# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_global #========================================================================== _audit_creation_method SHELXL-97 _audit_creation_date '9 November 2005' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H50 Co2 N6 O22 Tb2' _chemical_formula_weight 1234.42 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M p21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.3107(5) _cell_length_b 11.7100(5) _cell_length_c 15.4715(7) _cell_angle_alpha 90.00 _cell_angle_beta 102.871(2) _cell_angle_gamma 90.00 _cell_volume 1997.69(15) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 8596 _cell_measurement_theta_min 2.12 _cell_measurement_theta_max 30.12 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.052 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216 _exptl_absorpt_coefficient_mu 4.403 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.595 _exptl_absorpt_correction_T_max 0.644 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEX X8' _diffrn_measurement_method 'scans in phi and omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9293 _diffrn_reflns_av_R_equivalents 0.0295 _diffrn_reflns_av_sigmaI/netI 0.0346 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3372 _reflns_number_gt 3079 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex2 V2.0' _computing_cell_refinement 'Bruker Apex2 V2.0' _computing_data_reduction 'Bruker Apex2 V2.0' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-Seed _computing_publication_material CIFTAB _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 asymmetric unit contained half of the molecule, which lies upon a inversion centre. All the non-hydrogen atoms are refined anisotropically and all hydrogen atoms are placed in calculated positions, except for the H-atom of the hydroxide ligand which was found. ; _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^)+(0.0226P)^2^+1.1401P] 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_number_reflns 3372 _refine_ls_number_parameters 268 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0242 _refine_ls_R_factor_gt 0.0211 _refine_ls_wR_factor_ref 0.0526 _refine_ls_wR_factor_gt 0.0509 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.003 _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 Tb1 Tb 0.872103(13) 0.393530(11) 0.512886(9) 0.01315(7) Uani 1 1 d . . . Co2 Co 1.16262(4) 0.33378(3) 0.53461(3) 0.01136(10) Uani 1 1 d . . . O10 O 0.8009(2) 0.39808(18) 0.64765(16) 0.0227(6) Uani 1 1 d . . . O9 O 0.6604(2) 0.37809(19) 0.52840(16) 0.0229(5) Uani 1 1 d . . . O7 O 0.8231(2) 0.18981(18) 0.51947(15) 0.0233(5) Uani 1 1 d . . . O1 O 1.0447(2) 0.42066(17) 0.44799(14) 0.0128(5) Uani 1 1 d D . . O2 O 1.21755(19) 0.47515(16) 0.58703(13) 0.0143(5) Uani 1 1 d . . . O3 O 1.04255(19) 0.32759(17) 0.60135(13) 0.0146(5) Uani 1 1 d . . . O6 O 0.8020(2) 0.26615(19) 0.39039(15) 0.0261(6) Uani 1 1 d . . . O5 O 1.0993(2) 0.19446(17) 0.48221(14) 0.0147(5) Uani 1 1 d . . . O4 O 1.2789(2) 0.35027(17) 0.46542(14) 0.0161(5) Uani 1 1 d . . . O11 O 0.6123(2) 0.3814(2) 0.65604(18) 0.0317(6) Uani 1 1 d . . . O8 O 0.7580(3) 0.0868(2) 0.40271(19) 0.0339(7) Uani 1 1 d . . . N3 N 0.6878(3) 0.3855(2) 0.6118(2) 0.0202(7) Uani 1 1 d . . . N2 N 0.7931(3) 0.1771(2) 0.43736(19) 0.0210(6) Uani 1 1 d . . . C12 C 1.1243(3) 0.1529(3) 0.4120(2) 0.0155(7) Uani 1 1 d . . . C13 C 1.0570(3) 0.0457(3) 0.3790(2) 0.0208(7) Uani 1 1 d . . . H13A H 1.0881 -0.0164 0.4179 0.031 Uiso 1 1 calc R . . H13B H 1.0674 0.0290 0.3204 0.031 Uiso 1 1 calc R . . H13C H 0.9723 0.0559 0.3775 0.031 Uiso 1 1 calc R . . C10 C 1.2844(3) 0.2891(3) 0.3981(2) 0.0176(7) Uani 1 1 d . . . C11 C 1.2086(3) 0.1971(3) 0.3680(2) 0.0220(8) Uani 1 1 d . . . H11 H 1.2148 0.1629 0.3149 0.026 Uiso 1 1 calc R . . C9 C 1.3810(3) 0.3220(3) 0.3510(2) 0.0292(9) Uani 1 1 d . . . H9A H 1.3586 0.3918 0.3190 0.044 Uiso 1 1 calc R . . H9B H 1.3903 0.2627 0.3102 0.044 Uiso 1 1 calc R . . H9C H 1.4562 0.3327 0.3934 0.044 Uiso 1 1 calc R . . C3 C 1.0798(3) 0.2680(3) 0.6825(2) 0.0184(7) Uani 1 1 d . . . H3A H 1.0137 0.2211 0.6930 0.022 Uiso 1 1 calc R . . H3B H 1.1016 0.3220 0.7310 0.022 Uiso 1 1 calc R . . C4 C 1.1872(3) 0.1937(3) 0.6787(2) 0.0163(7) Uani 1 1 d . . . H4A H 1.2287 0.1716 0.7382 0.020 Uiso 1 1 calc R . . H4B H 1.1603 0.1250 0.6451 0.020 Uiso 1 1 calc R . . N1 N 1.2718(2) 0.2595(2) 0.63519(17) 0.0136(5) Uani 1 1 d . . . C5 C 1.3636(3) 0.1821(3) 0.6085(2) 0.0172(7) Uani 1 1 d . . . H5A H 1.4185 0.2284 0.5833 0.021 Uiso 1 1 calc R . . H5B H 1.3215 0.1311 0.5624 0.021 Uiso 1 1 calc R . . C2 C 1.3340(3) 0.3544(3) 0.6944(2) 0.0164(7) Uani 1 1 d . . . H2A H 1.2899 0.3709 0.7401 0.020 Uiso 1 1 calc R . . H2B H 1.4158 0.3318 0.7229 0.020 Uiso 1 1 calc R . . C1 C 1.3370(3) 0.4589(3) 0.6378(2) 0.0165(7) Uani 1 1 d . . . H1A H 1.3631 0.5251 0.6749 0.020 Uiso 1 1 calc R . . H1B H 1.3928 0.4476 0.5992 0.020 Uiso 1 1 calc R . . C6 C 1.4385(3) 0.1103(3) 0.6832(2) 0.0219(8) Uani 1 1 d . . . H6A H 1.3846 0.0667 0.7114 0.026 Uiso 1 1 calc R . . H6B H 1.4867 0.1601 0.7274 0.026 Uiso 1 1 calc R . . C7 C 1.5223(3) 0.0284(3) 0.6477(3) 0.0298(9) Uani 1 1 d . . . H7A H 1.5604 -0.0227 0.6952 0.036 Uiso 1 1 calc R . . H7B H 1.4737 -0.0177 0.6010 0.036 Uiso 1 1 calc R . . C8 C 1.6193(4) 0.0868(3) 0.6122(3) 0.0428(11) Uani 1 1 d . . . H8A H 1.5826 0.1355 0.5636 0.064 Uiso 1 1 calc R . . H8B H 1.6686 0.0306 0.5919 0.064 Uiso 1 1 calc R . . H8C H 1.6689 0.1319 0.6582 0.064 Uiso 1 1 calc R . . H1 H 1.046(4) 0.389(3) 0.3967(16) 0.051 Uiso 1 1 d 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 Tb1 0.01247(11) 0.01188(10) 0.01507(10) 0.00138(5) 0.00298(7) -0.00031(5) Co2 0.0122(2) 0.0104(2) 0.0120(2) -0.00045(16) 0.00373(18) 0.00028(16) O10 0.0159(15) 0.0302(14) 0.0219(13) -0.0011(10) 0.0038(12) -0.0033(10) O9 0.0197(15) 0.0262(13) 0.0228(14) 0.0044(10) 0.0050(11) -0.0003(10) O7 0.0286(15) 0.0179(12) 0.0228(13) 0.0035(10) 0.0042(11) -0.0023(10) O1 0.0131(13) 0.0125(10) 0.0127(11) -0.0016(8) 0.0023(10) 0.0008(8) O2 0.0146(13) 0.0110(10) 0.0166(11) -0.0016(8) 0.0019(10) -0.0002(8) O3 0.0147(12) 0.0153(11) 0.0150(11) 0.0018(8) 0.0062(10) 0.0007(9) O6 0.0401(16) 0.0183(12) 0.0194(12) 0.0001(10) 0.0055(11) -0.0061(10) O5 0.0153(12) 0.0126(11) 0.0170(12) -0.0002(8) 0.0053(10) 0.0007(9) O4 0.0170(13) 0.0155(11) 0.0173(11) -0.0002(9) 0.0068(10) -0.0008(9) O11 0.0248(16) 0.0400(16) 0.0360(16) 0.0074(12) 0.0191(14) 0.0047(11) O8 0.0377(18) 0.0200(13) 0.0453(17) -0.0114(12) 0.0119(14) -0.0120(11) N3 0.0182(19) 0.0196(15) 0.0256(17) 0.0058(12) 0.0110(15) 0.0015(11) N2 0.0200(17) 0.0159(14) 0.0276(17) -0.0020(12) 0.0068(14) -0.0026(11) C12 0.0146(18) 0.0129(15) 0.0161(16) 0.0013(12) -0.0029(14) 0.0071(12) C13 0.025(2) 0.0142(16) 0.0210(17) -0.0017(13) 0.0011(15) -0.0003(14) C10 0.0215(19) 0.0180(16) 0.0139(16) 0.0021(13) 0.0055(14) 0.0080(13) C11 0.032(2) 0.0211(17) 0.0152(17) -0.0044(13) 0.0094(16) 0.0020(15) C9 0.032(2) 0.033(2) 0.029(2) -0.0042(16) 0.0194(18) -0.0052(17) C3 0.0177(19) 0.0256(18) 0.0126(16) 0.0051(13) 0.0047(14) 0.0011(13) C4 0.0172(19) 0.0176(16) 0.0147(16) 0.0046(12) 0.0048(14) -0.0037(13) N1 0.0119(14) 0.0129(13) 0.0156(13) 0.0013(10) 0.0019(11) 0.0009(10) C5 0.0167(19) 0.0154(16) 0.0194(17) 0.0013(13) 0.0040(14) 0.0042(13) C2 0.0146(18) 0.0184(16) 0.0152(16) -0.0016(13) 0.0010(14) -0.0015(13) C1 0.0128(18) 0.0143(16) 0.0197(17) -0.0010(13) -0.0023(14) -0.0002(12) C6 0.020(2) 0.0198(18) 0.0237(19) 0.0047(13) 0.0010(16) 0.0037(13) C7 0.028(2) 0.0224(19) 0.039(2) 0.0095(16) 0.0064(18) 0.0086(15) C8 0.032(3) 0.036(2) 0.065(3) 0.009(2) 0.019(2) 0.0120(18) _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 Tb1 O3 2.238(2) . ? Tb1 O2 2.255(2) 3_766 ? Tb1 O1 2.394(2) 3_766 ? Tb1 O10 2.397(2) . ? Tb1 O6 2.403(2) . ? Tb1 O1 2.407(2) . ? Tb1 O7 2.456(2) . ? Tb1 O9 2.466(2) . ? Tb1 N3 2.849(3) . ? Tb1 N2 2.850(3) . ? Tb1 Co2 3.2806(4) 3_766 ? Tb1 Tb1 3.9066(3) 3_766 ? Co2 O4 1.881(2) . ? Co2 O3 1.8816(19) . ? Co2 O2 1.887(2) . ? Co2 O5 1.890(2) . ? Co2 O1 1.953(2) . ? Co2 N1 1.962(3) . ? Co2 Tb1 3.2806(4) 3_766 ? O10 N3 1.284(4) . ? O9 N3 1.262(4) . ? O7 N2 1.249(4) . ? O1 Tb1 2.394(2) 3_766 ? O1 H1 0.880(10) . ? O2 C1 1.416(4) . ? O2 Tb1 2.255(2) 3_766 ? O3 C3 1.416(4) . ? O6 N2 1.288(3) . ? O5 C12 1.278(4) . ? O4 C10 1.277(4) . ? O11 N3 1.209(4) . ? O8 N2 1.211(4) . ? C12 C11 1.389(4) . ? C12 C13 1.497(5) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C10 C11 1.391(5) . ? C10 C9 1.493(4) . ? C11 H11 0.9300 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C3 C4 1.506(4) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 N1 1.500(4) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? N1 C5 1.503(4) . ? N1 C2 1.511(4) . ? C5 C6 1.524(4) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C2 C1 1.509(4) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C6 C7 1.533(5) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.498(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Tb1 O2 148.10(7) . 3_766 ? O3 Tb1 O1 85.55(8) . 3_766 ? O2 Tb1 O1 69.21(7) 3_766 3_766 ? O3 Tb1 O10 83.47(8) . . ? O2 Tb1 O10 113.22(8) 3_766 . ? O1 Tb1 O10 87.09(7) 3_766 . ? O3 Tb1 O6 110.86(8) . . ? O2 Tb1 O6 82.16(8) 3_766 . ? O1 Tb1 O6 143.65(7) 3_766 . ? O10 Tb1 O6 125.72(8) . . ? O3 Tb1 O1 68.44(7) . . ? O2 Tb1 O1 84.64(7) 3_766 . ? O1 Tb1 O1 71.08(8) 3_766 . ? O10 Tb1 O1 145.16(8) . . ? O6 Tb1 O1 84.76(8) . . ? O3 Tb1 O7 79.13(8) . . ? O2 Tb1 O7 128.28(8) 3_766 . ? O1 Tb1 O7 162.12(8) 3_766 . ? O10 Tb1 O7 82.11(7) . . ? O6 Tb1 O7 52.56(8) . . ? O1 Tb1 O7 110.92(7) . . ? O3 Tb1 O9 129.64(7) . . ? O2 Tb1 O9 79.55(7) 3_766 . ? O1 Tb1 O9 112.19(7) 3_766 . ? O10 Tb1 O9 52.79(8) . . ? O6 Tb1 O9 82.78(8) . . ? O1 Tb1 O9 161.04(8) . . ? O7 Tb1 O9 72.04(8) . . ? O3 Tb1 N3 107.08(8) . . ? O2 Tb1 N3 96.87(8) 3_766 . ? O1 Tb1 N3 100.80(7) 3_766 . ? O10 Tb1 N3 26.59(9) . . ? O6 Tb1 N3 104.53(8) . . ? O1 Tb1 N3 170.70(8) . . ? O7 Tb1 N3 75.34(7) . . ? O9 Tb1 N3 26.21(9) . . ? O3 Tb1 N2 95.31(8) . . ? O2 Tb1 N2 105.86(8) 3_766 . ? O1 Tb1 N2 168.97(7) 3_766 . ? O10 Tb1 N2 103.94(8) . . ? O6 Tb1 N2 26.69(8) . . ? O1 Tb1 N2 98.96(7) . . ? O7 Tb1 N2 25.88(8) . . ? O9 Tb1 N2 75.64(8) . . ? N3 Tb1 N2 89.48(8) . . ? O3 Tb1 Co2 121.10(5) . 3_766 ? O2 Tb1 Co2 33.85(5) 3_766 3_766 ? O1 Tb1 Co2 36.18(5) 3_766 3_766 ? O10 Tb1 Co2 97.27(5) . 3_766 ? O6 Tb1 Co2 115.18(6) . 3_766 ? O1 Tb1 Co2 81.13(5) . 3_766 ? O7 Tb1 Co2 159.67(6) . 3_766 ? O9 Tb1 Co2 91.30(5) . 3_766 ? N3 Tb1 Co2 94.98(5) . 3_766 ? N2 Tb1 Co2 139.71(6) . 3_766 ? O3 Tb1 Tb1 74.10(5) . 3_766 ? O2 Tb1 Tb1 74.03(5) 3_766 3_766 ? O1 Tb1 Tb1 35.65(5) 3_766 3_766 ? O10 Tb1 Tb1 118.33(6) . 3_766 ? O6 Tb1 Tb1 115.94(5) . 3_766 ? O1 Tb1 Tb1 35.44(5) . 3_766 ? O7 Tb1 Tb1 143.45(6) . 3_766 ? O9 Tb1 Tb1 144.50(5) . 3_766 ? N3 Tb1 Tb1 136.29(6) . 3_766 ? N2 Tb1 Tb1 134.23(5) . 3_766 ? Co2 Tb1 Tb1 53.862(8) 3_766 3_766 ? O4 Co2 O3 176.02(9) . . ? O4 Co2 O2 87.11(9) . . ? O3 Co2 O2 90.38(9) . . ? O4 Co2 O5 95.21(9) . . ? O3 Co2 O5 87.20(9) . . ? O2 Co2 O5 177.01(9) . . ? O4 Co2 O1 90.76(9) . . ? O3 Co2 O1 86.01(9) . . ? O2 Co2 O1 86.97(9) . . ? O5 Co2 O1 91.12(9) . . ? O4 Co2 N1 95.77(10) . . ? O3 Co2 N1 87.22(10) . . ? O2 Co2 N1 87.67(10) . . ? O5 Co2 N1 93.96(10) . . ? O1 Co2 N1 171.33(9) . . ? O4 Co2 Tb1 80.60(6) . 3_766 ? O3 Co2 Tb1 95.48(6) . 3_766 ? O2 Co2 Tb1 41.74(6) . 3_766 ? O5 Co2 Tb1 136.79(7) . 3_766 ? O1 Co2 Tb1 46.36(6) . 3_766 ? N1 Co2 Tb1 129.22(8) . 3_766 ? N3 O10 Tb1 96.74(18) . . ? N3 O9 Tb1 94.13(19) . . ? N2 O7 Tb1 94.97(17) . . ? Co2 O1 Tb1 97.47(9) . 3_766 ? Co2 O1 Tb1 97.96(8) . . ? Tb1 O1 Tb1 108.92(8) 3_766 . ? Co2 O1 H1 104(3) . . ? Tb1 O1 H1 122(3) 3_766 . ? Tb1 O1 H1 120(3) . . ? C1 O2 Co2 107.62(17) . . ? C1 O2 Tb1 134.41(18) . 3_766 ? Co2 O2 Tb1 104.41(9) . 3_766 ? C3 O3 Co2 113.39(18) . . ? C3 O3 Tb1 139.26(18) . . ? Co2 O3 Tb1 106.24(9) . . ? N2 O6 Tb1 96.39(18) . . ? C12 O5 Co2 124.0(2) . . ? C10 O4 Co2 125.0(2) . . ? O11 N3 O9 122.2(3) . . ? O11 N3 O10 121.5(3) . . ? O9 N3 O10 116.3(3) . . ? O11 N3 Tb1 178.0(3) . . ? O9 N3 Tb1 59.67(15) . . ? O10 N3 Tb1 56.67(15) . . ? O8 N2 O7 122.9(3) . . ? O8 N2 O6 121.1(3) . . ? O7 N2 O6 116.1(3) . . ? O8 N2 Tb1 177.9(3) . . ? O7 N2 Tb1 59.16(15) . . ? O6 N2 Tb1 56.92(15) . . ? O5 C12 C11 125.5(3) . . ? O5 C12 C13 114.7(3) . . ? C11 C12 C13 119.8(3) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O4 C10 C11 124.7(3) . . ? O4 C10 C9 115.3(3) . . ? C11 C10 C9 120.0(3) . . ? C12 C11 C10 124.3(3) . . ? C12 C11 H11 117.8 . . ? C10 C11 H11 117.8 . . ? C10 C9 H9A 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C10 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O3 C3 C4 109.4(2) . . ? O3 C3 H3A 109.8 . . ? C4 C3 H3A 109.8 . . ? O3 C3 H3B 109.8 . . ? C4 C3 H3B 109.8 . . ? H3A C3 H3B 108.2 . . ? N1 C4 C3 108.8(2) . . ? N1 C4 H4A 109.9 . . ? C3 C4 H4A 109.9 . . ? N1 C4 H4B 109.9 . . ? C3 C4 H4B 109.9 . . ? H4A C4 H4B 108.3 . . ? C4 N1 C5 111.3(2) . . ? C4 N1 C2 111.3(2) . . ? C5 N1 C2 110.7(2) . . ? C4 N1 Co2 103.40(19) . . ? C5 N1 Co2 113.65(19) . . ? C2 N1 Co2 106.28(18) . . ? N1 C5 C6 115.2(3) . . ? N1 C5 H5A 108.5 . . ? C6 C5 H5A 108.5 . . ? N1 C5 H5B 108.5 . . ? C6 C5 H5B 108.5 . . ? H5A C5 H5B 107.5 . . ? C1 C2 N1 108.2(3) . . ? C1 C2 H2A 110.1 . . ? N1 C2 H2A 110.1 . . ? C1 C2 H2B 110.1 . . ? N1 C2 H2B 110.1 . . ? H2A C2 H2B 108.4 . . ? O2 C1 C2 106.8(2) . . ? O2 C1 H1A 110.4 . . ? C2 C1 H1A 110.4 . . ? O2 C1 H1B 110.4 . . ? C2 C1 H1B 110.4 . . ? H1A C1 H1B 108.6 . . ? C5 C6 C7 111.0(3) . . ? C5 C6 H6A 109.4 . . ? C7 C6 H6A 109.4 . . ? C5 C6 H6B 109.4 . . ? C7 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? C8 C7 C6 114.1(3) . . ? C8 C7 H7A 108.7 . . ? C6 C7 H7A 108.7 . . ? C8 C7 H7B 108.7 . . ? C6 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 0.576 _refine_diff_density_min -0.576 _refine_diff_density_rms 0.097 _database_code_depnum_ccdc_archive 'CCDC 941360' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_global #========================================================================== _audit_creation_method SHELXL-97 _audit_creation_date '9 November 2005' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H50 Co2 Dy2 N6 O22' _chemical_formula_weight 1241.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M p21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.310(2) _cell_length_b 11.725(2) _cell_length_c 15.497(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.90(3) _cell_angle_gamma 90.00 _cell_volume 2003.2(7) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 8643 _cell_measurement_theta_min 2.12 _cell_measurement_theta_max 28.12 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.058 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1220 _exptl_absorpt_coefficient_mu 4.591 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.346 _exptl_absorpt_correction_T_max 0.632 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'APEX X8' _diffrn_measurement_method 'scans in phi and omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 12647 _diffrn_reflns_av_R_equivalents 0.1015 _diffrn_reflns_av_sigmaI/netI 0.0843 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3472 _reflns_number_gt 3226 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex2 V2.0' _computing_cell_refinement 'Bruker Apex2 V2.0' _computing_data_reduction 'Bruker Apex2 V2.0' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-Seed _computing_publication_material CIFTAB _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 asymmetric unit contained half of the molecule, which lies upon a inversion centre. All the non-hydrogen atoms are refined anisotropically and all hydrogen atoms are placed in calculated positions, except for the H-atom of the hydroxide ligand which was found. The large residual electron denisity is found within 1.01 A of the Dy(III) ion. ; _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^)+(0.0876P)^2^+6.8514P] 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_number_reflns 3472 _refine_ls_number_parameters 268 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0639 _refine_ls_R_factor_gt 0.0608 _refine_ls_wR_factor_ref 0.1525 _refine_ls_wR_factor_gt 0.1487 _refine_ls_goodness_of_fit_ref 1.138 _refine_ls_restrained_S_all 1.138 _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 Dy1 Dy 0.62689(3) 0.39401(3) -0.01236(2) 0.01669(19) Uani 1 1 d . . . Co1 Co 0.66256(7) 0.66625(7) 0.03341(6) 0.0140(2) Uani 1 1 d . . . O1 O 0.5448(5) 0.5788(4) -0.0524(3) 0.0175(10) Uani 1 1 d . . . O2 O 0.5424(4) 0.6725(4) 0.1001(3) 0.0190(10) Uani 1 1 d . . . O3 O 0.7174(4) 0.5243(4) 0.0859(3) 0.0167(10) Uani 1 1 d . . . O4 O 0.5962(5) 0.8058(4) -0.0199(3) 0.0208(10) Uani 1 1 d . . . O5 O 0.7798(4) 0.6493(4) -0.0357(3) 0.0171(9) Uani 1 1 d . . . O6 O 0.6979(5) 0.3994(5) -0.1464(4) 0.0288(13) Uani 1 1 d . . . O7 O 0.8395(5) 0.3781(5) -0.0265(4) 0.0261(12) Uani 1 1 d . . . O8 O 0.8864(6) 0.3811(5) -0.1549(4) 0.0373(15) Uani 1 1 d . . . O9 O 0.6764(5) 0.1914(4) -0.0193(3) 0.0271(11) Uani 1 1 d . . . O10 O 0.6952(6) 0.2667(5) 0.1089(4) 0.0308(12) Uani 1 1 d . . . O11 O 0.7408(6) 0.0875(5) 0.0973(5) 0.0380(15) Uani 1 1 d . . . N1 N 0.7721(5) 0.7411(5) 0.1347(4) 0.0172(12) Uani 1 1 d . . . N2 N 0.8111(7) 0.3852(5) -0.1106(5) 0.0268(16) Uani 1 1 d . . . N3 N 0.7056(6) 0.1775(5) 0.0629(4) 0.0239(13) Uani 1 1 d . . . C1 C 0.5786(6) 0.7319(7) 0.1807(4) 0.0211(15) Uani 1 1 d . . . H1A H 0.6000 0.6769 0.2302 0.025 Uiso 1 1 calc R . . H1B H 0.5109 0.7799 0.1907 0.025 Uiso 1 1 calc R . . C2 C 0.6873(6) 0.8062(6) 0.1775(4) 0.0192(14) Uani 1 1 d . . . H2A H 0.6603 0.8764 0.1433 0.023 Uiso 1 1 calc R . . H2B H 0.7292 0.8285 0.2382 0.023 Uiso 1 1 calc R . . C3 C 0.8374(6) 0.5402(6) 0.1366(5) 0.0215(14) Uani 1 1 d . . . H3A H 0.8943 0.5518 0.0972 0.026 Uiso 1 1 calc R . . H3B H 0.8640 0.4728 0.1744 0.026 Uiso 1 1 calc R . . C4 C 0.8336(6) 0.6460(6) 0.1935(5) 0.0198(14) Uani 1 1 d . . . H4A H 0.7884 0.6291 0.2398 0.024 Uiso 1 1 calc R . . H4B H 0.9171 0.6690 0.2229 0.024 Uiso 1 1 calc R . . C5 C 0.8632(6) 0.8176(6) 0.1084(5) 0.0205(14) Uani 1 1 d . . . H5A H 0.8203 0.8689 0.0608 0.025 Uiso 1 1 calc R . . H5B H 0.9196 0.7701 0.0832 0.025 Uiso 1 1 calc R . . C6 C 0.9374(7) 0.8904(6) 0.1827(6) 0.0267(18) Uani 1 1 d . . . H6A H 0.9862 0.8402 0.2285 0.032 Uiso 1 1 calc R . . H6B H 0.8820 0.9354 0.2107 0.032 Uiso 1 1 calc R . . C7 C 1.0218(7) 0.9712(7) 0.1473(6) 0.0353(19) Uani 1 1 d . . . H7A H 0.9722 1.0185 0.0999 0.042 Uiso 1 1 calc R . . H7B H 1.0609 1.0231 0.1957 0.042 Uiso 1 1 calc R . . C8 C 1.1190(9) 0.9134(9) 0.1113(8) 0.045(2) Uani 1 1 d . . . H8A H 1.1612 0.8575 0.1545 0.067 Uiso 1 1 calc R . . H8B H 1.1772 0.9704 0.1002 0.067 Uiso 1 1 calc R . . H8C H 1.0823 0.8744 0.0559 0.067 Uiso 1 1 calc R . . C9 C 0.5569(7) 0.9553(6) -0.1214(5) 0.0243(15) Uani 1 1 d . . . H9A H 0.4702 0.9451 -0.1237 0.036 Uiso 1 1 calc R . . H9B H 0.5684 0.9731 -0.1808 0.036 Uiso 1 1 calc R . . H9C H 0.5884 1.0182 -0.0811 0.036 Uiso 1 1 calc R . . C10 C 0.6238(6) 0.8476(6) -0.0887(5) 0.0187(14) Uani 1 1 d . . . C11 C 0.7091(7) 0.8030(6) -0.1334(5) 0.0249(16) Uani 1 1 d . . . H11 H 0.7159 0.8378 -0.1874 0.030 Uiso 1 1 calc R . . C12 C 0.7844(6) 0.7103(6) -0.1026(4) 0.0192(14) Uani 1 1 d . . . C13 C 0.8805(8) 0.6785(8) -0.1508(6) 0.0346(19) Uani 1 1 d . . . H13A H 0.9601 0.6811 -0.1097 0.052 Uiso 1 1 calc R . . H13B H 0.8792 0.7323 -0.1993 0.052 Uiso 1 1 calc R . . H13C H 0.8653 0.6012 -0.1747 0.052 Uiso 1 1 calc R . . H5 H 0.526(12) 0.601(9) -0.097(8) 0.042 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.0131(3) 0.0146(3) 0.0204(3) -0.00115(10) -0.00045(16) 0.00016(10) Co1 0.0113(4) 0.0121(5) 0.0171(5) 0.0005(3) 0.0004(3) -0.0004(3) O1 0.021(2) 0.014(2) 0.017(2) 0.000(2) 0.002(2) -0.001(2) O2 0.015(2) 0.019(3) 0.022(2) -0.0037(19) 0.0019(19) -0.0012(18) O3 0.014(2) 0.014(3) 0.020(2) 0.0022(19) -0.0026(18) -0.0023(17) O4 0.017(2) 0.023(3) 0.021(2) 0.000(2) 0.0006(18) -0.002(2) O5 0.014(2) 0.016(2) 0.020(2) 0.0019(19) 0.0002(18) -0.0015(18) O6 0.022(3) 0.037(4) 0.027(3) 0.000(2) 0.005(2) 0.001(2) O7 0.019(3) 0.028(3) 0.029(3) -0.006(2) 0.001(2) -0.002(2) O8 0.030(3) 0.048(4) 0.037(3) -0.010(3) 0.014(3) -0.007(3) O9 0.030(3) 0.018(3) 0.031(3) -0.003(2) 0.001(2) 0.002(2) O10 0.043(3) 0.022(3) 0.027(3) 0.000(2) 0.006(2) 0.008(2) O11 0.044(4) 0.016(3) 0.052(4) 0.009(3) 0.007(3) 0.009(2) N1 0.013(3) 0.015(3) 0.021(3) 0.000(2) -0.002(2) 0.003(2) N2 0.024(4) 0.025(4) 0.034(4) -0.006(3) 0.012(3) -0.005(2) N3 0.021(3) 0.017(3) 0.032(3) 0.002(3) 0.003(3) -0.002(2) C1 0.017(3) 0.029(4) 0.016(3) -0.001(3) 0.003(3) 0.000(3) C2 0.023(3) 0.014(3) 0.019(3) -0.006(3) 0.002(3) 0.003(3) C3 0.016(3) 0.021(4) 0.025(3) -0.001(3) 0.000(3) -0.003(3) C4 0.019(3) 0.016(4) 0.021(3) 0.002(3) -0.004(3) 0.003(3) C5 0.013(3) 0.023(4) 0.023(3) 0.000(3) -0.002(3) -0.003(3) C6 0.017(4) 0.027(5) 0.033(4) -0.004(3) -0.003(3) -0.006(3) C7 0.027(4) 0.029(5) 0.049(5) -0.005(4) 0.006(4) -0.005(3) C8 0.030(5) 0.035(5) 0.068(7) -0.006(5) 0.009(5) -0.005(4) C9 0.024(3) 0.015(4) 0.029(4) 0.006(3) -0.006(3) 0.002(3) C10 0.015(3) 0.013(4) 0.024(3) -0.007(3) -0.005(3) -0.004(3) C11 0.031(4) 0.018(4) 0.026(4) 0.005(3) 0.007(3) -0.002(3) C12 0.018(3) 0.020(4) 0.019(3) 0.000(3) 0.001(3) -0.005(3) C13 0.038(5) 0.035(5) 0.035(4) 0.004(4) 0.016(4) 0.006(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O2 2.227(5) 3_665 ? Dy1 O3 2.237(5) . ? Dy1 O1 2.384(5) . ? Dy1 O6 2.389(6) . ? Dy1 O10 2.390(5) . ? Dy1 O1 2.399(5) 3_665 ? Dy1 O9 2.449(5) . ? Dy1 O7 2.469(5) . ? Co1 O2 1.884(5) . ? Co1 O5 1.892(5) . ? Co1 O3 1.895(5) . ? Co1 O4 1.909(5) . ? Co1 O1 1.950(5) . ? Co1 N1 1.975(6) . ? Co1 Dy1 3.2933(11) 3_665 ? O1 Dy1 2.399(5) 3_665 ? O1 H5 0.72(12) . ? O2 C1 1.407(8) . ? O2 Dy1 2.227(5) 3_665 ? O3 C3 1.421(8) . ? O4 C10 1.274(9) . ? O5 C12 1.271(8) . ? O6 N2 1.287(10) . ? O7 N2 1.274(10) . ? O8 N2 1.209(9) . ? O9 N3 1.253(8) . ? O10 N3 1.286(8) . ? O11 N3 1.208(9) . ? N1 C5 1.490(9) . ? N1 C2 1.491(8) . ? N1 C4 1.508(9) . ? C1 C2 1.517(10) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.528(10) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.527(10) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.531(11) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.501(13) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.501(10) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.408(10) . ? C11 C12 1.398(11) . ? C11 H11 0.9500 . ? C12 C13 1.497(10) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? 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 O2 Dy1 O3 148.78(17) 3_665 . ? O2 Dy1 O1 85.85(18) 3_665 . ? O3 Dy1 O1 69.44(17) . . ? O2 Dy1 O6 83.58(19) 3_665 . ? O3 Dy1 O6 112.46(18) . . ? O1 Dy1 O6 86.36(18) . . ? O2 Dy1 O10 110.2(2) 3_665 . ? O3 Dy1 O10 82.70(19) . . ? O1 Dy1 O10 144.23(18) . . ? O6 Dy1 O10 126.01(19) . . ? O2 Dy1 O1 68.68(17) 3_665 3_665 ? O3 Dy1 O1 85.09(17) . 3_665 ? O1 Dy1 O1 71.6(2) . 3_665 ? O6 Dy1 O1 145.21(19) . 3_665 ? O10 Dy1 O1 84.47(18) . 3_665 ? O2 Dy1 O9 78.89(18) 3_665 . ? O3 Dy1 O9 128.18(17) . . ? O1 Dy1 O9 161.77(18) . . ? O6 Dy1 O9 82.11(18) . . ? O10 Dy1 O9 52.52(18) . . ? O1 Dy1 O9 111.23(18) 3_665 . ? O2 Dy1 O7 129.83(17) 3_665 . ? O3 Dy1 O7 78.77(17) . . ? O1 Dy1 O7 112.07(18) . . ? O6 Dy1 O7 53.3(2) . . ? O10 Dy1 O7 82.7(2) . . ? O1 Dy1 O7 160.48(19) 3_665 . ? O9 Dy1 O7 71.69(18) . . ? O2 Co1 O5 176.0(2) . . ? O2 Co1 O3 90.3(2) . . ? O5 Co1 O3 87.0(2) . . ? O2 Co1 O4 86.7(2) . . ? O5 Co1 O4 95.9(2) . . ? O3 Co1 O4 176.1(2) . . ? O2 Co1 O1 85.9(2) . . ? O5 Co1 O1 90.9(2) . . ? O3 Co1 O1 86.5(2) . . ? O4 Co1 O1 90.8(2) . . ? O2 Co1 N1 87.0(2) . . ? O5 Co1 N1 95.9(2) . . ? O3 Co1 N1 87.8(2) . . ? O4 Co1 N1 94.5(2) . . ? O1 Co1 N1 170.9(2) . . ? O2 Co1 Dy1 40.51(15) . 3_665 ? O5 Co1 Dy1 136.73(14) . 3_665 ? O3 Co1 Dy1 94.41(14) . 3_665 ? O4 Co1 Dy1 81.67(15) . 3_665 ? O1 Co1 Dy1 46.17(15) . 3_665 ? N1 Co1 Dy1 127.38(16) . 3_665 ? Co1 O1 Dy1 97.7(2) . . ? Co1 O1 Dy1 97.9(2) . 3_665 ? Dy1 O1 Dy1 108.4(2) . 3_665 ? Co1 O1 H5 118(9) . . ? Dy1 O1 H5 127(8) . . ? Dy1 O1 H5 104(10) 3_665 . ? C1 O2 Co1 113.8(4) . . ? C1 O2 Dy1 139.0(4) . 3_665 ? Co1 O2 Dy1 106.1(2) . 3_665 ? C3 O3 Co1 107.6(4) . . ? C3 O3 Dy1 134.5(4) . . ? Co1 O3 Dy1 104.6(2) . . ? C10 O4 Co1 123.1(5) . . ? C12 O5 Co1 124.4(5) . . ? N2 O6 Dy1 96.7(4) . . ? N2 O7 Dy1 93.3(4) . . ? N3 O9 Dy1 95.3(4) . . ? N3 O10 Dy1 97.2(4) . . ? C5 N1 C2 111.5(6) . . ? C5 N1 C4 110.9(5) . . ? C2 N1 C4 111.5(5) . . ? C5 N1 Co1 113.5(4) . . ? C2 N1 Co1 103.3(4) . . ? C4 N1 Co1 105.9(4) . . ? O8 N2 O7 122.0(7) . . ? O8 N2 O6 121.3(7) . . ? O7 N2 O6 116.7(6) . . ? O11 N3 O9 123.2(7) . . ? O11 N3 O10 121.8(7) . . ? O9 N3 O10 115.0(6) . . ? O2 C1 C2 109.4(5) . . ? O2 C1 H1A 109.8 . . ? C2 C1 H1A 109.8 . . ? O2 C1 H1B 109.8 . . ? C2 C1 H1B 109.8 . . ? H1A C1 H1B 108.2 . . ? N1 C2 C1 109.1(6) . . ? N1 C2 H2A 109.9 . . ? C1 C2 H2A 109.9 . . ? N1 C2 H2B 109.9 . . ? C1 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? O3 C3 C4 106.2(6) . . ? O3 C3 H3A 110.5 . . ? C4 C3 H3A 110.5 . . ? O3 C3 H3B 110.5 . . ? C4 C3 H3B 110.5 . . ? H3A C3 H3B 108.7 . . ? N1 C4 C3 108.7(6) . . ? N1 C4 H4A 110.0 . . ? C3 C4 H4A 110.0 . . ? N1 C4 H4B 110.0 . . ? C3 C4 H4B 110.0 . . ? H4A C4 H4B 108.3 . . ? N1 C5 C6 115.3(6) . . ? N1 C5 H5A 108.5 . . ? C6 C5 H5A 108.5 . . ? N1 C5 H5B 108.5 . . ? C6 C5 H5B 108.5 . . ? H5A C5 H5B 107.5 . . ? C5 C6 C7 110.9(7) . . ? C5 C6 H6A 109.5 . . ? C7 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 108.0 . . ? C8 C7 C6 114.9(8) . . ? C8 C7 H7A 108.5 . . ? C6 C7 H7A 108.5 . . ? C8 C7 H7B 108.5 . . ? C6 C7 H7B 108.5 . . ? H7A C7 H7B 107.5 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 H9A 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C10 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O4 C10 C11 126.2(7) . . ? O4 C10 C9 114.0(6) . . ? C11 C10 C9 119.7(6) . . ? C12 C11 C10 123.6(7) . . ? C12 C11 H11 118.2 . . ? C10 C11 H11 118.2 . . ? O5 C12 C11 125.7(6) . . ? O5 C12 C13 115.7(6) . . ? C11 C12 C13 118.6(6) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 3.141 _refine_diff_density_min -3.057 _refine_diff_density_rms 0.325 _database_code_depnum_ccdc_archive 'CCDC 941361'