# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Clotilde Policar' _publ_contact_author_address ; Institut de Chimie Moleculaire et des Materiaux d'Orsay Universite PARIS XI LCBB, ICMMO B\^at. 420 ORSAY F-91405 FRANCE ; _publ_contact_author_email CPOLICAR@ICMO.U-PSUD.FR _publ_section_title ; Superoxide Dismutase Activity of Cobalt(II) Complexes Based on a Sugar Plateform. ; loop_ _publ_author_name 'Clotilde Policar' 'Francois Bellot' 'Renaud Hardre' 'Giorgio Pelosi' 'Michel Therisod' data_1 _database_code_depnum_ccdc_archive 'CCDC 264230' _chemical_name_systematic ; [3,4,6-tri-O-(2-picolyl)-1,2-O-ethylidene-^[$B&A^[(B-D-galactopyranose] cobalt(II) bis(hexafluorophosphate) ; _chemical_melting_point ? _chemical_formula_sum 'C26 H29 Co F12 N3 O6 P2' _chemical_formula_weight 828.39 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' P P 0.1023 0.0942 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 10.1390(10) _cell_length_b 16.795(2) _cell_length_c 18.882(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3215.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _exptl_crystal_density_diffrn 1.711 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1676 _exptl_absorpt_coefficient_mu 0.749 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.22 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.81944 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'Bruker AXS SADABS (1999)' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 26171 _diffrn_reflns_av_R_equivalents 0.0310 _diffrn_reflns_av_sigmaI/netI 0.0223 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 23.26 _reflns_number_total 4616 _reflns_number_gt 4124 _reflns_threshold_expression >2sigma(I) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0724P)^2^+0.1761P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.007(17) _refine_ls_number_reflns 4616 _refine_ls_number_parameters 471 _refine_ls_number_restraints 0 #_refine_ls_R_factor_all 0.0430 _refine_ls_R_factor_all 0.0430 _refine_ls_R_factor_gt 0.0372 _refine_ls_wR_factor_ref 0.1034 _refine_ls_wR_factor_gt 0.0999 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.044 _refine_ls_shift/su_mean 0.005 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 0.57113(5) 0.06379(3) 0.27585(3) 0.04519(16) Uani 1 1 d . . . P1 P 0.39157(14) -0.20311(8) 0.63738(8) 0.0744(4) Uani 1 1 d . . . P2 P 0.47665(13) 0.12853(8) 0.55109(7) 0.0609(3) Uani 1 1 d . . . F1 F 0.3989(9) -0.2460(4) 0.7100(3) 0.211(3) Uani 1 1 d . . . F2 F 0.5174(6) -0.1621(4) 0.6619(4) 0.217(3) Uani 1 1 d . . . F3 F 0.4693(5) -0.2762(3) 0.6058(3) 0.154(2) Uani 1 1 d . . . F4 F 0.3087(6) -0.1388(4) 0.6726(4) 0.193(3) Uani 1 1 d . . . F5 F 0.2648(5) -0.2541(4) 0.6181(4) 0.171(2) Uani 1 1 d . . . F6 F 0.3866(11) -0.1688(3) 0.5652(3) 0.236(4) Uani 1 1 d . . . F7 F 0.4347(4) 0.1020(2) 0.47393(16) 0.1048(11) Uani 1 1 d . . . F8 F 0.5188(3) 0.1553(2) 0.62832(16) 0.0944(10) Uani 1 1 d . . . F9 F 0.4283(5) 0.0483(2) 0.5816(2) 0.1371(16) Uani 1 1 d . . . F10 F 0.3400(4) 0.1688(3) 0.5603(3) 0.151(2) Uani 1 1 d . . . F11 F 0.5392(5) 0.2080(2) 0.5205(2) 0.1311(15) Uani 1 1 d . . . F12 F 0.6179(4) 0.0889(3) 0.5405(2) 0.1218(14) Uani 1 1 d . . . O1 O 0.9463(3) 0.01646(18) 0.30875(15) 0.0586(7) Uani 1 1 d . . . O2 O 0.7445(3) 0.13122(15) 0.31891(15) 0.0483(6) Uani 1 1 d . . . O3 O 0.6167(3) 0.00662(16) 0.36759(15) 0.0514(7) Uani 1 1 d . . . O4 O 0.7110(3) -0.01790(16) 0.23557(15) 0.0535(7) Uani 1 1 d . . . O5 O 0.9561(3) 0.0830(2) 0.46887(16) 0.0658(8) Uani 1 1 d . . . O6 O 1.1083(3) 0.0353(2) 0.39318(19) 0.0826(11) Uani 1 1 d . . . N3 N 0.5951(3) 0.1023(2) 0.17322(17) 0.0524(8) Uani 1 1 d . . . N2 N 0.4156(3) -0.01655(18) 0.28885(18) 0.0512(8) Uani 1 1 d . . . N1 N 0.4846(3) 0.1676(2) 0.31648(17) 0.0472(8) Uani 1 1 d . . . C1 C 1.0141(4) 0.0729(3) 0.3499(2) 0.0592(11) Uani 1 1 d . . . C2 C 0.9249(5) 0.1177(3) 0.4028(2) 0.0547(10) Uani 1 1 d . . . C3 C 0.7781(4) 0.1021(3) 0.3884(2) 0.0474(10) Uani 1 1 d . . . C4 C 0.7528(4) 0.0129(3) 0.3902(2) 0.0522(10) Uani 1 1 d . . . C5 C 0.8485(4) -0.0333(3) 0.3417(3) 0.0571(11) Uani 1 1 d . . . C6 C 0.7810(4) -0.0738(2) 0.2792(3) 0.0602(11) Uani 1 1 d . . . H1A H 0.8469 -0.1009 0.2508 0.072 Uiso 1 1 calc R . . H1B H 0.7198 -0.1135 0.2968 0.072 Uiso 1 1 calc R . . C19 C 0.7830(5) 0.0130(3) 0.1767(2) 0.0632(12) Uani 1 1 d . . . H7A H 0.8042 -0.0297 0.1441 0.076 Uiso 1 1 calc R . . H7B H 0.8649 0.0365 0.1930 0.076 Uiso 1 1 calc R . . C20 C 0.7026(4) 0.0742(3) 0.1399(2) 0.0527(10) Uani 1 1 d . . . C21 C 0.7407(5) 0.1025(3) 0.0744(2) 0.0712(14) Uani 1 1 d . . . H9 H 0.8158 0.0827 0.0523 0.085 Uiso 1 1 calc R . . C22 C 0.6656(6) 0.1608(3) 0.0423(3) 0.0787(15) Uani 1 1 d . . . H10 H 0.6910 0.1820 -0.0011 0.094 Uiso 1 1 calc R . . C23 C 0.5543(6) 0.1868(3) 0.0748(2) 0.0723(14) Uani 1 1 d . . . H11 H 0.5011 0.2246 0.0529 0.087 Uiso 1 1 calc R . . C24 C 0.5207(5) 0.1570(3) 0.1398(2) 0.0653(12) Uani 1 1 d . . . H12 H 0.4441 0.1752 0.1616 0.078 Uiso 1 1 calc R . . C13 C 0.5356(4) -0.0548(3) 0.3958(2) 0.0582(11) Uani 1 1 d . . . H13A H 0.5062 -0.0410 0.4432 0.070 Uiso 1 1 calc R . . H13B H 0.5841 -0.1045 0.3983 0.070 Uiso 1 1 calc R . . C14 C 0.4188(4) -0.0630(2) 0.3465(2) 0.0527(9) Uani 1 1 d . . . C15 C 0.3207(5) -0.1177(3) 0.3609(3) 0.0701(13) Uani 1 1 d . . . H15 H 0.3241 -0.1487 0.4016 0.084 Uiso 1 1 calc R . . C16 C 0.2184(5) -0.1254(3) 0.3141(3) 0.0775(15) Uani 1 1 d . . . H16 H 0.1520 -0.1623 0.3228 0.093 Uiso 1 1 calc R . . C17 C 0.2135(5) -0.0797(3) 0.2552(3) 0.0748(15) Uani 1 1 d . . . H17 H 0.1443 -0.0848 0.2233 0.090 Uiso 1 1 calc R . . C18 C 0.3139(4) -0.0249(3) 0.2434(3) 0.0613(12) Uani 1 1 d . . . H18 H 0.3109 0.0068 0.2031 0.074 Uiso 1 1 calc R . . C7 C 0.7103(4) 0.2135(3) 0.3162(3) 0.0624(12) Uani 1 1 d . . . H19A H 0.7282 0.2340 0.2691 0.075 Uiso 1 1 calc R . . H19B H 0.7647 0.2428 0.3495 0.075 Uiso 1 1 calc R . . C8 C 0.5679(5) 0.2268(2) 0.3337(2) 0.0520(10) Uani 1 1 d . . . C9 C 0.5241(6) 0.2955(3) 0.3661(3) 0.0738(14) Uani 1 1 d . . . H21 H 0.5836 0.3349 0.3795 0.089 Uiso 1 1 calc R . . C10 C 0.3914(6) 0.3050(3) 0.3784(3) 0.0848(17) Uani 1 1 d . . . H22 H 0.3598 0.3517 0.3987 0.102 Uiso 1 1 calc R . . C11 C 0.3051(6) 0.2445(4) 0.3602(3) 0.0796(16) Uani 1 1 d . . . H23 H 0.2151 0.2498 0.3685 0.096 Uiso 1 1 calc R . . C12 C 0.3548(5) 0.1767(3) 0.3297(3) 0.0633(12) Uani 1 1 d . . . H24 H 0.2972 0.1357 0.3178 0.076 Uiso 1 1 calc R . . C25 C 1.0889(6) 0.0609(4) 0.4646(3) 0.0851(15) Uani 1 1 d . . . H25 H 1.1439 0.1078 0.4735 0.102 Uiso 1 1 calc R . . C26 C 1.1238(6) -0.0016(4) 0.5157(4) 0.102(2) Uani 1 1 d . . . H26A H 1.2157 -0.0144 0.5111 0.153 Uiso 1 1 calc R . . H26B H 1.0719 -0.0483 0.5066 0.153 Uiso 1 1 calc R . . H26C H 1.1067 0.0170 0.5629 0.153 Uiso 1 1 calc R . . H3 H 0.894(6) -0.077(3) 0.362(3) 0.101(19) Uiso 1 1 d . . . H4 H 0.727(4) 0.123(2) 0.423(2) 0.054(12) Uiso 1 1 d . . . H10' H 0.773(4) -0.002(2) 0.438(2) 0.040(10) Uiso 1 1 d . . . H11' H 0.947(4) 0.172(2) 0.3995(17) 0.036(9) Uiso 1 1 d . . . H40 H 1.053(5) 0.105(3) 0.305(3) 0.075(14) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0417(3) 0.0454(3) 0.0485(3) 0.0021(2) 0.0023(2) 0.0025(2) P1 0.0747(9) 0.0644(8) 0.0842(9) -0.0130(7) 0.0111(7) -0.0018(7) P2 0.0569(7) 0.0700(7) 0.0557(7) -0.0020(6) 0.0008(5) 0.0048(6) F1 0.341(10) 0.184(5) 0.108(3) 0.018(3) -0.004(5) -0.060(6) F2 0.166(5) 0.268(7) 0.216(6) -0.101(5) 0.028(4) -0.131(5) F3 0.135(4) 0.149(3) 0.178(4) -0.062(3) -0.033(3) 0.061(3) F4 0.159(5) 0.167(5) 0.254(7) -0.109(5) 0.037(5) 0.035(4) F5 0.101(3) 0.184(5) 0.229(6) -0.086(4) -0.002(4) -0.020(3) F6 0.460(13) 0.138(4) 0.110(4) 0.037(3) 0.001(6) 0.046(6) F7 0.125(3) 0.125(3) 0.0636(17) -0.0246(17) -0.0191(18) 0.037(2) F8 0.082(2) 0.133(3) 0.0688(17) -0.0183(18) -0.0002(16) -0.0237(19) F9 0.182(4) 0.116(3) 0.113(3) 0.016(2) -0.007(3) -0.070(3) F10 0.080(2) 0.226(5) 0.148(3) -0.095(4) -0.030(2) 0.068(3) F11 0.166(4) 0.108(3) 0.120(3) 0.037(2) -0.014(3) -0.025(3) F12 0.091(2) 0.181(4) 0.093(2) 0.014(3) 0.0092(19) 0.059(3) O1 0.0420(16) 0.0743(19) 0.0594(16) -0.0090(15) 0.0048(13) 0.0039(15) O2 0.0428(15) 0.0445(15) 0.0577(17) -0.0013(13) -0.0008(13) 0.0026(12) O3 0.0441(15) 0.0538(16) 0.0564(16) 0.0135(13) -0.0025(13) -0.0055(13) O4 0.0519(16) 0.0538(16) 0.0548(17) -0.0044(14) 0.0020(14) 0.0088(13) O5 0.0452(18) 0.092(2) 0.0604(18) -0.0105(16) -0.0087(14) 0.0076(16) O6 0.052(2) 0.113(3) 0.083(2) -0.026(2) -0.0168(17) 0.0209(19) N3 0.051(2) 0.0566(19) 0.0496(19) -0.0018(16) 0.0037(17) 0.0068(17) N2 0.0434(18) 0.0508(19) 0.059(2) -0.0091(16) 0.0002(17) 0.0020(16) N1 0.0427(19) 0.0519(19) 0.0471(18) -0.0010(15) -0.0021(16) 0.0032(16) C1 0.034(2) 0.079(3) 0.065(3) -0.006(3) -0.003(2) 0.002(2) C2 0.046(2) 0.056(3) 0.062(3) -0.009(2) -0.008(2) -0.003(2) C3 0.036(2) 0.055(2) 0.051(2) -0.0101(19) 0.0001(19) 0.0062(19) C4 0.042(2) 0.067(3) 0.047(2) 0.009(2) -0.0040(18) -0.003(2) C5 0.050(3) 0.049(2) 0.073(3) -0.002(2) -0.007(2) 0.007(2) C6 0.061(3) 0.047(2) 0.072(3) -0.007(2) -0.007(2) 0.010(2) C19 0.053(3) 0.080(3) 0.056(3) -0.004(2) 0.012(2) 0.009(2) C20 0.050(2) 0.065(3) 0.044(2) -0.005(2) -0.0026(19) -0.007(2) C21 0.062(3) 0.106(4) 0.047(3) -0.004(3) 0.011(2) -0.013(3) C22 0.092(4) 0.099(4) 0.045(3) 0.014(3) -0.001(3) -0.016(3) C23 0.093(4) 0.070(3) 0.054(3) 0.010(2) -0.010(3) -0.001(3) C24 0.067(3) 0.068(3) 0.061(3) 0.003(2) -0.005(2) 0.009(2) C13 0.049(2) 0.057(2) 0.069(3) 0.014(2) 0.001(2) -0.008(2) C14 0.049(2) 0.0424(19) 0.067(3) -0.003(2) 0.008(2) -0.005(2) C15 0.058(3) 0.054(3) 0.099(4) -0.002(3) 0.009(3) -0.003(2) C16 0.053(3) 0.068(3) 0.112(5) -0.025(3) 0.012(3) -0.023(2) C17 0.045(3) 0.081(4) 0.099(4) -0.032(3) -0.003(2) -0.006(2) C18 0.048(3) 0.069(3) 0.067(3) -0.012(2) -0.004(2) 0.004(2) C7 0.059(3) 0.048(2) 0.081(3) 0.003(2) -0.007(2) -0.001(2) C8 0.059(2) 0.041(2) 0.056(2) 0.0032(18) -0.008(2) 0.009(2) C9 0.085(4) 0.047(2) 0.090(3) -0.008(2) -0.023(3) 0.010(2) C10 0.096(5) 0.072(3) 0.086(4) -0.016(3) -0.006(3) 0.037(3) C11 0.065(3) 0.098(4) 0.076(3) -0.003(3) 0.004(3) 0.041(3) C12 0.052(3) 0.068(3) 0.070(3) -0.005(2) 0.003(2) 0.013(2) C25 0.069(3) 0.110(4) 0.076(3) 0.000(3) -0.011(3) 0.010(4) C26 0.093(4) 0.095(4) 0.118(5) 0.025(4) -0.021(4) 0.006(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O3 2.034(3) . ? Co1 N3 2.057(3) . ? Co1 N2 2.090(3) . ? Co1 N1 2.097(3) . ? Co1 O4 2.115(3) . ? Co1 O2 2.244(3) . ? P1 F6 1.481(5) . ? P1 F4 1.522(5) . ? P1 F2 1.522(5) . ? P1 F1 1.551(5) . ? P1 F3 1.576(4) . ? P1 F5 1.587(5) . ? P2 F9 1.546(4) . ? P2 F10 1.551(4) . ? P2 F7 1.582(3) . ? P2 F8 1.585(3) . ? P2 F11 1.587(4) . ? P2 F12 1.592(4) . ? O1 C1 1.405(5) . ? O1 C5 1.438(5) . ? O2 C7 1.427(5) . ? O2 C3 1.441(5) . ? O3 C13 1.424(5) . ? O3 C4 1.448(5) . ? O4 C19 1.428(5) . ? O4 C6 1.436(5) . ? O5 C25 1.398(6) . ? O5 C2 1.414(5) . ? O6 C1 1.406(6) . ? O6 C25 1.429(6) . ? N3 C20 1.344(5) . ? N3 C24 1.346(6) . ? N2 C14 1.340(5) . ? N2 C18 1.349(5) . ? N1 C8 1.344(5) . ? N1 C12 1.349(5) . ? C1 C2 1.543(6) . ? C1 H40 1.08(5) . ? C2 C3 1.535(6) . ? C2 H11 0.94(4) . ? C3 C4 1.521(6) . ? C3 H4 0.91(4) . ? C4 C5 1.544(6) . ? C4 H10 0.95(4) . ? C5 C6 1.524(6) . ? C5 H3 0.94(6) . ? C6 H1A 0.9700 . ? C6 H1B 0.9700 . ? C19 C20 1.484(6) . ? C19 H7A 0.9700 . ? C19 H7B 0.9700 . ? C20 C21 1.379(7) . ? C21 C22 1.381(7) . ? C21 H9 0.9300 . ? C22 C23 1.356(8) . ? C22 H10 0.9300 . ? C23 C24 1.369(7) . ? C23 H11 0.9300 . ? C24 H12 0.9300 . ? C13 C14 1.512(6) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.381(6) . ? C15 C16 1.369(8) . ? C15 H15 0.9300 . ? C16 C17 1.352(8) . ? C16 H16 0.9300 . ? C17 C18 1.390(7) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C7 C8 1.498(6) . ? C7 H19A 0.9700 . ? C7 H19B 0.9700 . ? C8 C9 1.380(6) . ? C9 C10 1.374(8) . ? C9 H21 0.9300 . ? C10 C11 1.383(8) . ? C10 H22 0.9300 . ? C11 C12 1.373(7) . ? C11 H23 0.9300 . ? C12 H24 0.9300 . ? C25 C26 1.470(8) . ? C25 H25 0.9800 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? 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 Co1 N3 157.48(12) . . ? O3 Co1 N2 76.49(12) . . ? N3 Co1 N2 113.75(14) . . ? O3 Co1 N1 100.14(12) . . ? N3 Co1 N1 97.63(13) . . ? N2 Co1 N1 100.27(13) . . ? O3 Co1 O4 81.23(11) . . ? N3 Co1 O4 77.63(12) . . ? N2 Co1 O4 97.43(12) . . ? N1 Co1 O4 162.08(12) . . ? O3 Co1 O2 75.62(10) . . ? N3 Co1 O2 95.16(12) . . ? N2 Co1 O2 150.99(12) . . ? N1 Co1 O2 77.04(11) . . ? O4 Co1 O2 86.11(10) . . ? F6 P1 F4 96.2(4) . . ? F6 P1 F2 97.6(5) . . ? F4 P1 F2 90.5(4) . . ? F6 P1 F1 175.1(3) . . ? F4 P1 F1 88.3(4) . . ? F2 P1 F1 84.4(4) . . ? F6 P1 F3 88.4(3) . . ? F4 P1 F3 174.0(4) . . ? F2 P1 F3 92.8(3) . . ? F1 P1 F3 87.0(3) . . ? F6 P1 F5 88.3(4) . . ? F4 P1 F5 92.1(3) . . ? F2 P1 F5 173.3(4) . . ? F1 P1 F5 89.5(4) . . ? F3 P1 F5 84.1(3) . . ? F9 P2 F10 93.2(3) . . ? F9 P2 F7 90.7(2) . . ? F10 P2 F7 89.2(2) . . ? F9 P2 F8 89.4(2) . . ? F10 P2 F8 90.8(2) . . ? F7 P2 F8 179.9(3) . . ? F9 P2 F11 174.9(3) . . ? F10 P2 F11 91.8(3) . . ? F7 P2 F11 90.5(2) . . ? F8 P2 F11 89.3(2) . . ? F9 P2 F12 88.2(3) . . ? F10 P2 F12 178.6(3) . . ? F7 P2 F12 90.5(2) . . ? F8 P2 F12 89.5(2) . . ? F11 P2 F12 86.9(3) . . ? C1 O1 C5 119.3(3) . . ? C7 O2 C3 114.7(3) . . ? C7 O2 Co1 106.6(2) . . ? C3 O2 Co1 110.1(2) . . ? C13 O3 C4 119.5(3) . . ? C13 O3 Co1 122.0(2) . . ? C4 O3 Co1 115.7(2) . . ? C19 O4 C6 115.6(3) . . ? C19 O4 Co1 112.8(2) . . ? C6 O4 Co1 123.3(3) . . ? C25 O5 C2 105.9(4) . . ? C1 O6 C25 108.6(4) . . ? C20 N3 C24 118.3(4) . . ? C20 N3 Co1 115.3(3) . . ? C24 N3 Co1 126.1(3) . . ? C14 N2 C18 118.3(4) . . ? C14 N2 Co1 116.9(3) . . ? C18 N2 Co1 124.7(3) . . ? C8 N1 C12 119.0(4) . . ? C8 N1 Co1 116.1(3) . . ? C12 N1 Co1 124.8(3) . . ? O1 C1 O6 110.5(4) . . ? O1 C1 C2 113.6(4) . . ? O6 C1 C2 104.0(4) . . ? O1 C1 H40 95(2) . . ? O6 C1 H40 116(3) . . ? C2 C1 H40 118(3) . . ? O5 C2 C3 107.6(4) . . ? O5 C2 C1 103.8(3) . . ? C3 C2 C1 111.8(3) . . ? O5 C2 H11 114(2) . . ? C3 C2 H11 113(2) . . ? C1 C2 H11 107(2) . . ? O2 C3 C4 108.3(3) . . ? O2 C3 C2 109.4(4) . . ? C4 C3 C2 109.1(3) . . ? O2 C3 H4 113(3) . . ? C4 C3 H4 106(3) . . ? C2 C3 H4 111(3) . . ? O3 C4 C3 103.1(3) . . ? O3 C4 C5 112.7(4) . . ? C3 C4 C5 112.1(4) . . ? O3 C4 H10 117(2) . . ? C3 C4 H10 104(2) . . ? C5 C4 H10 107(2) . . ? O1 C5 C6 103.5(4) . . ? O1 C5 C4 113.4(3) . . ? C6 C5 C4 113.7(4) . . ? O1 C5 H3 107(4) . . ? C6 C5 H3 101(4) . . ? C4 C5 H3 117(4) . . ? O4 C6 C5 112.0(3) . . ? O4 C6 H1A 109.2 . . ? C5 C6 H1A 109.2 . . ? O4 C6 H1B 109.2 . . ? C5 C6 H1B 109.2 . . ? H1A C6 H1B 107.9 . . ? O4 C19 C20 109.6(3) . . ? O4 C19 H7A 109.8 . . ? C20 C19 H7A 109.8 . . ? O4 C19 H7B 109.7 . . ? C20 C19 H7B 109.7 . . ? H7A C19 H7B 108.2 . . ? N3 C20 C21 121.8(4) . . ? N3 C20 C19 118.0(4) . . ? C21 C20 C19 120.2(4) . . ? C20 C21 C22 118.9(5) . . ? C20 C21 H9 120.5 . . ? C22 C21 H9 120.6 . . ? C23 C22 C21 119.2(4) . . ? C23 C22 H10 120.4 . . ? C21 C22 H10 120.4 . . ? C22 C23 C24 119.7(5) . . ? C22 C23 H11 120.2 . . ? C24 C23 H11 120.2 . . ? N3 C24 C23 122.0(5) . . ? N3 C24 H12 119.0 . . ? C23 C24 H12 119.0 . . ? O3 C13 C14 106.7(3) . . ? O3 C13 H13A 110.4 . . ? C14 C13 H13A 110.4 . . ? O3 C13 H13B 110.4 . . ? C14 C13 H13B 110.4 . . ? H13A C13 H13B 108.6 . . ? N2 C14 C15 122.0(4) . . ? N2 C14 C13 117.8(3) . . ? C15 C14 C13 120.2(4) . . ? C16 C15 C14 118.8(5) . . ? C16 C15 H15 120.6 . . ? C14 C15 H15 120.6 . . ? C17 C16 C15 120.3(5) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C16 C17 C18 118.7(5) . . ? C16 C17 H17 120.6 . . ? C18 C17 H17 120.6 . . ? N2 C18 C17 121.8(5) . . ? N2 C18 H18 119.1 . . ? C17 C18 H18 119.1 . . ? O2 C7 C8 111.8(4) . . ? O2 C7 H19A 109.3 . . ? C8 C7 H19A 109.3 . . ? O2 C7 H19B 109.3 . . ? C8 C7 H19B 109.3 . . ? H19A C7 H19B 107.9 . . ? N1 C8 C9 121.6(4) . . ? N1 C8 C7 116.2(4) . . ? C9 C8 C7 122.1(4) . . ? C10 C9 C8 119.1(5) . . ? C10 C9 H21 120.5 . . ? C8 C9 H21 120.5 . . ? C9 C10 C11 119.6(5) . . ? C9 C10 H22 120.2 . . ? C11 C10 H22 120.2 . . ? C12 C11 C10 118.7(5) . . ? C12 C11 H23 120.6 . . ? C10 C11 H23 120.6 . . ? N1 C12 C11 122.0(5) . . ? N1 C12 H24 119.0 . . ? C11 C12 H24 119.0 . . ? O5 C25 O6 105.5(4) . . ? O5 C25 C26 112.6(5) . . ? O6 C25 C26 111.8(5) . . ? O5 C25 H25 109.0 . . ? O6 C25 H25 109.0 . . ? C26 C25 H25 109.0 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.394 _refine_diff_density_min -0.284 _refine_diff_density_rms 0.050 _chemical_name_common ; (3,4,6-tri-O-(2-picolyl)-1,2-O-ethylidene-$($B&A!((B-D- galactopyranose) cobalt(ii) bis(hexafluorophosphate) ; data_2 _database_code_depnum_ccdc_archive 'CCDC 264231' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [3,4,6-tri-O-(2-picolyl)-galactal]cobalt(II)bis(hexafluorophosphate) ; _chemical_melting_point ? _chemical_formula_sum 'C24 H25 Co F12 N3 O4 P2' _chemical_formula_weight 768.34 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.233(5) _cell_length_b 10.440(5) _cell_length_c 15.360(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.166(5) _cell_angle_gamma 90.00 _cell_volume 1480.6(12) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _exptl_crystal_density_diffrn 1.723 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 774 _exptl_absorpt_coefficient_mu 0.801 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.72 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.20 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.81944 _exptl_absorpt_correction_T_max 0.90300 _exptl_absorpt_process_details 'Bruker AXS SADABS (1999)' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 12045 _diffrn_reflns_av_R_equivalents 0.0403 _diffrn_reflns_av_sigmaI/netI 0.0611 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 23.29 _reflns_number_total 4276 _reflns_number_gt 3229 _reflns_threshold_expression >2sigma(I) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0456P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.023(18) _refine_ls_number_reflns 4276 _refine_ls_number_parameters 423 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0580 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.0896 _refine_ls_wR_factor_gt 0.0842 _refine_ls_goodness_of_fit_ref 0.910 _refine_ls_restrained_S_all 0.910 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.95565(6) 0.19597(6) 0.30621(4) 0.0474(2) Uani 1 1 d . . . P1 P 0.74847(19) 0.2192(2) -0.08335(11) 0.0809(6) Uani 1 1 d . . . P2 P 0.46943(16) 0.51177(16) 0.41460(10) 0.0652(5) Uani 1 1 d . . . F1 F 0.6540(7) 0.1348(6) -0.1441(4) 0.196(3) Uani 1 1 d . . . F2 F 0.8300(8) 0.2644(6) -0.1648(4) 0.198(3) Uani 1 1 d . . . F3 F 0.8637(5) 0.1107(5) -0.0739(3) 0.1424(19) Uani 1 1 d . . . F4 F 0.6731(5) 0.1653(7) -0.0003(3) 0.169(2) Uani 1 1 d . . . F5 F 0.6426(8) 0.3274(7) -0.0949(4) 0.228(4) Uani 1 1 d . . . F6 F 0.8392(7) 0.3023(5) -0.0218(4) 0.169(2) Uani 1 1 d . . . F7 F 0.6320(3) 0.5347(4) 0.3847(2) 0.0919(11) Uani 1 1 d . . . F8 F 0.4939(5) 0.3634(4) 0.3948(4) 0.1403(18) Uani 1 1 d . . . F9 F 0.4155(4) 0.5224(7) 0.3223(3) 0.167(3) Uani 1 1 d . . . F10 F 0.4558(5) 0.6480(4) 0.4403(5) 0.205(3) Uani 1 1 d . . . F11 F 0.5301(4) 0.4811(6) 0.5086(3) 0.1353(19) Uani 1 1 d . . . F12 F 0.3083(4) 0.4833(5) 0.4447(2) 0.1104(14) Uani 1 1 d . . . O1 O 1.4140(4) 0.1587(4) 0.1745(3) 0.0769(12) Uani 1 1 d . . . O2 O 1.0211(3) 0.1339(3) 0.1846(2) 0.0556(9) Uani 1 1 d . . . O3 O 1.1205(3) 0.3366(3) 0.2766(2) 0.0535(9) Uani 1 1 d . . . O4 O 1.1489(3) 0.1043(3) 0.3499(2) 0.0520(9) Uani 1 1 d . . . N1 N 0.8171(4) 0.0457(4) 0.2807(3) 0.0453(11) Uani 1 1 d . . . N2 N 0.8347(5) 0.3439(4) 0.2487(3) 0.0498(12) Uani 1 1 d . . . N3 N 0.9497(4) 0.2313(4) 0.4369(3) 0.0497(11) Uani 1 1 d . . . C1 C 1.3514(7) 0.1300(7) 0.0980(5) 0.086(2) Uani 1 1 d . . . H42 H 1.4084 0.0889 0.0567 0.103 Uiso 1 1 calc R . . C2 C 1.2122(7) 0.1557(7) 0.0755(4) 0.083(2) Uani 1 1 d . . . H38 H 1.1785 0.1313 0.0209 0.100 Uiso 1 1 calc R . . C3 C 1.1128(6) 0.2219(6) 0.1360(3) 0.0653(16) Uani 1 1 d . . . H35 H 1.0529 0.2838 0.1042 0.078 Uiso 1 1 calc R . . C4 C 1.2047(6) 0.2907(6) 0.2041(4) 0.0623(16) Uani 1 1 d . . . H23 H 1.2539 0.3633 0.1766 0.075 Uiso 1 1 calc R . . C5 C 1.3169(5) 0.2016(7) 0.2429(3) 0.0610(13) Uani 1 1 d . . . H20 H 1.3745 0.2514 0.2845 0.073 Uiso 1 1 calc R . . C6 C 1.2665(6) 0.0810(6) 0.2892(4) 0.0591(16) Uani 1 1 d . . . C7 C 0.9169(6) 0.0626(6) 0.1358(3) 0.0724(18) Uani 1 1 d . . . H40A H 0.9651 -0.0019 0.1008 0.087 Uiso 1 1 calc R . . H40B H 0.8636 0.1191 0.0972 0.087 Uiso 1 1 calc R . . C8 C 0.8157(5) 0.0002(5) 0.1988(4) 0.0535(14) Uani 1 1 d . . . C9 C 0.7187(7) -0.0951(6) 0.1735(4) 0.0714(18) Uani 1 1 d . . . H44 H 0.7168 -0.1243 0.1163 0.086 Uiso 1 1 calc R . . C10 C 0.6266(6) -0.1448(6) 0.2339(5) 0.080(2) Uani 1 1 d . . . H39 H 0.5622 -0.2091 0.2180 0.095 Uiso 1 1 calc R . . C11 C 0.6282(6) -0.1011(5) 0.3170(4) 0.0647(16) Uani 1 1 d . . . H26 H 0.5656 -0.1347 0.3584 0.078 Uiso 1 1 calc R . . C12 C 0.7256(5) -0.0052(5) 0.3385(4) 0.0564(14) Uani 1 1 d . . . H102 H 0.7274 0.0251 0.3955 0.068 Uiso 1 1 calc R . . C13 C 1.0573(6) 0.4622(5) 0.2697(4) 0.0640(16) Uani 1 1 d . . . H17A H 1.1166 0.5154 0.2322 0.077 Uiso 1 1 calc R . . H17B H 1.0540 0.5018 0.3267 0.077 Uiso 1 1 calc R . . C14 C 0.9067(5) 0.4532(5) 0.2328(3) 0.0514(14) Uani 1 1 d . . . C15 C 0.8436(7) 0.5514(5) 0.1850(4) 0.0643(16) Uani 1 1 d . . . H100 H 0.8945 0.6267 0.1744 0.077 Uiso 1 1 calc R . . C16 C 0.7062(8) 0.5365(7) 0.1537(4) 0.075(2) Uani 1 1 d . . . H37 H 0.6630 0.6022 0.1220 0.090 Uiso 1 1 calc R . . C17 C 0.6317(6) 0.4254(6) 0.1687(4) 0.0653(16) Uani 1 1 d . . . H36 H 0.5385 0.4136 0.1472 0.078 Uiso 1 1 calc R . . C18 C 0.6991(6) 0.3331(6) 0.2163(3) 0.0595(15) Uani 1 1 d . . . H30 H 0.6487 0.2576 0.2271 0.071 Uiso 1 1 calc R . . C19 C 1.1975(5) 0.1549(5) 0.4316(3) 0.0624(16) Uani 1 1 d . . . H16A H 1.2658 0.2240 0.4217 0.075 Uiso 1 1 calc R . . H16B H 1.2464 0.0885 0.4646 0.075 Uiso 1 1 calc R . . C20 C 1.0700(5) 0.2042(5) 0.4823(3) 0.0462(11) Uani 1 1 d . . . C21 C 1.0802(7) 0.2227(6) 0.5708(4) 0.0697(17) Uani 1 1 d . . . H27 H 1.1647 0.2028 0.6010 0.084 Uiso 1 1 calc R . . C22 C 0.9605(9) 0.2719(6) 0.6136(4) 0.081(2) Uani 1 1 d . . . H46 H 0.9637 0.2848 0.6735 0.097 Uiso 1 1 calc R . . C23 C 0.8380(7) 0.3015(6) 0.5679(4) 0.0704(17) Uani 1 1 d . . . H31 H 0.7579 0.3359 0.5961 0.084 Uiso 1 1 calc R . . C24 C 0.8350(6) 0.2800(5) 0.4804(4) 0.0588(14) Uani 1 1 d . . . H22 H 0.7511 0.2995 0.4495 0.071 Uiso 1 1 calc R . . H101 H 1.221(6) 0.023(5) 0.239(4) 0.081(18) Uiso 1 1 d . . . H106 H 1.340(5) 0.045(4) 0.323(3) 0.044(13) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0398(3) 0.0509(4) 0.0516(4) 0.0021(4) -0.0028(3) -0.0018(4) P1 0.0785(11) 0.0966(15) 0.0675(11) -0.0044(11) -0.0138(9) 0.0194(12) P2 0.0552(10) 0.0760(12) 0.0643(11) -0.0079(9) 0.0017(8) -0.0117(8) F1 0.205(6) 0.191(6) 0.190(6) -0.027(4) -0.108(5) -0.025(5) F2 0.247(7) 0.240(8) 0.107(4) 0.071(4) 0.035(4) 0.031(6) F3 0.148(4) 0.174(4) 0.105(3) 0.021(3) 0.021(3) 0.090(4) F4 0.113(3) 0.252(8) 0.142(4) 0.041(5) 0.051(3) 0.027(4) F5 0.267(8) 0.217(7) 0.200(6) -0.064(5) -0.112(6) 0.160(6) F6 0.212(6) 0.153(5) 0.140(4) -0.023(4) -0.064(4) -0.048(4) F7 0.057(2) 0.128(3) 0.091(2) -0.008(2) 0.0112(18) -0.025(2) F8 0.112(3) 0.088(3) 0.221(5) -0.036(3) -0.024(3) -0.002(3) F9 0.082(3) 0.331(9) 0.088(3) 0.056(4) -0.014(2) -0.004(4) F10 0.114(4) 0.081(4) 0.421(10) -0.086(4) 0.084(5) -0.006(3) F11 0.109(4) 0.219(6) 0.078(3) 0.012(3) -0.006(2) -0.048(4) F12 0.065(2) 0.168(4) 0.098(3) -0.034(3) 0.0210(19) -0.031(3) O1 0.046(2) 0.094(4) 0.091(3) -0.012(2) 0.018(2) -0.002(2) O2 0.0438(19) 0.069(2) 0.054(2) -0.0021(18) 0.0035(17) -0.0095(18) O3 0.042(2) 0.045(2) 0.073(3) 0.0034(19) -0.0009(19) -0.0018(17) O4 0.046(2) 0.054(2) 0.056(2) -0.0054(18) -0.0080(18) 0.0066(18) N1 0.039(3) 0.047(3) 0.050(3) 0.002(2) -0.004(2) -0.002(2) N2 0.041(3) 0.058(3) 0.050(3) 0.001(2) 0.003(2) 0.000(2) N3 0.045(2) 0.050(3) 0.054(3) 0.003(2) -0.005(2) 0.003(2) C1 0.072(5) 0.108(5) 0.079(5) -0.037(4) 0.029(4) -0.018(4) C2 0.081(4) 0.114(6) 0.055(4) -0.017(4) 0.023(3) -0.021(4) C3 0.055(3) 0.081(5) 0.060(3) 0.010(3) 0.011(3) -0.013(3) C4 0.048(3) 0.063(4) 0.075(4) -0.004(3) 0.013(3) -0.009(3) C5 0.045(3) 0.073(4) 0.064(3) 0.001(4) 0.004(2) 0.008(4) C6 0.047(4) 0.068(4) 0.062(4) -0.008(3) -0.003(3) 0.019(3) C7 0.076(4) 0.094(5) 0.047(3) -0.011(3) -0.003(3) -0.016(4) C8 0.045(3) 0.061(4) 0.055(4) -0.011(3) -0.008(3) 0.002(3) C9 0.063(4) 0.078(5) 0.074(5) -0.021(4) -0.003(4) -0.011(4) C10 0.052(4) 0.068(5) 0.119(6) -0.016(4) -0.017(4) -0.008(3) C11 0.052(4) 0.053(4) 0.089(5) -0.006(3) 0.005(3) -0.014(3) C12 0.044(3) 0.058(4) 0.068(4) 0.002(3) 0.004(3) 0.003(3) C13 0.062(4) 0.041(3) 0.089(4) 0.007(3) -0.001(3) 0.005(3) C14 0.047(3) 0.043(3) 0.064(4) 0.006(3) 0.009(3) 0.008(3) C15 0.068(4) 0.057(4) 0.068(4) 0.020(3) 0.019(3) 0.014(3) C16 0.068(5) 0.082(5) 0.075(4) 0.028(4) 0.007(4) 0.032(4) C17 0.052(4) 0.081(5) 0.063(4) 0.005(3) -0.006(3) 0.013(4) C18 0.040(3) 0.075(4) 0.063(4) 0.004(3) 0.005(3) 0.007(3) C19 0.046(3) 0.073(4) 0.068(4) -0.013(3) -0.013(3) 0.003(3) C20 0.049(3) 0.039(3) 0.050(3) -0.004(3) -0.012(2) -0.003(3) C21 0.073(4) 0.079(5) 0.057(4) -0.004(3) -0.007(3) -0.010(4) C22 0.123(6) 0.063(4) 0.056(4) -0.018(3) 0.002(4) -0.004(4) C23 0.067(4) 0.072(4) 0.072(5) -0.013(4) 0.010(4) 0.002(3) C24 0.051(3) 0.060(4) 0.065(4) -0.004(3) 0.003(3) 0.009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N3 2.042(4) . ? Co1 N1 2.061(4) . ? Co1 O2 2.069(3) . ? Co1 N2 2.099(4) . ? Co1 O4 2.132(3) . ? Co1 O3 2.164(3) . ? P1 F5 1.504(6) . ? P1 F6 1.530(5) . ? P1 F2 1.536(6) . ? P1 F1 1.550(5) . ? P1 F4 1.560(5) . ? P1 F3 1.561(5) . ? P2 F10 1.482(5) . ? P2 F9 1.505(4) . ? P2 F11 1.580(5) . ? P2 F12 1.587(4) . ? P2 F7 1.589(3) . ? P2 F8 1.595(4) . ? O1 C1 1.342(7) . ? O1 C5 1.454(6) . ? O2 C7 1.428(6) . ? O2 C3 1.456(6) . ? O3 C13 1.439(6) . ? O3 C4 1.441(6) . ? O4 C19 1.433(6) . ? O4 C6 1.454(6) . ? N1 C12 1.338(6) . ? N1 C8 1.346(6) . ? N2 C14 1.343(6) . ? N2 C18 1.351(6) . ? N3 C20 1.341(5) . ? N3 C24 1.353(6) . ? C1 C2 1.357(8) . ? C2 C3 1.479(8) . ? C3 C4 1.524(7) . ? C4 C5 1.513(7) . ? C5 C6 1.520(8) . ? C7 C8 1.496(7) . ? C8 C9 1.393(7) . ? C9 C10 1.363(8) . ? C10 C11 1.355(8) . ? C11 C12 1.385(7) . ? C13 C14 1.502(7) . ? C14 C15 1.388(7) . ? C15 C16 1.364(8) . ? C16 C17 1.368(8) . ? C17 C18 1.360(7) . ? C19 C20 1.503(7) . ? C20 C21 1.376(6) . ? C21 C22 1.386(8) . ? C22 C23 1.365(8) . ? C23 C24 1.363(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 N3 Co1 N1 107.79(16) . . ? N3 Co1 O2 162.34(14) . . ? N1 Co1 O2 76.88(16) . . ? N3 Co1 N2 105.36(16) . . ? N1 Co1 N2 98.69(15) . . ? O2 Co1 N2 90.40(15) . . ? N3 Co1 O4 78.27(14) . . ? N1 Co1 O4 103.69(14) . . ? O2 Co1 O4 84.08(13) . . ? N2 Co1 O4 155.02(16) . . ? N3 Co1 O3 96.07(14) . . ? N1 Co1 O3 155.90(16) . . ? O2 Co1 O3 79.32(13) . . ? N2 Co1 O3 77.63(16) . . ? O4 Co1 O3 77.41(13) . . ? F5 P1 F6 90.1(4) . . ? F5 P1 F2 89.6(4) . . ? F6 P1 F2 93.5(4) . . ? F5 P1 F1 89.6(4) . . ? F6 P1 F1 178.7(4) . . ? F2 P1 F1 87.7(4) . . ? F5 P1 F4 94.4(4) . . ? F6 P1 F4 86.8(3) . . ? F2 P1 F4 176.0(3) . . ? F1 P1 F4 92.0(4) . . ? F5 P1 F3 177.3(4) . . ? F6 P1 F3 89.0(3) . . ? F2 P1 F3 87.9(3) . . ? F1 P1 F3 91.4(3) . . ? F4 P1 F3 88.1(3) . . ? F10 P2 F9 98.7(4) . . ? F10 P2 F11 88.9(4) . . ? F9 P2 F11 172.3(4) . . ? F10 P2 F12 91.3(3) . . ? F9 P2 F12 88.8(2) . . ? F11 P2 F12 91.5(2) . . ? F10 P2 F7 90.8(2) . . ? F9 P2 F7 91.5(2) . . ? F11 P2 F7 87.8(2) . . ? F12 P2 F7 177.9(3) . . ? F10 P2 F8 174.6(4) . . ? F9 P2 F8 86.5(3) . . ? F11 P2 F8 85.8(3) . . ? F12 P2 F8 90.4(3) . . ? F7 P2 F8 87.5(3) . . ? C1 O1 C5 115.8(4) . . ? C7 O2 C3 116.9(4) . . ? C7 O2 Co1 116.0(3) . . ? C3 O2 Co1 115.9(3) . . ? C13 O3 C4 117.7(4) . . ? C13 O3 Co1 110.4(3) . . ? C4 O3 Co1 108.6(3) . . ? C19 O4 C6 113.1(4) . . ? C19 O4 Co1 111.7(3) . . ? C6 O4 Co1 120.0(3) . . ? C12 N1 C8 118.5(5) . . ? C12 N1 Co1 124.7(4) . . ? C8 N1 Co1 116.8(3) . . ? C14 N2 C18 117.6(5) . . ? C14 N2 Co1 116.0(3) . . ? C18 N2 Co1 125.8(4) . . ? C20 N3 C24 118.1(4) . . ? C20 N3 Co1 116.7(3) . . ? C24 N3 Co1 125.3(3) . . ? O1 C1 C2 125.8(6) . . ? C1 C2 C3 121.4(6) . . ? O2 C3 C2 113.0(5) . . ? O2 C3 C4 105.6(4) . . ? C2 C3 C4 107.8(5) . . ? O3 C4 C5 105.7(4) . . ? O3 C4 C3 112.7(4) . . ? C5 C4 C3 111.0(5) . . ? O1 C5 C4 109.2(4) . . ? O1 C5 C6 105.9(5) . . ? C4 C5 C6 118.9(4) . . ? O4 C6 C5 113.1(4) . . ? O2 C7 C8 108.0(4) . . ? N1 C8 C9 121.1(5) . . ? N1 C8 C7 116.5(5) . . ? C9 C8 C7 122.2(5) . . ? C10 C9 C8 118.9(6) . . ? C11 C10 C9 120.5(6) . . ? C10 C11 C12 118.3(6) . . ? N1 C12 C11 122.6(5) . . ? O3 C13 C14 110.2(4) . . ? N2 C14 C15 121.1(5) . . ? N2 C14 C13 116.2(4) . . ? C15 C14 C13 122.7(5) . . ? C16 C15 C14 119.4(6) . . ? C15 C16 C17 120.3(6) . . ? C18 C17 C16 117.5(6) . . ? N2 C18 C17 124.1(6) . . ? O4 C19 C20 109.7(4) . . ? N3 C20 C21 122.6(5) . . ? N3 C20 C19 116.9(4) . . ? C21 C20 C19 120.5(5) . . ? C20 C21 C22 117.9(6) . . ? C23 C22 C21 120.1(6) . . ? C24 C23 C22 118.9(6) . . ? N3 C24 C23 122.4(5) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.29 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.351 _refine_diff_density_min -0.268 _refine_diff_density_rms 0.047 _chemical_name_common ;(3,4,6-tri-O-(2-picolyl)- galactal)cobalt(ii)bis(hexafluorophosphate) ;