# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Jun Tao' _publ_contact_author_email TAOJUN@XMU.EDU.CN _publ_section_title ; Synthesis, crystal structure and magnetic properties of a mixed-valence pentanuclear cobalt complex ; loop_ _publ_author_name 'Jun Tao.' 'Li-Li Hu.' 'Rongbin Huang.' 'Zhong-Quan Jia.' 'Lan-Sun Zheng.' # Attachment 'crystal_data-revised.txt' #==================================================================== data_1 _database_code_depnum_ccdc_archive 'CCDC 694931' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H61 Co5 N4 O22.50' _chemical_formula_weight 1348.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5216(2) _cell_length_b 11.6982(3) _cell_length_c 23.8356(6) _cell_angle_alpha 92.693(2) _cell_angle_beta 92.320(2) _cell_angle_gamma 97.910(2) _cell_volume 2623.82(11) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6760 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 27.00 _exptl_crystal_description block _exptl_crystal_colour red-brown _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.707 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1384 _exptl_absorpt_coefficient_mu 1.635 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.738 _exptl_absorpt_correction_T_max 0.849 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19332 _diffrn_reflns_av_R_equivalents 0.0518 _diffrn_reflns_av_sigmaI/netI 0.1147 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 27.00 _reflns_number_total 10915 _reflns_number_gt 6760 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The O3W is half occupied and hydrogens cannot be fixed. Checkcif reports a larger than usual U(eq) range across all of the carbon atoms. This is probably due to the larger ellipsoids of the carbon atoms in the methyl groups (C46 and C48) where they are able to move about their positions slightly. ; _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^)+(0.0551P)^2^+0.1601P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10915 _refine_ls_number_parameters 721 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1121 _refine_ls_R_factor_gt 0.0647 _refine_ls_wR_factor_ref 0.1308 _refine_ls_wR_factor_gt 0.1204 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.04726(7) -0.20413(6) 0.13716(3) 0.01362(17) Uani 1 1 d . . . Co2 Co 0.36541(7) 0.22421(6) 0.36425(3) 0.01514(17) Uani 1 1 d . . . Co3 Co 0.18056(7) -0.01739(6) 0.26984(3) 0.01464(17) Uani 1 1 d . . . Co4 Co 0.28494(7) -0.00907(6) 0.15909(3) 0.01427(17) Uani 1 1 d . . . Co5 Co 0.29338(7) 0.20952(6) 0.24029(3) 0.01559(17) Uani 1 1 d . . . O1 O -0.0224(3) -0.3388(3) 0.17378(16) 0.0184(8) Uani 1 1 d . . . O2 O 0.1274(3) -0.0718(3) 0.10013(15) 0.0153(8) Uani 1 1 d . . . O3 O 0.1371(3) 0.0827(3) 0.20289(15) 0.0152(8) Uani 1 1 d . . . O4 O -0.3091(3) -0.0413(3) 0.09252(16) 0.0219(9) Uani 1 1 d . . . H4 H -0.3229 -0.0189 0.0596 0.026 Uiso 1 1 d R . . N1 N -0.0861(4) -0.1102(4) 0.16366(18) 0.0137(9) Uani 1 1 d . . . C1 C -0.1318(5) -0.3482(5) 0.2067(2) 0.0177(12) Uani 1 1 d . . . C2 C -0.1788(6) -0.4561(5) 0.2270(3) 0.0298(15) Uani 1 1 d . . . H2A H -0.1340 -0.5189 0.2162 0.036 Uiso 1 1 calc R . . C3 C -0.2889(6) -0.4721(6) 0.2621(3) 0.0368(17) Uani 1 1 d . . . H3A H -0.3181 -0.5452 0.2747 0.044 Uiso 1 1 calc R . . C4 C -0.3570(6) -0.3802(5) 0.2790(3) 0.0338(15) Uani 1 1 d . . . H4A H -0.4305 -0.3908 0.3037 0.041 Uiso 1 1 calc R . . C5 C -0.3157(5) -0.2745(5) 0.2594(2) 0.0225(13) Uani 1 1 d . . . H5A H -0.3624 -0.2132 0.2708 0.027 Uiso 1 1 calc R . . C6 C -0.2048(5) -0.2542(5) 0.2223(2) 0.0153(11) Uani 1 1 d . . . C7 C -0.1777(5) -0.1419(4) 0.1995(2) 0.0153(11) Uani 1 1 d . . . H7A H -0.2325 -0.0869 0.2122 0.018 Uiso 1 1 calc R . . C8 C -0.0717(5) 0.0064(4) 0.1408(2) 0.0129(11) Uani 1 1 d . . . C9 C -0.0023(5) 0.0975(4) 0.1848(2) 0.0165(12) Uani 1 1 d . . . H9A H 0.0004 0.1730 0.1694 0.020 Uiso 1 1 calc R . . H9B H -0.0608 0.0962 0.2172 0.020 Uiso 1 1 calc R . . C10 C 0.0192(5) -0.0024(4) 0.0892(2) 0.0153(11) Uani 1 1 d . . . H10A H -0.0406 -0.0360 0.0571 0.018 Uiso 1 1 calc R . . H10B H 0.0620 0.0743 0.0803 0.018 Uiso 1 1 calc R . . C11 C -0.2151(5) 0.0443(5) 0.1233(2) 0.0183(12) Uani 1 1 d . . . H11A H -0.2605 0.0676 0.1568 0.022 Uiso 1 1 calc R . . H11B H -0.1974 0.1113 0.1008 0.022 Uiso 1 1 calc R . . O5 O -0.0785(3) -0.2527(3) 0.07505(15) 0.0166(8) Uani 1 1 d . . . O6 O 0.1797(3) -0.1497(3) 0.19925(15) 0.0117(7) Uani 1 1 d . . . O7 O 0.4403(3) -0.1148(3) 0.13431(17) 0.0222(9) Uani 1 1 d . . . H7 H 0.5225 -0.0759 0.1343 0.027 Uiso 1 1 d R . . O8 O 0.1859(4) -0.4847(3) 0.18050(17) 0.0240(9) Uani 1 1 d . . . H8 H 0.1224 -0.4404 0.1785 0.029 Uiso 1 1 d R . . N2 N 0.1919(4) -0.2881(3) 0.11281(19) 0.0146(10) Uani 1 1 d . . . C12 C -0.0384(5) -0.2891(5) 0.0264(2) 0.0169(11) Uani 1 1 d . . . C13 C -0.1333(6) -0.2926(5) -0.0213(3) 0.0252(14) Uani 1 1 d . . . H13A H -0.2194 -0.2647 -0.0174 0.030 Uiso 1 1 calc R . . C14 C -0.1015(6) -0.3359(5) -0.0725(3) 0.0274(14) Uani 1 1 d . . . H14A H -0.1653 -0.3357 -0.1031 0.033 Uiso 1 1 calc R . . C15 C 0.0256(6) -0.3805(5) -0.0798(3) 0.0305(15) Uani 1 1 d . . . H15A H 0.0455 -0.4122 -0.1146 0.037 Uiso 1 1 calc R . . C16 C 0.1205(6) -0.3769(5) -0.0348(2) 0.0263(14) Uani 1 1 d . . . H16A H 0.2060 -0.4054 -0.0395 0.032 Uiso 1 1 calc R . . C17 C 0.0917(5) -0.3311(5) 0.0183(2) 0.0181(12) Uani 1 1 d . . . C18 C 0.1977(5) -0.3329(5) 0.0634(2) 0.0192(12) Uani 1 1 d . . . H18A H 0.2759 -0.3696 0.0557 0.023 Uiso 1 1 calc R . . C19 C 0.3063(5) -0.2964(5) 0.1569(2) 0.0172(12) Uani 1 1 d . . . C20 C 0.2636(5) -0.2388(5) 0.2111(2) 0.0188(12) Uani 1 1 d . . . H20A H 0.2099 -0.2962 0.2328 0.023 Uiso 1 1 calc R . . H20B H 0.3482 -0.2059 0.2334 0.023 Uiso 1 1 calc R . . C21 C 0.4475(5) -0.2352(5) 0.1373(2) 0.0202(12) Uani 1 1 d . . . H21A H 0.5244 -0.2467 0.1635 0.024 Uiso 1 1 calc R . . H21B H 0.4664 -0.2675 0.1006 0.024 Uiso 1 1 calc R . . C22 C 0.3177(5) -0.4233(5) 0.1655(2) 0.0211(12) Uani 1 1 d . . . H22A H 0.3470 -0.4587 0.1311 0.025 Uiso 1 1 calc R . . H22B H 0.3897 -0.4286 0.1949 0.025 Uiso 1 1 calc R . . O9 O 0.2700(3) 0.1777(3) 0.42883(15) 0.0194(8) Uani 1 1 d . . . O10 O 0.4488(3) 0.2741(3) 0.29705(15) 0.0149(8) Uani 1 1 d . . . O11 O 0.3746(3) 0.0440(3) 0.23794(15) 0.0151(8) Uani 1 1 d . . . O12 O 0.7226(4) -0.0374(3) 0.33058(18) 0.0296(10) Uani 1 1 d . . . H12 H 0.8069 -0.0501 0.3252 0.035 Uiso 1 1 d R . . N3 N 0.4676(4) 0.0966(4) 0.35732(19) 0.0168(10) Uani 1 1 d . . . C23 C 0.2771(5) 0.0802(5) 0.4525(2) 0.0179(12) Uani 1 1 d . . . C24 C 0.1894(5) 0.0522(5) 0.4972(2) 0.0243(13) Uani 1 1 d . . . H24A H 0.1282 0.1034 0.5085 0.029 Uiso 1 1 calc R . . C25 C 0.1909(6) -0.0475(6) 0.5247(3) 0.0305(15) Uani 1 1 d . . . H25A H 0.1306 -0.0629 0.5539 0.037 Uiso 1 1 calc R . . C26 C 0.2808(6) -0.1263(5) 0.5096(3) 0.0306(15) Uani 1 1 d . . . H26A H 0.2817 -0.1937 0.5287 0.037 Uiso 1 1 calc R . . C27 C 0.3683(6) -0.1028(5) 0.4663(3) 0.0240(13) Uani 1 1 d . . . H27A H 0.4299 -0.1548 0.4563 0.029 Uiso 1 1 calc R . . C28 C 0.3675(5) -0.0017(5) 0.4361(2) 0.0189(12) Uani 1 1 d . . . C29 C 0.4585(5) 0.0130(5) 0.3898(2) 0.0202(12) Uani 1 1 d . . . H29A H 0.5161 -0.0438 0.3829 0.024 Uiso 1 1 calc R . . C30 C 0.5660(5) 0.1040(4) 0.3095(2) 0.0169(12) Uani 1 1 d . . . C31 C 0.5790(5) 0.2290(5) 0.2926(2) 0.0201(12) Uani 1 1 d . . . H31A H 0.6515 0.2759 0.3167 0.024 Uiso 1 1 calc R . . H31B H 0.6084 0.2332 0.2542 0.024 Uiso 1 1 calc R . . C32 C 0.5040(5) 0.0190(5) 0.2619(2) 0.0185(12) Uani 1 1 d . . . H32A H 0.5723 0.0188 0.2328 0.022 Uiso 1 1 calc R . . H32B H 0.4890 -0.0579 0.2760 0.022 Uiso 1 1 calc R . . C33 C 0.7158(5) 0.0823(5) 0.3272(3) 0.0215(13) Uani 1 1 d . . . H33A H 0.7820 0.1141 0.3002 0.026 Uiso 1 1 calc R . . H33B H 0.7435 0.1215 0.3636 0.026 Uiso 1 1 calc R . . O13 O 0.5219(3) 0.3014(3) 0.40730(16) 0.0215(9) Uani 1 1 d . . . O14 O 0.2088(3) 0.1463(3) 0.31587(15) 0.0138(8) Uani 1 1 d . . . O15 O 0.1638(4) 0.3427(3) 0.24689(16) 0.0237(9) Uani 1 1 d . . . H15 H 0.1986 0.4003 0.2290 0.028 Uiso 1 1 d R . . O16 O 0.0327(4) 0.3040(4) 0.44200(18) 0.0364(11) Uani 1 1 d . . . H16 H 0.1024 0.2660 0.4394 0.044 Uiso 1 1 d R . . N4 N 0.2592(4) 0.3490(4) 0.36571(19) 0.0166(10) Uani 1 1 d . . . C34 C 0.5469(5) 0.4128(5) 0.4174(2) 0.0198(12) Uani 1 1 d . . . C35 C 0.6808(6) 0.4606(5) 0.4417(3) 0.0282(14) Uani 1 1 d . . . H35A H 0.7480 0.4120 0.4493 0.034 Uiso 1 1 calc R . . C36 C 0.7142(6) 0.5765(6) 0.4543(3) 0.0390(17) Uani 1 1 d . . . H36A H 0.8039 0.6053 0.4699 0.047 Uiso 1 1 calc R . . C37 C 0.6169(6) 0.6522(6) 0.4442(3) 0.0440(19) Uani 1 1 d . . . H37A H 0.6404 0.7308 0.4534 0.053 Uiso 1 1 calc R . . C38 C 0.4863(6) 0.6092(5) 0.4206(3) 0.0353(16) Uani 1 1 d . . . H38A H 0.4206 0.6595 0.4139 0.042 Uiso 1 1 calc R . . C39 C 0.4487(6) 0.4908(5) 0.4062(3) 0.0250(13) Uani 1 1 d . . . C40 C 0.3074(6) 0.4519(5) 0.3837(3) 0.0241(13) Uani 1 1 d . . . H40A H 0.2452 0.5065 0.3822 0.029 Uiso 1 1 calc R . . C41 C 0.1088(5) 0.3183(5) 0.3449(2) 0.0197(12) Uani 1 1 d . . . C42 C 0.0828(5) 0.1874(4) 0.3333(2) 0.0173(12) Uani 1 1 d . . . H42A H 0.0518 0.1503 0.3671 0.021 Uiso 1 1 calc R . . H42B H 0.0081 0.1677 0.3041 0.021 Uiso 1 1 calc R . . C43 C 0.0811(6) 0.3800(5) 0.2915(2) 0.0253(13) Uani 1 1 d . . . H43A H -0.0189 0.3639 0.2802 0.030 Uiso 1 1 calc R . . H43B H 0.1051 0.4628 0.2989 0.030 Uiso 1 1 calc R . . C44 C 0.0076(5) 0.3519(5) 0.3894(2) 0.0234(13) Uani 1 1 d . . . H44A H 0.0187 0.4354 0.3947 0.028 Uiso 1 1 calc R . . H44B H -0.0895 0.3255 0.3760 0.028 Uiso 1 1 calc R . . O17 O -0.0046(3) -0.0742(3) 0.31292(16) 0.0218(9) Uani 1 1 d . . . O18 O 0.1938(4) -0.1449(3) 0.32643(16) 0.0216(9) Uani 1 1 d . . . C45 C 0.0649(6) -0.1448(5) 0.3379(2) 0.0203(12) Uani 1 1 d . . . C46 C -0.0024(7) -0.2240(6) 0.3788(3) 0.0460(19) Uani 1 1 d . . . H46A H 0.0656 -0.2701 0.3931 0.069 Uiso 1 1 calc R . . H46B H -0.0816 -0.2735 0.3606 0.069 Uiso 1 1 calc R . . H46C H -0.0349 -0.1796 0.4094 0.069 Uiso 1 1 calc R . . O19 O 0.3942(4) 0.1151(3) 0.11556(17) 0.0256(9) Uani 1 1 d . . . O20 O 0.3831(4) 0.2727(3) 0.17076(17) 0.0239(9) Uani 1 1 d . . . C47 C 0.4248(5) 0.2209(5) 0.1286(2) 0.0210(13) Uani 1 1 d . . . C48 C 0.5243(7) 0.2907(6) 0.0911(3) 0.0431(18) Uani 1 1 d . . . H48A H 0.5488 0.2414 0.0607 0.065 Uiso 1 1 calc R . . H48B H 0.6089 0.3235 0.1126 0.065 Uiso 1 1 calc R . . H48C H 0.4785 0.3516 0.0761 0.065 Uiso 1 1 calc R . . O1W O -0.3225(4) 0.0277(4) -0.01245(18) 0.0436(12) Uani 1 1 d . . . H1WA H -0.2507 0.0589 -0.0290 0.052 Uiso 1 1 d R . . H1WB H -0.3686 -0.0233 -0.0353 0.052 Uiso 1 1 d R . . O2W O 0.6734(4) -0.4110(4) 0.0900(2) 0.0485(13) Uani 1 1 d . . . H2WA H 0.7413 -0.3619 0.0804 0.058 Uiso 1 1 d R . . H2WB H 0.6098 -0.4215 0.0635 0.058 Uiso 1 1 d R . . O3W O 0.4478(9) -0.4689(10) 0.0170(4) 0.057(3) Uani 0.50 1 d P . . 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 0.0120(4) 0.0123(4) 0.0166(4) -0.0001(3) 0.0005(3) 0.0019(3) Co2 0.0148(4) 0.0113(4) 0.0189(4) -0.0010(3) -0.0005(3) 0.0009(3) Co3 0.0138(4) 0.0128(4) 0.0175(4) 0.0011(3) 0.0015(3) 0.0025(3) Co4 0.0132(4) 0.0138(4) 0.0155(4) 0.0015(3) 0.0009(3) 0.0008(3) Co5 0.0150(4) 0.0137(4) 0.0177(4) 0.0019(3) 0.0002(3) 0.0009(3) O1 0.0155(19) 0.0158(19) 0.025(2) -0.0002(17) 0.0039(16) 0.0052(15) O2 0.0136(18) 0.0159(19) 0.017(2) 0.0014(16) 0.0015(15) 0.0054(15) O3 0.0125(17) 0.0142(19) 0.019(2) 0.0007(16) -0.0001(15) 0.0017(15) O4 0.0119(18) 0.031(2) 0.022(2) 0.0058(19) -0.0036(15) 0.0017(16) N1 0.010(2) 0.014(2) 0.017(2) 0.0004(19) -0.0004(18) 0.0021(17) C1 0.013(3) 0.018(3) 0.021(3) 0.003(2) -0.004(2) -0.002(2) C2 0.035(3) 0.016(3) 0.042(4) 0.012(3) 0.008(3) 0.011(3) C3 0.040(4) 0.026(4) 0.046(4) 0.017(3) 0.014(3) 0.005(3) C4 0.032(3) 0.035(4) 0.035(4) 0.008(3) 0.017(3) -0.001(3) C5 0.022(3) 0.018(3) 0.029(3) 0.001(3) 0.005(2) 0.006(2) C6 0.014(3) 0.016(3) 0.016(3) 0.001(2) 0.000(2) 0.002(2) C7 0.012(3) 0.016(3) 0.019(3) -0.002(2) 0.000(2) 0.004(2) C8 0.011(2) 0.010(3) 0.018(3) 0.005(2) 0.001(2) -0.001(2) C9 0.013(3) 0.015(3) 0.022(3) 0.003(2) 0.002(2) 0.005(2) C10 0.015(3) 0.012(3) 0.019(3) 0.006(2) 0.001(2) -0.001(2) C11 0.011(3) 0.017(3) 0.027(3) 0.004(3) 0.001(2) 0.005(2) O5 0.0111(17) 0.0168(19) 0.020(2) -0.0055(17) -0.0026(15) -0.0007(15) O6 0.0108(17) 0.0031(16) 0.021(2) 0.0009(15) -0.0007(14) 0.0008(13) O7 0.0118(18) 0.018(2) 0.037(2) 0.0009(19) 0.0069(17) -0.0005(15) O8 0.020(2) 0.014(2) 0.038(3) 0.0033(19) 0.0012(17) 0.0018(16) N2 0.011(2) 0.007(2) 0.025(3) 0.003(2) -0.0001(19) -0.0027(17) C12 0.020(3) 0.014(3) 0.016(3) 0.002(2) 0.001(2) -0.003(2) C13 0.023(3) 0.022(3) 0.030(4) 0.003(3) -0.006(3) 0.003(2) C14 0.029(3) 0.024(3) 0.026(3) 0.001(3) -0.008(3) -0.004(3) C15 0.035(4) 0.034(4) 0.021(3) -0.005(3) 0.000(3) 0.001(3) C16 0.027(3) 0.027(3) 0.023(3) -0.007(3) 0.003(3) 0.001(3) C17 0.019(3) 0.016(3) 0.019(3) 0.003(2) 0.001(2) 0.001(2) C18 0.015(3) 0.023(3) 0.020(3) 0.000(3) 0.003(2) 0.003(2) C19 0.010(3) 0.022(3) 0.020(3) 0.004(2) -0.003(2) 0.002(2) C20 0.025(3) 0.014(3) 0.017(3) 0.000(2) -0.002(2) 0.001(2) C21 0.015(3) 0.017(3) 0.029(3) 0.003(3) 0.002(2) 0.003(2) C22 0.020(3) 0.020(3) 0.024(3) 0.003(3) 0.000(2) 0.006(2) O9 0.022(2) 0.019(2) 0.018(2) -0.0004(17) 0.0035(16) 0.0059(16) O10 0.0112(17) 0.0104(18) 0.022(2) 0.0020(16) 0.0006(15) -0.0019(14) O11 0.0144(18) 0.0119(18) 0.019(2) 0.0012(16) -0.0020(15) 0.0027(14) O12 0.0138(19) 0.028(2) 0.048(3) 0.000(2) -0.0004(18) 0.0085(17) N3 0.010(2) 0.023(3) 0.017(2) -0.001(2) -0.0011(18) 0.0001(18) C23 0.013(3) 0.019(3) 0.020(3) 0.001(2) -0.003(2) -0.003(2) C24 0.016(3) 0.030(3) 0.027(3) 0.006(3) 0.003(2) 0.003(2) C25 0.019(3) 0.046(4) 0.026(3) 0.010(3) 0.005(3) -0.001(3) C26 0.033(3) 0.030(4) 0.028(4) 0.011(3) -0.002(3) -0.001(3) C27 0.023(3) 0.015(3) 0.033(4) 0.002(3) -0.006(3) 0.001(2) C28 0.019(3) 0.021(3) 0.016(3) -0.002(2) -0.002(2) 0.002(2) C29 0.019(3) 0.020(3) 0.023(3) -0.001(3) -0.003(2) 0.007(2) C30 0.015(3) 0.014(3) 0.022(3) 0.003(2) 0.003(2) 0.000(2) C31 0.014(3) 0.022(3) 0.022(3) -0.001(3) -0.001(2) -0.005(2) C32 0.013(3) 0.019(3) 0.023(3) 0.000(2) 0.002(2) 0.001(2) C33 0.014(3) 0.022(3) 0.028(3) -0.003(3) -0.002(2) 0.002(2) O13 0.0210(19) 0.014(2) 0.028(2) -0.0051(18) -0.0042(17) -0.0007(16) O14 0.0089(17) 0.0120(18) 0.021(2) -0.0030(16) 0.0042(14) 0.0018(14) O15 0.028(2) 0.016(2) 0.029(2) 0.0059(18) 0.0070(18) 0.0068(17) O16 0.037(2) 0.045(3) 0.030(3) -0.001(2) 0.013(2) 0.014(2) N4 0.014(2) 0.016(2) 0.020(2) 0.000(2) 0.0032(18) 0.0012(18) C34 0.019(3) 0.020(3) 0.019(3) -0.003(2) 0.005(2) -0.005(2) C35 0.030(3) 0.023(3) 0.028(3) -0.006(3) -0.002(3) -0.005(3) C36 0.026(3) 0.040(4) 0.046(4) -0.013(4) 0.002(3) -0.007(3) C37 0.038(4) 0.022(3) 0.067(5) -0.021(4) 0.006(4) -0.010(3) C38 0.036(4) 0.014(3) 0.055(5) -0.009(3) 0.006(3) 0.000(3) C39 0.025(3) 0.023(3) 0.025(3) -0.006(3) 0.007(2) -0.002(2) C40 0.027(3) 0.017(3) 0.031(3) 0.002(3) 0.010(3) 0.009(2) C41 0.014(3) 0.019(3) 0.027(3) 0.004(3) 0.001(2) 0.005(2) C42 0.008(2) 0.018(3) 0.026(3) -0.002(2) 0.003(2) 0.004(2) C43 0.024(3) 0.023(3) 0.032(3) 0.005(3) 0.003(3) 0.011(2) C44 0.020(3) 0.021(3) 0.029(3) -0.002(3) 0.005(2) 0.003(2) O17 0.0167(19) 0.022(2) 0.027(2) 0.0026(19) 0.0031(16) 0.0027(16) O18 0.023(2) 0.019(2) 0.023(2) 0.0014(18) 0.0011(17) 0.0059(16) C45 0.023(3) 0.013(3) 0.023(3) -0.005(2) 0.002(2) -0.004(2) C46 0.050(4) 0.046(5) 0.045(5) 0.019(4) 0.020(4) 0.007(3) O19 0.032(2) 0.020(2) 0.025(2) 0.0035(19) 0.0065(18) 0.0013(18) O20 0.032(2) 0.015(2) 0.025(2) 0.0025(18) 0.0032(18) 0.0008(17) C47 0.014(3) 0.022(3) 0.026(3) 0.008(3) 0.001(2) -0.002(2) C48 0.048(4) 0.029(4) 0.052(5) 0.008(4) 0.026(4) -0.008(3) O1W 0.042(3) 0.064(3) 0.020(2) 0.002(2) 0.007(2) -0.011(2) O2W 0.028(2) 0.054(3) 0.058(3) -0.012(3) 0.003(2) -0.009(2) O3W 0.046(6) 0.088(9) 0.040(6) -0.001(6) -0.007(5) 0.031(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O5 1.881(3) . ? Co1 O1 1.890(4) . ? Co1 N2 1.893(4) . ? Co1 N1 1.898(4) . ? Co1 O2 1.901(4) . ? Co1 O6 1.930(3) . ? Co1 Co4 2.9955(10) . ? Co2 O13 1.872(4) . ? Co2 O9 1.883(4) . ? Co2 N4 1.887(4) . ? Co2 N3 1.896(4) . ? Co2 O10 1.897(4) . ? Co2 O14 1.942(3) . ? Co2 Co5 2.9976(10) . ? Co3 O18 2.070(4) . ? Co3 O11 2.075(3) . ? Co3 O3 2.084(3) . ? Co3 O17 2.120(4) . ? Co3 O14 2.140(3) . ? Co3 O6 2.231(3) . ? Co3 C45 2.446(6) . ? Co3 Co5 2.8545(10) . ? Co3 Co4 2.8591(10) . ? Co4 O19 2.021(4) . ? Co4 O2 2.048(3) . ? Co4 O11 2.064(3) . ? Co4 O6 2.097(3) . ? Co4 O7 2.138(3) . ? Co4 O3 2.157(3) . ? Co5 O10 2.007(3) . ? Co5 O20 2.019(4) . ? Co5 O3 2.090(3) . ? Co5 O15 2.120(3) . ? Co5 O14 2.126(4) . ? Co5 O11 2.181(3) . ? O1 C1 1.324(6) . ? O2 C10 1.420(5) . ? O3 C9 1.414(5) . ? O4 C11 1.404(6) . ? N1 C7 1.276(6) . ? N1 C8 1.484(6) . ? C1 C2 1.395(7) . ? C1 C6 1.423(7) . ? C2 C3 1.366(8) . ? C3 C4 1.383(8) . ? C4 C5 1.356(8) . ? C5 C6 1.406(7) . ? C6 C7 1.439(7) . ? C8 C9 1.522(7) . ? C8 C10 1.540(7) . ? C8 C11 1.540(6) . ? O5 C12 1.306(6) . ? O6 C20 1.430(5) . ? O7 C21 1.424(6) . ? O8 C22 1.426(6) . ? N2 C18 1.273(7) . ? N2 C19 1.500(6) . ? C12 C17 1.411(7) . ? C12 C13 1.418(7) . ? C13 C14 1.362(8) . ? C14 C15 1.397(8) . ? C15 C16 1.370(8) . ? C16 C17 1.403(8) . ? C17 C18 1.446(7) . ? C19 C20 1.524(7) . ? C19 C22 1.525(7) . ? C19 C21 1.535(7) . ? O9 C23 1.305(6) . ? O10 C31 1.418(6) . ? O11 C32 1.410(5) . ? O12 C33 1.417(6) . ? N3 C29 1.272(7) . ? N3 C30 1.503(7) . ? C23 C24 1.403(8) . ? C23 C28 1.425(7) . ? C24 C25 1.366(8) . ? C25 C26 1.386(8) . ? C26 C27 1.368(8) . ? C27 C28 1.413(7) . ? C28 C29 1.433(8) . ? C30 C32 1.517(7) . ? C30 C31 1.524(7) . ? C30 C33 1.529(6) . ? O13 C34 1.301(6) . ? O14 C42 1.423(5) . ? O15 C43 1.436(7) . ? O16 C44 1.421(7) . ? N4 C40 1.276(7) . ? N4 C41 1.487(6) . ? C34 C35 1.410(7) . ? C34 C39 1.420(7) . ? C35 C36 1.366(9) . ? C36 C37 1.388(9) . ? C37 C38 1.363(8) . ? C38 C39 1.404(8) . ? C39 C40 1.434(7) . ? C41 C43 1.524(8) . ? C41 C42 1.527(7) . ? C41 C44 1.535(7) . ? O17 C45 1.280(6) . ? O18 C45 1.268(6) . ? C45 C46 1.481(8) . ? O19 C47 1.253(7) . ? O20 C47 1.256(7) . ? C47 C48 1.513(8) . ? O3W O3W 1.543(19) 2_645 ? 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 O5 Co1 O1 89.95(15) . . ? O5 Co1 N2 95.08(17) . . ? O1 Co1 N2 85.68(16) . . ? O5 Co1 N1 88.55(16) . . ? O1 Co1 N1 97.18(17) . . ? N2 Co1 N1 175.39(18) . . ? O5 Co1 O2 91.36(15) . . ? O1 Co1 O2 176.76(14) . . ? N2 Co1 O2 91.26(16) . . ? N1 Co1 O2 85.81(16) . . ? O5 Co1 O6 177.84(15) . . ? O1 Co1 O6 92.18(15) . . ? N2 Co1 O6 84.75(16) . . ? N1 Co1 O6 91.51(16) . . ? O2 Co1 O6 86.49(14) . . ? O5 Co1 Co4 133.72(11) . . ? O1 Co1 Co4 135.85(11) . . ? N2 Co1 Co4 84.37(12) . . ? N1 Co1 Co4 91.07(13) . . ? O2 Co1 Co4 42.53(10) . . ? O6 Co1 Co4 44.12(10) . . ? O13 Co2 O9 92.17(17) . . ? O13 Co2 N4 95.82(17) . . ? O9 Co2 N4 86.05(17) . . ? O13 Co2 N3 87.32(16) . . ? O9 Co2 N3 96.48(17) . . ? N4 Co2 N3 175.90(19) . . ? O13 Co2 O10 90.78(16) . . ? O9 Co2 O10 175.80(14) . . ? N4 Co2 O10 90.68(17) . . ? N3 Co2 O10 86.64(17) . . ? O13 Co2 O14 176.81(16) . . ? O9 Co2 O14 91.01(15) . . ? N4 Co2 O14 84.58(16) . . ? N3 Co2 O14 92.13(16) . . ? O10 Co2 O14 86.05(15) . . ? O13 Co2 Co5 131.89(12) . . ? O9 Co2 Co5 135.61(11) . . ? N4 Co2 Co5 84.56(14) . . ? N3 Co2 Co5 91.39(14) . . ? O10 Co2 Co5 41.20(10) . . ? O14 Co2 Co5 44.96(10) . . ? O18 Co3 O11 113.19(13) . . ? O18 Co3 O3 167.42(14) . . ? O11 Co3 O3 73.40(12) . . ? O18 Co3 O17 62.77(14) . . ? O11 Co3 O17 172.53(14) . . ? O3 Co3 O17 111.85(13) . . ? O18 Co3 O14 108.21(14) . . ? O11 Co3 O14 83.76(13) . . ? O3 Co3 O14 82.72(14) . . ? O17 Co3 O14 91.56(14) . . ? O18 Co3 O6 89.37(14) . . ? O11 Co3 O6 81.64(13) . . ? O3 Co3 O6 80.87(13) . . ? O17 Co3 O6 104.17(14) . . ? O14 Co3 O6 160.57(13) . . ? O18 Co3 C45 31.22(15) . . ? O11 Co3 C45 144.11(15) . . ? O3 Co3 C45 142.23(15) . . ? O17 Co3 C45 31.55(15) . . ? O14 Co3 C45 101.74(16) . . ? O6 Co3 C45 97.60(15) . . ? O18 Co3 Co5 145.51(11) . . ? O11 Co3 Co5 49.46(9) . . ? O3 Co3 Co5 46.95(9) . . ? O17 Co3 Co5 129.94(10) . . ? O14 Co3 Co5 47.78(10) . . ? O6 Co3 Co5 112.81(9) . . ? C45 Co3 Co5 149.45(13) . . ? O18 Co3 Co4 127.58(11) . . ? O11 Co3 Co4 46.15(10) . . ? O3 Co3 Co4 48.70(9) . . ? O17 Co3 Co4 141.30(11) . . ? O14 Co3 Co4 114.01(10) . . ? O6 Co3 Co4 46.67(9) . . ? C45 Co3 Co4 144.24(13) . . ? Co5 Co3 Co4 66.28(3) . . ? O19 Co4 O2 99.85(15) . . ? O19 Co4 O11 97.72(15) . . ? O2 Co4 O11 157.12(14) . . ? O19 Co4 O6 174.45(15) . . ? O2 Co4 O6 78.58(13) . . ? O11 Co4 O6 85.21(14) . . ? O19 Co4 O7 85.97(14) . . ? O2 Co4 O7 98.40(14) . . ? O11 Co4 O7 97.33(14) . . ? O6 Co4 O7 88.98(13) . . ? O19 Co4 O3 103.02(14) . . ? O2 Co4 O3 89.66(13) . . ? O11 Co4 O3 72.12(13) . . ? O6 Co4 O3 82.34(13) . . ? O7 Co4 O3 166.79(14) . . ? O19 Co4 Co3 134.37(12) . . ? O2 Co4 Co3 110.80(10) . . ? O11 Co4 Co3 46.48(9) . . ? O6 Co4 Co3 50.69(10) . . ? O7 Co4 Co3 120.35(11) . . ? O3 Co4 Co3 46.55(9) . . ? O19 Co4 Co1 137.99(12) . . ? O2 Co4 Co1 38.88(10) . . ? O11 Co4 Co1 124.06(10) . . ? O6 Co4 Co1 39.85(9) . . ? O7 Co4 Co1 92.26(10) . . ? O3 Co4 Co1 87.46(9) . . ? Co3 Co4 Co1 81.60(3) . . ? O10 Co5 O20 98.44(15) . . ? O10 Co5 O3 155.34(14) . . ? O20 Co5 O3 99.78(15) . . ? O10 Co5 O15 99.07(14) . . ? O20 Co5 O15 92.58(15) . . ? O3 Co5 O15 96.58(13) . . ? O10 Co5 O14 78.64(13) . . ? O20 Co5 O14 177.06(14) . . ? O3 Co5 O14 82.94(13) . . ? O15 Co5 O14 88.21(13) . . ? O10 Co5 O11 89.93(13) . . ? O20 Co5 O11 98.14(14) . . ? O3 Co5 O11 71.16(12) . . ? O15 Co5 O11 164.86(14) . . ? O14 Co5 O11 81.62(13) . . ? O10 Co5 Co3 108.64(10) . . ? O20 Co5 Co3 133.29(11) . . ? O3 Co5 Co3 46.78(9) . . ? O15 Co5 Co3 118.74(10) . . ? O14 Co5 Co3 48.22(9) . . ? O11 Co5 Co3 46.33(9) . . ? O10 Co5 Co2 38.52(10) . . ? O20 Co5 Co2 136.89(11) . . ? O3 Co5 Co2 121.98(10) . . ? O15 Co5 Co2 92.76(11) . . ? O14 Co5 Co2 40.20(9) . . ? O11 Co5 Co2 86.71(9) . . ? Co3 Co5 Co2 78.98(3) . . ? C1 O1 Co1 124.9(3) . . ? C10 O2 Co1 108.5(3) . . ? C10 O2 Co4 117.6(3) . . ? Co1 O2 Co4 98.60(15) . . ? C9 O3 Co3 123.0(3) . . ? C9 O3 Co5 126.8(3) . . ? Co3 O3 Co5 86.27(12) . . ? C9 O3 Co4 128.0(3) . . ? Co3 O3 Co4 84.75(12) . . ? Co5 O3 Co4 94.67(12) . . ? C7 N1 C8 122.1(4) . . ? C7 N1 Co1 123.6(4) . . ? C8 N1 Co1 114.2(3) . . ? O1 C1 C2 118.4(5) . . ? O1 C1 C6 123.6(5) . . ? C2 C1 C6 118.0(5) . . ? C3 C2 C1 121.9(5) . . ? C2 C3 C4 120.4(6) . . ? C5 C4 C3 119.3(6) . . ? C4 C5 C6 122.4(5) . . ? C5 C6 C1 117.9(5) . . ? C5 C6 C7 118.3(5) . . ? C1 C6 C7 123.6(5) . . ? N1 C7 C6 126.6(5) . . ? N1 C8 C9 110.7(4) . . ? N1 C8 C10 104.9(4) . . ? C9 C8 C10 112.1(4) . . ? N1 C8 C11 113.3(4) . . ? C9 C8 C11 105.9(4) . . ? C10 C8 C11 110.1(4) . . ? O3 C9 C8 114.3(4) . . ? O2 C10 C8 110.5(4) . . ? O4 C11 C8 114.3(4) . . ? C12 O5 Co1 123.8(3) . . ? C20 O6 Co1 108.5(3) . . ? C20 O6 Co4 115.0(3) . . ? Co1 O6 Co4 96.03(15) . . ? C20 O6 Co3 113.9(3) . . ? Co1 O6 Co3 133.68(15) . . ? Co4 O6 Co3 82.64(12) . . ? C21 O7 Co4 132.6(3) . . ? C18 N2 C19 120.8(4) . . ? C18 N2 Co1 124.9(3) . . ? C19 N2 Co1 114.2(3) . . ? O5 C12 C17 124.1(5) . . ? O5 C12 C13 118.7(5) . . ? C17 C12 C13 117.1(5) . . ? C14 C13 C12 121.7(5) . . ? C13 C14 C15 120.9(5) . . ? C16 C15 C14 118.9(6) . . ? C15 C16 C17 121.5(5) . . ? C16 C17 C12 119.9(5) . . ? C16 C17 C18 117.3(5) . . ? C12 C17 C18 122.8(5) . . ? N2 C18 C17 124.9(5) . . ? N2 C19 C20 107.2(4) . . ? N2 C19 C22 109.4(4) . . ? C20 C19 C22 110.0(4) . . ? N2 C19 C21 108.7(4) . . ? C20 C19 C21 111.5(4) . . ? C22 C19 C21 109.9(4) . . ? O6 C20 C19 111.0(4) . . ? O7 C21 C19 109.6(4) . . ? O8 C22 C19 111.5(4) . . ? C23 O9 Co2 124.8(3) . . ? C31 O10 Co2 108.4(3) . . ? C31 O10 Co5 116.0(3) . . ? Co2 O10 Co5 100.28(14) . . ? C32 O11 Co4 127.4(3) . . ? C32 O11 Co3 122.0(3) . . ? Co4 O11 Co3 87.37(12) . . ? C32 O11 Co5 127.7(3) . . ? Co4 O11 Co5 94.72(13) . . ? Co3 O11 Co5 84.21(12) . . ? C29 N3 C30 122.0(4) . . ? C29 N3 Co2 124.8(4) . . ? C30 N3 Co2 113.2(3) . . ? O9 C23 C24 118.5(5) . . ? O9 C23 C28 124.8(5) . . ? C24 C23 C28 116.8(5) . . ? C25 C24 C23 122.3(5) . . ? C24 C25 C26 121.1(6) . . ? C27 C26 C25 118.8(6) . . ? C26 C27 C28 121.7(5) . . ? C27 C28 C23 119.4(5) . . ? C27 C28 C29 117.7(5) . . ? C23 C28 C29 123.0(5) . . ? N3 C29 C28 125.9(5) . . ? N3 C30 C32 109.4(4) . . ? N3 C30 C31 105.5(4) . . ? C32 C30 C31 112.4(4) . . ? N3 C30 C33 112.5(4) . . ? C32 C30 C33 110.5(4) . . ? C31 C30 C33 106.5(4) . . ? O10 C31 C30 111.7(4) . . ? O11 C32 C30 113.6(4) . . ? O12 C33 C30 111.2(4) . . ? C34 O13 Co2 124.6(3) . . ? C42 O14 Co2 107.6(3) . . ? C42 O14 Co5 116.8(3) . . ? Co2 O14 Co5 94.84(14) . . ? C42 O14 Co3 116.1(3) . . ? Co2 O14 Co3 131.52(15) . . ? Co5 O14 Co3 84.00(13) . . ? C43 O15 Co5 132.0(3) . . ? C40 N4 C41 120.9(4) . . ? C40 N4 Co2 124.7(4) . . ? C41 N4 Co2 114.5(3) . . ? O13 C34 C35 118.1(5) . . ? O13 C34 C39 125.0(5) . . ? C35 C34 C39 116.9(5) . . ? C36 C35 C34 121.5(6) . . ? C35 C36 C37 121.3(6) . . ? C38 C37 C36 118.8(6) . . ? C37 C38 C39 121.6(6) . . ? C38 C39 C34 119.8(5) . . ? C38 C39 C40 118.2(5) . . ? C34 C39 C40 122.0(5) . . ? N4 C40 C39 125.9(5) . . ? N4 C41 C43 110.5(4) . . ? N4 C41 C42 107.0(4) . . ? C43 C41 C42 110.5(5) . . ? N4 C41 C44 110.9(5) . . ? C43 C41 C44 108.8(4) . . ? C42 C41 C44 109.1(4) . . ? O14 C42 C41 110.6(4) . . ? O15 C43 C41 110.8(4) . . ? O16 C44 C41 112.5(4) . . ? C45 O17 Co3 88.4(3) . . ? C45 O18 Co3 91.0(3) . . ? O18 C45 O17 117.8(5) . . ? O18 C45 C46 120.9(5) . . ? O17 C45 C46 121.3(5) . . ? O18 C45 Co3 57.8(3) . . ? O17 C45 Co3 60.0(3) . . ? C46 C45 Co3 178.6(4) . . ? C47 O19 Co4 128.6(4) . . ? C47 O20 Co5 130.2(4) . . ? O19 C47 O20 125.6(5) . . ? O19 C47 C48 116.8(5) . . ? O20 C47 C48 117.6(5) . . ? 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 O4 H4 O1W 0.85 1.83 2.668(6) 170.9 . O7 H7 O4 0.85 1.93 2.672(5) 145.5 1_655 O8 H8 O1 0.85 1.94 2.793(5) 179.8 . O12 H12 O17 0.85 1.89 2.736(5) 178.6 1_655 O15 H15 O8 0.85 1.83 2.615(5) 153.2 1_565 O16 H16 O9 0.85 2.03 2.884(5) 176.9 . O1W H1WA O2 0.85 2.10 2.870(5) 150.3 2 O1W H1WB O19 0.85 2.14 2.909(6) 150.6 2 O2W H2WA O5 0.85 2.01 2.839(5) 166.7 1_655 O2W H2WB O3W 0.85 1.87 2.701(10) 166.3 . O2W H2WB O3W 0.85 2.26 2.965(12) 140.1 2_645 _diffrn_measured_fraction_theta_max 0.953 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.726 _refine_diff_density_min -0.615 _refine_diff_density_rms 0.114