Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_lez04 _database_code_CSD 195120 _journal_coden_Cambridge 182 loop_ _publ_author_name _publ_author_address 'Mund, Garry' ; Department of Chemistry Simon Fraser University Burnaby, B.C. Canada V5A 1S6 ; 'Gabert, Andrea J.' ; Department of Chemistry Simon Fraser University Burnaby, B.C. Canada V5A 1S6 ; 'Batchelor, Raymond J. ' ; Department of Chemistry Simon Fraser University Burnaby, B.C. Canada V5A 1S6 ; 'Britten, James F. ' ; Department of Chemistry McMaster University Hamilton, Ont. Canada L8S 4M1 ; 'Leznoff, Daniel B.' ; Department of Chemistry Simon Fraser University Burnaby, B.C. Canada V5A 1S6 ; _publ_contact_author_name 'Prof Daniel Leznoff' _publ_contact_author_address ; Chemistry Simon Fraser University 8888 University Drive Burnaby British Columbia V5A 1S6 CANADA ; _publ_contact_author_phone 604-291-4887 _publ_contact_author_fax 604-291-3765 _publ_contact_author_email dleznoff@sfu.ca _publ_requested_journal 'Chemical Communications' _publ_section_title ; A rare ether-bridged cobalt complex which gives rise to an unusual 'serpentine' metal-ligand binding motif ; _publ_section_references ; Gabe, E.J., Le Page, Y., Charland,.J.-P., Lee, F.L. and White, P.S. (1989) J. Appl. Cryst., 22, 384-387. International Tables for X-ray Crystallography, Vol. IV, (1974) Kynoch Press, Birmingham, England. Johnson, C.K., (1976) ORTEP - A Fortran Thermal Ellipsoid Plot Program, Technical Report ORNL-5138, Oak Ridge National Lab., U.S.A. Le Page, Y., (1988) J. Appl. Cryst., 21, 983-984. Le Page, Y. and Gabe, E.J., (1979) J. Appl. Cryst., 12, 464-466. # SIR92 # Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 # CRYSTALS # Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W. (1996) CRYSTALS Issue 10. Chemical Crystallography Laboratory, OXFORD, UK. #ORTEP3 # Farrugia, L.J. (1997) J. Appl. Cryst. 30, 565. #CAMERON # Watkin, D.J., Prout, C.K. & Pearce, L.J. (1997) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H68 Co2 N4 O2 Si4' _chemical_formula_weight 915.24 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' 'Si' 'Si' 0.0817 0.0704 '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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.132(11) _cell_length_b 13.972(8) _cell_length_c 19.761(12) _cell_angle_alpha 90.00 _cell_angle_beta 107.854(10) _cell_angle_gamma 90.00 _cell_volume 4765(5) _cell_formula_units_Z 4 _cell_measurement_temperature 153.0(2) _cell_measurement_reflns_used 850 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 19.01 _exptl_crystal_description chunk _exptl_crystal_colour dark _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.276 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1944 _exptl_absorpt_coefficient_mu 0.835 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.52 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; The air sensitive sample consisted of several randomly oriented crystals fused together. 47 inaccurate measurements were removed from the refinement. ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _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 12941 _diffrn_reflns_av_R_equivalents 0.1680 _diffrn_reflns_av_sigmaI/netI 0.1582 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 22.50 _reflns_number_total 3068 _reflns_number_gt 1756 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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. The air sensitive sample consisted of several randomly oriented crystals fused together. 47 inaccurate measurements were removed from the refinement. ; _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^)+(0.0667P)^2^+48.3242P] 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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0015(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3068 _refine_ls_number_parameters 248 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1760 _refine_ls_R_factor_gt 0.0986 _refine_ls_wR_factor_ref 0.2095 _refine_ls_wR_factor_gt 0.1868 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _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 0.06016(7) 0.19016(9) 0.23319(8) 0.0320(6) Uani 1 1 d . . . Si1 Si 0.1952(2) 0.3199(3) 0.3152(2) 0.0593(12) Uani 1 1 d . . . Si2 Si 0.10609(16) 0.20886(19) 0.40270(18) 0.0357(9) Uani 1 1 d . . . O1 O 0.1508(5) 0.2919(6) 0.3738(4) 0.060(3) Uani 1 1 d . . . N1 N 0.1359(4) 0.2853(5) 0.2330(5) 0.0307(17) Uani 1 1 d . . . N2 N 0.0451(4) 0.1474(5) 0.3273(5) 0.0307(17) Uani 1 1 d . . . C10 C 0.1438(5) 0.3277(6) 0.1713(6) 0.030(3) Uani 1 1 d . . . C11 C 0.1023(6) 0.4095(7) 0.1438(7) 0.041(3) Uani 1 1 d . . . C12 C 0.1100(7) 0.4526(8) 0.0855(9) 0.063(4) Uani 1 1 d . . . H12A H 0.0831 0.5110 0.0704 0.075 Uiso 1 1 calc R . . C13 C 0.1560(8) 0.4153(9) 0.0455(8) 0.062(4) Uani 1 1 d . . . C14 C 0.1971(6) 0.3323(8) 0.0746(7) 0.051(4) Uani 1 1 d . . . H14A H 0.2312 0.3057 0.0514 0.061 Uiso 1 1 calc R . . C15 C 0.1913(6) 0.2872(7) 0.1339(7) 0.037(3) Uani 1 1 d . . . C16 C 0.2143(9) 0.4511(9) 0.3223(8) 0.093(6) Uani 1 1 d . . . H16A H 0.1649 0.4858 0.3100 0.139 Uiso 1 1 calc R . . H16B H 0.2429 0.4696 0.2896 0.139 Uiso 1 1 calc R . . H16C H 0.2450 0.4670 0.3711 0.139 Uiso 1 1 calc R . . C17 C 0.2922(7) 0.2562(11) 0.3399(9) 0.095(6) Uani 1 1 d . . . H17A H 0.2837 0.1869 0.3370 0.143 Uiso 1 1 calc R . . H17B H 0.3225 0.2736 0.3885 0.143 Uiso 1 1 calc R . . H17C H 0.3203 0.2753 0.3069 0.143 Uiso 1 1 calc R . . C20 C 0.0414(5) 0.0452(7) 0.3410(6) 0.033(3) Uani 1 1 d . . . C21 C 0.0913(5) -0.0197(7) 0.3200(6) 0.031(3) Uani 1 1 d . . . C22 C 0.0840(6) -0.1182(7) 0.3303(7) 0.045(3) Uani 1 1 d . . . H22A H 0.1175 -0.1608 0.3163 0.054 Uiso 1 1 calc R . . C23 C 0.0306(6) -0.1560(6) 0.3595(7) 0.041(3) Uani 1 1 d . . . C24 C -0.0162(6) -0.0922(7) 0.3820(7) 0.044(3) Uani 1 1 d . . . H24A H -0.0528 -0.1163 0.4033 0.053 Uiso 1 1 calc R . . C25 C -0.0103(6) 0.0065(7) 0.3739(6) 0.036(3) Uani 1 1 d . . . C26 C 0.0554(7) 0.2694(8) 0.4581(7) 0.061(4) Uani 1 1 d . . . H26A H 0.0174 0.3145 0.4288 0.091 Uiso 1 1 calc R . . H26B H 0.0930 0.3043 0.4965 0.091 Uiso 1 1 calc R . . H26C H 0.0287 0.2218 0.4785 0.091 Uiso 1 1 calc R . . C27 C 0.1765(6) 0.1256(8) 0.4611(7) 0.057(4) Uani 1 1 d . . . H27A H 0.2046 0.0916 0.4332 0.085 Uiso 1 1 calc R . . H27B H 0.1489 0.0793 0.4818 0.085 Uiso 1 1 calc R . . H27C H 0.2133 0.1617 0.4993 0.085 Uiso 1 1 calc R . . C111 C 0.0461(7) 0.4556(9) 0.1769(9) 0.080(5) Uani 1 1 d . . . H11A H 0.0233 0.5126 0.1495 0.120 Uiso 1 1 calc R . . H11B H 0.0737 0.4740 0.2260 0.120 Uiso 1 1 calc R . . H11C H 0.0050 0.4100 0.1766 0.120 Uiso 1 1 calc R . . C131 C 0.1608(9) 0.4600(11) -0.0235(8) 0.108(7) Uani 1 1 d . . . H13A H 0.1955 0.4218 -0.0422 0.161 Uiso 1 1 calc R . . H13B H 0.1809 0.5254 -0.0142 0.161 Uiso 1 1 calc R . . H13C H 0.1091 0.4615 -0.0585 0.161 Uiso 1 1 calc R . . C151 C 0.2378(6) 0.1988(8) 0.1603(8) 0.074(5) Uani 1 1 d . . . H15A H 0.2668 0.1815 0.1276 0.111 Uiso 1 1 calc R . . H15B H 0.2030 0.1463 0.1630 0.111 Uiso 1 1 calc R . . H15C H 0.2742 0.2109 0.2077 0.111 Uiso 1 1 calc R . . C211 C 0.1547(6) 0.0133(7) 0.2890(7) 0.044(3) Uani 1 1 d . . . H21A H 0.1811 -0.0428 0.2776 0.066 Uiso 1 1 calc R . . H21B H 0.1922 0.0530 0.3240 0.066 Uiso 1 1 calc R . . H21C H 0.1314 0.0506 0.2458 0.066 Uiso 1 1 calc R . . C231 C 0.0235(7) -0.2648(8) 0.3684(8) 0.070(5) Uani 1 1 d . . . H23A H -0.0175 -0.2777 0.3900 0.104 Uiso 1 1 calc R . . H23B H 0.0728 -0.2900 0.3992 0.104 Uiso 1 1 calc R . . H23C H 0.0106 -0.2958 0.3218 0.104 Uiso 1 1 calc R . . C251 C -0.0597(6) 0.0706(7) 0.4065(7) 0.047(3) Uani 1 1 d . . . H25A H -0.0919 0.0304 0.4268 0.070 Uiso 1 1 calc R . . H25B H -0.0931 0.1117 0.3694 0.070 Uiso 1 1 calc R . . H25C H -0.0256 0.1105 0.4439 0.070 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0143(7) 0.0173(7) 0.0636(12) -0.0003(8) 0.0108(7) -0.0076(6) Si1 0.058(2) 0.052(2) 0.065(3) -0.003(2) 0.015(2) -0.0397(19) Si2 0.0216(16) 0.0230(16) 0.059(2) 0.0025(16) 0.0073(16) -0.0026(12) O1 0.067(6) 0.056(5) 0.055(6) 0.004(5) 0.017(5) -0.043(4) N1 0.015(3) 0.015(3) 0.062(5) 0.007(3) 0.013(3) -0.004(2) N2 0.015(3) 0.015(3) 0.062(5) 0.007(3) 0.013(3) -0.004(2) C10 0.019(6) 0.004(5) 0.069(9) 0.001(5) 0.015(6) -0.007(4) C11 0.025(6) 0.025(6) 0.070(10) 0.014(7) 0.010(7) -0.004(5) C12 0.032(8) 0.029(7) 0.100(13) 0.003(8) -0.021(8) -0.001(6) C13 0.066(10) 0.039(8) 0.070(11) 0.019(8) 0.004(9) -0.034(7) C14 0.045(8) 0.048(8) 0.074(11) -0.026(8) 0.038(7) -0.029(6) C15 0.023(6) 0.018(6) 0.073(10) -0.002(6) 0.019(6) -0.006(4) C16 0.138(14) 0.050(9) 0.121(15) -0.040(9) 0.084(12) -0.070(9) C17 0.049(9) 0.100(12) 0.117(15) 0.019(10) -0.003(10) -0.039(8) C20 0.022(6) 0.024(6) 0.046(8) 0.009(6) 0.000(6) 0.014(5) C21 0.011(5) 0.028(6) 0.056(8) 0.004(6) 0.011(5) 0.000(4) C22 0.034(7) 0.022(6) 0.080(10) 0.009(6) 0.017(7) 0.015(5) C23 0.034(7) 0.012(5) 0.080(10) 0.012(6) 0.022(7) 0.001(5) C24 0.026(6) 0.040(7) 0.068(10) 0.017(7) 0.019(6) -0.001(5) C25 0.019(6) 0.024(6) 0.062(9) -0.002(6) 0.007(6) -0.008(4) C26 0.050(8) 0.050(8) 0.074(10) -0.016(7) 0.006(7) 0.019(6) C27 0.026(7) 0.049(7) 0.079(10) -0.018(7) -0.007(7) -0.007(6) C111 0.053(9) 0.046(8) 0.139(15) -0.009(9) 0.026(10) 0.014(7) C131 0.110(14) 0.107(13) 0.084(13) 0.019(10) -0.002(10) -0.083(11) C151 0.026(7) 0.043(7) 0.154(15) -0.013(9) 0.031(8) -0.002(6) C211 0.029(6) 0.026(6) 0.080(10) -0.010(6) 0.023(7) 0.005(5) C231 0.044(8) 0.033(7) 0.136(15) 0.015(8) 0.035(9) 0.000(6) C251 0.031(7) 0.036(6) 0.079(10) 0.000(7) 0.025(7) -0.003(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N1 1.912(7) . ? Co1 N2 2.007(8) 2 ? Co1 N2 2.050(9) . ? Co1 Co1 2.468(3) 2 ? Si1 O1 1.645(8) . ? Si1 N1 1.720(9) . ? Si1 C16 1.863(11) . ? Si1 C17 1.897(14) . ? Si2 O1 1.617(7) . ? Si2 N2 1.780(9) . ? Si2 C26 1.838(11) . ? Si2 C27 1.847(12) . ? N1 C10 1.401(12) . ? N2 C20 1.459(12) . ? N2 Co1 2.007(8) 2 ? C10 C11 1.385(14) . ? C10 C15 1.414(14) . ? C11 C12 1.344(17) . ? C11 C111 1.514(16) . ? C12 C13 1.413(18) . ? C13 C14 1.403(17) . ? C13 C131 1.527(18) . ? C14 C15 1.364(15) . ? C15 C151 1.496(15) . ? C20 C25 1.404(14) . ? C20 C21 1.428(13) . ? C21 C22 1.404(13) . ? C21 C211 1.529(13) . ? C22 C23 1.375(14) . ? C23 C24 1.394(14) . ? C23 C231 1.540(14) . ? C24 C25 1.395(13) . ? C25 C251 1.542(14) . ? 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 N1 Co1 N2 139.3(4) . 2 ? N1 Co1 N2 120.0(4) . . ? N2 Co1 N2 95.0(4) 2 . ? N1 Co1 Co1 134.0(2) . 2 ? N2 Co1 Co1 53.3(2) 2 2 ? N2 Co1 Co1 51.7(2) . 2 ? O1 Si1 N1 107.4(4) . . ? O1 Si1 C16 107.5(6) . . ? N1 Si1 C16 113.3(6) . . ? O1 Si1 C17 108.8(6) . . ? N1 Si1 C17 111.9(6) . . ? C16 Si1 C17 107.8(7) . . ? O1 Si2 N2 107.5(4) . . ? O1 Si2 C26 106.1(5) . . ? N2 Si2 C26 115.1(5) . . ? O1 Si2 C27 110.4(5) . . ? N2 Si2 C27 110.6(4) . . ? C26 Si2 C27 107.1(6) . . ? Si2 O1 Si1 145.6(6) . . ? C10 N1 Si1 120.1(6) . . ? C10 N1 Co1 124.1(6) . . ? Si1 N1 Co1 115.8(5) . . ? C20 N2 Si2 111.7(7) . . ? C20 N2 Co1 108.2(6) . 2 ? Si2 N2 Co1 126.1(4) . 2 ? C20 N2 Co1 118.6(7) . . ? Si2 N2 Co1 113.4(4) . . ? Co1 N2 Co1 74.9(3) 2 . ? C11 C10 N1 120.2(9) . . ? C11 C10 C15 118.0(10) . . ? N1 C10 C15 121.8(8) . . ? C12 C11 C10 121.4(11) . . ? C12 C11 C111 116.1(11) . . ? C10 C11 C111 122.5(12) . . ? C11 C12 C13 123.2(11) . . ? C14 C13 C12 114.0(12) . . ? C14 C13 C131 122.4(15) . . ? C12 C13 C131 123.6(14) . . ? C15 C14 C13 124.2(12) . . ? C14 C15 C10 119.1(9) . . ? C14 C15 C151 119.7(11) . . ? C10 C15 C151 121.1(11) . . ? C25 C20 C21 117.5(9) . . ? C25 C20 N2 122.5(9) . . ? C21 C20 N2 120.0(9) . . ? C22 C21 C20 119.0(9) . . ? C22 C21 C211 117.9(9) . . ? C20 C21 C211 123.1(9) . . ? C23 C22 C21 123.2(10) . . ? C22 C23 C24 117.6(9) . . ? C22 C23 C231 121.4(10) . . ? C24 C23 C231 120.9(10) . . ? C23 C24 C25 121.3(10) . . ? C24 C25 C20 121.3(10) . . ? C24 C25 C251 116.8(10) . . ? C20 C25 C251 121.8(9) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.619 _refine_diff_density_min -0.780 _refine_diff_density_rms 0.106 data_nonco _database_code_CSD 195025 _journal_coden_Cambridge 182 loop_ _publ_author_name _publ_author_address 'Mund, Garry' ; Department of Chemistry Simon Fraser University Burnaby, B.C. Canada V5A 1S6 ; 'Gabert, Andrea J.' ; Department of Chemistry Simon Fraser University Burnaby, B.C. Canada V5A 1S6 ; 'Batchelor, Raymond J. ' ; Department of Chemistry Simon Fraser University Burnaby, B.C. Canada V5A 1S6 ; 'Britten, James F. ' ; Department of Chemistry McMaster University Hamilton, Ont. Canada L8S 4M1 ; 'Leznoff, Daniel B.' ; Department of Chemistry Simon Fraser University Burnaby, B.C. Canada V5A 1S6 ; _publ_contact_author_name 'Prof Daniel Leznoff' _publ_contact_author_address ; Chemistry Simon Fraser University 8888 University Drive Burnaby British Columbia V5A 1S6 CANADA ; _publ_contact_author_phone 604-291-4887 _publ_contact_author_fax 604-291-3765 _publ_contact_author_email dleznoff@sfu.ca _publ_requested_journal 'Chemical Communications' _publ_section_title ; A rare ether-bridged cobalt complex which gives rise to an unusual 'serpentine' metal-ligand binding motif ; _publ_section_references ; Gabe, E.J., Le Page, Y., Charland,.J.-P., Lee, F.L. and White, P.S. (1989) J. Appl. Cryst., 22, 384-387. International Tables for X-ray Crystallography, Vol. IV, (1974) Kynoch Press, Birmingham, England. Johnson, C.K., (1976) ORTEP - A Fortran Thermal Ellipsoid Plot Program, Technical Report ORNL-5138, Oak Ridge National Lab., U.S.A. Le Page, Y., (1988) J. Appl. Cryst., 21, 983-984. Le Page, Y. and Gabe, E.J., (1979) J. Appl. Cryst., 12, 464-466. # SIR92 # Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 # CRYSTALS # Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W. (1996) CRYSTALS Issue 10. Chemical Crystallography Laboratory, OXFORD, UK. #ORTEP3 # Farrugia, L.J. (1997) J. Appl. Cryst. 30, 565. #CAMERON # Watkin, D.J., Prout, C.K. & Pearce, L.J. (1997) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; #========================================================================== #========================================================================== _chemical_name_systematic ; ? ; # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment constr #********************************************************************** # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al 2001) ; _computing_molecular_graphics ; ORTEP3 (Farrugia) ; #============================================================= _cell_length_a 10.899(2) _cell_angle_alpha 88.90(1) _cell_length_b 15.104(3) _cell_angle_beta 84.64(2) _cell_length_c 18.012(2) _cell_angle_gamma 69.22(2) _cell_volume 2759.8 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'Co ' 0.2990 0.9730 12.2841 4.2791 7.3409 0.2784 4.0034 13.5359 2.3488 71.1693 1.0118 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International_Tables_Vol_IV_Table_2.2B' 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C56 H84 Co2 N4 O2 ' _chemical_formula_moiety ' C56 H84 Co2 N4 O2 ' _chemical_compound_source ; ? ; _chemical_formula_weight 963.18 _cell_measurement_reflns_used 28 _cell_measurement_theta_min 12.00 _cell_measurement_theta_max 17.50 _cell_measurement_temperature 293 _cell_formula_units_Z 2 _exptl_crystal_description ? _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.30 _exptl_crystal_density_diffrn 1.159 _exptl_crystal_density_meas ? _exptl_crystal_F_000 1037.305 _exptl_absorpt_coefficient_mu 0.639 _diffrn_measurement_device_type ; Nonius CAD-4 ; _diffrn_radiation_monochromator graphite _computing_data_collection ; NRC DIFRAC ; _computing_data_reduction ; NRCVAX DATRD2 ; _computing_cell_refinement ; NRC DIFRAC ; _computing_structure_solution ; SIR92 (Altomare et al, 1994) ; _diffrn_measurement_method \w/2\q _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6370 _exptl_absorpt_correction_T_max 0.8442 _diffrn_standards_number 2 _diffrn_standards_interval_count 300 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 -3 2 0 1 5 _diffrn_reflns_number 10093 _diffrn_reflns_av_R_equivalents 0.039 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_reduction_process ? _diffrn_standards_decay_% 3. _diffrn_ambient_temperature 293 _reflns_number_total 9759 _reflns_number_observed 4528 _refine_diff_density_min -0.4(2) _refine_diff_density_max 0.5(2) _reflns_observed_criterion 'Inet > 2.5\s(Inet)' _refine_ls_number_reflns 4528 _refine_ls_number_parameters 581 _refine_ls_R_factor_obs 0.050 _refine_ls_wR_factor_obs 0.052 _refine_ls_goodness_of_fit_obs 2.2 _refine_ls_shift/esd_max 0.001 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ; w = 1/(.140E-01*F +0.00 *\s^2^(F ) + 0.00 ) ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.70930 # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 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_occupancy _atom_site_thermal_displace_type CO1 CO 0.95722(7) 0.28645(5) 0.25272(4) 0.0682 1.0000 Uani CO2 CO 0.99062(7) 0.03316(5) 0.24871(4) 0.0640 1.0000 Uani N1 N 1.1311(4) 0.2700(3) 0.2552(2) 0.0594 1.0000 Uani N2 N 0.7783(4) 0.3402(3) 0.2504(2) 0.0676 1.0000 Uani N3 N 0.9329(4) 0.0273(3) 0.1567(2) 0.0551 1.0000 Uani N4 N 1.0381(4) -0.0036(3) 0.3436(2) 0.0547 1.0000 Uani O1 O 0.8913(4) 0.1791(2) 0.3199(2) 0.0855 1.0000 Uani O2 O 1.0666(4) 0.1392(2) 0.1835(2) 0.0817 1.0000 Uani C1 C 1.2255(6) 0.1779(5) 0.2353(5) 0.1482 1.0000 Uani C2 C 1.2047(6) 0.1271(5) 0.1827(4) 0.1128 1.0000 Uani C3 C 1.0342(8) 0.1352(5) 0.1080(4) 0.1205 1.0000 Uani C4 C 0.9325(7) 0.1031(5) 0.1044(3) 0.1091 1.0000 Uani C5 C 1.0047(9) 0.0654(4) 0.4017(4) 0.1582 1.0000 Uani C6 C 0.9458(8) 0.1540(5) 0.3912(4) 0.1285 1.0000 Uani C7 C 0.7476(6) 0.2193(5) 0.3274(5) 0.1313 1.0000 Uani C8 C 0.6995(6) 0.2838(5) 0.2739(5) 0.1371 1.0000 Uani C10 C 1.1827(5) 0.3421(3) 0.2650(3) 0.0603 1.0000 Uani C11 C 1.1601(6) 0.4165(4) 0.2141(3) 0.0817 1.0000 Uani C12 C 1.2179(8) 0.4835(5) 0.2232(4) 0.1148 1.0000 Uani C13 C 1.2900(9) 0.4821(6) 0.2812(5) 0.1297 1.0000 Uani C14 C 1.3085(7) 0.4115(5) 0.3317(4) 0.1075 1.0000 Uani C15 C 1.2547(5) 0.3417(4) 0.3252(3) 0.0738 1.0000 Uani C20 C 0.7099(5) 0.4365(4) 0.2336(4) 0.0784 1.0000 Uani C21 C 0.6550(6) 0.4600(4) 0.1651(4) 0.0914 1.0000 Uani C22 C 0.5937(7) 0.5547(5) 0.1492(5) 0.1322 1.0000 Uani C23 C 0.5853(9) 0.6244(5) 0.1980(6) 0.1510 1.0000 Uani C24 C 0.6389(8) 0.6018(5) 0.2646(5) 0.1490 1.0000 Uani C25 C 0.7004(6) 0.5078(5) 0.2831(4) 0.1042 1.0000 Uani C30 C 0.9033(6) -0.0491(4) 0.1288(3) 0.0630 1.0000 Uani C31 C 0.9968(6) -0.1415(4) 0.1274(3) 0.0735 1.0000 Uani C32 C 0.9660(8) -0.2152(5) 0.1003(4) 0.1036 1.0000 Uani C33 C 0.845(1) -0.2001(6) 0.0758(4) 0.1245 1.0000 Uani C34 C 0.7509(8) -0.1105(6) 0.0796(4) 0.1080 1.0000 Uani C35 C 0.7766(6) -0.0346(5) 0.1060(3) 0.0790 1.0000 Uani C40 C 1.0830(5) -0.0991(4) 0.3664(3) 0.0614 1.0000 Uani C41 C 1.2129(6) -0.1425(4) 0.3844(3) 0.0779 1.0000 Uani C42 C 1.2548(8) -0.2364(5) 0.4074(4) 0.1135 1.0000 Uani C43 C 1.171(1) -0.2860(5) 0.4118(4) 0.1190 1.0000 Uani C44 C 1.0450(8) -0.2445(5) 0.3920(4) 0.1027 1.0000 Uani C45 C 0.9991(7) -0.1514(4) 0.3689(3) 0.0804 1.0000 Uani C110 C 1.0835(7) 0.4224(5) 0.1469(4) 0.1088 1.0000 Uani C111 C 0.9811(8) 0.5206(5) 0.1377(5) 0.1605 1.0000 Uani C112 C 1.1744(9) 0.3879(6) 0.0760(4) 0.1646 1.0000 Uani C150 C 1.2658(6) 0.2693(5) 0.3869(3) 0.0936 1.0000 Uani C151 C 1.1790(11) 0.3156(7) 0.4542(5) 0.2370 1.0000 Uani C152 C 1.4060(8) 0.2169(7) 0.4040(5) 0.1971 1.0000 Uani C210 C 0.6666(7) 0.3857(5) 0.1082(4) 0.1009 1.0000 Uani C211 C 0.7441(9) 0.3955(6) 0.0380(5) 0.1685 1.0000 Uani C212 C 0.5342(8) 0.3828(6) 0.0924(5) 0.1773 1.0000 Uani C250 C 0.754(1) 0.4851(5) 0.3591(5) 0.1421 1.0000 Uani C251 C 0.8573(9) 0.5298(7) 0.3694(5) 0.1901 1.0000 Uani C252 C 0.6472(11) 0.5134(8) 0.4225(5) 0.2123 1.0000 Uani C310 C 1.1325(6) -0.1614(4) 0.1537(3) 0.0830 1.0000 Uani C311 C 1.2290(6) -0.1489(4) 0.0925(4) 0.1090 1.0000 Uani C312 C 1.1916(7) -0.2578(4) 0.1889(4) 0.1088 1.0000 Uani C350 C 0.6667(6) 0.0597(5) 0.1185(4) 0.0928 1.0000 Uani C351 C 0.6065(6) 0.0702(5) 0.1982(4) 0.1285 1.0000 Uani C352 C 0.5595(7) 0.0813(5) 0.0649(4) 0.1338 1.0000 Uani C410 C 1.3099(6) -0.0928(4) 0.3740(4) 0.0929 1.0000 Uani C411 C 1.4117(7) -0.1180(6) 0.4316(4) 0.1543 1.0000 Uani C412 C 1.3794(7) -0.1101(5) 0.2965(4) 0.1263 1.0000 Uani C450 C 0.8583(8) -0.1086(5) 0.3484(4) 0.1043 1.0000 Uani C451 C 0.8123(7) -0.1758(5) 0.3070(4) 0.1392 1.0000 Uani C452 C 0.7631(7) -0.0665(6) 0.4138(5) 0.1666 1.0000 Uani H11 H 1.3065(6) 0.1862(5) 0.2202(5) 0.1750 1.0000 Uiso H12 H 1.2343(6) 0.1413(5) 0.2793(5) 0.1750 1.0000 Uiso H21 H 1.2333(6) 0.1461(5) 0.1356(4) 0.208(12) 1.0000 Uiso H22 H 1.2540(6) 0.0622(5) 0.1900(4) 0.208(12) 1.0000 Uiso H31 H 1.1097(8) 0.0939(5) 0.0792(4) 0.241(12) 1.0000 Uiso H32 H 1.0100(8) 0.1970(5) 0.0879(4) 0.241(12) 1.0000 Uiso H41 H 0.9369(7) 0.0798(5) 0.0553(3) 0.224(12) 1.0000 Uiso H42 H 0.8522(7) 0.1549(5) 0.1148(3) 0.224(12) 1.0000 Uiso H51 H 1.0851(9) 0.0597(4) 0.4213(4) 0.239(12) 1.0000 Uiso H52 H 0.9498(9) 0.0476(4) 0.4386(4) 0.239(12) 1.0000 Uiso H61 H 1.0075(8) 0.1846(5) 0.3953(4) 0.216(12) 1.0000 Uiso H62 H 0.8755(8) 0.1771(5) 0.4293(4) 0.216(12) 1.0000 Uiso H71 H 0.7187(6) 0.2495(5) 0.3749(5) 0.226(12) 1.0000 Uiso H72 H 0.7142(6) 0.1695(5) 0.3236(5) 0.226(12) 1.0000 Uiso H81 H 0.6148(6) 0.3256(5) 0.2927(5) 0.238(12) 1.0000 Uiso H82 H 0.6917(6) 0.2506(5) 0.2314(5) 0.238(12) 1.0000 Uiso H121 H 1.2067(8) 0.5322(5) 0.1875(4) 0.137(7) 1.0000 Uiso H131 H 1.3268(9) 0.5297(6) 0.2864(5) 0.160(7) 1.0000 Uiso H141 H 1.3592(7) 0.4100(5) 0.3721(4) 0.127(7) 1.0000 Uiso H221 H 0.5566(7) 0.5713(5) 0.1030(5) 0.127(7) 1.0000 Uiso H231 H 0.5422(9) 0.6888(5) 0.1858(6) 0.145(7) 1.0000 Uiso H241 H 0.6341(8) 0.6507(5) 0.2984(5) 0.148(7) 1.0000 Uiso H321 H 1.0298(8) -0.2775(5) 0.0986(4) 0.114(7) 1.0000 Uiso H331 H 0.826(1) -0.2513(6) 0.0562(4) 0.151(7) 1.0000 Uiso H341 H 0.6665(8) -0.1009(6) 0.0636(4) 0.125(7) 1.0000 Uiso H421 H 1.3426(8) -0.2663(5) 0.4200(4) 0.104(7) 1.0000 Uiso H431 H 1.200(1) -0.3495(5) 0.4288(4) 0.114(7) 1.0000 Uiso H441 H 0.9883(8) -0.2801(5) 0.3941(4) 0.107(7) 1.0000 Uiso H1101 H 1.0360(7) 0.3808(5) 0.1562(4) 0.125(7) 1.0000 Uiso H1111 H 0.9360(8) 0.5206(5) 0.0950(5) 0.195(5) 1.0000 Uiso H1112 H 1.0237(8) 0.5657(5) 0.1316(5) 0.195(5) 1.0000 Uiso H1113 H 0.9197(8) 0.5368(5) 0.1807(5) 0.195(5) 1.0000 Uiso H1121 H 1.1232(9) 0.3926(6) 0.0352(4) 0.198(5) 1.0000 Uiso H1122 H 1.2275(9) 0.4258(6) 0.0670(4) 0.198(5) 1.0000 Uiso H1123 H 1.2293(9) 0.3238(6) 0.0815(4) 0.198(5) 1.0000 Uiso H1501 H 1.2365(6) 0.2220(5) 0.3693(3) 0.096(7) 1.0000 Uiso H1511 H 1.1864(11) 0.2701(7) 0.4924(5) 0.251(5) 1.0000 Uiso H1512 H 1.2049(11) 0.3649(7) 0.4711(5) 0.251(5) 1.0000 Uiso H1513 H 1.0902(11) 0.3412(7) 0.4423(5) 0.251(5) 1.0000 Uiso H1521 H 1.4069(8) 0.1730(7) 0.4426(5) 0.238(5) 1.0000 Uiso H1522 H 1.4431(8) 0.2609(7) 0.4197(5) 0.238(5) 1.0000 Uiso H1523 H 1.4562(8) 0.1839(7) 0.3605(5) 0.238(5) 1.0000 Uiso H2101 H 0.7137(7) 0.3268(5) 0.1295(4) 0.097(7) 1.0000 Uiso H2111 H 0.7492(9) 0.3473(6) 0.0034(5) 0.196(5) 1.0000 Uiso H2112 H 0.8305(9) 0.3896(6) 0.0485(5) 0.196(5) 1.0000 Uiso H2113 H 0.7021(9) 0.4558(6) 0.0172(5) 0.196(5) 1.0000 Uiso H2121 H 0.5467(8) 0.3348(6) 0.0562(5) 0.209(5) 1.0000 Uiso H2122 H 0.4819(8) 0.4424(6) 0.0742(5) 0.209(5) 1.0000 Uiso H2123 H 0.4908(8) 0.3694(6) 0.1371(5) 0.209(5) 1.0000 Uiso H2501 H 0.796(1) 0.4182(5) 0.3602(5) 0.144(7) 1.0000 Uiso H2511 H 0.8888(9) 0.5144(7) 0.4172(5) 0.210(5) 1.0000 Uiso H2512 H 0.8185(9) 0.5967(7) 0.3656(5) 0.210(5) 1.0000 Uiso H2513 H 0.9286(9) 0.5062(7) 0.3319(5) 0.210(5) 1.0000 Uiso H2521 H 0.6852(11) 0.4980(8) 0.4685(5) 0.247(5) 1.0000 Uiso H2522 H 0.6002(11) 0.5797(8) 0.4211(5) 0.247(5) 1.0000 Uiso H2523 H 0.5883(11) 0.4805(8) 0.4177(5) 0.247(5) 1.0000 Uiso H3101 H 1.1176(6) -0.1152(4) 0.1919(3) 0.078(7) 1.0000 Uiso H3111 H 1.3123(6) -0.1620(4) 0.1112(4) 0.130(5) 1.0000 Uiso H3112 H 1.2380(6) -0.1913(4) 0.0524(4) 0.130(5) 1.0000 Uiso H3113 H 1.1976(6) -0.0856(4) 0.0754(4) 0.130(5) 1.0000 Uiso H3121 H 1.2759(7) -0.2650(4) 0.2039(4) 0.118(5) 1.0000 Uiso H3122 H 1.2003(7) -0.3061(4) 0.1537(4) 0.118(5) 1.0000 Uiso H3123 H 1.1355(7) -0.2626(4) 0.2313(4) 0.118(5) 1.0000 Uiso H3501 H 0.7074(6) 0.1053(5) 0.1082(4) 0.096(7) 1.0000 Uiso H3511 H 0.5375(6) 0.1301(5) 0.2050(4) 0.147(5) 1.0000 Uiso H3512 H 0.6721(6) 0.0659(5) 0.2307(4) 0.147(5) 1.0000 Uiso H3513 H 0.5721(6) 0.0213(5) 0.2090(4) 0.147(5) 1.0000 Uiso H3521 H 0.4945(7) 0.1418(5) 0.0767(4) 0.163(5) 1.0000 Uiso H3522 H 0.5975(7) 0.0810(5) 0.0152(4) 0.163(5) 1.0000 Uiso H3523 H 0.5198(7) 0.0344(5) 0.0694(4) 0.163(5) 1.0000 Uiso H4101 H 1.2590(6) -0.0275(4) 0.3813(4) 0.084(7) 1.0000 Uiso H4111 H 1.4696(7) -0.0839(6) 0.4215(4) 0.176(5) 1.0000 Uiso H4112 H 1.4609(7) -0.1840(6) 0.4289(4) 0.176(5) 1.0000 Uiso H4113 H 1.3676(7) -0.1016(6) 0.4802(4) 0.176(5) 1.0000 Uiso H4121 H 1.4404(7) -0.0780(5) 0.2910(4) 0.152(5) 1.0000 Uiso H4122 H 1.4251(7) -0.1762(5) 0.2886(4) 0.152(5) 1.0000 Uiso H4123 H 1.3165(7) -0.0872(5) 0.2610(4) 0.152(5) 1.0000 Uiso H4501 H 0.8600(8) -0.0597(5) 0.3148(4) 0.114(7) 1.0000 Uiso H4511 H 0.7238(7) -0.1441(5) 0.2961(4) 0.179(5) 1.0000 Uiso H4512 H 0.8174(7) -0.2290(5) 0.3371(4) 0.179(5) 1.0000 Uiso H4513 H 0.8671(7) -0.1962(5) 0.2618(4) 0.179(5) 1.0000 Uiso H4521 H 0.6766(7) -0.0407(6) 0.3983(5) 0.189(5) 1.0000 Uiso H4522 H 0.7850(7) -0.0177(6) 0.4352(5) 0.189(5) 1.0000 Uiso H4523 H 0.7667(7) -0.1141(6) 0.4496(5) 0.189(5) 1.0000 Uiso 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 0.0479(5) 0.0609(5) 0.0956(6) 0.0119(4) -0.0129(4) -0.0181(4) Co2 0.0795(6) 0.0679(5) 0.0498(4) 0.0123(3) -0.0203(4) -0.0296(4) N1 0.051(3) 0.053(2) 0.077(3) 0.004(2) -0.011(2) -0.020(2) N2 0.045(3) 0.059(3) 0.094(3) 0.016(2) -0.013(2) -0.011(2) N3 0.067(3) 0.059(2) 0.048(2) 0.009(2) -0.011(2) -0.033(2) N4 0.060(3) 0.056(2) 0.046(2) 0.005(2) -0.011(2) -0.016(2) O1 0.070(3) 0.074(2) 0.099(3) 0.024(2) -0.017(2) -0.008(2) O2 0.088(3) 0.089(3) 0.090(3) -0.000(2) -0.022(2) -0.055(2) C1 0.049(4) 0.111(6) 0.278(11) -0.094(6) -0.013(5) -0.015(4) C2 0.075(5) 0.098(5) 0.167(7) -0.039(5) -0.001(5) -0.033(4) C3 0.205(8) 0.138(6) 0.078(5) 0.038(4) -0.048(5) -0.127(6) C4 0.160(7) 0.145(6) 0.075(4) 0.052(4) -0.057(4) -0.111(5) C5 0.27(1) 0.065(4) 0.084(5) -0.016(4) -0.080(6) 0.028(5) C6 0.198(8) 0.084(5) 0.078(5) -0.004(4) -0.049(5) -0.010(5) C7 0.066(5) 0.131(6) 0.188(8) 0.067(6) -0.002(5) -0.030(4) C8 0.058(4) 0.137(6) 0.219(9) 0.103(6) -0.033(5) -0.037(4) C10 0.061(3) 0.064(3) 0.063(4) -0.006(3) -0.003(3) -0.033(3) C11 0.098(5) 0.079(4) 0.087(4) 0.012(3) -0.018(4) -0.052(4) C12 0.165(7) 0.099(5) 0.119(6) 0.024(4) -0.028(5) -0.091(5) C13 0.190(9) 0.124(6) 0.125(7) -0.013(5) -0.021(6) -0.114(6) C14 0.128(6) 0.138(6) 0.091(5) -0.015(5) -0.021(4) -0.085(5) C15 0.080(4) 0.093(4) 0.061(4) -0.007(3) -0.003(3) -0.046(3) C20 0.051(3) 0.058(4) 0.110(5) 0.003(4) -0.006(3) 0.000(3) C21 0.071(4) 0.067(4) 0.114(5) 0.019(4) -0.020(4) 0.004(3) C22 0.126(6) 0.090(5) 0.140(7) 0.019(5) -0.047(5) 0.019(5) C23 0.160(8) 0.071(5) 0.172(9) 0.015(6) -0.041(7) 0.027(5) C24 0.163(8) 0.070(5) 0.175(9) -0.022(5) -0.047(7) 0.015(5) C25 0.102(5) 0.072(5) 0.119(6) -0.006(4) -0.034(5) -0.001(4) C30 0.077(4) 0.082(4) 0.043(3) -0.000(3) -0.003(3) -0.045(3) C31 0.097(5) 0.070(4) 0.060(4) -0.003(3) -0.004(3) -0.039(4) C32 0.141(7) 0.081(5) 0.101(5) -0.015(4) -0.001(5) -0.057(5) C33 0.167(9) 0.129(7) 0.121(6) -0.033(5) -0.001(6) -0.107(7) C34 0.115(6) 0.140(6) 0.097(5) -0.017(5) -0.006(4) -0.080(6) C35 0.081(5) 0.110(5) 0.067(4) -0.009(3) -0.008(3) -0.059(4) C40 0.069(4) 0.064(3) 0.042(3) 0.010(2) -0.000(3) -0.015(3) C41 0.073(4) 0.076(4) 0.070(4) 0.019(3) -0.009(3) -0.008(3) C42 0.096(6) 0.100(6) 0.104(5) 0.032(4) -0.003(4) 0.012(5) C43 0.149(8) 0.069(5) 0.106(6) 0.032(4) 0.011(6) -0.005(5) C44 0.128(6) 0.089(5) 0.091(5) 0.023(4) 0.014(5) -0.044(5) C45 0.091(5) 0.072(4) 0.074(4) 0.021(3) 0.001(4) -0.026(4) C110 0.137(6) 0.106(5) 0.120(6) 0.053(5) -0.056(5) -0.079(5) C111 0.164(8) 0.144(7) 0.191(9) 0.088(6) -0.075(7) -0.067(6) C112 0.22(1) 0.185(9) 0.105(7) 0.016(6) -0.061(7) -0.078(8) C150 0.089(5) 0.128(5) 0.074(4) 0.010(4) -0.014(4) -0.048(4) C151 0.299(14) 0.237(11) 0.106(7) 0.032(7) 0.084(8) -0.04(1) C152 0.122(7) 0.318(13) 0.168(8) 0.129(9) -0.076(6) -0.089(8) C210 0.099(5) 0.090(5) 0.103(6) 0.021(4) -0.033(5) -0.015(4) C211 0.20(1) 0.168(8) 0.131(8) -0.015(6) 0.013(7) -0.070(7) C212 0.133(8) 0.21(1) 0.187(9) -0.008(7) -0.048(7) -0.058(7) C250 0.174(9) 0.086(5) 0.149(8) -0.031(5) -0.048(8) -0.015(5) C251 0.176(9) 0.20(1) 0.164(9) -0.054(7) -0.060(8) -0.013(8) C252 0.242(13) 0.251(12) 0.136(8) 0.001(8) -0.031(9) -0.07(1) C310 0.107(5) 0.058(4) 0.079(4) -0.003(3) -0.015(4) -0.022(3) C311 0.097(5) 0.125(6) 0.115(6) 0.028(4) -0.017(5) -0.051(4) C312 0.126(6) 0.079(4) 0.103(5) 0.008(4) 0.003(4) -0.018(4) C350 0.070(4) 0.131(6) 0.089(5) -0.003(4) -0.006(4) -0.049(4) C351 0.085(5) 0.181(7) 0.112(6) -0.006(5) -0.001(5) -0.040(5) C352 0.101(5) 0.188(8) 0.130(6) 0.024(5) -0.043(5) -0.066(5) C410 0.069(4) 0.094(5) 0.096(5) 0.003(4) -0.022(4) -0.002(4) C411 0.098(5) 0.24(1) 0.116(6) 0.018(6) -0.046(5) -0.038(6) C412 0.116(6) 0.168(7) 0.108(6) 0.015(5) -0.007(5) -0.069(5) C450 0.108(6) 0.108(5) 0.118(6) 0.037(5) -0.010(5) -0.066(5) C451 0.144(7) 0.185(8) 0.130(6) 0.020(6) -0.007(5) -0.111(6) C452 0.098(6) 0.169(8) 0.217(11) -0.032(7) -0.003(7) -0.029(6) _refine_ls_extinction_method 'None' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Co1 . Co2 . 3.716(1) yes Co1 . N1 . 1.827(4) yes Co1 . N2 . 1.832(4) yes Co1 . O1 . 2.279(4) yes Co1 . O2 . 2.423(4) yes Co2 . O1 . 2.415(4) yes Co2 . O2 . 2.306(4) yes Co2 . N3 . 1.841(4) yes Co2 . N4 . 1.850(4) yes N1 . C1 . 1.434(6) yes N1 . C10 . 1.410(5) yes N2 . C8 . 1.441(7) yes N2 . C20 . 1.421(6) yes N3 . C4 . 1.467(6) yes N3 . C30 . 1.417(6) yes N4 . C5 . 1.420(6) yes N4 . C40 . 1.416(5) yes O1 . C6 . 1.453(6) yes O1 . C7 . 1.459(7) yes O2 . C2 . 1.449(6) yes O2 . C3 . 1.445(6) yes C1 . C2 . 1.315(8) yes C3 . C4 . 1.366(8) yes C5 . C6 . 1.281(7) yes C7 . C8 . 1.358(8) yes C10 . C11 . 1.405(7) yes C10 . C15 . 1.396(7) yes C11 . C12 . 1.387(8) yes C11 . C110 . 1.516(8) yes C12 . C13 . 1.360(9) yes C13 . C14 . 1.359(9) yes C14 . C15 . 1.388(8) yes C15 . C150 . 1.525(7) yes C20 . C21 . 1.406(8) yes C20 . C25 . 1.379(7) yes C21 . C22 . 1.383(8) yes C21 . C210 . 1.498(8) yes C22 . C23 . 1.356(9) yes C23 . C24 . 1.37(1) yes C24 . C25 . 1.388(8) yes C25 . C250 . 1.52(1) yes C30 . C31 . 1.404(7) yes C30 . C35 . 1.418(7) yes C31 . C32 . 1.382(7) yes C31 . C310 . 1.521(7) yes C32 . C33 . 1.367(9) yes C33 . C34 . 1.377(9) yes C34 . C35 . 1.375(8) yes C35 . C350 . 1.506(8) yes C40 . C41 . 1.399(7) yes C40 . C45 . 1.402(7) yes C41 . C42 . 1.394(8) yes C41 . C410 . 1.495(8) yes C42 . C43 . 1.372(9) yes C43 . C44 . 1.366(9) yes C44 . C45 . 1.385(8) yes C45 . C450 . 1.518(8) yes C110 . C111 . 1.525(9) yes C110 . C112 . 1.518(9) yes C150 . C151 . 1.484(9) yes C150 . C152 . 1.509(9) yes C210 . C211 . 1.490(9) yes C210 . C212 . 1.513(9) yes C250 . C251 . 1.528(11) yes C250 . C252 . 1.505(11) yes C310 . C311 . 1.508(8) yes C310 . C312 . 1.521(7) yes C350 . C351 . 1.508(8) yes C350 . C352 . 1.528(8) yes C410 . C411 . 1.535(7) yes C410 . C412 . 1.505(8) yes C450 . C451 . 1.515(8) yes C450 . C452 . 1.483(9) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 . Co1 . O2 . 76.08(13) yes N1 . Co1 . N2 . 162.83(17) yes N1 . Co1 . O1 . 114.52(15) yes N1 . Co1 . O2 . 77.70(15) yes N2 . Co1 . O1 . 79.61(16) yes N3 . Co2 . N4 . 158.42(16) yes Co1 . N1 . C1 . 117.1(3) yes Co1 . N1 . C10 . 126.1(3) yes C1 . N1 . C10 . 116.2(4) yes Co1 . N2 . C8 . 118.0(3) yes Co1 . N2 . C20 . 124.5(3) yes C8 . N2 . C20 . 117.2(4) yes Co2 . N3 . C4 . 117.1(3) yes Co2 . N3 . C30 . 125.7(3) yes C4 . N3 . C30 . 116.8(4) yes Co2 . N4 . C5 . 119.7(3) yes Co2 . N4 . C40 . 123.4(3) yes C5 . N4 . C40 . 115.7(4) yes Co1 . O1 . C6 . 115.6(4) yes Co1 . O1 . C7 . 105.3(3) yes C6 . O1 . C7 . 112.6(5) yes C2 . O2 . C3 . 109.4(5) yes N1 . C1 . C2 . 120.4(6) yes O2 . C2 . C1 . 111.9(6) yes O2 . C3 . C4 . 112.3(5) yes N3 . C4 . C3 . 114.6(5) yes N4 . C5 . C6 . 122.8(6) yes O1 . C6 . C5 . 116.1(5) yes O1 . C7 . C8 . 112.3(6) yes N2 . C8 . C7 . 115.6(6) yes N1 . C10 . C11 . 119.8(5) yes N1 . C10 . C15 . 121.2(5) yes C11 . C10 . C15 . 119.0(5) yes C10 . C11 . C12 . 118.2(6) yes C10 . C11 . C110 . 122.5(5) yes C12 . C11 . C110 . 119.1(6) yes C11 . C12 . C13 . 122.6(7) yes C12 . C13 . C14 . 119.0(6) yes C13 . C14 . C15 . 121.2(6) yes C10 . C15 . C14 . 119.8(6) yes C10 . C15 . C150 . 120.2(5) yes C14 . C15 . C150 . 119.8(6) yes N2 . C20 . C21 . 120.0(5) yes N2 . C20 . C25 . 120.5(6) yes C21 . C20 . C25 . 119.5(5) yes C20 . C21 . C22 . 118.6(7) yes C20 . C21 . C210 . 121.7(5) yes C22 . C21 . C210 . 119.7(7) yes C21 . C22 . C23 . 121.7(7) yes C22 . C23 . C24 . 120.0(7) yes C23 . C24 . C25 . 120.3(7) yes C20 . C25 . C24 . 120.1(7) yes C20 . C25 . C250 . 121.0(6) yes C24 . C25 . C250 . 118.9(7) yes N3 . C30 . C31 . 120.3(5) yes N3 . C30 . C35 . 120.6(5) yes C31 . C30 . C35 . 119.0(5) yes C30 . C31 . C32 . 119.4(6) yes C30 . C31 . C310 . 121.1(5) yes C32 . C31 . C310 . 119.4(6) yes C31 . C32 . C33 . 121.1(7) yes C32 . C33 . C34 . 120.0(7) yes C33 . C34 . C35 . 121.2(7) yes C30 . C35 . C34 . 119.2(6) yes C30 . C35 . C350 . 120.7(5) yes C34 . C35 . C350 . 119.8(6) yes N4 . C40 . C41 . 119.9(5) yes N4 . C40 . C45 . 120.3(5) yes C41 . C40 . C45 . 119.8(5) yes C40 . C41 . C42 . 119.0(6) yes C40 . C41 . C410 . 121.4(5) yes C42 . C41 . C410 . 119.5(6) yes C41 . C42 . C43 . 120.8(7) yes C42 . C43 . C44 . 120.2(7) yes C43 . C44 . C45 . 121.1(7) yes C40 . C45 . C44 . 119.2(6) yes C40 . C45 . C450 . 122.0(5) yes C44 . C45 . C450 . 118.8(6) yes C11 . C110 . C111 . 112.8(6) yes C11 . C110 . C112 . 111.8(6) yes C111 . C110 . C112 . 111.7(6) yes C15 . C150 . C151 . 109.9(6) yes C15 . C150 . C152 . 113.2(6) yes C151 . C150 . C152 . 112.2(7) yes C21 . C210 . C211 . 112.0(6) yes C21 . C210 . C212 . 112.7(6) yes C211 . C210 . C212 . 111.0(7) yes C25 . C250 . C251 . 111.6(8) yes C25 . C250 . C252 . 112.5(8) yes C251 . C250 . C252 . 110.4(7) yes C31 . C310 . C311 . 112.2(5) yes C31 . C310 . C312 . 114.5(5) yes C311 . C310 . C312 . 109.6(5) yes C35 . C350 . C351 . 110.7(6) yes C35 . C350 . C352 . 115.1(5) yes C351 . C350 . C352 . 110.4(5) yes C41 . C410 . C411 . 114.3(6) yes C41 . C410 . C412 . 110.8(5) yes C411 . C410 . C412 . 109.7(5) yes C45 . C450 . C451 . 114.4(6) yes C45 . C450 . C452 . 112.5(6) yes C451 . C450 . C452 . 109.8(6) yes