6) -0.001(4) -0.017(6) 0.018(5) N71 0.052(8) 0.036(7) 0.040(7) 0.019(6) 0.015(7) 0.018(6) C72 0.043(9) 0.033(8) 0.052(10) 0.016(8) 0.003(8) 0.013(7) C73 0.057(10) 0.061(11) 0.069(11) 0.044(9) 0.038(9) 0.033(9) N81 0.26(4) 0.089(18) 0.15(3) -0.022(17) -0.05(3) 0.09(2) C82 0.103(18) 0.095(17) 0.067(14) 0.016(13) 0.002(13) 0.063(16) C83 0.109(18) 0.067(13) 0.073(14) 0.009(11) 0.018(13) 0.042(13) N11 0.046(9) 0.026(7) 0.055(9) 0.010(6) -0.002(7) 0.012(6) O11 0.042(7) 0.043(7) 0.115(11) 0.005(7) 0.015(7) 0.028(6) O12 0.069(8) 0.044(7) 0.062(8) 0.012(6) 0.014(6) 0.017(6) O13 0.039(7) 0.067(8) 0.099(10) 0.029(7) 0.006(6) 0.033(6) N20 0.049(7) 0.023(6) 0.038(7) 0.013(6) 0.005(6) 0.010(6) O21 0.062(7) 0.056(7) 0.050(7) 0.024(6) 0.006(6) 0.025(6) O22 0.052(7) 0.039(6) 0.046(6) 0.018(5) 0.004(5) 0.009(5) O23 0.087(10) 0.112(12) 0.069(9) 0.052(9) -0.010(8) 0.026(9) _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 N71 2.109(13) . ? Co N1 2.131(11) . ? Co N20 2.134(11) 1_676 ? Co O21 2.205(11) . ? Co O22 2.213(10) . ? Co O11 2.213(14) . ? Co O12 2.346(13) . ? N1 C2 1.32(2) . ? N1 C6 1.323(19) . ? C2 C3 1.40(2) . ? C3 C4 1.37(2) . ? C4 C5 1.35(2) . ? C4 O3 1.397(16) . ? C5 C6 1.39(2) . ? C7 O1 1.212(17) . ? C7 O3 1.348(17) . ? C7 C8 1.514(19) . ? C8 C13 1.37(2) . ? C8 C9 1.40(2) . ? C9 C10 1.371(19) . ? C10 C11 1.39(2) . ? C11 C12 1.37(2) . ? C11 C14 1.49(2) . ? C12 C13 1.397(19) . ? C14 O2 1.22(2) . ? C14 O4 1.374(19) . ? C15 C19 1.35(2) . ? C15 C16 1.36(2) . ? C15 O4 1.397(17) . ? C16 C17 1.37(2) . ? C17 N20 1.313(18) . ? C18 N20 1.347(19) . ? C18 C19 1.39(2) . ? N21 O23 1.220(16) . ? N21 O21 1.254(14) . ? N21 O22 1.282(14) . ? N71 C72 1.095(16) . ? C72 C73 1.48(2) . ? N81 C82 1.08(2) . ? C82 C83 1.48(2) . ? N11 O13 1.191(16) . ? N11 O12 1.298(17) . ? N11 O11 1.301(18) . ? N20 Co 2.134(11) 1_434 ? 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 N71 Co N1 91.8(5) . . ? N71 Co N20 93.9(5) . 1_676 ? N1 Co N20 173.7(5) . 1_676 ? N71 Co O21 85.2(5) . . ? N1 Co O21 88.5(5) . . ? N20 Co O21 89.4(4) 1_676 . ? N71 Co O22 142.5(5) . . ? N1 Co O22 85.8(4) . . ? N20 Co O22 88.1(4) 1_676 . ? O21 Co O22 57.3(4) . . ? N71 Co O11 80.9(5) . . ? N1 Co O11 94.7(5) . . ? N20 Co O11 88.8(4) 1_676 . ? O21 Co O11 165.8(5) . . ? O22 Co O11 136.7(5) . . ? N71 Co O12 137.7(5) . . ? N1 Co O12 89.6(4) . . ? N20 Co O12 87.9(4) 1_676 . ? O21 Co O12 137.1(5) . . ? O22 Co O12 79.8(5) . . ? O11 Co O12 56.9(5) . . ? C2 N1 C6 116.0(13) . . ? C2 N1 Co 123.4(11) . . ? C6 N1 Co 120.2(10) . . ? N1 C2 C3 124.5(16) . . ? C4 C3 C2 116.6(16) . . ? C5 C4 C3 120.6(14) . . ? C5 C4 O3 120.8(14) . . ? C3 C4 O3 118.4(15) . . ? C4 C5 C6 117.9(15) . . ? N1 C6 C5 124.1(15) . . ? O1 C7 O3 124.5(12) . . ? O1 C7 C8 123.7(13) . . ? O3 C7 C8 111.7(13) . . ? C13 C8 C9 121.2(12) . . ? C13 C8 C7 118.2(13) . . ? C9 C8 C7 120.6(12) . . ? C10 C9 C8 118.4(13) . . ? C9 C10 C11 120.5(14) . . ? C12 C11 C10 121.3(13) . . ? C12 C11 C14 122.0(14) . . ? C10 C11 C14 116.6(14) . . ? C11 C12 C13 118.6(13) . . ? C8 C13 C12 120.0(13) . . ? O2 C14 O4 121.1(14) . . ? O2 C14 C11 126.0(15) . . ? O4 C14 C11 112.7(14) . . ? C19 C15 C16 122.4(14) . . ? C19 C15 O4 118.2(15) . . ? C16 C15 O4 119.2(15) . . ? C15 C16 C17 116.0(15) . . ? N20 C17 C16 125.8(15) . . ? N20 C18 C19 123.3(14) . . ? C15 C19 C18 116.6(15) . . ? O23 N21 O21 124.4(13) . . ? O23 N21 O22 122.1(12) . . ? O21 N21 O22 113.3(10) . . ? C7 O3 C4 117.5(12) . . ? C14 O4 C15 117.4(12) . . ? C72 N71 Co 173.6(13) . . ? N71 C72 C73 176.7(17) . . ? N81 C82 C83 171(3) . . ? O13 N11 O12 126.0(15) . . ? O13 N11 O11 120.3(15) . . ? O12 N11 O11 113.7(14) . . ? N11 O11 Co 97.8(11) . . ? N11 O12 Co 91.7(9) . . ? C17 N20 C18 115.9(12) . . ? C17 N20 Co 123.9(10) . 1_434 ? C18 N20 Co 120.2(9) . 1_434 ? N21 O21 Co 95.1(8) . . ? N21 O22 Co 93.9(7) . . ? _diffrn_measured_fraction_theta_max 0.788 _diffrn_reflns_theta_full 24.28 _diffrn_measured_fraction_theta_full 0.788 _refine_diff_density_max 1.720 _refine_diff_density_min -0.622 _refine_diff_density_rms 0.163 data_3 _database_code_CSD 173815 _diffrn_measurement_domega 0.30 _diffrn_measurement_rtime 20.15 _chemical_formula_sum 'C46 H40 Cl4 Co N6 O10' _chemical_formula_weight 1037.57 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' 'Cl' 'Cl' 0.1484 0.1585 '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 Monoclnic _symmetry_space_group_name_H-M 'P 21/c' #(#14) 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 13.338(4) _cell_length_b 15.531(5) _cell_length_c 12.136(4) _cell_angle_alpha 90.00 _cell_angle_beta 113.020(10) _cell_angle_gamma 90.00 _cell_volume 2313.8(13) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 931 _cell_measurement_theta_min 2 _cell_measurement_theta_max 23 _exptl_crystal_description plate _exptl_crystal_colour pink _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.489 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1066 _exptl_absorpt_coefficient_mu 0.667 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_T_max 1.00 _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 SMART _diffrn_detector_type CCD_plate _diffrn_measurement_method omega-scan _diffrn_standards_decay_% 17 _diffrn_reflns_number 25292 _diffrn_reflns_av_R_equivalents 0.0669 _diffrn_reflns_av_sigmaI/netI 0.0543 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 27.10 _reflns_number_total 5068 _reflns_number_observed 3251 _reflns_observed_criterion >2sigma(I) _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SCHAKAL _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^)+(0.1060P)^2^+3.7245P] 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_number_reflns 5068 _refine_ls_number_parameters 313 _refine_ls_number_restraints 27 _refine_ls_R_factor_all 0.1123 _refine_ls_R_factor_obs 0.0696 _refine_ls_wR_factor_all 0.2196 _refine_ls_wR_factor_obs 0.1885 _refine_ls_goodness_of_fit_all 1.042 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.3624(4) 0.0077(3) 0.6488(4) 0.0583(11) Uani 1 1 d D . . O11 O 0.3854(2) 0.03960(19) 0.5667(3) 0.0421(7) Uani 1 1 d D A . O12 O 0.3519(6) -0.0711(4) 0.6542(5) 0.085(3) Uani 0.710(12) 1 d PD A 1 O13 O 0.3452(16) 0.0534(5) 0.7185(11) 0.200(8) Uani 0.710(12) 1 d PD A 1 O12B O 0.2724(10) -0.0152(12) 0.6325(13) 0.087(6) Uiso 0.290(12) 1 d PD A 2 O13B O 0.4225(10) 0.0376(10) 0.7502(9) 0.057(4) Uiso 0.290(12) 1 d PD A 2 Co Co 0.5000 0.0000 0.5000 0.0324(2) Uani 1 2 d S . . N11 N 0.3883(3) -0.1017(2) 0.3894(3) 0.0356(8) Uani 1 1 d . A . O1 O 0.2020(3) 0.2256(2) -0.0413(2) 0.0484(8) Uani 1 1 d . . . O2 O -0.0916(3) 0.26174(19) -0.5550(2) 0.0473(8) Uani 1 1 d . . . N7 N 0.4193(3) 0.0901(2) 0.3515(3) 0.0379(8) Uani 1 1 d . A . C8 C 0.0286(3) 0.2655(3) -0.3534(3) 0.0360(9) Uani 1 1 d . . . C9 C 0.1456(3) 0.2727(3) -0.1413(3) 0.0371(9) Uani 1 1 d . . . C10 C 0.0913(3) 0.2225(3) -0.2453(3) 0.0349(9) Uani 1 1 d . . . C12 C 0.2564(4) 0.2702(3) 0.0675(3) 0.0398(10) Uani 1 1 d . . . H12A H 0.2044 0.3033 0.0879 0.048 Uiso 1 1 calc R . . H12B H 0.3093 0.3098 0.0591 0.048 Uiso 1 1 calc R . . C13 C -0.0281(3) 0.2154(3) -0.4566(3) 0.0383(9) Uani 1 1 d . . . C14 C 0.3128(3) 0.2060(3) 0.1645(3) 0.0368(9) Uani 1 1 d . . . C15 C 0.2401(3) -0.2203(3) 0.2388(3) 0.0396(10) Uani 1 1 d . . . C16 C 0.1406(4) 0.3609(3) -0.1451(4) 0.0424(10) Uani 1 1 d . . . H16 H 0.1765 0.3931 -0.0763 0.051 Uiso 1 1 calc R . . C17 C 0.0457(4) 0.0864(3) -0.3462(4) 0.0476(11) Uani 1 1 d . . . H17 H 0.0529 0.0269 -0.3450 0.057 Uiso 1 1 calc R . . C18 C 0.0982(4) 0.1315(3) -0.2444(4) 0.0447(11) Uani 1 1 d . . . H18 H 0.1390 0.1027 -0.1738 0.054 Uiso 1 1 calc R . . C19 C -0.1599(4) 0.2159(3) -0.6574(4) 0.0473(11) Uani 1 1 d . . . H19A H -0.1980 0.1704 -0.6348 0.057 Uiso 1 1 calc R . . H19B H -0.1172 0.1902 -0.6976 0.057 Uiso 1 1 calc R . . C20 C -0.0196(4) 0.1275(3) -0.4538(4) 0.0433(10) Uani 1 1 d . . . H20 H -0.0566 0.0952 -0.5222 0.052 Uiso 1 1 calc R . . C21 C 0.0260(4) 0.3571(3) -0.3560(4) 0.0427(10) Uani 1 1 d . . . H21 H -0.0130 0.3859 -0.4271 0.051 Uiso 1 1 calc R . . C22 C 0.3467(4) -0.2176(3) 0.2497(4) 0.0500(12) Uani 1 1 d . A . H22 H 0.3710 -0.2558 0.2066 0.060 Uiso 1 1 calc R . . C23 C 0.4167(4) -0.1586(3) 0.3243(4) 0.0433(10) Uani 1 1 d . . . H23 H 0.4883 -0.1580 0.3300 0.052 Uiso 1 1 calc R A . C24 C 0.0806(4) 0.4021(3) -0.2542(4) 0.0470(11) Uani 1 1 d . . . H24 H 0.0782 0.4620 -0.2568 0.056 Uiso 1 1 calc R . . C25 C 0.4190(4) 0.1754(3) 0.3697(4) 0.0498(12) Uani 1 1 d . . . H25 H 0.4555 0.1961 0.4471 0.060 Uiso 1 1 calc R A . C26 C 0.2846(4) -0.1046(4) 0.3776(4) 0.0541(13) Uani 1 1 d . . . H26 H 0.2620 -0.0662 0.4220 0.065 Uiso 1 1 calc R A . C28 C 0.3120(5) 0.1193(3) 0.1453(4) 0.0596(14) Uani 1 1 d . A . H28 H 0.2750 0.0971 0.0689 0.072 Uiso 1 1 calc R . . C30 C 0.2093(4) -0.1613(4) 0.3031(5) 0.0559(13) Uani 1 1 d . A . H30 H 0.1375 -0.1595 0.2965 0.067 Uiso 1 1 calc R . . C31 C 0.3679(4) 0.2335(3) 0.2804(4) 0.0509(12) Uani 1 1 d . A . H31 H 0.3704 0.2919 0.2983 0.061 Uiso 1 1 calc R . . C32 C 0.3660(5) 0.0646(3) 0.2397(4) 0.0599(14) Uani 1 1 d . . . H32 H 0.3649 0.0060 0.2235 0.072 Uiso 1 1 calc R A . C1S C 0.3609(8) -0.0599(7) -0.0566(10) 0.134(4) Uani 1 1 d . . . H10S H 0.3460 -0.0450 -0.1392 0.161 Uiso 1 1 calc R . . H11S H 0.3846 -0.0076 -0.0098 0.161 Uiso 1 1 calc R . . Cl1 Cl 0.4628(3) -0.1275(3) -0.0118(5) 0.229(2) Uani 1 1 d . . . Cl2 Cl 0.2420(3) -0.0909(2) -0.0493(3) 0.1673(13) 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 N1 0.064(3) 0.065(3) 0.052(2) 0.002(2) 0.029(2) 0.006(2) O11 0.0476(17) 0.0407(17) 0.0403(16) 0.0036(13) 0.0196(14) 0.0032(14) O12 0.128(6) 0.053(4) 0.078(4) 0.006(3) 0.043(4) -0.036(4) O13 0.43(2) 0.100(7) 0.184(10) 0.060(7) 0.245(14) 0.115(10) Co 0.0329(4) 0.0344(4) 0.0232(4) 0.0012(3) 0.0036(3) 0.0016(3) N11 0.0346(18) 0.0396(19) 0.0240(15) -0.0023(14) 0.0021(13) -0.0010(14) O1 0.062(2) 0.0394(17) 0.0260(14) 0.0051(12) -0.0022(14) 0.0020(14) O2 0.0531(19) 0.0400(17) 0.0286(15) 0.0059(12) -0.0057(13) 0.0039(14) N7 0.0399(19) 0.042(2) 0.0258(16) 0.0036(14) 0.0059(14) 0.0029(15) C8 0.034(2) 0.040(2) 0.0284(19) 0.0063(16) 0.0066(16) 0.0065(17) C9 0.039(2) 0.038(2) 0.0275(19) 0.0070(16) 0.0056(17) 0.0028(17) C10 0.035(2) 0.036(2) 0.0283(19) 0.0068(16) 0.0066(16) 0.0047(16) C12 0.045(2) 0.042(2) 0.0247(19) 0.0056(17) 0.0049(17) -0.0003(18) C13 0.039(2) 0.041(2) 0.0264(19) 0.0042(17) 0.0036(17) 0.0073(18) C14 0.037(2) 0.043(2) 0.0270(19) 0.0055(17) 0.0080(16) 0.0020(17) C15 0.041(2) 0.040(2) 0.0249(19) 0.0005(17) -0.0005(17) -0.0010(18) C16 0.047(2) 0.039(2) 0.031(2) -0.0010(17) 0.0049(18) -0.0005(19) C17 0.058(3) 0.034(2) 0.043(2) 0.0033(19) 0.012(2) 0.009(2) C18 0.052(3) 0.040(2) 0.031(2) 0.0108(18) 0.0052(19) 0.009(2) C19 0.047(3) 0.043(2) 0.034(2) 0.0000(19) -0.0029(19) 0.004(2) C20 0.051(3) 0.039(2) 0.033(2) -0.0021(18) 0.0073(19) 0.0063(19) C21 0.050(3) 0.036(2) 0.032(2) 0.0083(17) 0.0048(19) 0.0056(19) C22 0.046(3) 0.056(3) 0.043(2) -0.015(2) 0.012(2) -0.001(2) C23 0.036(2) 0.046(3) 0.043(2) -0.010(2) 0.0097(19) -0.0010(18) C24 0.054(3) 0.033(2) 0.042(2) 0.0053(19) 0.007(2) 0.0039(19) C25 0.059(3) 0.048(3) 0.025(2) 0.0005(19) -0.0020(19) -0.002(2) C26 0.045(3) 0.066(3) 0.049(3) -0.025(2) 0.016(2) -0.008(2) C28 0.082(4) 0.049(3) 0.025(2) -0.0016(19) -0.003(2) 0.001(3) C30 0.035(2) 0.072(3) 0.057(3) -0.020(3) 0.014(2) -0.009(2) C31 0.068(3) 0.035(2) 0.034(2) 0.0022(18) 0.003(2) 0.001(2) C32 0.087(4) 0.040(3) 0.032(2) 0.002(2) 0.001(2) 0.006(3) C1S 0.144(8) 0.118(8) 0.162(10) 0.039(7) 0.082(8) 0.012(7) Cl1 0.148(3) 0.149(3) 0.300(5) 0.044(3) -0.010(3) 0.021(2) Cl2 0.156(3) 0.183(3) 0.185(3) -0.043(3) 0.091(2) -0.062(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 N1 O12B 1.192(10) . ? N1 O13 1.193(7) . ? N1 O12 1.237(6) . ? N1 O11 1.254(5) . ? N1 O13B 1.265(10) . ? O11 Co 2.082(3) . ? Co O11 2.082(3) 3_656 ? Co N7 2.201(3) . ? Co N7 2.201(3) 3_656 ? Co N11 2.225(3) . ? Co N11 2.225(3) 3_656 ? N11 C26 1.334(6) . ? N11 C23 1.335(6) . ? O1 C9 1.363(5) . ? O1 C12 1.414(5) . ? O2 C13 1.368(5) . ? O2 C19 1.412(5) . ? N7 C32 1.322(6) . ? N7 C25 1.344(6) . ? C8 C13 1.416(6) . ? C8 C10 1.418(5) . ? C8 C21 1.422(6) . ? C9 C16 1.372(6) . ? C9 C10 1.418(6) . ? C10 C18 1.416(6) . ? C12 C14 1.501(6) . ? C13 C20 1.370(6) . ? C14 C28 1.367(7) . ? C14 C31 1.376(6) . ? C15 C30 1.368(7) . ? C15 C22 1.375(6) . ? C15 C19 1.508(6) 2_544 ? C16 C24 1.405(6) . ? C17 C18 1.353(6) . ? C17 C20 1.407(6) . ? C19 C15 1.508(6) 2_554 ? C21 C24 1.357(6) . ? C22 C23 1.368(6) . ? C25 C31 1.369(6) . ? C26 C30 1.375(7) . ? C28 C32 1.380(6) . ? C1S Cl1 1.633(10) . ? C1S Cl2 1.694(10) . ? 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 O13 N1 O12 119.6(6) . . ? O12B N1 O11 122.0(8) . . ? O13 N1 O11 120.2(6) . . ? O12 N1 O11 120.1(5) . . ? O12B N1 O13B 119.0(9) . . ? O11 N1 O13B 111.7(6) . . ? N1 O11 Co 129.6(3) . . ? O11 Co O11 180.0 3_656 . ? O11 Co N7 93.90(12) 3_656 . ? O11 Co N7 86.10(12) . . ? O11 Co N7 86.10(12) 3_656 3_656 ? O11 Co N7 93.90(12) . 3_656 ? N7 Co N7 180.00(14) . 3_656 ? O11 Co N11 88.64(12) 3_656 . ? O11 Co N11 91.36(12) . . ? N7 Co N11 87.69(13) . . ? N7 Co N11 92.31(13) 3_656 . ? O11 Co N11 91.36(12) 3_656 3_656 ? O11 Co N11 88.64(12) . 3_656 ? N7 Co N11 92.31(13) . 3_656 ? N7 Co N11 87.69(13) 3_656 3_656 ? N11 Co N11 180.00(13) . 3_656 ? C26 N11 C23 115.8(4) . . ? C26 N11 Co 120.7(3) . . ? C23 N11 Co 123.3(3) . . ? C9 O1 C12 118.1(3) . . ? C13 O2 C19 118.0(3) . . ? C32 N7 C25 115.4(4) . . ? C32 N7 Co 123.0(3) . . ? C25 N7 Co 121.6(3) . . ? C13 C8 C10 118.5(4) . . ? C13 C8 C21 122.0(4) . . ? C10 C8 C21 119.5(4) . . ? O1 C9 C16 124.6(4) . . ? O1 C9 C10 114.2(4) . . ? C16 C9 C10 121.2(4) . . ? C18 C10 C8 119.4(4) . . ? C18 C10 C9 122.2(3) . . ? C8 C10 C9 118.4(4) . . ? O1 C12 C14 108.9(3) . . ? O2 C13 C20 124.3(4) . . ? O2 C13 C8 114.6(4) . . ? C20 C13 C8 121.0(4) . . ? C28 C14 C31 116.4(4) . . ? C28 C14 C12 123.6(4) . . ? C31 C14 C12 120.0(4) . . ? C30 C15 C22 117.0(4) . . ? C30 C15 C19 121.3(4) . 2_544 ? C22 C15 C19 121.7(4) . 2_544 ? C9 C16 C24 119.3(4) . . ? C18 C17 C20 121.6(4) . . ? C17 C18 C10 120.0(4) . . ? O2 C19 C15 107.1(4) . 2_554 ? C13 C20 C17 119.3(4) . . ? C24 C21 C8 119.7(4) . . ? C23 C22 C15 119.8(4) . . ? N11 C23 C22 123.8(4) . . ? C21 C24 C16 121.9(4) . . ? N7 C25 C31 123.5(4) . . ? N11 C26 C30 123.5(4) . . ? C14 C28 C32 119.9(4) . . ? C15 C30 C26 120.0(4) . . ? C25 C31 C14 120.4(4) . . ? N7 C32 C28 124.4(5) . . ? Cl1 C1S Cl2 118.3(6) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.731 _refine_diff_density_min -1.187 _refine_diff_density_rms 0.089 data_4 _database_code_CSD 173816 _diffrn_measurement_domega 0.30 _diffrn_measurement_rtime 30.15 _chemical_formula_sum 'C120 H120 Co N14 O18' _chemical_formula_weight 2105.23 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' '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' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.554(5) _cell_length_b 18.420(5) _cell_length_c 23.888(5) _cell_angle_alpha 89.018(5) _cell_angle_beta 87.264(5) _cell_angle_gamma 87.106(5) _cell_volume 5510(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5697 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.269 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2218 _exptl_absorpt_coefficient_mu 0.230 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 1.00 _exptl_absorpt_correction_T_max 0.20 _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 SMART _diffrn_detector_type CCD_plate _diffrn_measurement_method omega-scan _diffrn_standards_decay_% 0 _diffrn_reflns_number 40207 _diffrn_reflns_av_R_equivalents 0.0635 _diffrn_reflns_av_sigmaI/netI 0.1214 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 0.85 _diffrn_reflns_theta_max 25.93 _reflns_number_total 18283 _reflns_number_observed 8014 _reflns_observed_criterion >2sigma(I) _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SCHAKAL _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^)+(0.0529P)^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_number_reflns 18283 _refine_ls_number_parameters 1382 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1080 _refine_ls_R_factor_obs 0.0482 _refine_ls_wR_factor_all 0.1183 _refine_ls_wR_factor_obs 0.1038 _refine_ls_goodness_of_fit_all 0.733 _refine_ls_restrained_S_all 0.733 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.002 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 0.26704(3) -0.49727(2) 0.247506(17) 0.04264(13) Uani 1 1 d . . . O1 O 0.40567(14) -0.44784(9) 0.27148(8) 0.0565(6) Uani 1 1 d . . . H1A H 0.4673 -0.4712 0.2528 0.085 Uiso 1 1 d R . . H1B H 0.4112 -0.4530 0.3113 0.085 Uiso 1 1 d R . . O2 O 0.12853(14) -0.54949(10) 0.22364(8) 0.0569(6) Uani 1 1 d . . . H2A H 0.1190 -0.5409 0.1844 0.085 Uiso 1 1 d R . . H2B H 0.0672 -0.5298 0.2449 0.085 Uiso 1 1 d R . . O3 O 0.19420(14) -0.48880(10) 0.32839(8) 0.0591(6) Uani 1 1 d . . . H3A H 0.2443 -0.5057 0.3554 0.089 Uiso 1 1 d R . . H3B H 0.1332 -0.5183 0.3309 0.089 Uiso 1 1 d R . . O4 O 0.33951(15) -0.50513(10) 0.16620(8) 0.0610(6) Uani 1 1 d . . . H4A H 0.2850 -0.5062 0.1394 0.091 Uiso 1 1 d R . . H4B H 0.3815 -0.4636 0.1587 0.091 Uiso 1 1 d R . . N1 N 0.33949(18) -0.60100(13) 0.26638(11) 0.0475(7) Uani 1 1 d . . . N2 N 0.7039(2) -1.39356(14) 0.50239(13) 0.0631(8) Uani 1 1 d . . . C1 C 0.3294(2) -0.65721(17) 0.23242(13) 0.0541(9) Uani 1 1 d . . . H1 H 0.2981 -0.6478 0.1984 0.065 Uiso 1 1 calc R . . C2 C 0.3622(2) -0.72778(16) 0.24456(14) 0.0575(9) Uani 1 1 d . . . H2 H 0.3534 -0.7643 0.2190 0.069 Uiso 1 1 calc R . . C3 C 0.4082(2) -0.74406(17) 0.29480(15) 0.0545(9) Uani 1 1 d . . . C4 C 0.4233(2) -0.68580(18) 0.32973(14) 0.0617(9) Uani 1 1 d . . . H4 H 0.4569 -0.6939 0.3633 0.074 Uiso 1 1 calc R . . C5 C 0.3883(2) -0.61568(16) 0.31456(13) 0.0579(9) Uani 1 1 d . . . H5 H 0.3990 -0.5777 0.3385 0.070 Uiso 1 1 calc R . . C6 C 0.4368(2) -0.82082(17) 0.30838(15) 0.0626(10) Uani 1 1 d . . . H6 H 0.4282 -0.8547 0.2807 0.075 Uiso 1 1 calc R . . C7 C 0.4731(2) -0.84537(17) 0.35562(15) 0.0639(10) Uani 1 1 d . . . H7 H 0.4841 -0.8113 0.3828 0.077 Uiso 1 1 calc R . . C8 C 0.4984(2) -0.92308(17) 0.37018(14) 0.0507(9) Uani 1 1 d . . . C9 C 0.5451(2) -0.93920(16) 0.42072(14) 0.0583(9) Uani 1 1 d . . . H9 H 0.5573 -0.9017 0.4448 0.070 Uiso 1 1 calc R . . C10 C 0.5737(2) -1.01011(18) 0.43586(13) 0.0576(9) Uani 1 1 d . . . H10 H 0.6056 -1.0195 0.4698 0.069 Uiso 1 1 calc R . . C11 C 0.5554(2) -1.06782(16) 0.40106(14) 0.0495(8) Uani 1 1 d . . . C12 C 0.5085(2) -1.05156(16) 0.35044(13) 0.0553(9) Uani 1 1 d . . . H12 H 0.4963 -1.0890 0.3262 0.066 Uiso 1 1 calc R . . C13 C 0.4798(2) -0.98064(18) 0.33558(14) 0.0569(9) Uani 1 1 d . . . H13 H 0.4474 -0.9712 0.3018 0.068 Uiso 1 1 calc R . . C14 C 0.5827(2) -1.14483(16) 0.41489(14) 0.0576(9) Uani 1 1 d . . . H14 H 0.5669 -1.1787 0.3885 0.069 Uiso 1 1 calc R . . C15 C 0.6264(2) -1.17045(17) 0.45995(15) 0.0641(10) Uani 1 1 d . . . H15 H 0.6435 -1.1369 0.4864 0.077 Uiso 1 1 calc R . . C16 C 0.7244(3) -1.3390(2) 0.53508(15) 0.0681(10) Uani 1 1 d . . . H16 H 0.7576 -1.3500 0.5684 0.082 Uiso 1 1 calc R . . C17 C 0.6993(2) -1.26686(17) 0.52273(14) 0.0640(10) Uani 1 1 d . . . H17 H 0.7144 -1.2310 0.5477 0.077 Uiso 1 1 calc R . . C18 C 0.6515(2) -1.24805(17) 0.47288(14) 0.0526(9) Uani 1 1 d . . . C19 C 0.6307(2) -1.30499(17) 0.43883(14) 0.0581(9) Uani 1 1 d . . . H19 H 0.5980 -1.2955 0.4052 0.070 Uiso 1 1 calc R . . C20 C 0.6580(2) -1.37634(17) 0.45429(14) 0.0613(9) Uani 1 1 d . . . H20 H 0.6437 -1.4135 0.4303 0.074 Uiso 1 1 calc R . . N3 N 0.19246(18) -0.39376(13) 0.22863(10) 0.0472(7) Uani 1 1 d . . . N4 N -0.2285(2) 0.39021(14) -0.00185(12) 0.0611(8) Uani 1 1 d . . . C21 C 0.1997(2) -0.33724(17) 0.26272(13) 0.0536(8) Uani 1 1 d . . . H21 H 0.2319 -0.3459 0.2966 0.064 Uiso 1 1 calc R . . C22 C 0.1629(2) -0.26782(16) 0.25094(14) 0.0564(9) Uani 1 1 d . . . H22 H 0.1702 -0.2312 0.2766 0.068 Uiso 1 1 calc R . . C23 C 0.1148(2) -0.25194(17) 0.20072(14) 0.0514(9) Uani 1 1 d . . . C24 C 0.1037(2) -0.31024(17) 0.16573(13) 0.0567(9) Uani 1 1 d . . . H24 H 0.0698 -0.3029 0.1322 0.068 Uiso 1 1 calc R . . C25 C 0.1428(2) -0.37934(16) 0.18053(13) 0.0538(9) Uani 1 1 d . . . H25 H 0.1344 -0.4174 0.1563 0.065 Uiso 1 1 calc R . . C26 C 0.0822(2) -0.17617(17) 0.18753(14) 0.0608(9) Uani 1 1 d . . . H26 H 0.0929 -0.1420 0.2147 0.073 Uiso 1 1 calc R . . C27 C 0.0399(2) -0.15177(16) 0.14162(14) 0.0575(9) Uani 1 1 d . . . H27 H 0.0264 -0.1861 0.1151 0.069 Uiso 1 1 calc R . . C28 C 0.0110(2) -0.07459(16) 0.12748(14) 0.0498(9) Uani 1 1 d . . . C29 C 0.0297(2) -0.01662(17) 0.16141(13) 0.0542(9) Uani 1 1 d . . . H29 H 0.0637 -0.0254 0.1948 0.065 Uiso 1 1 calc R . . C30 C -0.0015(2) 0.05399(16) 0.14660(13) 0.0523(8) Uani 1 1 d . . . H30 H 0.0121 0.0919 0.1701 0.063 Uiso 1 1 calc R . . C31 C -0.0533(2) 0.06920(16) 0.09657(14) 0.0469(8) Uani 1 1 d . . . C32 C -0.0722(2) 0.01056(17) 0.06315(13) 0.0550(9) Uani 1 1 d . . . H32 H -0.1072 0.0189 0.0300 0.066 Uiso 1 1 calc R . . C33 C -0.0403(2) -0.05987(16) 0.07798(13) 0.0563(9) Uani 1 1 d . . . H33 H -0.0533 -0.0979 0.0545 0.068 Uiso 1 1 calc R . . C34 C -0.0839(2) 0.14512(16) 0.08288(13) 0.0539(9) Uani 1 1 d . . . H34 H -0.0653 0.1798 0.1080 0.065 Uiso 1 1 calc R . . C35 C -0.1345(2) 0.16940(16) 0.03913(14) 0.0597(9) Uani 1 1 d . . . H35 H -0.1538 0.1351 0.0138 0.072 Uiso 1 1 calc R . . C36 C -0.1766(2) 0.37462(17) 0.04473(14) 0.0607(9) Uani 1 1 d . . . H36 H -0.1621 0.4124 0.0681 0.073 Uiso 1 1 calc R . . C37 C -0.1436(2) 0.30400(18) 0.05963(14) 0.0578(9) Uani 1 1 d . . . H37 H -0.1075 0.2955 0.0924 0.069 Uiso 1 1 calc R . . C38 C -0.1637(2) 0.24665(17) 0.02634(14) 0.0524(9) Uani 1 1 d . . . C39 C -0.2175(2) 0.26343(17) -0.02212(14) 0.0610(9) Uani 1 1 d . . . H39 H -0.2331 0.2269 -0.0464 0.073 Uiso 1 1 calc R . . C40 C -0.2475(2) 0.33480(19) -0.03377(14) 0.0621(9) Uani 1 1 d . . . H40 H -0.2835 0.3447 -0.0664 0.075 Uiso 1 1 calc R . . N5 N 0.0130(2) 0.34806(15) 0.36335(12) 0.0668(8) Uani 1 1 d . . . N6 N 0.3721(3) -0.44092(17) 0.61441(16) 0.0901(10) Uani 1 1 d . . . C41 C -0.0244(3) 0.33073(19) 0.41424(15) 0.0714(10) Uani 1 1 d . . . H41 H -0.0696 0.3645 0.4332 0.086 Uiso 1 1 calc R . . C42 C -0.0003(3) 0.26584(19) 0.44058(14) 0.0676(10) Uani 1 1 d . . . H42 H -0.0292 0.2568 0.4764 0.081 Uiso 1 1 calc R . . C43 C 0.0661(3) 0.21387(17) 0.41472(15) 0.0558(9) Uani 1 1 d . . . C44 C 0.1060(3) 0.23062(18) 0.36122(15) 0.0646(10) Uani 1 1 d . . . H44 H 0.1511 0.1976 0.3413 0.078 Uiso 1 1 calc R . . C45 C 0.0768(3) 0.2984(2) 0.33794(14) 0.0703(10) Uani 1 1 d . . . H45 H 0.1042 0.3093 0.3021 0.084 Uiso 1 1 calc R . . C46 C 0.0905(3) 0.14383(19) 0.44583(15) 0.0682(10) Uani 1 1 d . . . H46 H 0.0573 0.1389 0.4812 0.082 Uiso 1 1 calc R . . C47 C 0.1513(3) 0.09075(19) 0.42910(15) 0.0673(10) Uani 1 1 d . . . H47 H 0.1845 0.0956 0.3937 0.081 Uiso 1 1 calc R . . C48 C 0.1753(2) 0.02137(17) 0.46009(14) 0.0524(9) Uani 1 1 d . . . C49 C 0.1335(2) 0.00576(17) 0.51406(14) 0.0605(9) Uani 1 1 d . . . H49 H 0.0886 0.0401 0.5326 0.073 Uiso 1 1 calc R . . C50 C 0.1580(2) -0.05978(18) 0.53991(14) 0.0602(9) Uani 1 1 d . . . H50 H 0.1283 -0.0690 0.5756 0.072 Uiso 1 1 calc R . . C51 C 0.2254(3) -0.11228(17) 0.51457(14) 0.0541(9) Uani 1 1 d . . . C52 C 0.2665(3) -0.09808(17) 0.46111(15) 0.0636(10) Uani 1 1 d . . . H52 H 0.3106 -0.1330 0.4426 0.076 Uiso 1 1 calc R . . C53 C 0.2424(3) -0.03161(19) 0.43463(14) 0.0649(10) Uani 1 1 d . . . H53 H 0.2721 -0.0226 0.3989 0.078 Uiso 1 1 calc R . . C54 C 0.2489(3) -0.18180(18) 0.54592(15) 0.0667(10) Uani 1 1 d . . . H54 H 0.2136 -0.1863 0.5808 0.080 Uiso 1 1 calc R . . C55 C 0.3108(3) -0.23568(19) 0.53115(15) 0.0715(10) Uani 1 1 d . . . H55 H 0.3475 -0.2310 0.4966 0.086 Uiso 1 1 calc R . . C56 C 0.3089(3) -0.3893(2) 0.63738(16) 0.0821(11) Uani 1 1 d . . . H56 H 0.2764 -0.3994 0.6723 0.099 Uiso 1 1 calc R . . C57 C 0.2869(3) -0.32230(18) 0.61417(14) 0.0678(10) Uani 1 1 d . . . H57 H 0.2420 -0.2886 0.6335 0.081 Uiso 1 1 calc R . . C58 C 0.3315(3) -0.30437(17) 0.56191(15) 0.0584(9) Uani 1 1 d . . . C59 C 0.3992(3) -0.3580(2) 0.53729(15) 0.0738(11) Uani 1 1 d . . . H59 H 0.4327 -0.3497 0.5024 0.089 Uiso 1 1 calc R . . C60 C 0.4167(3) -0.4240(2) 0.5651(2) 0.0890(13) Uani 1 1 d . . . H60 H 0.4630 -0.4587 0.5478 0.107 Uiso 1 1 calc R . . N7 N -0.0909(2) 0.37821(15) 0.55900(11) 0.0656(8) Uani 1 1 d . . . N8 N 0.2942(2) -0.40902(15) 0.80070(11) 0.0662(8) Uani 1 1 d . . . C61 C -0.1451(3) 0.31997(19) 0.57255(13) 0.0618(9) Uani 1 1 d . . . H61 H -0.2184 0.3230 0.5681 0.074 Uiso 1 1 calc R . . C62 C -0.1005(2) 0.25493(16) 0.59285(13) 0.0562(9) Uani 1 1 d . . . H62 H -0.1430 0.2159 0.6012 0.067 Uiso 1 1 calc R . . C63 C 0.0090(2) 0.24905(17) 0.60049(12) 0.0499(8) Uani 1 1 d . . . C64 C 0.0662(3) 0.30978(17) 0.58644(13) 0.0622(9) Uani 1 1 d . . . H64 H 0.1396 0.3086 0.5904 0.075 Uiso 1 1 calc R . . C65 C 0.0138(3) 0.37197(18) 0.56658(14) 0.0714(10) Uani 1 1 d . . . H65 H 0.0540 0.4121 0.5579 0.086 Uiso 1 1 calc R . . C66 C 0.0626(2) 0.18228(16) 0.62203(13) 0.0563(9) Uani 1 1 d . . . H66 H 0.1367 0.1815 0.6226 0.068 Uiso 1 1 calc R . . C67 C 0.0159(2) 0.12323(16) 0.64074(12) 0.0536(9) Uani 1 1 d . . . H67 H -0.0582 0.1251 0.6403 0.064 Uiso 1 1 calc R . . C68 C 0.0663(2) 0.05482(16) 0.66218(12) 0.0472(8) Uani 1 1 d . . . C69 C 0.0022(2) -0.00212(16) 0.67823(12) 0.0508(8) Uani 1 1 d . . . H69 H -0.0714 0.0042 0.6757 0.061 Uiso 1 1 calc R . . C70 C 0.0451(2) -0.06800(16) 0.69787(12) 0.0512(8) Uani 1 1 d . . . H70 H 0.0002 -0.1050 0.7083 0.061 Uiso 1 1 calc R . . C71 C 0.1552(2) -0.07919(16) 0.70217(12) 0.0463(8) Uani 1 1 d . . . C72 C 0.2192(2) -0.02226(17) 0.68592(13) 0.0555(9) Uani 1 1 d . . . H72 H 0.2928 -0.0286 0.6882 0.067 Uiso 1 1 calc R . . C73 C 0.1761(2) 0.04366(16) 0.66643(13) 0.0563(9) Uani 1 1 d . . . H73 H 0.2210 0.0808 0.6561 0.068 Uiso 1 1 calc R . . C74 C 0.2045(2) -0.14788(16) 0.72328(12) 0.0536(9) Uani 1 1 d . . . H74 H 0.2787 -0.1511 0.7230 0.064 Uiso 1 1 calc R . . C75 C 0.1546(2) -0.20587(16) 0.74274(13) 0.0562(9) Uani 1 1 d . . . H75 H 0.0803 -0.2026 0.7433 0.067 Uiso 1 1 calc R . . C76 C 0.1900(3) -0.39832(17) 0.79485(14) 0.0710(10) Uani 1 1 d . . . H76 H 0.1464 -0.4367 0.8034 0.085 Uiso 1 1 calc R . . C77 C 0.1424(2) -0.33261(18) 0.77651(13) 0.0651(10) Uani 1 1 d . . . H77 H 0.0689 -0.3280 0.7731 0.078 Uiso 1 1 calc R . . C78 C 0.2045(2) -0.27445(17) 0.76340(12) 0.0489(8) Uani 1 1 d . . . C79 C 0.3136(2) -0.28582(17) 0.76964(14) 0.0657(10) Uani 1 1 d . . . H79 H 0.3594 -0.2485 0.7615 0.079 Uiso 1 1 calc R . . C80 C 0.3539(3) -0.35308(19) 0.78803(14) 0.0700(10) Uani 1 1 d . . . H80 H 0.4272 -0.3594 0.7917 0.084 Uiso 1 1 calc R . . N9 N 0.0808(2) -0.55589(15) -0.09384(14) 0.0693(8) Uani 1 1 d . . . N10 N 0.5161(2) -1.33986(14) 0.13475(12) 0.0628(8) Uani 1 1 d . . . C81 C 0.0570(3) -0.58974(19) -0.04478(16) 0.0741(11) Uani 1 1 d . . . H81 H 0.0112 -0.5654 -0.0188 0.089 Uiso 1 1 calc R . . C82 C 0.0970(3) -0.65891(18) -0.03079(15) 0.0677(10) Uani 1 1 d . . . H82 H 0.0777 -0.6797 0.0037 0.081 Uiso 1 1 calc R . . C83 C 0.1654(2) -0.69694(17) -0.06803(15) 0.0549(9) Uani 1 1 d . . . C84 C 0.1895(3) -0.66151(19) -0.11839(15) 0.0693(10) Uani 1 1 d . . . H84 H 0.2350 -0.6844 -0.1453 0.083 Uiso 1 1 calc R . . C85 C 0.1469(3) -0.5933(2) -0.12870(15) 0.0770(11) Uani 1 1 d . . . H85 H 0.1658 -0.5713 -0.1628 0.092 Uiso 1 1 calc R . . C86 C 0.2129(2) -0.77065(17) -0.05787(15) 0.0625(9) Uani 1 1 d . . . H86 H 0.2527 -0.7925 -0.0874 0.075 Uiso 1 1 calc R . . C87 C 0.2039(2) -0.80789(18) -0.01072(14) 0.0609(9) Uani 1 1 d . . . H87 H 0.1625 -0.7859 0.0182 0.073 Uiso 1 1 calc R . . C88 C 0.2523(2) -0.88115(16) 0.00151(14) 0.0493(8) Uani 1 1 d . . . C89 C 0.2296(2) -0.91162(17) 0.05445(14) 0.0573(9) Uani 1 1 d . . . H89 H 0.1857 -0.8857 0.0803 0.069 Uiso 1 1 calc R . . C90 C 0.2716(2) -0.97974(17) 0.06882(13) 0.0565(9) Uani 1 1 d . . . H90 H 0.2542 -0.9992 0.1041 0.068 Uiso 1 1 calc R . . C91 C 0.3386(2) -1.01985(16) 0.03217(14) 0.0494(8) Uani 1 1 d . . . C92 C 0.3617(2) -0.98876(17) -0.02064(13) 0.0592(9) Uani 1 1 d . . . H92 H 0.4062 -1.0145 -0.0464 0.071 Uiso 1 1 calc R . . C93 C 0.3200(2) -0.92115(18) -0.03523(13) 0.0595(9) Uani 1 1 d . . . H93 H 0.3375 -0.9017 -0.0705 0.071 Uiso 1 1 calc R . . C94 C 0.3864(2) -1.09303(17) 0.04516(14) 0.0581(9) Uani 1 1 d . . . H94 H 0.4267 -1.1162 0.0164 0.070 Uiso 1 1 calc R . . C95 C 0.3774(2) -1.12857(17) 0.09335(14) 0.0579(9) Uani 1 1 d . . . H95 H 0.3363 -1.1061 0.1222 0.069 Uiso 1 1 calc R . . C96 C 0.4506(3) -1.30164(18) 0.16922(14) 0.0640(10) Uani 1 1 d . . . H96 H 0.4338 -1.3221 0.2042 0.077 Uiso 1 1 calc R . . C97 C 0.4049(2) -1.23351(17) 0.15733(14) 0.0606(9) Uani 1 1 d . . . H97 H 0.3599 -1.2095 0.1838 0.073 Uiso 1 1 calc R . . C98 C 0.4274(2) -1.20153(16) 0.10533(14) 0.0503(8) Uani 1 1 d . . . C99 C 0.4960(2) -1.24098(18) 0.06910(14) 0.0617(9) Uani 1 1 d . . . H99 H 0.5143 -1.2217 0.0339 0.074 Uiso 1 1 calc R . . C100 C 0.5379(3) -1.30909(18) 0.08465(15) 0.0656(10) Uani 1 1 d . . . H100 H 0.5832 -1.3345 0.0591 0.079 Uiso 1 1 calc R . . N11 N 0.1717(2) -0.58723(15) -0.29691(11) 0.0659(8) Uani 1 1 d . . . N12 N 0.6004(2) -1.36598(15) -0.05766(11) 0.0614(8) Uani 1 1 d . . . C101 C 0.1148(3) -0.64323(19) -0.27965(14) 0.0682(10) Uani 1 1 d . . . H101 H 0.0408 -0.6368 -0.2788 0.082 Uiso 1 1 calc R . . C102 C 0.1579(2) -0.71012(17) -0.26299(13) 0.0639(10) Uani 1 1 d . . . H102 H 0.1136 -0.7471 -0.2517 0.077 Uiso 1 1 calc R . . C103 C 0.2686(2) -0.72155(17) -0.26335(12) 0.0522(8) Uani 1 1 d . . . C104 C 0.3277(2) -0.66360(18) -0.28179(13) 0.0627(9) Uani 1 1 d . . . H104 H 0.4019 -0.6683 -0.2833 0.075 Uiso 1 1 calc R . . C105 C 0.2770(3) -0.59849(18) -0.29808(14) 0.0698(10) Uani 1 1 d . . . H105 H 0.3190 -0.5607 -0.3105 0.084 Uiso 1 1 calc R . . C106 C 0.3230(2) -0.78942(17) -0.24437(12) 0.0554(9) Uani 1 1 d . . . H106 H 0.3972 -0.7917 -0.2477 0.066 Uiso 1 1 calc R . . C107 C 0.2773(2) -0.84789(17) -0.22287(12) 0.0563(9) Uani 1 1 d . . . H107 H 0.2030 -0.8455 -0.2203 0.068 Uiso 1 1 calc R . . C108 C 0.3297(2) -0.91587(17) -0.20265(12) 0.0489(8) Uani 1 1 d . . . C109 C 0.2691(2) -0.97351(17) -0.18447(13) 0.0576(9) Uani 1 1 d . . . H109 H 0.1950 -0.9683 -0.1850 0.069 Uiso 1 1 calc R . . C110 C 0.3157(2) -1.03836(17) -0.16569(13) 0.0581(9) Uani 1 1 d . . . H110 H 0.2726 -1.0760 -0.1543 0.070 Uiso 1 1 calc R . . C111 C 0.4259(2) -1.04828(16) -0.16357(12) 0.0479(8) Uani 1 1 d . . . C112 C 0.4870(2) -0.99114(17) -0.18173(12) 0.0541(9) Uani 1 1 d . . . H112 H 0.5610 -0.9966 -0.1810 0.065 Uiso 1 1 calc R . . C113 C 0.4407(2) -0.92578(16) -0.20109(12) 0.0534(8) Uani 1 1 d . . . H113 H 0.4839 -0.8884 -0.2131 0.064 Uiso 1 1 calc R . . C114 C 0.4801(2) -1.11497(17) -0.14178(12) 0.0533(9) Uani 1 1 d . . . H114 H 0.5543 -1.1156 -0.1429 0.064 Uiso 1 1 calc R . . C115 C 0.4366(2) -1.17418(17) -0.12080(13) 0.0576(9) Uani 1 1 d . . . H115 H 0.3625 -1.1747 -0.1197 0.069 Uiso 1 1 calc R . . C116 C 0.4959(3) -1.36132(18) -0.06284(14) 0.0717(10) Uani 1 1 d . . . H116 H 0.4573 -1.4015 -0.0523 0.086 Uiso 1 1 calc R . . C117 C 0.4407(3) -1.30050(18) -0.08292(14) 0.0664(10) Uani 1 1 d . . . H117 H 0.3671 -1.3006 -0.0856 0.080 Uiso 1 1 calc R . . C118 C 0.4946(2) -1.23920(17) -0.09907(12) 0.0508(8) Uani 1 1 d . . . C119 C 0.6047(2) -1.24352(16) -0.09378(13) 0.0560(9) Uani 1 1 d . . . H119 H 0.6456 -1.2042 -0.1038 0.067 Uiso 1 1 calc R . . C120 C 0.6528(3) -1.30797(19) -0.07322(13) 0.0617(9) Uani 1 1 d . . . H120 H 0.7265 -1.3102 -0.0703 0.074 Uiso 1 1 calc R . . N1S N 0.2054(2) -0.87260(18) 0.22778(14) 0.0666(8) Uani 1 1 d . . . O1S O 0.1360(2) -0.81996(13) 0.22789(10) 0.0828(8) Uani 1 1 d . . . O2S O 0.21306(19) -0.91137(14) 0.27089(12) 0.0907(8) Uani 1 1 d . . . O3S O 0.2634(2) -0.88355(15) 0.18612(11) 0.1038(10) Uani 1 1 d . . . N2S N 0.3690(2) -0.21764(17) 0.33613(14) 0.0649(8) Uani 1 1 d . . . O4S O 0.4295(2) -0.23245(16) 0.29758(12) 0.1159(11) Uani 1 1 d . . . O5S O 0.3688(2) -0.25290(13) 0.38161(11) 0.0872(8) Uani 1 1 d . . . O6S O 0.3016(2) -0.16416(14) 0.33343(11) 0.0874(8) Uani 1 1 d . . . O1A O -0.01082(14) -0.52057(10) 0.31004(8) 0.0678(6) Uani 1 1 d . . . H1A1 H -0.0400 -0.5618 0.3302 0.081 Uiso 1 1 d R . . H1A2 H -0.0614 -0.4795 0.3058 0.081 Uiso 1 1 d R . . O2A O 0.54679(15) -0.47805(11) 0.18184(9) 0.0737(7) Uani 1 1 d . . . H2A1 H 0.5762 -0.4368 0.1618 0.088 Uiso 1 1 d R . . H2A2 H 0.5964 -0.5198 0.1852 0.088 Uiso 1 1 d R . . O3A O 0.06514(16) -0.56493(10) 0.11636(8) 0.0665(6) Uani 1 1 d . . . H3A1 H 0.0105 -0.5284 0.1082 0.100 Uiso 1 1 d R . . H3A3 H 0.1254 -0.5598 0.0906 0.100 Uiso 1 1 d R . . O4A O 0.43020(17) -0.40376(12) 0.37580(9) 0.0851(7) Uani 1 1 d . . . H4A1 H 0.4146 -0.3523 0.3777 0.128 Uiso 1 1 d R . . H4A3 H 0.3820 -0.4284 0.4011 0.128 Uiso 1 1 d R . . O5A O 0.26434(16) -0.47957(10) 0.43461(8) 0.0635(6) Uani 1 1 d . . . H5A1 H 0.2799 -0.5274 0.4496 0.095 Uiso 1 1 d R . . H5A2 H 0.2096 -0.4552 0.4579 0.095 Uiso 1 1 d R . . O6A O 0.25173(15) -0.51858(10) 0.06379(8) 0.0606(6) Uani 1 1 d . . . H6A2 H 0.2961 -0.5519 0.0414 0.091 Uiso 1 1 d R . . H6A3 H 0.2474 -0.4720 0.0451 0.091 Uiso 1 1 d R . . O7A O 0.26926(18) -1.0679(2) 0.23645(12) 0.0988(9) Uani 1 1 d . . . H107' H 0.2708 -1.0238 0.2462 0.14(2) Uiso 1 1 d R . . H207 H 0.2868 -1.0945 0.2643 0.112(18) Uiso 1 1 d R . . O8A O 0.0965(2) -0.73112(13) 0.12815(15) 0.0981(8) Uani 1 1 d . . . H108 H 0.1176 -0.7530 0.1575 0.089(15) Uiso 1 1 d R . . H208 H 0.1444 -0.7386 0.1022 0.36(5) Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co 0.0454(3) 0.0399(2) 0.0418(3) 0.01034(17) -0.0083(2) 0.00726(18) O1 0.0513(12) 0.0598(14) 0.0577(14) 0.0067(11) -0.0041(11) 0.0041(10) O2 0.0512(13) 0.0658(14) 0.0526(14) 0.0094(11) -0.0062(10) 0.0073(10) O3 0.0568(13) 0.0726(15) 0.0476(14) 0.0129(11) -0.0057(11) -0.0024(11) O4 0.0649(14) 0.0674(15) 0.0504(14) 0.0087(11) -0.0020(11) -0.0059(11) N1 0.0494(16) 0.0408(16) 0.0524(19) 0.0085(14) -0.0135(13) 0.0044(12) N2 0.0691(19) 0.0475(19) 0.072(2) 0.0174(17) -0.0071(17) 0.0051(15) C1 0.055(2) 0.048(2) 0.059(2) 0.0095(18) -0.0107(17) 0.0062(17) C2 0.059(2) 0.047(2) 0.066(3) 0.0081(18) -0.0087(19) 0.0030(17) C3 0.054(2) 0.038(2) 0.070(3) 0.0096(19) 0.0036(18) 0.0042(16) C4 0.062(2) 0.063(2) 0.060(2) 0.021(2) -0.0200(18) 0.0079(18) C5 0.068(2) 0.048(2) 0.058(2) 0.0079(17) -0.0194(18) 0.0114(17) C6 0.063(2) 0.051(2) 0.073(3) 0.0086(19) -0.0066(19) 0.0074(17) C7 0.058(2) 0.055(2) 0.077(3) 0.011(2) -0.004(2) 0.0090(17) C8 0.0433(19) 0.041(2) 0.067(3) 0.0147(19) -0.0014(17) 0.0030(16) C9 0.064(2) 0.044(2) 0.067(3) 0.0039(18) -0.0122(19) 0.0042(17) C10 0.059(2) 0.058(2) 0.056(2) 0.0187(19) -0.0155(17) 0.0037(18) C11 0.0454(19) 0.038(2) 0.064(3) 0.0134(18) -0.0025(17) 0.0022(15) C12 0.058(2) 0.047(2) 0.061(2) 0.0079(17) -0.0100(18) -0.0009(16) C13 0.053(2) 0.056(2) 0.062(2) 0.0198(19) -0.0135(17) 0.0011(17) C14 0.056(2) 0.048(2) 0.069(3) 0.0164(18) -0.0046(18) 0.0013(16) C15 0.067(2) 0.049(2) 0.076(3) 0.009(2) -0.009(2) 0.0034(18) C16 0.072(2) 0.065(3) 0.067(3) 0.022(2) -0.020(2) 0.009(2) C17 0.072(2) 0.051(2) 0.069(3) 0.0049(19) -0.016(2) 0.0027(18) C18 0.047(2) 0.041(2) 0.069(3) 0.0170(19) -0.0067(18) 0.0018(16) C19 0.060(2) 0.053(2) 0.062(2) 0.0185(19) -0.0146(18) -0.0009(18) C20 0.068(2) 0.048(2) 0.068(3) 0.0101(19) -0.010(2) -0.0016(17) N3 0.0512(16) 0.0425(17) 0.0478(18) 0.0064(14) -0.0098(13) 0.0037(12) N4 0.0672(19) 0.0446(18) 0.071(2) 0.0184(16) -0.0133(16) 0.0060(14) C21 0.054(2) 0.050(2) 0.058(2) 0.0073(18) -0.0143(17) 0.0047(17) C22 0.059(2) 0.044(2) 0.066(3) 0.0040(17) -0.0129(18) 0.0044(16) C23 0.0449(19) 0.040(2) 0.068(3) 0.0080(19) 0.0015(17) 0.0044(16) C24 0.058(2) 0.056(2) 0.055(2) 0.0184(19) -0.0144(17) 0.0070(17) C25 0.065(2) 0.046(2) 0.050(2) 0.0066(16) -0.0154(18) 0.0072(16) C26 0.063(2) 0.053(2) 0.066(3) 0.0083(19) -0.0104(19) 0.0086(17) C27 0.052(2) 0.050(2) 0.070(3) 0.0109(18) -0.0075(18) 0.0092(16) C28 0.0427(19) 0.042(2) 0.063(2) 0.0132(19) -0.0013(17) 0.0081(16) C29 0.049(2) 0.057(2) 0.056(2) 0.0146(19) -0.0133(17) 0.0035(17) C30 0.052(2) 0.047(2) 0.059(2) 0.0022(17) -0.0103(17) 0.0012(16) C31 0.0412(18) 0.040(2) 0.058(2) 0.0105(17) -0.0008(16) 0.0031(15) C32 0.054(2) 0.055(2) 0.056(2) 0.0160(19) -0.0137(17) 0.0019(17) C33 0.064(2) 0.044(2) 0.062(2) 0.0053(17) -0.0151(18) 0.0043(16) C34 0.052(2) 0.047(2) 0.062(2) 0.0119(17) -0.0049(18) 0.0034(16) C35 0.060(2) 0.050(2) 0.069(3) 0.0067(19) -0.0119(19) 0.0061(17) C36 0.063(2) 0.050(2) 0.070(3) 0.0104(18) -0.0146(19) 0.0003(17) C37 0.054(2) 0.057(2) 0.063(2) 0.0158(19) -0.0183(17) 0.0013(17) C38 0.049(2) 0.040(2) 0.068(3) 0.0138(19) -0.0054(18) 0.0022(16) C39 0.069(2) 0.050(2) 0.064(3) 0.0063(18) -0.0129(19) 0.0052(17) C40 0.063(2) 0.059(3) 0.063(3) 0.019(2) -0.0147(19) 0.0059(19) N5 0.070(2) 0.067(2) 0.062(2) 0.0183(17) -0.0021(17) 0.0176(16) N6 0.108(3) 0.068(2) 0.093(3) 0.012(2) -0.007(2) 0.010(2) C41 0.075(3) 0.070(3) 0.066(3) 0.011(2) 0.002(2) 0.026(2) C42 0.070(2) 0.079(3) 0.052(2) 0.013(2) 0.0036(19) 0.010(2) C43 0.061(2) 0.051(2) 0.056(3) 0.0111(18) -0.0154(19) 0.0020(18) C44 0.069(2) 0.064(2) 0.059(3) -0.0032(19) -0.004(2) 0.0156(19) C45 0.071(2) 0.085(3) 0.053(2) 0.021(2) 0.001(2) 0.010(2) C46 0.070(2) 0.067(3) 0.066(3) 0.002(2) -0.003(2) 0.006(2) C47 0.063(2) 0.071(3) 0.068(3) 0.000(2) -0.009(2) 0.000(2) C48 0.057(2) 0.048(2) 0.053(2) 0.0093(18) -0.0128(18) 0.0004(17) C49 0.067(2) 0.058(2) 0.054(2) -0.0029(18) 0.0012(19) 0.0165(18) C50 0.068(2) 0.062(2) 0.049(2) 0.0091(18) 0.0024(18) 0.0064(19) C51 0.061(2) 0.050(2) 0.051(2) 0.0076(18) -0.0109(18) -0.0005(18) C52 0.070(2) 0.054(2) 0.064(3) -0.0055(19) -0.001(2) 0.0143(18) C53 0.070(2) 0.074(3) 0.050(2) 0.004(2) 0.0056(19) 0.001(2) C54 0.068(2) 0.060(2) 0.072(3) 0.001(2) -0.012(2) 0.001(2) C55 0.070(3) 0.066(3) 0.079(3) 0.001(2) -0.012(2) 0.000(2) C56 0.107(3) 0.070(3) 0.066(3) 0.017(2) 0.004(2) 0.014(2) C57 0.084(3) 0.061(2) 0.056(3) 0.0018(19) 0.003(2) 0.012(2) C58 0.065(2) 0.048(2) 0.062(3) 0.0105(19) -0.017(2) -0.0030(18) C59 0.080(3) 0.071(3) 0.069(3) -0.002(2) 0.014(2) -0.005(2) C60 0.093(3) 0.055(3) 0.116(4) -0.012(3) 0.009(3) 0.017(2) N7 0.073(2) 0.053(2) 0.068(2) 0.0149(15) 0.0077(17) 0.0078(17) N8 0.067(2) 0.062(2) 0.068(2) 0.0202(16) -0.0047(16) 0.0165(17) C61 0.055(2) 0.059(2) 0.069(3) 0.0090(19) 0.0030(18) 0.0138(19) C62 0.057(2) 0.047(2) 0.063(2) 0.0086(17) 0.0068(18) 0.0008(17) C63 0.053(2) 0.052(2) 0.043(2) 0.0062(16) 0.0053(16) 0.0065(17) C64 0.056(2) 0.051(2) 0.078(3) 0.0123(19) 0.0026(19) -0.0028(18) C65 0.076(3) 0.051(2) 0.085(3) 0.016(2) 0.006(2) -0.004(2) C66 0.050(2) 0.050(2) 0.068(2) 0.0086(18) 0.0023(17) 0.0037(17) C67 0.051(2) 0.053(2) 0.055(2) 0.0051(17) 0.0039(17) 0.0105(17) C68 0.048(2) 0.048(2) 0.043(2) 0.0028(16) 0.0037(16) 0.0034(17) C69 0.0430(19) 0.052(2) 0.057(2) 0.0083(17) 0.0021(16) 0.0045(17) C70 0.048(2) 0.048(2) 0.057(2) 0.0138(16) 0.0043(16) -0.0015(16) C71 0.048(2) 0.045(2) 0.045(2) 0.0054(15) 0.0018(16) 0.0019(16) C72 0.0434(19) 0.058(2) 0.065(2) 0.0079(18) -0.0019(17) 0.0048(17) C73 0.052(2) 0.051(2) 0.065(2) 0.0118(18) 0.0025(18) -0.0043(17) C74 0.048(2) 0.055(2) 0.057(2) 0.0072(18) -0.0013(17) 0.0111(17) C75 0.048(2) 0.053(2) 0.065(2) 0.0109(18) 0.0015(17) 0.0104(17) C76 0.070(3) 0.054(2) 0.087(3) 0.024(2) 0.002(2) 0.0036(19) C77 0.050(2) 0.062(2) 0.082(3) 0.022(2) -0.0030(19) 0.0045(19) C78 0.045(2) 0.051(2) 0.049(2) 0.0079(16) -0.0011(16) 0.0072(17) C79 0.055(2) 0.059(2) 0.083(3) 0.0158(19) -0.0087(19) -0.0033(18) C80 0.059(2) 0.067(3) 0.083(3) 0.020(2) -0.015(2) 0.012(2) N9 0.072(2) 0.060(2) 0.074(2) 0.0115(18) -0.0114(18) 0.0138(16) N10 0.0662(19) 0.0570(19) 0.063(2) 0.0164(16) -0.0033(16) 0.0111(15) C81 0.072(3) 0.067(3) 0.080(3) -0.001(2) 0.002(2) 0.017(2) C82 0.071(2) 0.064(3) 0.065(3) 0.012(2) 0.004(2) 0.008(2) C83 0.050(2) 0.052(2) 0.064(3) 0.0004(19) -0.0147(18) 0.0022(17) C84 0.076(2) 0.069(3) 0.060(3) 0.006(2) 0.001(2) 0.021(2) C85 0.086(3) 0.077(3) 0.064(3) 0.018(2) -0.001(2) 0.018(2) C86 0.066(2) 0.064(2) 0.058(3) 0.0032(19) -0.0128(19) 0.0064(18) C87 0.060(2) 0.066(2) 0.059(2) 0.0014(19) -0.0132(19) -0.0071(18) C88 0.050(2) 0.046(2) 0.053(2) 0.0047(17) -0.0131(17) 0.0014(16) C89 0.055(2) 0.061(2) 0.055(2) 0.0024(18) -0.0008(18) 0.0067(17) C90 0.060(2) 0.059(2) 0.049(2) 0.0137(18) 0.0002(18) 0.0034(18) C91 0.049(2) 0.049(2) 0.050(2) 0.0047(18) -0.0079(17) 0.0025(16) C92 0.064(2) 0.062(2) 0.050(2) 0.0000(18) 0.0009(18) 0.0113(18) C93 0.069(2) 0.062(2) 0.047(2) 0.0124(18) -0.0052(18) 0.0034(19) C94 0.062(2) 0.061(2) 0.052(2) 0.0067(18) -0.0098(18) -0.0010(17) C95 0.062(2) 0.060(2) 0.052(2) 0.0046(18) -0.0060(18) -0.0019(17) C96 0.073(2) 0.063(3) 0.055(2) 0.0205(19) -0.002(2) 0.002(2) C97 0.063(2) 0.062(2) 0.055(2) 0.0102(18) 0.0009(18) 0.0050(18) C98 0.049(2) 0.049(2) 0.053(2) 0.0069(18) -0.0101(17) 0.0018(16) C99 0.067(2) 0.070(3) 0.047(2) 0.0197(19) -0.0031(19) 0.0020(19) C100 0.067(2) 0.067(3) 0.061(3) 0.006(2) 0.000(2) 0.0108(19) N11 0.062(2) 0.060(2) 0.074(2) 0.0166(16) -0.0035(16) 0.0102(16) N12 0.065(2) 0.055(2) 0.062(2) 0.0102(15) 0.0029(16) 0.0084(16) C101 0.048(2) 0.075(3) 0.080(3) 0.012(2) -0.0049(19) 0.015(2) C102 0.050(2) 0.062(2) 0.077(3) 0.0185(19) 0.0029(19) 0.0029(18) C103 0.050(2) 0.057(2) 0.049(2) 0.0060(17) -0.0015(16) 0.0069(18) C104 0.051(2) 0.061(2) 0.075(3) 0.0206(19) -0.0010(18) -0.0013(19) C105 0.066(3) 0.058(2) 0.085(3) 0.021(2) -0.005(2) -0.001(2) C106 0.050(2) 0.055(2) 0.059(2) 0.0112(18) 0.0022(17) 0.0047(17) C107 0.047(2) 0.060(2) 0.060(2) 0.0075(18) -0.0028(17) 0.0083(17) C108 0.048(2) 0.052(2) 0.046(2) 0.0049(16) 0.0011(16) 0.0022(17) C109 0.0414(19) 0.065(2) 0.066(2) 0.0142(19) 0.0008(17) 0.0002(18) C110 0.055(2) 0.053(2) 0.065(2) 0.0172(18) 0.0018(18) -0.0038(17) C111 0.045(2) 0.052(2) 0.045(2) 0.0018(16) 0.0032(16) 0.0059(17) C112 0.0433(19) 0.057(2) 0.061(2) 0.0076(18) 0.0000(17) 0.0017(17) C113 0.051(2) 0.050(2) 0.059(2) 0.0081(17) 0.0012(17) -0.0027(16) C114 0.051(2) 0.053(2) 0.055(2) 0.0044(17) 0.0047(17) 0.0069(17) C115 0.048(2) 0.058(2) 0.065(2) 0.0091(19) 0.0023(17) 0.0030(17) C116 0.069(3) 0.058(3) 0.086(3) 0.019(2) 0.010(2) -0.001(2) C117 0.053(2) 0.063(3) 0.081(3) 0.016(2) 0.0055(19) 0.0028(19) C118 0.053(2) 0.051(2) 0.047(2) 0.0069(16) 0.0034(17) 0.0053(17) C119 0.059(2) 0.050(2) 0.059(2) 0.0078(17) -0.0035(18) -0.0033(17) C120 0.056(2) 0.065(3) 0.063(2) 0.0052(19) -0.0071(18) 0.006(2) N1S 0.056(2) 0.075(2) 0.070(3) -0.002(2) 0.0010(19) -0.0168(18) O1S 0.0802(18) 0.0789(19) 0.087(2) 0.0057(15) 0.0073(15) 0.0033(15) O2S 0.0844(18) 0.102(2) 0.083(2) 0.0209(17) 0.0049(16) 0.0028(15) O3S 0.101(2) 0.129(2) 0.077(2) -0.0165(17) 0.0420(17) -0.0006(17) N2S 0.061(2) 0.068(2) 0.067(2) -0.0045(19) -0.0035(19) -0.0114(18) O4S 0.106(2) 0.149(3) 0.087(2) -0.0193(19) 0.0508(19) -0.0009(19) O5S 0.104(2) 0.0784(19) 0.077(2) 0.0107(15) 0.0064(16) 0.0013(14) O6S 0.0934(19) 0.0797(19) 0.088(2) 0.0038(15) -0.0025(16) 0.0010(16) O1A 0.0571(13) 0.0599(15) 0.0835(17) 0.0286(12) 0.0049(12) 0.0083(11) O2A 0.0582(14) 0.0617(15) 0.0973(19) 0.0286(13) 0.0064(13) 0.0151(11) O3A 0.0687(14) 0.0697(15) 0.0604(15) 0.0121(12) -0.0121(12) 0.0093(11) O4A 0.0843(17) 0.0933(19) 0.0788(18) -0.0077(14) -0.0119(14) -0.0052(14) O5A 0.0893(16) 0.0454(13) 0.0533(14) 0.0138(10) -0.0047(12) 0.0182(11) O6A 0.0768(15) 0.0489(13) 0.0536(14) 0.0135(11) -0.0016(12) 0.0153(11) O7A 0.104(2) 0.094(2) 0.100(2) 0.012(2) -0.0227(17) -0.0109(16) O8A 0.099(2) 0.097(2) 0.098(2) 0.0137(18) -0.0090(19) -0.0046(15) _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 O3 2.1027(19) . ? Co O4 2.1091(19) . ? Co O1 2.1116(19) . ? Co N1 2.125(2) . ? Co N3 2.132(2) . ? Co O2 2.1345(19) . ? N1 C1 1.341(3) . ? N1 C5 1.347(3) . ? N2 C16 1.326(4) . ? N2 C20 1.337(4) . ? C1 C2 1.374(4) . ? C2 C3 1.379(4) . ? C3 C4 1.396(4) . ? C3 C6 1.476(4) . ? C4 C5 1.391(4) . ? C6 C7 1.302(4) . ? C7 C8 1.490(4) . ? C8 C9 1.388(4) . ? C8 C13 1.391(4) . ? C9 C10 1.384(4) . ? C10 C11 1.396(4) . ? C11 C12 1.391(4) . ? C11 C14 1.478(4) . ? C12 C13 1.382(4) . ? C14 C15 1.302(4) . ? C15 C18 1.479(4) . ? C16 C17 1.380(4) . ? C17 C18 1.390(4) . ? C18 C19 1.381(4) . ? C19 C20 1.390(4) . ? N3 C21 1.342(3) . ? N3 C25 1.350(3) . ? N4 C40 1.322(4) . ? N4 C36 1.336(4) . ? C21 C22 1.367(4) . ? C22 C23 1.389(4) . ? C23 C24 1.389(4) . ? C23 C26 1.467(4) . ? C24 C25 1.387(4) . ? C26 C27 1.305(4) . ? C27 C28 1.487(4) . ? C28 C29 1.387(4) . ? C28 C33 1.389(4) . ? C29 C30 1.384(4) . ? C30 C31 1.405(4) . ? C31 C32 1.391(4) . ? C31 C34 1.467(4) . ? C32 C33 1.384(4) . ? C34 C35 1.309(4) . ? C35 C38 1.482(4) . ? C36 C37 1.391(4) . ? C37 C38 1.374(4) . ? C38 C39 1.390(4) . ? C39 C40 1.376(4) . ? N5 C41 1.322(4) . ? N5 C45 1.322(4) . ? N6 C56 1.317(4) . ? N6 C60 1.319(5) . ? C41 C42 1.368(4) . ? C42 C43 1.373(4) . ? C43 C44 1.385(4) . ? C43 C46 1.503(4) . ? C44 C45 1.396(4) . ? C46 C47 1.268(4) . ? C47 C48 1.491(4) . ? C48 C53 1.386(4) . ? C48 C49 1.399(4) . ? C49 C50 1.374(4) . ? C50 C51 1.380(4) . ? C51 C52 1.381(4) . ? C51 C54 1.496(4) . ? C52 C53 1.395(4) . ? C54 C55 1.274(4) . ? C55 C58 1.470(4) . ? C56 C57 1.366(4) . ? C57 C58 1.385(4) . ? C58 C59 1.390(4) . ? C59 C60 1.389(5) . ? N7 C61 1.326(4) . ? N7 C65 1.334(4) . ? N8 C80 1.327(4) . ? N8 C76 1.326(4) . ? C61 C62 1.386(4) . ? C62 C63 1.394(4) . ? C63 C64 1.387(4) . ? C63 C66 1.469(4) . ? C64 C65 1.380(4) . ? C66 C67 1.323(4) . ? C67 C68 1.476(4) . ? C68 C69 1.392(4) . ? C68 C73 1.392(4) . ? C69 C70 1.386(3) . ? C70 C71 1.396(4) . ? C71 C72 1.392(4) . ? C71 C74 1.472(4) . ? C72 C73 1.386(4) . ? C74 C75 1.332(4) . ? C75 C78 1.470(4) . ? C76 C77 1.396(4) . ? C77 C78 1.379(4) . ? C78 C79 1.390(4) . ? C79 C80 1.387(4) . ? N9 C85 1.324(4) . ? N9 C81 1.346(4) . ? N10 C96 1.322(4) . ? N10 C100 1.338(4) . ? C81 C82 1.387(4) . ? C82 C83 1.381(4) . ? C83 C84 1.387(4) . ? C83 C86 1.476(4) . ? C84 C85 1.364(4) . ? C86 C87 1.312(4) . ? C87 C88 1.482(4) . ? C88 C93 1.387(4) . ? C88 C89 1.397(4) . ? C89 C90 1.380(4) . ? C90 C91 1.382(4) . ? C91 C92 1.400(4) . ? C91 C94 1.481(4) . ? C92 C93 1.372(4) . ? C94 C95 1.317(4) . ? C95 C98 1.484(4) . ? C96 C97 1.384(4) . ? C97 C98 1.388(4) . ? C98 C99 1.380(4) . ? C99 C100 1.387(4) . ? N11 C105 1.327(4) . ? N11 C101 1.333(4) . ? N12 C120 1.322(4) . ? N12 C116 1.321(4) . ? C101 C102 1.380(4) . ? C102 C103 1.395(4) . ? C103 C104 1.385(4) . ? C103 C106 1.469(4) . ? C104 C105 1.388(4) . ? C106 C107 1.330(4) . ? C107 C108 1.470(4) . ? C108 C109 1.389(4) . ? C108 C113 1.399(4) . ? C109 C110 1.381(4) . ? C110 C111 1.390(4) . ? C111 C112 1.385(4) . ? C111 C114 1.473(4) . ? C112 C113 1.392(4) . ? C114 C115 1.324(4) . ? C115 C118 1.470(4) . ? C116 C117 1.379(4) . ? C117 C118 1.385(4) . ? C118 C119 1.392(4) . ? C119 C120 1.397(4) . ? N1S O3S 1.218(3) . ? N1S O2S 1.248(3) . ? N1S O1S 1.271(3) . ? N2S O4S 1.192(3) . ? N2S O5S 1.256(3) . ? N2S O6S 1.268(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Co O4 179.62(8) . . ? O3 Co O1 92.63(8) . . ? O4 Co O1 87.42(8) . . ? O3 Co N1 92.07(9) . . ? O4 Co N1 88.31(8) . . ? O1 Co N1 89.67(8) . . ? O3 Co N3 87.67(8) . . ? O4 Co N3 91.95(8) . . ? O1 Co N3 91.00(8) . . ? N1 Co N3 179.29(9) . . ? O3 Co O2 87.44(8) . . ? O4 Co O2 92.51(8) . . ? O1 Co O2 178.76(7) . . ? N1 Co O2 89.09(8) . . ? N3 Co O2 90.24(8) . . ? C1 N1 C5 116.6(3) . . ? C1 N1 Co 120.4(2) . . ? C5 N1 Co 122.7(2) . . ? C16 N2 C20 116.9(3) . . ? N1 C1 C2 124.4(3) . . ? C1 C2 C3 119.6(3) . . ? C2 C3 C4 116.8(3) . . ? C2 C3 C6 118.6(3) . . ? C4 C3 C6 124.6(3) . . ? C5 C4 C3 120.3(3) . . ? N1 C5 C4 122.2(3) . . ? C7 C6 C3 125.8(3) . . ? C6 C7 C8 125.9(3) . . ? C9 C8 C13 117.9(3) . . ? C9 C8 C7 118.3(3) . . ? C13 C8 C7 123.8(3) . . ? C10 C9 C8 121.1(3) . . ? C9 C10 C11 121.0(3) . . ? C12 C11 C10 117.8(3) . . ? C12 C11 C14 118.4(3) . . ? C10 C11 C14 123.9(3) . . ? C13 C12 C11 121.0(3) . . ? C12 C13 C8 121.2(3) . . ? C15 C14 C11 127.2(3) . . ? C14 C15 C18 125.9(3) . . ? N2 C16 C17 124.0(3) . . ? C16 C17 C18 119.8(3) . . ? C19 C18 C17 116.1(3) . . ? C19 C18 C15 124.8(3) . . ? C17 C18 C15 119.1(3) . . ? C18 C19 C20 120.8(3) . . ? N2 C20 C19 122.4(3) . . ? C21 N3 C25 116.0(3) . . ? C21 N3 Co 121.0(2) . . ? C25 N3 Co 122.9(2) . . ? C40 N4 C36 116.7(3) . . ? N3 C21 C22 124.4(3) . . ? C21 C22 C23 120.1(3) . . ? C22 C23 C24 116.3(3) . . ? C22 C23 C26 119.0(3) . . ? C24 C23 C26 124.8(3) . . ? C25 C24 C23 120.4(3) . . ? N3 C25 C24 122.8(3) . . ? C27 C26 C23 126.7(3) . . ? C26 C27 C28 126.5(3) . . ? C29 C28 C33 118.1(3) . . ? C29 C28 C27 124.0(3) . . ? C33 C28 C27 117.9(3) . . ? C30 C29 C28 121.3(3) . . ? C29 C30 C31 120.9(3) . . ? C32 C31 C30 117.2(3) . . ? C32 C31 C34 124.3(3) . . ? C30 C31 C34 118.5(3) . . ? C33 C32 C31 121.6(3) . . ? C32 C33 C28 120.9(3) . . ? C35 C34 C31 127.1(3) . . ? C34 C35 C38 125.8(3) . . ? N4 C36 C37 122.5(3) . . ? C38 C37 C36 120.6(3) . . ? C37 C38 C39 116.5(3) . . ? C37 C38 C35 124.8(3) . . ? C39 C38 C35 118.6(3) . . ? C40 C39 C38 119.2(3) . . ? N4 C40 C39 124.5(3) . . ? C41 N5 C45 116.1(3) . . ? C56 N6 C60 115.1(4) . . ? N5 C41 C42 123.7(3) . . ? C41 C42 C43 120.8(3) . . ? C42 C43 C44 116.6(3) . . ? C42 C43 C46 118.5(3) . . ? C44 C43 C46 124.9(3) . . ? C43 C44 C45 118.3(3) . . ? N5 C45 C44 124.5(3) . . ? C47 C46 C43 127.1(4) . . ? C46 C47 C48 127.0(4) . . ? C53 C48 C49 117.1(3) . . ? C53 C48 C47 119.1(3) . . ? C49 C48 C47 123.8(3) . . ? C50 C49 C48 120.7(3) . . ? C49 C50 C51 122.0(3) . . ? C52 C51 C50 118.0(3) . . ? C52 C51 C54 123.4(3) . . ? C50 C51 C54 118.6(3) . . ? C51 C52 C53 120.3(3) . . ? C48 C53 C52 121.8(3) . . ? C55 C54 C51 128.6(4) . . ? C54 C55 C58 128.0(4) . . ? N6 C56 C57 125.4(4) . . ? C56 C57 C58 120.1(3) . . ? C57 C58 C59 115.3(3) . . ? C57 C58 C55 125.6(3) . . ? C59 C58 C55 119.1(4) . . ? C60 C59 C58 119.7(3) . . ? N6 C60 C59 124.4(4) . . ? C61 N7 C65 115.8(3) . . ? C80 N8 C76 116.5(3) . . ? N7 C61 C62 124.8(3) . . ? C61 C62 C63 118.9(3) . . ? C64 C63 C62 116.6(3) . . ? C64 C63 C66 120.9(3) . . ? C62 C63 C66 122.5(3) . . ? C65 C64 C63 119.8(3) . . ? N7 C65 C64 124.1(3) . . ? C67 C66 C63 126.4(3) . . ? C66 C67 C68 128.3(3) . . ? C69 C68 C73 117.8(3) . . ? C69 C68 C67 119.1(3) . . ? C73 C68 C67 123.1(3) . . ? C70 C69 C68 121.7(3) . . ? C69 C70 C71 120.5(3) . . ? C72 C71 C70 117.6(3) . . ? C72 C71 C74 119.8(3) . . ? C70 C71 C74 122.6(3) . . ? C73 C72 C71 121.8(3) . . ? C72 C73 C68 120.6(3) . . ? C75 C74 C71 127.2(3) . . ? C74 C75 C78 126.8(3) . . ? N8 C76 C77 123.5(3) . . ? C78 C77 C76 120.0(3) . . ? C77 C78 C79 116.4(3) . . ? C77 C78 C75 119.9(3) . . ? C79 C78 C75 123.7(3) . . ? C80 C79 C78 119.7(3) . . ? N8 C80 C79 124.0(3) . . ? C85 N9 C81 115.1(3) . . ? C96 N10 C100 116.0(3) . . ? N9 C81 C82 123.6(3) . . ? C83 C82 C81 120.1(3) . . ? C82 C83 C84 115.8(3) . . ? C82 C83 C86 125.0(3) . . ? C84 C83 C86 119.2(3) . . ? C85 C84 C83 120.3(3) . . ? N9 C85 C84 125.0(3) . . ? C87 C86 C83 125.5(3) . . ? C86 C87 C88 127.1(3) . . ? C93 C88 C89 117.5(3) . . ? C93 C88 C87 124.9(3) . . ? C89 C88 C87 117.5(3) . . ? C90 C89 C88 120.8(3) . . ? C89 C90 C91 121.7(3) . . ? C90 C91 C92 117.2(3) . . ? C90 C91 C94 124.3(3) . . ? C92 C91 C94 118.6(3) . . ? C93 C92 C91 121.4(3) . . ? C92 C93 C88 121.3(3) . . ? C95 C94 C91 126.5(3) . . ? C94 C95 C98 125.3(3) . . ? N10 C96 C97 125.1(3) . . ? C96 C97 C98 119.0(3) . . ? C99 C98 C97 116.3(3) . . ? C99 C98 C95 125.5(3) . . ? C97 C98 C95 118.2(3) . . ? C98 C99 C100 120.7(3) . . ? N10 C100 C99 123.0(3) . . ? C105 N11 C101 116.1(3) . . ? C120 N12 C116 116.4(3) . . ? N11 C101 C102 124.7(3) . . ? C101 C102 C103 119.3(3) . . ? C104 C103 C102 116.1(3) . . ? C104 C103 C106 120.0(3) . . ? C102 C103 C106 123.9(3) . . ? C103 C104 C105 120.4(3) . . ? N11 C105 C104 123.5(3) . . ? C107 C106 C103 126.8(3) . . ? C106 C107 C108 128.0(3) . . ? C109 C108 C113 117.4(3) . . ? C109 C108 C107 120.3(3) . . ? C113 C108 C107 122.3(3) . . ? C110 C109 C108 121.8(3) . . ? C109 C110 C111 121.1(3) . . ? C112 C111 C110 117.5(3) . . ? C112 C111 C114 118.9(3) . . ? C110 C111 C114 123.6(3) . . ? C111 C112 C113 121.8(3) . . ? C112 C113 C108 120.4(3) . . ? C115 C114 C111 128.3(3) . . ? C114 C115 C118 126.1(3) . . ? N12 C116 C117 124.0(3) . . ? C116 C117 C118 120.2(3) . . ? C117 C118 C119 116.3(3) . . ? C117 C118 C115 120.7(3) . . ? C119 C118 C115 123.1(3) . . ? C118 C119 C120 118.9(3) . . ? N12 C120 C119 124.3(3) . . ? O3S N1S O2S 121.7(3) . . ? O3S N1S O1S 119.5(3) . . ? O2S N1S O1S 118.7(3) . . ? O4S N2S O5S 122.5(4) . . ? O4S N2S O6S 121.2(3) . . ? O5S N2S O6S 116.3(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1A O2A 0.96 1.93 2.759(3) 143.3 . O1 H1B O4A 0.96 1.83 2.671(3) 144.1 . O2 H2A O3A 0.96 1.86 2.743(3) 151.9 . O2 H2B O1A 0.96 1.81 2.684(3) 150.7 . O3 H3A O5A 0.96 1.99 2.736(3) 132.9 . O3 H3B O1A 0.96 1.90 2.725(3) 142.4 . O4 H4A O6A 0.96 1.89 2.751(3) 147.3 . O4 H4B O2A 0.96 2.17 2.719(3) 114.6 . O1A H1A1 N5 0.97 1.93 2.725(3) 137.6 1_545 O1A H1A2 N11 0.97 1.82 2.785(3) 171.1 2_545 O2A H2A1 N10 0.97 2.01 2.782(3) 134.7 1_565 O2A H2A2 N8 0.97 1.89 2.849(3) 170.3 2_646 O3A H3A1 N9 0.96 1.92 2.870(3) 170.5 2_545 O3A H3A3 O6A 0.96 1.87 2.771(3) 154.6 . O4A H4A1 O5S 0.96 1.89 2.850(3) 174.1 . O4A H4A3 O5A 0.96 1.93 2.865(3) 165.0 . O5A H5A1 N2 0.96 1.85 2.780(3) 163.3 2_636 O5A H5A2 N7 0.96 2.05 2.796(3) 132.7 2_556 O6A H6A2 N12 0.96 1.99 2.752(3) 135.0 2_635 O6A H6A3 N4 0.96 1.82 2.778(3) 171.5 2 O7A H107 O2S 0.85 2.24 3.051(4) 159.8 . O7A H207 O6S 0.85 2.08 2.924(4) 169.9 1_545 O8A H108 O1S 0.85 2.08 2.915(4) 166.3 . _diffrn_measured_fraction_theta_max 0.849 _diffrn_reflns_theta_full 25.93 _diffrn_measured_fraction_theta_full 0.849 _refine_diff_density_max 0.323 _refine_diff_density_min -0.395 _refine_diff_density_rms 0.059 # * END data_5 _database_code_CSD 173817 _diffrn_measurement_domega 0.30 _diffrn_measurement_rtime 64.6 _chemical_formula_sum 'C24 H20 Co N4 O8' _chemical_formula_weight 551.37 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' #(#2) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.172(5) _cell_length_b 8.482(5) _cell_length_c 17.977(5) _cell_angle_alpha 81.230(5) _cell_angle_beta 89.940(5) _cell_angle_gamma 75.460(5) _cell_volume 1191.2(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 792 _cell_measurement_theta_min 2 _cell_measurement_theta_max 18 _exptl_crystal_description plate _exptl_crystal_colour violet _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.537 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 566 _exptl_absorpt_coefficient_mu 0.779 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.75 _exptl_absorpt_correction_T_max 1.00 _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 SMART _diffrn_detector_type CCD_plate _diffrn_measurement_method omega-scan _diffrn_standards_decay_% 0. _diffrn_reflns_number 10293 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.4498 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 23.97 _reflns_number_total 10293 _reflns_number_observed 4019 _reflns_observed_criterion >2sigma(I) _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SCHAKAL _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^)+(0.1000P)^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_number_reflns 10293 _refine_ls_number_parameters 339 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2367 _refine_ls_R_factor_obs 0.1138 _refine_ls_wR_factor_all 0.3586 _refine_ls_wR_factor_obs 0.2706 _refine_ls_goodness_of_fit_all 0.783 _refine_ls_restrained_S_all 0.783 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0.002 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 0.4035(2) 0.3896(3) 0.73396(10) 0.0443(5) Uani 1 1 d . . . N1 N 0.1560(14) 0.3029(14) 0.6745(7) 0.056(3) Uani 1 1 d . . . O11 O 0.0419(11) 0.2770(12) 0.6409(6) 0.070(3) Uani 1 1 d . . . O12 O 0.1752(11) 0.2815(12) 0.7463(5) 0.067(3) Uani 1 1 d . . . O13 O 0.2744(11) 0.3575(11) 0.6422(5) 0.058(2) Uani 1 1 d . . . N2 N 0.3062(17) 0.6222(19) 0.8114(7) 0.066(4) Uani 1 1 d . . . O21 O 0.2576(14) 0.7494(17) 0.8403(8) 0.113(5) Uani 1 1 d . . . O22 O 0.2212(12) 0.6104(14) 0.7521(5) 0.076(3) Uani 1 1 d . . . O23 O 0.4284(14) 0.5023(16) 0.8343(5) 0.092(4) Uani 1 1 d . . . C4 C 1.1592(14) 0.8342(15) 0.5675(7) 0.042(3) Uani 1 1 d . . . C6 C 0.9394(13) 0.7053(14) 0.5528(6) 0.038(3) Uani 1 1 d . . . H6A H 1.0183 0.6153 0.5341 0.046 Uiso 1 1 calc R . . H6B H 0.8861 0.7851 0.5097 0.046 Uiso 1 1 calc R . . C7 C 0.8048(15) 0.6305(17) 0.6740(7) 0.050(3) Uani 1 1 d . . . H7 H 0.8815 0.6683 0.7002 0.060 Uiso 1 1 calc R . . C8 C 0.9681(17) -0.9141(15) 0.9851(7) 0.052(4) Uani 1 1 d . . . C10 C 0.6884(16) 0.5650(16) 0.7120(6) 0.054(4) Uani 1 1 d . . . H10 H 0.6865 0.5619 0.7640 0.065 Uiso 1 1 calc R . . C11 C 1.2490(15) 0.8989(16) 0.6133(7) 0.046(4) Uani 1 1 d . . . H11 H 1.2173 0.9019 0.6629 0.056 Uiso 1 1 calc R . . C12 C 1.3322(15) 0.9027(14) 0.4683(7) 0.045(3) Uani 1 1 d . . . H12 H 1.3588 0.9041 0.4179 0.054 Uiso 1 1 calc R . . C13 C 0.5016(17) 0.0426(18) 0.8191(8) 0.060(4) Uani 1 1 d . . . H13 H 0.3868 0.0667 0.8287 0.071 Uiso 1 1 calc R . . C16 C 0.6969(15) 0.5806(16) 0.5602(6) 0.048(3) Uani 1 1 d . . . H16 H 0.6988 0.5823 0.5084 0.057 Uiso 1 1 calc R . . C18 C 0.8110(14) 0.6420(14) 0.5943(6) 0.036(3) Uani 1 1 d . . . C19 C 0.8523(18) -0.5721(18) 0.9279(7) 0.054(4) Uani 1 1 d . . . C21 C 1.4321(13) 0.9646(15) 0.5122(6) 0.039(3) Uani 1 1 d . . . C23 C 0.5789(14) 0.5161(16) 0.6006(7) 0.051(3) Uani 1 1 d . . . H23 H 0.5007 0.4805 0.5743 0.061 Uiso 1 1 calc R . . C24 C 0.7714(17) -0.1402(18) 0.8410(7) 0.055(4) Uani 1 1 d . . . C26 C 1.3859(18) 0.9605(17) 0.5893(6) 0.048(3) Uani 1 1 d . . . H26 H 1.4470 0.9988 0.6231 0.058 Uiso 1 1 calc R . . C27 C 0.5986(17) -0.1106(18) 0.8471(8) 0.061(4) Uani 1 1 d . . . H27 H 0.5497 -0.1928 0.8697 0.073 Uiso 1 1 calc R . . C28 C 0.8819(15) -0.3119(15) 0.8699(7) 0.048(3) Uani 1 1 d . . . H28A H 0.9415 -0.3597 0.8288 0.057 Uiso 1 1 calc R . . H28B H 0.9649 -0.3060 0.9073 0.057 Uiso 1 1 calc R . . C29 C 0.7442(18) -0.6629(19) 0.9625(8) 0.074(5) Uani 1 1 d . . . H29 H 0.6303 -0.6115 0.9659 0.089 Uiso 1 1 calc R . . C31 C 0.805(2) -0.8306(19) 0.9923(9) 0.077(5) Uani 1 1 d . . . H31 H 0.7321 -0.8861 1.0178 0.093 Uiso 1 1 calc R . . C32 C 1.1977(15) 0.8394(17) 0.4908(6) 0.047(4) Uani 1 1 d . . . H32 H 1.1353 0.8019 0.4573 0.056 Uiso 1 1 calc R . . C34 C 1.017(2) -0.652(2) 0.9221(10) 0.098(6) Uani 1 1 d . . . H34 H 1.0919 -0.5955 0.8992 0.118 Uiso 1 1 calc R . . C35 C 1.073(2) -0.8219(18) 0.9511(9) 0.084(6) Uani 1 1 d . . . H35 H 1.1868 -0.8743 0.9471 0.101 Uiso 1 1 calc R . . C37 C 0.7294(14) 0.1266(19) 0.7707(7) 0.058(4) Uani 1 1 d . . . H37 H 0.7773 0.2067 0.7450 0.070 Uiso 1 1 calc R . . C39 C 0.8370(16) -0.0272(17) 0.8002(7) 0.055(4) Uani 1 1 d . . . H39 H 0.9521 -0.0502 0.7914 0.066 Uiso 1 1 calc R . . O1 O 1.0270(10) 0.7789(10) 0.5966(4) 0.048(2) Uani 1 1 d . . . O2 O 0.7768(11) -0.4090(11) 0.9020(5) 0.060(3) Uani 1 1 d . . . N3 N 0.5701(11) 0.5014(12) 0.6774(5) 0.038(2) Uani 1 1 d . . . N4 N 0.5630(12) 0.1639(13) 0.7775(6) 0.048(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 Co 0.0442(9) 0.0577(11) 0.0318(8) -0.0013(11) -0.0002(10) -0.0180(8) N1 0.045(7) 0.057(8) 0.073(9) -0.016(7) 0.003(7) -0.022(6) O11 0.043(5) 0.086(8) 0.090(8) -0.040(6) -0.002(6) -0.017(6) O12 0.064(6) 0.094(8) 0.040(6) 0.001(5) 0.007(5) -0.021(6) O13 0.062(6) 0.077(7) 0.045(5) -0.018(5) 0.012(5) -0.033(6) N2 0.060(9) 0.090(11) 0.054(8) -0.016(8) 0.020(7) -0.030(8) O21 0.081(9) 0.126(12) 0.161(13) -0.095(11) 0.045(8) -0.035(8) O22 0.062(6) 0.112(9) 0.049(7) -0.018(6) -0.005(5) -0.007(6) O23 0.087(8) 0.120(10) 0.036(6) 0.009(6) -0.004(5) 0.023(8) C4 0.024(6) 0.049(9) 0.056(8) -0.008(7) -0.001(6) -0.016(6) C6 0.026(6) 0.051(9) 0.038(7) -0.004(6) -0.012(6) -0.011(6) C7 0.044(8) 0.080(10) 0.040(7) -0.026(7) 0.007(6) -0.035(8) C8 0.070(10) 0.042(8) 0.036(8) -0.002(6) -0.002(7) -0.003(8) C10 0.071(9) 0.076(10) 0.027(7) -0.010(7) 0.002(7) -0.037(8) C11 0.053(8) 0.066(10) 0.028(7) -0.008(7) 0.008(6) -0.032(8) C12 0.050(8) 0.053(9) 0.034(7) -0.007(6) -0.009(6) -0.016(7) C13 0.038(8) 0.052(10) 0.082(11) 0.005(9) -0.008(8) -0.010(8) C16 0.047(8) 0.076(10) 0.022(6) -0.010(7) 0.010(6) -0.017(8) C18 0.036(7) 0.039(8) 0.032(7) -0.003(6) -0.005(6) -0.010(6) C19 0.062(9) 0.054(10) 0.048(8) -0.016(7) 0.008(7) -0.014(8) C21 0.031(7) 0.045(8) 0.044(8) -0.008(7) -0.002(6) -0.015(6) C23 0.038(8) 0.052(9) 0.064(9) 0.000(7) -0.007(6) -0.019(7) C24 0.059(9) 0.075(11) 0.028(7) -0.004(7) -0.010(7) -0.013(9) C26 0.052(7) 0.066(10) 0.039(7) -0.026(7) 0.005(7) -0.029(7) C27 0.050(9) 0.051(10) 0.068(10) 0.021(8) -0.002(8) -0.007(8) C28 0.048(8) 0.060(9) 0.032(7) 0.007(7) 0.001(6) -0.015(7) C29 0.060(9) 0.069(12) 0.092(12) 0.004(10) 0.004(9) -0.024(9) C31 0.084(12) 0.049(10) 0.091(12) 0.019(9) -0.014(10) -0.020(9) C32 0.043(8) 0.073(10) 0.035(7) -0.011(7) 0.010(6) -0.032(8) C34 0.120(16) 0.065(12) 0.094(14) 0.015(10) 0.055(12) -0.011(11) C35 0.101(12) 0.053(11) 0.087(11) 0.017(9) 0.055(11) -0.015(10) C37 0.025(7) 0.089(12) 0.063(9) 0.005(8) 0.002(6) -0.028(8) C39 0.034(7) 0.062(9) 0.063(9) 0.017(8) -0.002(7) -0.015(7) O1 0.050(5) 0.067(6) 0.041(5) -0.011(4) 0.005(4) -0.036(5) O2 0.053(6) 0.047(6) 0.072(6) 0.007(5) -0.004(5) -0.006(5) N3 0.042(6) 0.043(7) 0.029(5) -0.004(5) -0.010(5) -0.008(5) N4 0.034(6) 0.052(7) 0.055(7) 0.003(6) 0.003(5) -0.011(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 Co N3 2.034(9) . ? Co O13 2.047(8) . ? Co N4 2.066(10) . ? Co O22 2.149(10) . ? Co O23 2.199(11) . ? Co O12 2.273(9) . ? N1 O11 1.195(12) . ? N1 O12 1.279(13) . ? N1 O13 1.277(12) . ? N2 O21 1.243(15) . ? N2 O23 1.251(15) . ? N2 O22 1.303(14) . ? C4 C11 1.364(15) . ? C4 O1 1.356(12) . ? C4 C32 1.410(15) . ? C6 O1 1.378(12) . ? C6 C18 1.451(14) . ? C7 C10 1.352(15) . ? C7 C18 1.422(15) . ? C8 C31 1.358(19) . ? C8 C35 1.383(18) . ? C8 C8 1.44(2) 2_737 ? C10 N3 1.407(14) . ? C11 C26 1.391(16) . ? C12 C21 1.381(15) . ? C12 C32 1.375(15) . ? C13 N4 1.376(16) . ? C13 C27 1.362(18) . ? C16 C18 1.363(15) . ? C16 C23 1.378(15) . ? C19 C34 1.357(19) . ? C19 O2 1.373(15) . ? C19 C29 1.398(18) . ? C21 C26 1.435(15) . ? C21 C21 1.43(2) 2_876 ? C23 N3 1.371(14) . ? C24 C39 1.337(17) . ? C24 C27 1.378(18) . ? C24 C28 1.522(16) . ? C28 O2 1.400(13) . ? C29 C31 1.40(2) . ? C34 C35 1.41(2) . ? C37 N4 1.327(13) . ? C37 C39 1.404(16) . ? 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 N3 Co O13 97.7(4) . . ? N3 Co N4 100.6(4) . . ? O13 Co N4 107.7(4) . . ? N3 Co O22 97.1(4) . . ? O13 Co O22 94.6(4) . . ? N4 Co O22 149.2(4) . . ? N3 Co O23 92.0(4) . . ? O13 Co O23 153.7(4) . . ? N4 Co O23 94.4(4) . . ? O22 Co O23 59.8(4) . . ? N3 Co O12 155.8(4) . . ? O13 Co O12 58.3(3) . . ? N4 Co O12 91.0(4) . . ? O22 Co O12 82.8(4) . . ? O23 Co O12 108.4(4) . . ? O11 N1 O12 125.1(12) . . ? O11 N1 O13 123.3(12) . . ? O12 N1 O13 111.5(10) . . ? N1 O12 Co 89.6(7) . . ? N1 O13 Co 100.4(7) . . ? O21 N2 O23 126.3(15) . . ? O21 N2 O22 117.5(14) . . ? O23 N2 O22 116.2(14) . . ? N2 O22 Co 92.0(9) . . ? N2 O23 Co 91.2(8) . . ? C11 C4 O1 118.1(11) . . ? C11 C4 C32 119.2(11) . . ? O1 C4 C32 122.5(11) . . ? O1 C6 C18 112.1(10) . . ? C10 C7 C18 120.6(11) . . ? C31 C8 C35 116.1(13) . . ? C31 C8 C8 122.5(17) . 2_737 ? C35 C8 C8 121.2(16) . 2_737 ? C7 C10 N3 123.6(10) . . ? C4 C11 C26 123.0(11) . . ? C21 C12 C32 127.1(12) . . ? N4 C13 C27 124.0(13) . . ? C18 C16 C23 121.7(10) . . ? C16 C18 C7 116.2(10) . . ? C16 C18 C6 122.2(10) . . ? C7 C18 C6 121.5(10) . . ? C34 C19 O2 127.1(14) . . ? C34 C19 C29 117.9(15) . . ? O2 C19 C29 115.0(13) . . ? C12 C21 C26 114.4(10) . . ? C12 C21 C21 126.8(14) . 2_876 ? C26 C21 C21 118.7(14) . 2_876 ? N3 C23 C16 123.8(11) . . ? C39 C24 C27 119.7(13) . . ? C39 C24 C28 120.5(12) . . ? C27 C24 C28 119.0(12) . . ? C11 C26 C21 119.5(11) . . ? C24 C27 C13 118.1(14) . . ? O2 C28 C24 108.0(9) . . ? C31 C29 C19 120.9(15) . . ? C8 C31 C29 122.0(15) . . ? C12 C32 C4 116.5(11) . . ? C19 C34 C35 119.7(16) . . ? C8 C35 C34 123.2(16) . . ? N4 C37 C39 123.5(12) . . ? C24 C39 C37 119.0(12) . . ? C4 O1 C6 119.3(9) . . ? C19 O2 C28 116.8(9) . . ? C23 N3 C10 114.0(10) . . ? C23 N3 Co 121.5(8) . . ? C10 N3 Co 124.4(7) . . ? C37 N4 C13 115.2(12) . . ? C37 N4 Co 123.8(10) . . ? C13 N4 Co 121.0(8) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 23.97 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 1.512 _refine_diff_density_min -1.304 _refine_diff_density_rms 0.191 data_6 _database_code_CSD 173818 _diffrn_measurement_domega 0.30 _diffrn_measurement_rtime 43 _chemical_formula_sum 'C51 H46 Co N6 O11' _chemical_formula_weight 977.87 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' #(#2) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3200(10) _cell_length_b 13.2610(10) _cell_length_c 16.0010(10) _cell_angle_alpha 92.380(10) _cell_angle_beta 99.640(10) _cell_angle_gamma 98.530(10) _cell_volume 2336.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 925 _cell_measurement_theta_min 4. _cell_measurement_theta_max 46. _exptl_crystal_description plate _exptl_crystal_colour violet _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 1.390 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1018 _exptl_absorpt_coefficient_mu 0.437 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 1.00 _exptl_absorpt_correction_T_max 0.89 _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 SMART _diffrn_detector_type CCD_plate _diffrn_measurement_method omega-scan _diffrn_standards_decay_% 0 _diffrn_reflns_number 20146 _diffrn_reflns_av_R_equivalents 0.0349 _diffrn_reflns_av_sigmaI/netI 0.0491 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8183 _reflns_number_observed 5503 _reflns_observed_criterion >2sigma(I) _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SCHAKAL _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^)+(0.0548P)^2^+1.6247P] 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_number_reflns 8183 _refine_ls_number_parameters 622 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0883 _refine_ls_R_factor_obs 0.0492 _refine_ls_wR_factor_all 0.1342 _refine_ls_wR_factor_obs 0.1138 _refine_ls_goodness_of_fit_all 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.039 _refine_ls_shift/su_mean 0.002 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 0.65833(4) 0.26349(3) 0.49035(3) 0.04639(15) Uani 1 1 d . . . O2 O 1.09964(19) 0.57686(16) 0.79189(14) 0.0494(6) Uani 1 1 d . . . O3 O 1.8207(2) 0.98224(17) 1.14670(14) 0.0522(6) Uani 1 1 d . . . C4 C 1.1950(3) 0.6418(2) 0.84042(19) 0.0399(7) Uani 1 1 d . . . O5 O 0.3924(2) 0.56791(17) 0.17693(14) 0.0531(6) Uani 1 1 d . . . O6 O -0.2196(2) 0.1059(2) -0.23040(19) 0.0763(8) Uani 1 1 d . . . C7 C -0.1393(3) 0.1685(3) -0.1675(2) 0.0514(9) Uani 1 1 d . . . C8 C 1.3285(3) 0.8000(2) 0.8783(2) 0.0471(8) Uani 1 1 d . . . H8 H 1.3508 0.8683 0.8684 0.056 Uiso 1 1 calc R . . N9 N 0.6132(2) 0.3613(2) 0.39170(17) 0.0470(7) Uani 1 1 d . . . C10 C 0.3130(3) 0.4948(2) 0.12357(19) 0.0432(8) Uani 1 1 d . . . C11 C 1.2600(3) 0.5985(2) 0.9067(2) 0.0438(8) Uani 1 1 d . . . H11 H 1.2368 0.5305 0.9169 0.053 Uiso 1 1 calc R . . C12 C 0.0399(3) 0.2929(2) -0.04926(19) 0.0403(7) Uani 1 1 d . . . C13 C 0.1347(3) 0.3603(2) 0.01263(19) 0.0386(7) Uani 1 1 d . . . C14 C 1.3592(3) 0.6562(2) 0.9577(2) 0.0439(8) Uani 1 1 d . . . H14 H 1.4024 0.6263 1.0022 0.053 Uiso 1 1 calc R . . C15 C 1.0174(3) 0.6201(3) 0.7327(2) 0.0497(8) Uani 1 1 d . . . H15A H 1.0614 0.6627 0.6966 0.060 Uiso 1 1 calc R . . H15B H 0.9726 0.6624 0.7624 0.060 Uiso 1 1 calc R . . C16 C 1.5074(3) 0.8189(2) 0.9968(2) 0.0413(7) Uani 1 1 d . . . C17 C 1.5377(3) 0.8089(2) 1.0839(2) 0.0465(8) Uani 1 1 d . . . H17 H 1.4861 0.7648 1.1104 0.056 Uiso 1 1 calc R . . C18 C 0.1920(3) 0.5027(3) 0.1184(2) 0.0459(8) Uani 1 1 d . . . H18 H 0.1693 0.5530 0.1518 0.055 Uiso 1 1 calc R . . C19 C 0.7550(3) 0.4792(3) 0.5751(2) 0.0522(9) Uani 1 1 d . . . H19 H 0.6872 0.4952 0.5400 0.063 Uiso 1 1 calc R . . C20 C 0.9506(3) 0.4346(3) 0.6796(2) 0.0594(10) Uani 1 1 d . . . H20 H 1.0165 0.4163 0.7153 0.071 Uiso 1 1 calc R . . C21 C 1.3964(3) 0.7583(2) 0.94404(19) 0.0398(7) Uani 1 1 d . . . N22 N 2.2081(3) 1.1984(2) 1.2910(2) 0.0634(8) Uani 1 1 d . . . C23 C 0.9313(3) 0.5354(2) 0.6797(2) 0.0429(8) Uani 1 1 d . . . C24 C -0.0236(3) 0.1944(3) -0.1847(2) 0.0551(9) Uani 1 1 d . . . H24 H -0.0047 0.1704 -0.2355 0.066 Uiso 1 1 calc R . . O25 O 0.7868(3) 0.1496(2) 0.51925(19) 0.0824(9) Uani 1 1 d . . . C26 C 1.6922(3) 0.9407(3) 1.0071(2) 0.0515(9) Uani 1 1 d . . . H26 H 1.7439 0.9850 0.9809 0.062 Uiso 1 1 calc R . . C27 C 1.2276(3) 0.7431(2) 0.8265(2) 0.0464(8) Uani 1 1 d . . . H27 H 1.1828 0.7731 0.7829 0.056 Uiso 1 1 calc R . . N28 N 0.5196(3) 0.2624(3) 0.6075(2) 0.0638(9) Uani 1 1 d . . . C29 C -0.0771(3) 0.2657(3) -0.0344(2) 0.0516(9) Uani 1 1 d . . . H29 H -0.0964 0.2892 0.0164 0.062 Uiso 1 1 calc R . . C30 C 0.6965(3) 0.4221(3) 0.3596(2) 0.0495(8) Uani 1 1 d . . . H30 H 0.7779 0.4217 0.3817 0.059 Uiso 1 1 calc R . . C31 C 0.8298(3) 0.5562(3) 0.6268(2) 0.0501(8) Uani 1 1 d . . . H31 H 0.8121 0.6224 0.6261 0.060 Uiso 1 1 calc R . . C32 C 0.8707(3) 0.3620(3) 0.6260(2) 0.0638(11) Uani 1 1 d . . . H32 H 0.8846 0.2947 0.6270 0.077 Uiso 1 1 calc R . . C33 C 0.1042(3) 0.4364(2) 0.0640(2) 0.0442(8) Uani 1 1 d . . . H33 H 0.0230 0.4427 0.0615 0.053 Uiso 1 1 calc R . . C34 C 0.2565(3) 0.3517(2) 0.0207(2) 0.0446(8) Uani 1 1 d . . . H34 H 0.2793 0.3006 -0.0119 0.053 Uiso 1 1 calc R . . C35 C 1.9132(3) 1.0343(3) 1.1074(2) 0.0566(9) Uani 1 1 d . . . H35A H 1.8801 1.0834 1.0706 0.068 Uiso 1 1 calc R . . H35B H 1.9435 0.9857 1.0727 0.068 Uiso 1 1 calc R . . C36 C 2.1136(3) 1.1454(3) 1.1478(2) 0.0567(9) Uani 1 1 d . . . H36 H 2.1175 1.1479 1.0903 0.068 Uiso 1 1 calc R . . O37 O 0.6035(3) 0.2101(2) 0.60571(19) 0.0789(8) Uani 1 1 d . . . C38 C 2.0153(3) 1.0886(2) 1.1735(2) 0.0462(8) Uani 1 1 d . . . C39 C 1.7198(3) 0.9297(2) 1.0939(2) 0.0446(8) Uani 1 1 d . . . N40 N 0.8512(3) 0.1746(3) 0.4645(2) 0.0598(8) Uani 1 1 d . . . C41 C -0.4117(3) 0.0084(3) -0.2910(2) 0.0574(9) Uani 1 1 d . . . O42 O 0.8258(3) 0.2471(2) 0.4254(2) 0.0870(9) Uani 1 1 d . . . C43 C 1.6426(3) 0.8631(3) 1.1317(2) 0.0477(8) Uani 1 1 d . . . H43 H 1.6612 0.8547 1.1896 0.057 Uiso 1 1 calc R . . C44 C 0.6686(3) 0.4851(2) 0.2958(2) 0.0464(8) Uani 1 1 d . . . H44 H 0.7303 0.5255 0.2751 0.056 Uiso 1 1 calc R . . N45 N 0.7748(2) 0.3821(2) 0.57272(17) 0.0494(7) Uani 1 1 d . . . C46 C 0.5480(3) 0.4881(2) 0.26221(19) 0.0423(8) Uani 1 1 d . . . C47 C 1.5872(3) 0.8854(3) 0.9600(2) 0.0510(9) Uani 1 1 d . . . H47 H 1.5696 0.8931 0.9020 0.061 Uiso 1 1 calc R . . N48 N -0.5457(3) -0.1396(2) -0.41033(18) 0.0538(7) Uani 1 1 d . . . C49 C 0.3453(3) 0.4169(2) 0.0759(2) 0.0454(8) Uani 1 1 d . . . H49 H 0.4263 0.4085 0.0810 0.054 Uiso 1 1 calc R . . O50 O 0.4987(3) 0.3150(3) 0.5458(2) 0.0841(9) Uani 1 1 d . . . C51 C -0.3682(4) -0.0122(3) -0.3634(3) 0.0677(11) Uani 1 1 d . . . H51 H -0.2940 0.0216 -0.3729 0.081 Uiso 1 1 calc R . . C52 C -0.1664(3) 0.2047(3) -0.0921(2) 0.0563(9) Uani 1 1 d . . . H52 H -0.2443 0.1882 -0.0801 0.068 Uiso 1 1 calc R . . C53 C 0.0642(3) 0.2558(3) -0.1265(2) 0.0497(8) Uani 1 1 d . . . H53 H 0.1416 0.2729 -0.1391 0.060 Uiso 1 1 calc R . . C54 C 2.1138(4) 1.1424(3) 1.3145(3) 0.0687(11) Uani 1 1 d . . . H54 H 2.1130 1.1398 1.3724 0.082 Uiso 1 1 calc R . . O55 O 0.4631(3) 0.2595(3) 0.66607(19) 0.0947(10) Uani 1 1 d . . . C56 C 2.2059(3) 1.1983(3) 1.2079(3) 0.0631(10) Uani 1 1 d . . . H56 H 2.2709 1.2363 1.1889 0.076 Uiso 1 1 calc R . . C57 C 2.0165(3) 1.0876(3) 1.2591(2) 0.0592(10) Uani 1 1 d . . . H57 H 1.9524 1.0505 1.2797 0.071 Uiso 1 1 calc R . . C58 C 0.4970(3) 0.3638(3) 0.3590(2) 0.0548(9) Uani 1 1 d . . . H58 H 0.4372 0.3218 0.3803 0.066 Uiso 1 1 calc R . . C59 C 0.4616(3) 0.4254(3) 0.2955(2) 0.0519(9) Uani 1 1 d . . . H59 H 0.3796 0.4247 0.2750 0.062 Uiso 1 1 calc R . . C61 C 0.5175(3) 0.5593(3) 0.1944(2) 0.0529(9) Uani 1 1 d . . . H61A H 0.5641 0.6266 0.2119 0.063 Uiso 1 1 calc R . . H61B H 0.5416 0.5355 0.1427 0.063 Uiso 1 1 calc R . . C63 C -0.5187(4) -0.0395(3) -0.2784(3) 0.0789(13) Uani 1 1 d . . . H63 H -0.5503 -0.0228 -0.2306 0.095 Uiso 1 1 calc R . . C65 C -0.3380(4) 0.0902(3) -0.2232(3) 0.0758(12) Uani 1 1 d . . . H65A H -0.3702 0.1538 -0.2298 0.091 Uiso 1 1 calc R . . H65B H -0.3459 0.0684 -0.1670 0.091 Uiso 1 1 calc R . . O68 O 0.9325(3) 0.1283(3) 0.4544(3) 0.1123(13) Uani 1 1 d . . . C69 C -0.5796(4) -0.1128(3) -0.3372(3) 0.0785(13) Uani 1 1 d . . . H69 H -0.6520 -0.1481 -0.3260 0.094 Uiso 1 1 calc R . . C72 C -0.4430(3) -0.0893(3) -0.4253(3) 0.0641(10) Uani 1 1 d . . . H72 H -0.4176 -0.1033 -0.4763 0.077 Uiso 1 1 calc R . . O1S O 0.1793(4) 0.2649(3) 0.6958(2) 0.1131(12) Uani 1 1 d . . . C3S C 0.1834(5) 0.2909(4) 0.5530(3) 0.0899(15) Uani 1 1 d . . . H3S1 H 0.1751 0.3593 0.5706 0.135 Uiso 1 1 calc R . . H3S2 H 0.1170 0.2636 0.5086 0.135 Uiso 1 1 calc R . . H3S3 H 0.2585 0.2920 0.5324 0.135 Uiso 1 1 calc R . . C1S C 0.1898(6) 0.1172(4) 0.6113(4) 0.121(2) Uani 1 1 d . . . H1S1 H 0.1867 0.0843 0.6633 0.182 Uiso 1 1 calc R . . H1S2 H 0.2645 0.1101 0.5924 0.182 Uiso 1 1 calc R . . H1S3 H 0.1227 0.0861 0.5687 0.182 Uiso 1 1 calc R . . C2S C 0.1829(4) 0.2267(4) 0.6256(3) 0.0751(12) 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 0.0428(3) 0.0448(3) 0.0455(3) -0.0007(2) -0.0001(2) -0.0026(2) O2 0.0416(12) 0.0452(13) 0.0529(14) -0.0003(11) -0.0075(10) -0.0020(10) O3 0.0459(13) 0.0530(14) 0.0481(13) 0.0000(11) -0.0027(11) -0.0102(11) C4 0.0344(17) 0.0410(18) 0.0411(18) -0.0048(14) 0.0043(14) 0.0003(14) O5 0.0496(14) 0.0443(13) 0.0574(15) -0.0057(11) -0.0091(11) 0.0048(11) O6 0.0431(15) 0.0706(18) 0.103(2) -0.0187(16) -0.0039(14) -0.0042(13) C7 0.046(2) 0.046(2) 0.054(2) -0.0073(17) -0.0052(16) 0.0014(16) C8 0.0453(19) 0.0386(18) 0.052(2) 0.0056(15) -0.0007(16) -0.0002(15) N9 0.0357(15) 0.0513(17) 0.0479(16) 0.0009(13) -0.0010(12) -0.0025(13) C10 0.0458(19) 0.0399(18) 0.0395(18) 0.0084(15) -0.0032(14) 0.0034(15) C11 0.0402(18) 0.0386(18) 0.0495(19) 0.0038(15) 0.0045(15) -0.0005(14) C12 0.0385(18) 0.0391(17) 0.0418(18) 0.0049(14) 0.0016(14) 0.0071(14) C13 0.0407(18) 0.0377(17) 0.0370(17) 0.0059(14) 0.0044(14) 0.0063(14) C14 0.0404(18) 0.0458(19) 0.0445(18) 0.0073(15) 0.0044(14) 0.0057(15) C15 0.0428(19) 0.050(2) 0.050(2) -0.0030(16) -0.0046(16) 0.0007(16) C16 0.0385(17) 0.0387(17) 0.0444(18) -0.0006(14) 0.0023(14) 0.0055(14) C17 0.0453(19) 0.0468(19) 0.0440(19) 0.0036(15) 0.0059(15) -0.0017(15) C18 0.052(2) 0.0453(19) 0.0408(18) 0.0017(15) 0.0057(15) 0.0117(16) C19 0.045(2) 0.050(2) 0.054(2) -0.0001(17) -0.0095(16) 0.0037(16) C20 0.052(2) 0.055(2) 0.061(2) -0.0047(18) -0.0161(18) 0.0065(18) C21 0.0341(16) 0.0431(18) 0.0403(17) -0.0001(14) 0.0038(14) 0.0044(14) N22 0.0523(19) 0.0562(19) 0.072(2) -0.0046(17) -0.0055(16) -0.0018(15) C23 0.0366(17) 0.0451(19) 0.0427(18) -0.0036(15) 0.0046(14) -0.0026(15) C24 0.049(2) 0.062(2) 0.049(2) -0.0098(17) 0.0037(16) 0.0013(18) O25 0.079(2) 0.084(2) 0.081(2) -0.0049(17) 0.0216(17) -0.0028(16) C26 0.052(2) 0.048(2) 0.047(2) 0.0086(16) 0.0011(16) -0.0090(16) C27 0.0445(19) 0.0454(19) 0.0446(19) 0.0029(15) -0.0041(15) 0.0050(15) N28 0.059(2) 0.069(2) 0.058(2) -0.0082(18) 0.0141(18) -0.0082(18) C29 0.044(2) 0.058(2) 0.051(2) -0.0066(17) 0.0087(16) 0.0023(17) C30 0.0346(18) 0.053(2) 0.057(2) -0.0006(17) 0.0026(15) -0.0001(16) C31 0.050(2) 0.0424(19) 0.053(2) 0.0007(16) -0.0040(16) 0.0067(16) C32 0.061(2) 0.048(2) 0.072(3) -0.0067(19) -0.015(2) 0.0093(18) C33 0.0360(17) 0.051(2) 0.0451(18) 0.0051(16) 0.0025(14) 0.0091(15) C34 0.0451(19) 0.0421(18) 0.0458(19) -0.0010(15) 0.0052(15) 0.0092(15) C35 0.052(2) 0.057(2) 0.051(2) 0.0032(17) -0.0014(17) -0.0103(18) C36 0.052(2) 0.057(2) 0.056(2) 0.0013(18) 0.0064(17) -0.0035(18) O37 0.094(2) 0.0633(18) 0.089(2) 0.0074(15) 0.0389(18) 0.0166(17) C38 0.0428(19) 0.0402(18) 0.051(2) 0.0008(15) 0.0004(15) -0.0005(15) C39 0.0415(18) 0.0427(18) 0.0443(19) -0.0040(15) -0.0018(15) 0.0022(15) N40 0.0444(18) 0.060(2) 0.073(2) -0.0106(18) 0.0151(17) 0.0025(17) C41 0.058(2) 0.070(3) 0.042(2) 0.0048(18) 0.0009(17) 0.014(2) O42 0.091(2) 0.074(2) 0.093(2) 0.0140(18) 0.0090(18) 0.0096(18) C43 0.048(2) 0.053(2) 0.0371(18) 0.0007(15) 0.0007(15) 0.0002(16) C44 0.0363(18) 0.048(2) 0.052(2) 0.0044(16) 0.0066(15) -0.0035(15) N45 0.0449(16) 0.0461(17) 0.0496(17) -0.0063(13) -0.0058(13) 0.0009(13) C46 0.0422(18) 0.0403(18) 0.0391(17) -0.0041(14) 0.0010(14) -0.0016(15) C47 0.050(2) 0.054(2) 0.0427(19) 0.0076(16) -0.0030(16) -0.0038(17) N48 0.0571(19) 0.0464(17) 0.0492(18) -0.0015(14) -0.0025(14) -0.0049(14) C49 0.0365(18) 0.0484(19) 0.0499(19) 0.0000(16) 0.0010(15) 0.0104(15) O50 0.0658(19) 0.109(2) 0.076(2) 0.0176(19) 0.0094(15) 0.0084(17) C51 0.055(2) 0.045(2) 0.103(3) 0.018(2) 0.019(2) -0.0008(18) C52 0.0366(19) 0.058(2) 0.070(2) -0.0065(19) 0.0097(17) -0.0018(16) C53 0.0423(19) 0.054(2) 0.050(2) -0.0010(17) 0.0087(16) 0.0007(16) C54 0.065(3) 0.075(3) 0.055(2) -0.003(2) -0.005(2) -0.006(2) O55 0.093(2) 0.125(3) 0.072(2) -0.0100(19) 0.0389(18) 0.011(2) C56 0.046(2) 0.057(2) 0.078(3) 0.003(2) 0.0044(19) -0.0100(18) C57 0.054(2) 0.064(2) 0.051(2) 0.0010(18) 0.0045(17) -0.0104(18) C58 0.041(2) 0.065(2) 0.054(2) 0.0092(18) 0.0044(16) -0.0061(17) C59 0.0350(18) 0.063(2) 0.051(2) 0.0095(18) -0.0045(15) -0.0015(16) C61 0.049(2) 0.050(2) 0.052(2) 0.0025(17) -0.0041(16) -0.0027(16) C63 0.083(3) 0.083(3) 0.062(3) -0.007(2) 0.014(2) -0.013(3) C65 0.085(3) 0.074(3) 0.064(3) 0.001(2) 0.015(2) -0.001(2) O68 0.075(2) 0.105(3) 0.166(4) -0.017(2) 0.038(2) 0.032(2) C69 0.089(3) 0.077(3) 0.055(3) -0.011(2) 0.005(2) -0.019(2) C72 0.060(2) 0.050(2) 0.075(3) 0.0023(19) 0.001(2) -0.0046(19) O1S 0.137(3) 0.126(3) 0.087(2) 0.012(2) 0.056(2) 0.014(2) C3S 0.103(4) 0.083(3) 0.071(3) 0.015(3) -0.001(3) -0.008(3) C1S 0.150(5) 0.074(4) 0.120(5) 0.009(3) -0.008(4) -0.012(3) C2S 0.069(3) 0.085(3) 0.068(3) 0.010(2) 0.015(2) -0.004(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 N9 2.129(3) . ? Co1 N45 2.140(3) . ? Co1 N48 2.150(3) 2 ? Co1 O37 2.157(3) . ? Co1 O25 2.257(3) . ? Co1 O50 2.318(3) . ? Co1 O42 2.342(3) . ? O2 C4 1.378(3) . ? O2 C15 1.415(4) . ? O3 C39 1.377(4) . ? O3 C35 1.418(4) . ? C4 C27 1.377(4) . ? C4 C11 1.382(4) . ? O5 C10 1.376(4) . ? O5 C61 1.420(4) . ? O6 C65 1.350(5) . ? O6 C7 1.389(4) . ? C7 C52 1.378(5) . ? C7 C24 1.380(5) . ? C8 C21 1.381(4) . ? C8 C27 1.392(4) . ? N9 C30 1.331(4) . ? N9 C58 1.337(4) . ? C10 C18 1.378(4) . ? C10 C49 1.386(4) . ? C11 C14 1.378(4) . ? C12 C29 1.383(4) . ? C12 C53 1.396(4) . ? C12 C13 1.489(4) . ? C13 C34 1.385(4) . ? C13 C33 1.393(4) . ? C14 C21 1.395(4) . ? C15 C23 1.500(4) . ? C16 C47 1.387(4) . ? C16 C17 1.396(4) . ? C16 C21 1.492(4) . ? C17 C43 1.381(4) . ? C18 C33 1.380(4) . ? C19 N45 1.339(4) . ? C19 C31 1.372(4) . ? C20 C32 1.376(5) . ? C20 C23 1.385(5) . ? N22 C54 1.325(5) . ? N22 C56 1.326(5) . ? C23 C31 1.378(4) . ? C24 C53 1.379(4) . ? O25 N40 1.255(4) . ? C26 C47 1.383(4) . ? C26 C39 1.390(4) . ? N28 O55 1.219(4) . ? N28 O50 1.243(4) . ? N28 O37 1.259(4) . ? C29 C52 1.383(5) . ? C30 C44 1.372(5) . ? C32 N45 1.330(4) . ? C34 C49 1.386(4) . ? C35 C38 1.501(4) . ? C36 C56 1.378(5) . ? C36 C38 1.380(5) . ? C38 C57 1.367(5) . ? C39 C43 1.379(4) . ? N40 O68 1.208(4) . ? N40 O42 1.212(4) . ? C41 C63 1.331(5) . ? C41 C51 1.366(5) . ? C41 C65 1.543(5) . ? C44 C46 1.389(4) . ? C46 C59 1.379(4) . ? C46 C61 1.498(4) . ? N48 C72 1.315(5) . ? N48 C69 1.342(5) . ? N48 Co1 2.150(3) 2 ? C51 C72 1.456(5) . ? C54 C57 1.383(5) . ? C58 C59 1.375(5) . ? C63 C69 1.346(5) . ? O1S C2S 1.223(5) . ? C3S C2S 1.469(6) . ? C1S C2S 1.476(7) . ? 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 N9 Co1 N45 94.46(10) . . ? N9 Co1 N48 87.80(10) . 2 ? N45 Co1 N48 177.49(11) . 2 ? N9 Co1 O37 141.62(12) . . ? N45 Co1 O37 84.63(11) . . ? N48 Co1 O37 94.27(11) 2 . ? N9 Co1 O25 137.21(11) . . ? N45 Co1 O25 93.11(11) . . ? N48 Co1 O25 84.49(11) 2 . ? O37 Co1 O25 81.01(12) . . ? N9 Co1 O50 85.31(11) . . ? N45 Co1 O50 87.04(11) . . ? N48 Co1 O50 94.23(11) 2 . ? O37 Co1 O50 56.32(11) . . ? O25 Co1 O50 137.16(12) . . ? N9 Co1 O42 84.70(11) . . ? N45 Co1 O42 86.80(11) . . ? N48 Co1 O42 92.35(11) 2 . ? O37 Co1 O42 133.35(12) . . ? O25 Co1 O42 53.77(11) . . ? O50 Co1 O42 167.81(12) . . ? C4 O2 C15 117.9(2) . . ? C39 O3 C35 117.0(2) . . ? O2 C4 C27 124.5(3) . . ? O2 C4 C11 115.4(3) . . ? C27 C4 C11 120.1(3) . . ? C10 O5 C61 119.5(3) . . ? C65 O6 C7 117.6(3) . . ? C52 C7 C24 119.5(3) . . ? C52 C7 O6 125.6(3) . . ? C24 C7 O6 114.9(3) . . ? C21 C8 C27 122.0(3) . . ? C30 N9 C58 116.9(3) . . ? C30 N9 Co1 122.9(2) . . ? C58 N9 Co1 120.2(2) . . ? O5 C10 C18 115.3(3) . . ? O5 C10 C49 125.5(3) . . ? C18 C10 C49 119.2(3) . . ? C14 C11 C4 120.0(3) . . ? C29 C12 C53 116.5(3) . . ? C29 C12 C13 122.0(3) . . ? C53 C12 C13 121.5(3) . . ? C34 C13 C33 117.2(3) . . ? C34 C13 C12 121.8(3) . . ? C33 C13 C12 121.0(3) . . ? C11 C14 C21 121.4(3) . . ? O2 C15 C23 108.8(3) . . ? C47 C16 C17 117.2(3) . . ? C47 C16 C21 120.8(3) . . ? C17 C16 C21 121.9(3) . . ? C43 C17 C16 121.5(3) . . ? C10 C18 C33 120.5(3) . . ? N45 C19 C31 123.3(3) . . ? C32 C20 C23 119.0(3) . . ? C8 C21 C14 117.4(3) . . ? C8 C21 C16 121.4(3) . . ? C14 C21 C16 121.2(3) . . ? C54 N22 C56 115.4(3) . . ? C31 C23 C20 117.1(3) . . ? C31 C23 C15 120.4(3) . . ? C20 C23 C15 122.5(3) . . ? C53 C24 C7 120.1(3) . . ? N40 O25 Co1 96.9(2) . . ? C47 C26 C39 119.6(3) . . ? C4 C27 C8 119.1(3) . . ? O55 N28 O50 123.4(4) . . ? O55 N28 O37 121.1(4) . . ? O50 N28 O37 115.6(3) . . ? C52 C29 C12 122.5(3) . . ? N9 C30 C44 123.4(3) . . ? C19 C31 C23 120.0(3) . . ? N45 C32 C20 124.2(3) . . ? C18 C33 C13 121.4(3) . . ? C13 C34 C49 121.9(3) . . ? O3 C35 C38 110.2(3) . . ? C56 C36 C38 119.6(3) . . ? N28 O37 Co1 97.6(2) . . ? C57 C38 C36 116.9(3) . . ? C57 C38 C35 124.0(3) . . ? C36 C38 C35 119.1(3) . . ? O3 C39 C43 116.3(3) . . ? O3 C39 C26 124.2(3) . . ? C43 C39 C26 119.5(3) . . ? O68 N40 O42 124.7(4) . . ? O68 N40 O25 120.3(4) . . ? O42 N40 O25 115.1(3) . . ? C63 C41 C51 121.0(4) . . ? C63 C41 C65 119.0(4) . . ? C51 C41 C65 119.9(4) . . ? N40 O42 Co1 94.1(2) . . ? C39 C43 C17 120.2(3) . . ? C30 C44 C46 119.7(3) . . ? C32 N45 C19 116.3(3) . . ? C32 N45 Co1 121.0(2) . . ? C19 N45 Co1 122.7(2) . . ? C59 C46 C44 116.9(3) . . ? C59 C46 C61 123.4(3) . . ? C44 C46 C61 119.7(3) . . ? C26 C47 C16 122.0(3) . . ? C72 N48 C69 116.5(3) . . ? C72 N48 Co1 125.5(3) . 2 ? C69 N48 Co1 118.0(3) . 2 ? C34 C49 C10 119.7(3) . . ? N28 O50 Co1 90.4(2) . . ? C41 C51 C72 117.2(4) . . ? C7 C52 C29 119.6(3) . . ? C24 C53 C12 121.8(3) . . ? N22 C54 C57 124.6(4) . . ? N22 C56 C36 124.2(4) . . ? C38 C57 C54 119.3(4) . . ? N9 C58 C59 123.1(3) . . ? C58 C59 C46 119.9(3) . . ? O5 C61 C46 113.5(3) . . ? C41 C63 C69 117.9(4) . . ? O6 C65 C41 111.0(3) . . ? N48 C69 C63 126.1(4) . . ? N48 C72 C51 121.2(4) . . ? O1S C2S C3S 119.8(5) . . ? O1S C2S C1S 122.0(5) . . ? C3S C2S C1S 118.2(5) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.703 _refine_diff_density_min -0.301 _refine_diff_density_rms 0.049 #END