Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Clotilde Policar' _publ_contact_author_address ; Institut de Chimie Moleculaire et des Materiaux d'Orsay ECBB, ICMMO Universite PARIS XI Bat. 420 ORSAY F-91405 FRANCE ; _publ_contact_author_email CPOLICAR@ICMO.U-PSUD.FR _publ_section_title ; Glycoligands and Co(II) glycocomplexes. Investigation of the variation of the sugar-scaffold on the structure and chirality measured by circular dichroism. ; loop_ _publ_author_name 'Clotilde Policar' 'Federico Cisnetti' 'Michel Desmadril' 'Regis Guillot' 'Giorgio Pelosi' data_325GuillotICMMO1 _database_code_depnum_ccdc_archive 'CCDC 614621' _audit_creation_method SHELXL-97 _chemical_name_systematic '[3,5,6-tri-O-(2-picolyl)-1,2-isopropylidene-\a-D-glucofuranose] CoII (PF6)2' _chemical_name_common ;(3,5,6-tri-O-(2-picolyl)-1,2-isopropylidene-alpha-D- glucofuranose) CoII (PF6)2 ; _chemical_melting_point ? _chemical_formula_moiety 'C27 H31 Co N3 O6, 2(F6 P), H2 O' _chemical_formula_sum 'C27 H33 Co F12 N3 O7 P2' _chemical_formula_weight 860.42 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 'P 21' _symmetry_int_tables_number 4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.132(5) _cell_length_b 19.071(5) _cell_length_c 9.973(5) _cell_angle_alpha 90. _cell_angle_beta 104.076(5) _cell_angle_gamma 90. _cell_volume 1684.7(13) _cell_formula_units_Z 2 _cell_measurement_temperature 100(1) _cell_measurement_reflns_used 9440 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 28.67 _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_max 0.220 _exptl_crystal_size_mid 0.130 _exptl_crystal_size_min 0.090 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.692 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 870 _exptl_absorpt_coefficient_mu 0.720 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.894 _exptl_absorpt_correction_T_max 0.941 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(1) _diffrn_radiation_wavelength 0.71069 _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 19463 _diffrn_reflns_av_R_equivalents 0.0222 _diffrn_reflns_av_sigmaI/netI 0.0433 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 29.85 _reflns_number_total 7818 _reflns_number_gt 6875 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0372P)^2^+0.8081P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.005(10) _refine_ls_number_reflns 7818 _refine_ls_number_parameters 469 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0441 _refine_ls_R_factor_gt 0.0349 _refine_ls_wR_factor_ref 0.0844 _refine_ls_wR_factor_gt 0.0812 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.017 _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 0.16057(4) 0.278326(17) 0.75204(3) 0.01791(8) Uani 1 1 d . . . O1 O 0.7678(3) 0.41954(16) 0.9028(3) 0.0511(7) Uani 1 1 d . . . O2 O 0.5974(2) 0.46968(12) 1.0076(2) 0.0362(5) Uani 1 1 d . . . O3 O 0.2832(2) 0.37546(9) 0.78683(18) 0.0185(4) Uani 1 1 d . . . O4 O 0.6038(2) 0.32518(11) 0.8938(2) 0.0283(4) Uani 1 1 d . . . O5 O 0.3571(2) 0.23115(10) 0.8443(2) 0.0244(4) Uani 1 1 d . . . O6 O 0.1755(2) 0.29541(9) 0.97154(18) 0.0194(4) Uani 1 1 d . . . N3 N -0.0010(2) 0.34693(11) 0.6527(2) 0.0190(4) Uani 1 1 d . . . N5 N 0.2136(3) 0.22060(13) 0.5915(2) 0.0241(5) Uani 1 1 d . . . N6 N 0.0069(3) 0.20418(11) 0.7995(2) 0.0213(5) Uani 1 1 d . . . C1 C 0.6259(3) 0.39243(19) 0.8393(3) 0.0350(8) Uani 1 1 d . . . H1 H 0.6107 0.3907 0.7387 0.042 Uiso 1 1 calc R . . C2 C 0.5129(3) 0.44066(16) 0.8802(3) 0.0299(7) Uani 1 1 d . . . H2 H 0.4715 0.4761 0.8101 0.036 Uiso 1 1 calc R . . C3 C 0.3938(3) 0.39236(13) 0.9128(3) 0.0201(5) Uani 1 1 d . . . H3 H 0.3462 0.4134 0.9812 0.024 Uiso 1 1 calc R . . C4 C 0.4927(3) 0.32979(15) 0.9735(3) 0.0208(5) Uani 1 1 d . . . H4 H 0.5459 0.3423 1.0681 0.025 Uiso 1 1 calc R . . C5 C 0.4262(3) 0.25760(14) 0.9790(3) 0.0223(6) Uani 1 1 d . . . H5 H 0.5065 0.2254 1.0247 0.027 Uiso 1 1 calc R . . C6 C 0.3006(3) 0.25565(14) 1.0544(3) 0.0213(5) Uani 1 1 d . . . H6A H 0.2701 0.2076 1.0648 0.026 Uiso 1 1 calc R . . H6B H 0.3344 0.2764 1.1455 0.026 Uiso 1 1 calc R . . C10 C 0.7538(4) 0.4681(2) 1.0069(4) 0.0464(10) Uani 1 1 d . . . C11 C 0.8434(4) 0.4444(3) 1.1450(4) 0.0666(14) Uani 1 1 d . . . H11A H 0.9487 0.4439 1.1458 0.100 Uiso 1 1 calc R . . H11B H 0.8121 0.3980 1.1633 0.100 Uiso 1 1 calc R . . H11C H 0.8270 0.4759 1.2150 0.100 Uiso 1 1 calc R . . C12 C 0.8009(5) 0.5406(3) 0.9697(4) 0.0709(15) Uani 1 1 d . . . H12A H 0.9060 0.5401 0.9694 0.106 Uiso 1 1 calc R . . H12B H 0.7846 0.5740 1.0365 0.106 Uiso 1 1 calc R . . H12C H 0.7420 0.5535 0.8796 0.106 Uiso 1 1 calc R . . C30 C 0.1938(3) 0.43573(14) 0.7302(3) 0.0228(6) Uani 1 1 d . . . H30A H 0.2430 0.4605 0.6684 0.027 Uiso 1 1 calc R . . H30B H 0.1869 0.4674 0.8046 0.027 Uiso 1 1 calc R . . C31 C 0.0378(3) 0.41460(14) 0.6527(3) 0.0192(5) Uani 1 1 d . . . C32 C -0.0626(3) 0.46534(15) 0.5839(3) 0.0254(6) Uani 1 1 d . . . H32 H -0.0341 0.5122 0.5857 0.030 Uiso 1 1 calc R . . C33 C -0.2048(3) 0.44472(17) 0.5132(3) 0.0302(7) Uani 1 1 d . . . H33 H -0.2739 0.4777 0.4671 0.036 Uiso 1 1 calc R . . C34 C -0.2443(3) 0.37483(17) 0.5110(3) 0.0298(7) Uani 1 1 d . . . H34 H -0.3394 0.3600 0.4624 0.036 Uiso 1 1 calc R . . C35 C -0.1406(3) 0.32780(16) 0.5818(3) 0.0244(6) Uani 1 1 d . . . H35 H -0.1675 0.2807 0.5810 0.029 Uiso 1 1 calc R . . C50 C 0.4446(4) 0.1959(2) 0.7653(4) 0.0462(10) Uani 1 1 d . . . H50A H 0.4806 0.1514 0.8078 0.055 Uiso 1 1 calc R . . H50B H 0.5310 0.2242 0.7591 0.055 Uiso 1 1 calc R . . C51 C 0.3425(3) 0.18439(18) 0.6239(3) 0.0332(7) Uani 1 1 d . . . C52 C 0.3857(4) 0.1388(2) 0.5324(4) 0.0440(9) Uani 1 1 d . . . H52 H 0.4766 0.1146 0.5576 0.053 Uiso 1 1 calc R . . C53 C 0.2907(4) 0.1301(2) 0.4030(3) 0.0403(8) Uani 1 1 d . . . H53 H 0.3161 0.0993 0.3399 0.048 Uiso 1 1 calc R . . C54 C 0.1586(4) 0.16732(17) 0.3684(3) 0.0320(7) Uani 1 1 d . . . H54 H 0.0931 0.1622 0.2816 0.038 Uiso 1 1 calc R . . C55 C 0.1244(3) 0.21233(15) 0.4638(3) 0.0249(6) Uani 1 1 d . . . H55 H 0.0356 0.2382 0.4390 0.030 Uiso 1 1 calc R . . C60 C 0.0329(3) 0.27855(17) 0.9995(3) 0.0233(5) Uani 1 1 d . . . H60A H -0.0358 0.3178 0.9738 0.028 Uiso 1 1 calc R . . H60B H 0.0464 0.2700 1.0976 0.028 Uiso 1 1 calc R . . C61 C -0.0334(3) 0.21415(14) 0.9189(3) 0.0219(6) Uani 1 1 d . . . C62 C -0.1304(3) 0.17004(15) 0.9634(3) 0.0254(6) Uani 1 1 d . . . H62 H -0.1554 0.1782 1.0470 0.030 Uiso 1 1 calc R . . C63 C -0.1909(3) 0.11293(16) 0.8816(3) 0.0301(7) Uani 1 1 d . . . H63 H -0.2579 0.0826 0.9090 0.036 Uiso 1 1 calc R . . C64 C -0.1495(3) 0.10230(15) 0.7595(3) 0.0287(6) Uani 1 1 d . . . H64 H -0.1871 0.0643 0.7032 0.034 Uiso 1 1 calc R . . C65 C -0.0514(3) 0.14896(14) 0.7220(3) 0.0255(6) Uani 1 1 d . . . H65 H -0.0244 0.1417 0.6389 0.031 Uiso 1 1 calc R . . P1 P 0.30374(9) 0.40683(4) 0.35008(8) 0.03059(18) Uani 1 1 d . . . F1 F 0.4140(2) 0.47202(13) 0.3959(3) 0.0622(7) Uani 1 1 d . . . F2 F 0.4342(2) 0.36849(11) 0.2942(2) 0.0453(5) Uani 1 1 d . . . F3 F 0.3647(3) 0.37325(16) 0.4978(2) 0.0783(9) Uani 1 1 d . . . F4 F 0.1936(2) 0.34173(11) 0.3021(2) 0.0491(5) Uani 1 1 d . . . F5 F 0.1754(2) 0.44745(11) 0.40131(19) 0.0386(4) Uani 1 1 d . . . F6 F 0.2448(2) 0.44026(10) 0.20100(18) 0.0347(4) Uani 1 1 d . . . P2 P 0.31605(9) 0.64173(4) 0.69781(8) 0.02451(15) Uani 1 1 d . . . F7 F 0.39491(19) 0.57512(8) 0.64852(17) 0.0284(4) Uani 1 1 d . . . F8 F 0.3441(3) 0.60910(13) 0.8487(2) 0.0642(8) Uani 1 1 d . . . F9 F 0.4738(2) 0.68066(12) 0.7405(2) 0.0504(6) Uani 1 1 d . . . F10 F 0.2365(2) 0.70838(10) 0.7488(2) 0.0427(5) Uani 1 1 d . . . F11 F 0.1585(2) 0.60324(12) 0.6552(4) 0.0751(9) Uani 1 1 d . . . F12 F 0.2895(3) 0.67473(11) 0.5481(2) 0.0535(6) Uani 1 1 d . . . O1W O 0.5455(6) 0.5378(3) 0.2216(6) 0.1315(18) Uani 1 1 d U . . 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 0.01420(17) 0.01774(15) 0.02024(15) 0.00036(15) 0.00118(12) 0.00069(15) O1 0.0194(13) 0.0717(19) 0.0578(17) 0.0145(15) 0.0012(11) -0.0108(12) O2 0.0269(12) 0.0352(12) 0.0365(12) 0.0087(9) -0.0115(9) -0.0132(9) O3 0.0128(9) 0.0203(9) 0.0191(9) 0.0025(7) -0.0024(7) 0.0004(7) O4 0.0172(10) 0.0412(12) 0.0266(10) 0.0068(9) 0.0054(8) 0.0052(9) O5 0.0192(10) 0.0262(10) 0.0244(10) -0.0046(8) -0.0014(8) 0.0064(8) O6 0.0162(10) 0.0197(10) 0.0217(9) 0.0012(7) 0.0036(7) 0.0006(7) N3 0.0147(11) 0.0221(11) 0.0192(10) -0.0016(8) 0.0020(8) 0.0018(9) N5 0.0184(12) 0.0285(12) 0.0245(12) -0.0036(10) 0.0033(9) -0.0055(10) N6 0.0203(12) 0.0178(10) 0.0240(11) 0.0022(8) 0.0020(9) 0.0012(9) C1 0.0165(16) 0.054(2) 0.0320(16) 0.0155(14) 0.0002(12) -0.0060(14) C2 0.0206(15) 0.0350(16) 0.0272(15) 0.0142(12) -0.0074(12) -0.0065(12) C3 0.0158(14) 0.0217(13) 0.0195(12) 0.0036(10) -0.0021(10) -0.0053(10) C4 0.0141(13) 0.0294(13) 0.0166(12) 0.0011(10) -0.0007(10) 0.0016(11) C5 0.0188(14) 0.0231(13) 0.0216(13) 0.0021(10) -0.0014(10) 0.0048(10) C6 0.0207(14) 0.0199(12) 0.0210(13) 0.0035(9) 0.0009(10) -0.0010(10) C10 0.0235(18) 0.068(2) 0.0381(19) 0.0244(18) -0.0111(14) -0.0230(17) C11 0.030(2) 0.107(4) 0.052(2) 0.039(2) -0.0121(18) -0.013(2) C12 0.070(3) 0.081(3) 0.048(2) 0.022(2) -0.012(2) -0.052(3) C30 0.0194(15) 0.0178(12) 0.0265(14) 0.0009(10) -0.0033(11) 0.0010(10) C31 0.0170(13) 0.0210(12) 0.0184(12) -0.0010(10) 0.0021(10) 0.0020(10) C32 0.0220(15) 0.0258(14) 0.0265(14) 0.0018(11) 0.0021(11) 0.0047(11) C33 0.0231(16) 0.0379(16) 0.0265(15) 0.0042(12) -0.0001(12) 0.0116(13) C34 0.0170(15) 0.0422(18) 0.0263(15) 0.0017(13) -0.0024(12) 0.0000(13) C35 0.0153(14) 0.0310(14) 0.0241(13) -0.0008(11) -0.0005(10) -0.0020(11) C50 0.0214(17) 0.070(3) 0.0411(19) -0.0279(18) -0.0045(14) 0.0160(16) C51 0.0210(16) 0.0428(18) 0.0351(16) -0.0134(14) 0.0055(13) 0.0024(13) C52 0.0230(18) 0.059(2) 0.050(2) -0.0254(18) 0.0086(15) 0.0021(16) C53 0.034(2) 0.056(2) 0.0372(18) -0.0197(16) 0.0214(15) -0.0116(16) C54 0.0325(18) 0.0384(17) 0.0268(15) -0.0074(12) 0.0106(13) -0.0134(14) C55 0.0234(15) 0.0290(14) 0.0217(13) 0.0021(11) 0.0040(11) -0.0057(12) C60 0.0221(13) 0.0246(12) 0.0247(12) 0.0018(13) 0.0084(10) 0.0018(14) C61 0.0152(14) 0.0201(12) 0.0270(14) 0.0038(10) -0.0011(11) 0.0004(10) C62 0.0179(15) 0.0310(15) 0.0272(14) 0.0067(12) 0.0054(11) 0.0027(12) C63 0.0169(15) 0.0269(14) 0.0440(17) 0.0110(12) 0.0025(13) -0.0031(11) C64 0.0248(16) 0.0200(13) 0.0356(16) 0.0006(11) -0.0040(12) -0.0030(11) C65 0.0234(15) 0.0226(13) 0.0269(13) -0.0004(11) -0.0006(11) -0.0007(11) P1 0.0246(4) 0.0360(4) 0.0267(4) -0.0080(3) -0.0024(3) 0.0114(3) F1 0.0325(12) 0.0671(15) 0.0832(17) -0.0540(14) 0.0068(11) -0.0078(11) F2 0.0261(10) 0.0572(13) 0.0455(11) -0.0279(10) -0.0050(8) 0.0164(9) F3 0.094(2) 0.096(2) 0.0337(12) 0.0082(12) -0.0067(12) 0.0559(17) F4 0.0539(13) 0.0343(11) 0.0598(13) 0.0004(9) 0.0152(10) -0.0059(10) F5 0.0345(11) 0.0523(12) 0.0308(9) -0.0004(8) 0.0114(8) 0.0138(9) F6 0.0338(10) 0.0419(10) 0.0290(9) -0.0004(7) 0.0091(8) 0.0055(8) P2 0.0223(4) 0.0222(3) 0.0273(4) 0.0009(3) 0.0028(3) 0.0016(3) F7 0.0285(10) 0.0243(8) 0.0335(9) 0.0011(7) 0.0100(7) 0.0018(7) F8 0.0910(19) 0.0700(15) 0.0471(13) 0.0304(11) 0.0467(13) 0.0480(14) F9 0.0351(12) 0.0610(13) 0.0542(13) -0.0347(11) 0.0090(9) -0.0176(10) F10 0.0525(13) 0.0306(9) 0.0483(12) 0.0002(8) 0.0185(10) 0.0132(9) F11 0.0214(12) 0.0424(12) 0.160(3) -0.0237(15) 0.0200(14) -0.0062(9) F12 0.0901(18) 0.0369(11) 0.0276(10) 0.0023(9) 0.0030(10) 0.0217(11) O1W 0.117(4) 0.114(4) 0.158(5) -0.018(4) 0.024(3) 0.015(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co O5 2.019(2) . ? Co N3 2.039(2) . ? Co N5 2.095(2) . ? Co N6 2.125(2) . ? Co O3 2.1488(19) . ? Co O6 2.184(2) . ? O1 C1 1.396(4) . ? O1 C10 1.420(5) . ? O2 C2 1.428(4) . ? O2 C10 1.430(4) . ? O3 C30 1.443(3) . ? O3 C3 1.444(3) . ? O4 C1 1.426(4) . ? O4 C4 1.435(3) . ? O5 C50 1.420(4) . ? O5 C5 1.430(3) . ? O6 C60 1.432(3) . ? O6 C6 1.451(3) . ? N3 C31 1.338(3) . ? N3 C35 1.349(4) . ? N5 C51 1.335(4) . ? N5 C55 1.344(4) . ? N6 C65 1.338(4) . ? N6 C61 1.343(4) . ? C1 C2 1.511(5) . ? C1 H1 0.9800 . ? C2 C3 1.520(4) . ? C2 H2 0.9800 . ? C3 C4 1.530(4) . ? C3 H3 0.9800 . ? C4 C5 1.511(4) . ? C4 H4 0.9800 . ? C5 C6 1.517(4) . ? C5 H5 0.9800 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C10 C11 1.492(5) . ? C10 C12 1.521(5) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C30 C31 1.501(4) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.394(4) . ? C32 C33 1.375(4) . ? C32 H32 0.9300 . ? C33 C34 1.379(4) . ? C33 H33 0.9300 . ? C34 C35 1.369(4) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C50 C51 1.505(4) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 C52 1.386(4) . ? C52 C53 1.378(5) . ? C52 H52 0.9300 . ? C53 C54 1.369(5) . ? C53 H53 0.9300 . ? C54 C55 1.373(4) . ? C54 H54 0.9300 . ? C55 H55 0.9300 . ? C60 C61 1.512(4) . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? C61 C62 1.371(4) . ? C62 C63 1.392(4) . ? C62 H62 0.9300 . ? C63 C64 1.376(5) . ? C63 H63 0.9300 . ? C64 C65 1.377(4) . ? C64 H64 0.9300 . ? C65 H65 0.9300 . ? P1 F3 1.579(2) . ? P1 F6 1.587(2) . ? P1 F5 1.590(2) . ? P1 F1 1.595(2) . ? P1 F4 1.596(2) . ? P1 F2 1.609(2) . ? P2 F11 1.579(2) . ? P2 F9 1.584(2) . ? P2 F12 1.584(2) . ? P2 F8 1.591(2) . ? P2 F7 1.5956(18) . ? P2 F10 1.607(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Co N3 164.87(9) . . ? O5 Co N5 76.63(9) . . ? N3 Co N5 103.89(9) . . ? O5 Co N6 99.45(9) . . ? N3 Co N6 95.53(9) . . ? N5 Co N6 96.22(9) . . ? O5 Co O3 86.55(8) . . ? N3 Co O3 79.18(8) . . ? N5 Co O3 111.60(8) . . ? N6 Co O3 152.16(8) . . ? O5 Co O6 77.18(7) . . ? N3 Co O6 104.64(8) . . ? N5 Co O6 151.03(8) . . ? N6 Co O6 76.10(8) . . ? O3 Co O6 78.85(7) . . ? C1 O1 C10 109.5(3) . . ? C2 O2 C10 108.2(3) . . ? C30 O3 C3 111.85(19) . . ? C30 O3 Co 113.60(14) . . ? C3 O3 Co 124.04(14) . . ? C1 O4 C4 109.9(2) . . ? C50 O5 C5 120.6(2) . . ? C50 O5 Co 121.08(19) . . ? C5 O5 Co 114.26(15) . . ? C60 O6 C6 113.52(19) . . ? C60 O6 Co 108.88(14) . . ? C6 O6 Co 109.95(14) . . ? C31 N3 C35 118.5(2) . . ? C31 N3 Co 117.29(18) . . ? C35 N3 Co 124.11(19) . . ? C51 N5 C55 117.7(3) . . ? C51 N5 Co 116.15(19) . . ? C55 N5 Co 125.9(2) . . ? C65 N6 C61 117.9(2) . . ? C65 N6 Co 125.9(2) . . ? C61 N6 Co 116.20(18) . . ? O1 C1 O4 111.2(2) . . ? O1 C1 C2 105.8(3) . . ? O4 C1 C2 106.0(2) . . ? O1 C1 H1 111.2 . . ? O4 C1 H1 111.2 . . ? C2 C1 H1 111.2 . . ? O2 C2 C1 102.6(2) . . ? O2 C2 C3 107.8(2) . . ? C1 C2 C3 105.1(2) . . ? O2 C2 H2 113.5 . . ? C1 C2 H2 113.5 . . ? C3 C2 H2 113.5 . . ? O3 C3 C2 109.6(2) . . ? O3 C3 C4 113.0(2) . . ? C2 C3 C4 99.9(2) . . ? O3 C3 H3 111.3 . . ? C2 C3 H3 111.3 . . ? C4 C3 H3 111.3 . . ? O4 C4 C5 108.0(2) . . ? O4 C4 C3 104.9(2) . . ? C5 C4 C3 121.4(2) . . ? O4 C4 H4 107.3 . . ? C5 C4 H4 107.3 . . ? C3 C4 H4 107.3 . . ? O5 C5 C4 112.1(2) . . ? O5 C5 C6 104.1(2) . . ? C4 C5 C6 113.5(2) . . ? O5 C5 H5 109.0 . . ? C4 C5 H5 109.0 . . ? C6 C5 H5 109.0 . . ? O6 C6 C5 106.9(2) . . ? O6 C6 H6A 110.3 . . ? C5 C6 H6A 110.3 . . ? O6 C6 H6B 110.3 . . ? C5 C6 H6B 110.3 . . ? H6A C6 H6B 108.6 . . ? O1 C10 O2 106.6(3) . . ? O1 C10 C11 110.5(4) . . ? O2 C10 C11 109.0(3) . . ? O1 C10 C12 109.5(3) . . ? O2 C10 C12 108.9(4) . . ? C11 C10 C12 112.1(3) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O3 C30 C31 111.3(2) . . ? O3 C30 H30A 109.4 . . ? C31 C30 H30A 109.4 . . ? O3 C30 H30B 109.4 . . ? C31 C30 H30B 109.4 . . ? H30A C30 H30B 108.0 . . ? N3 C31 C32 121.8(2) . . ? N3 C31 C30 118.5(2) . . ? C32 C31 C30 119.7(2) . . ? C33 C32 C31 118.7(3) . . ? C33 C32 H32 120.7 . . ? C31 C32 H32 120.7 . . ? C32 C33 C34 119.7(3) . . ? C32 C33 H33 120.2 . . ? C34 C33 H33 120.2 . . ? C35 C34 C33 118.7(3) . . ? C35 C34 H34 120.7 . . ? C33 C34 H34 120.7 . . ? N3 C35 C34 122.7(3) . . ? N3 C35 H35 118.7 . . ? C34 C35 H35 118.7 . . ? O5 C50 C51 106.6(2) . . ? O5 C50 H50A 110.4 . . ? C51 C50 H50A 110.4 . . ? O5 C50 H50B 110.4 . . ? C51 C50 H50B 110.4 . . ? H50A C50 H50B 108.6 . . ? N5 C51 C52 122.7(3) . . ? N5 C51 C50 117.4(3) . . ? C52 C51 C50 119.9(3) . . ? C53 C52 C51 118.5(3) . . ? C53 C52 H52 120.7 . . ? C51 C52 H52 120.7 . . ? C54 C53 C52 119.3(3) . . ? C54 C53 H53 120.4 . . ? C52 C53 H53 120.4 . . ? C53 C54 C55 119.0(3) . . ? C53 C54 H54 120.5 . . ? C55 C54 H54 120.5 . . ? N5 C55 C54 122.8(3) . . ? N5 C55 H55 118.6 . . ? C54 C55 H55 118.6 . . ? O6 C60 C61 110.1(2) . . ? O6 C60 H60A 109.6 . . ? C61 C60 H60A 109.6 . . ? O6 C60 H60B 109.6 . . ? C61 C60 H60B 109.6 . . ? H60A C60 H60B 108.1 . . ? N6 C61 C62 122.6(3) . . ? N6 C61 C60 115.2(2) . . ? C62 C61 C60 122.2(3) . . ? C61 C62 C63 119.1(3) . . ? C61 C62 H62 120.4 . . ? C63 C62 H62 120.4 . . ? C64 C63 C62 118.6(3) . . ? C64 C63 H63 120.7 . . ? C62 C63 H63 120.7 . . ? C63 C64 C65 118.8(3) . . ? C63 C64 H64 120.6 . . ? C65 C64 H64 120.6 . . ? N6 C65 C64 123.1(3) . . ? N6 C65 H65 118.5 . . ? C64 C65 H65 118.5 . . ? F3 P1 F6 179.11(14) . . ? F3 P1 F5 91.03(13) . . ? F6 P1 F5 89.82(10) . . ? F3 P1 F1 89.67(17) . . ? F6 P1 F1 90.09(14) . . ? F5 P1 F1 89.53(12) . . ? F3 P1 F4 91.02(16) . . ? F6 P1 F4 89.22(11) . . ? F5 P1 F4 90.87(12) . . ? F1 P1 F4 179.20(14) . . ? F3 P1 F2 90.94(13) . . ? F6 P1 F2 88.20(11) . . ? F5 P1 F2 177.59(13) . . ? F1 P1 F2 89.10(12) . . ? F4 P1 F2 90.48(12) . . ? F11 P2 F9 179.74(13) . . ? F11 P2 F12 90.60(16) . . ? F9 P2 F12 89.31(14) . . ? F11 P2 F8 89.97(17) . . ? F9 P2 F8 90.11(15) . . ? F12 P2 F8 179.41(17) . . ? F11 P2 F7 89.83(12) . . ? F9 P2 F7 90.41(11) . . ? F12 P2 F7 90.17(10) . . ? F8 P2 F7 89.95(11) . . ? F11 P2 F10 90.02(12) . . ? F9 P2 F10 89.73(12) . . ? F12 P2 F10 90.37(11) . . ? F8 P2 F10 89.51(11) . . ? F7 P2 F10 179.44(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 Co O3 C30 176.77(17) . . . . ? N3 Co O3 C30 1.83(17) . . . . ? N5 Co O3 C30 102.62(18) . . . . ? N6 Co O3 C30 -79.4(2) . . . . ? O6 Co O3 C30 -105.62(17) . . . . ? O5 Co O3 C3 -41.50(19) . . . . ? N3 Co O3 C3 143.6(2) . . . . ? N5 Co O3 C3 -115.7(2) . . . . ? N6 Co O3 C3 62.3(3) . . . . ? O6 Co O3 C3 36.11(19) . . . . ? N3 Co O5 C50 -83.3(4) . . . . ? N5 Co O5 C50 10.5(3) . . . . ? N6 Co O5 C50 104.7(3) . . . . ? O3 Co O5 C50 -102.7(3) . . . . ? O6 Co O5 C50 178.0(3) . . . . ? N3 Co O5 C5 74.2(4) . . . . ? N5 Co O5 C5 167.98(19) . . . . ? N6 Co O5 C5 -97.81(18) . . . . ? O3 Co O5 C5 54.81(18) . . . . ? O6 Co O5 C5 -24.53(17) . . . . ? O5 Co O6 C60 -133.27(18) . . . . ? N3 Co O6 C60 62.19(18) . . . . ? N5 Co O6 C60 -107.5(2) . . . . ? N6 Co O6 C60 -29.99(17) . . . . ? O3 Co O6 C60 137.76(17) . . . . ? O5 Co O6 C6 -8.33(15) . . . . ? N3 Co O6 C6 -172.87(15) . . . . ? N5 Co O6 C6 17.5(2) . . . . ? N6 Co O6 C6 94.96(16) . . . . ? O3 Co O6 C6 -97.30(15) . . . . ? O5 Co N3 C31 -19.3(4) . . . . ? N5 Co N3 C31 -109.38(19) . . . . ? N6 Co N3 C31 152.80(19) . . . . ? O3 Co N3 C31 0.43(18) . . . . ? O6 Co N3 C31 75.75(19) . . . . ? O5 Co N3 C35 157.2(3) . . . . ? N5 Co N3 C35 67.1(2) . . . . ? N6 Co N3 C35 -30.7(2) . . . . ? O3 Co N3 C35 176.9(2) . . . . ? O6 Co N3 C35 -107.7(2) . . . . ? O5 Co N5 C51 -1.1(2) . . . . ? N3 Co N5 C51 163.3(2) . . . . ? N6 Co N5 C51 -99.4(2) . . . . ? O3 Co N5 C51 79.7(2) . . . . ? O6 Co N5 C51 -26.9(3) . . . . ? O5 Co N5 C55 173.0(2) . . . . ? N3 Co N5 C55 -22.5(2) . . . . ? N6 Co N5 C55 74.7(2) . . . . ? O3 Co N5 C55 -106.2(2) . . . . ? O6 Co N5 C55 147.2(2) . . . . ? O5 Co N6 C65 -90.1(2) . . . . ? N3 Co N6 C65 92.0(2) . . . . ? N5 Co N6 C65 -12.6(2) . . . . ? O3 Co N6 C65 169.30(19) . . . . ? O6 Co N6 C65 -164.2(2) . . . . ? O5 Co N6 C61 89.47(19) . . . . ? N3 Co N6 C61 -88.44(19) . . . . ? N5 Co N6 C61 166.90(19) . . . . ? O3 Co N6 C61 -11.2(3) . . . . ? O6 Co N6 C61 15.30(18) . . . . ? C10 O1 C1 O4 -99.2(3) . . . . ? C10 O1 C1 C2 15.4(3) . . . . ? C4 O4 C1 O1 110.5(3) . . . . ? C4 O4 C1 C2 -4.1(3) . . . . ? C10 O2 C2 C1 26.3(3) . . . . ? C10 O2 C2 C3 136.9(3) . . . . ? O1 C1 C2 O2 -25.4(3) . . . . ? O4 C1 C2 O2 92.8(3) . . . . ? O1 C1 C2 C3 -138.0(2) . . . . ? O4 C1 C2 C3 -19.8(3) . . . . ? C30 O3 C3 C2 -68.2(3) . . . . ? Co O3 C3 C2 149.48(18) . . . . ? C30 O3 C3 C4 -178.7(2) . . . . ? Co O3 C3 C4 39.0(3) . . . . ? O2 C2 C3 O3 166.0(2) . . . . ? C1 C2 C3 O3 -85.0(3) . . . . ? O2 C2 C3 C4 -75.0(3) . . . . ? C1 C2 C3 C4 33.9(3) . . . . ? C1 O4 C4 C5 157.0(2) . . . . ? C1 O4 C4 C3 26.2(3) . . . . ? O3 C3 C4 O4 79.8(3) . . . . ? C2 C3 C4 O4 -36.5(3) . . . . ? O3 C3 C4 C5 -42.7(3) . . . . ? C2 C3 C4 C5 -159.0(2) . . . . ? C50 O5 C5 C4 85.3(3) . . . . ? Co O5 C5 C4 -72.3(2) . . . . ? C50 O5 C5 C6 -151.6(3) . . . . ? Co O5 C5 C6 50.8(2) . . . . ? O4 C4 C5 O5 -59.4(3) . . . . ? C3 C4 C5 O5 61.6(3) . . . . ? O4 C4 C5 C6 -177.0(2) . . . . ? C3 C4 C5 C6 -56.0(3) . . . . ? C60 O6 C6 C5 158.8(2) . . . . ? Co O6 C6 C5 36.6(2) . . . . ? O5 C5 C6 O6 -55.3(2) . . . . ? C4 C5 C6 O6 66.9(3) . . . . ? C1 O1 C10 O2 0.8(3) . . . . ? C1 O1 C10 C11 119.1(3) . . . . ? C1 O1 C10 C12 -116.9(3) . . . . ? C2 O2 C10 O1 -17.9(3) . . . . ? C2 O2 C10 C11 -137.2(4) . . . . ? C2 O2 C10 C12 100.1(3) . . . . ? C3 O3 C30 C31 -149.9(2) . . . . ? Co O3 C30 C31 -3.5(3) . . . . ? C35 N3 C31 C32 1.1(4) . . . . ? Co N3 C31 C32 177.9(2) . . . . ? C35 N3 C31 C30 -179.3(2) . . . . ? Co N3 C31 C30 -2.6(3) . . . . ? O3 C30 C31 N3 4.1(3) . . . . ? O3 C30 C31 C32 -176.4(2) . . . . ? N3 C31 C32 C33 -0.7(4) . . . . ? C30 C31 C32 C33 179.8(3) . . . . ? C31 C32 C33 C34 -0.5(4) . . . . ? C32 C33 C34 C35 1.0(5) . . . . ? C31 N3 C35 C34 -0.5(4) . . . . ? Co N3 C35 C34 -177.0(2) . . . . ? C33 C34 C35 N3 -0.6(5) . . . . ? C5 O5 C50 C51 -172.3(3) . . . . ? Co O5 C50 C51 -16.2(4) . . . . ? C55 N5 C51 C52 -0.7(5) . . . . ? Co N5 C51 C52 173.9(3) . . . . ? C55 N5 C51 C50 177.8(3) . . . . ? Co N5 C51 C50 -7.6(4) . . . . ? O5 C50 C51 N5 14.6(5) . . . . ? O5 C50 C51 C52 -166.8(3) . . . . ? N5 C51 C52 C53 -0.6(6) . . . . ? C50 C51 C52 C53 -179.1(4) . . . . ? C51 C52 C53 C54 1.0(6) . . . . ? C52 C53 C54 C55 0.0(5) . . . . ? C51 N5 C55 C54 1.7(4) . . . . ? Co N5 C55 C54 -172.3(2) . . . . ? C53 C54 C55 N5 -1.4(5) . . . . ? C6 O6 C60 C61 -83.3(3) . . . . ? Co O6 C60 C61 39.5(2) . . . . ? C65 N6 C61 C62 0.3(4) . . . . ? Co N6 C61 C62 -179.3(2) . . . . ? C65 N6 C61 C60 -178.4(2) . . . . ? Co N6 C61 C60 2.1(3) . . . . ? O6 C60 C61 N6 -28.6(3) . . . . ? O6 C60 C61 C62 152.8(2) . . . . ? N6 C61 C62 C63 -0.6(4) . . . . ? C60 C61 C62 C63 178.0(3) . . . . ? C61 C62 C63 C64 0.8(4) . . . . ? C62 C63 C64 C65 -0.8(4) . . . . ? C61 N6 C65 C64 -0.2(4) . . . . ? Co N6 C65 C64 179.3(2) . . . . ? C63 C64 C65 N6 0.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.869 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.608 _refine_diff_density_min -0.495 _refine_diff_density_rms 0.063 # Attachment '4cif.txt' data_344GuillotICMMO4 _database_code_depnum_ccdc_archive 'CCDC 614623' _audit_creation_method SHELXL-97 _chemical_name_systematic '[2,3,5-tri-O-(2-picolyl)-\a-D-methyl-lyxofuranoside Co(II)] 2(ClO4)' _chemical_name_common ;(2,3,5-tri-O-(2-picolyl)-alpha-D-methyl-lyxofuranoside Co(ii)) 2(ClO4) ; _chemical_melting_point ? _chemical_formula_moiety 'C24 H27 Co N3 O5, 2(Cl O4)' _chemical_formula_sum 'C24 H27 Cl2 Co N3 O13' _chemical_formula_weight 695.32 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 orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_int_tables_number 19 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 10.004(5) _cell_length_b 15.277(5) _cell_length_c 18.573(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2838.5(19) _cell_formula_units_Z 4 _cell_measurement_temperature 100(1) _cell_measurement_reflns_used 7220 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 30.56 _exptl_crystal_description plate _exptl_crystal_colour pink _exptl_crystal_size_max 0.230 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.080 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.627 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1428 _exptl_absorpt_coefficient_mu 0.865 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.832 _exptl_absorpt_correction_T_max 0.941 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(1) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'kappa X8 APEX II Bruker ICMMO' _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 19202 _diffrn_reflns_av_R_equivalents 0.0223 _diffrn_reflns_av_sigmaI/netI 0.0342 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 30.73 _reflns_number_total 7299 _reflns_number_gt 6865 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0435P)^2^+1.5081P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.021(11) _refine_ls_number_reflns 7299 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0363 _refine_ls_R_factor_gt 0.0335 _refine_ls_wR_factor_ref 0.0853 _refine_ls_wR_factor_gt 0.0841 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.10406(3) 0.944533(19) 0.712292(15) 0.01522(7) Uani 1 1 d . . . O1 O 0.48650(17) 0.94553(13) 0.51912(9) 0.0262(4) Uani 1 1 d . . . O2 O 0.24167(17) 0.87134(10) 0.64761(9) 0.0208(3) Uani 1 1 d . . . O3 O 0.13764(18) 1.02326(14) 0.62441(10) 0.0336(5) Uani 1 1 d . . . O4 O 0.47210(17) 0.97828(11) 0.64153(9) 0.0223(3) Uani 1 1 d . . . O5 O 0.26946(17) 1.01630(10) 0.74914(9) 0.0195(3) Uani 1 1 d . . . N2 N -0.01200(19) 0.83632(13) 0.67756(10) 0.0184(4) Uani 1 1 d . . . N3 N -0.05945(19) 1.02981(11) 0.70893(11) 0.0169(3) Uani 1 1 d . . . N5 N 0.13235(18) 0.89790(11) 0.81547(10) 0.0158(4) Uani 1 1 d . . . C1 C 0.4440(2) 0.91598(15) 0.58638(13) 0.0196(4) Uani 1 1 d . . . H1 H 0.4820 0.8585 0.5978 0.024 Uiso 1 1 calc R . . C2 C 0.2936(2) 0.91284(15) 0.58354(13) 0.0188(4) Uani 1 1 d . . . H2 H 0.2597 0.8863 0.5391 0.023 Uiso 1 1 calc R . . C3 C 0.2615(2) 1.01093(15) 0.58904(13) 0.0218(5) Uani 1 1 d . . . H3 H 0.2595 1.0376 0.5411 0.026 Uiso 1 1 calc R . . C4 C 0.3781(2) 1.04854(15) 0.63361(13) 0.0223(5) Uani 1 1 d . . . H4 H 0.4203 1.0962 0.6065 0.027 Uiso 1 1 calc R . . C5 C 0.3395(3) 1.08185(14) 0.70748(14) 0.0248(5) Uani 1 1 d . . . H5A H 0.4195 1.0995 0.7332 0.030 Uiso 1 1 calc R . . H5B H 0.2829 1.1330 0.7022 0.030 Uiso 1 1 calc R . . C10 C 0.6288(3) 0.9529(2) 0.51463(17) 0.0417(7) Uani 1 1 d . . . H10A H 0.6534 0.9736 0.4677 0.063 Uiso 1 1 calc R . . H10B H 0.6687 0.8966 0.5228 0.063 Uiso 1 1 calc R . . H10C H 0.6600 0.9934 0.5504 0.063 Uiso 1 1 calc R . . C20 C 0.2031(3) 0.78084(15) 0.63834(15) 0.0252(5) Uani 1 1 d . . . H20A H 0.2478 0.7450 0.6741 0.030 Uiso 1 1 calc R . . H20B H 0.2303 0.7607 0.5910 0.030 Uiso 1 1 calc R . . C21 C 0.0544(2) 0.77144(14) 0.64622(13) 0.0193(4) Uani 1 1 d . . . C22 C -0.0101(3) 0.69529(15) 0.62326(13) 0.0258(5) Uani 1 1 d . . . H22 H 0.0381 0.6509 0.6008 0.031 Uiso 1 1 calc R . . C23 C -0.1458(3) 0.68652(17) 0.63421(14) 0.0295(6) Uani 1 1 d . . . H23 H -0.1901 0.6361 0.6194 0.035 Uiso 1 1 calc R . . C24 C -0.2152(3) 0.75363(17) 0.66749(14) 0.0265(5) Uani 1 1 d . . . H24 H -0.3066 0.7489 0.6759 0.032 Uiso 1 1 calc R . . C25 C -0.1456(2) 0.82803(16) 0.68799(13) 0.0218(5) Uani 1 1 d . . . H25 H -0.1920 0.8738 0.7096 0.026 Uiso 1 1 calc R . . C30 C 0.0294(2) 1.06269(17) 0.58964(13) 0.0240(5) Uani 1 1 d . . . H30A H -0.0018 1.0264 0.5502 0.029 Uiso 1 1 calc R . . H30B H 0.0546 1.1195 0.5707 0.029 Uiso 1 1 calc R . . C31 C -0.0780(2) 1.07219(13) 0.64639(13) 0.0174(4) Uani 1 1 d . . . C32 C -0.1918(2) 1.12260(15) 0.63337(14) 0.0230(5) Uani 1 1 d . . . H32 H -0.2037 1.1500 0.5891 0.028 Uiso 1 1 calc R . . C33 C -0.2859(2) 1.13126(15) 0.68670(15) 0.0255(5) Uani 1 1 d . . . H33 H -0.3617 1.1653 0.6792 0.031 Uiso 1 1 calc R . . C34 C -0.2669(2) 1.08892(15) 0.75173(14) 0.0237(5) Uani 1 1 d . . . H34 H -0.3293 1.0940 0.7886 0.028 Uiso 1 1 calc R . . C35 C -0.1531(2) 1.03900(14) 0.76051(13) 0.0207(4) Uani 1 1 d . . . H35 H -0.1404 1.0103 0.8041 0.025 Uiso 1 1 calc R . . C50 C 0.3496(2) 0.96504(15) 0.79740(12) 0.0204(4) Uani 1 1 d . . . H50A H 0.4036 1.0029 0.8276 0.024 Uiso 1 1 calc R . . H50B H 0.4086 0.9267 0.7705 0.024 Uiso 1 1 calc R . . C51 C 0.2552(2) 0.91240(14) 0.84248(12) 0.0165(4) Uani 1 1 d . . . C52 C 0.2923(2) 0.87978(14) 0.90916(13) 0.0195(4) Uani 1 1 d . . . H52 H 0.3780 0.8896 0.9268 0.023 Uiso 1 1 calc R . . C53 C 0.2010(3) 0.83263(14) 0.94912(13) 0.0210(5) Uani 1 1 d . . . H53 H 0.2251 0.8091 0.9934 0.025 Uiso 1 1 calc R . . C54 C 0.0724(2) 0.82074(14) 0.92229(12) 0.0208(4) Uani 1 1 d . . . H54 H 0.0079 0.7916 0.9493 0.025 Uiso 1 1 calc R . . C55 C 0.0427(2) 0.85306(14) 0.85485(13) 0.0195(4) Uani 1 1 d . . . H55 H -0.0421 0.8435 0.8360 0.023 Uiso 1 1 calc R . . Cl1 Cl 0.01038(6) 0.85220(4) 0.44252(3) 0.02557(13) Uani 1 1 d . . . O10 O -0.4496(2) 0.77375(14) 0.84088(12) 0.0375(5) Uani 1 1 d . . . O11 O -0.3910(2) 0.83323(13) 0.95293(10) 0.0324(4) Uani 1 1 d . . . O12 O -0.23272(17) 0.75192(11) 0.88642(10) 0.0229(3) Uani 1 1 d . . . O13 O -0.3001(2) 0.89154(13) 0.84707(12) 0.0388(5) Uani 1 1 d . . . Cl2 Cl -0.34381(5) 0.81297(3) 0.88188(3) 0.01746(10) Uani 1 1 d . . . O20 O 0.0860(2) 0.93157(12) 0.45073(11) 0.0375(5) Uani 1 1 d . . . O21 O -0.1127(3) 0.8564(2) 0.47922(18) 0.0756(9) Uani 1 1 d . . . O22 O 0.0905(2) 0.78166(13) 0.47188(11) 0.0381(5) Uani 1 1 d . . . O23 O -0.0096(2) 0.83481(14) 0.36663(11) 0.0371(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 0.01245(12) 0.02012(13) 0.01308(14) 0.00443(10) -0.00003(11) -0.00020(11) O1 0.0185(8) 0.0378(9) 0.0223(9) -0.0042(8) 0.0059(7) -0.0040(7) O2 0.0201(8) 0.0212(7) 0.0210(8) 0.0003(6) 0.0014(7) -0.0017(6) O3 0.0184(9) 0.0555(12) 0.0269(10) 0.0246(9) 0.0082(7) 0.0138(8) O4 0.0171(8) 0.0267(8) 0.0229(9) -0.0044(7) 0.0002(7) -0.0001(6) O5 0.0199(8) 0.0196(7) 0.0189(8) 0.0019(6) 0.0026(7) -0.0043(6) N2 0.0175(9) 0.0224(9) 0.0154(9) 0.0042(7) -0.0010(8) -0.0028(7) N3 0.0169(8) 0.0165(8) 0.0172(9) -0.0007(7) 0.0015(8) -0.0019(6) N5 0.0157(9) 0.0173(8) 0.0145(9) 0.0017(6) 0.0006(7) -0.0014(6) C1 0.0168(10) 0.0218(10) 0.0202(11) -0.0030(8) 0.0047(9) 0.0027(8) C2 0.0161(10) 0.0245(10) 0.0159(11) 0.0004(8) 0.0012(9) -0.0001(8) C3 0.0181(11) 0.0269(11) 0.0203(12) 0.0100(9) 0.0073(9) 0.0057(9) C4 0.0219(11) 0.0191(9) 0.0260(12) 0.0018(8) 0.0075(9) -0.0013(9) C5 0.0307(12) 0.0178(9) 0.0259(12) -0.0009(9) 0.0104(11) -0.0079(9) C10 0.0212(13) 0.065(2) 0.0393(16) -0.0174(15) 0.0125(11) -0.0122(13) C20 0.0236(12) 0.0179(10) 0.0342(14) -0.0003(9) 0.0034(10) 0.0024(9) C21 0.0231(11) 0.0200(10) 0.0148(11) 0.0044(8) -0.0013(9) -0.0020(8) C22 0.0364(14) 0.0211(10) 0.0200(12) -0.0002(9) -0.0034(10) -0.0022(10) C23 0.0358(14) 0.0256(11) 0.0271(13) 0.0022(9) -0.0099(11) -0.0097(10) C24 0.0209(11) 0.0303(12) 0.0282(14) 0.0037(10) -0.0067(10) -0.0088(10) C25 0.0173(10) 0.0277(11) 0.0204(11) 0.0001(9) -0.0005(9) -0.0045(9) C30 0.0195(11) 0.0336(12) 0.0188(11) 0.0079(9) 0.0002(9) 0.0068(9) C31 0.0161(10) 0.0153(9) 0.0209(11) 0.0018(7) 0.0006(8) -0.0015(7) C32 0.0219(11) 0.0196(10) 0.0274(13) 0.0048(9) -0.0030(10) 0.0007(8) C33 0.0183(11) 0.0183(10) 0.0398(15) -0.0021(9) -0.0001(11) 0.0026(8) C34 0.0189(11) 0.0224(10) 0.0297(14) -0.0046(9) 0.0074(10) -0.0020(8) C35 0.0223(10) 0.0196(10) 0.0203(11) -0.0007(8) 0.0029(9) -0.0031(8) C50 0.0166(9) 0.0296(11) 0.0149(11) 0.0006(8) -0.0012(8) -0.0033(8) C51 0.0169(10) 0.0177(9) 0.0150(10) -0.0030(7) -0.0002(8) 0.0008(8) C52 0.0175(10) 0.0228(10) 0.0183(11) -0.0037(8) -0.0039(9) 0.0035(8) C53 0.0311(12) 0.0179(10) 0.0140(11) 0.0014(8) -0.0043(9) 0.0005(8) C54 0.0287(12) 0.0191(9) 0.0146(11) 0.0046(8) 0.0003(9) -0.0032(8) C55 0.0180(10) 0.0216(10) 0.0189(11) 0.0051(8) -0.0007(9) -0.0011(8) Cl1 0.0175(3) 0.0314(3) 0.0278(3) 0.0007(2) 0.0023(2) -0.0017(2) O10 0.0255(9) 0.0384(10) 0.0486(13) -0.0139(9) -0.0122(9) 0.0013(8) O11 0.0331(10) 0.0473(11) 0.0168(8) 0.0010(7) 0.0051(8) 0.0146(9) O12 0.0180(8) 0.0255(8) 0.0252(9) 0.0023(7) 0.0032(7) 0.0052(6) O13 0.0414(12) 0.0285(9) 0.0466(13) 0.0167(9) 0.0150(10) 0.0011(8) Cl2 0.0172(2) 0.0189(2) 0.0163(3) 0.00220(18) 0.00205(19) 0.00018(18) O20 0.0519(13) 0.0283(9) 0.0321(10) 0.0003(7) -0.0128(10) -0.0055(9) O21 0.0352(14) 0.109(2) 0.083(2) -0.0127(18) 0.0298(15) 0.0006(16) O22 0.0530(13) 0.0306(9) 0.0306(11) 0.0067(8) -0.0036(10) 0.0025(9) O23 0.0354(11) 0.0443(11) 0.0317(11) -0.0016(9) -0.0144(9) 0.0027(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 O3 2.0551(18) . ? Co N5 2.0639(19) . ? Co N3 2.092(2) . ? Co O5 2.0996(18) . ? Co N2 2.121(2) . ? Co O2 2.1421(18) . ? O1 C1 1.395(3) . ? O1 C10 1.431(3) . ? O2 C2 1.445(3) . ? O2 C20 1.446(3) . ? O3 C30 1.397(3) . ? O3 C3 1.415(3) . ? O4 C1 1.426(3) . ? O4 C4 1.434(3) . ? O5 C50 1.435(3) . ? O5 C5 1.447(3) . ? N2 C21 1.328(3) . ? N2 C25 1.356(3) . ? N3 C31 1.343(3) . ? N3 C35 1.347(3) . ? N5 C55 1.345(3) . ? N5 C51 1.346(3) . ? C1 C2 1.507(3) . ? C1 H1 0.9800 . ? C2 C3 1.536(3) . ? C2 H2 0.9800 . ? C3 C4 1.542(4) . ? C3 H3 0.9800 . ? C4 C5 1.513(3) . ? C4 H4 0.9800 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C20 C21 1.501(4) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.397(3) . ? C22 C23 1.379(4) . ? C22 H22 0.9300 . ? C23 C24 1.384(4) . ? C23 H23 0.9300 . ? C24 C25 1.386(3) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C30 C31 1.512(3) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.396(3) . ? C32 C33 1.373(4) . ? C32 H32 0.9300 . ? C33 C34 1.383(4) . ? C33 H33 0.9300 . ? C34 C35 1.381(3) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C50 C51 1.496(3) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 C52 1.386(3) . ? C52 C53 1.380(3) . ? C52 H52 0.9300 . ? C53 C54 1.391(3) . ? C53 H53 0.9300 . ? C54 C55 1.379(3) . ? C54 H54 0.9300 . ? C55 H55 0.9300 . ? Cl1 O21 1.409(3) . ? Cl1 O20 1.437(2) . ? Cl1 O23 1.448(2) . ? Cl1 O22 1.449(2) . ? O10 Cl2 1.435(2) . ? O11 Cl2 1.4355(19) . ? O12 Cl2 1.4533(17) . ? O13 Cl2 1.432(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Co N5 156.49(8) . . ? O3 Co N3 74.91(7) . . ? N5 Co N3 110.48(8) . . ? O3 Co O5 79.89(8) . . ? N5 Co O5 76.68(7) . . ? N3 Co O5 107.50(7) . . ? O3 Co N2 107.70(9) . . ? N5 Co N2 95.07(7) . . ? N3 Co N2 92.77(8) . . ? O5 Co N2 159.67(7) . . ? O3 Co O2 75.82(7) . . ? N5 Co O2 104.62(7) . . ? N3 Co O2 144.17(7) . . ? O5 Co O2 87.07(7) . . ? N2 Co O2 76.96(8) . . ? C1 O1 C10 112.4(2) . . ? C2 O2 C20 114.68(19) . . ? C2 O2 Co 117.63(13) . . ? C20 O2 Co 113.23(14) . . ? C30 O3 C3 121.43(18) . . ? C30 O3 Co 119.52(14) . . ? C3 O3 Co 115.71(14) . . ? C1 O4 C4 107.27(17) . . ? C50 O5 C5 116.19(19) . . ? C50 O5 Co 111.02(13) . . ? C5 O5 Co 124.67(15) . . ? C21 N2 C25 119.1(2) . . ? C21 N2 Co 116.18(16) . . ? C25 N2 Co 124.67(17) . . ? C31 N3 C35 118.0(2) . . ? C31 N3 Co 115.72(15) . . ? C35 N3 Co 125.96(16) . . ? C55 N5 C51 119.3(2) . . ? C55 N5 Co 126.11(16) . . ? C51 N5 Co 114.49(14) . . ? O1 C1 O4 111.55(19) . . ? O1 C1 C2 106.4(2) . . ? O4 C1 C2 104.06(18) . . ? O1 C1 H1 111.5 . . ? O4 C1 H1 111.5 . . ? C2 C1 H1 111.5 . . ? O2 C2 C1 110.12(19) . . ? O2 C2 C3 107.36(18) . . ? C1 C2 C3 100.08(18) . . ? O2 C2 H2 112.8 . . ? C1 C2 H2 112.8 . . ? C3 C2 H2 112.8 . . ? O3 C3 C2 110.09(19) . . ? O3 C3 C4 111.3(2) . . ? C2 C3 C4 103.98(18) . . ? O3 C3 H3 110.4 . . ? C2 C3 H3 110.4 . . ? C4 C3 H3 110.4 . . ? O4 C4 C5 109.0(2) . . ? O4 C4 C3 105.79(18) . . ? C5 C4 C3 114.8(2) . . ? O4 C4 H4 109.0 . . ? C5 C4 H4 109.0 . . ? C3 C4 H4 109.0 . . ? O5 C5 C4 112.08(18) . . ? O5 C5 H5A 109.2 . . ? C4 C5 H5A 109.2 . . ? O5 C5 H5B 109.2 . . ? C4 C5 H5B 109.2 . . ? H5A C5 H5B 107.9 . . ? O1 C10 H10A 109.5 . . ? O1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? O1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O2 C20 C21 110.15(19) . . ? O2 C20 H20A 109.6 . . ? C21 C20 H20A 109.6 . . ? O2 C20 H20B 109.6 . . ? C21 C20 H20B 109.6 . . ? H20A C20 H20B 108.1 . . ? N2 C21 C22 121.6(2) . . ? N2 C21 C20 117.9(2) . . ? C22 C21 C20 120.5(2) . . ? C23 C22 C21 119.4(2) . . ? C23 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? C22 C23 C24 119.2(2) . . ? C22 C23 H23 120.4 . . ? C24 C23 H23 120.4 . . ? C23 C24 C25 118.5(2) . . ? C23 C24 H24 120.7 . . ? C25 C24 H24 120.7 . . ? N2 C25 C24 122.2(2) . . ? N2 C25 H25 118.9 . . ? C24 C25 H25 118.9 . . ? O3 C30 C31 105.65(19) . . ? O3 C30 H30A 110.6 . . ? C31 C30 H30A 110.6 . . ? O3 C30 H30B 110.6 . . ? C31 C30 H30B 110.6 . . ? H30A C30 H30B 108.7 . . ? N3 C31 C32 121.9(2) . . ? N3 C31 C30 117.31(19) . . ? C32 C31 C30 120.8(2) . . ? C33 C32 C31 119.2(2) . . ? C33 C32 H32 120.4 . . ? C31 C32 H32 120.4 . . ? C32 C33 C34 119.4(2) . . ? C32 C33 H33 120.3 . . ? C34 C33 H33 120.3 . . ? C35 C34 C33 118.3(2) . . ? C35 C34 H34 120.8 . . ? C33 C34 H34 120.8 . . ? N3 C35 C34 123.2(2) . . ? N3 C35 H35 118.4 . . ? C34 C35 H35 118.4 . . ? O5 C50 C51 106.90(19) . . ? O5 C50 H50A 110.3 . . ? C51 C50 H50A 110.3 . . ? O5 C50 H50B 110.3 . . ? C51 C50 H50B 110.3 . . ? H50A C50 H50B 108.6 . . ? N5 C51 C52 121.2(2) . . ? N5 C51 C50 117.1(2) . . ? C52 C51 C50 121.7(2) . . ? C53 C52 C51 119.4(2) . . ? C53 C52 H52 120.3 . . ? C51 C52 H52 120.3 . . ? C52 C53 C54 119.2(2) . . ? C52 C53 H53 120.4 . . ? C54 C53 H53 120.4 . . ? C55 C54 C53 118.5(2) . . ? C55 C54 H54 120.7 . . ? C53 C54 H54 120.7 . . ? N5 C55 C54 122.2(2) . . ? N5 C55 H55 118.9 . . ? C54 C55 H55 118.9 . . ? O21 Cl1 O20 111.72(18) . . ? O21 Cl1 O23 111.02(17) . . ? O20 Cl1 O23 109.31(13) . . ? O21 Cl1 O22 109.57(18) . . ? O20 Cl1 O22 107.24(13) . . ? O23 Cl1 O22 107.83(12) . . ? O13 Cl2 O10 109.62(14) . . ? O13 Cl2 O11 109.56(13) . . ? O10 Cl2 O11 109.58(14) . . ? O13 Cl2 O12 109.30(12) . . ? O10 Cl2 O12 109.08(12) . . ? O11 Cl2 O12 109.67(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Co O2 C2 4.72(15) . . . . ? N5 Co O2 C2 -151.01(15) . . . . ? N3 Co O2 C2 40.7(2) . . . . ? O5 Co O2 C2 -75.59(15) . . . . ? N2 Co O2 C2 117.08(16) . . . . ? O3 Co O2 C20 -132.80(17) . . . . ? N5 Co O2 C20 71.48(17) . . . . ? N3 Co O2 C20 -96.77(18) . . . . ? O5 Co O2 C20 146.89(16) . . . . ? N2 Co O2 C20 -20.43(16) . . . . ? N5 Co O3 C30 -132.0(2) . . . . ? N3 Co O3 C30 -25.25(19) . . . . ? O5 Co O3 C30 -136.6(2) . . . . ? N2 Co O3 C30 62.8(2) . . . . ? O2 Co O3 C30 133.9(2) . . . . ? N5 Co O3 C3 68.3(3) . . . . ? N3 Co O3 C3 175.1(2) . . . . ? O5 Co O3 C3 63.69(19) . . . . ? N2 Co O3 C3 -96.86(19) . . . . ? O2 Co O3 C3 -25.83(18) . . . . ? O3 Co O5 C50 -148.94(15) . . . . ? N5 Co O5 C50 32.94(14) . . . . ? N3 Co O5 C50 140.54(14) . . . . ? N2 Co O5 C50 -34.9(3) . . . . ? O2 Co O5 C50 -72.83(15) . . . . ? O3 Co O5 C5 -1.72(17) . . . . ? N5 Co O5 C5 -179.84(18) . . . . ? N3 Co O5 C5 -72.24(18) . . . . ? N2 Co O5 C5 112.4(2) . . . . ? O2 Co O5 C5 74.39(17) . . . . ? O3 Co N2 C21 81.44(17) . . . . ? N5 Co N2 C21 -92.67(17) . . . . ? N3 Co N2 C21 156.48(16) . . . . ? O5 Co N2 C21 -27.9(3) . . . . ? O2 Co N2 C21 11.19(16) . . . . ? O3 Co N2 C25 -101.49(19) . . . . ? N5 Co N2 C25 84.4(2) . . . . ? N3 Co N2 C25 -26.5(2) . . . . ? O5 Co N2 C25 149.2(2) . . . . ? O2 Co N2 C25 -171.7(2) . . . . ? O3 Co N3 C31 16.56(15) . . . . ? N5 Co N3 C31 172.51(14) . . . . ? O5 Co N3 C31 90.56(16) . . . . ? N2 Co N3 C31 -91.03(16) . . . . ? O2 Co N3 C31 -19.6(2) . . . . ? O3 Co N3 C35 -170.3(2) . . . . ? N5 Co N3 C35 -14.4(2) . . . . ? O5 Co N3 C35 -96.32(18) . . . . ? N2 Co N3 C35 82.08(19) . . . . ? O2 Co N3 C35 153.47(16) . . . . ? O3 Co N5 C55 157.93(19) . . . . ? N3 Co N5 C55 58.61(19) . . . . ? O5 Co N5 C55 162.58(19) . . . . ? N2 Co N5 C55 -36.26(19) . . . . ? O2 Co N5 C55 -114.08(18) . . . . ? O3 Co N5 C51 -24.8(3) . . . . ? N3 Co N5 C51 -124.08(15) . . . . ? O5 Co N5 C51 -20.11(15) . . . . ? N2 Co N5 C51 141.05(15) . . . . ? O2 Co N5 C51 63.23(16) . . . . ? C10 O1 C1 O4 66.2(3) . . . . ? C10 O1 C1 C2 179.1(2) . . . . ? C4 O4 C1 O1 74.1(2) . . . . ? C4 O4 C1 C2 -40.3(2) . . . . ? C20 O2 C2 C1 -100.7(2) . . . . ? Co O2 C2 C1 122.43(16) . . . . ? C20 O2 C2 C3 151.30(19) . . . . ? Co O2 C2 C3 14.4(2) . . . . ? O1 C1 C2 O2 172.05(17) . . . . ? O4 C1 C2 O2 -70.0(2) . . . . ? O1 C1 C2 C3 -75.1(2) . . . . ? O4 C1 C2 C3 42.8(2) . . . . ? C30 O3 C3 C2 -117.7(3) . . . . ? Co O3 C3 C2 41.6(3) . . . . ? C30 O3 C3 C4 127.5(2) . . . . ? Co O3 C3 C4 -73.2(2) . . . . ? O2 C2 C3 O3 -34.2(3) . . . . ? C1 C2 C3 O3 -149.2(2) . . . . ? O2 C2 C3 C4 85.1(2) . . . . ? C1 C2 C3 C4 -29.8(2) . . . . ? C1 O4 C4 C5 143.80(19) . . . . ? C1 O4 C4 C3 19.9(2) . . . . ? O3 C3 C4 O4 126.00(19) . . . . ? C2 C3 C4 O4 7.5(2) . . . . ? O3 C3 C4 C5 5.8(3) . . . . ? C2 C3 C4 C5 -112.7(2) . . . . ? C50 O5 C5 C4 95.1(2) . . . . ? Co O5 C5 C4 -50.6(3) . . . . ? O4 C4 C5 O5 -64.4(3) . . . . ? C3 C4 C5 O5 54.0(3) . . . . ? C2 O2 C20 C21 -113.1(2) . . . . ? Co O2 C20 C21 25.7(3) . . . . ? C25 N2 C21 C22 0.5(3) . . . . ? Co N2 C21 C22 177.77(18) . . . . ? C25 N2 C21 C20 -177.4(2) . . . . ? Co N2 C21 C20 -0.1(3) . . . . ? O2 C20 C21 N2 -17.1(3) . . . . ? O2 C20 C21 C22 165.0(2) . . . . ? N2 C21 C22 C23 -0.9(4) . . . . ? C20 C21 C22 C23 176.9(2) . . . . ? C21 C22 C23 C24 0.3(4) . . . . ? C22 C23 C24 C25 0.7(4) . . . . ? C21 N2 C25 C24 0.5(4) . . . . ? Co N2 C25 C24 -176.49(18) . . . . ? C23 C24 C25 N2 -1.1(4) . . . . ? C3 O3 C30 C31 -174.5(2) . . . . ? Co O3 C30 C31 27.0(3) . . . . ? C35 N3 C31 C32 -1.7(3) . . . . ? Co N3 C31 C32 171.94(17) . . . . ? C35 N3 C31 C30 178.8(2) . . . . ? Co N3 C31 C30 -7.5(3) . . . . ? O3 C30 C31 N3 -11.5(3) . . . . ? O3 C30 C31 C32 169.0(2) . . . . ? N3 C31 C32 C33 1.9(3) . . . . ? C30 C31 C32 C33 -178.6(2) . . . . ? C31 C32 C33 C34 -0.9(4) . . . . ? C32 C33 C34 C35 -0.1(3) . . . . ? C31 N3 C35 C34 0.7(3) . . . . ? Co N3 C35 C34 -172.29(17) . . . . ? C33 C34 C35 N3 0.2(4) . . . . ? C5 O5 C50 C51 171.31(17) . . . . ? Co O5 C50 C51 -38.4(2) . . . . ? C55 N5 C51 C52 1.9(3) . . . . ? Co N5 C51 C52 -175.58(16) . . . . ? C55 N5 C51 C50 -178.12(19) . . . . ? Co N5 C51 C50 4.4(2) . . . . ? O5 C50 C51 N5 22.7(3) . . . . ? O5 C50 C51 C52 -157.3(2) . . . . ? N5 C51 C52 C53 -1.0(3) . . . . ? C50 C51 C52 C53 179.1(2) . . . . ? C51 C52 C53 C54 -1.6(3) . . . . ? C52 C53 C54 C55 3.1(3) . . . . ? C51 N5 C55 C54 -0.3(3) . . . . ? Co N5 C55 C54 176.87(17) . . . . ? C53 C54 C55 N5 -2.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.855 _diffrn_reflns_theta_full 30.73 _diffrn_measured_fraction_theta_full 0.855 _refine_diff_density_max 0.664 _refine_diff_density_min -0.568 _refine_diff_density_rms 0.077 data_517GuillotICMMO _database_code_depnum_ccdc_archive 'CCDC 614625' _audit_creation_method SHELXL-97 _chemical_name_systematic '[3,5,6-tri-O-(2-picolyl)-1,2-isopropylidene-\a-L-glucofuranose Co(II)] (PF6)2' _chemical_name_common ; (3,5,6-tri-O-(2-picolyl)-1,2-isopropylidene-alpha-L- glucofuranose Co(ii)) (PF6)2 ; _chemical_melting_point ? _chemical_formula_moiety 'C27 H31 Co N3 O6, 2(F6 P), H2 O' _chemical_formula_sum 'C27 H33 Co F12 N3 O7 P2' _chemical_formula_weight 860.42 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 'P 21' _symmetry_int_tables_number 4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.1512(7) _cell_length_b 19.1282(15) _cell_length_c 10.0022(8) _cell_angle_alpha 90.00 _cell_angle_beta 104.1590(10) _cell_angle_gamma 90.00 _cell_volume 1697.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(1) _cell_measurement_reflns_used 5248 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 32.65 _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_max 0.120 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.070 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.679 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 870 _exptl_absorpt_coefficient_mu 0.714 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.915 _exptl_absorpt_correction_T_max 0.952 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(1) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'kappa APEX II Bruker ICMMO' _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 14987 _diffrn_reflns_av_R_equivalents 0.0230 _diffrn_reflns_av_sigmaI/netI 0.0528 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 36.43 _reflns_number_total 9158 _reflns_number_gt 7537 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0470P)^2^+1.4059P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.020(13) _refine_ls_number_reflns 9158 _refine_ls_number_parameters 469 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0652 _refine_ls_R_factor_gt 0.0491 _refine_ls_wR_factor_ref 0.1213 _refine_ls_wR_factor_gt 0.1152 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _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 Co Co 0.83965(5) 0.86618(2) 0.75300(3) 0.01616(8) Uani 1 1 d . . . O1 O 0.2315(4) 0.7258(2) 0.6030(3) 0.0462(8) Uani 1 1 d . . . O2 O 0.4001(3) 0.67644(16) 0.4949(3) 0.0354(7) Uani 1 1 d . . . O3 O 0.7163(3) 0.76914(12) 0.71672(19) 0.0170(4) Uani 1 1 d . . . O4 O 0.3956(3) 0.81994(15) 0.6091(2) 0.0258(5) Uani 1 1 d . . . O5 O 0.6432(3) 0.91340(13) 0.6615(2) 0.0218(5) Uani 1 1 d . . . O6 O 0.8249(3) 0.84978(11) 0.53396(19) 0.0183(4) Uani 1 1 d . . . N3 N 1.0002(3) 0.79695(14) 0.8507(2) 0.0173(5) Uani 1 1 d . . . N5 N 0.7869(3) 0.92361(16) 0.9136(2) 0.0218(5) Uani 1 1 d . . . N6 N 0.9928(3) 0.94055(14) 0.7069(3) 0.0199(5) Uani 1 1 d . . . C1 C 0.3726(4) 0.7534(2) 0.6637(3) 0.0312(8) Uani 1 1 d . . . H1 H 0.3891 0.7555 0.7642 0.037 Uiso 1 1 calc R . . C2 C 0.4862(4) 0.7044(2) 0.6227(3) 0.0269(7) Uani 1 1 d . . . H2 H 0.5270 0.6687 0.6920 0.032 Uiso 1 1 calc R . . C3 C 0.6056(4) 0.75261(16) 0.5904(3) 0.0174(5) Uani 1 1 d . . . H3 H 0.6530 0.7317 0.5221 0.021 Uiso 1 1 calc R . . C4 C 0.5077(4) 0.81532(17) 0.5302(3) 0.0181(5) Uani 1 1 d . . . H4 H 0.4550 0.8031 0.4356 0.022 Uiso 1 1 calc R . . C5 C 0.5748(4) 0.88741(16) 0.5256(3) 0.0187(6) Uani 1 1 d . . . H5 H 0.4948 0.9196 0.4801 0.022 Uiso 1 1 calc R . . C6 C 0.7006(4) 0.88971(17) 0.4514(3) 0.0210(6) Uani 1 1 d . . . H6A H 0.6672 0.8694 0.3601 0.025 Uiso 1 1 calc R . . H6B H 0.7313 0.9376 0.4420 0.025 Uiso 1 1 calc R . . C10 C 0.2446(5) 0.6785(3) 0.4956(4) 0.0434(12) Uani 1 1 d . . . C11 C 0.1553(6) 0.7056(4) 0.3583(5) 0.0612(18) Uani 1 1 d . . . H11A H 0.0503 0.7071 0.3577 0.092 Uiso 1 1 calc R . . H11B H 0.1695 0.6752 0.2861 0.092 Uiso 1 1 calc R . . H11C H 0.1892 0.7518 0.3435 0.092 Uiso 1 1 calc R . . C12 C 0.1947(8) 0.6056(4) 0.5280(5) 0.070(2) Uani 1 1 d . . . H12A H 0.0901 0.6067 0.5291 0.105 Uiso 1 1 calc R . . H12B H 0.2538 0.5909 0.6165 0.105 Uiso 1 1 calc R . . H12C H 0.2089 0.5734 0.4586 0.105 Uiso 1 1 calc R . . C30 C 0.8061(4) 0.70888(16) 0.7728(3) 0.0207(6) Uani 1 1 d . . . H30A H 0.8122 0.6774 0.6983 0.025 Uiso 1 1 calc R . . H30B H 0.7573 0.6841 0.8345 0.025 Uiso 1 1 calc R . . C31 C 0.9615(4) 0.72927(16) 0.8494(3) 0.0172(5) Uani 1 1 d . . . C32 C 1.0626(4) 0.67841(19) 0.9165(3) 0.0229(6) Uani 1 1 d . . . H32 H 1.0345 0.6316 0.9123 0.027 Uiso 1 1 calc R . . C33 C 1.2030(4) 0.6982(2) 0.9882(3) 0.0282(7) Uani 1 1 d . . . H33 H 1.2709 0.6649 1.0346 0.034 Uiso 1 1 calc R . . C34 C 1.2441(4) 0.7682(2) 0.9916(3) 0.0273(7) Uani 1 1 d . . . H34 H 1.3396 0.7825 1.0398 0.033 Uiso 1 1 calc R . . C35 C 1.1400(4) 0.81624(19) 0.9219(3) 0.0220(6) Uani 1 1 d . . . H35 H 1.1667 0.8632 0.9240 0.026 Uiso 1 1 calc R . . C50 C 0.5550(5) 0.9473(3) 0.7419(4) 0.0435(12) Uani 1 1 d . . . H50A H 0.4702 0.9182 0.7483 0.052 Uiso 1 1 calc R . . H50B H 0.5169 0.9915 0.7003 0.052 Uiso 1 1 calc R . . C51 C 0.6579(4) 0.9589(2) 0.8833(4) 0.0307(8) Uani 1 1 d . . . C52 C 0.6144(5) 1.0046(3) 0.9739(4) 0.0403(10) Uani 1 1 d . . . H52 H 0.5231 1.0283 0.9486 0.048 Uiso 1 1 calc R . . C53 C 0.7099(5) 1.0139(2) 1.1027(4) 0.0366(10) Uani 1 1 d . . . H53 H 0.6850 1.0449 1.1653 0.044 Uiso 1 1 calc R . . C54 C 0.8418(4) 0.9769(2) 1.1368(3) 0.0289(8) Uani 1 1 d . . . H54 H 0.9073 0.9821 1.2234 0.035 Uiso 1 1 calc R . . C55 C 0.8769(4) 0.93161(19) 1.0417(3) 0.0239(6) Uani 1 1 d . . . H55 H 0.9655 0.9058 1.0666 0.029 Uiso 1 1 calc R . . C60 C 0.9679(3) 0.8667(2) 0.5066(3) 0.0209(5) Uani 1 1 d . . . H60A H 0.9547 0.8754 0.4088 0.025 Uiso 1 1 calc R . . H60B H 1.0365 0.8276 0.5321 0.025 Uiso 1 1 calc R . . C61 C 1.0338(4) 0.93078(17) 0.5876(3) 0.0199(6) Uani 1 1 d . . . C62 C 1.1304(4) 0.97477(19) 0.5422(3) 0.0231(6) Uani 1 1 d . . . H62 H 1.1548 0.9667 0.4586 0.028 Uiso 1 1 calc R . . C63 C 1.1916(4) 1.0322(2) 0.6251(4) 0.0269(7) Uani 1 1 d . . . H63 H 1.2586 1.0625 0.5982 0.032 Uiso 1 1 calc R . . C64 C 1.1498(4) 1.04247(18) 0.7476(4) 0.0271(7) Uani 1 1 d . . . H64 H 1.1875 1.0801 0.8044 0.033 Uiso 1 1 calc R . . C65 C 1.0512(4) 0.99595(18) 0.7841(3) 0.0236(6) Uani 1 1 d . . . H65 H 1.0236 1.0033 0.8665 0.028 Uiso 1 1 calc R . . O1W O 0.4525(7) 0.6068(3) 0.2781(6) 0.0877(16) Uani 1 1 d . . . P1 P 0.30276(12) 0.23912(5) 0.84698(8) 0.0272(2) Uani 1 1 d . . . F1 F 0.4138(3) 0.17453(18) 0.8992(3) 0.0552(9) Uani 1 1 d . . . F2 F 0.4341(3) 0.27599(15) 0.7901(2) 0.0418(7) Uani 1 1 d . . . F3 F 0.3624(4) 0.2755(2) 0.9923(3) 0.0683(11) Uani 1 1 d . . . F4 F 0.1927(3) 0.30384(14) 0.7946(3) 0.0434(6) Uani 1 1 d . . . F5 F 0.1744(3) 0.19943(15) 0.9002(2) 0.0376(6) Uani 1 1 d . . . F6 F 0.2449(3) 0.20314(13) 0.6999(2) 0.0324(5) Uani 1 1 d . . . P2 P 0.68447(11) 0.50281(5) 0.79788(8) 0.02260(17) Uani 1 1 d . . . F7 F 0.6059(2) 0.56911(11) 0.8489(2) 0.0269(4) Uani 1 1 d . . . F8 F 0.6576(4) 0.53663(18) 0.6486(3) 0.0646(11) Uani 1 1 d . . . F9 F 0.5259(3) 0.46440(17) 0.7526(3) 0.0492(7) Uani 1 1 d . . . F10 F 0.7641(3) 0.43659(13) 0.7456(3) 0.0399(6) Uani 1 1 d . . . F11 F 0.8427(3) 0.54104(17) 0.8445(5) 0.0696(11) Uani 1 1 d . . . F12 F 0.7100(4) 0.46822(15) 0.9461(2) 0.0514(8) 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 0.0147(2) 0.01465(15) 0.01780(13) 0.00018(15) 0.00142(12) 0.00068(17) O1 0.0206(18) 0.064(2) 0.0506(16) 0.0140(16) 0.0023(12) -0.0122(15) O2 0.0294(18) 0.0307(14) 0.0357(12) 0.0042(11) -0.0120(11) -0.0127(12) O3 0.0135(12) 0.0179(9) 0.0169(8) 0.0017(7) -0.0017(7) 0.0002(8) O4 0.0181(14) 0.0364(14) 0.0239(9) 0.0057(9) 0.0070(9) 0.0038(10) O5 0.0168(13) 0.0250(11) 0.0211(8) -0.0049(8) -0.0005(8) 0.0059(9) O6 0.0178(13) 0.0175(10) 0.0190(8) 0.0024(7) 0.0034(7) 0.0006(8) N3 0.0133(14) 0.0194(12) 0.0181(9) 0.0000(8) 0.0016(8) 0.0007(10) N5 0.0179(16) 0.0264(14) 0.0206(10) -0.0045(9) 0.0038(9) -0.0038(11) N6 0.0218(16) 0.0159(11) 0.0207(9) 0.0026(8) 0.0028(9) 0.0004(10) C1 0.021(2) 0.047(2) 0.0242(13) 0.0108(14) 0.0038(12) -0.0061(16) C2 0.021(2) 0.0307(17) 0.0236(12) 0.0118(12) -0.0056(11) -0.0071(14) C3 0.0160(17) 0.0176(12) 0.0160(9) 0.0017(9) -0.0007(9) -0.0023(11) C4 0.0131(16) 0.0255(14) 0.0144(9) 0.0035(9) 0.0008(9) 0.0023(11) C5 0.0160(17) 0.0186(12) 0.0179(10) 0.0018(9) -0.0024(9) 0.0031(11) C6 0.0226(19) 0.0187(12) 0.0186(10) 0.0033(9) -0.0011(10) 0.0004(12) C10 0.022(2) 0.061(3) 0.0384(18) 0.0242(19) -0.0101(15) -0.022(2) C11 0.035(3) 0.102(5) 0.041(2) 0.032(3) -0.0031(19) 0.001(3) C12 0.074(4) 0.080(4) 0.046(2) 0.018(3) -0.006(2) -0.054(4) C30 0.0198(19) 0.0149(12) 0.0226(11) 0.0014(9) -0.0039(10) 0.0015(11) C31 0.0160(17) 0.0179(12) 0.0173(9) 0.0002(9) 0.0031(9) 0.0018(11) C32 0.0197(19) 0.0224(15) 0.0238(12) 0.0026(11) 0.0001(11) 0.0043(13) C33 0.022(2) 0.0330(18) 0.0268(13) 0.0044(13) -0.0002(12) 0.0114(15) C34 0.019(2) 0.0366(19) 0.0231(12) 0.0010(12) -0.0017(11) 0.0004(15) C35 0.0183(18) 0.0244(15) 0.0211(11) -0.0010(11) 0.0004(10) -0.0011(12) C50 0.023(2) 0.061(3) 0.0408(18) -0.029(2) -0.0026(15) 0.015(2) C51 0.021(2) 0.039(2) 0.0319(14) -0.0158(14) 0.0052(13) 0.0005(15) C52 0.024(2) 0.057(3) 0.0394(18) -0.0229(19) 0.0063(15) 0.004(2) C53 0.038(3) 0.045(2) 0.0334(16) -0.0195(16) 0.0197(16) -0.0098(18) C54 0.032(2) 0.0348(19) 0.0227(12) -0.0084(12) 0.0114(12) -0.0110(15) C55 0.0252(19) 0.0285(16) 0.0190(11) -0.0002(11) 0.0074(11) -0.0052(13) C60 0.0194(16) 0.0223(12) 0.0223(10) -0.0003(13) 0.0073(9) 0.0003(15) C61 0.0145(17) 0.0174(13) 0.0261(12) 0.0047(10) 0.0020(11) -0.0002(11) C62 0.0173(18) 0.0265(16) 0.0264(12) 0.0065(12) 0.0069(11) 0.0012(13) C63 0.015(2) 0.0253(16) 0.0372(15) 0.0066(13) 0.0014(13) -0.0016(13) C64 0.024(2) 0.0174(14) 0.0359(15) 0.0013(12) -0.0006(13) -0.0043(13) C65 0.0237(19) 0.0211(14) 0.0236(11) 0.0025(10) 0.0011(11) -0.0013(12) O1W 0.098(4) 0.076(4) 0.089(3) -0.012(3) 0.022(3) 0.006(3) P1 0.0236(5) 0.0320(5) 0.0224(3) 0.0065(3) -0.0014(3) -0.0098(4) F1 0.0316(16) 0.0592(19) 0.0705(18) 0.0460(16) 0.0043(13) 0.0062(13) F2 0.0267(15) 0.0496(16) 0.0437(12) 0.0222(11) -0.0015(9) -0.0150(12) F3 0.084(3) 0.083(3) 0.0284(11) -0.0096(13) -0.0054(12) -0.043(2) F4 0.0453(17) 0.0307(13) 0.0537(13) -0.0012(11) 0.0114(11) 0.0051(12) F5 0.0345(14) 0.0531(16) 0.0273(9) 0.0002(10) 0.0113(9) -0.0149(12) F6 0.0346(14) 0.0363(12) 0.0271(9) -0.0007(8) 0.0092(8) -0.0039(10) P2 0.0225(5) 0.0196(4) 0.0243(3) 0.0012(3) 0.0032(3) 0.0007(3) F7 0.0290(13) 0.0206(9) 0.0327(9) 0.0018(8) 0.0106(8) 0.0018(8) F8 0.096(3) 0.068(2) 0.0468(13) 0.0345(14) 0.0503(16) 0.0523(19) F9 0.0366(17) 0.0601(19) 0.0509(13) -0.0357(14) 0.0104(11) -0.0205(14) F10 0.0512(17) 0.0258(11) 0.0463(12) -0.0006(10) 0.0189(11) 0.0115(11) F11 0.0227(18) 0.0370(16) 0.149(3) -0.021(2) 0.0208(19) -0.0066(12) F12 0.090(2) 0.0356(14) 0.0230(9) 0.0048(9) 0.0029(11) 0.0211(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 O5 2.020(2) . ? Co N3 2.041(3) . ? Co N5 2.098(3) . ? Co N6 2.125(3) . ? Co O3 2.157(2) . ? Co O6 2.1846(19) . ? O1 C1 1.390(5) . ? O1 C10 1.433(7) . ? O2 C10 1.425(6) . ? O2 C2 1.431(4) . ? O3 C30 1.447(4) . ? O3 C3 1.448(3) . ? O4 C1 1.421(5) . ? O4 C4 1.442(4) . ? O5 C50 1.426(4) . ? O5 C5 1.439(3) . ? O6 C60 1.438(4) . ? O6 C6 1.450(4) . ? N3 C31 1.341(4) . ? N3 C35 1.354(4) . ? N5 C51 1.329(5) . ? N5 C55 1.352(4) . ? N6 C65 1.343(4) . ? N6 C61 1.348(4) . ? C1 C2 1.528(6) . ? C1 H1 0.9800 . ? C2 C3 1.523(5) . ? C2 H2 0.9800 . ? C3 C4 1.530(4) . ? C3 H3 0.9800 . ? C4 C5 1.515(5) . ? C4 H4 0.9800 . ? C5 C6 1.515(5) . ? C5 H5 0.9800 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C10 C11 1.509(5) . ? C10 C12 1.526(7) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C30 C31 1.493(5) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.396(4) . ? C32 C33 1.362(5) . ? C32 H32 0.9300 . ? C33 C34 1.390(6) . ? C33 H33 0.9300 . ? C34 C35 1.383(5) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C50 C51 1.511(5) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 C52 1.385(5) . ? C52 C53 1.380(6) . ? C52 H52 0.9300 . ? C53 C54 1.370(6) . ? C53 H53 0.9300 . ? C54 C55 1.381(5) . ? C54 H54 0.9300 . ? C55 H55 0.9300 . ? C60 C61 1.511(5) . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? C61 C62 1.376(5) . ? C62 C63 1.407(5) . ? C62 H62 0.9300 . ? C63 C64 1.385(5) . ? C63 H63 0.9300 . ? C64 C65 1.379(5) . ? C64 H64 0.9300 . ? C65 H65 0.9300 . ? P1 F3 1.583(3) . ? P1 F6 1.593(2) . ? P1 F5 1.596(2) . ? P1 F4 1.601(3) . ? P1 F1 1.604(3) . ? P1 F2 1.613(3) . ? P2 F11 1.587(3) . ? P2 F12 1.588(2) . ? P2 F8 1.591(2) . ? P2 F9 1.591(3) . ? P2 F7 1.602(2) . ? P2 F10 1.611(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Co N3 164.53(11) . . ? O5 Co N5 76.49(10) . . ? N3 Co N5 104.29(10) . . ? O5 Co N6 99.41(11) . . ? N3 Co N6 95.88(11) . . ? N5 Co N6 95.92(11) . . ? O5 Co O3 86.42(10) . . ? N3 Co O3 78.93(10) . . ? N5 Co O3 111.75(10) . . ? N6 Co O3 152.30(9) . . ? O5 Co O6 77.32(8) . . ? N3 Co O6 104.33(9) . . ? N5 Co O6 150.93(10) . . ? N6 Co O6 76.15(9) . . ? O3 Co O6 78.83(8) . . ? C1 O1 C10 109.1(3) . . ? C10 O2 C2 108.5(3) . . ? C30 O3 C3 112.0(2) . . ? C30 O3 Co 113.34(18) . . ? C3 O3 Co 124.09(17) . . ? C1 O4 C4 110.3(3) . . ? C50 O5 C5 120.9(3) . . ? C50 O5 Co 120.8(2) . . ? C5 O5 Co 113.99(19) . . ? C60 O6 C6 113.4(2) . . ? C60 O6 Co 108.86(16) . . ? C6 O6 Co 110.04(17) . . ? C31 N3 C35 118.8(3) . . ? C31 N3 Co 117.7(2) . . ? C35 N3 Co 123.5(2) . . ? C51 N5 C55 117.4(3) . . ? C51 N5 Co 116.7(2) . . ? C55 N5 Co 125.7(2) . . ? C65 N6 C61 117.4(3) . . ? C65 N6 Co 126.5(2) . . ? C61 N6 Co 116.1(2) . . ? O1 C1 O4 112.4(3) . . ? O1 C1 C2 105.7(3) . . ? O4 C1 C2 105.8(3) . . ? O1 C1 H1 110.9 . . ? O4 C1 H1 110.9 . . ? C2 C1 H1 110.9 . . ? O2 C2 C3 107.7(3) . . ? O2 C2 C1 101.9(3) . . ? C3 C2 C1 104.8(3) . . ? O2 C2 H2 113.8 . . ? C3 C2 H2 113.8 . . ? C1 C2 H2 113.8 . . ? O3 C3 C2 109.4(2) . . ? O3 C3 C4 112.9(2) . . ? C2 C3 C4 100.2(3) . . ? O3 C3 H3 111.3 . . ? C2 C3 H3 111.3 . . ? C4 C3 H3 111.3 . . ? O4 C4 C5 108.0(3) . . ? O4 C4 C3 105.0(2) . . ? C5 C4 C3 121.5(3) . . ? O4 C4 H4 107.2 . . ? C5 C4 H4 107.2 . . ? C3 C4 H4 107.2 . . ? O5 C5 C4 111.8(2) . . ? O5 C5 C6 104.2(3) . . ? C4 C5 C6 113.8(3) . . ? O5 C5 H5 108.9 . . ? C4 C5 H5 108.9 . . ? C6 C5 H5 108.9 . . ? O6 C6 C5 106.9(2) . . ? O6 C6 H6A 110.3 . . ? C5 C6 H6A 110.3 . . ? O6 C6 H6B 110.3 . . ? C5 C6 H6B 110.3 . . ? H6A C6 H6B 108.6 . . ? O2 C10 O1 106.7(3) . . ? O2 C10 C11 108.9(4) . . ? O1 C10 C11 109.8(5) . . ? O2 C10 C12 109.1(5) . . ? O1 C10 C12 109.5(4) . . ? C11 C10 C12 112.6(4) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O3 C30 C31 111.7(3) . . ? O3 C30 H30A 109.3 . . ? C31 C30 H30A 109.3 . . ? O3 C30 H30B 109.3 . . ? C31 C30 H30B 109.3 . . ? H30A C30 H30B 107.9 . . ? N3 C31 C32 121.7(3) . . ? N3 C31 C30 118.2(3) . . ? C32 C31 C30 120.1(3) . . ? C33 C32 C31 119.2(3) . . ? C33 C32 H32 120.4 . . ? C31 C32 H32 120.4 . . ? C32 C33 C34 119.7(3) . . ? C32 C33 H33 120.2 . . ? C34 C33 H33 120.2 . . ? C35 C34 C33 118.6(3) . . ? C35 C34 H34 120.7 . . ? C33 C34 H34 120.7 . . ? N3 C35 C34 122.0(3) . . ? N3 C35 H35 119.0 . . ? C34 C35 H35 119.0 . . ? O5 C50 C51 106.6(3) . . ? O5 C50 H50A 110.4 . . ? C51 C50 H50A 110.4 . . ? O5 C50 H50B 110.4 . . ? C51 C50 H50B 110.4 . . ? H50A C50 H50B 108.6 . . ? N5 C51 C52 123.5(3) . . ? N5 C51 C50 116.9(3) . . ? C52 C51 C50 119.5(4) . . ? C53 C52 C51 118.4(4) . . ? C53 C52 H52 120.8 . . ? C51 C52 H52 120.8 . . ? C54 C53 C52 118.9(3) . . ? C54 C53 H53 120.5 . . ? C52 C53 H53 120.5 . . ? C53 C54 C55 119.5(3) . . ? C53 C54 H54 120.3 . . ? C55 C54 H54 120.3 . . ? N5 C55 C54 122.2(3) . . ? N5 C55 H55 118.9 . . ? C54 C55 H55 118.9 . . ? O6 C60 C61 110.0(2) . . ? O6 C60 H60A 109.7 . . ? C61 C60 H60A 109.7 . . ? O6 C60 H60B 109.7 . . ? C61 C60 H60B 109.7 . . ? H60A C60 H60B 108.2 . . ? N6 C61 C62 123.2(3) . . ? N6 C61 C60 115.2(3) . . ? C62 C61 C60 121.5(3) . . ? C61 C62 C63 118.6(3) . . ? C61 C62 H62 120.7 . . ? C63 C62 H62 120.7 . . ? C64 C63 C62 118.4(3) . . ? C64 C63 H63 120.8 . . ? C62 C63 H63 120.8 . . ? C65 C64 C63 118.9(3) . . ? C65 C64 H64 120.5 . . ? C63 C64 H64 120.5 . . ? N6 C65 C64 123.5(3) . . ? N6 C65 H65 118.3 . . ? C64 C65 H65 118.3 . . ? F3 P1 F6 179.04(17) . . ? F3 P1 F5 91.11(16) . . ? F6 P1 F5 89.85(13) . . ? F3 P1 F4 90.5(2) . . ? F6 P1 F4 89.53(14) . . ? F5 P1 F4 91.24(16) . . ? F3 P1 F1 89.5(2) . . ? F6 P1 F1 90.50(17) . . ? F5 P1 F1 89.09(15) . . ? F4 P1 F1 179.67(17) . . ? F3 P1 F2 90.71(16) . . ? F6 P1 F2 88.33(14) . . ? F5 P1 F2 177.43(17) . . ? F4 P1 F2 90.56(15) . . ? F1 P1 F2 89.11(15) . . ? F11 P2 F12 90.1(2) . . ? F11 P2 F8 90.5(2) . . ? F12 P2 F8 179.3(2) . . ? F11 P2 F9 179.5(2) . . ? F12 P2 F9 89.37(18) . . ? F8 P2 F9 90.0(2) . . ? F11 P2 F7 89.45(15) . . ? F12 P2 F7 90.42(13) . . ? F8 P2 F7 89.94(13) . . ? F9 P2 F7 90.38(14) . . ? F11 P2 F10 90.29(16) . . ? F12 P2 F10 90.04(14) . . ? F8 P2 F10 89.60(14) . . ? F9 P2 F10 89.88(16) . . ? F7 P2 F10 179.47(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 Co O3 C30 -176.71(19) . . . . ? N3 Co O3 C30 -1.68(18) . . . . ? N5 Co O3 C30 -102.8(2) . . . . ? N6 Co O3 C30 79.8(3) . . . . ? O6 Co O3 C30 105.52(19) . . . . ? O5 Co O3 C3 41.6(2) . . . . ? N3 Co O3 C3 -143.3(2) . . . . ? N5 Co O3 C3 115.5(2) . . . . ? N6 Co O3 C3 -61.9(3) . . . . ? O6 Co O3 C3 -36.1(2) . . . . ? N3 Co O5 C50 83.0(5) . . . . ? N5 Co O5 C50 -11.8(3) . . . . ? N6 Co O5 C50 -105.6(3) . . . . ? O3 Co O5 C50 101.6(3) . . . . ? O6 Co O5 C50 -179.0(3) . . . . ? N3 Co O5 C5 -73.8(4) . . . . ? N5 Co O5 C5 -168.6(2) . . . . ? N6 Co O5 C5 97.5(2) . . . . ? O3 Co O5 C5 -55.3(2) . . . . ? O6 Co O5 C5 24.1(2) . . . . ? O5 Co O6 C60 133.4(2) . . . . ? N3 Co O6 C60 -62.4(2) . . . . ? N5 Co O6 C60 107.2(3) . . . . ? N6 Co O6 C60 30.2(2) . . . . ? O3 Co O6 C60 -137.8(2) . . . . ? O5 Co O6 C6 8.58(19) . . . . ? N3 Co O6 C6 172.76(19) . . . . ? N5 Co O6 C6 -17.6(3) . . . . ? N6 Co O6 C6 -94.6(2) . . . . ? O3 Co O6 C6 97.38(19) . . . . ? O5 Co N3 C31 18.7(5) . . . . ? N5 Co N3 C31 109.6(2) . . . . ? N6 Co N3 C31 -152.7(2) . . . . ? O3 Co N3 C31 -0.25(19) . . . . ? O6 Co N3 C31 -75.6(2) . . . . ? O5 Co N3 C35 -157.8(3) . . . . ? N5 Co N3 C35 -66.9(2) . . . . ? N6 Co N3 C35 30.8(2) . . . . ? O3 Co N3 C35 -176.8(2) . . . . ? O6 Co N3 C35 107.9(2) . . . . ? O5 Co N5 C51 2.1(3) . . . . ? N3 Co N5 C51 -162.0(3) . . . . ? N6 Co N5 C51 100.3(3) . . . . ? O3 Co N5 C51 -78.4(3) . . . . ? O6 Co N5 C51 28.3(4) . . . . ? O5 Co N5 C55 -173.1(3) . . . . ? N3 Co N5 C55 22.8(3) . . . . ? N6 Co N5 C55 -74.8(3) . . . . ? O3 Co N5 C55 106.4(3) . . . . ? O6 Co N5 C55 -146.8(3) . . . . ? O5 Co N6 C65 89.7(3) . . . . ? N3 Co N6 C65 -92.7(3) . . . . ? N5 Co N6 C65 12.4(3) . . . . ? O3 Co N6 C65 -170.0(2) . . . . ? O6 Co N6 C65 164.0(3) . . . . ? O5 Co N6 C61 -89.9(2) . . . . ? N3 Co N6 C61 87.7(2) . . . . ? N5 Co N6 C61 -167.2(2) . . . . ? O3 Co N6 C61 10.4(4) . . . . ? O6 Co N6 C61 -15.6(2) . . . . ? C10 O1 C1 O4 97.0(4) . . . . ? C10 O1 C1 C2 -18.0(4) . . . . ? C4 O4 C1 O1 -111.3(3) . . . . ? C4 O4 C1 C2 3.5(3) . . . . ? C10 O2 C2 C3 -136.6(3) . . . . ? C10 O2 C2 C1 -26.6(4) . . . . ? O1 C1 C2 O2 27.2(3) . . . . ? O4 C1 C2 O2 -92.2(3) . . . . ? O1 C1 C2 C3 139.4(3) . . . . ? O4 C1 C2 C3 20.0(3) . . . . ? C30 O3 C3 C2 68.5(3) . . . . ? Co O3 C3 C2 -149.4(2) . . . . ? C30 O3 C3 C4 179.2(2) . . . . ? Co O3 C3 C4 -38.7(3) . . . . ? O2 C2 C3 O3 -166.8(3) . . . . ? C1 C2 C3 O3 85.2(3) . . . . ? O2 C2 C3 C4 74.3(3) . . . . ? C1 C2 C3 C4 -33.7(3) . . . . ? C1 O4 C4 C5 -156.7(3) . . . . ? C1 O4 C4 C3 -25.6(3) . . . . ? O3 C3 C4 O4 -80.2(3) . . . . ? C2 C3 C4 O4 36.1(3) . . . . ? O3 C3 C4 C5 42.6(3) . . . . ? C2 C3 C4 C5 158.8(3) . . . . ? C50 O5 C5 C4 -83.9(4) . . . . ? Co O5 C5 C4 72.9(3) . . . . ? C50 O5 C5 C6 152.7(4) . . . . ? Co O5 C5 C6 -50.5(3) . . . . ? O4 C4 C5 O5 59.4(3) . . . . ? C3 C4 C5 O5 -61.9(3) . . . . ? O4 C4 C5 C6 177.2(2) . . . . ? C3 C4 C5 C6 55.9(3) . . . . ? C60 O6 C6 C5 -159.1(2) . . . . ? Co O6 C6 C5 -36.9(3) . . . . ? O5 C5 C6 O6 55.4(3) . . . . ? C4 C5 C6 O6 -66.7(3) . . . . ? C2 O2 C10 O1 16.9(4) . . . . ? C2 O2 C10 C11 135.4(5) . . . . ? C2 O2 C10 C12 -101.3(4) . . . . ? C1 O1 C10 O2 1.5(4) . . . . ? C1 O1 C10 C11 -116.3(4) . . . . ? C1 O1 C10 C12 119.5(4) . . . . ? C3 O3 C30 C31 149.5(2) . . . . ? Co O3 C30 C31 3.1(3) . . . . ? C35 N3 C31 C32 -1.7(4) . . . . ? Co N3 C31 C32 -178.3(2) . . . . ? C35 N3 C31 C30 178.8(3) . . . . ? Co N3 C31 C30 2.2(3) . . . . ? O3 C30 C31 N3 -3.5(4) . . . . ? O3 C30 C31 C32 177.0(2) . . . . ? N3 C31 C32 C33 1.8(4) . . . . ? C30 C31 C32 C33 -178.7(3) . . . . ? C31 C32 C33 C34 -1.0(5) . . . . ? C32 C33 C34 C35 0.3(5) . . . . ? C31 N3 C35 C34 0.9(4) . . . . ? Co N3 C35 C34 177.3(2) . . . . ? C33 C34 C35 N3 -0.2(5) . . . . ? C5 O5 C50 C51 172.8(3) . . . . ? Co O5 C50 C51 17.5(5) . . . . ? C55 N5 C51 C52 2.1(6) . . . . ? Co N5 C51 C52 -173.4(4) . . . . ? C55 N5 C51 C50 -177.5(4) . . . . ? Co N5 C51 C50 7.0(5) . . . . ? O5 C50 C51 N5 -15.0(6) . . . . ? O5 C50 C51 C52 165.4(4) . . . . ? N5 C51 C52 C53 0.0(7) . . . . ? C50 C51 C52 C53 179.6(5) . . . . ? C51 C52 C53 C54 -1.3(7) . . . . ? C52 C53 C54 C55 0.6(6) . . . . ? C51 N5 C55 C54 -2.9(5) . . . . ? Co N5 C55 C54 172.2(3) . . . . ? C53 C54 C55 N5 1.6(5) . . . . ? C6 O6 C60 C61 83.1(3) . . . . ? Co O6 C60 C61 -39.7(3) . . . . ? C65 N6 C61 C62 -0.5(5) . . . . ? Co N6 C61 C62 179.1(3) . . . . ? C65 N6 C61 C60 178.5(3) . . . . ? Co N6 C61 C60 -1.8(4) . . . . ? O6 C60 C61 N6 28.5(4) . . . . ? O6 C60 C61 C62 -152.4(3) . . . . ? N6 C61 C62 C63 1.1(5) . . . . ? C60 C61 C62 C63 -177.9(3) . . . . ? C61 C62 C63 C64 -1.1(5) . . . . ? C62 C63 C64 C65 0.5(5) . . . . ? C61 N6 C65 C64 -0.1(5) . . . . ? Co N6 C65 C64 -179.7(3) . . . . ? C63 C64 C65 N6 0.1(6) . . . . ? _diffrn_measured_fraction_theta_max 0.769 _diffrn_reflns_theta_full 36.43 _diffrn_measured_fraction_theta_full 0.769 _refine_diff_density_max 0.765 _refine_diff_density_min -0.604 _refine_diff_density_rms 0.082